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Modeling and Simulation of NOx Absorption in
Pilot-Scale Packed Columns

Article in AIChE Journal · March 1991
DOI: 10.1002/aic.690370303

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Jo~hi. the third was 800 mm ID and 3 m tall. Joshi et al. and N204' there exists a certain limiting concentra- these aspects of NO. NO. absorption. substantially reduces (even three !O four times) the rates of J AIChE Journal March 1991 Vol. The gas phase reactions and equilibria. India Absorption of nitrogen oxides was studied in three packed columns in series. :"10. N204. nitric acid and Carleton and Valentin (1968). an increase in the concentration of nitric acid. The variation in the rates of absorption with chemical reaction (of NOb N203. (1985) have reviewed NO. Koval and Peters (1960). Suchak. (1975) and Joshi et al. Simultaneous absorption of many gases occurs followed various aspect. acid are different from those in water. The formation of nitric acid in the gas phase is also considered in the model. Holma and Sohlo (1979). for a given set of partial pressures of Sherwood et al. The NOx gas is a mixture of several components consisting in this direction. B. the of nitric acid. lowing important features are included in the-'process design. It is known that. Further. The rates of absorption of N02. K. Favorable agreement is shown between the model predictions and the ex- perimental observations. of NO. absorption. and chemical reaction. N20J. Two were 254 mm ID and 6 m tall. Absorption f was alsostudied in two packed columns of 800 mm ID. and liquid phase reactions are included in the model. nitrous acid. operated in series. and N204) with respect to acid concentration is considered.3 323 \ . substantial heat effects are associated with NO. 37. J. Hoftizer and Kwanten (1972).!- Ie: t- ":s l. gas in water results into two oxyacids. and packed bubble columns used for the manufacture gases occurs preceded by chemical reaction. The reasons are: in the process design. 1980. tion of nitric acid beyond which no absorption of N204 and N02 occurs (Carberry. N02. and Selby and Counce (1988) have reported 3. interface equilibria. University of Bombay. Heterogeneous gas-liquid equilibria are included in the model for the first time. N02. Heterogeneous equilibria prevail between gas phase and . This heterogeneous equilibrium Correspondence concerning this arllde should be addressed to j. N02. (1985).s of the process design of packed columns. f statutory regulations' for a clean environment. simultaneous desorption of many columns. temperature variations need to be taken into account compared with other absorption operations. Matunga.b. ical reaction whereas the desorption of NO. it is nec- facture of nitric acid. The rates decrease with 4. and the absorption Andrew and Hanson (1961). d Modeling and Simulation of NOx Absorption in Pilot-Scale Packed Columns N. 2. of Chemical Technology. There have been outstanding attempts I. Introduction Absorption of NOx gas is an important step in the manu. flue gases has received considerable attention due to stringent the rates of mass transfer. Joshi Dept. and HN02 I. Absorption of NOx gas is probably the most complex when therefore. B. gas phase mass transfer. R. plate by chemical reaction. gas and liquid phases. Jethani. Specific rates of absorption were measured using a stirred cell with a flat interface. 2. Several reversible and irreversible reactions occur in bbth Emig et al. from the off-gases/ essary to understand the combined effects of several equilibria. Koukolik and Marek (1968). A mathematical model is developed for an adiabatic operation. 400019. Solutions of mixed nitric and sulfuric acids were used as absorbents. For the process design of NO< absorption towers. 1958). Counce and Perona (1979a. N203' and N204 in nitric is preceded by chemical reaction. etc. N20s. (1979). N203' and N204 is accompanied by chem. The removal of NO. liquid phase components. Bombay. of N20. and J. These attempts will be strengthened if the fol- absorption of N02. Makhotkin and Shamsutdinov (1976). Also. For example. For instance. 7 and 10 m tall. 1983)..

HNO]. 4 log.'l~~'. there has been no study when the nitric acid contains ? some other electrolyte..0.7. The concentration pro- the model development. (1985) and above four features. It is the gas phase. Carleton and Valentine (1968). HNO) formation needs to be included 5 log. All the components of NOx are in equlibrium with each other.. However. NO~.I 2 loglo K2 = 2.'. In the published literature. H. RaNZ04. NZ03. Solutions of mixed nitric and RaNOZ.lIT . A comparison is presented between the model predictions and the experimental obser. the N~OJ. Simulation of large-size absorbers increases confidence in Rates of Gas Phase Mass Transfer. particularly at high temperatures and high partial pres. NOz.072/ T ..PNOZ] (7) sulfuric acids were used as solvents.-p'. it was thought desirable to simulate large-scale absorbers.0..993/T . At the interface..-<.. No.o K5 = 2. the partial pressure of NO changes with Nitric oxide undergoes irreversible oxidation with oxygen in respect to distance from the interface up to the bulk gas. are summarized in Table I.. gas equilibria are defined by following equations: "5 (5) 3NO~«) + H~O(g) . The volumetric some experimental data have been collected on pilot-scale ab.3 AIChE Journal ~ . which is generally the case in most industrial absorbers.S . phase mass transfer rates have been written in the form of 2NO~(g) N~04(g) (2) Eqs. below was no appreciable enhancement in the mass transfer rate of 250 ppm of NOn the reaction is first order in both NO as well NO due to chemical reaction. There is scant information available regarding large-scale simulation. and ~.051.G = (kG~) HZO [P~zo . at the interface. NO. as O~.01 of the tOtal volume. N~O]. (1979).757 atm-' in the mathematical model. . RaNZ03. . Complex equilibria prevail in the gas phase. 6 to 12. This aspect has not been included in the mathematical models reported so far. The described by following equations: rates of gas phase mass transfer are likely to change due to the equilibrium reactions.l7/T-6.can be and water were assumed to be in equilibrium at all points. PNZ04] (8) vations.005-0. Similar assumptions have been made by Andrew "" .o KJ = 2. N~O].. equations: vestigation carried out by Counce and Perona (1983). the transfer of NO is ac- 2NO(g) + OZ(g) -'1 2NOz(g) (I) companied by oxidation. 4.G = (k~)HN03 [P~NO) . the following points may be noted.G = (k~) NZ04 [P~Z04 . Gas Phase Reactions duction increases as the nitric acid concentration approaches Eq. and Holma et al..] and Hanson (1961). = PN~04 . and HNO~ are assumed to be always in equilibrium with NO(g) + NO~(g) + H~O(g) -= HNO~(g) (4) each other. _c. and NZ04.. p~zo] (12) presence of water vapor. It was found that the film volume con- dimerization of :--10followed by oxidation by oxygen to form stitutes about 0. No.8.G = (k~)HNO~ [P~NOZ . there is a possibility of enhancement in the rate of mass transfer. PNZ03] (9) RaHN03. I loglO K. (1979). HNOz.p~o] (6) Further. = 652.I phase.Therefore. However. The mathematical model presented in this work includes the constants Kz . for simplicity. "4 Nz04. Emig et (3) al. Nz04. The oxidation reaction is second order with respect to extent of NO oxidation in the film was negligible and there NO and first order with respect to oxygen.P~NOZ] (11 ) Gas Phase Reactions and Equilibria.G = (kG~)NOZ [P~oz .. the gas K:. NOx is a mixture of various nitrogen oxides. In the gas film. there ~ist the oxyacids HNOz and HN03. the absorbent was invariably water except in the in. Equilibrium and Rate Constants the equilibrium value. NO.7328 atm-I sures of NOx.. which . The oxidation reaction is expressed as: likely that the rate of NO oxidation in the film is different from the rate in the bulk. A substantial quantity of nitric acid is formed in the gas 3 log.P~N03] (10) Mathematical Model Model for overall rate of absorption RaHNOZ. NO~. kG. 2HN01(~1 + NO(g) K.o K4=2. In the RaHZO. NZ03.' . Therefore. Therefore.. K5 were reported by Joshi et al. Table 1. A detailed energy balance also needs to be incorporated in the model..9. Therefore.226 "atm-' 3. In the gas film NO. ~ Joshi et al. 2.234 atm . At this stage. (13) . .(PNO~)- The reaction rate constant k) and the gas phase equilibria 324 March 1991\ Vol. -. '.G = (k~)NZO) [P~Z03 . ':':':'. '~~. and the extent of re. Thus..'.I. ~ absorption of NOz. 1.. Further. although files for the gas film are shown in Figure 1. rates of gas phase mass transfer are given by the following sorbers.G= (k~)NO [PNO. It is believed that NO oxidation proceeds by of DG.8/T. (1985) have reviewed the published literature on The volume of the gas film can be estimated on the basis NO oxidation. RaNO. NO(g) + NO~(gl -= NzO](g) Interface Equilibria. and NZ04.OO3.7356 atm . 37.

. 20 3 HNO'+T' 3HN02 3N02 + H20 ~ 2HN03.188 X 107 12. 20 4 NQ. posing to form nitric acid: )2 (PHN02 K4=. and N204 is accompanied by chemical reaction within the liquid film. PNHO HN03 T HN02 + NO 3 NOi'NOit-H20 ~ 2HNOt-PHHO 2 1 P~N02 i PH 0 I BULK GAS I I GAS FILM I I LlOUID FILM I IBULK LIQUID I Figure 1. (PNO) (PN02) HN02 in bulk in the liquid phase is considered to be decom- . Nitrogen oxides when absorbed in aqueous sulfuric acid solution. (1985). HN02(/) + HN03(/) (21) K3= .58 . absorption of NOx is also limited by nitric acid concentration in the liquid phase bulk and the partial pressure (17) PHN03= f[T. Carberry (1958) made a plot of max- imum attainable concentration of nitric acid as a function of P~ Hx= [A *]x (18) parameter K6 defined as where x denotes the component.O -. (PNO) (PN02) . The concentration profiles for different species in the sulfuric acid solution is a function of temperature and nitric liquid film are given in Figure 1.3 325 AIChE Journal . An empirical equation (Matasa and Tonca. (PH20) (15) 3HN02(/) . cone (HN03)] of NO at the interface. . (1985) that the absorption ofN02. No. conc(HN03)] (16) However. It has been illustrated by acid concentration: Joshi et al. Mechanism of NOx absorption into water. The values of Hx have been compiled by Joshi et al. 1973) obtained The followi~g reactions occur in the liquid phase: from various plots is of the form: 2N02(l) + H20(/) . K6 = (p bP~o) 3/2 (23) N204 Liquid Phase Reactions. HN03(/) + 2NO(/) + H20(/) (22) HN03 and H20 are at their saturation concentrations at the Mass Transfer with Chemical Reaction in the Liquid o~erface.-N02 ~ N203-PN H.. HN03(/) + HN02(l) (19) InKH = 2. P~203 (14) N204(/) + H20(/) . 2HN02(l) (20) where March 1991 Vol. 37.571 X 104 11.4. NO PNO 2NO + 02-2N02. NP3. form nitrous and nitric acid. P N02 2N02 ~ N20.424W (24) N203(/) + H20(/) .-PN . p~20=f [T. The vapor pressure of H20 or HN03 over aqueous Film.

C) PNo2 + 112(RaHNo2. HN02.C) + 112 (RaHN02.L . b PHN02) (32) GAS OUT IN Nitrous acid in bulk decomposes to form HN03 and NO in ~LlQUID the liquid phase. Since the latter has limited solubility. Eqs.~. RaHN03.P~203) (31) .3 AIChE Journal -~ . The N02 balance at the interface gives: l GAS IN I 1 (RaN02'C . it was found necessary to reduce them to a set of tW equations in terms of ~o and ~02' The procedure is describel 112 in appendix B. 24.. .RaN204.'-_:-:':'~_":".~"':"1( KH= ~o =Kr2 K6 (101.L + )"RaN02.C) L (QUID OUT + (RaN203. ~.. it de- sorbs.G.33)2 (25) RaNO. and 25 were solved incl.L -RaHN02.L 5. RaH20. N02.L (33) '0' Overall Volumetric Rates of Absorption. N203. These are provided by the material balance of divalent and tetravalent nitrogen oxides across the interface.. N204."".L=~ (HNo2)3/2 [2/3 (kD)NOil2 (Pf-l02-P~02)3/2 (29) lowing differential equations.:. i I i I I RaN20. H20. 2.G 1 dh H PN02' PN204' PN203' PHN02' PH20' Plmo3 3. No. The following assumptions were made PHN02 = (K 4 PNo PN02 PH20 ) 112 (28) I. RaHN02. 1 The limiting partial pressures of N02.. and HN02 order to attain convergence under varied parametric condi based on heterogeneous equilibria would be tions.""'U".C) (34) I" D ~ Figure 2. Gas and liquid phases flow in a countercurrent plug flo\l manner No absorption takes place when~204 =d204' The net driving . PNo2- b . and HN02..ng partial pressures PN204' PN02' 4.. The NO balance at the interface gives: ances. Component balance in gas phase RaN204.C) (3~ and W is the maximum attainable HN03 concentration in weight fraction.. b b b b for simulation studies. RaN02.RaNO. ( ) P~204 K2 (26) Model for column performance b PN203 = K 3 PNOb b PN02 (27) Model Equations.. Rate of desorption of NO from liquid to gas phase RaNO. The rate of desorption of NO is given as 4 2 1 2 RaNO.. N204. The packed column has been modele..G... Liquid holdup is uniform throughout the column force is thus the difference between the interfacial and limiting 3. N203.L =)" RaN203.L +)" RaN204..L.ependentIy whil of sulfuric acid is !:iiscussed later.~. Partial pressures of NO. Gases follow ideal gas behavior partial pressures of N02... Volumetric rates of gas phase mass transfer: RaNO.~".. There are twenty-three equations.RaHN02. and 26-35 are coupled algebraic equations..G.. N203. 37.:. RaN203.L.G..L. 6-15.""". 6-18 and 23-33.L + )"RaHN02.L =~ HN203 [(kD)N20i/2 (P~203 .G. Overall rates of absorption are computed by solving Eqs. The method for determining K6 in the presence Equations 16-18. RaN20. RaN02.~.G. Heterogeneous equilibrium parameter b b b b K6' limit\._.L . 2.d =. ".RaN02. whereas the unknowns are: 1. Figure 2.L -RaN203.. Rates of mass transfer with chemical reaction in the liquid film: RaN02.'i"'t: . P~204) (30) a. RaHN02.L =~ HN204 [(kD)N20JI/2 (P~204 .L = kL~ HHN02 (PHN02 . PNO.L .RaN203. 23..":. The column operates at steady state The volumetric absorption rates of different species are: Mass Balance. RaHN02. results in the fol.L PN203' PHN02 Ih Two more equations are needed to make the model consistent. Differential element for mass and energy bal.. .<. Divalent nitrogen balance RaN203..2(RaN204. Mass balance across a differential heigh! dh at height h from the bottom. 4. and HNO 3 at mter f ace.G = (RaN203. i RaN204. 326 March 1~1 Vol.L .~ .

g) + N02tg). 6-18.H. Equations were solved numerically by the Newton-Raphson upecific rates of absorption of N204 were measured exper..C per kmol N~O" formed NO. Equations A9-All. Estimation of Design Parameters.c. and 26-28 results in the element.H1..' ' . 23. AIChE Journal March 1991 Vol. Balance for nitric acid dX HNO.". was to achieve a single positive gas and liquid phase temperatures are the same..72 [ dh = . The four unknowns are the moll mol inerts of NO. decomposed t. obviated the need for a scaling algorithm. Water-vapor balance NO. taneous algebraic equations. The main ob- phase and the interface is always saturated with water vapor. The values of physicochemical tions into two polynomial equations. N02.99 ..o' S (38) ~= -c [RaH20. formation of N203 and N204 in the gas phase.5. 022 per kmol N~O.'':

''.L + 2/3RaN203.. ' ' ' "'.5 (RaHN02.C + 2RaN204.. t. 023 per kmol HNO.H12 = . then the temperature change under adiabatic condi.5. 025 per kmol of HN02 absorbed t.'. has parameters such as reaction rate constants. and diffusivities depend lected-the interfacial partial pressures of NO and N02-are upon temperature. interfacial and limiting partial pressure values of N204' N203.c .1.~. has been included in Table 2.= -2 C [kJ (p~O)2 (P02) Ed (39) dh Eq. L [4!3RaN204.. liberated because of various reactions always present in greater magnitude than other components in the gas and liquid phases.. Mahajani and Joshi (1990) have developed general design procedures and derived 1. and total moles in the gas phase.y "'''"'i.92 .C . 37.5. absorbed t.:"'.L + 1/3RaHNo2. and 26- of HN02.:''. RaHNO. N203' N204' and For the estimation of interface composition. matrix method for nonlinear equations.-'t: t dYNO' S [F O 2 Table 2.. Substitut- If QT is the total heat change per unit time in the differential ing these values in Eqs. 32.C+ 1!2RaHNo. the gebraic and analytical in nature. 1S Eq. The design parameters in.) + N02(g) + H~O(g)-2 HN02tg) t. The intricate algebraic reductions of these twenty-one equa- significant heat changes occur. = + 2.d (37) per kmol N~O) formed 3N02(g) + H~Otg)-2HN03(g) + NOtg) tJi6= .!:~i. This is discussed in a later section.('\i:"'""..4. fective interfacial area.H9= . N20J(g) t. Heat.?".. Estimation of interface composition Heat Balance. H20. Because of these reactions.. 23. It of NOx' These two equations were numerically solved by the will be assumed that the heat liberated is taken up by the liquid Newton-Raphson and Gauss-Jordan method. Details are given in appendix C.7 per kmol NO oxidized dYI" S. 024 per kmol HNO.-RaNO. . No. N~04(g) t. which was al- Further. Oxidation of NO.. 5. In addition. The variables se- stants.77 per kmol HNO. Eqs. appendix A.o'. finite solution with minimum numerical iterations. is endothermic. Estimation of gas phase composition rational correlations for hydrodynamics and mass transfer characteristics in packed columns.3. tions is given by: and HN02. S T=~mOC~ (41) ~ =. form a set of four simul- clude gas. absorbed t:. Equations 36-40 are coupled linear differential equations.H. 2..:o. vapor pressures.. we need to solve the liquid phase reactions are exothermic.". ~= -c l'''i( " Std.C + RaHN02. it was ~ssumed that at any point in the column. Eqs.L + RaHNO"C where T is the temperature change across the differential ele- + 2/3RaN02.H. Oxygen balance Eq. RaNO.. Heat of Reaction (25°C) + 0.39 dYo. absorption of N02.. equilibrium con. ' 2N02(. = ..RaHNO"C>J (36) Reactions kJ x 10" ReaClions in GaS Phase b.~~~{''.99 Eq.+RaN20. 021 per kmol N~O" absorbed t. The method of solution involved the following five steps.36 Eq. 020 per kmol ReaClions in the Liquid Phase NO.H. Heats of Reaction P NO) PU2 Ec.''. = ..03 d.14 Component balance in liquid phase e. ""'. solubilities. imentally to estimate H(kD)l/2 values..C.C T RaI'02'C + 2RaN20.3 327 . 13-15.c+ 1!2RaHNo2. Further details pertaining to the heat balance are given in appendix D.'.2N02". however. To- o tal mass balance is established across the differentia) height Method of Solution on solving these equations simultaneously.H-= -2. formed c. Balance for total reactive nitrogen " 2NO '" + 02(Ri .L1 (40) ment. we need to know the values or "ffusivity and solubility. jective behind using this composite technique.. The decomposition twenty-one equations simultaneously.~:".H'1 = ..05 I per kmol HN02 formed dYH. absorbed t. = . Al and A2.'"..d Eq.=-3.and liquid-side mass transfer coefficients and ef.HIO=-3.

Effect of nitric acid concentration on e. they constitute a boundary value problem. '0 z EQUlll BRIA AND RATE DEPENDENCE 4. :--JzO). The kinetics of absorption of NO. then it can be seen from Figure 3 that and 31. Eq. Estimation of H. .CONCENTRATION details are given later. The effect of energy balance is shown in Figureconcentratio 5.. MODEL EXCLUDING HETEROGENEOUS thought desirable to undertake a systematic investigation. Integration was carried out up to the top of the WEIGHT PERCENT. It is obviol 4. Therefore. isothermal case is higher than in the adiabatic case. In one set of experiments (solid lines) air was adde used.. The flow rate and composition of the incoming gas phase are known. They carried out experiments with 0. 10 solved simultaneously by the fourth-order ". the concentration o '. substantial when NO~ partial pressure and temperature af high... Therefore. in mixed acid z ON HNO. Runge-Kutta method. The composition is shown in Figure 4. iation of [H( kD)I'ZJNz04 with respect to HNO) concentration The role of heterogeneous equilibria with respect to N has been reported by Lefers and Van der Berg (1982). Inerts flow rate=2. as expected. Provision was made for the formation of HNO) in the that the difference in these two cases will depend upon tt gas phase.0 kmol/s known at the inlet and exit of a differential height. Further. NOr gas. the flow rate and concentration of incoming mixed 20 -. 3. Joshi et al. As- suming that all the sensible heat is taken up by the liquid phase. MODEL INCLUDING HETEROGENEOUS . EQUILIBRIA AND RATE DEPENOENCE .O. a: 3. The equations were . 5. CONCENTRATION .--. centration has a small effect on the extent of NOr remo Discussion of the Model However. is not included.15x 1O-4kmol/s Liquid inlet temperature 303 K Liquid superficiaJ velocity= 5. If this feat by seJ.NITRIC ACID column. Kameoka and Pigford (1977) have shown that the rates of absorption of NZ04 in water and aqueous sulfuric acid solution are practically the 80 same.. 60 trations. concentration. 23-28.. and NZ04 in water has been extensively studied in the literature. The ~ 50 EQUiliBRIA AND INCLUDING RATE o> DEPENDENCE ON HNO. Figure 3 shows the relative importance of the rate dep the change in temperature across the differential height was ences on the :--JHO)concentration and the heterogeneous e estimated. solutions has not been studied in the past. four new rates of absorption. In both of the sets the rate dependence on HNO) . temperllture difference across the column. 29. Some results will now 5e given to demonstrate the relative The formation of HNO) in the gas phase was found to t importance of these features. formation ca 328 March 1991 Vol. DI-D27... The rates of chemical reaction and mass transfer are also known. Similarly.!with respect to HNO) concentration was included (for instance.. the actual concentration of nitric acid. HNO) for a given gas phase NO. u ON HNO. Solution of heat balance equations -Air = 7 mm/s flow rate 5. removal does not depend appreciably on HN Water have been summarized by Joshi et al.JkD)~/2 values Absorption of NOz.cting appropriate values of H(kD)'/z in Eqs.3 of oUtgoing nitric acid (at the bottom of the column) was o 10 15 20 25 30 35 '0 '5 50 assumed. The reduction in the rates of absorption of :--JOz. First of all. composition concentratior and temperat and :--J. A comparison was made between the calculated and Figure 3. tions.. (1985).. the extent of NO. whereas in the second set (broken lines) air was added. appendix D. Q...:. Further.. At higher concentrations of sulfuric acid. the rates are 70 likely to decrease. The heterogeneous equilibria between gas and liquid phase seen that the rise in temperature.. the of NOx absorption. It was found that the gas phase HNO. . reduces the exte species have been included through Eqs.09 NHzS04 solu- tions.-.99 x IO-'kmol/s = method of interval halving. removal in tJ 3.- -=':-":---: 21 acid (at the top of the column) are known. The values of H(kD)lIz for the case of absorption in extent of NO... No. 37. For this purpose Eqs. MODEL EXCLUDING HETEROGENEOUS is a mixture of sulfuric and nitric acids at different concen... were libria.. it was o 2. 30. guess value at the bottom of the column was varied using the NOx flow rate 0. (1985) have 90 critically reviewed the previous work. It can 2.. Solutions of ordinary differential equations . For convergence. the heterogeneous equilibria markedly influence In the mathematical model developed in this work. of absorption... the heterogeneous equilil features have been included: successfully predict the maximum attainable I.. Complete heat balance has been established. To start the integration procedure. . % . It can be seen that the extc same variation was assumed in the case of NOz and NzO) of NOr removal strongly depends upon HNO) absorption. NzO). CONCENTRATION a: 30 Equations 36-40 are five coupled ordinary differential equa. in the present work the absorbent 1. The var. 54% in set I and 39070in set 2).3 AIChE Journa .1 X 10-4 kmol/s = From steps 1-4 the concentrations of all the species are 'Uu Air flow rate =0.: -.

Effect of nitric acid concentration on extent product gas from the pilot plant for producing oxalic acid.. 30.5 Liquid superficial veloc. N0'. It may be emphasized that the relative importance NO.(kN/m') are favored. The I stream was passed through a condenser where the outlet tem- I Packed column dia. The com.re increase with an increase in temperature.' 0-6 0-8 .6 m Packing. 1.. H(kD)I/2 increases with an increase in temperature.0 of NO" IN" is 0. At low HNO) concentrations.36x IO-"s-I :'11.3 329 . o '0 respect to different species. It can be seen that NO" absorption is 2 10 Adiabatic Ie maximum when the air flow rme is 4 x 10-4 kmol/s. .3 rate dependence on nitric acid concentration Case 2. the value of absorption parameter kLa. 77 kN/m' - ~e of the above two factors depends upon HNO) concentration NO'/N'. 323 K at 0 m hI. 1. NO< removal extent of NOx absorption. The o o 0'2 0. These two opposite factors result in an optimum flow i .5 ~\ and column height. The measurement of these indio . gas partial press. Adiabatic " AIChE Journal March 1991 Vol. Model predictions excluding heterogeneous equilibria and 80 . at high Packed column dia. Cone" WI./ tt" A gas stream constituting 19-20% NOt was obtained as a Figure 4.5x 10-"5-1 '00 0'.2. 37.0 m U Packing. However. 101..I 80 idation. .4.5 .154 m'/mJ Je Liquid temp. 0. Outlet Conc.\ I rate. the rates ~ of absorption can be determined if we know the value of the o> % combined parameter Hx(kD)V2 as described by Eqs... 1. 4 mm/s 0. .5 2. 29. -llI Experimental Work and Discussion 60 Measurement of specific rates of absorption :: .1 and at 30°C. Model predictions excluding heterogeneous equilibria and :: including rate dependence on nitric acid concentration . 38 mm Intalox saddles HNO) concentrations an optimum temperature was observed. 6 mm/s Gas superficial veloc. wI.0 kN/m' temperature. 5 50 1sothermal ~ 6 50 whereas it decreases the gas phase residence time for NO ox. Fortunately.re Figure 5. vidual parameters is extremely difficult. However.125 m'/mJ Liquid inlet temp.1 m/s kaO. Effect of isothermal/adiabatic operation on The effect of temperature on the extent of NO" removal is he shown in Figure 6. 07.0.. 0'. . . Case HNO. Joshi et al. Liquid superficial veloc.. 3 2 30 ~'0 UI 4 2 45 a: . and orders with Z II. it is desirable to o know the values of diffusivity. gas partial press. rate constant.. Line No. . The gas stream was at 65°C and contained water vapor. 709. 0. is practically independent of temperature.. bined effect of the above two factors results in an optimum :Jt Total press.10 5 15 :tJI 6 30 'no 7 45 al. hI. 0.33 kN/m' 2 NO. Total press. (1985) have discussed this subject in detail. HNO. Model predictions including heterogeneous equilibria and 0 Z 60 rate dependence on HNOJ concentration II. I m/ s :TIt kaO. Case 3. . 38 mm Intalox saddles . UI ex: 20 and 31. 298 K ..6 m. Experiments for determining Hx(kD)V2 values for N02 and N204 in water and mixed solutions of nitric and sulfuric acids 7 were conducted in a stirred cell of 95 mm ID. 3 30 Isothermal te 4 30 Adiabatic crease in the air flow rate increases the oxygen partial pressure.9x 1O-4kmol/mJ's.25 x 10-' kmol/mJ's'(kN/m') !nt kLa. 1 10 Isothermal shown in Figure 7. 10 kN/m' Case I. 0 Any -'< 1 ld. The contriburion was found to HEIGHT IN METERS .. . . 0. 2 > 2 15 ui. Temperature was maintained by using a constant-temperature bath.0 experimental setup is shown in Figure 8. h~ 'la contribute up to 20070to the overall rate of absorption when 0.. NO oxidation and the formation of N204 Gas superficial veloc. For the estimation of rates of absorption.. 070 Case ~ The effect of air flow rate on the extent of NO< removal is . 0. :'110. . Line No. At low temperatures. of NOx absorption.0 . An in.

GAS STREAM FROM PROCESS 20 'f. The gas stream was introduced to the stirred Cf a~125 m2/m3 through a rotameter. = 6 mm/s Gas superficial veloc.(kN/m2) for NO kLa= 1.~~. ~..n.. Effect of temperature and nitric acid concen. perature was controlled to equal the desired temperature in In all the experiments. Effect of air flow rate on extent of NO" al Packed column ilia. Figure 7. We assumed complete backmixed behavior.. wt/wt 50 'I.10 -4 kmol/s a NO.U)4kmol(s = LI..4. =0..25 x 1O-3kmollm3..~. saturated with water vapor. The gas stream leaving the condenser was and absorption was carried out for 300 s. WATER IN CD STrRRED CELL 95 mm DIAMETER WATER EJECTOR o CONSTANT TEMPERATURE BATH 0~TO G) TEMPERATURE TRANSMETER (CONTACT THERMOMETER) CD TEMPERATURE CONTROLLER o HEATING PAD G) TT o ROTAMETER G) WATER JET EJECTOR CD 2 -4-.o:... hI. = 0.33 kN/m' NO.:: -30'1. Total press. I>.. =0. (96 'f. CONCENTRATION = 0 'I.-.) CD Figure 8. ~(). Experimental setup in stirred cell. gas partial press. FLOW ~% '0 % IU 50 COl FLOW = 2'15.. .".s. = satUrated rates of absorption by about 5070.-. During this peri. AIR FLOW RATE IN k malls.:. 60 100 .5 m sorption Packing = 38 mm Intalox saddles Liquid superficial veloc. NO. It was analyzed for divalent and there was no appreciable change in the absorbent quanti tetravalent nitrogen oxides.5 30 INLET HNO.. NO. .'.. the absorbent quantity was 120 rn the stirred cell. = 10"10excess the extreme plug flow and back mixed behaviors will differ tl H20 partial press. 330 Mardh 1991 Vol.. INLET TEMPERATURE = 303 K SUPERFICIAL LIQUID VELOCITY = 7 mm Is 20 10 5 10 15 20 25 30 35 50 55 '0 '5 TEMPERATURE. 3 AIChE Jour '''''-. The flow rate was adjusted'in such a w.~::. a 70 a ._~'~'i:.~~~t . 104 tration on extent of NO" absorption.~ . o 2 6 8 10 12 Figure 6.I I <t ~60 1. = 33 kN/m2 that the extent of absorption was less than 10070.. '0 'I.05 nated the uncertainty regarding gas phase backmixing becau O2 partial press..I 0:: 0:: NO"/NO~ = 2... --20'1. = 303. "c o .This elirn NO'/N" = 0.. 37..'~" .--....s-1 of NOz. Over 96070of NOx was in the form because of either evaporation or condensation.6 m.« "-"'~:<:.1 m/s kaD= 1.~ 70 10 'I.. 90 >C >C a a z 50 z 80 I>...5 x 1O-2.

12 pseudo mth-order reaction regime.8 96070of the NOx gas used in the experiments.67 rls. For mixed acid solutions: cell [HJ/2 (2/3kD) 1/2]N02.10 It taining nitric acid and 40% sulfuric acid were used as absorb.(kNlm2) at 30.44 x 1O-1i 41. [H(kD)1/2]NZ04 was found to increase 10 2.60 Water.29 dence indicates that the absorption operation falls in a fast 15. 25.519x 10-6 47. The effect of stirrer speed was investigated in the range of Table 3.. Since the absorption operation was found to be independent of kL.60 form to the instantaneous reaction regime.water . [H(kD) 1/2]'1. It can be seen .267x 1O-3W~) (45) ~the The specific rate of formation of HNOJ by the absorption etely of NOx gas is given by the following equation: For water and nitric acid (Lefers and Van der Berg.H2S04 (PN02)J/2 (43) were found to be much lower than those found in water. 3 331 i . 40070sulfuric acid.10 various acid concentrations are given in Table 3. The values of H(kD)I/2 for NZ04 at Wt. These values were used for determining K6 from Eq. in 400.70x 10-6 36. A few experiments were also conducted to evaluate the Temp.HZS04 was obtained from Eq. Nitric acid.C [kmol/m2. 30.s(kN/m') conditions the partial pressure of divalent nitrogen oxides tpNo and PN20J)was negligible.s.10H2S04 at 30'C . is because the activity of water decreases in the presence of The interfacial partial pressures of N02 and N204 are related sulfuric acid.36 of nitric acid. This value is in agree- Acid Concentration ment with those reported in the literature (Sherwood et aI. I (PNO» 312 (44) assumed to vary (with respect to concentration of acids and . It also indicates complete homogeneity of wt. it means that absorption does not con. 44 by using the experimental values of the specific rate of formation of HNOJ. and mixed acid solutions con.168xlO-1i 38.10HNO.95 5. 43: The equivalent nitric acid concentration was estimated on the basis of the same [H(kD) 1/2] values..33 rls..WII.H2S04 [H (kD) 1I2]N204. 40 3.215 -IA2~ . [H3/2 2 (2/3kD)1/2]NO"water The values of [H(kD) 1/2]N20Jand [HJ/2(2/3 kD) 1'2]'102were +3 [H ( kD ) 112] N204.7IRT (I .1o [kmol/m3. The following equation is obtained by substituting 46 were used for the estimation of K6 values for mixed acids.0 wt. 13 and 42 in Eq.and liquid.67 Temp. Joshi et aI.O. 0.616 [H3/2 (2/3kD) (42) = 3. 40 wt. :"-10.93 '-.C.04 Equiv.water way [H(kD) 1I2]N204 x 1O-5e-6263. 40 wt.285. 0.0 2. without any Sulfuric Acid vortex. This also indicates that there is no effect of gas. 1975. [H(kD) I'''' '"]NZ04. Table 4 gives the values . Under these [H(kD)II2]N. Experimental Values of [H(kDl/2]N204 for 40% 0. 0.10 ents. Nitric Acid Concentration EquivalenCto Mixed 7.HZS04(K2(PNOZ)" i for nitric acid concentration equivalent to mixed acid concen- RHNOJ=4/3 tration. 0. Sulfuric acid. This .water H(kD) 1I2]N204. The liquid surface was flat. in Water that the value decreases with an increase in the concentration 5 2. s(kN/m2») x 106 the liquid phase.10 side mass transfer coefficients (kG and kd when the speed Nitric Acid [H(kD) 112)N204'. 37..0 2. It was thought desirable to 15 1.H2S04 PN204 [H(kD) 1/2]'1204values in the presence of 40% sulfuric acid +2/3 [H3/2(2/3kD)1I2]N02.66 X 10-2 W:" :imi. Eqs..97 develop a correlation for [H(kD)II2]NZ04 in the range of tem- ~al AIChE Journal March 1991 Vol. The following It was assumed that correlations were found to hold. Sulfuric acid cone.0 0. 1I2]N02. 0. wt.55 with an increase in temperature. It was observed that the specific rate of absorption was 070 NOx= 19 independent of the stirrer speed when the speed exceeded 0.167 to 1. perature and concentration covered in this work. It was expected that the values ab. [H(kD) I12)N204' effect of temperature on the values of the absorption parameter .H2S04 ause -1.0 1. 0. tem?erature) in an identical manner to that of [H(kD) 1/2]'1204' The value of [H(kD) li2]NZ04.6x 10-6 kmol/m'.3 Tetravalent nitrogen oxides (NO!) constituted more than 20 2.1.8JJe-I. The values of [H(kD) 1/2]given by Eqs.' 30'C for water=7. s(kN/m2») X 106 Hx(kD)~2.O. 10. 45 and by Eq. of [H312(2/3 kD)1I2]N02 and [H(kD)II2]N204 in H2S04 would be lower than those in water due to the presence of electrolyte. 1985).0 2. The value of [H(kD) 1/2]N204for water was found to be Table 4.. 20. exceeds 0. 1982): mL -fioei RHNOJ = 4/3RNZ04 + 2/3RN02 Wi( I [H( kD) 1/Z]N204 IO[-3. All the above evi.6x 10-6 kmol/m2. 13. 20 O. HNO.C rls. Further. 0.JIT (46) ntity = = 4/3 [H( kD) 1I2]N204.

m3/hr 3 3 9 carbon dioxide (some COz is generated due to complete oxi.. gases and entered the liquid circulation 100 currently operated packed columns in series.. .6 3 tetravalent nitrogen oxides. Details pertaining of column 3.~. 11/0).5 m2 2. The liquid product from the reactors consisted of sulfuri acid (40 wt... 11/0nitric acid).and ur Absorption of NDx in a series of packed columns reacted nitric acid (0. counter- recovery of NO.350 1.Oxalic acid was separated b cooling crystallization. 1981): Packed height 4. 37. support plates (d) C6H1Z06+ 12HNOJ-6COz+ 12HzO+6NO+6NOz Liquid distributor 1 1 I Plate heat exchanger 2. circulation loop of column 1..350 gaseous feed for column 1.5 5.5 dation). Polypro. To this stream.5 m2 None These reactions were carried out in two stirred-tank reactOr~ Pump operated in series. 11/0).25 column 1 and the remaining gases entered column 2 and sub 070NOx at inlet 20-23 8-12 3-6 sequently column 3.. The experimental setup and overflow of the column 2 stOrage tank was added to tt is shown in Figure 9. Vol.0 m + 9 NOz Packing type Pall ring Pall ring Intalox saddle (b) 4C6H1206 + 18HNOJ + 3HzO-12CzHz04' 2HzO Size 16 mm 16mm 25 mm Material SS 316 SS 316 Ceramic + 9NzO 2 2 I (c) C6H 1206 + 6HNOJ .254 m 0.8 m 1. . '. Details of Experimental Setup generated in the manufacture of oxalic acid.. 1985) for 9511/0conversion of divalent t( VL 5-6 mm/s 10. The overflow from the colum first two columns were 0.2-0. The column 3 is given in Table 5.2-0..product oxalic acid (11-12 wt. 2HzO + 6NO No.25 0.350 1. The oxidation Diameter 0.column absorption system.. Column 1 Column 2 Column 3 11/0sulfuric acid and 14-15 wt. a measurec pylene quantity of air was continuously added. The gaseous mixtUfi Experimental Conditions was passed through a column that provided sufficient residenci 5-6 mm/s 5-6 mm/s time (Joshi et aI.8 m reactions are as follows (Kirk and Othmer.254 m 0. The volumetric flow rate of this stream was measurec Material Polypro.. The oxidized stream formed th HN03 cone.. . The off-gases consist main!y of NOx ane Capacity. Head. The overflow of column 1 w: These three columns were used for the recovery of NOx gases C.8 mID. The average composition of the liquid phase fc to column dimensions and internals are given in Table 5. The third 3 stOrage tank was added to the circulation loop of column: column was 0. No.. Three.AIR PHE 2 = PLATE HEAT EXCHANGER 2 SP 1 =SAMPLE POINT 1 R3 SP 2 =SAMPLE POINT 2 SP 3 = SAMPLE POINT 3 @) CP 2 CP3 CP1 Figure 9. The mother liquor was used for th Experiments were conducted in three continuous.5 wt. m/s 0. SS 316 pylene using a precalibrated orifice meter.8 m 4.~" -' Table 5.. wt. 070 1.. and 3 m tall. kg/m3 Va. 11/0). .3CzHz04 .3 0..1 =COLUMN1 C2 =COLUMN 2 C3 =COLUMN 3 CP1 = CENTRIFUGAL PUMP 1 CP 2 = CENTRIFUGAL PUMP 2 CP3 CENTRIFUGAL PUMP 3 = R1 = ROTAMETER 1 R2 = ROTAMETER 2 R3 = ROTAMETER 3 PHE 1 = PLATE HEAT EXCHANGER 1 NOX. m water 18 18 22.~~ '.5 m (a) C6H1206 + 12HNOJ-3CzHz04' 2HzO + 31'1z0 + 3NO Total height 6. Some NOx absorption occurred il PL.3 cUChE JoUi 332 Mar~h 1991 \.0 m 3.0 m 6.2-0.254 m ID and 6 m tall. The prqcess con- sists of oxidation of monosaccharides using mixed acid (40 wt.

Table 7. kg/m3 1. centrifugal pumps excess quantity of sodium hydroxide.7 32 HZS04 Experiment 36. at inlet 14 columns in Tables 6 and 8.78 x 10-4 kmolls NO'IN" =0.0 m Total height For the purpose of comparison..9 ActUal NO'IN' at Outlet Simulation 0.14 0. R2. plate heat exchanger chromatograph. IN.9 4. . columns CP I. A favorable comparison (within I5OJo Packing type Intalox saddle Intalox saddle for column I and within 5% for columns 2 and 3) can be seen Size 37 mm 37 mm Material between the predicted and experimental values of conversion Ceramic Ceramic with respect to NOx' The predicted temperarure of the column No.2 5. 37. m3/h Experiments were also carried out in two 0. superficial liquid velocity. Two-column absorption system. Atm.14 OJoNO. No. Comparison between Model Predictions and Experimental Observations VENT 4 Total gas flow =:. GJo Nitric acid 11. the plate heat exchanger was incorporated to maintain the temperature within :I::I 0c.1 13.1 Average Conc.27 12. Liquid Temp. The details of the equipment are given in Experimental Conditions Table 7.350 1.655 0.0 32. concentration was measured by fixing the acid mixture in an Ct. and even then the agreement is 7 good.C At inlet 31 31 31 At our let OIL Simulation 3:.0 32 recycled ###BOT_TEXT### the reactors after adjusting acid concentration (by adding concentrated nitric and sulfuric acids). The percentage Diameter 0.~--~------- --- Column] Column 2 Column 3 ActUal Removal of No" GJo Simulation 52..3 333 . m of water 25 25 columns operated in series.3 31.72 Air flow = 4. Capacity. are markedly different for the first 0. C2. CP2.25 6. wI.0 41.3 4.350 VG. kmol/s NO. Table (I. mls inlet values of NO. The composition of the gas and the temperarure were meas- y CP1 y CP2 ured at the inlets and outlets of the columns. AIChE Journal March 1991 Vol.25 41. The flow sheet is given in Figure Material SS 316 SS 316 10. OJo 6. It may be emphasized that the PL.~_. and the concentra- Column 1 Column 2 tions of various species are given Table 5. rmameters sodium nitrate and sodium sulfate were measured using an ion PHE.70 Equilibrium Removal of NO" GJo Simulation 54.0 m2 None This was because the column was not insulated and the heat Pump losses were not included in the model. sample points standard samples of NaN03 and Na2S04' The liquid phase flow rate was measured by using a precalibrated rotameter.~.63 0.0m 6.629 0. Calibration charts were constructed by using SPI. support plates 2 2 Liquid distribuwr I outlet is somewhat higher than the measured temperature. The concentrations of R I.0 m 10.80 m 0.0 m are also given in Table 6.688 Experiment 0. flow = 1. The liquid phase concentrations and flow rates were also measured. It can be seen that HN03 cone. the results of model predictions 7.5 Pressure Atm.05 3.5 12. Details of Experimental Setup Details pertaining to the superficial gas velocity.0 2.80 m removal of NOx in all the columns is summarized in Table 6. temperature of operation. Liquid phase Figure 10.] x 10. A comparison between model predictions and exper- VL 5-6 mmls 5-6 mmls imental observations is given in Table 8.] 7 X 10-4 kmolls -_. In each recycle srream.5 the agreement is within 5%.1 Sulfuric acid 40. The qualitative description of the process is the same as that for Figure 9. I I Plate heat exchanger 15. Packed height 6. The liquid phase in all three columns was circulated ###BOT_TEXT### get a sufficiently good @ @ flow rate for wening of the packings.565 0.8 m ID packed 15 15 Head. Atm.85 Experiment 59. SP2._~.

as she However. Therefore. Pressure 18-19 kN/m:! panial pressure of tetravalent nitrogen Liquid Temp. "III. 9. Experimental Observations N:!04 with respect [0 concentration of nitric acid 2. :'-. absorption were not considered in the present model. absorption is high in the bottom region.. 5 6 8 250 mm ID column (column 1 in Table 5).I.1 X 10-4 kmol Total flow rate of gas phase 1.267 X II - ~ .. the extent of NO..o3kmo~. the specific rates of absorptie Simulation 58 23. x'0') kmol~/ s erogeneous equilibrium was practically established. The results are given in Figure 11.0 Specific rates of absorption of N:!OJ in water and mix Experiment Actual NO" /N" at outlet solutions of sulfuric and nitric acids were measured in 8 Simulation 0. Complete energy balance Column I Column 2 Total The new model is capable of incorporating the effects C imum permissible concemration of nitric acid on N Actual Removal of NOn % sorption. Therefore. This was indeed found to t pressures for a given nitric acid concentration. flow=3. :'-. absorption. the contrib [0 the extent 0 Therefore.66x lO 'e Simulation 37. 60 Mixed acid concentration is given in Table 6 z o . PERCENTAGE NO. ..8 56.\IChE March 1991 V III. "10 Simulation 39.0].333 No.. Tables 6 and 8 show a compa UJZO FLOW RATE OF NO.()4=3. the HNO:! concentration exceeds about -+m.'" 90 Table 9. at I m height. :'-. '0 = 0. 29-32. °C At Inlet 31 31 <>263. Comparison between Model Predictions and I. The following correlation was found to holt Sulfuric acid 42. AT THE BOTTOM NO" / z . in the present set of experiments.78 x 10-4 kmc 80 Flow rate of NO.0 43..5 x 10-4 kmolls nitric acid concentration NO"/N" =0."'t. Figure II. Variations in the rates of absorption of NO. As a result.. Simulation 55.74 x 10-3 kmolls 4.' - ._j. Formation of nitric acid in the gas phase Air flow = 1.. the rate of NO.5 tration. the rate becomes very low when the packed height Figures 9 and IQ.0 [.9 77. Effect of column height on the extent of NOx absorption.3 81.3 Average cone. 23-28. Removal of :"'10" 070 mixed acid solutions. this work.0 range of 0-20 wr. The gas and I o HEIGHT FROM THE BOTTOM. for large packed A mathematical model has been developed in whic new features have been included. the extent of NOx removal was measured i o 3 .81..- Hr(l-1. as report NO:! and N:P.2 ~ o 50 COLUMN DIAMETER = 1.318 0. 'Column I.0 2.226 water were found to agree with the published literal Equilib. 37. J 334 " ..Is between predictions and experimental observations wherl FLOW RATE OF AIR = .._.3 20. (U2 NO" IN" ratio at boltom 4. /. Eqs. The observed rares of absor~ Experiment 0.~J. As the height increases.7 77.107 3. Extent of NOx Removal in 250 mm ID Colum 7. 070 found to decrease with an increase in the nitric acid :O. removal is controlled by he UJ l- X TOTAL GAS FLOW RATE = 2.I: Total gas flow=2. At the bottom. Removal of NO.C I- 30 = z TOTAL PRESSURE ~ 101 '33 kN / m heights./S geneous equilibrium. = 6 '10' kmol. Heterogeneous equilibria between NO.3 31."9s".I. most of the liquid phase was recycled. the driving force contin. AT THE INLET = Z.0 32..9 21. . 1)10HNO.Z5m 41. Eqs.. It can be seen from Figure II It may be noted that in all five packed columns stud that the rate of NO.616x 10 At outlet [H(kD)i :!IN. Table 5 o AVERAGE TEMPERATURE 33. Above a certain height-say 4 m in Figure II-the overall absorption operation is controlled by the ox. are high compared with the equilibrium partial Counce and Perona (1983). in 40 wr.7 Experiment 36.l7x 10-4 km( Flow rate of air ~ 70 Column details are given in Table 5 u '" Superficial liquid velocity 6 mm/s "'" Q. uously decreases. Atm. 070sulfuric acid Atm. These are: Table 8. 10 In order to check the validity of the mass transfer Eqs. Thus. .8 m height is given in Ta':>le 6 o.itricacid 6.7 VI Experimental CD . the partial pressures of liquid phase attains a constant composition.5x 10-3 kmol/s NO.239 cell with tlat interface.1. Conclusions idation of NO in the gas phase. 29-32.331 0. The agreement between the model predi The extent of NOx absorption increases with an increase in and experimental observations can be seen to be within the packed height. In 1 m packed height. SUPERFICIAL LIQUID VELOCITY = 6 mm/s Extent of removal at 4. heterogeneous equilibrium cond are not established and the rate of mass transfer is th( trolling step. m samples were withdrawn at a distance of 1 m from the bt and at the top of the column. is high at of HNO:! formation and decomposition the bottom.

. m ( Yx). kcal/s (1983 ).2 = absorption factOr for fast pseudofirst-order reaction YNO. 55 S = cross-sectional area of column. Rax:o = rate of gas phase mass transfer of component x. Chem. H. = forward reaction rate constant for reaction n exponent of nominal packing diameter. = Yx at exit of differential height :quid H(kD) 112= absorption factOr for fast pseudo first-order reaction. Valentin. (kN/m2) Greek letters mm KH = heterogeneous equilibrium constant..(1958). Rax L = rate of absorption of component x. (kN/m2). = kmol divalent nitrogen per kmol inerts . K WN = wt. = total moles divalent nitrogen oxides NO!. kmollm3'(kN/m2) ed in ko = physical gas-side mass transfer coefficient. m (X). 361 \ Qc = total heat changes in gas phase.n = backward reaction rate constant for reaction n . (kN/m2) 51770. Eq. Eqs. Eng.and p." Chem. 3 335 i ( . Eq.' . m Yx mol gaseous component x per mol inert 1 the H = tOtal height of packed column. 4th Eur. m/s [A. 61 ES = fractional solid holdup N. kmoll(m3s) is served between the model predictions and experimental ob. kmollm2. Chem. m /Joo= viscosity of gas L = flow rate of liquid. Scl. G. ( Yx). I = characteristic length of packing. - Andrew. 35. (suppl. kcalls Carra. 189 = heat changes due to oxidation of NO in bulk gas. P. kcal/ s Carberry.. = heat changes due to formation of N20] in bulk gas. J. m2/s (X)o = component X oxidized in differential volume ~isan f = friction factOr (X)v = component X vaporized in differential volume . "The Dynamics' of Nitrous Gas t. 22.(kD)'. = kmol reactive nitrogen per kmol inerts H.). K a = interfacial area. kg/m3 tions K6 = heterogeneous equilibrium constant.] = saturation concentration of gas phase reactant in Vo = superficial gas velocity. C3 = 1i by k. Eq. kmoll(m3s) ReL = Reynolds number for liquid )i 5 s = exponent. m2/s (X). and F. ~. = mass velocity of liquid. Pigford. m2/s3 = T = total Pr = toral pressure of gas. m2/s (X)f = component X formed in differential volume Do = diffusivity in gas phase. 329 <~~ ) Qr = total heat change. partial pressure of inert in bulk of gas = a absorption p.. Eng. m2 Notation Seo = Schmidt number for gas T = temperature. kmollm3. A. A favorable agreement was ob. s /Jow= viscosity oi water Lw = latent heat of vaporization of water. kcallkmol € = voidage mO mass flow rate of liquid. (kN/m2) Z = coefficient. t ihe = heat changes due l0 formation of HN02 in bulk gas. kmol/s /JoL= viscosity of liquid L.. kmolls = EO = fractional gas holdup iour m = coefficient. 61 EL = fractional liquid holdup n = exponent. I = inlet condition i = partial pressure of component x in bulk of gas phase L. frac. Carleton. ~able for component x. s YHo. 34. Q6 = heat changes due to water evaporation in bulk gas. kmoll s G. Chem. Eq. Eqs. kg/m3 ###BOT_TEXT###. Hw = solubility in water. K a~ = dry area of packing per unit volume. C3 'Y= :true k . = component X at inlet of differential volume [era- DL = diffusivity in liquid phase... het. = equilibrium constant for reaction n PL = density of liquid. Eq. H. Symp. QL = toral heat changes in liquid phase. kN/m2 . kcallkmol phase per kmol inerts con. s YT = total moles gas per mol inert h = height from bottOm of packed bed. m/s {3 exponent of superficial liquid velocity.::J>= pressure drop in packed column v = vapor (acid x = x in NO. = = parrial pressure of component x in bulk of gas e exit condition p. "Some Remarks on Chemical Equilibrium and Kinetics td at Q. in bulk gas. C3 nthe kL = physical liquid-side mass transfer coefficient. and D. = Yx at inlet of differential height kmol/m2. Eq. J. m2/m3 t!.. Proc. K) 800 mm ID packed columns. (g) = gas phase ::a\~ p.T = temperature difference. kmol water in form of oxyacids and free water in gas tions 2 = lli = standard heat of reaction. In kcal/ s Literature Cited \ere Q] heat changes due = kcal/s to formation of HNO] in bulk gas. Pm = power consumed per unit weight of gas holdup. 55 tions HNO = solubility of NO in water." = coefficiem. Ind. S. s = [[Om YN. Eq. Pergamon. Eng. X(/) = component X in aqueous phase ares. Hanson. ~es: kcal/ s . 37. limiting partial pressure of component x at gas-liquid = = f formation interface = p~ = partial pressure of component x at gas-liquid interface G. NO. Eq. kg/m2. s. Oxford. In' Absorption of NOx gases was carried out in 254 mm and R = universal gas constant. = solubility in electrolyte. 9. Absorption.en- Q. Scl. m2/m3 VL = superficial liquid velocity. (m3.~al AIChE Journal March 1991 Vol. = component X at exit of differential volume Dx = diffusivity of component x. kmol/m3. Q. Sci. t kcal/ s Reaction Eng. . = mass flow rate of gas stream kg/m2. = tOtal moles tetravalent nitrogen oxides Subscripts . ~o. trred kcaJ/ s !~ :n Q2 = heat changes due to formation of N20. F = packing factor X(g) = component X in gas phase G = flow rate of inerts. (/) liquid phase ab. Eng. 14. m/s liquid phase W = wt. Fundam. 105 (1961).~nd = tOtal moles NO. kcal/s (1968). O?o HN03 in mixed acid dh = differential height of column Xx = kmol x ions per kmol water dp = nominal size of packings. kN/m2)/(kmol.. L. HN03 in aqueous nitric acid solution e~ = average specific heat of liquid phase. and R." Chem. )L' 5 servations. C9 K. kcallkmol. in the Nitrogen Dioxide-Water System. kmollm2. S. 36 Po = density of gas. 36 ex = coefficient. (kN/m2).

" + 2 ( YNZ03) + Y HN03 + Y HNOZ (i G. New York . H. Wohlfahrt. J. 3rd ed. \lakhotkin." Ind.. Sci. 19. R. J. YN' = YNO + YNOZ + 2( YNZ04) Chern. in terms of YNO... Eng. YT( Y. 37.. R.. 33. "A Mathematical Model for an Absorption Tower of Nitrogen Oxides in Nitric Acid Production. Perona. E. Gases.. 52. Counce. Sada.. 1011 (1960)... Proc. Kondo." Chern.). Demonstrated by In computing gas phase equilibria. Sada. Kobayashi. YNO" YH.jPT Y'IOY'Io:YH:o) Sci. 1. Gas-Liquid Reactions.. V. Kita. and E. Eng.+ YHNO] For known molar concentrations of inerts. Co. and P. Van der Berg. Chern. YHZO" = YHZO + 0. and T. K. ( YHN03) Kirk and Othmer. 426 (1980). and F. "A Mathematical Model for Ni- YNZ ] =K]YNOYNO. Des. V. Japan. Chern. "Estimate Tower Pressure Drop. and 1. Juvekar. Selby. Eng. [KSPT( YNOZ) YHZOi ' Y'\Io] . V.~. 1917 ( 1988).Y~~ I (K.. E. Pangarkar. 163 (1977) . C. J AIChE JOUi . 29. V. Shamsutdinov. total reactive nitrogen per mole of inert. Sohlo. "-'. .. V.. Chern. YNZ03." (in preparation. Eng.. Eng. 20. PTIYT . and A.. (f YHN03- (1970)." Chern... Matasa. and J.o. J. E. "Absorption of N02/N204 into ( YHN03) + 0. Eng.. Develop." Chern. 32. J. Res. Sherwood. Encyclopedia of Chernical Technology. and YT are obtained. 135 (1979)." Ind.5( YHNOZ) (. Basi!: Nitrogen Cornpounds. Marek..!.K]PT YNO YNoz =0 (A Gas Phase Equilibria I/Z The total number of moles in the gas per mole of inert is YT( YH~O" . F. . I. A6. and J.. YNO' = YNO + YNZ03 + 0. "Reaction of Aqueous Nitrogen Diox. R.1/2 Y~~ I (K4PTYNO Y"o~ YHZO) obtained by adding ratios of all gaseous species to mole '01' 3 i/2 + [K.5(YHNOZ) ..K] YNo YNo:] =0 (P Nitrogen Oxide Gas Mixtures. . Hoffmann. and J. YHZO) .562 (l979a). Wilke. Hence Y for the Production of Nitric Acid.. YT( 1) Y'IO + Y"o~ -+-YH:o + Yo: + Pub. They are: 19(9)." AIChE J.o. and J. Chern.. J. "Aqueous Scrubbing' of Dilute . M.6070 Perforations. R." Ind.::. Chern. P.O~YH~O)I/Z Appendix A. New York (1973). Koukolik. Mahajani.. Chern.PT Y"o~ Y"o. A. V.. Chern. u ° trogen Oxide Absorption in a Sieve Plate Column.. N. 16. 1171 (1977). G. Tekhnol. Counce. 18. and M. Hoftizer.5 Diluted and Concentrated Nitric Acid. McGraw-HilI.. 347 (1968). V. "Absorption with Si- multaneous Complex Reactions in Both Phases. When these are sub Mahajani. Perona.5 Wiley. 1.. (sup pI. A7: and A8. Honhabel. B. whereas the extent of oxidation at any moment is expres Kameoka.. Eng.26 (1983). Y"o:) ." Cornput..YHNO~'and YH Sept. June 27. Estimation of Partial Pressures of 3 I!2 ] Various Gaseous Components on the Basis of . No.~. Chemical yj. J. P.1411 (1976). J. "Absorption of NO. 18.. 23. Y'IO" YH. Pigford. t NO~.YV~ {[K. "Scrubbing of Gaseous Nitrogen Oxides in Packed Towers. equilibrium partial pressure -r YHNO. water vapor per mole of inert. Fundarn. T." Chern. 400 (l979b).623 (1981).. It is expressed as: ide." Chern. : + [KSPT( YNO/ YH~oIY'lo]1 I . -[K.. S. Eng. Eng. L: "Absorption of NO in Aqueous Solutions or KMnO. moles of divalent nitrogen per mole into Water.Pr( Y'IO~)3 YH~O'Y'lO]li~ + (K.jPT Y:-ooY"oz YH~o Onda.. all the gaseous species in the bulk gas can be estimated \ 336 March 1991 Vol. Counce. and 1.. S. and J.. M..67 (1983). .jPTY'IOY'.. YNZ04 = Kz( YNOZ)zPTIYT u sorption in a Sieve Plate Column. B. G. 1990). Lefers.. "Gas-Liquid Interfacial Area of where a Sieve Plate with Down Comers and 0. Joshi. I (1985). 3. M. YHZO' is moles of water in the form of oxyacids and I Koval. Pergamon. 16. Equations A2 to A5 express YNZ04.. AI. and Alkaline Sodium inert: Sulfite Aqueous Solutions.2PT[K~( Y"o~): cGraw-Hill. 132 (1982). Sulfuric Acid. Oxford. 211 (1982). four equations in Y A Quick Look. "Absorption of Nitrous Gases. Develop.~' Counce." J. T."". New York (1975). Sodium Hydroxide. we assume that then the Modeling and Calculation of Counter-Current Flow Columns no formation or removal of reactive nitrogen." Cornput. and NO" to (N") ratio. "Absorption of Nitrogen Dioxide in the form of YNO'.." Ind.. Peters. R. "Figuring Packed-Tower Diameter. L. and J. YT= Y"o+ Y'Io~+ Y'I~().~. and C.. Pigford. Perona. Fundarn. J. Syrnp. "Gaseous Nitrogen Oxide Ab.Vfass Transfer.""":'-". A. Ita. ~ . . Kwanten. and R. Kumazawa. and U. Perona. K. (l Proc. London (1972). B. "Mass Transfer in Packed Column: tuted in Eqs.. Tonca.. Chern. Eng.. 143 (1979). Proc.. 18 (1970). Eng..Y'IO. Des... 3.. V. and K. ." Ind. Cornrnun. Eng. oxygen. K. H. M. React. Eng. 3.0. 27. Hayakawa. and YT.* . Eng. . R. I/Z Ks( YNOZ)3yHzO PT Danckwerts. Chern. [ Y NO Y TJ Emig..K:PT (Y'IO~)~]=O Eng. and R. Butterworths. K. Gas Purification Processes for Air Pollution Control. (. and V. YNO) -1/2 Y~~ [(K. New York. M. Niranjan. YHNOZ= (K4YNOYNOzYHZOPTIYT)1/Z Counce. V. G. is expressed as: Holma.. . G.j+ Y'I~(). W. J. 4th Eur. Kudo. Chern. Khirn.. "Salting Out Parameters of Gas Solubility in Aqueous Salt Solutions.. Mahajani. Joshi. YT( YNO* . M. L.PT (Y'\I0z) YH~oIYNo] =0 (A inert. Eng.." Ind.. Khirn.O + Y(h -r I (AI) . B. + Y H. Joshi.

Az (p{. HN02. 3.2 (C6) by EL= l1.9x IO-SReLO.o) + A3 (p{.=3A) type of packing. No.. and 26-35 into Eqs.j: :: and Values for Ct. 37. 6-15.)N204 ~ of j 0. A9-A12 simultaneously for Yr.. B 12 ( PNO + B S ( PNO I i ) ( PN02 ) all the packings. B S ( PNO + B 6 (PN02 ) 2 + B 7 [PINOPN02 i . . and 'Y for different pac kings are as in Table B I [P iNOZ - i 1/3 I B 2 ( PNO ) ]3/2 + B JPN02 + B ~ [ (PN02 ) I 2 AI. 34 and 35: 812=As (A5) 1/3]312 A I [PN02 . 1982) used to deter- mine flooding conditions is: (A6) where In Y=.53X 1O-4+2.oZ)2 .:) Bo = 3A5 'nal AIChE Journal March 1991 Vol...66(. A2-A5. Mahajani and Joshi (1990) have developed correlations :) for gas-side and liquid-side mass transfer coefficients based i ) 213 ] i .7s1d. IIZ and Physical Properties . Compositions of HN03.1 A3 = (2K2 ~ HNZ04 [(kD)N20/12) 13 - Y= (A7) PL PG A4= I/(Kz K~/3) free As= (K3 ~HNZOJ [(Dk)NZO/I2J/3 X =~: ~:r/2 IIZ A7 = (K4 pkzo) KL'!. K3 (kG~)NZOJ P=Z(dp)-S (C2) .z= (kG~)NOP~O+ (kG'!.(k~)N02PRi02 .)HNO:PHNO/2+(kG~)N20~Ri203 Ct VL(3(dp)r '!. 26-35 8ll = . 6-15.0814 In X. . + B 10 ( PN02PNO 062 ) 1/2 T' B II =0 (B2) k (GRT) I (Pm/) 'I PG 1/3 Px 0) 0. (3. A2 (p{.. i i 1!1 .AS(PNO) ] + A9(PNO) (PNOZ)+AlO(PNO) (PNOZ) The column diameter was estimated on the basis of flooding + A I iPNO + A 12 = 0 (Bl) calculations.(k~)HN02PHNO/2 (A4) The following two equations are obtained by substituting . 23.(kG~)N203PRi203 . solving Eqs. All = . B<=A4 Liquid holdup in the packed column is computed as 'oral B~ = 2K2 (kG'!. 1. (C3) E' .(A8) As = 1/ (K~I2K~/3) A9 =. The correlation (Mahajani. i ) 4/3 ] B 2 ( PNO on turbulence intensity.)HNO/2 The correlation employed for computing the effective in- Y"Q.)NO terfacial area (Joshi et aI.HHNO/6 I/Z Packing factor P was calculated from the equation.G 1 J (Sed G) i where where Pm is the power consumption per unit mass of the gas Ill) BI=3AI fap vl B2 = A2 Pm= [6(E-Ed] 4 (C5) B) = (kG~ON02 -: I is the characteristic length of packing. Eqs. 23. They have shown that the following correlation for the gas-side mass transfer coefficient holds for i I ) 1/2 I ) 213 ] + B 9 [( PNOPN02 . 0.A4 (p~O)2I3] + As[P~~oz . N203' and N204 are (A2) obtzained from equilibria relations.1273 (In X)2 (CI) AI = I~ (HNOZ)3/Z[(2/3 kD)NOZ]1/2)/3 ~ssed where Ie of Az= I/K~/ZK6113 (O*)2p J1. Estimation of Design Parameters Y~*.553 (C4) DG l J1. its value depends on 2) B..2(kG~)N204PRi204 Eqs. 89=3A7 810= -AIO (A3) Appendix B. Table AI. 1985) in packed column is A. .O)4/3] + A7[ (PNO) 112(p~OZ) IIZ ~re IS Appendix C. Simplification of Eqs.1. YNO' YN02' and 8s = .~.3 337 .flNO) bsti.(kG'!. 2/3 112 . . AIO= .(K4 pkzo)112 (kG'!. .3861.A9 YH o.

LSdh (0 Values of coefficient 1/ are listed in Table AI. (HNO)j=G( YHNO). 37.cSdh ([ 10glO(He/Hw) = -f. The value of ig f( ILL E HNO) was estimated from the vapor press un: of HNO) OV nitric acid. Values of Constants in Eqs. The value of ig for HN02 was assumed to be t1 The specific surface area is calculated from the packing same as that of HNO).YHN0Jol)+ RaHNO).463.K. (1970) have reported the values of salting-out paramete dp VL PL for various cations.1. The rate of formation of N20) from NO and N02 in tl from the following correlation: differential element is given by: 0.090 and The rate of heat generation due to N20~ formation is: 0.96 -1.0 contribution of the solute gas. and gases. 1983) Q. For this purpose.178 (CI2) 3.337 . The rate of formation of NZ04 from N02 in the diff( ential element is given by. " """. Liquid-side mass transfer coefficient kL has been estimated I.~h"'~' .015 0.and i. Pressure drop in the packed column was estimated by the The rate of heat generation due to NzO) formation is: following correlation (Niranjan et a!. 1985). (0 (N204)j= (N204)h .e .0 0.'.478 7..913 4.403 27. respectively (Joshi et a!.33 x H"o) =.53 -1.3 AIChE Jourr ( .(N204)i + (N204)a (T/298.74 .ldp 0.(NZO)i + (NZO)a (NzO)j= G ( Y"zo).' .4 19.07 O.i) + Ra"204.533 2. YN204.7 Intalox saddles 2. to the following steps.5 (0 (kd/Dd =1/ReL ( ) P:~L (C9) (NzO)j= (NZO)e . = (NzOJ)j ilii4 (0 f( G* )2a p (M'/h) (ClO) = [6 PC(E-Ed] 2. :"/0.' .+i.484 kmol/mJ.091 1.+i. Oiffusivities of gases vary with temperatUre and pressure..l (CI3) - where The rate of heat liberated due to HNOJ formation is.6 0.(HN02)i + (HNOzJa (0 338 March 1991 Vol. anions. the following correction was used..'..'"" ".1 843 0.are contributions of carions and anions of the elec- trolyte.4 Pall rings 2. The solubility of NO in water is given by the following equation: Q2 = (N204)j ilii) (I: roglo (101. (kN I K. ~ Table AI. 2.e. CI-Cll f a {3 Z s 10-2 Pac kings m n=-y "X Raschig rings 3.25dp 28.Y"Z0Jol) + Ra"ZO).5dp 8.76 4.5 0.800 1.LSdh The solubility of HNOJ and HNOc in water is 2. kmol/mJ.2)L75(101. (1977). Q) ([ Hw=solubility in water. The value of ig for N ReL= (C7) gas was reported by Sada et al. The rate of formation of HNO) in the differential elem( is given by: The solubility of NO and HNOc in the presence of electrolytes like HzSO~ and HNOJ was estimated by using the fullowing (HNO)j= (HNOJ)e . The rate of formation of HN02 in the differential elem( is given by: i.e. Heat Changes Gas phase heat changes Values of m and n for different packings are given in Table Contribution to the heat changes from the gas phase are d\ AI.".(HNO)i + (HNO)a ([ equation. respectively.32IT + 2.17 3.=salting-out parameter = i. (kN/mz).(kN/mC) = (HNOJ)j ilii6 mC) Hel = solubility in electrolyte solution. kmol/mJ. to the salting-out parameter and i" is the (HN02)r= (HN02)e . Oanckwerts (1970) and One where the Reynolds number is given by et a!.03 6..33/ ?T) (CII) Dx=DdS'C (0 (N204)j= G( Y"204. diameter as ap=m(dp)n (C8) Appendix D. 4. 1.

e-1I2 YHNO).)+ 1/2 HN03. (01) The rate of heat generation due to NO oxidation is given by: Heats of reaction are summarized in Table 2.e-YH2o. 37.NO. 27. 1990.LMl9 + RaN203. (D6) l1enr {Oi) (08) ":: ID9) :nent DIO) --"al -\IChE Journal March 1991 Vol.LMls + RaN204. It reaction Jnda may be noted that NO is used in the N203 and HN02 formation In the absence of information on heats of dissolution of :eters and it is liberated during HN03 formation.i ~ due (4) 3 HN02(l)-HN03(l)+2 NO(g)+H20(/) (D23) -112 YHN02.3 339 View publication stats .GMlII + RaHNo2.LMlI3) S dh (D26) iffer~ (H20)u= (H20'e.f (DB) (2) N204(g) + H20(/) .f (1) 2 N02(g) + H20(/) .(RaN203.e.o = (NO'i.f+ 112 HN03.i. (04) + 1/2 YHN02.. The rate of heat liberated due to the oxidation of NO is Heat changes due to absorption with chemical estimated from the knowledge of the rate of NO oxidation.e.i+1I2 YHNO). No.e+ YN203. HN03(/) + HN02(/) (020) .f+ 1/2 HN02.112 HN02. YN203..e-l12 YHN03.) n the (5) HN03(g)-HN03(/) (D24) .112 RaHN03.L ..f (DI6) Total heat change in the differential volume is the summation (H20)u=G (YH2o.2 RaHt>i02. and rel'isian received .Vot'. 1990.G) S dh) (DI4) (6) HN02(g)-HN02(/) (025) .e+ 112 YHN02.LMlIO 1D3) The rate of water evaporation in the differential element + RaHNO).dS dh (DI7) Jfanuscripr received June 12.N203.i of all the heat changes. H20. YNO. .) + RaHN02.G Qr= QG -+ QL (D27) ID5) + 11. for given by: Reactions under consideration for the heat balance are: over e the NO.LSdh (Dll) Q6 = (H20)u Lw (DI8) 2 :) ~ The total heat change in the gas phase is given by: The rate of heat liberated due to HN02 formation is: QG=QI +Q2+Q3+Q4+QS+ Q6 (D 19) Q4= (HN02)fMl7 (DI2) 5. HN03(/) + HN02(l) (D2I) (3) N203(g) + H20(/) -2 HN02(l) (022) = G( YNO.e) .LMlI2 was obtained by material balance: + RaNo.YHN02.) + (112 RaHNO).L + 112 RaHN02. (HN02)f= G( YHN02.e-1I2 YHN02. gases the information on heats of formation of reactants and rNO The mass balance for NO across the differential element is products was used to compute the heats of reactions.i+ 112 YHN03.. (02) Qs = (NO)o Mil (D 15) Heat liberated due to absorption with chemical reaction in the liquid phase is expressed as: Heat changes due to water evaporation QL = (RaNo2.

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''.L + 2/3RaN203.. ' ' ' "'.5 (RaHN02.C + 2RaN204.. t. 023 per kmol HNO.H12 = . then the temperature change under adiabatic condi.5. 025 per kmol of HN02 absorbed t.'. has parameters such as reaction rate constants. and diffusivities depend lected-the interfacial partial pressures of NO and N02-are upon temperature. interfacial and limiting partial pressure values of N204' N203.c .1.~. has been included in Table 2.= -2 C [kJ (p~O)2 (P02) Ed (39) dh Eq. L [4!3RaN204.. liberated because of various reactions always present in greater magnitude than other components in the gas and liquid phases.. Mahajani and Joshi (1990) have developed general design procedures and derived 1. and total moles in the gas phase.y "'''"'i.92 .C . 37.5. absorbed t.:"'.L + 1/3RaHNo2. and 26- of HN02.:''. RaHNO. N203' N204' and For the estimation of interface composition. matrix method for nonlinear equations.-'t: t dYNO' S [F O 2 Table 2.. Substitut- If QT is the total heat change per unit time in the differential ing these values in Eqs. 32.C+ 1!2RaHNo. the gebraic and analytical in nature. 1S Eq. The design parameters in.) + N02(g) + H~O(g)-2 HN02tg) t. The intricate algebraic reductions of these twenty-one equa- significant heat changes occur. = + 2.d (37) per kmol N~O) formed 3N02(g) + H~Otg)-2HN03(g) + NOtg) tJi6= .!:~i. This is discussed in a later section.('\i:"'""..4. fective interfacial area.H9= . N20J(g) t. Heat.?".. Estimation of interface composition Heat Balance. H20. Because of these reactions.. 23. It of NOx' These two equations were numerically solved by the will be assumed that the heat liberated is taken up by the liquid Newton-Raphson and Gauss-Jordan method. Details are given in appendix C.7 per kmol NO oxidized dYI" S. 024 per kmol HNO.-RaNO. . No. N~04(g) t. which was al- Further. Oxidation of NO.. 5. In addition. The variables se- stants.77 per kmol HNO. Eqs. appendix A.o'. finite solution with minimum numerical iterations. is endothermic. Estimation of gas phase composition rational correlations for hydrodynamics and mass transfer characteristics in packed columns.3. tions is given by: and HN02. S T=~mOC~ (41) ~ =. form a set of four simul- clude gas. absorbed t:. Equations 36-40 are coupled linear differential equations.H. 2..:o. vapor pressures.. we need to solve the liquid phase reactions are exothermic.". ~= -c l'''i( " Std.C + RaHN02. it was ~ssumed that at any point in the column. Eqs.L + RaHNO"C where T is the temperature change across the differential ele- + 2/3RaN02.H. Oxygen balance Eq. RaNO.. Heat of Reaction (25°C) + 0.39 dYo. absorption of N02.. equilibrium con. ' 2N02(. = ..RaHNO"C>J (36) Reactions kJ x 10" ReaClions in GaS Phase b.~~~{''.99 Eq.+RaN20. 021 per kmol N~O" absorbed t. The method of solution involved the following five steps.36 Eq. 020 per kmol ReaClions in the Liquid Phase NO.H. Heats of Reaction P NO) PU2 Ec.''. = ..03 d.14 Component balance in liquid phase e. ""'. solubilities. imentally to estimate H(kD)l/2 values..C.C T RaI'02'C + 2RaN20.3 327 . 13-15.c+ 1!2RaHNo2. Further details pertaining to the heat balance are given in appendix D.'.2N02". however. To- o tal mass balance is established across the differentia) height Method of Solution on solving these equations simultaneously.H-= -2. formed c. Balance for total reactive nitrogen " 2NO '" + 02(Ri .L1 (40) ment. we need to know the values or "ffusivity and solubility. jective behind using this composite technique.. The decomposition twenty-one equations simultaneously.~:".H'1 = ..05 I per kmol HN02 formed dYH. absorbed t. = . Al and A2.'"..d Eq.=-3.and liquid-side mass transfer coefficients and ef.HIO=-3.

Effect of nitric acid concentration on e. they constitute a boundary value problem. '0 z EQUlll BRIA AND RATE DEPENDENCE 4. :--JzO). The kinetics of absorption of NO. then it can be seen from Figure 3 that and 31. Eq. Estimation of H. .CONCENTRATION details are given later. The effect of energy balance is shown in Figureconcentratio 5.. MODEL EXCLUDING HETEROGENEOUS thought desirable to undertake a systematic investigation. Integration was carried out up to the top of the WEIGHT PERCENT. It is obviol 4. Therefore. isothermal case is higher than in the adiabatic case. In one set of experiments (solid lines) air was adde used.. The flow rate and composition of the incoming gas phase are known. They carried out experiments with 0. 10 solved simultaneously by the fourth-order ". the concentration o '. substantial when NO~ partial pressure and temperature af high... Therefore. in mixed acid z ON HNO. Runge-Kutta method. The composition is shown in Figure 4. iation of [H( kD)I'ZJNz04 with respect to HNO) concentration The role of heterogeneous equilibria with respect to N has been reported by Lefers and Van der Berg (1982). Inerts flow rate=2. as expected. Provision was made for the formation of HNO) in the that the difference in these two cases will depend upon tt gas phase.0 kmol/s known at the inlet and exit of a differential height. Further. NOr gas. the flow rate and concentration of incoming mixed 20 -. 3. Joshi et al. As- suming that all the sensible heat is taken up by the liquid phase. MODEL INCLUDING HETEROGENEOUS . EQUILIBRIA AND RATE DEPENOENCE .O. a: 3. The equations were . 5. CONCENTRATION .--. centration has a small effect on the extent of NOr remo Discussion of the Model However. is not included.15x 1O-4kmol/s Liquid inlet temperature 303 K Liquid superficiaJ velocity= 5. If this feat by seJ.NITRIC ACID column. Kameoka and Pigford (1977) have shown that the rates of absorption of NZ04 in water and aqueous sulfuric acid solution are practically the 80 same.. 60 trations. concentration. 23-28.. and NZ04 in water has been extensively studied in the literature. The ~ 50 EQUiliBRIA AND INCLUDING RATE o> DEPENDENCE ON HNO. Figure 3 shows the relative importance of the rate dep the change in temperature across the differential height was ences on the :--JHO)concentration and the heterogeneous e estimated. solutions has not been studied in the past. four new rates of absorption. In both of the sets the rate dependence on HNO) . temperllture difference across the column. 29. Some results will now 5e given to demonstrate the relative The formation of HNO) in the gas phase was found to t importance of these features. formation ca 328 March 1991 Vol. DI-D27... The rates of chemical reaction and mass transfer are also known. Similarly.!with respect to HNO) concentration was included (for instance.. the actual concentration of nitric acid. HNO) for a given gas phase NO. u ON HNO. Solution of heat balance equations -Air = 7 mm/s flow rate 5. removal does not depend appreciably on HN Water have been summarized by Joshi et al.JkD)~/2 values Absorption of NOz.cting appropriate values of H(kD)'/z in Eqs.3 of oUtgoing nitric acid (at the bottom of the column) was o 10 15 20 25 30 35 '0 '5 50 assumed. The reduction in the rates of absorption of :--JOz. First of all. composition concentratior and temperat and :--J. A comparison was made between the calculated and Figure 3. tions.. (1985).. the extent of NO. whereas in the second set (broken lines) air was added. appendix D. Q...:. Further.. At higher concentrations of sulfuric acid. the rates are 70 likely to decrease. The heterogeneous equilibria between gas and liquid phase seen that the rise in temperature.. the of NOx absorption. It was found that the gas phase HNO. . reduces the exte species have been included through Eqs.09 NHzS04 solu- tions.-.99 x IO-'kmol/s = method of interval halving. removal in tJ 3.- -=':-":---: 21 acid (at the top of the column) are known. The values of H(kD)lIz for the case of absorption in extent of NO... No. 37. For this purpose Eqs. MODEL EXCLUDING HETEROGENEOUS is a mixture of sulfuric and nitric acids at different concen... were libria.. it was o 2. 30. guess value at the bottom of the column was varied using the NOx flow rate 0. (1985) have 90 critically reviewed the previous work. It can 2.. Solutions of ordinary differential equations . For convergence. the heterogeneous equilibria markedly influence In the mathematical model developed in this work. of absorption... the heterogeneous equilil features have been included: successfully predict the maximum attainable I.. Complete heat balance has been established. To start the integration procedure. . % . It can be seen that the extc same variation was assumed in the case of NOz and NzO) of NOr removal strongly depends upon HNO) absorption. NzO). CONCENTRATION a: 30 Equations 36-40 are five coupled ordinary differential equa. in the present work the absorbent 1. The var. 54% in set I and 39070in set 2).3 AIChE Journa .1 X 10-4 kmol/s = From steps 1-4 the concentrations of all the species are 'Uu Air flow rate =0.: -.

Effect of nitric acid concentration on extent product gas from the pilot plant for producing oxalic acid.. 30.5 Liquid superficial veloc. N0'. It may be emphasized that the relative importance NO.(kN/m') are favored. The I stream was passed through a condenser where the outlet tem- I Packed column dia. The com.re increase with an increase in temperature.' 0-6 0-8 .6 m Packing. 1.. H(kD)I/2 increases with an increase in temperature.0 of NO" IN" is 0. At low HNO) concentrations.36x IO-"s-I :'11.3 329 . o '0 respect to different species. It can be seen that NO" absorption is 2 10 Adiabatic Ie maximum when the air flow rme is 4 x 10-4 kmol/s. .3 rate dependence on nitric acid concentration Case 2. the value of absorption parameter kLa. 77 kN/m' - ~e of the above two factors depends upon HNO) concentration NO'/N'. 323 K at 0 m hI. 1. NO< removal extent of NOx absorption. The o o 0'2 0. These two opposite factors result in an optimum flow i .5 ~\ and column height. The measurement of these indio . gas partial press. Adiabatic " AIChE Journal March 1991 Vol. Model predictions excluding heterogeneous equilibria and 80 . at high Packed column dia. Cone" WI./ tt" A gas stream constituting 19-20% NOt was obtained as a Figure 4.5x 10-"5-1 '00 0'.2. 37.0 m U Packing. However. 101..I 80 idation. .4.5 .154 m'/mJ Je Liquid temp. 0. Outlet Conc.\ I rate. the rates ~ of absorption can be determined if we know the value of the o> % combined parameter Hx(kD)V2 as described by Eqs... 1. 4 mm/s 0. .5 2. 29. -llI Experimental Work and Discussion 60 Measurement of specific rates of absorption :: .1 and at 30°C. Model predictions excluding heterogeneous equilibria and :: including rate dependence on nitric acid concentration . 38 mm Intalox saddles HNO) concentrations an optimum temperature was observed. 6 mm/s Gas superficial veloc. wI.0 kN/m' temperature. 5 50 1sothermal ~ 6 50 whereas it decreases the gas phase residence time for NO ox. Fortunately.re Figure 5. vidual parameters is extremely difficult. However.125 m'/mJ Liquid inlet temp.1 m/s kaO. Effect of isothermal/adiabatic operation on The effect of temperature on the extent of NO" removal is he shown in Figure 6. 07.0.. 0'. . . Case HNO. Joshi et al. Liquid superficial veloc.. 3 2 30 ~'0 UI 4 2 45 a: . and orders with Z II. it is desirable to o know the values of diffusivity. gas partial press. rate constant.. Line No. . The gas stream was at 65°C and contained water vapor. 709. 0. is practically independent of temperature.. bined effect of the above two factors results in an optimum :Jt Total press.10 5 15 :tJI 6 30 'no 7 45 al. hI. 0.33 kN/m' 2 NO. Total press. (1985) have discussed this subject in detail. HNO. Model predictions including heterogeneous equilibria and 0 Z 60 rate dependence on HNOJ concentration II. I m/ s :TIt kaO. Case 3. . 38 mm Intalox saddles . UI ex: 20 and 31. 298 K ..6 m. Experiments for determining Hx(kD)V2 values for N02 and N204 in water and mixed solutions of nitric and sulfuric acids 7 were conducted in a stirred cell of 95 mm ID. 3 30 Isothermal te 4 30 Adiabatic crease in the air flow rate increases the oxygen partial pressure.9x 1O-4kmol/mJ's.25 x 10-' kmol/mJ's'(kN/m') !nt kLa. 1 10 Isothermal shown in Figure 7. 10 kN/m' Case I. 0 Any -'< 1 ld. The contriburion was found to HEIGHT IN METERS .. . . 0. 2 > 2 15 ui. Temperature was maintained by using a constant-temperature bath.0 experimental setup is shown in Figure 8. h~ 'la contribute up to 20070to the overall rate of absorption when 0.. NO oxidation and the formation of N204 Gas superficial veloc. For the estimation of rates of absorption.. 070 Case ~ The effect of air flow rate on the extent of NO< removal is . 0. :'110. . Line No. At low temperatures. of NOx absorption.0 . An in.

GAS STREAM FROM PROCESS 20 'f. The gas stream was introduced to the stirred Cf a~125 m2/m3 through a rotameter. = 6 mm/s Gas superficial veloc.(kN/m2) for NO kLa= 1.~~. ~..n.. Effect of temperature and nitric acid concen. perature was controlled to equal the desired temperature in In all the experiments. Effect of air flow rate on extent of NO" al Packed column ilia. Figure 7. We assumed complete backmixed behavior.. wt/wt 50 'I.10 -4 kmol/s a NO.U)4kmol(s = LI..4. =0..25 x 1O-3kmollm3..~. saturated with water vapor. The gas stream leaving the condenser was and absorption was carried out for 300 s. WATER IN CD STrRRED CELL 95 mm DIAMETER WATER EJECTOR o CONSTANT TEMPERATURE BATH 0~TO G) TEMPERATURE TRANSMETER (CONTACT THERMOMETER) CD TEMPERATURE CONTROLLER o HEATING PAD G) TT o ROTAMETER G) WATER JET EJECTOR CD 2 -4-.o:... hI. = 0.33 kN/m' NO.:: -30'1. Total press. I>.. =0. (96 'f. CONCENTRATION = 0 'I.-.) CD Figure 8. ~(). Experimental setup in stirred cell. gas partial press. FLOW ~% '0 % IU 50 COl FLOW = 2'15.. .".s. = satUrated rates of absorption by about 5070.-. During this peri. AIR FLOW RATE IN k malls.:. 60 100 .5 m sorption Packing = 38 mm Intalox saddles Liquid superficial veloc. NO. It was analyzed for divalent and there was no appreciable change in the absorbent quanti tetravalent nitrogen oxides.5 30 INLET HNO.. NO. .'.. the absorbent quantity was 120 rn the stirred cell. = 10"10excess the extreme plug flow and back mixed behaviors will differ tl H20 partial press. 330 Mardh 1991 Vol.. INLET TEMPERATURE = 303 K SUPERFICIAL LIQUID VELOCITY = 7 mm Is 20 10 5 10 15 20 25 30 35 50 55 '0 '5 TEMPERATURE. 3 AIChE Jour '''''-. The flow rate was adjusted'in such a w.~::. a 70 a ._~'~'i:.~~~t . 104 tration on extent of NO" absorption.~ . o 2 6 8 10 12 Figure 6.I I <t ~60 1. = 33 kN/m2 that the extent of absorption was less than 10070.. '0 'I.05 nated the uncertainty regarding gas phase backmixing becau O2 partial press..I 0:: 0:: NO"/NO~ = 2... --20'1. = 303. "c o .This elirn NO'/N" = 0.. 37..'~" .--....s-1 of NOz. Over 96070of NOx was in the form because of either evaporation or condensation.6 m.« "-"'~:<:.1 m/s kaD= 1.~ 70 10 'I.. 90 >C >C a a z 50 z 80 I>...5 x 1O-2.

12 pseudo mth-order reaction regime.8 96070of the NOx gas used in the experiments.67 rls. For mixed acid solutions: cell [HJ/2 (2/3kD) 1/2]N02.10 It taining nitric acid and 40% sulfuric acid were used as absorb.(kNlm2) at 30.44 x 1O-1i 41. [H(kD)1/2]NZ04 was found to increase 10 2.60 Water.29 dence indicates that the absorption operation falls in a fast 15. 25.519x 10-6 47. The effect of stirrer speed was investigated in the range of Table 3.. Since the absorption operation was found to be independent of kL.60 form to the instantaneous reaction regime.water . [H(kD) 1/2]'1. It can be seen .267x 1O-3W~) (45) ~the The specific rate of formation of HNOJ by the absorption etely of NOx gas is given by the following equation: For water and nitric acid (Lefers and Van der Berg.H2S04 (PN02)J/2 (43) were found to be much lower than those found in water. 3 331 i . 40070sulfuric acid.10 various acid concentrations are given in Table 3. The values of H(kD)I/2 for NZ04 at Wt. These values were used for determining K6 from Eq. in 400.70x 10-6 36. A few experiments were also conducted to evaluate the Temp.HZS04 was obtained from Eq. Nitric acid.C [kmol/m2. 30.s(kN/m') conditions the partial pressure of divalent nitrogen oxides tpNo and PN20J)was negligible.s.10H2S04 at 30'C . is because the activity of water decreases in the presence of The interfacial partial pressures of N02 and N204 are related sulfuric acid.36 of nitric acid. This value is in agree- Acid Concentration ment with those reported in the literature (Sherwood et aI. I (PNO» 312 (44) assumed to vary (with respect to concentration of acids and . It also indicates complete homogeneity of wt. it means that absorption does not con. 44 by using the experimental values of the specific rate of formation of HNOJ. and mixed acid solutions con.168xlO-1i 38.10HNO.95 5. 43: The equivalent nitric acid concentration was estimated on the basis of the same [H(kD) 1/2] values..33 rls..WII.H2S04 [H (kD) 1I2]N204. 40 3.215 -IA2~ . [H3/2 2 (2/3kD)1/2]NO"water The values of [H(kD) 1/2]N20Jand [HJ/2(2/3 kD) 1'2]'102were +3 [H ( kD ) 112] N204.7IRT (I .1o [kmol/m3. The following equation is obtained by substituting 46 were used for the estimation of K6 values for mixed acids.0 wt. 13 and 42 in Eq.and liquid.67 Temp. Joshi et aI.O. 0.616 [H3/2 (2/3kD) (42) = 3. 40 wt. :"-10.93 '-.C.04 Equiv.water way [H(kD) 1I2]N204 x 1O-5e-6263. 40 wt.285. 0.0 2. without any Sulfuric Acid vortex. This also indicates that there is no effect of gas. 1975. [H(kD) I'''' '"]NZ04. Table 4 gives the values . Under these [H(kD)II2]N. Experimental Values of [H(kDl/2]N204 for 40% 0. 0.10 ents. Nitric Acid Concentration EquivalenCto Mixed 7.HZS04(K2(PNOZ)" i for nitric acid concentration equivalent to mixed acid concen- RHNOJ=4/3 tration. 0. Sulfuric acid. This .water H(kD) 1I2]N204. The liquid surface was flat. in Water that the value decreases with an increase in the concentration 5 2. s(kN/m2») x 106 the liquid phase.10 side mass transfer coefficients (kG and kd when the speed Nitric Acid [H(kD) 112)N204'. 37..0 2. It was thought desirable to 15 1.H2S04 PN204 [H(kD) 1/2]'1204values in the presence of 40% sulfuric acid +2/3 [H3/2(2/3kD)1I2]N02.66 X 10-2 W:" :imi. Eqs..97 develop a correlation for [H(kD)II2]NZ04 in the range of tem- ~al AIChE Journal March 1991 Vol. The following It was assumed that correlations were found to hold. Sulfuric acid cone.0 0. 1I2]N02. 0. wt.55 with an increase in temperature. It was observed that the specific rate of absorption was 070 NOx= 19 independent of the stirrer speed when the speed exceeded 0.167 to 1. perature and concentration covered in this work. It was expected that the values ab. [H(kD) I12)N204' effect of temperature on the values of the absorption parameter .H2S04 ause -1.0 1. 0. tem?erature) in an identical manner to that of [H(kD) 1/2]'1204' The value of [H(kD) li2]NZ04.6x 10-6 kmol/m'.3 Tetravalent nitrogen oxides (NO!) constituted more than 20 2.1.8JJe-I. The values of [H(kD) 1/2]given by Eqs.' 30'C for water=7. s(kN/m2») X 106 Hx(kD)~2.O. 10. 45 and by Eq. of [H312(2/3 kD)1I2]N02 and [H(kD)II2]N204 in H2S04 would be lower than those in water due to the presence of electrolyte. 1985).0 2. The value of [H(kD) 1/2]N204for water was found to be Table 4.. 20. exceeds 0. 1982): mL -fioei RHNOJ = 4/3RNZ04 + 2/3RN02 Wi( I [H( kD) 1/Z]N204 IO[-3. All the above evi.6x 10-6 kmol/m2. 13. 20 O. HNO.C rls. Further. 0.JIT (46) ntity = = 4/3 [H( kD) 1I2]N204.

m3/hr 3 3 9 carbon dioxide (some COz is generated due to complete oxi.. gases and entered the liquid circulation 100 currently operated packed columns in series.. .6 3 tetravalent nitrogen oxides. Details pertaining of column 3.~. 11/0).5 m2 2. The liquid product from the reactors consisted of sulfuri acid (40 wt... 11/0nitric acid).and ur Absorption of NDx in a series of packed columns reacted nitric acid (0. counter- recovery of NO.350 1.Oxalic acid was separated b cooling crystallization. 1981): Packed height 4. 37. support plates (d) C6H1Z06+ 12HNOJ-6COz+ 12HzO+6NO+6NOz Liquid distributor 1 1 I Plate heat exchanger 2. circulation loop of column 1..350 gaseous feed for column 1.5 5.5 dation). Polypro. To this stream.5 m2 None These reactions were carried out in two stirred-tank reactOr~ Pump operated in series. 11/0).25 column 1 and the remaining gases entered column 2 and sub 070NOx at inlet 20-23 8-12 3-6 sequently column 3.. The experimental setup and overflow of the column 2 stOrage tank was added to tt is shown in Figure 9. Vol.0 m + 9 NOz Packing type Pall ring Pall ring Intalox saddle (b) 4C6H1206 + 18HNOJ + 3HzO-12CzHz04' 2HzO Size 16 mm 16mm 25 mm Material SS 316 SS 316 Ceramic + 9NzO 2 2 I (c) C6H 1206 + 6HNOJ .254 m 0.8 m 1. . '. Details of Experimental Setup generated in the manufacture of oxalic acid.. 1985) for 9511/0conversion of divalent t( VL 5-6 mm/s 10. The overflow from the colum first two columns were 0.2-0. The column 3 is given in Table 5.2-0..product oxalic acid (11-12 wt. 2HzO + 6NO No.25 0.350 1. The oxidation Diameter 0.column absorption system.. Column 1 Column 2 Column 3 11/0sulfuric acid and 14-15 wt. a measurec pylene quantity of air was continuously added. The gaseous mixtUfi Experimental Conditions was passed through a column that provided sufficient residenci 5-6 mm/s 5-6 mm/s time (Joshi et aI.8 m reactions are as follows (Kirk and Othmer.254 m 0. The volumetric flow rate of this stream was measurec Material Polypro.. The oxidized stream formed th HN03 cone.. . The off-gases consist main!y of NOx ane Capacity. Head. The overflow of column 1 w: These three columns were used for the recovery of NOx gases C.8 mID. The average composition of the liquid phase fc to column dimensions and internals are given in Table 5. The third 3 stOrage tank was added to the circulation loop of column: column was 0. No.. Three.AIR PHE 2 = PLATE HEAT EXCHANGER 2 SP 1 =SAMPLE POINT 1 R3 SP 2 =SAMPLE POINT 2 SP 3 = SAMPLE POINT 3 @) CP 2 CP3 CP1 Figure 9. The mother liquor was used for th Experiments were conducted in three continuous.5 wt. m/s 0. SS 316 pylene using a precalibrated orifice meter.8 m 4.~" -' Table 5.. wt. 070 1.. and 3 m tall. kg/m3 Va. 11/0). .3CzHz04 .3 0..1 =COLUMN1 C2 =COLUMN 2 C3 =COLUMN 3 CP1 = CENTRIFUGAL PUMP 1 CP 2 = CENTRIFUGAL PUMP 2 CP3 CENTRIFUGAL PUMP 3 = R1 = ROTAMETER 1 R2 = ROTAMETER 2 R3 = ROTAMETER 3 PHE 1 = PLATE HEAT EXCHANGER 1 NOX. m water 18 18 22.~~ '.5 m (a) C6H1206 + 12HNOJ-3CzHz04' 2HzO + 31'1z0 + 3NO Total height 6. Some NOx absorption occurred il PL.3 cUChE JoUi 332 Mar~h 1991 \.0 m 3.0 m 6.2-0.254 m ID and 6 m tall. The prqcess con- sists of oxidation of monosaccharides using mixed acid (40 wt.

Table 7. kg/m3 1. centrifugal pumps excess quantity of sodium hydroxide.7 32 HZS04 Experiment 36. at inlet 14 columns in Tables 6 and 8.78 x 10-4 kmolls NO'IN" =0.0 m Total height For the purpose of comparison..9 ActUal NO'IN' at Outlet Simulation 0.14 0. R2. plate heat exchanger chromatograph. IN.9 4. . columns CP I. A favorable comparison (within I5OJo Packing type Intalox saddle Intalox saddle for column I and within 5% for columns 2 and 3) can be seen Size 37 mm 37 mm Material between the predicted and experimental values of conversion Ceramic Ceramic with respect to NOx' The predicted temperarure of the column No.2 5. 37. m3/h Experiments were also carried out in two 0. superficial liquid velocity. Two-column absorption system. Atm.14 OJoNO. No. Comparison between Model Predictions and Experimental Observations VENT 4 Total gas flow =:. GJo Nitric acid 11. the plate heat exchanger was incorporated to maintain the temperature within :I::I 0c.1 13.1 Average Conc.27 12. Liquid Temp. The details of the equipment are given in Experimental Conditions Table 7.350 1.655 0.0 32. concentration was measured by fixing the acid mixture in an Ct. and even then the agreement is 7 good.C At inlet 31 31 31 At our let OIL Simulation 3:.0 32 recycled ###BOT_TEXT### the reactors after adjusting acid concentration (by adding concentrated nitric and sulfuric acids). The percentage Diameter 0.~--~------- --- Column] Column 2 Column 3 ActUal Removal of No" GJo Simulation 52..3 333 . m of water 25 25 columns operated in series.3 31.72 Air flow = 4. Capacity. are markedly different for the first 0. C2. CP2.25 6. wI.0 41.3 4.350 VG. kmol/s NO. Table (I. mls inlet values of NO. The composition of the gas and the temperarure were meas- y CP1 y CP2 ured at the inlets and outlets of the columns. AIChE Journal March 1991 Vol.25 41. The flow sheet is given in Figure Material SS 316 SS 316 10. OJo 6. It may be emphasized that the PL.~_. and the concentra- Column 1 Column 2 tions of various species are given Table 5. rmameters sodium nitrate and sodium sulfate were measured using an ion PHE.70 Equilibrium Removal of NO" GJo Simulation 54.0 m2 None This was because the column was not insulated and the heat Pump losses were not included in the model. sample points standard samples of NaN03 and Na2S04' The liquid phase flow rate was measured by using a precalibrated rotameter.~.63 0.0m 6.629 0. Calibration charts were constructed by using SPI. support plates 2 2 Liquid distribuwr I outlet is somewhat higher than the measured temperature. The concentrations of R I.0 m 10.80 m 0.0 m are also given in Table 6.688 Experiment 0. flow = 1. The liquid phase concentrations and flow rates were also measured. It can be seen that HN03 cone. the results of model predictions 7.5 Pressure Atm.05 3.5 12. Details of Experimental Setup Details pertaining to the superficial gas velocity.0 2.80 m removal of NOx in all the columns is summarized in Table 6. temperature of operation. Liquid phase Figure 10.] x 10. A comparison between model predictions and exper- VL 5-6 mmls 5-6 mmls imental observations is given in Table 8.] 7 X 10-4 kmolls -_. In each recycle srream.5 the agreement is within 5%.1 Sulfuric acid 40. The qualitative description of the process is the same as that for Figure 9. I I Plate heat exchanger 15. Packed height 6. The liquid phase in all three columns was circulated ###BOT_TEXT### get a sufficiently good @ @ flow rate for wening of the packings.565 0.8 m ID packed 15 15 Head. Atm.85 Experiment 59. SP2._~.

as she However. Therefore. Pressure 18-19 kN/m:! panial pressure of tetravalent nitrogen Liquid Temp. "III. 9. Experimental Observations N:!04 with respect [0 concentration of nitric acid 2. :'-. absorption were not considered in the present model. absorption is high in the bottom region.. 5 6 8 250 mm ID column (column 1 in Table 5).I.1 X 10-4 kmol Total flow rate of gas phase 1.267 X II - ~ .. the extent of NO..o3kmo~. the specific rates of absorptie Simulation 58 23. x'0') kmol~/ s erogeneous equilibrium was practically established. The results are given in Figure 11.0 Specific rates of absorption of N:!OJ in water and mix Experiment Actual NO" /N" at outlet solutions of sulfuric and nitric acids were measured in 8 Simulation 0. Complete energy balance Column I Column 2 Total The new model is capable of incorporating the effects C imum permissible concemration of nitric acid on N Actual Removal of NOn % sorption. Therefore. This was indeed found to t pressures for a given nitric acid concentration. flow=3. :'-. absorption. the contrib [0 the extent 0 Therefore.66x lO 'e Simulation 37. 60 Mixed acid concentration is given in Table 6 z o . PERCENTAGE NO. ..8 56.\IChE March 1991 V III. "10 Simulation 39.0].333 No.. Tables 6 and 8 show a compa UJZO FLOW RATE OF NO.()4=3. the HNO:! concentration exceeds about -+m.'" 90 Table 9. at I m height. :'-. '0 = 0. 29-32. °C At Inlet 31 31 <>263. Comparison between Model Predictions and I. The following correlation was found to holt Sulfuric acid 42. AT THE BOTTOM NO" / z . in the present set of experiments.78 x 10-4 kmc 80 Flow rate of NO.0 43..5 x 10-4 kmolls nitric acid concentration NO"/N" =0."'t. Figure II. Variations in the rates of absorption of NO. As a result.. Simulation 55.74 x 10-3 kmolls 4.' - ._j. Formation of nitric acid in the gas phase Air flow = 1.. the rate of NO.5 tration. the rate becomes very low when the packed height Figures 9 and IQ.0 [.9 77. Effect of column height on the extent of NOx absorption.3 81.3 Average cone. 23-28. Removal of :"'10" 070 mixed acid solutions. this work.0 range of 0-20 wr. The gas and I o HEIGHT FROM THE BOTTOM. for large packed A mathematical model has been developed in whic new features have been included. the extent of NOx removal was measured i o 3 .81..- Hr(l-1. as report NO:! and N:P.2 ~ o 50 COLUMN DIAMETER = 1.318 0. 'Column I.0 2.226 water were found to agree with the published literal Equilib. 37. J 334 " ..Is between predictions and experimental observations wherl FLOW RATE OF AIR = .._.3 20. (U2 NO" IN" ratio at boltom 4. /. Eqs. The observed rares of absor~ Experiment 0.~J. As the height increases.7 77.107 3. Extent of NOx Removal in 250 mm ID Colum 7. 070 found to decrease with an increase in the nitric acid :O. removal is controlled by he UJ l- X TOTAL GAS FLOW RATE = 2.I: Total gas flow=2. At the bottom. Removal of NO.C I- 30 = z TOTAL PRESSURE ~ 101 '33 kN / m heights./S geneous equilibrium. = 6 '10' kmol. Heterogeneous equilibria between NO.3 31."9s".I. most of the liquid phase was recycled. the driving force contin. AT THE INLET = Z.0 32..9 21. . 1)10HNO.Z5m 41. Eqs.. It can be seen from Figure II It may be noted that in all five packed columns stud that the rate of NO.616x 10 At outlet [H(kD)i :!IN. Table 5 o AVERAGE TEMPERATURE 33. Above a certain height-say 4 m in Figure II-the overall absorption operation is controlled by the ox. are high compared with the equilibrium partial Counce and Perona (1983). in 40 wr.7 Experiment 36.l7x 10-4 km( Flow rate of air ~ 70 Column details are given in Table 5 u '" Superficial liquid velocity 6 mm/s "'" Q. uously decreases. Atm. 070sulfuric acid Atm. These are: Table 8. 10 In order to check the validity of the mass transfer Eqs. Thus. .8 m height is given in Ta':>le 6 o.itricacid 6.7 VI Experimental CD . the partial pressures of liquid phase attains a constant composition.5x 10-3 kmol/s NO.239 cell with tlat interface.1. Conclusions idation of NO in the gas phase. 29-32.331 0. The agreement between the model predi The extent of NOx absorption increases with an increase in and experimental observations can be seen to be within the packed height. In 1 m packed height. SUPERFICIAL LIQUID VELOCITY = 6 mm/s Extent of removal at 4. heterogeneous equilibrium cond are not established and the rate of mass transfer is th( trolling step. m samples were withdrawn at a distance of 1 m from the bt and at the top of the column. is high at of HNO:! formation and decomposition the bottom.

. m ( Yx). kcal/s (1983 ).2 = absorption factOr for fast pseudofirst-order reaction YNO. 55 S = cross-sectional area of column. Rax:o = rate of gas phase mass transfer of component x. Chem. H. = forward reaction rate constant for reaction n exponent of nominal packing diameter. = Yx at exit of differential height :quid H(kD) 112= absorption factOr for fast pseudo first-order reaction. Valentin. (kN/m2) Greek letters mm KH = heterogeneous equilibrium constant..(1958). Rax L = rate of absorption of component x. (kN/m2). = kmol divalent nitrogen per kmol inerts . K WN = wt. = total moles divalent nitrogen oxides NO!. kmollm3'(kN/m2) ed in ko = physical gas-side mass transfer coefficient. m (X). 361 \ Qc = total heat changes in gas phase.n = backward reaction rate constant for reaction n . (kN/m2) 51770. Eq. Eqs. Eng.and p." Chem. 3 335 i ( . Eq.' . m Yx mol gaseous component x per mol inert 1 the H = tOtal height of packed column. 4th Eur. m/s [A. 61 ES = fractional solid holdup N. kmoll(m3s) is served between the model predictions and experimental ob. kmollm2. Chem. m /Joo= viscosity of gas L = flow rate of liquid. Scl. G. ( Yx). I = characteristic length of packing. - Andrew. 35. (suppl. kcalls Carra. 189 = heat changes due to oxidation of NO in bulk gas. P. kcal/ s Carberry.. = heat changes due to formation of N20] in bulk gas. J. m2/s (X)o = component X oxidized in differential volume ~isan f = friction factOr (X)v = component X vaporized in differential volume . "The Dynamics' of Nitrous Gas t. 22.(kD)'. = kmol reactive nitrogen per kmol inerts H.). K a = interfacial area. kg/m3 tions K6 = heterogeneous equilibrium constant.] = saturation concentration of gas phase reactant in Vo = superficial gas velocity. C3 = 1i by k. Eq. kmoll(m3s) ReL = Reynolds number for liquid )i 5 s = exponent. m2/s (X). and F. ~. = mass velocity of liquid. Pigford. m2/s3 = T = total Pr = toral pressure of gas. m2/s (X)f = component X formed in differential volume Do = diffusivity in gas phase. 329 <~~ ) Qr = total heat change. partial pressure of inert in bulk of gas = a absorption p.. Eng. m2 Notation Seo = Schmidt number for gas T = temperature. kmollm3. A. A favorable agreement was ob. s /Jow= viscosity oi water Lw = latent heat of vaporization of water. kcallkmol € = voidage mO mass flow rate of liquid. (kN/m2) Z = coefficient. t ihe = heat changes due l0 formation of HN02 in bulk gas. kmol/s /JoL= viscosity of liquid L.. kmolls = EO = fractional gas holdup iour m = coefficient. 61 EL = fractional liquid holdup n = exponent. I = inlet condition i = partial pressure of component x in bulk of gas phase L. frac. Carleton. ~able for component x. s YHo. 34. Q6 = heat changes due to water evaporation in bulk gas. kmoll s G. Chem. Eq. Eqs. kg/m3 ###BOT_TEXT###. Hw = solubility in water. K a~ = dry area of packing per unit volume. C3 'Y= :true k . = component X at inlet of differential volume [era- DL = diffusivity in liquid phase... het. = equilibrium constant for reaction n PL = density of liquid. Eq. H. Symp. QL = toral heat changes in liquid phase. kN/m2 . kcallkmol phase per kmol inerts con. s YT = total moles gas per mol inert h = height from bottOm of packed bed. m/s {3 exponent of superficial liquid velocity.::J>= pressure drop in packed column v = vapor (acid x = x in NO. = = parrial pressure of component x in bulk of gas e exit condition p. "Some Remarks on Chemical Equilibrium and Kinetics td at Q. in bulk gas. C3 nthe kL = physical liquid-side mass transfer coefficient. and D. = Yx at inlet of differential height kmol/m2. Eq. J. m2/m3 t!.. Proc. K) 800 mm ID packed columns. (g) = gas phase ::a\~ p.T = temperature difference. kmol water in form of oxyacids and free water in gas tions 2 = lli = standard heat of reaction. In kcal/ s Literature Cited \ere Q] heat changes due = kcal/s to formation of HNO] in bulk gas. Pm = power consumed per unit weight of gas holdup. 55 tions HNO = solubility of NO in water." = coefficiem. Ind. S. s = [[Om YN. Eq. Pergamon. Eng. X(/) = component X in aqueous phase ares. Hanson. ~es: kcal/ s . 37. limiting partial pressure of component x at gas-liquid = = f formation interface = p~ = partial pressure of component x at gas-liquid interface G. NO. Eq. kg/m2. s. Oxford. In' Absorption of NOx gases was carried out in 254 mm and R = universal gas constant. = solubility in electrolyte. 9. Absorption.en- Q. Scl. m2/m3 VL = superficial liquid velocity. (m3.~al AIChE Journal March 1991 Vol. = component X at exit of differential volume Dx = diffusivity of component x. kmol/m3. Q. Sci. t kcal/ s Reaction Eng. . = mass flow rate of gas stream kg/m2. = tOtal moles tetravalent nitrogen oxides Subscripts . ~o. trred kcaJ/ s !~ :n Q2 = heat changes due to formation of N20. F = packing factor X(g) = component X in gas phase G = flow rate of inerts. (/) liquid phase ab. Eng. 14. m/s liquid phase W = wt. Fundam. 105 (1961).~nd = tOtal moles NO. kcal/s (1968). O?o HN03 in mixed acid dh = differential height of column Xx = kmol x ions per kmol water dp = nominal size of packings. kN/m2)/(kmol.. L. HN03 in aqueous nitric acid solution e~ = average specific heat of liquid phase. and R." Chem. )L' 5 servations. C9 K. kcallkmol. in the Nitrogen Dioxide-Water System. kmollm2. S. 36 Po = density of gas. 36 ex = coefficient. (kN/m2).

" + 2 ( YNZ03) + Y HN03 + Y HNOZ (i G. New York . H. Wohlfahrt. J. 3rd ed. \lakhotkin." Ind.. Sci. 19. R. J. YN' = YNO + YNOZ + 2( YNZ04) Chern. in terms of YNO... Eng. YT( Y. 37.. R.. 33. "A Mathematical Model for an Absorption Tower of Nitrogen Oxides in Nitric Acid Production. Perona. E. Gases.. 52. Counce. Sada.. 1011 (1960)... Proc. Kondo." Chern.). Demonstrated by In computing gas phase equilibria. Sada. Kobayashi. YNO" YH.jPT Y'IOY'Io:YH:o) Sci. 1. Gas-Liquid Reactions.. V. Kita. and E. Eng.+ YHNO] For known molar concentrations of inerts. Co. and P. Van der Berg. Chern. YHZO" = YHZO + 0. and T. K. ( YHN03) Kirk and Othmer. 426 (1980). and F. "A Mathematical Model for Ni- YNZ ] =K]YNOYNO. Des. V. Japan. Chern. "Estimate Tower Pressure Drop. and 1. Juvekar. Selby. Eng. [KSPT( YNOZ) YHZOi ' Y'\Io] . V.~. 1917 ( 1988).Y~~ I (K.. E. Pangarkar. 163 (1977) . C. J AIChE JOUi . 29. V. Shamsutdinov. total reactive nitrogen per mole of inert. Sohlo. "-'. .. V.. Chern. YNZ03." (in preparation. Eng.. Eng. 20. PTIYT . and A.. (f YHN03- (1970)." Chern... Matasa. and J.o. J. E. "Absorption of N02/N204 into ( YHN03) + 0. Eng.. Develop." Chern. 32. J. Res. Sherwood. Encyclopedia of Chernical Technology. and YT are obtained. 135 (1979)." Ind.5( YHNOZ) (. Basi!: Nitrogen Cornpounds. Marek..!.K]PT YNO YNoz =0 (A Gas Phase Equilibria I/Z The total number of moles in the gas per mole of inert is YT( YH~O" . F. . I. A6. and J.. YNO' = YNO + YNZ03 + 0. "Reaction of Aqueous Nitrogen Diox. R.1/2 Y~~ I (K4PTYNO Y"o~ YHZO) obtained by adding ratios of all gaseous species to mole '01' 3 i/2 + [K.5(YHNOZ) ..K] YNo YNo:] =0 (P Nitrogen Oxide Gas Mixtures. . Hoffmann. and J. YHZO) .562 (l979a). Wilke. Hence Y for the Production of Nitric Acid.. YT( 1) Y'IO + Y"o~ -+-YH:o + Yo: + Pub. They are: 19(9)." AIChE J.o. and J. Chern.. J. "Aqueous Scrubbing' of Dilute . M.6070 Perforations. R." Ind.::. Chern. P.O~YH~O)I/Z Appendix A. New York (1973). Koukolik. Mahajani.. Chern.PT Y"o~ Y"o. A. V.. Chern. u ° trogen Oxide Absorption in a Sieve Plate Column.. N. 16. 1171 (1977). G. Tekhnol. Counce. 18. and M. Hoftizer.5 Diluted and Concentrated Nitric Acid. McGraw-HilI.. 347 (1968). V. "Absorption with Si- multaneous Complex Reactions in Both Phases. When these are sub Mahajani. Perona.5 Wiley. 1.. (sup pI. A7: and A8. Honhabel. B. whereas the extent of oxidation at any moment is expres Kameoka.. Eng.26 (1983). Y"o:) ." Cornput..YHNO~'and YH Sept. June 27. Estimation of Partial Pressures of 3 I!2 ] Various Gaseous Components on the Basis of . No.~. Chemical yj. J. P.1411 (1976). J. "Absorption of NO. 18.. 23. Y'IO" YH. Pigford. t NO~.YV~ {[K. "Scrubbing of Gaseous Nitrogen Oxides in Packed Towers. equilibrium partial pressure -r YHNO. water vapor per mole of inert. Fundarn. T." Chern. 400 (l979b).623 (1981).. It is expressed as: ide." Chern. : + [KSPT( YNO/ YH~oIY'lo]1 I . -[K.. S. Eng. Eng. L: "Absorption of NO in Aqueous Solutions or KMnO. moles of divalent nitrogen per mole into Water.Pr( Y'IO~)3 YH~O'Y'lO]li~ + (K.jPT Y:-ooY"oz YH~o Onda.. all the gaseous species in the bulk gas can be estimated \ 336 March 1991 Vol. Counce. and 1.. S. and J.. M..67 (1983). .jPTY'IOY'.. YNZ04 = Kz( YNOZ)zPTIYT u sorption in a Sieve Plate Column. B. G. 1990). Lefers.. "Gas-Liquid Interfacial Area of where a Sieve Plate with Down Comers and 0. Joshi. I (1985). 3. M. YHZO' is moles of water in the form of oxyacids and I Koval. Pergamon. 16. Equations A2 to A5 express YNZ04.. AI. and Alkaline Sodium inert: Sulfite Aqueous Solutions.2PT[K~( Y"o~): cGraw-Hill. 132 (1982). Sulfuric Acid. Oxford. 211 (1982). four equations in Y A Quick Look. "Absorption of Nitrous Gases. Develop.~' Counce." J. T."". New York (1975). Sodium Hydroxide. we assume that then the Modeling and Calculation of Counter-Current Flow Columns no formation or removal of reactive nitrogen." Cornput. and NO" to (N") ratio. "Absorption of Nitrogen Dioxide in the form of YNO'.." Ind.. Peters. R. "Figuring Packed-Tower Diameter. L. and J. YT= Y"o+ Y'Io~+ Y'I~().~. and C.. Pigford. Perona. Fundarn. J. Syrnp. "Gaseous Nitrogen Oxide Ab.Vfass Transfer.""":'-". A. Ita. ~ . . Kwanten. and R. Kumazawa. and U. Perona. K. (l Proc. London (1972). B. "Mass Transfer in Packed Column: tuted in Eqs.. Tonca.. Chern. Eng.. 143 (1979). Proc.. 18 (1970). Eng..Y'IO. Des... 3.. V. and K. ." Ind. Cornrnun. Eng. oxygen. K. H. M. React. Eng. 3.0. 27. Hayakawa. and YT.* . Eng. . R. I/Z Ks( YNOZ)3yHzO PT Danckwerts. Chern. [ Y NO Y TJ Emig..K:PT (Y'IO~)~]=O Eng. and R. Butterworths. K. Gas Purification Processes for Air Pollution Control. (. and V. YNO) -1/2 Y~~ [(K. New York. M. Niranjan. YHNOZ= (K4YNOYNOzYHZOPTIYT)1/Z Counce. V. G. is expressed as: Holma.. . G.j+ Y'I~(). W. J. 4th Eur. Kudo. Chern. Khirn.. "Salting Out Parameters of Gas Solubility in Aqueous Salt Solutions.. Mahajani. Joshi. YT( YNO* . M. L.PT (Y'\I0z) YH~oIYNo] =0 (A inert. Eng.." Ind.. Khirn.O + Y(h -r I (AI) . B. + Y H. Joshi.

Az (p{. HN02. 3.2 (C6) by EL= l1.9x IO-SReLO.o) + A3 (p{.=3A) type of packing. No.. and 26-35 into Eqs.j: :: and Values for Ct. 37. 6-15.)N204 ~ of j 0. A9-A12 simultaneously for Yr.. B 12 ( PNO + B S ( PNO I i ) ( PN02 ) all the packings. B S ( PNO + B 6 (PN02 ) 2 + B 7 [PINOPN02 i . . and 'Y for different pac kings are as in Table B I [P iNOZ - i 1/3 I B 2 ( PNO ) ]3/2 + B JPN02 + B ~ [ (PN02 ) I 2 AI. 34 and 35: 812=As (A5) 1/3]312 A I [PN02 . 1982) used to deter- mine flooding conditions is: (A6) where In Y=.53X 1O-4+2.oZ)2 .:) Bo = 3A5 'nal AIChE Journal March 1991 Vol...66(. A2-A5. Mahajani and Joshi (1990) have developed correlations :) for gas-side and liquid-side mass transfer coefficients based i ) 213 ] i .7s1d. IIZ and Physical Properties . Compositions of HN03.1 A3 = (2K2 ~ HNZ04 [(kD)N20/12) 13 - Y= (A7) PL PG A4= I/(Kz K~/3) free As= (K3 ~HNZOJ [(Dk)NZO/I2J/3 X =~: ~:r/2 IIZ A7 = (K4 pkzo) KL'!. K3 (kG~)NZOJ P=Z(dp)-S (C2) .z= (kG~)NOP~O+ (kG'!.(k~)N02PRi02 .)HNO:PHNO/2+(kG~)N20~Ri203 Ct VL(3(dp)r '!. 26-35 8ll = . 6-15.0814 In X. . + B 10 ( PN02PNO 062 ) 1/2 T' B II =0 (B2) k (GRT) I (Pm/) 'I PG 1/3 Px 0) 0. (3. A2 (p{.. i i 1!1 .AS(PNO) ] + A9(PNO) (PNOZ)+AlO(PNO) (PNOZ) The column diameter was estimated on the basis of flooding + A I iPNO + A 12 = 0 (Bl) calculations.(k~)HN02PHNO/2 (A4) The following two equations are obtained by substituting . 23.(kG~)N203PRi203 . solving Eqs. All = . B<=A4 Liquid holdup in the packed column is computed as 'oral B~ = 2K2 (kG'!. 1. (C3) E' .(A8) As = 1/ (K~I2K~/3) A9 =. The correlation (Mahajani. i ) 4/3 ] B 2 ( PNO on turbulence intensity.)HNO/2 The correlation employed for computing the effective in- Y"Q.)NO terfacial area (Joshi et aI.HHNO/6 I/Z Packing factor P was calculated from the equation.G 1 J (Sed G) i where where Pm is the power consumption per unit mass of the gas Ill) BI=3AI fap vl B2 = A2 Pm= [6(E-Ed] 4 (C5) B) = (kG~ON02 -: I is the characteristic length of packing. Eqs. 23. They have shown that the following correlation for the gas-side mass transfer coefficient holds for i I ) 1/2 I ) 213 ] + B 9 [( PNOPN02 . 0.A4 (p~O)2I3] + As[P~~oz . N203' and N204 are (A2) obtzained from equilibria relations.1273 (In X)2 (CI) AI = I~ (HNOZ)3/Z[(2/3 kD)NOZ]1/2)/3 ~ssed where Ie of Az= I/K~/ZK6113 (O*)2p J1. Estimation of Design Parameters Y~*.553 (C4) DG l J1. its value depends on 2) B..2(kG~)N204PRi204 Eqs. 89=3A7 810= -AIO (A3) Appendix B. Table AI. 1985) in packed column is A. .O)4/3] + A7[ (PNO) 112(p~OZ) IIZ ~re IS Appendix C. Simplification of Eqs.1. YNO' YN02' and 8s = .~.3 337 .flNO) bsti.(kG'!. 2/3 112 . . AIO= .(K4 pkzo)112 (kG'!. .3861.A9 YH o.

LSdh (0 Values of coefficient 1/ are listed in Table AI. (HNO)j=G( YHNO). 37.cSdh ([ 10glO(He/Hw) = -f. The value of ig f( ILL E HNO) was estimated from the vapor press un: of HNO) OV nitric acid. Values of Constants in Eqs. The value of ig for HN02 was assumed to be t1 The specific surface area is calculated from the packing same as that of HNO).YHN0Jol)+ RaHNO).463.K. (1970) have reported the values of salting-out paramete dp VL PL for various cations.1. The rate of formation of N20) from NO and N02 in tl from the following correlation: differential element is given by: 0.090 and The rate of heat generation due to N20~ formation is: 0.96 -1.0 contribution of the solute gas. and gases. 1983) Q. For this purpose.178 (CI2) 3.337 . The rate of formation of NZ04 from N02 in the diff( ential element is given by. " """. Liquid-side mass transfer coefficient kL has been estimated I.~h"'~' .015 0.and i. Pressure drop in the packed column was estimated by the The rate of heat generation due to NzO) formation is: following correlation (Niranjan et a!. 1985). (0 (N204)j= (N204)h .e .0 0.'.478 7..913 4.403 27. respectively (Joshi et a!.33 x H"o) =.53 -1.3 AIChE Jourr ( .(N204)i + (N204)a (T/298.74 .ldp 0.(NZO)i + (NZO)a (NzO)j= G ( Y"zo).' .4 19.07 O.i) + Ra"204.533 2. YN204.7 Intalox saddles 2. to the following steps.5 (0 (kd/Dd =1/ReL ( ) P:~L (C9) (NzO)j= (NZO)e . = (NzOJ)j ilii4 (0 f( G* )2a p (M'/h) (ClO) = [6 PC(E-Ed] 2. :"/0.' .+i.484 kmol/mJ.091 1.+i. Oiffusivities of gases vary with temperatUre and pressure..l (CI3) - where The rate of heat liberated due to HNOJ formation is.6 0.(HN02)i + (HNOzJa (0 338 March 1991 Vol. anions. the following correction was used..'..'"" ".1 843 0.are contributions of carions and anions of the elec- trolyte.4 Pall rings 2. The solubility of NO in water is given by the following equation: Q2 = (N204)j ilii) (I: roglo (101. (kN I K. ~ Table AI. 2.e. CI-Cll f a {3 Z s 10-2 Pac kings m n=-y "X Raschig rings 3.25dp 28.Y"Z0Jol) + Ra"ZO).5dp 8.76 4.5 0.800 1.LSdh The solubility of HNOJ and HNOc in water is 2. kmol/mJ.2)L75(101. (1977). Q) ([ Hw=solubility in water. The value of ig for N ReL= (C7) gas was reported by Sada et al. The rate of formation of HNO) in the differential elem( is given by: The solubility of NO and HNOc in the presence of electrolytes like HzSO~ and HNOJ was estimated by using the fullowing (HNO)j= (HNOJ)e . The rate of formation of HN02 in the differential elem( is given by: i.e. Heat Changes Gas phase heat changes Values of m and n for different packings are given in Table Contribution to the heat changes from the gas phase are d\ AI.".(HNO)i + (HNO)a ([ equation. respectively.32IT + 2.17 3.=salting-out parameter = i. (kN/mz).(kN/mC) = (HNOJ)j ilii6 mC) Hel = solubility in electrolyte solution. kmol/mJ. to the salting-out parameter and i" is the (HN02)r= (HN02)e . Oanckwerts (1970) and One where the Reynolds number is given by et a!.03 6..33/ ?T) (CII) Dx=DdS'C (0 (N204)j= G( Y"204. diameter as ap=m(dp)n (C8) Appendix D. 4. 1.

e-1I2 YHNO).)+ 1/2 HN03. (01) The rate of heat generation due to NO oxidation is given by: Heats of reaction are summarized in Table 2.e-YH2o. 37.NO. 27. 1990.LMl9 + RaN203. (D6) l1enr {Oi) (08) ":: ID9) :nent DIO) --"al -\IChE Journal March 1991 Vol.LMls + RaN204. It reaction Jnda may be noted that NO is used in the N203 and HN02 formation In the absence of information on heats of dissolution of :eters and it is liberated during HN03 formation.i ~ due (4) 3 HN02(l)-HN03(l)+2 NO(g)+H20(/) (D23) -112 YHN02.3 339 View publication stats .GMlII + RaHNo2.LMlI3) S dh (D26) iffer~ (H20)u= (H20'e.f (DB) (2) N204(g) + H20(/) .f (1) 2 N02(g) + H20(/) .(RaN203.e.o = (NO'i.f+ 112 HN03.i. (04) + 1/2 YHN02.. The rate of heat liberated due to the oxidation of NO is Heat changes due to absorption with chemical estimated from the knowledge of the rate of NO oxidation.e.i+1I2 YHNO). No.e+ YN203. HN03(/) + HN02(/) (020) .f+ 1/2 HN02.112 HN02. YN203..e-l12 YHN03.) n the (5) HN03(g)-HN03(/) (D24) .112 RaHN03.L ..f (DI6) Total heat change in the differential volume is the summation (H20)u=G (YH2o.2 RaHt>i02. and rel'isian received .Vot'. 1990.G) S dh) (DI4) (6) HN02(g)-HN02(/) (025) .e+ 112 YHN02.LMlIO 1D3) The rate of water evaporation in the differential element + RaHNO).dS dh (DI7) Jfanuscripr received June 12.N203.i of all the heat changes. H20. YNO. .) + RaHN02.G Qr= QG -+ QL (D27) ID5) + 11. for given by: Reactions under consideration for the heat balance are: over e the NO.LSdh (Dll) Q6 = (H20)u Lw (DI8) 2 :) ~ The total heat change in the gas phase is given by: The rate of heat liberated due to HN02 formation is: QG=QI +Q2+Q3+Q4+QS+ Q6 (D 19) Q4= (HN02)fMl7 (DI2) 5. HN03(/) + HN02(l) (D2I) (3) N203(g) + H20(/) -2 HN02(l) (022) = G( YNO.e) .LMlI2 was obtained by material balance: + RaNo.YHN02.) + (112 RaHNO).L + 112 RaHN02. (HN02)f= G( YHN02.e-1I2 YHN02. gases the information on heats of formation of reactants and rNO The mass balance for NO across the differential element is products was used to compute the heats of reactions.i+ 112 YHN03.. (02) Qs = (NO)o Mil (D 15) Heat liberated due to absorption with chemical reaction in the liquid phase is expressed as: Heat changes due to water evaporation QL = (RaNo2.

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