lolnlateletetetatatets EXPERIMENT (5) SOC@05D ABSORPTION WITH CHEMICAL REACTION iFT eT SOIT TPDSPECEOHOOROEODESCOROCROGOCE ABSORPTION WITH CHEMICAL REACTION Introduction Absorption is one of the very many separation processes used by the chemical engineer. In absorption a component of a gas stream is removed by passing the stream over the surface of a Kui, the component to be removed being preferentially soluble in the quid Large surface areas and inti The packing are divided into three principal types 1. Dumped packings (loose packing method) 2. Stacked packings (dense packing method) 3. Structured or ordered packings. Common dumped packings are illustrated in Figure 22.2 ‘The diameter of a packed absorption tower depends on the quantities of ‘gas and liquid handled, their properties, and the ratio of one stream to the other. The height of the tower, and hence the total volume of packing, depends on the magnitude of the desired Concentration changes and on the rate of mass transfer per unit of packed volume. Calculations of the tower height, therefore, coaeniteral balances, enthalpy balances, and estimates of driving force and mass marsha, coefficients, Absorption processes are classified into physical absorption (no chemical reaction) and absorption with chemical reaction (chemical reaction enhance the absorption). Common Sxamples of physical absorption are the removal of small percentages of ammonia, sefur dioxide, oF carbon dioxide from air using water. Examples of absorption wit veare al oF carbon dioxide from air using a solution of sodium hydroxide and sodium varbonse ty ‘Water and a scrubbing ammonia from gas streams using diluted acid solution<< 605 ‘niet @ @ te 0 @ FIGURE 222 Common tower packings: (a) Raschig rings: (b) metal Pll rng: () plastic Pall ring: (d) Ber saddle; () ceramic Inalox saddle; (/) plastic Super Inalox saddle; () metal Imalon sade SETI Steger es tame tig non nee ae fe wa adn « i c € € €Theoretical Background + PHYSICAL ABSORPTION Physical absorption is covered here to refresh your memory about the subject and introduce You to the topic of the experiment which is the absorption with chemical reaction Gna micro scale there is mass transfer of the soluble gas by convection, then by diffusion through a gas film at the surface of the liquid, and then through a liquid fm into she irene Of the Tiguid. The microscale mechanism of physical absorption is described in the figure below, ‘The mass transfer steps of the soluble gas are: 1. Mass transfer of the soluble gas from the gas bulk to the gas/liquid interface through the «gas film by diffusion 2 Mass transfer of the soluble gas from the gaviquid interface to the liquid bulk through the liquid film by diffusion {t's assumed that turbulent mixing produces a uniform composition of the solute of both {he gas and the liquid phases outside the film zones at any point along the flow path through the system. assume equilibrium at interface, or ° Pri = Hae Sa and take Ha. = constant, thos Pais Ha Cy:Principles of Absorption Instead the variation in composition are continuous from ne end of the equipment to the ther. Material balances for the portion of the column abort on arbitrary section as shown below by the dashed line are as follows Materia-balance diagram for packed column,Total material: £,4+V =1+V, a Component A: Lx, + Vy = Le + V,y, @) ‘Overall material balances are: Total material i, +0, = b+ V¥, @) Component A: Lky + Vidy = lat, + Vey, (4) Manipulating equation (2) yields the operating-line equation for a dforential-comtect qiuibment (this equation is analogous to the equation for the distillation column/stage contact equipment) ~ 4x, po (5) are transfer of @ soluble component from a gas mixture would cause a decrease in the total gas rate Vand an increase in the flow of liquid L, These changes make the operating line slightly curved as shown below (Figure 22.10). But for dilute mixtures, containing less than 10% of soluble gas, the effect of changes in the total low is usually ignored and the design is based on the average flow rates The average slope of the operating line is L/Y”, the ratio of the molar flows of the liquid and gas. A reducti L£ decreases the slope. Thus the minimum LIV, (Lf ug, is the slope ‘when the bottom compositions are (x.y, ) which le on the equilibrium line ee ehown in the figure below (Fig. 22.10). In any actual tower the liquid rate must be greater than this Iminimum to achieve the specified change in gas composition. ‘The /V’ tate important in the economics of absorption in a counter-curvent column, The driving force for man i ansfer is » ~ y", which is proportional to the vertical distance between the operating line and the ¢awifibrum Tie on Fig, 22.10. For more information see the attached reading material L yoty,Rate of Physical Absorption r=K,a(p—y* (3) r=K,ale—x) ) The interface composition (,,,) can be obtained from the operating-tine diagram using eq, (6) and (7) = ta 1 Xx ka 0% Hence, a line drawn from operating line with a slope ~k,a/k,a will intersect the equilibrium line at (x,, y,) as shown in Figure 22,12, 1 I m >= — 11 Ka” ka ka o 6 TOBA MN Ame « € e 2 Pease Cw?(a2) Where m isthe local slope of the equilibrium line (y" = mx’) FIGURE 2212 Location of iter Caleulation of Tower Height (Thi Sr your information = 66 is at uted for He assgnmeite) ‘The overall gas-film mass transfer coefficient is the common one used for absorption rate NTP. SBMA RM an ee c-<- FO SST TSP DBEIOTHSCOCHCOD000H0H0L80008 + Height of Transfer Unit (ATU) ATU = (20) HiT of @ wansfer unit can be defined as the height of a packed section required to accomplish a change in concentration equal to the average driving force in that section, Value of HTU of a particular system are sometimes available directly from the literature oy {fom pilot-plant tests, but often they must be estimated from empirical correlations for the individual coefficients or the individual height of a transfer unit.ABSORPTION WITH CHEMICAL REACTION If the gas reacts chemically with the liquid, or some Component in the liquid, then the fgaid prion in the liquid phase is low or zero, which enharoes mass transfer through the the solute over the solution, which greatly increases the driving force for mass transfer. If the reaction is essentially irreversible at absorption conditions, the equilibrium partial Pressure Case A 7 _ Instantaneous reaction with respect to mass transfer Case B > _ Instantaneous reaction; High C, Case C - Fast reaction; Second-order rate Case D > Fast reaction; High C,,, hence pseudo first-order rate CE and F ~ Intermediate rate with respect to mass transfer Case G ~ Slow reaction with respect to mass transfer Case H - Infinitely slow reaction @AMAMAANad~-es @ e © e@ @ @ @ 2 e 6 @ e e e e e e e e e ® @ e e 6 ® » . » » > » > , » ’ , 1 \ Note: If ken does not vary with substantial inercase in gas flow rate, that means there is major resistance to the absorption in the liquid phase. ‘The dependence of the overall mass {ransfer coefficient on the flow rates ( gas or Iquid) depends on the kinetic regime that the iracion belongs (0. If the reaction is instantancous or fast. ‘The mace transfer is the limiting step. If the reaction is very stow compared to the mass tronefen Fate, the Kinetic is Rie limiting step. In these cases the flow rates of gas and liquid aifer the kya differently, For more information read the extra reading material « Eso tit eaion a in ay 4g 3 ; econ ely i ai te i ayy ' i Pte os, Lit FIGURE I, Interface behavior or the liquid phase reaction Alfrom gas) + BBM liquid) —+ products (liquid) {or the complete range of rates of the reaction rate and the mast transfer rate, u( rateof takeup of 4 from £85 with reaction occuring | ‘888 with reaction occuring fate of take up of A for | straight mass transfer) For detailed information regarding the transfer rates and kinetic regimes, see Levenspiel (1972, Ch. 13), (1989, Ch. 41, 42). The absorber may be used to purify the gas stream by removing a contaminant, or it may be pied to concentrate a valuable component by removing it hones large proportion of diluent Bee clus if the problem is simply to remove carbon dioxide from air, a sodium hydroxide Solution may be used. If the problem is to extract and coneentnnce CO, for later use, then a NaHCO, (the reaction product of Na,CO, and CO, in water) or ethanolamine will release absorbed carbon dioxide by heating hydroxide solutions has been reported by ‘Tepe and Dodge (1943). Ka, the overall sede anster coefficient, was found to vary with sodium hydroxide concentration and Sodium carbonate concentration. Changes in the BAS rate were found to have a negligible effect on K,a, indicating the major resistance to absorption was in the liquid Phase; yet the effect of liquid rate was found to correspond to 19.28 rather than to the 06 or 0.7 power of Las is usualiy the case when absorption in the liquid occurs by diffusion alone. Temperature had a pronounced effect and K,a increased proportional fo 7. Harte et al. (1933) and Sherwood and Pigford (1952) AD sas 8 e< e @ > 2 9% > 3 vows@ @ @ @ e e® e e @ e e e e e @ @ 9 9 o r a > ». » >» » D ’ b , ’ ’ , ) ' Early work by Tepe and Dodge et al. (1943) was based on N Ke aR K, = overall absorption coeff, to moles/|r.f atm) @ = effective interfacial area per unit vol, f?, [pe N = moles CO, transferred/unit time, 1b moles/hr V = packed volume, #? Fq = log mean partial press. diff of CO,, atm + Ka calculation using Tepe et al’s approach Pow Min Pe Pt = molar flow rate of CO, transferred, 1b mole/ hr = Packed volume, # (calculated from the reactor bed dimension ) = log mean partial pressure difference of CO,, atm Pin Ap pe Prue 4... om 70s Partial pressure of CO, in gas and liquid phases repectively ‘overall mass transfer coefficient 1b mole/ hr f° aim effective interfacial area per unit volume, f/f? fb mole hr fP atm 13Tocstimate, Kya, N and AP., are needed first. They can be estimated as follows: ~ Estimation of V molar flow rate of CO, transferred, Ib mole/hr 3. Assuming constant flow rate of the total ges phase inlet flow rate = outlet flow rate ~ Correct the rotameter reading for the actual pressure and temperature then using Py n= Fez te calculate the total gas molar flow rate RT CO, me 2 we 2 1b mole/hr ~ Based on standard conditions €O,,, = SCP ( nie (= 1 mole/hr ssogag_f I B mole } 1b molefhr Tb mole NCOs, = COjq ~ COs 1 molefhr b. The more accurate method to use is the calculation based on the air flow (due to CO, tfansfer, the inlet gas flow rate would not be equal to the oulet ges flow rave particularly if there isa significant amount of CO, absorbed), pressure: ~ Calculate the molar flow rate of air which is equal to air out. 4 2PO@RBSTA TO NAA ame ee! 8@BEGe Wwe~ Calculatethe amount of N CO, transferred NCO,, = ”m T00 - Estimating Ap, ~ Pex and P,.., (partial pressure of CO, in gas Phase) are calculated using Henry’s law): total inlet gas pressure = p, Femara et = Prout The equilibrium partial pressure of CO, over alkaline % CO, % CO; “100 Pros Pr and pr: Partial pressures of CO, in gas and liqesid phases Solutions of sodium carbonate-bicarbonate 's predicted by the empirical equation developed by Harte, Baker and Pucell (1933). B72 Ny Poo, f IsPoo, = partial press, of CO,, mm Hg N= sodium normality S = solubility of CO, in water @ press, oft atm CO, gmols CO, /\ £ = temperature, °F J = faction of sodium in form of bicarbonate role HCO; | total mole J If there is OH in the solution => f= 0 (assuming no HCO; once OH existed). See the Section on determination of Na+ normalities Also f =0 for the following cases ~ Te the titration volumes (V; =V,); there is no HCO; excess than what is formed by reaction (2) (Ist titration) which already reacted ‘according to reaction (3) (2nd titration) as discussed ~ Ifyou started with Na,CO, IV, is greater than V, (rv, <¥,); there is no OH™ and only CO; and HCO, which HCO; is in excess than what is formed by reaction @. Normality of Na’ in form of NaHCO, : - aan ICO vot nce af Yah, LN of HC sample size sample size Normality of total Na* Normality of total Na Solubility data used for this equation was 3 MMM Km mee A wh od bu oo ie IS wtCc Preow Temperature Solubility 14°F 8, g mole CO,/é 59 0.0455 7 0.0336 95 0.0262 113 0.0215 The equation is known to hold only over the range from 65 to 150°F and for sodium normalities from 0.5 to 2.0, ~ The height of absorber tower with chemical reaction Levenspiel (1972) in Chapter 13, derived the equation to estimate the height of tower by Combining the rate equation and material balance for a differential element of tower volnve A (gas) +B (liquid) > products for dilute system iFDimensional characteristics of the packing material can be found in Perry's Handbook (1984), {able 18-5 (also see the reading material section) polyethylene. A waste tank to hold liquid discharge from the bottom of the column is 36 in ID by 4 f high, made of 16 ga type 304 stainless steel Pibing, valves and a circulating pump for the absorbent Solution are arranged as shown in Fig 1 The pump isa Lewis centrifugal, 1x1 1/4, with 93/4 Le 3500 spm motor Rotameters are used to measure the flow of both the liquid and the gas. Both rotameters are Sraduated in a scale from 0 to 100. Full scale for the Hquid rotameter is 4.70 gpm of liquid (water) with a density of 1.0 g/em3. The ‘ading must be corrected forthe density of the liquid. 18A water manometer connected to the inlet and outlet of the column enables measurement of the perce Crop through the column, as well as the gauge pressure at either ends ‘mercury Parometer on the balcony of the laboratory measures atmospherie pressure. A small sampling pump withdraws a small stream of gas from either the top or the bottom of the column. A rotameter with valve enables the sample flow to be maintained constant at Operation and Measurements A crlinder of pure carbon dioxide gas is used to provide a mixture of about 5% of that gas in the air admitted to the bottom of the column during the absorption experiment. Notice that an glecttical heating element on the gas line prevents clogging by carbon Minune "snow". It will be found that given setting of the CO, pressure regulator with & gives setting of the air flow valves will maintain the composition of gas to the tower quite constant ‘The absorbent is a solution of sodium hydroxide and/or sodium carbonate in water. The solution hould be about 0.4 N in sodium ion. It will be made up ftom either sodiany carbonate or sodium Hydroxide, or a mixture of the two. The TA will specify which is te he used. Notice that the actual concentration of CO; and HCO; ions in the fesh absorbent solution must be measured in any case, Which is to say that solid NOH and Na,CO,.10 HO both contain moisture and CO, in varying degrees, due to exposure to the atmosphere. It is therefore not possible to predict the Concentration of the absorbent solution very accurately even when it is prepared from carefully weighed material SAFETY PRECAUTIO’ SAFETY PRECAUTION Caustic soda can cause severe burns of the skin or eyes. A face mask MUST be worn when Cispensing the solid flake caustic (96.4% NaOH) to protect the Ines avd eves against dust Particles or splashing of the liquid from the feed tank mixer. (It should alee be obvious that the (ansparent shield must be pulled down over the face while the mask is in use Inthe shield is dirty, wash it. Dont lift a dirty shield to see more clearly. You might be seeing less clearly for the rest of our life.) Gauntlet type rubber gloves and a rubber apron must also be worn the solid caustic aera uce Considerable heat on dissolving Localized boiling can cause a violent eruption even when cold water is used. Do not add water to the solid. Pour the solia slowly into a well stirred volume of water so that the heat of solution is safely dissipated In case of accidental exposure to caustic, flush immediately with large amounts of water. Note the locations of the safety shower and eye bath before you begin! Any caustic left on the skin or clothing can penetrate into the skin where it will continue to bun Strong alkalis also damage Feather and cloth. Clean up and thoroughly flush away any accidental spills 1%CAUTION: Make sure to THOROUGHLY Clean the INSIDE of the gloves, the HEAD BAND of the face shield, and the aprons before use. Preparation of Feed Solution Unless a batch of feed solution has been Prepared beforehand, proceed as follows: |. Add water to the feed tank to a total depth of 200 to 250 gal (marked on the tank) 2. Calculate the weight of flake caustic (96.4% NaOH) and sodium carbonate (anhydrous) Fequired to obtain the desired concentration in the feed tank. The proportion of carbonate and caustic will be specified by the Teaching Assioiny Unless instructed otherwise, Pll be mea oximately 0.4 N sodium ion solution. This does net hare to be exact. You 4. Sample the solution in the tank and titrate it Two samples taken 5 minutes apart should give duplicate results before proceeding with chemical absorption. Turn off the agitator when the mixing is complete Using the pH Meter 1. Set the function selector to standby. (NOTE: Always set the function selector to standby 2 = z g g g g 2 8 2 & = 3 8 2 g £ a & & 8 8 z Make sure to remove the rubber sleeve from the electrode, 4. Put the electrode in the solution. Make sure the hole in the side of the electrode is covered by the solution. 5. Set the temperature control to room temperature. 20 OP SOMET ABD Ammann CHvoe e©. Tum the function selector from standby to pH. Adjust the standardize control unt the indicated pH agrees exactly with the pH of the buffer 7. Turn the function selector back to standby. 8. Remove the electrode system from the buffer and rinse it with distilled water. Ifa titration vot {© be started immediately, replace the electrode assembly in a beaker of deionized water. Doing a titration with the pH meter 1. Tum the selector to standby. 2. Raise the electrode assembly, rinse with distilled water, and lower it into the solution to be titrated. 3. Adjust temperature control to room temperature. 4. Turn the selector to pH. 5. Tum on the stirrer, and gradually add titrating reagent from the burette © Watch the pH indicator. As the end point is approached, slow down, adding one drop at atime, Stop and record the burete reading when the fist end point (pH=9 ) is reached 7. Repeat steps 5 and 6 until the second end point (pH=4.0) is reached 8. Turn the selector to standby. 9. Raise the electrode assembly from the solution and rinse with deionized water 10. Lower the electrode assembly into the next solution to be titrated, of 11. Always run samples in duplicate figures. If they do not, repeat with ore and if it agrees closely with one or the other of the original two, NOTE: ‘card the other When running titrations, remember that the pH meter is accurate to +2 PH. Do not Standardize at 7 more than once, This checks the circuitry, 2IFor your 1* endpoint (9), standardize with pH 10 buffer before titrating, ‘Then standardize to pH 4, for your 2 endpoint, before doing your 2 endpoint titration, Cali ig the Teledyne Gas Analyzer The instrument must have been tumed on for at least 20 minutes, to warm up and stabilize at Operating temperature, Air without carbon dioxide (that is, ordinary air, which normally has a CO, concentration of about 0.0396) is first Put through the instrument and the ZERO control is adjusted to give a zero reading on the meter. A standard mixture containing 10.0% co, calculations), The reaction 2NaOH + CO, > NaCO, + HO (0H-,c0;,.Na*) i) NasCOy + CO, + HO > 2NaHCO, (HUCOy, Na. co;) Q rmolatiy(y) = mol solte kg solvent mol solute Gh = mmotariy(M) = = ‘solution (24 equivalent solute nol, ‘mol solute General titration mole: N.Y, = N,V, For acid, » equals the number of hydrogens in the acid’s formula a 6 @ @ ° a 0 > 2 : 9 > WV eee ven= 1 <2 tor HP, HCL, HBr, HCN,.....etc mol For organic acids, 1 is the number of -COOH groups in the acid’s formula n= 1 <4 to HCOOH, CH,COOR mol For many bases, 1 is the number of OH groups in the formula of the base 23n=1~1 for NaOH, MOH. CsOHn=2 “4 for 4g (0H), Fe(OH), : mol mol eq =3L tor aon m3 ot AON), Fororgani bases, » isthe number of —N¥7, groups in the base's formula, n <1 for CH,NH,, NH,, C.H,NH, mol 2 €q solute ity(olsolute) (eg solut rmality, W,[ A solute) Molsolute ) normality, (ge) moter Hit sol. ji (easel is O4N of Nat = 2409. of Na" tit solution ~ For only NaO#H solution (Na, 04-)=>n=1 gm of NaOH gm 40 5 N= mol “tone =—mal_,.,{ e4solute 946.5 tit mot Where 9465 Jit = volume of the tank or the solution to be prepared For example, only, if W = 06, then (gm of NaOH tequired) =946.5 ir 400.60, 964 ry ‘more weight would be required to count for the absorbed moisture. > For only Na, CO, solution QNa*,CO)>n=2 24 ee Ww DMA AAA a wde e ® @ e e ® e e e e @ 6 e e e e e e e e @ e ¢ e ® ® ® . . » dD > d d > » » ' iD , , Note: Na,CO, comes as Na,CO,-10H,0 (onyerons){ stor =285 e), therefore the mo! required weight of Na,CO,- 10 HO that gives N’ normality will be equal to 286 (Mwt Na,CO, -10 HO) juired weight (Na,CO,-10 H,Q)= y Se need ill required weight (Nay N= yee (Mut Na,CO,) Y is the weight in gm of Na,CO, extra weight would be needed to count for the absorbed moisture. ~ Foramixture of NaOW and Na,CO, (Na*,OH”,CO;) xgm NaOH am 0.964 (purity) 2am Na,CO, ” 106 =— Ne _ mol __, of eg solue 946.5 lit 946.5 lit mol For example, only, ifa mixture of 60% NaOH and 40% Na,CO, is used then X= 6M pes (gm NaOH) Y= 0.4m (gm Na,CO,) (where m,oq is the total weight of the mixture) ited where N is known, By substituting x and y in the equation above, m,,., can be esti Then required x and y can be evaluated % Tepresents the weight of Na,CO, needed. Since we have Na,CO,- 10,0 therefore the required weight of Na,CO, - 10 H,0 is: 286 106 required weight (Na,CO, 10 H,0)= yx For both x and y, extra weight would be needed to count for the absorbed moisture Hint: Either OH” & CO or HCO; & CO; exist in water. We assume OH- & HCO; cannot exist in order to perform the titration calculation. Without considering this we cannot perform the calculation (see the reading materials), 207~ Add NaOH and Na,CO, to the feed tank which Contains 250 gallons of water and mix the Solution well Either free hydroxyl (OH) and carbonate ions (CO:,”) or free carbonate and bicarbonate ions COs, can occur together in water solution, but not all three at the same time. The amount of g.miture can be determined by a two step acid-base tirana. (Rattenbury, 1996; Snell and Biffen (1967); Hamilton and Simpson (1969). Titratng with standard hydrochloric acid HCL will fst neutralize any free hydroxyl ion Present; and also one-half equivalent of the carbonate NaOH + HCL > NaCl +H,0 a) Naz CO; + HCL > NaHCO; + NaCl 2) The end point for reactions (1) and (2) occurs at a PH of approximately ~9.0, It is determined using the Fisher Acumet Model 600 pH meter. Further titration to a pH of 4.0 neutralizes the remaining bicarbonate. Reactio 3 NaHCO, + HCL > 1,0 + NaCl +o, 8) ‘The pH change for the first end point is rather gradual and care ‘must be taken to observe the Point at which a pH of 9.0 is reached A sample size of 10 cm3 is recommended for titration with 1.0 N HCI. Dilute the sample to about 100 cm3 with deionized water. Allow the Pipette to drain into the receiving beaker Then touch the pipette tip to the side of the beaker to ara out th ~ Determination of Na* Normality by Titration. The titration perform with 1 VHCE standard. The titration consists of two steps, |. HCE will neutralize any free OH- then CO;. This is completed at pH ~ 9.0 (83 pH ‘eported in Chapter 17 attached). Designate the volume of HCC used as V, 261st titration consist of the following reactions (VY, -V, )HCE requir OH . ) q) a) required => OH” +H' 1,0) ¥, HCéat~8.3 069.0 pt ¥, HCt required=>CO; +H > HCO, | @ 2nd titration consist of the following reaction HCO; +H* CO, +H,0) V, HCtat~ 4.50140 pH @ Sinve all the formed HCO; is reacted with H', the volume of HCE required to neutralize the CO; is V,. ‘Therefore the volume of HCE required to neutralize OH” is V; ~ vy, These three cases can be encountered as: 1 Vi > Vy: Thereis OH and CO; in the solution only. (i.e. no HCO; exist or excess) Yi = Va + This cannot exist as long as there is Na,CO, Ttis not applicable 3K < Vz: There is CO; and HCO; in the solution with HCO;, more that what is formed by the reaction (2) above. Hence, the calculation is based on the assumption that OH does not exist. We assumed that OH and HCO," cannot exist together in order to perform the titration calculations Accordingly, the Na* normality can be determined for all the cases as follows Casel: > v, NV, = NY, worn; (eo: neutralized)+-(/, -V, (OH ~ neutratized)) ee AN of HCE sample size (is taken tobe ~ 25 m) . ° Case2:V, = V, 2B?Ifyou started with both NaOH and Na,CO,, this case is not applicable You only Bet Vi = V, ifyou started with Na,CO, only and there is no HCO; in excess than what is formed by reaction (2) Case), >» a b » » » ’ , , 24START FEEDING AIR TO THE COLUMN 1. Start the air pump using the push button 2. ‘Set the column inlet pressure to 3 inklg using the 885 rotameter valve and valve #3 CALIBRATE THE CO, ANALYZER 1. Allow air to run through the columa for about 20 ‘minutes to stabilize before calibrating the analyzer, n Tum the “in” switch on, 3. Set the CO: rotameter to 1.5 seth ‘4. Set the analyzer to 0, using the zero knob on the analyzer, 5. Open the main CO; valve above the white tank 6. Tum the “in” switeh off 7. Turn the “cal” switch off. 8. Adjust the span to read 10, using the span knob on the analyzer. 9. Tum the “cal” switch off 10. Close the main CO, valve. COLUMN OPERATION 1. Open the COs valve on the gray feed tank, 2. Tum the “in” switch on 3. Adjust the CO; feed nozzle until the analyzer reads 10. 4 Adjust the gas flow to the column to 30% max using the gas rotameter. 5. Be sure that the column inlet pressure is maintained at 3 inkg. & Close the yellow liquid valve behind the control panel to start the flow of liquid to the column. 7. At each of the 5 liquid flow rates, obtain the following: 30 BARnaaaa ~~ & & & eg VELseoe@e PVDVIUVOERYCOsialet concentration( using the gas analyzer switched to “in") CO» outlet concentration (using the gas analyzer switched to “off” and sample pump switched on) Ambient temperature and pressure Ait temperature Liquid and gas flow rates Change in pressure across the column Sample of the outlet liquid Adjust the gas flow to the column to 60% max using the gas rotameter Be sure that the column inlet pressure is maintained at 3 inkig Repeat step G, 3rReferences Tepe, LB. and Dodge, BF. Trans. AChE, 39, 255 (1943) Sherwood, TK, and Pigford, R.L., Adsorption and Extraction, New York, MoGraw-Hill Book Higbie, Zrans. 4.1.Chk, 31, 365 (1935) Danckwerts, P.V. and Sharma, MM, “Absorption of CO, Into Solutions of Alkatis and Amines (with some notes on Hydrogen Sulphide and Carbonyl Sulphide)" Chem. Engr. #202, p. CE244. 80 (Oct. 1966) Harte, CR, Baker, EM. and Purcell, HLH, Jnd. Eng. Chem., 25, 528 (1933) McCabe, W.L., Smith, J.C. & Harriott, P., Unit Operations of Chemical Engineering. 4th ed New York, McGraw-Hill Book Co. (1985) Pery, RH., Green, D.W., and Maloney, J.0,, editors, Perry's Chemical Engineers! Handbook, 6th ed., New York, McGraw-Hill Book Co. (1984) Rattenbury, EM. Introductory Titrimetric and Grevimetrie Analysis, Oxford, England, Pergamon Press (1966) Snell, and Biffen, Commercial Methods of Analysis , Chemical Publ. Co. (1967) Hamilton and Simpson, Calculations of Analytical Chemistry, New York, McGraw-Hill Book Co., (1969) Levenspiel, O., "Chemical Reaction Engineering”, 2nd ed., John Wiley & Sons, New York (1972) Levenspiel, O., "Chemical Reactor OmniBook", OSU Bookstores, Inc., Corvallis, OR (1989). NOMMAnn manana _ 32~ OOOO 9800900 009000060 00000 Assignment For pre-lab proposal, provide a detailed flow diagram (P&ID ~ Process and Instrumentation Diagram) showing all the related components and instruments, correctly labeled (e.g. value types, THE pee ete). DO NOT SIMPLY COPY THE ONES PROVIDED WHICH ARE USED IN ‘THE MANUAL ONLY AS A GUIDELINE. 1a. Evaluate the overall mass transfer coefficient, Ka, for the given packing as a function of flow rate, b. Investigate the effect of gas flow rate on the Ka and on the mole CO, transferred per unit time measured based on the material balance if gas stream (Change the gas flow rate significantly), material, identify the expected Kinetic regime for mass transfer and Teaction). Knowing the Kinetic regime would help analyze properly the effect of liquid flow rate, gas flow rate, concentrations, temperature, etc. Note: For each operating condition use the measured molar flow rate of CO, transferred based on the inlet and outlet gas phase measurements 2 transferred per unit time) via material balance in the liquid phase stream, Compare the results with that obtained by the gas phase measurements in (1) above Hints: 2NaOH + CO, > Na; CO, + H,O reaction (1) Na,CO, + HzO + CO, -» 2NaHCO, reaction (2) NaOH react = NaOH in the feed — NaOH in the product CO, consumed by reaction (1) = 1/2 NaOH react CO; consumed by reaction (2) = Na,CO, consumed by reaction @ ‘o'2l CO, consumed = CO, consumed by reaction(1) +CO, consumed by reaction(2) In practice, there is OH” and HCO; in the solution from reactions (1) and (2), but we assume they do not exist together for the purpose of performing titration analysis calculations (See the reading material)>. Discuss the advantage and disadvantage between the countercurrent and co-current gas/liquid contactors (reactor) used for absorption with chemical reaction. © Discuss the effect of L/V ratio on the performance and its economy of the physical absorption and the absorption with chemical reaction State the advantages and Aisadvantages of having high L/V. What do you recommend for optimum L/V ratio 4. Discuss and state the effect of temperature. Would it be changed inside the absorber? Why? 34 1G @ CSOSBE* IV See e @ @ e@ @ © @ e@ @ e @ @ e@ e e e e e e@ e e ® ® ® B DD > > > d » » , , Results and Data Analysis Oui ie Aesults and Data Analysis Outline errors, if any), statistical analysis numbers, trend of the experiment: Data analysis may include, but is not limited to, the following discussion outline: 1. Discuss the trend of K,a as a function of liquid flow rate Is the trend consistent with the ‘heory? Should this trend be obtained? Why? Discuss the effect of gas flow rate on the ,a. This should be compared at constant liquid flow rate, What does the effect tell you 2. Discuss the comparison of the mole CO, transferred per unit time obtained by gas stream and [quid stream material balance, IF there is a diserepancy, explain why. If your work is carefully and correctly done there should be good agreement 3. Discuss, compare and explain the assignment (3) briefly and concisely. In this assignment you need to read related subjects. Conclude and analyze. Feel free ee rely on any appropriate references, 3(TY VV V ew vsseKy 69 SSC OOLEEDD000NB AF - NINNT09 NOLLAYOSEV GIOVE “Leansiy Uy > x Ky qasy to ain Lk . L [= T NW ® ONWL "oud | a334 syo [F oe) } wav ALD PS *o> He Q © 6 Aoun— 4300» > go SQ © CAST sve Anan