ORIGINAL NATIONAL UNIVERSITY OF SINGAPORE EXAMINATION FOR THE DEGREE OF B. ENG. (CHEMICAL) CN 3132 ~ SEPARATION PROCESSES (Semester 1: 2015/2016) Nov / Dec 2015 ~Time Allowed 2.5 Hours CN 3132 INSTRUCTIONS TO CANDIDATES This is an OPEN 800K examination. The students are allowed to bring in the text book and the lecture notes. QUESTIONS DO NOT CARRY EQUAL MARKS. This examination paper contains FOUR questions and comprises TWENTY printed pages. ‘ANSWER ALL QUESTIONS AND ALL PARTS OF EACH QUESTION. Read each question carefully and fully before attempting it. ‘The symbols have their usual meanings. ‘Write your answers in the space provided below each question. Please write your matriculation number below number | ] ‘Question No. ipsa 1 23 2 a7 2 20 4 30 a Total 100Question 1 a) Tey data for water - glycerol, methanol — water and para-xylene — meta- xylene systems are shown in Figure Qla. Feed composition and separation requirements for each system are given in Table Qa. Clearly state in the last column of the table what separation method{s) will you recommend for each of them. Give reasons. (8 marks) cn3132 (Total 23 marks) —e-watersicerol aeMethenol mater -®-Paraxylenemeta ene i 350 £08 280 i § Eos no ? 5 i i Fos uo F 10 0 02 04 06 08 1 water) /sfmethanol /x(par xylene) Figure Qla: T-xy data for water ~ glycerol, methanol ~ water and para-xylene—meta-xylene systems. Table Qa: Feed compositions and separation requirements for the systems in Figure Qa System | Feed composition | Separation Recommended separation (mole ratio) | requirements method(s) with reasons Water - 60:40 290% glycerol elycerol purity with | high recovery Methanol- | 30:70 299% water methanol purity with high recovery Para-xylene — 50:50 Nearly pure meta-xylene para-xylene | and meta- | | xylene with high recovery3132 b) Acetic acid is the most widely used aliphatic carbonic acid. Apart from its use in the production of acetic-acid esters, it is frequently also employed as a solvent, for instance, during the production of cellulose acetate or during the manufacture of pharmaceutical products. Aqueous acetic acid is obtained as a rule during the foregoing processes. In most cases its recovery is of great economic significance. Your first assignment during your internship in a design company is to design a continuous multi-stage distillation unit to separate acetic acid from water. Your supervisor has given you Table Qib (below) and Figure Q1b (on page 4). Design the process and submit the result: Table Q1b. ‘Show all your calculations and drawings. (15 marks) Table Qi1b: Design specifications and results. Input / output Feed 1 composition ‘50 mole% acetic acid in water; 50% vaporized Feed 1 flow rate 100 kmol/h Feed 2 composition 25 mole % acetic acid in water; liquid at bubble point Feed 2 flow rate 100 kmol/h Acetic acid in top product 5 mole% Acetic acid in bottom product 95 mole% iH L/D ratio 2.6 Recovery of acetic acid in bottom product ‘Slope of the top operating line Slope of the middle operating line Number of ideal stages Optimum location of feed 1 (counted from the top) Optimum location of feed 2 (counted from the top)y (water) cn3232 "| 08 0.6 0.4 0.2 0 0 0.2 0.4 0.6 0.8 1 x (water) Figure Qib: x-y plot for water-acetic acid system.cn31323132 Question 2 (Total 27 marks) a) Arrefinery stream, flowing at a rate of 1000 moles/h and currently used for fuel, contains 72.5% Ho, 25% CH, and 2.5% C2Hs, It has been decided to recover Hz from this stream and send it to a hydrogenation reactor, which operates at 2500 kPa. An absorption process with n-octane as the solvent will be used to obtain a 95% pure H; stream. The absorber will be operated at 3000 kPa and 40 °C. Use mole ratio for your calculations, but as an approximation use V, = KiX, for equilibrium where i represents the absorbing components. Assume Hz is non-absorbing and n-octane is non-volatile. (i) Find the number of ideal stages for operating L/G, = 1.5 (L/G,)min- (il) Show that you have achieved required H, purity in the process you have designed. If it is more or less than the target Hz purity, discuss what should be done to achieve the target. (ii) Viscosity of n-octane is 0.51 cP. Estimate the overall tray efficiency. (15 marks; each part carries 5 marks)cn3132n3132cna132 b) Fractional extraction is important for pharmaceutical separation. Two chemically modified cephalosporin antibiotics, A and 8, are dissolved in water. A consultant was engaged to design the fractional extraction process to recover at least 80% of antibiotic A with at least 90% purity on a solvent free basis. Your manager has summarized the submitted design in Table Q2b and Figure Q2b. You responsibility is to check the design, report your findings in Table Q2b for the convenience of comparison and provide qualitative suggestions for improvements if the design is found inadequate. (12 marks) Table Q2b: Checklist for design check (no inputs required in the shaded boxes). Items From the consultant Result of your checking Design basis kg/h of the aqueous feed | containing 5 wt% A and 10 wt% B. Solvent 1 (pure amyl 2665 kg/h entering at the acetate) __| bottom and flowing up Solvent 2 (pure water) 2220 kg/h entering at the top and flowing down Equilibrium Ya Xa | (yand x are weight fraction | in solvent 1 and solvent 2 respectively) .6 Xe I Feed stage __| 4 from top Number of ideal stages 10 Design target 1 At least 80% recovery of antibiotic A in solvent 1 Design target 2 At least 90% purity of A in exit solvent 1 (on a solvent free basis) Weight fractions of A and B | 1.5x 10° and 2.6 x 10° in exit solvent 1 Weight fractions of A and B | 4.5x 10° and 1.35x 10° in exit solvent 2 ‘SUMMARY OF DESIGN CHECK Does it satisfy all the design criteria? If it does, is there any way to improve the design? If it doesn’t, why and what should be done?10 cnaa32 00008 20005 3 ocoone $ o.o0002 # ooo 0.00001 o ‘0.00002 ‘0.00008 0.00006 We fraction of Ain solvent 2 1.00003 i it faction of Bin solvent 0.00001 ° ‘0.00002 0.00008 0.00006 ‘We faction of Bin solvent 2 Figure Q2b: Equilibrium and operating lines for fractional extraction of antibiotics A and B.cur cn313212 cn3132 Question 3 (Total 20 marks) Pure water is used to absorb CO2 from a CO2/N2 mixed gas containing 5 vol% of CO; in an absorption tower. The Henry's constants are given in Table 3. 95% of CO2 needs to be removed after this process, which is operated at 20 °C with a total pressure of 15 atm. The ratio of the mass flow rates between water fed from the top of the tower and mixed gas fed from the bottom of the tower is 100. The densities of water and mixed gas inside the tower can be treated as unchanged. The overall gas phase volumetric mass transfer coefficient Kea [mol/(m?-s-atm)] remains unchanged under various pressures but is affected by ‘temperature T (K) as Kea « T?? a) What percent of the CO; in the feeding gas is absorbed if the total pressure to 20 atm while the rest conditions remain unchanged? (10 marks) increased b) What percent of the CO; in the feeding gas is absorbed if the operating temperature is reduced to 10°C while the rest conditions remain unchanged? (10 marks) Table Q3: Henry's law constants H (atm/mole fraction) of various gases in water. 0 35.200) 268, 3 39,6001 3s 10 44.200) 367 15 48,904) 23 20 53,600 483 as 1640 58,00 sas 0 S60) 2.0 09 35 2000 65.900) 676 40 20 69.60) 74s 45 72.900 ald so 76.100 Mt on a 82.100 1030 m 84.500 1190) so = Sasi 1350 % - $4,000 Lao 100 84,600) Ls13 cn313214 cn313215 cn313216 cnaa32 (Total 30 marks) Nitrogen gas containing 1.5 vol% of NH; is counter-currently scrubbed at 30 °C and 2 atm with pure water in a packed column of 6 m height, packed with % inch ceramic Intalox saddles (a = 1.04, B = 0.37). Inside the column, total gas flow rate is 1800 m°/h and liquid flow rate is 1500 kg/h to meet the pressure drop of 0.4 inches of water per foot that is below the flooding curve. At the column temperature, the equilibrium relationship is y = 0.5x. The overall gas phase volumetric mass transfer coefficient K,a is 0.1 kmol/(m*-s). a) Can this tower meet the requirement of 99% NHs removal rate? Why? (15 marks) b) Whats the actual NH; removal rate for this tower? (7 marks) ©) _Isit possible to meet the 99% NH; removal rate by increasing water flow rate? If so, to what extent? (8 marks)7 cn313218 cn313219 313220 cn3132 -END OF PAPER-