American Institute of Chemical Engineers STUDENT CONTEST PROBLEM 1966 VU 345 East 47 Street + New York, New York 10017CONTEST PROBLEM 1966 AMERICAN INSTITUTE OF CHEMICAL ENGINEERS STUDENT CHAPTERS ‘Open Only to Undergraduates oF Those Without @ Degree in Chemical Engineering DEADLINE FOR MAILING Solution must be postmarked not later then midnight, June 15, 1968 RULES OF THE CONTEST Solutions will be graded on (a) substantial correctness of results and sound- ness of conclusions, (b) ingenuity and logie employed, (e) accuracy of computes tions, and (¢) form of presentation. Accuracy of computations 18 intended to mean Primarily freedom trom mistakes; extreme precision is not necessary. It is to be assumed that the statementof the problem contains all the pertinent sta except for those readily available in handbooks and similar reference Works, The use of textbooks, handbooks, journal articles, and lecture notes 1s, Permitted. In cases where there is disagreement in the data reported in the lite erature, the values given in the statement of the problem have been chosen as being most nearly applicable, ‘The problem is not to be discussed with any person whatever until June 15, 1066, This is particularly important in cases whereneighboring institutions may ‘not begin the problem until after its completion by another chapter. Submission (of « solution for the competition implies adherence to the foregoing condition, ‘A period of not more than 80 consecutive days {e allowed for completion of the solution. This period may be selected at the discretion of the individual Counselor, but in order to beeligible or an gward a solution must be postmarked not later than midnight, June 18, 1966, ‘The finished report should be submitted to the chapter counselor within the thirty-day period. There should not be any variation in form or content between the Solution submitted to the chapter counselor and that sent to the ALCKE, of fice, The report should be neat and legible, but no part need be typewritten. ‘The solution should be accompanied by a letter of transmittal giving only the contestant's name, school address, home address, and student chepter, lightly attached to the report. This letter will be retained for identification by the feck Fetary of the Institute, The solution itself must bear no reference to the student's ‘name or institution by which it might be Identified. in this connection, graph Paper bearing the name of the institution should be avoided. Each counselor should select the best solution or solutions, not to exceed two m number, from his chapter and send these by registered mail to Mr. F. J. Van Antwerpen, Secretary American Institute of Chemical Engineers 345 East 47 Street New York, New York 1001770 THE CONTESTANT In the development of the 1968 Student Contest Problem an attempt has been made to emphasize the importance of time. The contestant, like his industrial counterpart, has a mited time to spend fon a study of process alternatives. Process engineers must decide early where the decisive lanues ‘and strive toward reaching the correct decisions on the issues, Time represests money to the chemical company; the quicker the feastaility and economies of process can be determined, the ‘more profit a company can make, STATEMENT OF THE PROBLEM ‘The subject of the 1968 probiem is the preliminary economuc process design ofa plant to man~ facture 4 monomeric chemical. The manufacturing company doesnot kxow very much about the prac ‘ets and needs a preliminary evaluation. The Sales Departivent approached the Research Laborator = ies about developing a process to produce the monomer for captive use, Continually increasing use Of the material in & specialty coating is expected. The Research Department has attempted several exploratory experiments with encouraging results. These results form the basis ofthe preliminary process design and economic evaluation. The following memoranda represett the total correspond ‘ence concerning the monomer. The student (s to assume the role of Me. Walker in solving the probs Jem, which is the preparation of a preliminary process-design and manufacturing cost estimate for {rhstyl methacrylate co: VR. Field P. Rinceton L Tower 1968 MEMORANDUM To: V. P. Walker, Process Engineer From: J. H. Sign, Chief Process Engineer Subject t-Bulpl Methacrylate, Manutacturi ‘The Costings Sales Department has requested the preparation of a manufacturing cost estimate for Production of t-butyl methacrylate, Current usage (of this raw material in Coating 262-X 1s, 200,000 1b,/mo, with requirements expected to increase to 41,000,000 tb./mo. by the second quarter of 1060, Becaise of tis predicted rapid growth in the use of the chemical, consideration Is to be given to eap= live manufacture. Please prepare preliminary process designs and comparative manulacturing Cost estimates for production of t-butyl methacry= late by both batch and continous processes. ‘The results of the intial laboratory experiments by Dr. Tower's group are attached. although Dr. Tower's experiments have found 60% conver= sion to be optimum for the batch reaction, this will fot necessarily be the ease na continuous process. ‘By copy of this memorandum, Mr. Rincelon is requested to forward to jou a summary of pertinent design data and cost-estimation factors, He should Cost Estimate also Include the specifications for the availabl 6,000-gal. batch reactor and associated distillation ‘column which would be used for batch production, ‘All the ‘equipment for a continuous process and Aaurliary. equipment for a bateh process must be purchased. Will you compare the costs ofthe two process as a tinction of the product output per month. In particular, what is the masimom capacity of a batch process employing the available equipment and at ‘hat level of output does it become economically ‘uvantageous for the company to change processes? ‘Any recommendations you may have for reducing costs will be welcome, Because of the urgency of this ‘cost estimate and the minimal data available from the laboratory, all necessary design informa tion may not be included. Therefore, state clearly ‘in your’ float report all umportant design asim” tons employed in your eatculations- Since it will require some time to puta processfon stream, your final report is needed as soon as possible. Therefore you may not be able to optimize both designs; however, we hope that you ean utline 4m sufficient detail how such optimizations (partic= larly of the eontinsous process) would be carried out for our final design. For your further information, background men oranda are attached. cei Je HL Sign, ‘Chiet Protes Mareh 1, 1966 Engineer MEMORANDUM, Tor From: Dr. V. R, Field, Director of Research RR. Vail, Sales Manager Subject: {-Buty! Methacrylate, Monomer for Spectatty Coating Following is a summary of our discussions of t-butyl metazcrylate held in my office on Fob- ruiry 28. ‘The sales volume for Costing 262-X increased Gramatically ast year to an equivalent t-butyl methacrylate usage of 200,000 To./mo. Market anal~ ysis leads us to believe monomer requirements wil Increase to more than 350,000 Ib./mo, by the end ofthis year and to 1,000,000 1b/meo. by 1966. ‘You speculated that the monomer could be mana~ ftactured for captive use at a cost significant below the 50 cents/Mb, we are now paying and that a proe~ fess could be developed which would not infringe on existing patents. T encourage you to initiate process studies aimed at captive manufacture of the monomer and to re= port the results to Mr. Sign for an early evaluation by his group. T believe it important to determine ‘manufacturing feasibility and to assess the econen= Jes of your processing Schemes at the earliest ma~ ment. cee: B. Vail ‘March 15, 1966 MEMORANDUM To: J. 1 Sign, Chiet Process Engineer From: V. R, Field, Director of Rereareh, Subject: t-Butyl Methacrylate: Laboratory Provess [At the request of Mr. Vall, several laboratory experiments were made to sythesice t-butyl meth- acrylate In the tached memorandum Dr. 1. Tower Summarizes the experimental results, which we ‘Bnd encouraging. The laboratory process described therein is a batch process. A corresponding con tinuous process has not been explored, but we thine that such a mode of operation is feasible. In the final design and cost report that your de- partment will issue, ve would seek your tasistance in selecting those areas in each process where ‘sigificant cost reduction might be aebieved. In particular, we want to know at what level of pro- ‘ition tt would be economically advantageous for ‘the company to change from one process t0 ti ‘other, In light of the growing demand for Coating 260-X, the rescite of our comparison wil be ime portant in determining the research path we shuldMareh 11, 1966 MEMORANDUM To: Dr. V. R. Feld, Director of Research, 4s recovered by venting the reactor to atmospheric From: I. Tower, Senior Chemist Subject: {=Buty! Metaerylate: Preliminary Laboratory Scouting Experiments suMMARY Several exploratory experiments have been carried out to aynthesize t-butyl methacrylate, The results of these preliminary experiments have heen ‘very encouraging. The chemistry of the reaction, the laboratory procedure, and pertinent results are ‘outlined below. ‘CHEMISTRY t-Butyl_ methacrylate is the reaction product of sethacrylie acid and Iscbutylene: cH, ccH,cooH + methacrylic acid (cHy),cCH, $2 cHreCH,coDeICH), Isobutytene {t-butyl methacrylate ‘The reaction is acid-catalyzed and is reversible, ‘The heat of reaction (sf) is 15,000 eal,/g.-mote. {An unavoidable side reaction produces the undesir~ Able compound discbutylene: 2{CHs)sCCH, — (CHs)sC=CHCICHA isobutylene itsobutylene Heat of reaction (aH) 1s 10,000 eal. /g.-mole LABORATORY PROCEDURE ‘The methacrylic acid and 100% sulfuric acid cat~ lyst are charged to a stirred, Jacketed 1-liter Autoclave (pressure rated at 1001 /aq 1. gauge). ‘The temperature of the material fed to the auto- ave ts 25°C,; the lobule (IB) is fed to the unit Sat 2 constant rate for 20 min., the batch temper~ ature being maintained at 25°C. with the maximum pressure of 35 Ib./eq. in. gauge observed atthe end ‘Of the IB. adcition, Aer the reactants have been held at 25°C. for 2 to,7 Ar., 0% (weight) caustic Sout 1s added to the reaction mass in a quantity to neutralize the sulfuric acid catalyst. The meth seiplic acid is excentially unatfected by the caustic, bt neutralization is required to prevent reversal fof the reaction when the isobutylene 1s Fecovered. ‘When the autoclave agitator 1a stopped, te con tents of the autoclave separate into two phases: fn organic phase containing t-butyl methacrylate (CEMA), isobutylene (IB), methacrylic acid (MAA), land diisobutylene (DIB), and an aqueous phase con” fining only dissolved Salta of neutralization. After Separation of the aqueous phase, pure isobutylene pressure and then heating to 50°C. The remainder Of the 1B, DIB, and t-BMA are recovered by dis~ uation. ‘The residue in the autoclave is primarily meth= acrylic acid, Actual experimental results and com- iments are contained in the next section, Percentage (of conversion per time forthe reaction is tabulated Under Comments, As noted in the Comments, 60% conversion has been found to be the best batch Op= erating point. EXPERIMENTAL RESULTS ‘A typical laboratory material balance for 60% Th MAA 344g. B 448.36. 1,304 3g SOR caustic solution 18.5 ‘Out Aqueous phase B ‘BMA MAA Reaction conditions; Reaction temperature 25°C. Reaction pressure 35 1b,/0q. in, (maximums) gauge ‘Time to food 1B "20 min. Conversion See Comments for ‘conversion table (COMMENTS ON LABORATORY EXPERIMENTS 1. Operation of reaction to 60% conversion is suggested for baten provess. 2, DIB formed during reaction appears to be related to product formed. Use ratio of Ol mole OfDIB per mole of -BMA formed. 3, Both neutralization of catalyst and phase sep aration of onganie-aqueous layers are extremely st, 1, Negligible quantity of organle is lost to water phase. Nil water is carried outwith organic phase, ‘The salts of neutralization remain dissolved in the aqueous phase. 5. The batch distillation of DIB from t-BMA and MAA requires reflux ratio of at least 30 to 1 ‘8. Temperature of materials at any time mustnot exceed 80°C. to avoid polymerization of MAA and BMA, 7. Weigit percentage composition of distil and resides at various stages of separation i follows: Distilate (average) Bottoms At end of 1B stip 99.808) 0,008 (1B) Atend of DIB strip 0.5 (t-BMA) 0,001 (DIB) At end of {BMA strip 99.9 (¢-BMA) 0.1 (-BMA) 8. Corrosion data obtained during rexetion and fistitition experiments indicate stainless tee! (8304) to be a suitable material of construction, Losses of t-EMA during neutralization, de~ cantation, and purification should be less than i. 10, Conversion of MAA vs. time. ‘Time (hr.)* % MAA converted a a 8s 8 a 8 6 ‘Time measured trom atart of IB feed, Apri 4, 1088 MEMORANDUM To: V. P. Walker, Process Engineer From: P, Rinceton, Process Cost Analyst ‘Subject: Design Factors and Cost Information for At Mr. Sign's request of April 1, 1906, the ol- lowing information is forwarded to'you for use in the preparation of the manufacturing cost for Baa, 1. Batch reactor ts normally operated at a5% of faut volume, continuous reactor at 100% of fall vol= ‘2, AML components are assumed to obey Raoult’s and Daltan’s laws. 3, All distillaiions may be taken as inary sep rations. 4, Pressures through any one distillation column may be considered uniform. 5. Columns normally purchased by the company have a 12-in. tray spacing with 1-i, liguid seals. ‘6. Overall plate efficiency of columis te 'T. Overall heat transfer coetsictents (U) nor- mally employed for designs, Btu. ir, (eq 8/P) ust u=40 Us i00 Condensers Jacket reactors ‘Steam reboilers 8, AN distillation columns will be operated at their maximum vapor rate (8). AML batch distilla~ ‘ons wil be Tun with a constant reflux rati. "2. 160-15. saturated steam is ueed in the re- boilers 10. For simplicity, 1 suggest that you evaluate the. continaous process at an operating level of 1,000,000 Tb./imo. and employ the Maix-tenths fae~ EMAC tor" to determine the equipment and plant snvest= rent at other levels of capacity; that is, eon By where I) fixed investment in plant and equip ‘ent at eapncity 2 4h fixed investment in plant and equip- iment at eapacity 1 Gr = capacity 1 Ce = capacity 2 11, Manpower requirements (each process to be run T days/iwk. around th clock) Continuous process 2 operators /etit Baten process 4 operators shit 12, The following equipment is available for te batch process: ‘Reactor —6,000-gal. 85 reactor topped with a sb-in.sdiameter, 22-plate bubble- feap column (12¢in, tray spacings). Equipment rated for 100 18. /aq 1. 5 yr old with original 1 cost of $800,000 tnelucing Bailing Is serviced with steam, water, and brine. 438, Storage tank sizing: ‘Final product, wk. storage Raw materials: I wi. storage Intermediates and recycles: 1 day14, Disposal of waste at no cost. LITERATURE CITED 15, Quality control and supplies for similar ma- ‘1+ Chilton, C.H., ed., “Cost Engineering inthe teriais usually run about §0'50/100 I. product. Process Industries,” MeGraw-Hill, New ‘York (1960). colts RAY material overhead is tBotraw mater 2, yahytnat #C., and CE. Dry, Chem ‘cal Engineering Plant Design,” 4 ed., 17, Equipment costs can be found in reterene MoGraw-Hill, New York, (1959). {and 2, all values being adjusted toan ENR = 1,000, 3, Perry, I HL," otk, “Chemseal Englneers? 18, Plant cost equals 3.8 times the installed "Wandbook,""4 ed, Sect. 18, P. 6, MeGraw- equipment costs Hill, New York (1065). TABLE 1. Coot Fstrs TABLE 2. Unies Labor '$3.00/manhour. {Gabor overhead 28% of labor cut Supervision 288 of labor Steam 1601./s9. i. $1.0071,000 Supervision overhead 35% of supervision abs. sat Depreciation (straight-line ‘Cooling waters 68°F. $1,00/10,000 gat. ‘method 10% of sevestment/ys. Chilled water 40°F. $2,00/10,000 gal. Repairs and matstenance Sof investment/ye. Brine 50°F. $15.00/10,000 gat. Property overhead Zi ot westment/ye, _*Maximam allowable temperature rise of 20°F. TABLE 3, Row Moi nd Products a 8 bi vauaSoutUOR) soe HoH Molecular weight eet 56.1 m2 Ge. Density, g/ml nC Feat of vaporization, ‘al. /g.-mole 7,200 5,215 9,500 16,000 Tye. (atm) 163 “6.9 to. ise TEC: (300 mim, 3g) 1 28.0 73108 Ch Bub) OF) 045 03008088 ost, $/100 0 | TO 12130 TABLE 4 Hoot Tovfr Ares of Jacket Agioed Reaction essa 100 8 1,000 10 10,000 0