复合萃取分离乙酸乙酯-乙醇-水

第4卷第4期南京师范大学学报工程技术版)Vol 4 No 4004 F 12 F JOURNAL OF NANJING NORMAL UNIVERSITY( ENGINEERING AND TECHNOLOGY )Dec 2004Composite Extraction Separation of Ethyl acetate-Ethanol-WaterGU Zhenggui, ZHI Huzheng, LIN JunSchool of Chemistry and Environmental Science, Nanjing Normal University Nanjing 210097, ChinaAbstract: The production technology of ethyl acetate was introduced in this work. Extraction separation results of ethyl ac-etate-ethanol- water were simulated with wilson equation By triangle-matrix method. Reflux ratio et al. effected on separationefficiency were discussed. Extraction separation apparatus was establishearation experiment of ethyl acetate-ethanolwater was studied by two extraction solvents composite extraction method is used for separation of ethyl acetate-ethanol-wter above 99% ethyl acetate can be obtained one time by composite extraction ethyl acetate recovery rate reached to above97% also above 95% ethanol can be obtained water quantity used is only twice times raw material this technology is simplend energy consumption is low. Iprovided a base for farther industry testKey words: composite extraction ethyl acetate ethanol water, simulaCLC number: TQ028, Document code: A, Article ID: 1672-1292( 2004 04-0064-040 Introductionwashing and azeotropic apparatus this technologycomplex using water quantity is four times moreEthyl acetate can be produced by kinds of meth- than raw material energy consumption is large. whenods but final products are composed of ethyl acetate, composite extraction methosed forer, paucity ethanol andacetic etheethyl acetate-ethanol-water above 99% ethyl acetate canEthanol and acetic ether can be easily disrobed in this be obtained one time by composite extraction 5], alsosolution, but in which ethyl acetate-ethanol-water can above 95 ethanol can be obtained water quantity usedconstitute binary and termary azeotropic solution which is only twice times raw material this technology is sim-can not be separated by distillation. Putting watering ple and energy consumption is lowand azeotropic distillation are adopted 2 in traditional in-In this work extractive separation results of ethyldustry from which 83 ethyl acetate azeotropic solution acetate-ethanol-water were simulated with ethylene glyc-in be formed combining more than twice times water erol and water by triangle matrix method the parameterwith azeotropic solution then mixed solution is putted of reflux ratio, theory plate, solvent ratio et al. wereinto settling vessel upper layer putted into distillation studied the separation apparatus was established, theis distillated above 99% ethyl acetate can be ob- separation experimental results were measured, and,under layer is returned into azeotropic tower, compared with the simulation all results were providedaste water quantity is 3. 45 times than product, reflux for farther industry researchratio of azeotropic distillation is above 5: 1, this technol1 Extractive simulation calculationgy which is composed of azeotropic distillation mixingsettling separation and distillation technology is compliExtractive distillation technology was designed ascate and demands large energy consumption at presentafter mixture solution of ethyl acetate-ethanolnew technology is developed which is composed of water was separated, above 99% ethyl acetate was obputting water extraction and azeotropic distillation]ower top, mixture solution with extractive a89%o Ethyl acetate 5% water and 6% ethanol were ob- genter bed was treated again extractive agent wastained by putting twice times water in raw material, circ中国煤化工under regeneration towerabove 99 0 ethyl acetate can be obtained by farther wabedlCNMHG the top was transferredReceived date 2004-06-05Biography: GU Zhenggu( 1962-), Associate professor, Professor of Hongkong remote education institute, Majemical separation and technolH4.万方数摇如mGU Zhenggui et al Composite Extraction Separation of Ethylacetate-Ethanol-W ato recovery tower, 95%o ethanol was obtained on the reGas liquid equilibrium data was provided accordingcovery tower top, bottom solution was transferred to ex- to literature 6-8) gas liquid equilibrium data of ethyl ac-tractive toweretate-ethanol-diethyl glycerol and ethyl acetate-water-di4 ethyl glycerol were measured in this paper, Wilson mod-el parameters were correlated with vle data by minimumvariance method model parameters of four compoundswere correlated by binary model parameters and vle da-ta of ternary system, model parameters were arranged inTable 1. Separation results of extraction tower regenative tower and recovery tower were simulated by tri-diagonal matrix method simulating calculation black diaextraction tower2、3、4. condensor、6、7. reboiledgram and calculation conditions were in literature 9)regenerative tower 9, recovery towerFig 1 Technology chart of composite extraction for ethylsimulating results were arranged in table 3 under condietate-ethanol-watertions of table 2Table 1 Model parameters of wilson equationSystemTenp/℃Ethano( 2) Ethyl acetate( 1) ethano( 2)rater(3)Cthyl acetat( 1) Ethyl acetatd1)ae(3)thylene glyco 4 ethylene glyco( 4) ethylene glyco 4) Wate( 3ethanol 2)5.3A32A14A210.12620.93781.14410.04771.37320.04122.30070.0064-0.13990.62700.07321,4060Table 2 Technical references of simulation calculationTable 3 Results of Simulation calculationnowConcentration massMaterialtraction Regeneration Recoverykg/h) ethyl acetate ethanol water ethylene glycol①0.21720.68140.10140.000Theory plate number/N78②Input place of material/NF8③30000.00000.00000.00001.0000Input place of solvent/Ns,0.00000.00001.00000.0000Input place of solvent/Ns31⑤99670.00100.17100.52700.3010Reflux ratio/R⑥69670.00130.24470.75390.0000Temperature of tower top/'t78.817930.00530.95050.04390.0000Temperature of tower bottom/C 97.2At N=78, NF=67, NS=13, MS2=31,R= rate were obtained on extractive tower top at N=78, RI4 other conditions were constant ) the effect of solvent =4, NS,=13, NS,=31proportion( S/F )on top concentration( Xd)and bottomconcentration( Xw)were shown in Fig. 2, the calcula2 Experimenttion results indicated that the overhead concentrationThe extractive distillation apparatus as Fig. 5 was(Xd)reached above 99. 5%, the bottom concentration established. At normal pressure, tower inside diameterXu)were under 0. 10% at S/F=1. 2: 1, S2/F=2 was 22 mm the inside was filled with 3 x 30 typeI the recovery rate reached above 97%,the effect of stainless steel helices raw material was measured byreflux ratio on Xd, Xw was arranged in Fig 3 at Sy/F standard system his packed height equivalent to a theo-1.2:1,S2/F=2: I ,the results indicated that reflux retical plate( HETP )was 27 mm tower pot was heatedratio(R=4)was better condition, the effect of theorby中国煤化工 l and solvent was mea-late number was arranged in Fig. 4 at above conditions, sureclid tower pot output thethe input situation of solvent(S1, S 2) has no effect onCNMHtheom at NS er material was drived out by vacuum pump, bottom out-=9-15, NS2= 28-37. The results indicated that flow material was transferred to regenerative tower, theabove 99. 5%o ethyl acetate and above 97% recovery南京师范大学学报(工程技术版第4卷第4期2004年)一Md-S1/FXw* S,/FXd- R-Xd- Sa/F0.5S1/F(S2/F=1.4:1)、S2/F(S1/F=2:1)Fig 2 Effect of solvent ratio on ethyl acetate Fig 3 Reflux ratio effect on ethyl acetate Fig 4 The effect of theoretical numberconcentration of tower top and bottonconcentration of tower top and bottomethyl acetate concentration of tower top andolvent was recirculated by disrobed alcohol and dehydrated the overhead material was transferred to the re-Table 4 Results of extraction separation experimentcovery tower. Esterification reaction mixture solution wasApparatused by hP chimatograph raw material was extracted by binary solvents conditions of experiment and separation were arop/℃77-78ranged in Table 4, the results indicated that aboveTemp. of bottom./℃99. 2% ethyl acetate was obtained by binary solvents, Tower high/m3.100.70ethyl acetate recovery rate reached to above 97%, alco-Distillation section/mhol aqueous was obtained with 0. 3 ethyl acetate( solExtraction first section/mvent S, was not in), above 95% ethanol was obtainedExtraction second section/nTop cone. of ethyl acetate0.992on recovery tower top, the experiment results were con0.00320.9502sistent with the simulation resultsT0.00470.0055of ethyl acetate0.00321.0000163 ConclusionSeparation results of ethyl acetate-ethanol-waterwere simulated with Wilson by triangle matrix methodthe calculation results provided conditions for experimentwater was extracted by binary solvents experiment resultswere consistent with simulation results ethyl acetate con-tent reached to above 99. 2% after extraction separationthe recovery rate reached to above 97%, the results ofexperiment and simulation provided for farther studiesand industrial test1. raw material tank 22 pump 3. glass rotameter A. tower pot samplingXd, Xw content of extraction tower top and botton( masstap 5, electric hot jacket 76, tower pot 77. towerpot thermometer :8.sol-N theory plate number of toweent tank 9 pump ;10. solvent tank 11 pump 12. glass rotameter ;INS AS2 input situation of extractive solventsglass rotameter 14. glass cellocotton 15. filler 16, tower top sampling中国煤化工 solvent kg/htap ;17. refluxmouth 18 tower top thermometer 19 condenser 20 elecCNMHGmagnetism bar 21. recovery sectieextraction section 23, extractive section 24 distillation sectionig.5 Experiment apparatus of extractive distillaGU Zhenggui et al Composite Extraction Separation of Ethylacetate-Ethanol-W aO3158277.X2003-09I References[5] Kato M, Konishi H, Hirata M. Measurement of vapor-liquie1 ] Zhang Sigui. Technology handbook of micro organic chemistrequilibrium data for ethyl acetate and ethanol[ J ]. J ChemM]. Beijing Science Press, 1992. 959-960Eng data,971l615)15-419[2 J Yu Hao. Chemical technology designing[ m ] shang[7 Lee Liangsun, Chem Chuan Huang Jinfeng. ExperimentsShanghai Science Technology Press, 1986. 206-312and correlations of phase equilibrium of ethanol-ethyl acetate-3 ]Wang Li, Xue Liangheng, Separation technology study of onewater ternary mixture J ]. J Chem Eng Jpn, 1996 29 3 )427step synthesis ethyl acetate(I J]. Modern Chemical 1996l611)8]Figurski G, Malanouski S K. Vapor-liquid equilibrium studies4 ]Bery loyd. Separation of ethyl acetate from ethanol byof the ethanol ethyl acetate systenl J ] Fluid phase equilihazeotropic distillation P ]. U. S patent 5993616,1999-06rium I998,1481-2):161-169[5 ]Gu Zhenggui, Zhi Huzhen. Composition extractive separate[9 Gu Zhenggui, Separation studies of benzene and thiopheneof ethyl acetate-ethanol-water P ]. Chinese patentfrom coal tat J ] Chemical Engineering 1992 ,20( 1 ) 25复合萃取分离乙酸乙酯-乙醇-水顾正桂职慧珍林军〔南京师范大学化学与环境科学学院江苏南京210007)[摘要]介绍了乙酸乙酯工艺提出了复合萃取法分离乙酸乙酯-乙醇水采用三对角距阵法模拟计算乙酸乙酯-乙醇-水分离结果建立萃取分离装置采用合适的萃取剂考察了不同溶剂比及回流比等因素对产品纯度的影响结果表明采用复合萃取分离法分离乙酸乙酯-乙醇水在溶剂比1:1:1,R=4时能一次得到高浓度9%酸乙酯同时得到95%的乙醇溶液,乙酸乙酯得率达到卯7%分离过程水的用量仅为原料的2倍能耗低为工业试验提供了基础数据[关键词]复合萃取乙酸乙酯乙醇水模拟实验[责仼编辑严海琳]中国煤化工CNMHG67