马来酸酐与乙醇胺的酰化反应的研究

28 151999- CHINA LEATHER Vol. 28 No. 15 Aug. 1999三Bf Study on Acylation of Maleic Anhydride with Ethanclamine二§本,712081)‰■(,oe,-16012) Lan Yunjun, Li Linsheng( Leather Engineering Dept., Northwest Institute of Light Industry, Xianyang 712081) Yang Jinzong (State Key Laboratory of Fine Chemicals,Dalian University of Technology, Dalian 116012)th-feT‰fi“‰士 <..+ f-f-fl-f-, HPLC- -..=...% =FEB SF-f fl E-fl Abstract The reaction product of ethanolamine with maleic anhydride is one of the intermediate for preparing dye -aidding amphoteric polymer tanning agents-PT. The action of dispersing medium and catalyst on the esterification and amidation of ethanol amine were explored. Under controlled conditions, there was no unreacted ethanolamine detected in acylation products by HPLC. Keywords amphoteric polymer tanning agent maleic anhydride maleic acid derivatives acylation esterification amidation.‰f‰ 55'Sp33PT‰ >>(RCOL)R>fls-f:(3)二R M-f=..: "B(1) (4),N-.>>. DM-mol/; HC-COOCH.CH:NHL FA)AR V-f=.. HNCHCHOH HC-COOH1.2-ml;(1)-156.11-KOH‰”,ta-1-(2)f1(2)HP1050- HOCHCHINH+ HC-CONHCHCH:OH HIC→ HC-COOHHP1047a,‰<甲Ta--‰ds254.6),ff-701C60:40(HCl‰p),十千°。 30min, <1....-- .. 2mol EB9mol1.3PTA-=‰‰七￥,‰‰mol-T10min HOOC -CH CH- ..mol ".(), COOCH2CH,NHOC-CH =CH- - "..-molDMFA 2PTA-I -COOH≤70C‰。2.2B-f号.3%1‰2‰B1-、f60~65c.---2.1--f号-fB≤,,‰‰H90c‰e90±1c-f-f十‰--ff-三---,eife---a升‰-f中‰<(+0H)100C-‰‰h-ff‰B什e,一 "-o.""," --f-,BT升-1.4PTA-1‰=n+(三Bh-ff二tce￥f七千 -1 +ss<...-ff-fi”+1.5~(mgKOH/g) 3g". =.-Sml~10ml- DMFABf--1‰二二fi-fi5mn-120.4120.4468.0468.0-fB二,‰eTo=0min118.4116.9442.1428.5-,0ml~30mlt=15min114.8112.0433.2418.0tii23t=30min112.1108.2425.0408.7 0. 5mol/1-="=60min 108.3102.8415.6393.4年15~4=90min104.999.1408.3384.5t=120min102.795.7402.7380.0tg=150min101.694.3400.8377.8m56.1110101100177 28 151999 CHINA LEATHER Vol. 28 No. 15 Aug. 1999“sf.‰-f‰,B-ff二-B-f-f-B2+-f1,‰B.2丰,一年1‰1丰三 f-,. -B ..() ;-0 ...-e-f -- DMFA$.-Tff13.03%B3060902015080 (Ao/2),....- fi-f> 100%fl, ", fidmfa--,:eTiO2·SO4Y=100%-X(2)ZrO2·SO4)二f11--1二‰什-f,2-二(A) +fI"TE-I-%:f‰ff450 Ao4402×X+Ao×Y=A(3)‰fTBT分升 >>fl +f-f=一1 >>flf,",,400聊X=0.5A0×100%(4)二DMFA2DMFA-f-f373000120156n)B-一f-tf氏,f-f年十 DMFA.2-f-,(Ao)--5.98%,f+fB---f9.79%f1 B-ffl --E22 EOmg KOH/..-% f-BfA1--二2-二 g... B...-ce-.丰+100%tfX) -...升-i什 _fl e..%X=(1-A/A)X100%(5)0+--f%‰-B-ffTE-fBfI￥frf1fT￥‰fe=frft三B-f2.5h-efte-f1-f1-h-正o1+t‰十一‰,3h%4)()‰‰‰f-fo一T‰二一-年￥f1%,-f一- DMFA- -BEEfl-714980166028151999 CHINA LEATHER Vol. 28 No. 15 Aug.1999…4)-f,, EB-f=PTA-1 -o<-e一一‰>-二542质峰5.705)6.26EA一。(-(2)B1 ->> .3 EA HPLC2.3B- toe s--f--...hPC-B-十七5.7060981,1996,7 -mol36~39B9mol什e2f、+千tr-+f,-f-f .4. PTA-I APLC十f-f‰.HPLC1992,290~291 ..PTA-I <--f--... 3-EGB/T73841996.--B-3‰e 4 T. Alfrey et al. ,J. A. C.S. 1945,67, foi... (1) EB -. 2044(Eng)二6.3%(W/)二1:1:1.02(11-:1998