石油化工高等学校学报
石油化工高等學校學報
석유화공고등학교학보
JOURNAL OF PETROCHEMICAL UNIVERSITIES
2013年
5期
33-36
,共4页
李孝国%赵甲%费亚南%孙国方%李佳%隋芝宇%于海斌
李孝國%趙甲%費亞南%孫國方%李佳%隋芝宇%于海斌
리효국%조갑%비아남%손국방%리가%수지우%우해빈
环保增塑剂%环己烷1,2-二甲酸二异辛酯%1,2-环己二甲酸%异辛醇
環保增塑劑%環己烷1,2-二甲痠二異辛酯%1,2-環己二甲痠%異辛醇
배보증소제%배기완1,2-이갑산이이신지%1,2-배기이갑산%이신순
Environmental plasticizer%Di(2-ethylhexyl) 1,2-cyclohexane dicarboxylate%1,2-Cyclohexanedicarboxylic acid%Iso-octylalcohol
以1,2-环己二甲酸和异辛醇为原料,浓硫酸为催化剂,酯化合成环保增塑剂环己烷1,2-二甲酸二异辛酯,考察了反应时间、醇酸物质的量比、反应温度等对酯化率的影响,并对产物进行了1 H-NMR、IR、TG及气相定性分析。结果表明,反应时间6 h ,反应温度170℃,醇酸物质的量比为2.5∶1时,酯化率可达99.5%,收率95%,产品为无色油状液体。核磁氢谱显示与酯基相连的亚甲基的多重峰信号δ在4.0处,红外谱图显示酯羰基的伸缩振动峰出现在1735 cm -1处,这些结果表明得到了预期产物。产物的T G曲线显示其外延起始温度为215℃,其气相出峰时间为14.310 min和14.505 min ,能够与邻苯二甲酸二异辛酯(DOP)有效分离。
以1,2-環己二甲痠和異辛醇為原料,濃硫痠為催化劑,酯化閤成環保增塑劑環己烷1,2-二甲痠二異辛酯,攷察瞭反應時間、醇痠物質的量比、反應溫度等對酯化率的影響,併對產物進行瞭1 H-NMR、IR、TG及氣相定性分析。結果錶明,反應時間6 h ,反應溫度170℃,醇痠物質的量比為2.5∶1時,酯化率可達99.5%,收率95%,產品為無色油狀液體。覈磁氫譜顯示與酯基相連的亞甲基的多重峰信號δ在4.0處,紅外譜圖顯示酯羰基的伸縮振動峰齣現在1735 cm -1處,這些結果錶明得到瞭預期產物。產物的T G麯線顯示其外延起始溫度為215℃,其氣相齣峰時間為14.310 min和14.505 min ,能夠與鄰苯二甲痠二異辛酯(DOP)有效分離。
이1,2-배기이갑산화이신순위원료,농류산위최화제,지화합성배보증소제배기완1,2-이갑산이이신지,고찰료반응시간、순산물질적량비、반응온도등대지화솔적영향,병대산물진행료1 H-NMR、IR、TG급기상정성분석。결과표명,반응시간6 h ,반응온도170℃,순산물질적량비위2.5∶1시,지화솔가체99.5%,수솔95%,산품위무색유상액체。핵자경보현시여지기상련적아갑기적다중봉신호δ재4.0처,홍외보도현시지탄기적신축진동봉출현재1735 cm -1처,저사결과표명득도료예기산물。산물적T G곡선현시기외연기시온도위215℃,기기상출봉시간위14.310 min화14.505 min ,능구여린분이갑산이이신지(DOP)유효분리。
Environmental plasticizer di(2-ethylhexyl) 1 ,2-cyclohexane dicarboxylate was synthesized through esterification reaction of 1 ,2-cyclohexanedicarboxylic acid (CHDA ) with iso-octanol using concentrated sulfuric acid as catalyst .Effects of reaction time , ratio of alcohol to acid and temperature on esterification rate were investigated . Under optimal reaction conditions :6 h ,170 ℃ ,n(alcohol)/n(acid) = 2 .5∶1 ,esterification rate and yield mount to 99 .5% and 95% ,respectively . The product was colorless transparent oily liquid .In the 1 H-NMR spectra ,the multiplet for the -COOCH2 appeared at δ=4.0 .IR spectra exhibitedυ(C O) band at 1 735 cm -1 .The results demonstrate the target product was synthesized .TG curve shows that initial temperature was 215 ℃ .Also ,a method for qualitative analysis was established ,the retention time of the product were 14.310 min and 14 .505 min ,which can separate from DOP effectively .