摘要
以生物基腰果酚(cardanol)为原料,对甲苯磺酸为催化剂,与乙酸酐进行酯化反应得到腰果酚乙酸酯(CA);然后,以甲酸为催化剂,双氧水为氧源合成环氧腰果酚乙酸酯(ECA)。考察了双氧水的质量分数、甲酸和双氧水用量、反应温度、反应时间等对产品环氧值的影响。确定了最佳工艺条件为:质量分数70%H2O2,n(甲酸)∶n(H2O2)∶n(CA中双键)=0.2∶1.5∶1、反应温度为65℃、反应时间为6 h。在最优条件下得到的产品为黄色透明油状液体,其环氧值可达到6.8%。采用傅里叶变换红外光谱(FTIR)对CA及ECA进行结构表征,并测定了ECA的酸值、加热减量、黏度、热重曲线等。结果表明,ECA符合环保增塑剂的产品性能要求。
Cardanol acetate(CA) was synthesized by esterification reaction of bio-based cardanol with acetic anhydride, with p-toluene sulfonic acid as catalyst. Then ECA was prepared by the epoxidation of cardanol acetate(CA) by hydrogen peroxide as a clean oxidant and formic acid as catalyst. Herein, the influences of several related factors, including the concentration of hydrogen peroxide (H2O2), the amounts of formic acid and hydrogen peroxide, reaction temperature, and reaction time, on the epoxy value of product were discussed. Based on the aforementioned rules, the optimum conditions were concluded as follows:70% H2O2 ,n(formic acid):n(H2O2):n(the amount of double bond in CA) = 0. 2:1.5:1 ,the reaction temperature was 65℃ and the reaction time was 6 h. Furthermore, the epoxy value of the final product under the present conditions was 6.8% and a yellow transparent oily liquid was obtained. Simultaneously,the acid value, heating loss, viscosity and TG curves of the product were also investigated, respectively. The results indicate that ECA can satisfy the requirements of plasticizer.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2014年第6期753-758,共6页
Fine Chemicals
基金
"十二五"国家科技计划课题(2012BAD32B03)~~
关键词
腰果酚
环氧腰果酚乙酸酯
增塑剂
环氧化反应
橡塑助剂
cardanol
epoxidized cardanol acetate
plasticizer
epoxidation
rubber and plastics auxiliaries