摘要
研究了响应面法优化4-丙烯酸羟丁酯(4-HBA)的微波合成工艺过程研究。在合成工艺中利用微波辐射法,以1,4-丁二醇(BDO)和丙烯酸(AA)为主要原料合成4-HBA。以4-HBA的酯化率为考察指标,探讨了反应温度、微波辐射时间、微波功率、催化剂用量及醇酸摩尔比等单因素对酯化反应的影响。基于单因素实验,固定反应温度110℃、微波功率700 W,采用Box-Behnken响应面法对微波合成工艺过程中的微波辐射时间、催化剂用量及醇酸摩尔比3个参数进行优化,得出最优的合成工艺条件为:n(BDO)∶n(AA)=2.9∶1,催化剂用量为3.52%(对反应物总质量),反应时间为26 min,在此最佳实验条件下进行重复实验3次,得到4-HBA的酯化率为70.04%。
Optimizing the microwave synthesis process of 4-hydroxybutyl acrylate(4-HBA)with response surface method was studied.4-HBA was synthesized with 1,4-butanediol(BDO)and acrylic acid(AA)as raw material by microwave irradiation method.The factors which can influence the esterification rate of 4-HBA such as reaction temperature,microwave irradiation,microwave power,catalyst dosage and molar ratio of alcohol to acid were explored and discussed.Based on the single factor experiment,in condition of 110℃fixed reaction temperature and 700 W microwave power,these three parameters of the microwave irradiation time,the microwave power,the catalyst dosage and molar ratio of alcohol to acid were optimized by using Box-Behnken response surface methodology.The best result is n(BDO)∶n(AA)=2.9∶1,catalyst ratio of 3.52%(the total mass of reactants),reaction time of 26 min,the esterification rate of 4-HBA could reach to 70.04%after repeated 3 times with the above optimal experiment conditions.
作者
来水利
高沁
蔡建华
陈军
LAI Shui-li;GAO Qin;CAI Jian-hua;CHEN Jun(Key Laboratory of Auxiliary Chemistry&technology for Chemical Industry,Ministry of Education,Shaanxi University of Science&Technology,Xi′an 710021,Shaanxi Province,China;Jiangxi United Chemical Co.,Ltd.,Jiujiang 330300,Jiangxi Province,China)
出处
《化学工程》
CAS
CSCD
北大核心
2018年第3期57-61,共5页
Chemical Engineering(China)
基金
陕西省科技攻关项目(2015SF266)
关键词
微波加热
酯化反应
响应面
4-丙烯酸羟丁酯
microwave heating
esterification reaction
response surface
4-hydroxybutyl acrylate
