摘要
以脂肪醇聚氧乙烯醚(AEO)和甲基丙烯酸丁酯(BMA)为原料,通过共沸分馏酯交换工艺合成了脂肪醇聚氧乙烯醚甲基丙烯酸酯(AEOMA)。通过在反应体系中引入共沸剂甲苯提高了酯交换反应的速率。确定了酯交换反应的最佳工艺条件:AEO用量0.10mol、n(BMA)∶n(AEO)=11、阻聚剂Z-701用量(占BMA的质量分数)0.30%、催化剂Ca2用量(占BMA的质量分数)2.0%、甲苯用量1.2mol、反应时间9h。在此条件下,AEO的转化率为97.0%。采用油水混合萃取分离工艺,提高了产品分离效率和产品纯度,使AEOMA的收率达95.0%,纯度达97.0%。红外光谱表征结果表明,AEO分子中的羟基全部转化为酯键,并在分子中引入了双键,生成了AEOMA。
Alkyl polyethyleneoxide ether methacrylate （AEOMA） was prepared from alkyl polyethyleneoxide ethers （ AEO ） and butyl methacrylate （ BMA ） by azeotropic-distillation transesterification. Addition of toluene to the reaction system can sharply accelerate the reaction and delete the necessity of adding polymerization inhibitor into vapor phase to prevent polymerizing of BMA in the phase. Toluene not only acts as entrainer of byproduct low alcohols to promote the proceeding of reaction but also greatly lowers concentration of BMA in vapor phase at same time, therefore its polymerization is avoided. The optimal conditions are as follows： n （BMA） ： n （AEO） 11, AEO 0. 10 mol, inhibiter Z-701 mass fraction 0.30% of BMA, catalyst Ca2 mass fraction 2.0% of BMA, toluene 1.2 mol,reaction time 9 h, conversion of AEO is 97.0%. The product and residual raw materials are separated with high productive efficiency through water/organic phase extraction. The materials in organic phase can be recycled. Yield of AEOMA is 95.0% and its purity is 97.0%. IR result shows that hydroxyl groups of AEO had transformed into ester groups.
出处
《石油化工》
CAS
CSCD
北大核心
2008年第2期174-177,共4页
Petrochemical Technology
