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摘要
以四甲基胍为开环催化剂,通过酯化闭环法合成甲基丙烯酸缩水甘油酯(GMA)。探究了各工艺条件对中间开环产物产率(Y1)及GMA产率(Y2)的影响。在单因素实验的基础上,以物料摩尔比、反应温度和催化剂质量分数为自变量,根据Box-Behnken试验设计原理,利用Design Expert软件模拟得到二次多项式回归方程的预测模型,优化GMA的合成工艺。方差分析结果表明,此回归模型对试验的拟合较好,可以对Y1和Y2进行很好地分析和预测,得到了各因素对Y1和Y2的响应曲面。最佳优化条件为:甲基丙烯酸与环氧氯丙烷的摩尔比为1:2.26,反应温度为81℃,催化剂质量分数为1.4%,优化后的Y1为73.25%,Y2为63.17%,实测值与预测值的相对误差分别为1.89%和0.96%,说明最佳优化工艺的可靠性较高。
Abstract
Glycidyl methacrylate (GMA) is synthesized through asymmetric ring-opening reaction of epichlorohydrin (ECH) with 1,1,3,3-tetramethylguanidine as ring-opening catalyst.The influences of various synthesis parameters on the yield (Y1) of intermediate ring-opening products and the yield (Y2) of GMA are investigated.Based on the single factor experiments and taking the molar ratio of materials,reaction temperature and catalyst dosage as variables,a prediction model in a form of quadratic polynomial regression equation is obtained through simulating by means of Design Expert software according to Box-Behnken experiment design principle.The synthesis process of GMA is optimized accordingly.The results of variance analysis reflect that this regression model can fit well for the experiments and can analyze and predict Y1 and Y2 well.The response surfaces of various factors on Y1 and Y2 are gained.The optimal conditions are as follows:the molar ratio between methacrylic acid and ECH is 1:2.26,reaction temperature is at 81℃ and mass fraction of catalyst is 1.4%.Under optimal conditions,Y1 and Y2 can reach 73.25% and 63.17%,respectively.The relative errors for real values and prediction values are 1.89% and 0.96%,respectively,showing that the optimal conditions have high reliability.
关键词
甲基丙烯酸缩水甘油酯
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响应面
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环氧化合物
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开环
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催化剂
Key words
glycidyl methacrylate
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response surface
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epoxide
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ring-opening
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catalyst
Author summay
孙永利(1967-),男,博士,研究员,研究方向为化工传质与分离及过程强化,sunyongli@tju.edu.cn
响应面法优化甲基丙烯酸缩水甘油酯合成工艺研究[J].
现代化工, 2018, 38(7): 154-158 DOI:10.16606/j.cnki.issn0253-4320.2018.07.035