响应面优化水性化环氧磷酸酯制备工艺  

Synthesis of waterborne epoxy phosphate ester by optimized response surface methodology

作　　者：付聪 袁爱群 白丽娟 黄增尉 Fu Cong;Yuan Aiqun;Bai Lijuan;Huang Zengwei(School of Chemistry and Chemical Engineering,Guangxi Minzu University,Nanning 530006,China)

机构地区：[1]广西民族大学化学化工学院,广西南宁530006

出　　处：《合成树脂及塑料》2022年第3期35-41,共7页China Synthetic Resin and Plastics

基　　金：国家自然科学基金(21666006)。

摘　　要：以磷酸和大分子环氧树脂为原料,磷钨酸为催化剂,制备了水性化环氧磷酸酯。采用单因素实验探究了环氧树脂与磷酸摩尔比、反应温度、搅拌速率、反应时间、溶剂用量以及催化剂用量对环氧基转化率的影响,通过响应面实验优化制备工艺,对得到的化学键合型环氧树脂进行表征,并对催化机理进行探究,测试其水性化性能。结果表明,固定搅拌速率100 r/min,环氧树脂与磷酸摩尔比3∶1,各因素对环氧基转化率的影响由大到小依次为:磷钨酸用量、反应温度、反应时间、溶剂用量。较优工艺为:磷钨酸用量1.15%(w),反应时间160 min,反应温度53℃,溶剂用量26 mL,此条件下环氧基转化率为93.27%,所制备的水性化环氧磷酸酯乳液水分散性、稳定性良好。Waterborne epoxy phosphate ester was prepared with phosphoric acid and macromolecular epoxy resin as raw materials and phosphotungstic acid as catalyst.The effects of mole ratio of epoxy to phosphoric acid,reaction temperature,stirring rate,reaction time,amount of solvent and catalyst on the conversion of epoxy group were investigated by single factor experiment.The preparation process was optimized by response surface methodology,and the obtained chemically-bonded epoxy emulsion was characterized.The catalytic mechanism was also explored to test its water-soluble property.The results show that the order of the factors affecting the conversion of epoxy group is as follows:phosphoric acid content,reaction temperature,reaction time,and solvent content when the molar ratio of epoxy to phosphoric acid is 3∶1 at 100 r/min.The conversion of epoxy group is 93.27%under the optimum conditions of 1.15%(w)of phosphoric acid,160 min of reaction time,53℃of reaction temperature and 26 mL of solvent.The waterborne epoxy phosphate ester prepared performs excellently in water dispersion and stability.

关 键 词：水性化环氧磷酸酯 化学键合 自乳化法 磷酸 

分 类 号：TQ62[化学工程—精细化工]