磷酸改性高环氧值环氧树脂  

Modification of epoxy resin with high epoxy value by phosphoric acid

作　　者：白丽娟 付聪 袁爱群 黄增尉 BAI Lijuan;FU Cong;YUAN Aiqun;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：《电镀与涂饰》2022年第20期1463-1470,共8页Electroplating & Finishing

基　　金：国家自然科学基金(21666006)。

摘　　要：在磷钨酸催化下,用磷酸改性高环氧值环氧树脂得到了水性化树脂。探究了环氧树脂与磷酸的物质的量比、磷钨酸加入量(相对于环氧树脂的质量)、温度、时间、丙酮加入量和搅拌速率对环氧基转化率的影响,采用正交试验法优化工艺条件,以傅里叶变换红外光谱(FT-IR)和核磁共振(NMR)表征产物,并测试其性能,建立了不同温度下的反应动力学模型。结果表明:在搅拌速率100 r/min的情况下,5个因素对转化率的影响次序为:温度>丙酮加入量>环氧树脂与磷酸的物质的量比>磷钨酸加入量>反应时间。较优的工艺条件为:环氧树脂与磷酸的物质的量比1∶2,磷钨酸量加入量1.3%,温度45℃,时间130 min,丙酮15 mL。环氧基转化率可达98.07%。该反应在35、45和55℃下均为二级反应,活化能约为26.6 kJ/mol。An epoxy resin with high epoxy value was modified by phosphoric acid under the catalysis of phosphotungstic acid.The effects of the factors i.e.molar ratio of epoxy to phosphoric acid,reaction temperature,amount of acetone,reaction time,phosphotungstic acid dosage(with respect to the mass of epoxy resin),and stirring speed on the conversion of epoxyl group were studied.The process conditions were optimized by orthogonal test.The product was characterized by Fourier-transform infrared(FT-IR)spectroscopy and nuclear magnetic resonance(NMR),and its properties were tested.The kinetic models for the reaction at different temperatures were established.The results showed that when the stirring rate was 100 r/min,the effects of the factors on conversion rate of epoxyl group were in the following descending order:reaction temperature>amount of acetone>molar ratio of epoxy to phosphoric acid>phosphotungstic acid dosage>reaction time.The conversion rate of epoxyl group could reach up to 98.07%under the optimized conditions:molar ratio of epoxy to phosphoric acid 1:2,phosphotungstic acid 1.3%,reaction temperature 45℃,reaction time 130 min,and acetone 15 mL.The reaction was second order at 35,45,and 55℃ with an activation energy about 26.6 kJ/mol.

关 键 词：水性环氧树脂 高环氧值 改性 磷酸 磷钨酸 

分 类 号：TQ62[化学工程—精细化工]