UV固化高活性乙烯基树脂的微反应器合成及性能研究  

Study on the microreactor synthesis and properties of UV-curable vinyl resin with high activity

作　　者：高景瑞 谢晖 黄莉 张利雄 王玲 戴俊峰 张明 宋向伟 GAO Jingrui;XIE Hui;HUANG Li;ZHANG Lixiong;WANG Ling;DAI Junfeng;ZHANG Ming;SONG Xiangwei(College of Chemical Engineering,Nanjing Tech University,Nanjing 211800,China)

机构地区：[1]南京工业大学化工学院,江苏南京211800

出　　处：《南京工业大学学报（自然科学版）》2023年第2期142-148,共7页Journal of Nanjing Tech University(Natural Science Edition)

摘　　要：为解决乙烯基树脂合成反应温度不易控制的问题,同时提高反应活性及韧性,在微反应器中利用甲基丙烯酸缩水甘油酯(GMA)对乙烯基树脂进行改性。在环氧树脂中n(环氧基);n(甲基丙烯酸(MAA))=1∶1、催化剂四丁基溴化铵(TBAB)的质量分数为1%、阻聚剂对羟基苯甲醚(MEHQ)的质量分数为0.2%、反应温度为150℃、流速为1.58 mL/min、停留时间为10 min的反应条件下,合成乙烯基树脂。再利用GMA进行改性,增加其双键含量,在n(羟基)∶n(GMA)=1∶1、催化剂三乙胺(TEA)的质量分数为1.5%、阻聚剂MEHQ的质量分数为0.2%、停留时间为15 min、流速为1.053 mL/min下反应,转化率高达90%以上,产物性能较好。通过凝胶渗透色谱(GPC)对产物表征,数据表明树脂分子量分布较均匀。采用傅里叶变换红外光谱仪(FT IR)对产物结构进行表征,表明成功制备出高活性乙烯基树脂。通过紫外光(UV)固化发现,与乙烯基树脂相比,高活性乙烯基树脂固化时间短,热稳定性好,柔韧性提高。To solve the problem of the synthesis reaction temperature of vinyl resin was not easy to control,and to improve the reaction activity and toughness,glycidyl methacrylate(GMA)was used to modify the vinyl resin in the microreactor.The vinyl resin was synthesized when n(epoxy group)∶n(methacrylic acid(MAA))=1∶1,the mass fraction of catalyst tetrabutylammonium bromide(TBAB)was 1%,the mass fraction of inhibitor p-hydroxyanisole(MEHQ)was 0.2%,the reaction temperature was 150℃,the flow rate was 1.58 mL/min,and the residence time was 10 min.Then,the GMA was modified to increase the content of double bond,n(hydroxyl)∶n(GMA)=1∶1,the mass fraction of catalyst triethylamine(TEA)was 1.5%,the mass fraction of inhibitor MEHQ was 0.2%,the residence time was 15 min,and the flow rate was 1.053 mL/min.The conversion rate was above 90%,and the product performance was good.The product was characterized by gel permeation chromatography(GPC),and the data showed that the molecular weight distribution of the resin was uniform.The structure of the product was characterized by Fourier transform infrared spectroscopy(FT-IR),indicating that the high activity vinyl resin was successfully prepared.Through UV-curing,it was found that compared with vinyl resin,high activity vinyl resin had shorter curing time,better thermal stability and higher flexibility.

关 键 词：微反应器 改性乙烯基树脂 甲基丙烯酸缩水甘油酯 双键含量 高活性 

分 类 号：TQ630.1[化学工程—精细化工]