可见光LED敏感的光产碱体系制备及应用  

Preparation and application of visible light LED sensitive photobase generator system

作　　者：碗梦迪 朱伟特 李治全 刘晓暄[1,2] Wan Mengdi;Zhu Weite;Li Zhiquan;Liu Xiaoxuan(School of Materials and Energy,Guangdong University of Technology,Guangzhou 510006,Guangdong,China;Guangdong Laboratory of Chemistry and Fine Chemical Industry Jieyang Center,Jieyang 522000,Guangdong,China)

机构地区：[1]广东工业大学材料与能源学院,广东广州510006 [2]化学与精细化工广东省实验室揭阳分中心,广东揭阳522000

出　　处：《中国胶粘剂》2024年第10期23-30,37,共9页China Adhesives

基　　金：揭阳市(扬帆计划)引进创新创业团队和领军人才项目(CXTD2021001)。

摘　　要：针对目前光产碱剂吸收波长短,难以与常用的可见光LED光源相匹配的问题,基于光敏化机理,本文通过将脒类光产碱剂的还原,合成了一种非离子型光产碱剂(PL-DBN),并对其结构进行表征。将其与光敏剂(CQ、COU和ITX)分别进行复配,制备了3种可见光敏感的光产碱体系(PL-DBN/CQ、PL-DBN/COU和PLDBN/ITX),系统探究了其光物理及光化学行为。研究结果表明:(1)核磁氢谱表明,CQ、COU和ITX成功制备了目标产物PL-DBN。(2)通过研究3种光敏剂的光吸收性能,决定选用不同吸收范围的光敏剂(CQ、COU和ITX)分别与PL-DBN复配。(3)通过稳态光解试验探究了不同光敏剂在405 nm光源下光解的效率,其中PL-DBN/ITX在405 nm LED光源辐照下光解速度较快,更适合用于复配光产碱体系。(4)通过紫外-可见吸收光谱的变化,得出光产碱体系光解后产生的碱性物质与苯酚红发生了酸碱中和反应,证明PL-DBN在405 nm光源辐照下可发生光致产碱反应。(5)通过差示扫描量热仪和傅里叶变换红外光谱仪考察了光照时间对巯基-环氧聚合动力学的影响。辐照10 min就可将体系的起始固化温度降低23℃,且光照10 min后再短时间加热,巯基和环氧官能团的转化率可缓慢增至95%以上。(6)将光热双重固化的巯基-环氧体系进行粘接强度的测试,光产碱催化的巯基-环氧体系具有暗固化特性,可在延时固化胶粘剂中应用,未来具有一定的应用潜力。In response to the current problem of short absorption wavelength of photobase generator,which was difficult to match with commonly used visible light LED sources,based on the photosensitization mechanism,in this paper,a non-ionic photobase generator(PL-DBN)was synthesized by reducing amidine photobase generator,and its structure was characterized.It was compounded with photosensitizers(CQ,COU and ITX),three kinds of visible light sensitive photobase generator systems(PL-DBN/CQ,PL-DBN/COU and PL-DBN/ITX)were prepared,and their photophysical and photochemical behaviors were systematically investigated.The research results showed that,(1)The nuclear magnetic hydrogen spectrum indicated that the target product PL-DBN was successfully prepared.(2)By studying the light absorption properties of three kinds of photosensitizers,it was decided to select photosensitizers(CQ,COU and ITX)with different absorption ranges to be compounded with PL-DBN,respectively.(3)The efficiency of photolysis of different photosensitizers under 405 nm light source was investigated through steady-state photolysis experiments.Among them,PL-DBN/ITX showed a faster photolysis rate under 405 nm LED light source irradiation,making it more suitable for use in composite photobase generator systems.(4)Through the changes in UV-visible absorption spectra,it was found that the alkaline substances produced by the photolysis of the photobase generator system underwent acid-base neutralization reaction with phenol red,proving that PL-DBN could undergo photo induced alkali production reaction under 405 nm light source irradiation.(5)The effect of irradiation time on the kinetics of thiol-epoxy polymerization was investigated by using differential scanning calorimetry and Fourier transform infrared spectroscopy.The initial curing temperature of the system could be reduced by 23℃after 10 minutes of irradiation,and the conversion rate of thiol and epoxy functional groups could slowly increase to over 95%during a short period of heating after 10 minutes of l

关 键 词：光产碱 脒类 光敏化 巯基-环氧 阴离子光聚合 

分 类 号：TQ430.4[化学工程]