CAJ | 학술논문

用N,N'-二甲基甲酰胺（DMF）作溶剂，对羟基苯甲酸甲酯作封闭剂，研究了其封闭甲苯-2,4二异氰酸酯（TDI）中封闭剂与TDI摩尔比、催化剂用量、反应温度与时间对封闭反应的影响。研究发现：当封闭剂与TDI摩尔比为3.0∶1、添加0.5%（基于TDI与封闭剂总质量）催化剂、反应温度80℃、反应3 h时能够获得99.81%的高封闭率。DSC测试显示，封闭产物在80℃以后即开始出现解封闭，但解封的高峰温度在124.7℃，完全解封的温度为130℃；利用红外光谱和核磁共振测试确定了封端产物的结构。
용N,N'-이갑기갑선알（DMF）작용제，대간기분갑산갑지작봉폐제，연구료기봉폐갑분-2,4이이청산지（TDI）중봉폐제여TDI마이비、최화제용량、반응온도여시간대봉폐반응적영향。연구발현：당봉폐제여TDI마이비위3.0∶1、첨가0.5%（기우TDI여봉폐제총질량）최화제、반응온도80℃、반응3 h시능구획득99.81%적고봉폐솔。DSC측시현시，봉폐산물재80℃이후즉개시출현해봉폐，단해봉적고봉온도재124.7℃，완전해봉적온도위130℃；이용홍외광보화핵자공진측시학정료봉단산물적결구。
A kind of blocked isocyanate adduct was synthesized by using methylparaben as blocking agent and N,N'-dimethylformamide (DMF) as solvent. The effects of molar ratio of blocking agent and toluene-2,4-diisocyanate (TDI),mass percent of catalyst,reaction temperature and reaction time on the blocking reaction were investigated. A high conversion of 99.81%for -NCO group was obtained, when molar ratio of blocking agent and TDI was 3.0∶1,reaction temperature was 80℃,reaction time was 3 h and mass percent of catalyst was 0.5% (based on total mass of blocking agent and TDI). Fourier transform infrared spectrometry (FTIR) and nuclear magnetic resonance (NMR) were used to determine the structure of the adduct. Differential scanning calorimetry (DSC) results showed that the adduct began to deblock at 80 ℃ while deblocking peak temperature was 124.7 ℃ and throughout deblocking temperature was 130℃.