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作 者:岳彦山[1] 张岩[1] 赵殊[1] 郭超[1] 王兴宁[1] 梁志斌[1]
机构地区:[1]黑龙江省阻燃材料分子设计与制备重点实验室,东北林业大学理学院,黑龙江哈尔滨150040
出 处:《中国胶粘剂》2010年第1期1-5,共5页China Adhesives
基 金:国家科技支撑计划课题资助项目(2006BAE03B06)
摘 要:以对氯苯酚作为多亚甲基多苯基多异氰酸酯(PAPI)的封闭剂、二月桂酸二丁基锡和三乙胺作为复合催化剂,研究了催化剂、投料配比、加料方式、反应温度和反应时间等对封闭反应的影响。采用红外光谱(FT-IR)法和核磁共振(NMR)法对-NCO含量的变化情况进行分析,并采用FT-IR法测定解封闭温度。结果表明:对氯苯酚封闭PAPI的适宜反应条件为n(-OH)/n(-NCO)=1.03、n(二月桂酸二丁基锡)∶n(三乙胺)∶n(对氯苯酚)=0.2∶0.2∶100、反应温度为40℃、PAPI溶液滴加到对氯苯酚溶液中的滴加时间为1 h以及反应时间为1 h;对氯苯酚封闭异氰酸酯的解封闭温度为87℃。With p-chlorophenol as blocking agent of muhimethylene muhiphenyl muhiisocyanate ( PAPI ), tin dibutyl dilaurate and triethylamine as composite catalyst, so the influences of different factors (such as catalyst, feeding proportion, charging wise, reaction temperature and reaction time) were investigated on blocking reaction. The changes of-NCO contents were analysed by Fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance (NMR), and the deblocking temperature was determined by FT-IR. The results showed that the deblocking temperature of isocyanate blocked by p-chlorophenol was 87℃. The optimum reaction condition for PAPI blocked by p-chlorophenol was obtained when molar ratio of n (-OH) :n (-NCO) was 1.03:1, molar ratio of n (tin dibutyl dilaurate ) : n ( triethylamine ) : n (p - chlorophenol ) was 0.2: 0.2: 100, reaction temperature was 40℃, dripping time (namely PAPI solution was introduced into p-chlorophenol solution) and reaction time were all 1 h.
关 键 词:多亚甲基多苯基多异氰酸酯 封闭 解封 对氯苯酚
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