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马来酰亚胺封端有机硅齐聚物的合成与表征
Synthesis and Characterization of Triethylene Glycol Bis[3-(3′,5′-di-tert-butyl-4′-hydroxyphenyl)] Propionate
【摘要】 以二苯基二氯硅烷和对苯二酚为原料,采用熔融缩聚反应合成了有机硅预聚物,FT-IR证明了其化学结构,研究表明高温、高真空、长时间的反应有利于预聚物分子量的增长;同时利用N-(4-羟基苯基)马来酰亚胺与有机硅预聚物溶液缩合,采用乙酸乙酯为溶剂,吡啶为缚酸剂,制备了马来酰亚胺封端有机硅齐聚物,利用FT-IR,1HNMR和DSC对其结构进行了表征,利用端基滴定法测定了齐聚物的分子量。
【Abstract】 Triethylene glycol bis[3-(3′,5′-di-tert-butyl-4′-hydroxyphenyl)] propionate is prepared with methyl-3-[3′,5′-di-tert-buty-4′-hydroxyphenyl] propionate and triethylene glycol as raw materials, organic tin as catalyst and under the trans-esterification reaction with toluene as solvent. The influences of temperature, time, catalyst and quantity of catalyst used, and molar ratio of raw materials on the yield of the product are studied through experimental test. The result shows that, the optimal conditions are as follows : reaction temperature 120~125℃; catalyst used tin and quantity 0.25g; reaction time 3.5h; molar ratio of methyl-3-[3′,5′-di-tert-butyl-4′-hydroxyphenyl] propionate to triethylene glycol 2.10∶1. The yield of the product under this condition is over 94% with melting point of the product 106~107℃. Elemental analysis, IR and ~1 HNMR characterized the structure of the product.
- 【文献出处】 河南化工 ,Henan Chemical Industry , 编辑部邮箱 ,2004年01期
- 【分类号】TQ324.21
- 【被引频次】3
- 【下载频次】113