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由异丁醛和苯甲酰氯为原料经缩合、歧化、酯化合成了4种新型内给电子体化合物2,2,4-三甲基-1,3-戊二醇双苯甲酸酯,重点考察了酯化反应的影响因素。实验表明,该内给电子体的适宜合成条件为:醇与苯甲酰氯的物质的量比为1∶2.3;催化剂三乙胺与苯甲酰氯的物质的量比为3.0∶1;反应时间为13 h;后处理时,用5%NaOH水溶液洗涤30 min可除去三乙胺和过量的酰氯,苯甲酸酯的收率最高可达93.0%,HPLC纯度>99.0%。用于丙烯聚合时催化剂催化活性可达到52 kgPP/gcat,同时聚丙烯的等规度为96.50,熔融指数18.24。
Four novel internal electron donor compounds, 2,2,4-trimethyl-1,3-pentanediol bisbenzoate, were synthesized by condensation, disproportionation and esterification of isobutyraldehyde and benzoyl chloride. Focus on the esterification reaction factors. Experiments show that the internal electron donors suitable synthesis conditions: alcohol and benzoyl chloride material ratio of 1: 2.3; catalyst triethylamine and benzoyl chloride material ratio of 3.0: 1; reaction time was 13 h; after the treatment, 5% NaOH aqueous solution was washed for 30 min to remove triethylamine and excess acid chloride. The yield of benzoate was up to 93.0% and the HPLC purity was> 99.0%. The catalytic activity of the catalyst for propylene polymerization can reach 52 kgPP / gcat, while the polypropylene has an isotacticity of 96.50 and a melt index of 18.24.