2,2,4-三甲基-1,3-戊二醇双苯甲酸酯类Z-N催化剂内给电子体的合成与应用  被引量:1

Synthesis and application of 2,2,4-trimethyl-1,3-pentanediol dibenzoate as internal electron donor in Z-N catalyst

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作  者:孙文姣[1] 刘敏[1] 许文倩[1] 李效军[1] 

机构地区:[1]河北工业大学化工学院,天津300130

出  处:《化学试剂》2011年第1期65-68,共4页Chemical Reagents

摘  要: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 compounds of 2,2,4-trimethyl-1,3-pentanediol dibenzoate functioning as internal donor were synthesized from isobutyraldehyde and benzoyl chloride through condensation,disproportionation and esterification.The key effects of esterification were studied.The optimum reaction conditions were as follows:the molar ratio of 2,2,4-trimethyl-1,3-pentanediol and benzoyl chloride was 1∶2.3;the molar ratio of triethylamine and benzoyl chloride was 3.0∶1;and the reaction time was 13 h.The product was washed with 5% NaOH aqueous solution for 30 min to remove triethylamine and surplus benzoyl chloride,and the yield of diesters reached 93.0% with its purity(analyzed by HPLC) exceeding 99.0%.The catalytic activity reached 5.2 kg of PP/g of catalyst when it was used for propylene polymerization,and the isotacticity of polypropylene was 96.50,with the melt index equating to 18.24.

关 键 词:内给电子体 2 2 4-三甲基-1 3-戊二醇双苯甲酸酯 合成 应用 

分 类 号:O625.5[理学—有机化学]

 

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