聚丙烯催化剂内给电子体环戊基-1,1-二甲醇二甲醚的合成

石油炼制与化工

聚丙烯催化剂内给电子体环戊基-1,1-二甲醇二甲醚的合成

许招会,江新涛,刘宏,廖维林

江西师范大学化学化工学院

收稿日期:2011-02-11 修回日期:2011-06-27 出版日期:2011-09-12 发布日期:2011-09-12
通讯作者: 许招会

SYNTHESIS OF POLYPROPYLENE CATALYST INTERNAL DONOR 1,1-CYCLOPENTYL DIMETHANOLDIMETHYL ETHER

xu zhao-hui

Received:2011-02-11 Revised:2011-06-27 Online:2011-09-12 Published:2011-09-12
Contact: xu zhao-hui

摘要/Abstract

摘要： 以丙二酸二乙酯和1,4-二溴丁烷为起始原料,经烷基化、酯还原和醚化反应合成环戊基-1,1-二甲醇二甲醚，分别考察关键因素对3步合成反应的影响。适宜的工艺条件为：①烷基化反应时，n(丙二酸二乙酯):n(CsOH):n(1,4-二溴丁烷)=1.0:2.2:1.4，CsOH 为催化剂，环戊基-1,1-二甲酸二乙酯的收率为93.0%；②酯还原反应时，以无水ZnCl2为催化剂，n(环戊基-1,1-二甲酸二乙酯):n(KBH4)=2.0:1.0，环戊基-1,1-二甲醇的收率为88.1%；③醚化反应时，以四丁基溴化铵为催化剂，n(环戊基-1,1-二甲醇):n(NaOH):n(碳酸二甲酯)= 1.0:8.0:2.4，环戊基-1,1-二甲醇二甲醚的收率为61.2%。以丙二酸二乙酯为计三步反应的总收率为50.1%。

关键词: 环戊基-1，1-二甲醇二甲醚, 丙二酸二乙酯, 1,4-二溴丁烷, 内给电子体

Abstract: 1,1-Cyclopentyl dimethanoldimethyl ether was synthesized from diethyl malonate and 1,4-dibromo butane by alkylation, ester reduction and etherification. The key factors affecting reactions were studied and the optimal reaction conditions were found as follows: (1) for alkylation, using CsOH as catalyst, n(diethyl malonate):n(CsOH):n(1,4-dibromo butane)=1.0:2.2:1.4, the yield of cyclobutane-1,1-dicarboxylic acid diethyl ester was 93.0%; (2)for ester reduction, using anhydro-ZnCl2 as catalyst, n(cyclopentyl-1,1-dicarboxylic acid diethyl ester):n(KBH4)=2.0:1.0, the yield of 1,1- cyclopentyl dimethanol was 88.1%; (3)for etherification, using tetrabutyl ammonium bromide as catalyst, n(1,1-cyclopentyl dimethanol)∶n(NaOH)∶n(dimethyl carbonate)=1.0∶8.0∶2.4, the yield of 1,1- cyclopentyl dimethanoldimethyl ether was 61.2%. The total yield of the objective product was 50.1% based on diethyl malonate.

Key words: 1,1- Cyclopentyl dimethanoldimethyl ether, diethyl malonate, 1,4-dibromo butane, internal donor

许招会,江新涛,刘宏,廖维林. 聚丙烯催化剂内给电子体环戊基-1,1-二甲醇二甲醚的合成[J]. 石油炼制与化工, doi: .

xu zhao-hui. SYNTHESIS OF POLYPROPYLENE CATALYST INTERNAL DONOR 1,1-CYCLOPENTYL DIMETHANOLDIMETHYL ETHER[J]. Petroleum Processing and Petrochemicals, doi: .