Synthesis of Polycarbonate Diols(PCDLs) via Two-step Process Using CH3COONa as an Effective Catalyst

doi:10.1007/s40242-018-7390-0

高等学校化学研究 ›› 2018, Vol. 34 ›› Issue (4): 578-583.doi: 10.1007/s40242-018-7390-0

Synthesis of Polycarbonate Diols(PCDLs) via Two-step Process Using CH₃COONa as an Effective Catalyst

SONG Menglu^1,2, YANG Xiangui¹, WANG Gongying¹

1. Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041, P. R. China;
2. University of Chinese Academy of Sciences, Beijing 100049, P. R. China

收稿日期:2017-12-05 出版日期:2018-08-01 发布日期:2018-03-29
通讯作者: YANG Xiangui E-mail:yangxg@cioc.ac.cn
基金资助:
Supported by the National Key Research and Development Program, China(No.2018YFB0605804), the Key Research and Innovation Program of Jiangsu Province, China(No.BE2015055), and the Science &Technology Pillar Program in Sichuan Province, China(No.2016GZ0228).

Synthesis of Polycarbonate Diols(PCDLs) via Two-step Process Using CH₃COONa as an Effective Catalyst

SONG Menglu^1,2, YANG Xiangui¹, WANG Gongying¹

1. Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041, P. R. China;
2. University of Chinese Academy of Sciences, Beijing 100049, P. R. China

Received:2017-12-05 Online:2018-08-01 Published:2018-03-29
Contact: YANG Xiangui E-mail:yangxg@cioc.ac.cn
Supported by:
Supported by the National Key Research and Development Program, China(No.2018YFB0605804), the Key Research and Innovation Program of Jiangsu Province, China(No.BE2015055), and the Science &Technology Pillar Program in Sichuan Province, China(No.2016GZ0228).

摘要/Abstract

摘要： Polycarbonate diols(PCDLs) with a number average molecular weight(M_n) of 2800 and a narrow polydispersity index(PDI=1.33) were synthesized from dimethyl carbonate(DMC) and 1,4-butanediol(BD) via a two-step process. The influences of the molar ratios of DMC to BD in the feedstock, polycondensation temperature and polycondensation time on the PCDLs preparation were studied. CH₃COONa showed the best catalytic performance among the catalysts studied. The highest BD conversion of 73.8% and PCDLs yield of 64.7% were achieved under its optimum reaction conditions. Furthermore, based on the results of ¹H NMR, the relationships between the ratio of end groups (-OCH₃/-OH) of oligomers, the M_n and chain-end constitute of resultant polycarbonates were also investigated. The results indicate that PCDLs can be synthesized when the oligomers mostly bear hydroxyl end groups. In contrast, it was impossible to prepare PCDLs when the oligomers were enriched with methyl carbonate end groups.

关键词: Polycarbonate diol(PCDL), CH₃COONa, Two-step process

Abstract: Polycarbonate diols(PCDLs) with a number average molecular weight(M_n) of 2800 and a narrow polydispersity index(PDI=1.33) were synthesized from dimethyl carbonate(DMC) and 1,4-butanediol(BD) via a two-step process. The influences of the molar ratios of DMC to BD in the feedstock, polycondensation temperature and polycondensation time on the PCDLs preparation were studied. CH₃COONa showed the best catalytic performance among the catalysts studied. The highest BD conversion of 73.8% and PCDLs yield of 64.7% were achieved under its optimum reaction conditions. Furthermore, based on the results of ¹H NMR, the relationships between the ratio of end groups (-OCH₃/-OH) of oligomers, the M_n and chain-end constitute of resultant polycarbonates were also investigated. The results indicate that PCDLs can be synthesized when the oligomers mostly bear hydroxyl end groups. In contrast, it was impossible to prepare PCDLs when the oligomers were enriched with methyl carbonate end groups.

Key words: Polycarbonate diol(PCDL), CH₃COONa, Two-step process

SONG Menglu, YANG Xiangui, WANG Gongying. Synthesis of Polycarbonate Diols(PCDLs) via Two-step Process Using CH₃COONa as an Effective Catalyst[J]. 高等学校化学研究, 2018, 34(4): 578-583.

SONG Menglu, YANG Xiangui, WANG Gongying. Synthesis of Polycarbonate Diols(PCDLs) via Two-step Process Using CH₃COONa as an Effective Catalyst[J]. Chemical Research in Chinese Universities, 2018, 34(4): 578-583.

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Synthesis of Polycarbonate Diols(PCDLs) via Two-step Process Using CH₃COONa as an Effective Catalyst

Synthesis of Polycarbonate Diols(PCDLs) via Two-step Process Using CH₃COONa as an Effective Catalyst

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