Chemical Research in Chinese Universities ›› 2018, Vol. 34 ›› Issue (4): 578-583.doi: 10.1007/s40242-018-7390-0

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

SONG Menglu1,2, YANG Xiangui1, WANG Gongying1   

  1. 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).

Abstract: Polycarbonate diols(PCDLs) with a number average molecular weight(Mn) 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 Mn 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