4, 4-(9-芴)二苯酚型聚碳酸酯的合成及其耐高温性能研究

陈宇宏; 杜力鹏; 王凯; 詹茂盛

doi:10.11777/j.issn1000-3304.2016.16079

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4, 4-(9-芴)二苯酚型聚碳酸酯的合成及其耐高温性能研究

研究论文 | 更新时间：2021-03-19

- 4, 4-(9-芴)二苯酚型聚碳酸酯的合成及其耐高温性能研究
- Studies on Synthesis and Thermal Properties of Polycarbonate Derived from 9, 9-Bis(4-hydroxyphenyl) Fluorene
- 高分子学报 2016年第9期页码：1273-1280
- 作者机构：
  
  1. 北京航空材料研究院透明件研究所,北京,100095
  2. 北京航空航天大学材料科学与工程学院,北京,100191
- 作者简介：
- 基金信息：
  
  航空科学基金（基金号2013ZF21011）资助项目()
- DOI：10.11777/j.issn1000-3304.2016.16079
  中图分类号：
- 纸质出版日期：2016-9-1，
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陈宇宏, 杜力鹏, 王凯, 詹茂盛. 4, 4-(9-芴)二苯酚型聚碳酸酯的合成及其耐高温性能研究[J]. 高分子学报, 2016,(9):1273-1280.

Chen Yu-hong, Du Li-peng, Wang Kai, Zhan Mao-sheng. Studies on Synthesis and Thermal Properties of Polycarbonate Derived from 9, 9-Bis(4-hydroxyphenyl) Fluorene[J]. Acta Polymerica Sinica, 2016,(9):1273-1280.
陈宇宏, 杜力鹏, 王凯, 詹茂盛. 4, 4-(9-芴)二苯酚型聚碳酸酯的合成及其耐高温性能研究[J]. 高分子学报, 2016,(9):1273-1280. DOI： 10.11777/j.issn1000-3304.2016.16079.

Chen Yu-hong, Du Li-peng, Wang Kai, Zhan Mao-sheng. Studies on Synthesis and Thermal Properties of Polycarbonate Derived from 9, 9-Bis(4-hydroxyphenyl) Fluorene[J]. Acta Polymerica Sinica, 2016,(9):1273-1280. DOI： 10.11777/j.issn1000-3304.2016.16079.

摘要

以4，4-（9-芴）二苯酚（BHPF）和碳酸二苯酯（DPC）为原料，采用熔融酯交换法合成了4，4-（9-芴）二苯酚型聚碳酸酯（BHPF-PC）.红外光谱、核磁共振碳谱及氢谱测试结果证实了所得聚合物的化学结构.采用了四苯基膦苯酚盐（C30H25OP）等2种季磷盐以及3种碱性无机盐催化剂作为合成聚碳酸酯的催化剂，结果四苯基膦苯酚盐的催化效果最好.分析了DPC/BHPF初始摩尔比对BHPF-PC的影响规律，随着DPC/BHPF初始摩尔比的增加，BHPF-PC的分子量呈现先增加后降低的趋势.进一步研究了聚合工艺包括缩聚时间和缩聚温度对BHPF-PC的影响，结果表明BHPF-PC分子量达到最大值所需要的时间随DPC/BHPF初始摩尔比的增加而增加.初始摩尔比为1.1：1的DPC和BHPF，在1×10-5 mol/mol（BHPF）的四苯基膦苯酚盐催化作用下，于330℃缩聚150 min可以获得分子量最大的BHPF-PC.最后研究了BHPF-PC的耐高温性能和光学性能，其Tg达到了275℃，空气中失重率为5%时的分解温度T5%为440℃，同时透光率达到了88.1%，表明BHPF-PC是一种具有优异耐高温性能的高光学透明材料.

Abstract

Bisphenol-fluorene polycarbonate (BHPF-PC) was synthesized by melt transesterification of 9

9-bis(4-hydroxyphenyl) fluorene (BHPF) and disphenyl carbonate(DPC).The chemical structure of the polymer was confirmed by a combination of FTIR

1H-NMR and 13C-NMR spectra tests.The influences of catalyst species and contents

the initial DPC/BHPF molar ratios

polymerization time and temperature on the chemophysical properties of BHPF-PC were investigated.Two kinds of quaternary phosphonium salts including tetraphenylphosphonium phenolate (C30H25OP) and three kinds of inorganic salts were used as catalysts for the polymerization preparation of BHPF-PC

among which C30H25OP showed the highest catalytic activity.The impact of the initial DPC/BHPF molar ratios on the molecular weight of BHPF-PC was analyzed based on GPC measurements

and it was found that the molecular weight increased sharply when DPC was used in slight excess and then decreased with further increase of DPC/BHPF molar ratio.Furthermore

the effect of preparing conditions

such as polymerization time and temperature on the molecular weight variation of BHPF-PC was evaluated.The result indicated that the reaction time for obtaining maximum molecular weight increases with increasing initial molar ratio of DPC to BHPF.The BHPF-PC prepared by the condensation of DPC and BHPF with molar ratio of 1.1:1 in the presence of 1×10-5 mol/mol of C30H25OP

a residence time of 150 minutes at 330℃

showed a desirably high molecular weight.Finally

the thermal and optical properties of BHPF-PC were evaluated.BHPF-PC has a glass transition temperature of 275℃

an initial decomposition temperature of 440℃ (T5%)

and a light transmittance of 88.1%

indicating that BHPF-PC is an optical transparent material having excellent resistance to high temperature.

关键词

4 4-(9-芴)二苯酚聚碳酸酯熔融酯交换四苯基膦苯酚盐

Keywords

9 9-Bis(4-hydroxyphenyl) fluorenePolycarbonateMelt transesterificationTetraphenyl-phosphonium phenolate

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