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1,8-辛二酸改性热致液晶共聚酯的制备及其性能

吕荣盛 高欣逸 蒋杰 赵世成 赵玲 奚桢浩

吕荣盛, 高欣逸, 蒋杰, 赵世成, 赵玲, 奚桢浩. 1,8-辛二酸改性热致液晶共聚酯的制备及其性能[J]. 功能高分子学报. doi: 10.14133/j.cnki.1008-9357.20220613001
引用本文: 吕荣盛, 高欣逸, 蒋杰, 赵世成, 赵玲, 奚桢浩. 1,8-辛二酸改性热致液晶共聚酯的制备及其性能[J]. 功能高分子学报. doi: 10.14133/j.cnki.1008-9357.20220613001
LYU Rongsheng, GAO Xinyi, JIANG Jie, ZHAO Shicheng, ZHAO Ling, XI Zhenhao. Synthesis and Properties of Thermotropic Liquid Crystal Copolyesters Modified by 1,8-Suberic Acid[J]. Journal of Functional Polymers. doi: 10.14133/j.cnki.1008-9357.20220613001
Citation: LYU Rongsheng, GAO Xinyi, JIANG Jie, ZHAO Shicheng, ZHAO Ling, XI Zhenhao. Synthesis and Properties of Thermotropic Liquid Crystal Copolyesters Modified by 1,8-Suberic Acid[J]. Journal of Functional Polymers. doi: 10.14133/j.cnki.1008-9357.20220613001

1,8-辛二酸改性热致液晶共聚酯的制备及其性能

doi: 10.14133/j.cnki.1008-9357.20220613001
基金项目: 国家自然科学基金面上项目(21878256);上海市优秀学术/技术带头人计划资助(21XD1433000)
详细信息
    作者简介:

    吕荣盛(1996—),男,硕士研究生,主要研究方向为聚合反应工程。E-mail:13601464070@163.com

    通讯作者:

    奚桢浩, E-mail:zhhxi@ecust.edu.cn

  • 中图分类号: TQ322.3

Synthesis and Properties of Thermotropic Liquid Crystal Copolyesters Modified by 1,8-Suberic Acid

  • 摘要: 以对羟基苯甲酸、对苯二甲酸和对苯二酚为共聚单体,经乙酰化和熔融缩聚两步法合成三元热致液晶共聚酯。引入长链脂肪族化合物1,8-辛二酸作为改性单体,按不同比例代替对苯二甲酸,制备了一系列含柔性链段的新型四元热致液晶共聚酯。通过傅里叶红外光谱(FT-IR)和核磁共振碳谱(13C-NMR)对共聚酯结构进行表征,采用差示扫描量热(DSC)和热失重分析(TGA)表征其热性能,采用偏光显微镜(POM)和X射线衍射(XRD)分析其液晶性能。研究表明,三元液晶共聚酯熔点达407 ℃,热稳定性优异。随着1,8-辛二酸含量增加,四元共聚酯熔点显著降至214 ℃,热稳定性较好,最大热分解温度达到428 ℃。该系列共聚酯显示了典型的向列型液晶织态结构。1,8-辛二酸的引入显著改善了液晶共聚酯的可加工性。

     

  • 图  1  单体的化学结构

    Figure  1.  Structures of monomers

    图  2  HBA与HQ的乙酰化反应

    Figure  2.  Reaction equation for acetylation of HBA and HQ

    图  3  样品的红外光谱图

    Figure  3.  FT-IR spectra of samples

    图  4  S-0的(a)红外光谱和13C-NMR谱图

    Figure  4.  (a) FT-IR and (b) 13C-NMR spectra of S-0

    图  5  S-0的(a)DSC曲线和TGA曲线

    Figure  5.  (a) DSC curve and (b) TGA curve of S-0

    图  6  420 ℃下S-0的织态结构

    Figure  6.  Polarized optical micrograph of S-0 at 420 ℃

    图  7  (a) 单体与S-20的红外光谱图;(b) S-20与S-0的红外光谱对比图

    Figure  7.  (a) FT-IR spectra of monomers and S-20; (b) FT-IR spectra of S-20 and S-0

    图  8  HBA/PTA/SuA/HQ共聚酯DSC曲线

    Figure  8.  DSC curves of HBA/PTA/SuA/HQ copolyesters

    图  9  HBA/PTA/SuA/HQ共聚酯的TGA曲线

    Figure  9.  TGA curves of HBA/PTA/SuA/HQ copolyesters

    图  10  HBA/PTA/SuA/HQ 共聚酯的 XRD 曲线

    Figure  10.  XRD patterns of HBA/PTA/SuA/HQ copolyesters

    图  11  HBA/PTA/SuA/HQ共聚酯POM图

    Figure  11.  POM diagrams of HBA/PTA/SuA/HQ copolyesters

    表  1  HBA/PTA/SuA/HQ共聚酯的熔点、热失重温度及残碳量

    Table  1.   The melting points, decomposition temperature and char yield of HBA/PTA/SuA/HQ copolyesters

    SampleTm /℃ΔHm /(J·g−1)Td5% /℃Td50% /℃Tdmax /℃Char yield /%( 800 ℃)
    S-203782.88445.0558.954831.3
    S-403301.18439.7552.054431.9
    S-602711.24400.9499.545227.6
    S-802251.13390.9462.644422.1
    S-1002140.97379.8443.442815.5
    Tm: Melting point; ΔHm: melting enthalpy; Td5%: Temperature at 5% mass loss; Td50%: Temperature at 50% mass loss; Tdmax: Temperature at maximum mass loss
    下载: 导出CSV

    表  2  HBA/SuA/PTA/HQ 共聚酯的XRD数据

    Table  2.   X-ray diffraction data of HBA/SuA/PTA/HQ copolyesters

    Sample2θ/ (°)d /nmXc /%
    S-2019.90.4425.2
    28.30.32
    S-4019.80.4527.8
    28.20.32
    S-6020.40.4429.3
    28.40.32
    S-8020.50.4430.5
    28.70.31
    S-10020.40.4332.2
    28.50.31
    2θ: Diffraction peak; d: Crystal plane distance; Xc: Crystallinity
    下载: 导出CSV
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出版历程
  • 收稿日期:  2022-06-13
  • 录用日期:  2022-09-20
  • 网络出版日期:  2022-09-23

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