纺织学报 ›› 2019, Vol. 40 ›› Issue (12): 152-161.doi: 10.13475/j.fzxb.20190905410

所属专题： 高性能纤维制备及应用

• 纺织科技新见解学术沙龙专栏:碳纤维及其复合材料制备技术及应用 • 上一篇    下一篇

高性能聚丙烯腈基碳纤维制备技术几点思考

张泽1,2, 徐卫军1, 康宏亮2, 徐坚2, 刘瑞刚2,3()   

  1. 1.兰州交通大学 机电工程学院, 甘肃 兰州 730070
    2.中国科学院化学研究所 北京分子 科学国家研究中心, 北京 100190
    3.中国科学院大学, 北京 100049
  • 收稿日期:2019-09-23 修回日期:2019-10-08 出版日期:2019-12-15 发布日期:2019-12-18
  • 通讯作者: 刘瑞刚
  • 作者简介:张泽(1994—),男,硕士生。主要研究方向为高性能纤维结构与性能。
  • 基金资助:
    国家高技术研究发展计划(863)项目(2015AA03A204)

Thoughts on preparation technology of high performance polyacrylonitrile-based carbon fibers

ZHANG Ze1,2, XU Weijun1, KANG Hongliang2, XU Jian2, LIU Ruigang2,3()   

  1. 1. School of Mechanical Engineering, Lanzhou Jiaotong University, Lanzhou, Gansu 730070, China
    2. Beijing National Laboratory for Molecular Science, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190, China
    3. University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2019-09-23 Revised:2019-10-08 Online:2019-12-15 Published:2019-12-18
  • Contact: LIU Ruigang

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摘要：

针对中国高性能聚丙烯腈(PAN)基碳纤维产业技术发展现状和存在的问题,就其生产过程中的一些基础问题进行总结,提出了研究和产业发展建议。在PAN原丝纺丝溶液制备过程中,可通过聚合工艺和设备的协同,实现PAN连续溶液聚合,得到均匀的PAN纺丝溶液。在原丝制备过程中,可通过凝固参数控制,调控PAN纺丝溶液细流的相分离过程,减小相分离过程形成的微孔尺寸;在干燥致密化和干热牵伸过程中,调控温湿度和张力,可控制微孔融合和PAN分子结晶与取向,制备出高品质碳纤维原丝。在预氧化和炭化过程中,通过对温度场和应力场的调控,控制预氧化过程的皮芯结构和炭化过程中的乱层石墨结构,可实现对碳纤维性能调控。

关键词: 聚丙烯腈基碳纤维, 连续聚合, 相分离, 结构与性能, 微缺陷

Abstract:

Polyacrylonitrile (PAN)-based carbon fibers were developed rapidly in the past twenty years in China. Based on the current state of the development of PAN-based carbon fibers, basic problems in the production process of PAN-based carbon fibers were considered and summarized. In the preparation of PAN spinning solution, continuous polymerization of PAN was realized by the cooperation of polymerization process and equipment, by which homogeneous PAN spinning solution with stable properties can be prepared. In the preparation of PAN precursor fibers, the phase separation process of PAN spinning solution was controlled by coagulation parameters to reduce the size of micro-pores formed during phase separation. The drying and hot-drawing procedures, the temperature, humidity and tension were carefully controlled to optimize the micro-pores fusion, crystallization and orientation of PAN molecule to prepare high-quality PAN precursor. In the stabilization and carbonization procedures, the skin-core and turbostratic graphite structure were controlled by adjusting temperature and stress fields to control the structure and properties of the resultant PAN-based carbon fibers.

Key words: polyacrylonitrile-based carbon fiber, continuous polymerization, phase separation, structure and property, micro-void

中图分类号: 

  • TQ536.2

图1

商用沥青和PAN基碳纤维的强度和模量"

图2

PAN基碳纤维生产流程"

图3

PAN均聚物和共聚物在空气气氛中的DSC曲线"

图4

PAN的熔点与其含水量的关系"

图5

PAN的氧化反应"

图6

PAN纤维在270 ℃下热处理皮层厚度和含氧量与时间关系"

表1

PAN炭化过程中气体释放"

温度/℃ 现象 原因
220 释放HCN并与O2发生化学反应 梯形聚合物的生成和氧化
260 基本没有变化,纤维模量不变 无链断裂
300 释放大量的CO2和H2O,同时释放CO、HCN和一些腈类化合物;纤维模量不变 CO2来源于氧化聚合物的羰基,无交联反应发生
400 释放CO2、H2O、CO、HCN和NH3,少量C3烃类和腈类化合物释放;纤维模量增大 分子内脱水交联
500 H2释放增加,同时释放少量NH3和HCN;纤维模量增大 脱氢交联
600 H2释放量减少,释放HCN和痕量的N2 脱氢交联
700 释放N2、HCN和H2;纤维模量增大 脱氢和释放N2交联
800 大量N2和H2释放,同时释放HCN;纤维模量增大 释放N2交联
900 N2释放量达到峰值,同时释放一些H2和痕量的HCN;纤维模量增大 脱N2交联
1 000 N2释放量下降到800 ℃时的水平,同时释放痕量H2;纤维模量增大 脱N2交联

图7

PAN基碳纤维的拉伸强度和拉伸模量随炭化温度的变化关系"

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