可纺中间相沥青的研究进展

doi:10.16085/j.issn.1000-6613.2023-0302

摘要/Abstract

摘要：

随着我国航空航天和电子等行业的快速发展，高性能沥青基碳纤维因其高模量和高导热等优异性能而受到广泛关注。其中，中间相沥青的制备是高性能沥青基碳纤维制备的首要环节，但因沥青组成结构复杂、杂原子较多、合成的中间相沥青产品性能不均一等因素限制，我国纺丝级中间相沥青量产化仍未实现，严重制约了相关产业的发展。本文综述了中间相沥青的形成过程和性质，对比了煤、石油、萘三种沥青原料的组成和分子结构，阐述了原料沥青中复杂成分对中间相沥青形成过程的影响以及常见的预处理方法，并对预处理方法的优缺点进行了比较，分析了直接热缩聚法、溶剂分离法、加氢改性法、催化改性法、共碳法以及其他方法的制备过程及其优缺点，并对中间相沥青形成过程中的影响因素进行了归纳总结。最后展望了中间相沥青的发展前景，针对目前的瓶颈问题提出了建议。研究者应从沥青原料出发，探究原料分子结构和工艺条件对中间相沥青结构的影响规律并阐明其机理。

关键词: 中间相沥青, 沥青基碳纤维, 原料预处理, 制备方法

Abstract:

With the rapid development of China's aerospace and electronics industries, high-performance pitch-based carbon fibers have attracted more and more attention because of its excellent properties such as high modulus and excellent thermal conductivity. Among these steps, the preparation of mesophase asphalt is the first step in the preparation of high-performance pitch-based carbon fibers. However, due to the complex structure of pitch and more heteroatoms, the properties of mesophase pitch products are not uniform. These facts lead to the situation that the industrial-scale production of spinning grade mesophase pitch has not yet been achieved in China, and thus seriously restricts the development of related industries. In this paper, the formation process and properties of mesophase pitch were reviewed. The composition and molecular structure of coal, petroleum and naphthalene were compared. The effects of complex components in raw pitch on the formation process of mesophase pitch and the common pretreatment methods were described, and the advantages and disadvantages of pretreatment methods were compared. The preparation process, advantages and disadvantages of direct thermal polycondensation, solvent separation, hydrogenation modification, catalytic modification, co-carbon method and other methods were analyzed, and the influencing factors in the formation of mesophase pitch were summarized. Finally, the development prospect of mesophase pitch was prospected, and suggestions were proposed to the current bottleneck problems. Researchers should start from the source of pitch raw materials to explore the influencing rules of their molecular structure and process conditions on the structure of mesophase pitch, and illuminate the proposed mechanism.

Key words: mesophase pitch, pitch-base carbon fiber, raw material pretreatment, preparation methods

中图分类号:

TQ342.742

高海港, 安高军, 鲁长波, 李艳香, 张玉明, 李望良. 可纺中间相沥青的研究进展[J]. 化工进展, 2024, 43(2): 1001-1012.

GAO Haigang, AN Gaojun, LU Changbo, LI Yanxiang, ZHANG Yuming, LI Wangliang. Research progress on spinnable mesophase pitch[J]. Chemical Industry and Engineering Progress, 2024, 43(2): 1001-1012.

图/表 7

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纤维类型	牌号	单丝直径/μm	拉伸强度/GPa	拉伸模量/GPa	热导率/W·m^-1·K^-1	断裂伸长/%	密度/g·cm^-3
PAN	T300	7	3.53	230	10	1.5	1.76
PAN	M60J	5	3.82	588	151	0.7	1.93
PAN	T1100	5	7.0	324	32	2.2	1.8
煤基	K13D2U	—	3.7	935	800	0.4	2.2
煤基	YS-95A	7	3.53	920	600	0.3	2.19
油基	K-1100	10	3.1	965	1100	0.2	2.2

纤维类型	牌号	单丝直径/μm	拉伸强度/GPa	拉伸模量/GPa	热导率/W·m^-1·K^-1	断裂伸长/%	密度/g·cm^-3
PAN	T300	7	3.53	230	10	1.5	1.76
PAN	M60J	5	3.82	588	151	0.7	1.93
PAN	T1100	5	7.0	324	32	2.2	1.8
煤基	K13D2U	—	3.7	935	800	0.4	2.2
煤基	YS-95A	7	3.53	920	600	0.3	2.19
油基	K-1100	10	3.1	965	1100	0.2	2.2

光学组织结构	单元光学组织尺寸/μm
各向同性	无光学活性
细粒马赛克型	直径 < 1.5
中等粒度马赛克型	1.5 < 直径 < 5.0
粗粒马赛克型	5.0 < 直径 < 10.0
中等流线型	流线长度 < 30，宽度 < 5
粗流线型	30 < 流线长度 < 60， 5 <宽度 < 10
广域流线型	流线长度 < 1.5，宽度 > 10
广域型	宽度 > 60

光学组织结构	单元光学组织尺寸/μm
各向同性	无光学活性
细粒马赛克型	直径 < 1.5
中等粒度马赛克型	1.5 < 直径 < 5.0
粗粒马赛克型	5.0 < 直径 < 10.0
中等流线型	流线长度 < 30，宽度 < 5
粗流线型	30 < 流线长度 < 60， 5 <宽度 < 10
广域流线型	流线长度 < 1.5，宽度 > 10
广域型	宽度 > 60

方法名称	处理目标	优点	缺点	影响因素
加热过滤法	去除喹啉不溶物、不溶性杂质	净化效果好，溶剂可回收，工艺简单	滤网强度、孔径要求较高，且需经常更换，滤材孔径和助滤剂粒径需微米级，成本较大	原料性质，溶剂种类和比例，滤材孔径及助滤剂粒径，过滤温度及压力
溶剂萃取法	去除轻、重组分，获得理想组分	净化效果好，溶剂可回收，成本低	溶剂用量大，部分溶剂难以脱除，操作烦琐且效率低	溶剂种类，萃取温度，萃取时间
溶剂沉降法	去除重组分，获得理想组分	溶剂可回收，设备成本低，工艺简单	分离效率低，产品质量不稳定，固体颗粒粒径为微米级时不易分离脱除，但加入沉降助剂和絮凝剂会增加成本且后期处理困难	溶剂种类和比例，萃取温度和沉降时间，沉降剂的种类和用量
超临界萃取法	去除全组分杂质，获得理想组分	原料适应性高，分离效果优异，溶剂可回收	工艺复杂，设备多且要求高，能耗和成本相对较高	原料本身性质，溶剂的种类，操作温度和压力
离心分离法	去除喹啉不溶物、较小杂质	分离能力强，效率高	处理量小，分离精度低且高黏度细微颗粒难以脱除；设备要求高，能耗和成本相对高	原料密度，溶剂比例、种类及用量，滤布目数，萃取温度和时间，离心转速和时间