碳纤维原丝中残留溶剂提取及测试技术研究

赵德明; 张顺; 丛佳玥; 王丹; 王陆; 李常清

doi:10.12338/j.issn.2096-9015.2021.0101

碳纤维原丝中残留溶剂提取及测试技术研究

doi: 10.12338/j.issn.2096-9015.2021.0101

1.
威海市产品质量标准计量检验研究院，威海 264200
2.
威海拓展纤维有限公司，威海 264211
3.
北京化工大学，北京 100029

基金项目: 威海市公益类科研机构基础研究经费（山东计量测试学会2020KJ27）

详细信息

作者简介:
赵德明（1982-），威海市产品质量标准计量检验研究院高级工程师，研究方向：产业计量、新材料计量、分析测试等，邮箱：80958128@qq.com

计量
- 文章访问数: 416
- HTML全文浏览量: 278
- PDF下载量: 36
- 被引次数: 0
出版历程
- 网络出版日期: 2021-08-18
- 刊出日期: 2021-12-01

Study on Techniques of Extraction and Testing of Residual Solvent in Carbon Fibers

1.
Weihai Academy of Product Quality Standard & Metrology Inspection, Weihai 264200, China
2.
Weihai TuoZhan Fibre Co. Ltd, Weihai 264211, China
3.
Beijing University of Chemical Technology, Beijing 100029, China

摘要

摘要: 聚丙烯腈(PAN)基碳纤维由于具有优异力学性能，广泛应用于航空航天、一般工业及高端体育用品等领域。高性能碳纤维制备技术关键之一在于原丝的高纯化、致密化，在原丝中残留溶剂二甲基亚砜（DMSO）提取、测试时，沸水会引起二甲基亚砜（DMSO）分解，严重影响纤维中残留溶剂的准确定量。国家碳纤维产业计量测试中心针对这一难题，探讨研究准确提取、定量原丝中残留溶剂二甲基亚砜（DMSO）系统方法，以水、乙醇、丙酮和环己烷为提取剂，研究提取剂种类、纤维质量、提取温度和时间、测试仪器方法对准确定量的影响。明确了各项提取条件和定量测试方法，为制备高性能纤维改进工艺控制提供计量测试服务保障。
- 产业计量 /
- 碳纤维原丝 /
- 残留溶剂 /
- 提取剂 /
- 定量
Abstract: Because of their excellent mechanical properties, polyacrylonitrile(PAN)-based carbon fibers are widely used in aerospace, general industry, high-end sports goods, etc. High purification and densification of carbon fiber precursors is one of the key techniques for the preparation of high-performance carbon fibers. During the extraction and testing of the residual solvent in carbon fiber precursors, boiling water causes the decomposition of the residual solvent in the dimethyl sulfoxide (DMSO), which seriously affects the accurate quantification of the residual solvent in the fibers. A systematic study of accurate extraction and quantification of residual solvent dimethyl sulfoxide (DMSO) in carbon fiber precursors was carried out at the National Measurement and Testing Center for Carbon Fiber Industry. Water, ethanol, acetone, and cyclohexane were used as extraction agents. The effects of extraction agent types, fiber quality, extraction temperature and time, and measuring instruments on the accurate quantification were studied. The extraction conditions and quantitative testing methods were proposed to provide measurement and testing services for improved process control of the preparation of high-performance fibers.
- industrial measurement /
- carbon fiber primordium /
- residual solvent /
- extracting agent /
- quantitative

HTML全文

图 1 二级质谱1.44/1.47 min

Figure 1. Secondary mass spectrometry was 1.44/1.47 min

下载: 全尺寸图片幻灯片

图 2 吸光度变化图

Figure 2. Changes in absorbance

下载: 全尺寸图片幻灯片

图 3 不同溶剂与PAN水洗纤维的接触角

Figure 3. Contact angle between different solvents and PAN washed fibers

下载: 全尺寸图片幻灯片

图 4 提取剂对PAN纤维残余溶剂提取量的影响

Figure 4. Effect of extractants on residual solvent extraction of PAN fibers

下载: 全尺寸图片幻灯片

图 5 纤维与提取剂固液比对PAN纤维残留溶剂提取量的影响

Figure 5. Solid-liquid ratio of fiber to extractant was significantly higher than that of residual solvent extraction amount of PAN fiber impact

下载: 全尺寸图片幻灯片

图 6 提取温度和时间对PAN纤维残留溶剂提取量的影响

Figure 6. Effect of extraction temperature and time on the amount of residual solvent extracted from the PAN fibers

下载: 全尺寸图片幻灯片

参考文献(18)

[1]	张健, 揣雪冰. 碳纤维的发展及其应用现状[J]. 化工管理, 2017(23): 60. doi: 10.3969/j.issn.1008-4800.2017.23.055
[2]	YOUE W J, LEE S M, LEE S S, et al. Characterization of carbon nanofiber mats produced from electrospun lignin-g-polyacrylonitrile copolymer[J]. International Journal of Biological Macromolecules, 2015(82): 497-504.
[3]	DARREN, A, BAKER, et al. Recent advances in low-cost carbon fiber manufacture from lignin[J]. Journal of Applied Polymer Science, 2013(130): 713-728.
[4]	罗益锋. 处于战略机遇期的全球碳纤维及其复合材料产业[J]. 高科技纤维与应用, 2019(2): 1-20. doi: 10.3969/j.issn.1007-9815.2019.02.001
[5]	顾佳杰. 碳纤维产业发展研究报告[J]. 上海化工, 2019(44): 32-36.
[6]	KAUR J, MILLINGTON K, SMITH S. Producing high-quality precursor polymer and fibers to achieve theoretical strength in carbon fibers: A revie[J]. Journal of Applied Polymer Science, 2016(133): 38.
[7]	赵晓莉, 齐暑华, 刘建军, 等. 干喷湿纺法制备T700级聚丙烯腈基碳纤维[J]. 工程塑料应用, 2019, 4(1): 67-71, 95. doi: 10.3969/j.issn.1001-3539.2019.01.012
[8]	陶磊, 黄元波, 郑云武, 等. 木质素制备低成本碳纤维的研究进展[J]. 高分子材料科学与工程, 2017(33): 179-185, 190.
[9]	WEI H, SUO X, LU C, et al. A comparison of coagulation and gelation on the structures and stabilization behaviors of polyacrylonitrile fibers[J]. Journal of Applied Polymer ence, 2020(137): 19.
[10]	S I Banduryan, M M Lovleca, G A Budnitskii. Formation of the Primary supramolecular structure of Some fiber types in conditions of wet spinning[J]. Fibre Chemistry, 2003, 35(5): 349-251. doi: 10.1023/B:FICH.0000012189.28557.db
[11]	M Murat Ozmen, Oguz Okay. Formation of macroporous poly(acrylamide) hydrogels in DMSO/water mixture: Transition from cryogelation to Phase separation copolymerization[J]. Reactive & Functional Polymers, 2008, 68(10): 1467-1475.
[12]	刘晗, 王晨晖, 谭晶, 等. 碳纤维缺陷演变及其原丝制备工艺研究进展[J]. 高科技纤维与应用, 2021, 46(1): 11-17. doi: 10.3969/j.issn.1007-9815.2021.01.001
[13]	李常清, 张顺, 陈栋, 等. 带型聚丙烯腈纤维制备及其预氧化反应特性研究[J]. 化工新型材料, 2019(47): 156-159.
[14]	支建海, 钱鑫, 张永刚, 等. 国产碳纤维增强树脂基复合材料的界面结合性能研究[J]. 合成纤维工业, 2018, 41(4): 14-17. doi: 10.3969/j.issn.1001-0041.2018.04.004
[15]	李颖华, 刘钟铃, 刘春明, 等. UV测试PAN原丝残余DMSO含量的影响因素研究[J]. 化工新型材料, 2016, 44(8): 178-180.
[16]	李常清, 徐樑华, 王晓玲, 等. 残余溶剂DMSO对PAN纤维结构及热性能的影响[J]. 高分子材料科学与工程, 2003, 19(4): 89-91. doi: 10.3321/j.issn:1000-7555.2003.04.023
[17]	张丽平, 李艳华, 陈秋飞, 等. 聚丙烯腈原丝中二甲基亚砜残留对碳纤维性能的影响[J]. 合成纤维, 2010(9): 13-15. doi: 10.3969/j.issn.1001-7054.2010.09.004
[18]	中国纺织工业联合会. 聚丙烯腈基碳纤维原丝残留溶剂测试方法: FZ/T 50032-2015[S]. 北京: 中国标准出版社, 2015.