Dimethyl sulfoxide (DMSO) solvent content in high performance polyacrylonitrile (PAN) carbon fiber precursor was an important index for product quality control.DMSO might be decomposed during extraction from PAN fiber in boiling water that would affect the accurate determination of residual DMSO content in PAN fiber.The thermal decomposition of DMSO at 100℃ was studied by LC-MS.It is found that dimethyl disulfide or dimethyl sulfone were produced,which indicated that boiling water was not suitable for extracting DMSO from PAN fiber.The UV absorption of DMSO in different organic solvents was studied by UV spectrophotometer.The UV sensitivity of DMSO in cyclohexane,acetone and ethanol decrease in turn,but they were more sensitive than water.PAN fiber was prepared by wet spinning process.The contact angle between different organic solvents and PAN fiber was studied by dynamic contact angle tester.The contact angle between solvent and PAN fiber was related to solvent polarity,and the contact angle of organic solvent with PAN fiber was smaller,which indicated that organic solvent was easier to infiltrate the fiber.The UV absorption sensitivity of DMSO in organic solvents and the wettability between organic solvents and PAN fibers were analyzed.The results shown that cyclohexane,acetone and ethanol were feasible as solvent extractants for DMSO residues in PAN fiber.
Cao Jinxi, Xu Lianghua, Zhao Deming, Wang Dan, Cong Jiayue, Li Changqing
. Feasibility study on organic extractant for residual solvent dimethyl sulfoxide in PAN fiber[J]. New Chemical Materials, 2021
, 49(12)
: 146
-149
.
DOI: 10.19817/j.cnki.issn 1006-3536.2021.12.030
[1] Banduryan S I,Lovleca M M,Budnitskii G A.Formation of the primary supramolecular structure of some fiber types in conditions of wet spinning[J].Fibre Chemistry,2003,35(5):349-251.
[2] Ozmen M M,Okay O.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.
[3] 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.
[4] 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.
[5] 上海市纺织工业技术监督所.FZ/T 50032—2015聚丙烯腈基碳纤维原丝残留溶剂测试方法[S].北京:中国标准出版社,2015.
[6] 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.
[7] Zeng X M,Ellinger J,Zhang Y W,et al.Determination of DMSO in PAN fibers by UV spectrophotometry[J].China Synthetic Fiber Industry China,2006,29(3):40-41.
[8] 刘建军,王成国,陈娟,等.高效液相色谱法测定聚丙烯腈基碳纤维原丝中的二甲基亚砜残留[J].色谱,2007,25(2):284-285.
[9] 范志先,贾淑敏,王树娟.化纤废水中二甲基亚砜和丙烯腈的高效液相色谱分析[J].中国环境监测,2010,28(6):45-48.
[10] 樊永惠,赵铁柱,杨彩宁,等.气相色谱法测定DIANP纯度标准物质中有机杂质[J].化学分析计量,2011,20(6):68-70.
[11] 连峰,刘栋,陈秋飞,等.DMSO稳定化及其分解副产物处理方法的探讨[J].高科技纤维与应用,2015,40(3):61-65.
[12] 李果.二甲基亚砜的稳定化及其汽液相平衡研究[D].北京:北京化工大学,2007.
