Synthesis of a hydroxylamino-modified silicone oil for use in a polyacrylonitrile oil emulsion in carbon fiber production
-
摘要: 为制备储存稳定、适合聚丙烯腈基（PAN）炭纤维原丝生产用油剂，利用三步法合成了一种具有自乳化特性的羟基氨基改性硅油（HA-PDMS），并与商业化的环氧改性硅油产品进行复配制备成炭纤维原丝油剂（P-OA）。在PAN生产线上，使用P-OA和日本竹本油剂（J-OA）分别生产上油的PAN原丝P-PAN和J-PAN；对P-PAN和J-PAN进行炭化处理制备相应炭纤维P-CF和J-CF。利用FT-IR和1H-NMR确认HA-PDMS结构；利用激光粒度分析仪、热重分析仪和表面张力仪对P-OA与J-OA进行特性分析；利用摩擦系数仪、毛羽量测试仪、纤维强力仪对上油后的原丝和炭化后的炭纤维进行测试表征和对比分析。结果表明，上油后的P-PAN单丝拉伸强度较J-PAN有所提高；炭化后P-CF较J-CF拉伸强度、拉伸模量均有提高，而毛羽量显著减小。
-
关键词:
- 羟基氨基改性硅油 /
- 聚丙烯腈基炭纤维原丝 /
- 油剂 /
- 炭纤维
Abstract: In order to prepare a stable oil emulsion suitable for polyacrylonitrile (PAN) in carbon fiber production, a hydroxylamino-modified silicone oil (HA-PDMS) was synthesized by a three-step procedure and mixed with a commercial epoxy-modified silicone oil in water to prepare an oil emulsion of PAN (P-OE) in carbon fiber preparation. The structure of the intermediate products and P-OE were analyzed by FT-IR and 1H-NMR. The major properties of P-OE were investigated by a laser particle size analyzer, thermogravimetric analyzer and surface tension instrument and compared with those of the commercial one used in Japan (J-OE). The polyacrylonitrile solution in dimethyl acetamide was drawn by wet spinning and impregnated in P-OE and J-OE to obtain P-PAN and J-PAN, respectively, which were carbonized to obtain carbon fibers P-CF and J-CF. The Roder friction coefficient, hairiness and tensile strength of P-PAN, J-PAN, P-CF and J-CF were tested to compare the performance of the two kinds of oil emulsions for use in PAN-based carbon fiber production. Results show that the tensile strength of P-PAN is higher than that of J-PAN. Compared with J-CF, the tensile strength and tensile modulus of P-CF are higher and the hairiness is greatly reduced. P-OE is superior to J-OE for the use as an oil emulsion of PAN in production of PAN-based carbon fibers. -
Frank E, Hermanutz F, Buchmeiser M R. Carbon Fibers:Precursors, manufacturing and properties[J]. Macromolecular Materials and Engineering, 2012, 297(6):493-501. Shirvanimoghaddam K, Salah U Hamin, Mohammad Karbalaei Akbari, et al. Carbon fiber reinforced metal matrix composites:Fabrication processes and properties[J]. Composites Part A:Applied Science and Manufacturing, 2017. 92:70-96. Yusof N, Ismail A F. Post spinning and pyrolysis processes of polyacrylonitrile (PAN)-based carbon fiber and activated carbon fiber:A review[J]. Journal of Analytical and Applied Pyrolysis, 2012. 93:1-13. Kaur J, K Millington, Smith S. Producing high-quality precursor polymer and fibers to achieve theoretical strength in carbon fibers:A review[J]. Journal of Applied Polymer Science, 2016. 133(38):43963. Wang Z Y, Li J H, Guo H J, et al. In situ synthesis of nano-sized silica enforced anionic polyester sizing agent and its effect on ILSS of carbon fiber composites[J]. Chemical Journal of Chinese Universities, 2019, 40(09):2005-2011. Hou Y P, Sun T Q, Wang H J, et al. Influence of ozone on chemical reactions during the stabilization of polyacrylonitrile as a carbon fiber precursor[J]. Journal of Applied Polymer Science, 2008. 108(6):3990-3996. Jia Y T, Ming L, Li J Z, et al. The research of the PAN based carbon fiber precursor finishing qualities[J]. Hi-Tech Fiber and Application, 2014, 39(01):52-55. Guan Y. Research development and application of oil agent used for PAN carbon fiber and/or its precursor[J]. New Chemical Materials, 2012, 40(06):1-4. 孙秀花. 碳纤维原丝用油剂主要成分分析及应用研究[D]. 2019, 长春工业大学. (Sun X H. Analysizing and application of oiling agent to polyacylonitrile(PAN)-based carbon fiber precursor[D]. 2019, Changchun University of Technology.) Zhao Y, Cui Q Q, Li G T, et al. Preparation and characterization of three-terminal epoxy-modified silicone oil[J]. New Chemical Materials, 2015, 43(12):140-142. Jia HF, Feng X, Li JH, et al. Preparation and characterization of terminal hydrogen silicone oil[C]. New Materials and Intelligent Manufacturing, 2018:173-175. 强杉杉. 高性能碳纤维专用油剂及上油工艺的研究[D]. 2008, 东华大学. (Qiang S S. Study on oil and oil finish for high performance carbon fiber[D]. 2008, Donghua University.) Zhang H L, Rao Q H, Li Y, et al. Preparation of epoxy-modified hydro-polysiloxane[J]. Thermosetting Resin, 2016, 31(03):30-34. Ran E Y, Zhang B C, Zhou R B, et al. Synthesis and properties of amino polyether modified silicone oil[J]. Chemical Industry and Engineering Progress, 2014, 33(02):445-452. Li JH, Jia HF, Feng X, et al., Preparation and characterization of side chain epoxy modified silicone oil for precursor fiber of carbon fiber[C]. New Materials and Intelligent Manufacturing, 2018:149-151. Somasundaran P, S C Mehta, P Purohit. Silicone emulsions[J]. Adv Colloid Interface Sci, 2006. 128-130:103-109. Hironobu Kunieda, Md Hemayet Uddin, Makiko Horii, et al. Effect of Hydrophilic- and Hydrophobic-Chain Lengths on the Phase Behavior of A? B-type Silicone Surfactants in Water[J]. The Journal of Physical Chemistry B, 2001. 105(23):5419-5426. Mehta S C, P Somasundaran. Mechanism of stabilization of silicone oil-water emulsions using hybrid siloxane polymers[J]. Langmuir, 2008. 24(9):4558-4563. Rui Li, Cheng Zhou, Yang Chen, et al. Preparation, characterization, and properties of organic silicone intermediate-modified epoxy resin copolymers[J]. High Performance Polymers, 2016. 29(1):36-45. Rashmi David, Raja V S, Singh S K, et al. Development of anti-corrosive paint with improved toughness using carboxyl terminated modified epoxy resin[J]. Progress in Organic Coatings, 2018. 120:58-70. He F. High performance carbon fiber precursor and oil agent[J]. Hi-Tech Fiber and Application, 2004, (05):1-5+10. Zhang L Z, Lv C X, Lv Y G, et al. The structure and thermal performance of PAN fibers during oxidative stabilization[J]. New Carbon Materials, 2005, (02):144-150. 单宏宇. 仿生非光滑耦合模具表面粘附性能研究[D]. 2009, 吉林大学. (Shan H Y. Study on adhesion property of moulds with biomimetic coupling non-smooth surface[D]. 2009, Jilin University.) Wang J F, Ma X L, Jiang Y L. Effects of polyacrylonitrile fiber spinning oil on properties of carbon fibers[J]. Synthetic Fiber in China, 2017, 46(08):34-37. -
下载:
点击查看大图
图(1)
计量
- 文章访问数: 775
- HTML全文浏览量: 389
- PDF下载量: 181
- 被引次数: 0
