羟基氨基改性硅油阳离子乳液的合成及其在炭纤维原丝油剂中的应用

Synthesis of a hydroxylamino-modified silicone oil for use in a polyacrylonitrile oil emulsion in carbon fiber production

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。

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.