四元共聚及氨化改性PAN原丝及其碳纤维研究  

A tetra-copolymerization and its ammoniating modification on PAN based precursors and carbon fibers

作　　者：李崇俊[1,2,3] 王华[1,2,3] 徐永花[1,2,3] 吴斌[1,2,3] 张勇[1,2,3] 许东[1,2,3] 

机构地区：[1]西安航天复合材料研究所 [2]西安康本材料有限公司,西安710089 [3]高性能碳纤维制造及应用国家地方联合工程研究中心,西安710089

出　　处：《高科技纤维与应用》2012年第3期11-19,36,共10页Hi-Tech Fiber and Application

摘　　要：在工程线上进行了四元共聚及四元氨化改性聚丙烯腈(PAN)原丝及其碳纤维研制。采用浊点测试法表征了含磺酸基第四单体纺丝液的亲水性,并确定了其共聚含量;通过动态机械分析(DMA)和差示扫描量热分析(DSC)分别测试了氨化前后原丝的玻璃化转变温度(Tg)和预氧化特性。采用质量膨润度、原丝碘吸附量、结晶取向度、原丝体密度等表征了氨化前后四元共聚原丝的结构致密性。结果表明,氨化改性较磺酸基第四单体可显著提高四元共聚纺丝液的亲水性;红外光谱证明第四单体共聚于PAN分子链中;氨化后PAN原丝Tg升高约2.6℃,达到111.28℃;氨化未改变预氧化的峰顶温度。质量膨润度及原丝体密度表明氨化提高了原丝的致密性,但结晶取向度和原丝拉伸模量下降。工程线上碳纤维生产结果表明,四元氨化改性碳纤维强度>3 500 MPa的合格率较四元共聚的提高12%,达到90%,同时钩接强力也由四元的76 N提高到87 N。A tetra-copolymer of polyacrylonitrile（PAN） precursor and carbon fibers,and its ammoniating modification,are made in engineering production line.The white turbidity point test is used to characterize the hydrophobicity of the dope with a sulfonic monomer,as well as to determine the concentration in the tetracopolymerization.The Infrared Spectrum is adopted to testify whether the fourth monomer is copolymerized in PAN structure.The Dynamic Mechanical Analysis（DMA） is used to test the glass transition temperature（Tg）,and Difference scanning Calorimeter（DSC） to thermal stabilization in the PAN precursors.The structural densification in PAN precursor is characterized by tests of swelling degree in weight,absorption of I（Iodine）,crystal orientation and density.The results show that ammoniating is more profound than the sulfonic monomer in improving the PAN dope hydrophobicity.The ammoniating precursor has an upgraded Tg by 2.6 ℃,up to 111.28 ℃,while nearly the same oxidation peak temperature as the tetra-copolymer.The ammoniating has improved the precursor densification from the points of swelling degree in weight and density;while lowering the crystal orientation and tension modulus.The statistical strength in engineering line shows that ratio of over 3 500 MPa is enlarged from 78.1% to 90.0%,meanwhile the knot force is improved from 76 N to 87 N.

关 键 词：聚丙烯腈原丝 四元共聚 氨化改性 碳纤维 性能 研究 

分 类 号：TQ342.31[化学工程—化纤工业] TQ342.742