二甲基亚砜法碳纤维用聚丙烯腈原丝的技术进展

介绍了碳纤维用二甲基亚砜法（DMSO）生产聚丙烯腈（PAN）原丝的技术新进展,并对国内DMSO法PAN原丝技术提出几点建议。     

两种DMSO法PAN原丝性能和结构的对比研究

对国产DMSO法聚丙烯腈(PAN)原丝与美国DMSO法PAN原丝的性能和结构进行了对比,找出了国产PAN原丝和美国PAN原丝在质量均一性、断面形状、取向度和结晶度、相对分子质量、共聚组分等方面存在的差别,为进一步提高我国PAN原丝的内在质量提供了科学依据。研究结果表明:美国PAN原丝比国产PAN原丝有较高的强度、模量、相对分子质量、结晶度及取向度,较低的纤度、断后延伸率及各种不均率等优良性能。     

溶剂中金属离子对聚丙烯腈基碳纤维及其原丝的影响

金属离子的含量对碳纤维及其原丝的质量有很大的影响。分析了溶剂二甲基亚砜(DMSO)中金属离子含量对聚丙烯腈(PAN)原液聚合、原丝及碳纤维性能的影响。试验表明:DMSO中金属离子的存在,会在聚合源头处影响聚合反应,造成物料均一性、可纺性、可牵伸性下降,使原丝及碳纤维性能下降;而几种金属离子中,铁离子的干扰破坏性最大。     

DMSO残余溶剂对PAN原丝质量的影响

二甲基亚砜（DMSO）的溶剂残余含量是衡量PAN原丝产品性能的关键指标,是PAN原丝表面及内部形成缺陷的主要成因,其残余含量的高低直接影响PAN原丝成品的产量和质量.实验表明：采用浸洗加喷涌的水洗方式,通过提高水洗温度和循环喷涌量可以有效降低原丝中残余DMSO的含量,从而提高PAN原丝的产品质量.     

北京化工大学的DMSO法PAN原丝小试课题通过国家石化局组织的专家技术鉴定

2000年12月22日,国家石化局在北京化工大学召开了“九五”科技攻关课题“DMSO法PAN原丝的小试鉴定,专家们认为该课题组研制的湿纺1K PAN原丝,基本上达到了相当于国外T300型的原丝指标,纤度为0.9-1.3 dtex,拉伸强度为7cN/dtex以上,断裂伸长为15％,模量≥90cN/dtex,用该复丝烧出的PAN基碳纤维,拉伸强度为3.7-3.8GPa,断裂伸长为1.3％-1.4％,模量为260-270GPa,与T300的PAN基碳纤维相比,模量高得多,而断裂伸长偏低,该成果处于国内领先。专家们希望继续做好基础研究工作,摸索出符合T300型碳纤维要求的3K-12K PAN原丝的最佳工艺条件和性能指标,为我国DMSO法PAN原丝的产业化作出贡献。     

干湿法制备异形PAN原丝及其力学性能的研究

对二甲基亚砜(DMSO)干湿法制备三角形截面聚丙烯腈(PAN)基碳纤维原丝的截面形成因素进行了研究,并比较了不同条件下纤维的性能。结果表明:在干湿法纺制三角形截面PAN基碳纤维原丝过程中,凝固浴条件对PAN纤维的截面影响非常明显,同时凝固浴条件和拉伸条件对纤维的力学性能也有非常显著的影响。     

水洗方法对PAN原丝及其碳纤维结构与性能的影响

在聚丙烯腈(PAN)基碳纤维生产中,分别采用浸涌式水洗、拍打式水洗、超声式水洗3种方法对PAN原丝进行水洗,讨论了PAN原丝的线密度对水洗效果的影响,以及3种水洗方法对PAN原丝及其碳纤维的结构与性能的影响。结果表明:在水洗流量1 m3/h、水洗温度60℃、水洗时间1.2 min的条件下,随着PAN原丝线密度的增加,原丝中二甲基亚砜(DMSO)残留量增加,浸涌式水洗受原丝线密度的影响较大,超声式水洗受原丝线密度的影响较小;在PAN原丝线密度为4.0 dtex时,PAN原丝经浸涌式、拍打式、超声式水洗后,DMSO残留量分别为1 000,200,90μg/g,相应碳纤维强度分别为5 139,5 120,4 930 MPa;浸涌式水洗对PAN纤维的损伤较小,超声式水洗对PAN纤维的损伤较大。     

DMSO法PAN原丝湿法纺丝工艺研究

通过实验对二甲基亚砜（DMSO）法聚丙烯腈（PAN）原丝的纤维凝固成形、水洗、牵伸、干燥定型条等湿法纺丝工艺对纤维性能的影响进行了研究,实验结果表明：增大喷丝板孔径,有利于提高原丝的取向度和干燥收缩率;调节凝固浴质量分数和温度,可生产出综合性能较好的原丝;提高水洗温度有利于制得性能好的原丝;热水、沸水和蒸汽3级牵伸工艺...     

水洗条件对聚丙烯腈碳纤维及其原丝性能的影响

对二甲基亚砜法(DMSO)生产聚丙烯腈(PAN)碳纤维原丝的水洗温度、时间、方式等进行探讨,进而对水洗工艺进行优化和改善。实验结果表明,控制单束12k PAN原丝水洗水用量在400~500 L/h,水洗温度在45℃,水洗时间在30~40 min,通过在水洗槽中增加拍打辊及V型隔板,可以实现丝束内DMSO残留质量分数≤0.07%。     

成都拟建年产5000吨高性能碳纤维项目

四川省华拓实业发展股份有限公司在成都市双流县拟建PAN树脂合成、PAN原丝、预氧化、碳化、碳纤维处理等五个车间．二条PAN原丝,三条碳纤维（CARBONFIBER）的生产线,形成年产PAN原丝10000吨,碳纤维4000吨,石墨碳纤维1000吨的生产能力。投资总额12．0506亿元。     

碳纤维用聚丙烯腈原丝制备技术的研究进展

碳纤维的品质在很大程度上取决于原丝。制造品质优异的原丝的主要制约因素有聚合体中共聚单体类型、纺丝方法及工艺、拉伸工艺、干燥致密化程度、上油工艺及油剂类型。本文从以上几个方面总结了日本文献中制取高性能碳纤维原丝的几种关键技术。     

凝固浴对PAN原丝性能的影响

在生产聚丙烯腈(PAN)炭纤维过程中,纺丝期间凝固浴的各种条件对纤维的成型和性能起着关键作用。本文介绍PAN高聚物在湿法一步法纺丝过程中二甲基亚砜(DMSO)凝固浴各种成型工艺条件对PAN原丝的结构、机械和物理性能的影响。     

PAN基碳纤维原丝产品均质性研究

从纺丝生产工艺方面对聚丙烯腈(PAN)原丝产品均质化的影响因素进行了试验探讨。研究表明:优质的PAN原丝是碳纤维发展的基础,而均质化差的PAN原丝将导致原丝产品质量的性能缺陷及生产波动,极大的影响原丝的加工性能。     

聚丙烯腈原丝中二甲基亚砜残留对碳纤维性能的影响

通过对水洗条件的改变,考察了PAN原丝中溶剂二甲基亚砜残留量对碳纤维性能的影响。在原丝中溶剂残留量较高的情况下,碳纤维的密度和强度大幅下降,同时原丝的截面形状和表面形态遭到破坏,影响了碳纤维的性能。     

Processing,structure, and properties of gel spun PAN and PAN/CNT fibers and gel spun PAN based carbon fibers

Polyacrylonitrile (PAN) and PAN/carbon nanotube (PAN/CNT) fibers were manufactured through dry‐jet wet spinning and gel spinning. Fiber coagulation occurred in a solvent‐free or solvent/nonsolvent coagulation bath mixture with temperatures ranging from ?50 to 25°C. The effect of fiber processing conditions was studied to understand their effect on the as‐spun fiber cross‐sectional shape, as well as the as‐spun fiber morphology. Increased coagulation bath temperature and a higher concentration of solvent in the coagulation bath medium resulted in more circular fibers and smoother fiber surface. as‐spun fibers were then drawn to investigate the relationship between as‐spun fiber processing conditions and the drawn precursor fiber structure and mechanical properties. PAN precursor fiber tows were then stabilized and carbonized in a continuous process for the manufacture of PAN based carbon fibers. Carbon fibers with tensile strengths as high as 5.8 GPa and tensile modulus as high as 375 GPa were produced. The highest strength PAN based carbon fibers were manufactured from as‐spun fibers with an irregular cross‐sectional shape produced using a ?50°C methanol coagulation bath, and exhibited a 61% increase in carbon fiber tensile strength as compared to the carbon fibers manufactured with a circular cross‐section. POLYM. ENG. SCI., 55:2603–2614, 2015. © 2015 Society of Plastics Engineers     

Structure and properties of partially cyclized polyacrylonitrile‐based carbon fiber—precursor fiber prepared by melt‐spun with ionic liquid as the medium of processing

Carbon fiber has many excellent properties. Currently, the precursor fiber of polyacrylonitrile (PAN)‐based carbon fiber is made from solution by wet or dry spinning process that requires expensive solvents and costly solvent recovery. To solve this problem, we developed a melt‐spun process with ionic liquid as the medium of processing. The melt‐spun precursor fiber exhibited partially cyclized structure. The structure and properties of the melt‐spun PAN precursor fiber were analyzed by combination of scanning electron microscope, Fourier transform infrared spectroscopy, differential scanning calorimetry, X‐ray diffraction, thermogravimetry, ultraviolet spectroscopy, flotation technique, sound velocity orientation test, linear density, and tensile strength tests. The results showed that the tensile strength of melt‐spun PAN precursor fiber was fairly high reached up to 7.0 cN/dtex. The reason was the low imperfect morphology and a cyclized structure formed by in situ chemical reaction during melt‐spun process. Due to the existence of partially cyclized structure in the melt‐spun PAN precursor fiber, exothermic process was mitigated and the heat evolved decreased during thermal stabilization stage in comparison with commercial precursor fibers produced by solution‐spun, which could shorten the residence time of thermal stabilization and reduce the cost of final carbon fiber. POLYM. ENG. SCI., 55:2722–2728, 2015. © 2015 Society of Plastics Engineers     

PAN原丝沸水收缩率影响因素的探讨

采用溶液聚合和湿法纺丝制备碳纤维用聚丙烯腈(PAN)原丝,探讨了共聚组成、凝固浴温度、凝固浴浓度、拉伸介质和热定型温度对PAN纤维沸水收缩率的影响。结果表明,采用二元共聚物丙烯腈/甲叉丁二酸的质量比为99/1,凝固浴温度为30℃、凝固剂中二甲基亚砜质量分数为70%,热定型温度为160℃,拉伸介质为加压饱和蒸汽时,制备的PAN原丝沸水收缩率最低。     

高性能聚丙烯腈基碳纤维的原丝

聚丙烯腈（PAN）原丝质量已经成为制约我国碳纤维工业发展的重要因素之一。这已引起国内专家的高度重视,已到了非解决不可的地步。本文将从聚合和纺丝两方面,系统的阐述制取高性能碳纤维原丝的几个要素。