干喷湿纺中聚丙烯腈初生纤维断裂行为研究

为了系统研究干喷湿纺中聚丙烯腈初生纤维的拉伸行为,利用SEM、纤维强伸度仪、XRD等手段,分析了凝固浴拉伸比、拉伸速率、微观结构和缺陷等对初生纤维断裂行为的影响。结果表明,干喷湿纺中,凝固浴拉伸比的提高有利于增加初生纤维的结晶度和断裂延伸率;同时发现,初生纤维内外部的缺陷以及拉伸的速率对初生纤维的断裂行为有重要影响。     

高性能碳纤维原丝与干喷湿纺

干喷湿纺兼备干法和湿法的优点,是新一代纺丝方法．此法在国外已用在工业生产线上,并纺出高性能PAN原丝和制得高质量碳纤维．此法还在完善和提高,普及已为期不远．     

聚丙烯腈原丝及其干喷湿纺

介绍了用于 PAN基碳纤维的聚丙烯腈原丝的发展历史 ,阐述了聚丙烯腈纺丝工艺中的主要工序和技术关键 ,指出了可以在聚合、纺丝过程中通过控制杂质及使用高相对分子质量的 PAN树脂纺制 PAN纤维等方法来提高原丝的性能。着重介绍了目前纺丝工艺中 PAN共聚体的制备、纺丝流体的流变行为及其凝固过程等重要工序的研究成果     

喷丝板对干喷湿纺法聚丙烯腈基碳纤维原丝的影响

从堵孔、表面腐蚀、喷丝孔腐蚀等喷丝板质量问题出发,分析了喷丝板对干喷湿纺法聚丙烯腈(PAN)基碳纤维原丝的单丝均一性、原丝及碳纤维的性能影响程度,为提高原丝、碳纤维质量提供一定的硬件设备理论基础。     

干-喷湿纺聚丙烯腈纤维拉伸工艺研究

研究了干 -喷湿纺聚丙烯腈 (PAN)初生纤维的喷丝头拉伸比和三级拉伸 (空气拉伸、DMF浴拉伸、热水和沸水拉伸、干热拉伸 )工艺中各拉伸比对纤维性能的影响。结果表明 :提高喷丝头拉伸比可明显地降低初生纤维的线密度 ,提高强度 ;三级拉伸工艺中各拉伸比的提高均有利于PAN纤维线密度的减小及其强度、声速取向度和抗张模量的提高 ;合理调配三级拉伸中各拉伸比可制得强度超过 7.0cN/dtex的PAN纤维     

干喷湿纺聚丙烯腈凝固丝的表征方法研究

以干喷湿纺聚丙烯腈(PAN)凝固丝为研究对象,通过优化试样处理方法和测试条件,建立了一套表征PAN凝固丝组成、形貌、结晶、取向及可拉伸性的方法。结果表明：采用擦拭法擦拭4次以上,PAN凝固丝的溶剂残留率保持稳定,萃取3 h以上可完全除去PAN凝固丝内的残留溶剂;在偏光显微镜和扫描电子显微镜下可分别观察PAN凝固丝的皮芯结构及截面的细微网状结构;PAN凝固丝的结晶度可直接使用X射线衍射仪分析计算,水洗温度对PAN凝固丝取向程度的测试结果影响较小;PAN凝固丝在空气中的自然拉伸比与在水浴中的最大拉伸倍数存在正相关性,自然拉伸比可作为衡量PAN凝固丝可拉伸性的参数。     

干喷湿纺聚丙烯腈原丝纺丝原液管道的设计

从聚丙烯腈原丝纺丝原液特性及干喷湿纺纺丝原液均一性要求出发,通过生产实践及理论分析,探讨了聚丙烯腈原丝纺丝原液管道在材质、管径、管道连接、保温、原液混合等方面的设计与改进。研究结果表明,干喷湿纺线实现了原液稳压、恒温和空气层高度可控性的输送,确保大批量的稳定化生产。     

湿纺凝固条件对PAN初生纤维形态结构的影响

分析了凝固浴温度、浓度、表观负拉伸等凝固条件对聚丙烯睛初生纤维形态结构的影响规律及作用机理,得出最佳的凝固工艺参数。结果表明:在其他凝固参数不变时,凝固浴温度、浓度及表观负拉伸均存在各自的临界值,低于或超过此临界值,初生纤维及原丝的性能均下降;采用凝固浴温度60℃、凝固浴质量分数为65％的最佳凝固工艺参数,可获得截面圆形且结构致密的初生纤维,并制得力学性能优异的原丝。     

干喷湿纺法制备T700级聚丙烯腈基碳纤维

采用丙烯腈、氨化试剂A、丙烯酸甲酯为聚合单体,以偶氮二异丁腈为引发剂,在溶剂二甲基亚砜中合成了聚丙烯腈原丝纺丝液,经干喷湿纺法纺丝制得聚丙烯腈原丝,经预氧化和炭化得到了T700级高性能聚丙烯腈基碳纤维。采用扫描电子显微镜,差示扫描量热仪,电子万能材料试验机对纤维的性能进行了研究。研究了空气层距离、喷丝头长径比、凝固浴浓度、空气拉伸比对干喷湿纺法制备纤维性能的影响。在空气层距离为40mm、凝固浴浓度为70%、喷丝头长径比为10.0、空气拉伸比为1.8条件下,采用干喷湿纺法制得的T700级聚丙烯腈基原丝及碳纤维的表面光滑、无沟槽,截面形貌为圆形;原丝的拉伸强度可达8.7cN/dtex,拉伸弹性模量可达154.7cN/dtex,碳纤维的拉伸强度可达5 750MPa,拉伸弹性模量可达220GPa。     

多元回归法分析干喷湿纺PAN/DMSO原液流变性能

应用多元回归分析确定了相对分子质量、温度、剪切速率、浓度4种主要因素对干喷湿纺聚丙烯 腈/二甲基亚砜(PAN/DMSO)纺丝原液粘度的影响。研究发现,纺丝原液粘度随着相对分子质量、浓度的增 大而增高,且过了临界相对分子质量、临界浓度后粘度会急剧增大。实验测得相对分子质量为7.8×104的 溶液临界浓度为11.5％。纺丝原液粘度随着温度、剪切速率的增大而降低,过了临界切变速率后粘度会急 剧下降,但在低剪切速率区粘度基本不变。通过多元线性回归模型,得出了多因子复合流变方程。     

聚丙烯腈纤维纺丝油剂对碳纤维性能的影响

研究了3种聚丙烯腈纤维油剂对原丝纺丝、预氧化和碳化过程的影响。结果表明:纺丝上油率与上油浓度成正比,二油工序纤维上油率受油剂浓度影响大;油剂对预氧化反应有阻碍作用,上油率越大,阻碍作用越大,但其可使预氧化过程易于控制;使用油剂可提高碳纤维的力学性能,与未上油原丝制得的碳纤维相比,上油率为1.0%时,3种油剂使碳纤维拉伸强度分别提高了8.81%、9.85%和11.74%。     

Fabrication of Regenerated Cellulose Fibers with Good Strength and Biocompatibility from Green Spinning Process of Ionic Liquid

In this study, 1-ethyl-3-methylimidazolium diethyl phosphate, having the advantages of regulating the performance of cellulose dissolution and degradation, simplicity in synthesis, is chosen as solvent to dissolve wood pulp cellulose for regenerated cellulose fibers (RCFs) manufacture using dry-jet wet spinning equipment. The effect of draw ratios on RCFs’ mechanical properties in three bathes, including coagulation bath, stretch bath, and washing bath is investigated and a series of RCFs with high strength are obtained. The morphology, crystallinity, thermal stability, and dyeing behavior of the prepared RCFs are analyzed and discussed. More importantly, the biocompatibility of the RCFs, which is first performed, demonstrated that the toxicity of RCFs is as low as the viscose fibers. These RCFs could be easily dyed by natural turmeric and antibacterial fibers are obtained finally. In conclusion, this work provides tools for achievement of RCFs with good strength and environmental friendliness by changing the draw ratios, and also further develops a new green process for fabricating RCFs based on ionic liquids.     

干湿纺中聚丙烯腈原丝凝固成形的探讨

介绍了聚丙烯腈（PAN）碳纤维原丝在以温度为主导的热致变和浓度为主导的双扩散致变下的成形过程,分析了凝固pH及牵伸率等对凝固成形的影响,并对干湿纺下淬火成膜,膜内液滴变化、细颈区拉伸等作出新的解释,从而对干湿纺下凝固成形的机理有一定的宏观把握,为纺出高品质的PAN原丝奠定理论基础.     

喷丝温度对PAN中空纤维成形与性能的影响

利用双弧狭缝孔形喷丝板,采用干喷湿法纺丝工艺,研究了PAN纺丝液在40～70℃喷丝温度范围内,对中空初生纤维成形与性能的影响。结果表明:喷丝温度对纤维截面的成形、外皮层厚度、异形度、中空度、声速取向等均会产生影响。随喷丝温度的增加,初生纤维外皮层厚度减小,纤维内外沿异形度逐渐降低且差距逐渐增加,中空度与声速取向在低温段降低幅度较大,而在高温段降幅减缓。     

Effect of DMSO/H2O coagulation bath on the structure and property of polyacrylonitrile fibers during wet‐spinning

The effect of coagulation bath condition on the structure and property of the nascent fibers and polyacrylonitrile fibers during wet‐spinning is studied. The best coagulation condition to produce polyacrylonitrile fibers has been found by examination of EA, XRD, SEM, and so on. The results indicated that when the coagulation bath was DMSO/H₂O system, the temperature was 60°C, the concentration was 65%, the minus stretch ratio was ?10%, fine crystallites and high degree of crystallization in the nascent fibers and polyacrylonitrile fibers could be achieved, and less solvents remained in the nascent fibers with circular cross section morphology. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

Study on the Coagulation Process of Polyacrylonitrile Nascent Fibers during Wet-spinning

Summary The coagulation process of polyacrylonitrile (PAN) precursor during wet-spinning was studied by chemical method based on the KMnO₄ titration. Experiments were performed with gelled solutions of PAN in dimethyl sulphoxide (DMSO) to determine the diffusion rate of solvent during the coagulation. The experimental datas about solvent diffusion coeffecient were calculated by using diffusion equation, which reflected the coagulation process of nascent fibers. At the same time, the effects of coagulation on the residual solvent content, the change of morphology of nascent fibers, the crystallization degree and the stress-strain curves were studied by use of X-ray diffraction, SEM, single fiber tensible test and so on. The results elucidated the relationship between coagulation process and the structure and property of PAN nascent fibers.     

聚丙烯腈基碳纤维生产工艺特性研究

以丙烯酸 (AA)为第二共聚单体与丙烯腈 (AN)进行溶液聚合 ,偶氮二异丁腈(AIBN)为引发剂 ,二甲基亚砜 (DMSO)作为溶剂合成聚丙烯腈 (PAN)原丝纺丝溶液。研究了单体浓度、引发剂的用量等对聚合反应的影响。探讨了聚丙烯腈原丝及其预氧丝、碳纤维制备的工艺过程 ,对纤维的结构和性能进行了 SEM和 TEM分析     

沸水再拉伸速率对聚丙烯腈纤维结构与性能的影响

以1-丁基-3-甲基咪唑氯盐([BMIM]Cl)为溶剂溶解聚丙烯腈(PAN)制成PAN纺丝原液,采用干喷湿法纺丝,经过凝固、预拉伸、沸水拉伸制得PAN纤维,对所得PAN纤维进行沸水再拉伸处理,研究了沸水再拉伸速率对PAN纤维结构和性能的影响。结果表明:PAN纤维中残留质量分数为4.38%的离子液体,为沸水再拉伸起到了增塑作用;随着沸水再拉伸速率的增大,PAN纤维的力学性能提高,断裂强度由2.69cN/dtex提高到4.33 cN/dtex,而断裂伸长率由26%减小到20%,纤维的玻璃化转变温度、晶区取向度、双折射率、结晶度、晶粒尺寸均增大。