干湿法PAN纤维截面成形条件的研究

对干湿法纺丝中PAN纤维的截面形状影响因素进行了研究。研究发现,凝固浴浓度和温度是影响纤维截面的主要因素,随着凝固浴浓度的增大和温度的升高,纤维截面逐渐由扁平形变为圆形,纤维截面的异形度逐渐减小;干湿法比湿法纺丝更有利于得到圆形截面的纤维;随着空气层高度的增大,纤维截面的异形度减小,但当空气层高度超过10mm时,纤维截面形状不再变化;在一定条件下,喷丝头拉伸比对纤维的截面形状有一定影响,后拉伸过程和干燥对纤维截而形状基本上没影响。     

紫外分光光度法测定PAN纤维中的DMSO含量

用蒸馏水为萃取剂萃取出聚丙烯腈纤维中的DMSO,然后用紫外分光光度法测定其含量。测定的最佳线性浓度为:4．5× 10-10～1．6×10-9mol／L,DMSO最大吸收波长为208 nm, 检测限为1．9×10-9 mol/L,相关系数为0．999 8,相对标准偏差小于0．5％;与其它常用的测定方法相比,解决了从纤维中分离DMSO的难题,具有简便、快速、准确和低成本的特点。     

三角形PAN纤维湿法纺丝工艺研究

采用三角形喷丝板,以二甲基亚砜为溶剂,进行聚丙烯腈(PAN)湿法纺丝。探讨凝固成形条件及后拉伸对三角形PAN纤维截面形状、声速和力学性能的影响。结果表明:随着凝固浴浓度的升高,PAN初生纤维的异形度降低,声速和力学性能均先升高后降低;随着凝固浴温度的升高,PAN初生纤维的异形度增大,声速和力学性能均降低;随着喷丝头拉伸比的增加,PAN初生纤维的异形度增加,声速和力学性能也都呈上升趋势,随着后拉伸的进行,三角形PAN纤维的异形度基本保持不变,其力学性能和声速均逐渐升高。     

PAN/DMSO溶液的挤出对初生纤维结构的影响

应用扫描电子显微镜(SEM)和X射线衍射仪(XRD)研究了在一定的凝固条件下,挤出剪切速率(.γ)对聚丙烯腈(PAN)初生纤维聚集态及形态结构的影响规律。结果表明:随着.γ的增加,初生纤维的结晶度增大,晶粒尺寸减小;初生纤维的表面上产生了沿着轴向分布的沟槽,.γ越高,沟槽越深,初生纤维的截面结构变得不均匀,出现了一些大孔和皮芯结构;随着.γ的增加;初生纤维中的二甲基亚砜(DMSO)残留量增加。控制.γ在11 721~14 651 s-1,PAN/DMSO溶液流动性能好,可获得表面沟槽均匀、缺陷少、晶粒尺寸小且结晶度高的结构致密的PAN初生纤维。     

凝固条件对PAN初生纤维微结构的影响

通过湿法纺丝工艺制备聚丙烯腈(PAN)初生纤维,借助于X射线衍射仪、声速仪、扫描电子显微镜、小角X光散射仪等,研究了凝固浴温度、凝固浴浓度、喷丝头拉伸等凝固条件对初生纤维晶态结构、取向结构、形态结构的影响。结果表明:PAN纤维的凝聚态结构和形态结构在初生纤维形成时已基本形成;PAN初生纤维的结晶度达40%以上,其结晶度和结晶尺寸受凝固浴温度和浓度的影响;PAN初生纤维和原丝的晶区取向和全取向随着喷丝头拉伸的增大而增大;PAN初生纤维具有沿纤维轴向高度取向的沟槽,通过改变成形条件,可以获得沟槽浅且规整性完美的纤维表面;提高凝固浴浓度,可以形成结构均质、致密的PAN初生纤维,避免皮芯结构及芯部出现较多孔洞。     

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。     

凝固条件对PAN初生纤维微孔结构形态的影响

采用一维多取向小角X射线散射研究了聚丙烯腈细流在凝固过程中,凝固浴温度、浓度以及喷丝头拉伸比对初生纤维中微孔结构形态的影响。结果表明,凝固温度由30％提高到60℃时,微孔沿纤维轴取向增强,微孔尺寸减小,但微孔数量增加;凝固浴质量分数由67．5％升高到76．0％,微孔数量减少,但微孔尺寸变大,微孔沿纤维轴取向减弱;喷丝头拉伸比为-36．7％-10％时,微孔尺寸和取向角都增大。在凝固浴温度为52-55℃,凝固浴质量分数为70％,选择负拉伸能得到性能优异的初生纤维。     

纺丝速度对干湿法PAN纤维形貌和结构的影响

采用在线张力仪、光学显微镜、声速仪、紫外光谱、比表面积测定仪等手段研究了干湿法聚丙烯腈(PAN)纤维制备过程中纺丝速度对纤维形貌和结构的影响。结果表明随纺丝速度的提高凝固丝条上的张力线性增大,初生纤维的全取向程度也随之增大;凝固效果没有受到速度变化的影响,没有大的孔洞缺陷生成,纤维的力学性能没有受到影响。     

剥离型复合纤维截面形状对质量的影响

阐述了剥离型复合纤维截面形状变化对纤维质量的影响,以及生产过程中影响纤维截面形状变异的主要因素和控制办法。     

截面形状对聚酰胺6/石墨烯复合纤维性能的影响

通过母粒共混熔融纺丝法制备了圆形、三角形和十字形截面的聚酰胺6/石墨烯复合纤维。采用光学显微镜观察了纤维的截面形貌并计算其异形度,采用负离子测试仪、远红外发射率测试仪、恒温恒湿干燥箱表征了不同截面纤维的负离子释放性能、远红外辐射性能和纤维吸湿及其干燥速度。研究表明:圆形、三角形和十字形截面纤维的异形度分别达到6.31%、34.80%和58.29%。相对而言,异形度增大,会明显影响纤维的负离子释放浓度、吸湿速度及干燥速度,其中十字形截面纤维的负离子释放浓度最高达到1 820个/cm~3;另一方面,异形度的变化不会对纤维远红外辐射能力产生明显的影响,其远红外发射率在0.90～0.93,远红外辐射温升约为1.70℃。     

Investigating the jet stretch in the wet spinning of PAN fiber

The jet stretch of wet‐spun PAN fiber and its effects on the cross‐section shape and properties of fibers were investigated for the PAN‐DMSO‐H₂O system. Evidently, the spinning parameters, such as dope temperature, bath concentration, and bath temperature, influenced the jet stretch. Also, under uniform conditions, the postdrawing ratio changed as well as that of jet stretch. When coagulation temperature was 35°C simultaneously with bath concentration of 70%, jet stretch impacted obviously the cross‐section shapes of PAN fiber, but had little effect when the temperature was below 10°C or above 70°C. As the jet stretch ratio increased, the crystallinity, crystal size, sonic orientation, and mechanical properties of the as‐spun fiber changed rapidly to a major value for jet stretch ratio of 0.9 where the cross section of as‐spun fiber was circular. With further increasing of jet stretch ratio, the properties changed slightly but the fiber shape was not circular. The results indicated that appropriate jet stretch, under milder formation conditions in wet‐spinning, could result in the higher postdrawing ratio and circular profile of PAN fiber, which were helpful to produce round PAN precursor with minor titer and perfect properties for carbon fiber. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

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     

硫氢酸钠湿法腈纶增白工艺探讨

对硫氢酸钠湿法二步法腈纶进行增白,探讨了主要增白工艺条件对增白效果的影响。认为低线密度纤维增白效果较好。另外,生产中增白母液喷淋量控制在15～20m~3/h,浓度0.8％～1.5％,增白前纤维黄度控制小于8,增白剂用量小于0.5％,增白时间5s,所得纤维的增白效果明显。     

湿法腈纶质量控制的影响因素

浅析了影响腈纶生产质量稳定的控制因素,主要包括原液质量、纤维成形工艺等。正常生产中,控制聚丙烯腈(PAN)浆化液质量分数为26%,PAN溶液质量分数为13.5%,凝固浴硫氰酸钠质量分数为8%～12%,以及严格控制其他工艺条件,有利于生产稳定。     

二甲基亚砜法聚丙烯腈原丝干湿纺与湿纺成形工艺的比较

对二甲基亚砜(DMSO)法聚丙烯腈(PAN)原丝干湿纺和湿纺成形工艺进行比较,得出两种不同的成形工艺对PAN原丝表面光洁性和横截面形状的影响。实验表明:干湿纺成形纤维表面光洁,湿纺成形纤维表面凹凸有沟槽;不同的凝固浴浓度条件下,湿纺纤维横截面从圆形到非圆形再到圆形变化,干湿纺纤维横截面从圆形到非圆形变化。     

Investigation the jet stretch in PAN fiber dry‐jet wet spinning for PAN‐DMSO‐H2O system

The jet stretch of dry‐jet wet spun PAN fiber and its effects on the cross‐section shape of fibers were investigated for a PAN‐DMSO‐H₂O system. Clearly, the spinning parameters, such as dope temperature, bath concentration, bath temperature, and air gap, all influenced the jet stretch. Also, under uniform conditions, the postdrawing ratio as well as that of jet stretch changed. Under given conditions, as the bath temperature was below 30°C or above 45°C, jet stretch had little effect on the cross‐sectional shapes of PAN fiber. Within the temperature of 30–45°C, fiber's cross‐section shapes change obviously from round over an approximate circular shape into to an elliptical or a flat shape. The scope of jet stretch produced PAN fiber with circular cross‐section was bigger than that in wet spinning. These results indicated that appropriate air gap height, under milder formation conditions in dry‐jet wet spinning, could result in higher jet stretch and higher postdrawing ratio. The appropriate jet stretch and postdrawing ratio could result in circular profile of PAN fiber, which were helpful to produce round PAN precursor with finer size and better properties for carbon fiber. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

凝固浴氨化对PAN湿法纺丝凝固行为的影响

在二甲基亚砜/水(DMSO/H_2O)凝固体系中加入氨水,以pH值控制凝固浴氨化程度,研究了凝固浴氨化对聚丙烯腈(PAN)湿法纺丝凝固行为的影响;采用扫描电子显微镜表征PAN初生纤维的皮层结构,采用卡尔费休水分仪和气相色谱仪研究了氨化对水和DMSO扩散系数的影响。结果表明:当凝固浴pH值为8.0时,PAN初生纤维的皮层最薄;随着凝固浴pH值的增大,水的扩散系数逐渐减小,DMSO的扩散系数(D_(DMSO))先减小后增大,当pH值为8.0时,D_(DMSO)出现最小值;氨化的作用机理是通过氨与水和DMSO分子间的氢键作用来实现的。     

Investigating the spinnability in the dry‐jet wet spinning of PAN precursor fiber

The spinnability of a spinning solution using DMSO as the solvent was investigated for dry‐jet wet spinning of PAN precursor fiber. Among many variables responsible for spinnability, the coagulating conditions, the air gap length, the nonsolvent content in spinning solution, and the spinning temperature have been viewed as the key factors, and they were investigated in this study. It was found however, unlike in the wet spinning, the spinnability in dry‐jet wet spinning process was barely influenced by the coagulating conditions, likely attributable to the existence of the air gap. However, the spinnability worsened when the air gap was longer than 30 mm. The quality of the spinning solution deteriorated with the increasing water content in it. The spinnability improved when the spinning temperature was maintained between 60 and 72°C and turned down once the temperature was over 72°C. The experimental results indicated that all the factors should be comprehensively considered to ensure good spinnability in dry‐jet wet spinning process. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008