CN105603397B - 一种磁性金属长纤维管的制备方法 - Google Patents
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Abstract
一种磁性金属长纤维管的制备方法为:聚丙烯连续性纤维的表面处理:分别采用氢氧化钠溶液进行化学除油,铬酐和硫酸溶液表面粗化处理,酸性的锡盐溶液进行纤维的敏化,硝酸银和氨水溶液进行纤维表面的活化,甲醛溶液对纤维进行还原;纤维的化学镀铜,纤维的电镀(铁或镍),聚丙烯纤维的去除,纤维金属管的还原。本工艺可制备不同管径、不同截面形状的连续性磁性金属和层状复合磁性金属纤维管。
Description
技术领域
本发明涉及功能化金属纤维管制备的技术领域,尤其是涉及一种磁性金属长纤维管的制备方法。
背景技术
金属纤维与有机、无机纤维相比,具有高的弹性、高的耐磨性、好的通气性、导电性、导磁性、导热性以及自润滑性和烧结性,应用范围广阔,前景引人瞩目。目前主要应用于:导电塑料,高压带电作业服,微波防护服、汽车消声器,热交换器等。而具有中空结构的磁性金属纤维管在作为电磁波吸收剂使用时,可表现出更好的电磁波衰减效果和更低的密度。目前来看,磁性金属纤维管的生产方法主要有静电纺丝法(王美策等,一种基于单通道电纺丝法制备金属纳米纤维管的方法[P],中国发明专利,申请号:201310525512.5,2013-10-30),以及静电纺丝和金属气相沉淀技术相结合法(金翼水. 高功能性金属纳米纤维的制造及其性能评估. 国外化纤技术,2011,40(10),47-49.)。此类方法制备金属纤维管长度尺寸有限。
发明内容
本发明要解决的技术问题是提供一种磁性金属长纤维管的制备方法,首先,对长聚丙烯纤维表面处理(粗化、活化、敏化)、化学镀及电镀(铁或镍)制成连续性复合纤维、复合纤维经分解、裂解、燃烧,还原形成(铁或镍)磁性金属长纤维管。
本发明解决其技术问题所采用的技术方案,包括以下步骤:
(1)聚丙烯连续性纤维的表面处理:采用10~20%wt的氢氧化钠溶液进行化学除油,采用铬酐和硫酸溶液进行纤维表面的粗化,采用酸性的锡盐溶液进行纤维的敏化,敏化后纤维的清洗,采用硝酸银和氨水溶液进行纤维表面的活化,活化后的纤维经甲醛溶液还原;
(2)纤维的化学镀铜,其溶液成分为:酒石酸钾钠10~20g/L ,氢氧化钠2~5g/L,硫酸铜2~4g/L ,氯化镍,0.2~1g/L, 甲醛1~3g/L,化学镀时间为2-8min;
(3)纤维的电镀(铁或镍),电镀铁的溶液主盐组成为硫酸亚铁和氯化亚铁,以及硼酸、络合剂、稳定剂,溶液pH=1~2;电镀镍的溶液组成为硫酸镍、硼酸、氯化钠、络合剂,溶液pH=2~3;
(4)聚丙烯纤维的去除,复合纤维在400~500℃氧化性气氛下氧化1-3h;
(5)纤维金属管的还原,在还原性气氛的保护下,200~500℃保温0.2-1.5h,自然冷却至室温,获得磁性金属长纤维管。
本发明的优点是:
(1)选择不同直径或异形截面的聚丙烯纤维,可制备不同规铬和断面形状的磁性金属长纤维管;
(2)由于聚丙烯纤维的分解、裂解、燃烧的不彻底,管内留存了残炭,一方面为磁性金属氧化物还原成金属提供合适的还原剂,提高反应速度,另一方面,当磁性金属长纤维管作为电磁波吸收剂使用时,管内残炭的反射和吸收作用(Xie W, Cheng H F, Chu Z Y, et al. Effect of FSS on microwave absorbing properties of hollow-porous carbonfiber composites. Materials and Design, 2009, 30(4): 1201−1204.),将增强电磁波的衰减效果;
(3)可通过调整电镀主盐的组成及工艺,即可获得具有不同磁性金属成分的长纤维管。
具体实施方式:
以下结合实施例对本发明作进一步说明:
实施例1:φ0.012 mm纤维铁管的成形工艺
(1)聚丙烯连续性纤维直径为φ0.006 mm,先采用10%wt氢氧化钠溶液进行化学除油5min;粗化的水溶液配比为80g/L 铬酐、300ml/L 硫酸,粗化处理温度为60℃,粗化处理时间20min;敏化液组成为氯化锡8g/L,盐酸40ml/L ,敏化处理时间3min;采用硝酸银和氨水溶液进行纤维表面的活化,活化后的纤维经甲醛溶液还原;
(2)纤维的化学镀铜,其溶液成分为:酒石酸钾钠10 g/L ,氢氧化钠2.5g/L,硫酸铜2g/L ,氯化镍0.2g/L, 甲醛1.2 g/L,化学镀时间为3min;
(3)纤维镀铁,电镀液组成为硫酸亚铁100g/L,氯化亚铁200g/L,硼酸45g/L,络合剂微量,稳定剂微量,pH=1~2,电镀时间为15min;
(4)聚丙烯纤维的去除,复合纤维在450 ℃空气气氛下氧化1.5 h;
(5)纤维铁管的还原,在氢气气氛下,300℃保温0.5h,自然冷却至室温,获得φ 0.012 mm长纤维铁管。
实施例2:φ0.012 mm纤维镍管的成形工艺
(1)聚丙烯连续性纤维直径为φ0.006 mm,先采用10%wt氢氧化钠溶液进行化学除油5min;粗化的水溶液配比为80g/L 铬酐、300ml/L 硫酸,粗化处理温度为60℃,粗化处理时间20min;敏化液组成为氯化锡8g/L,盐酸40ml/L ,敏化处理时间3min;采用硝酸银和氨水溶液进行纤维表面的活化,活化后的纤维经甲醛溶液还原;
(2)纤维的化学镀铜,其溶液成分为:酒石酸钾钠10 g/L ,氢氧化钠2.5g/L,硫酸铜2g/L ,氯化镍0.2g/L, 甲醛1.2 g/L,化学镀时间为5min;
(3)纤维镀镍,电镀液组成为,硫酸镍220g/L,硼酸38g/L,氯化钠10g/L,络合剂微量,pH=2~3,电镀时间为20min;
(4)聚丙烯纤维的去除,复合纤维在450 ℃空气气氛下氧化1.5 h;
(5)长纤维镍管的还原,在氢气气氛下,300℃保温0.5h,自然冷却至室温,获得φ 0.012 mm长纤维镍管。
Claims (1)
1.一种磁性金属长纤维管的制备方法,其特征在于,制备步骤为:
(1)聚丙烯连续性纤维的表面处理:采用10~20%wt的氢氧化钠溶液进行化学除油,采用铬酐和硫酸溶液进行纤维表面的粗化,采用酸性的锡盐溶液进行纤维的敏化,敏化后纤维的清洗,采用硝酸银和氨水溶液进行纤维表面的活化,活化后的纤维经甲醛溶液还原;
(2)纤维的化学镀铜,其溶液成分为:酒石酸钾钠10~20g/L,氢氧化钠2~5g/L,硫酸铜2~4g/L,氯化镍,0.2-1g/L,甲醛1~3g/L,化学镀时间为2-8min;
(3)纤维的电镀:电镀铁的溶液主盐组成为硫酸亚铁和氯化亚铁,以及硼酸、络合剂、稳定剂,溶液pH=1-2;电镀镍的溶液组成为硫酸镍、硼酸、氯化钠、络合剂,溶液pH=2-3;
(4)聚丙烯纤维的去除,复合纤维在400~500℃氧化性气氛下氧化1-3h;
(5)纤维金属管的还原,在还原性气氛的保护下,200~500℃保温0.2-1.5h,自然冷却至室温,获得磁性金属长纤维管。
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CN101113568A (zh) * | 2007-08-07 | 2008-01-30 | 东华大学 | 一种黑色金属化电磁屏蔽织物及其制备方法 |
CN102701603A (zh) * | 2012-05-29 | 2012-10-03 | 中南大学 | 一种玻璃纤维表面铜/锌涂层的制备方法 |
CN102899890A (zh) * | 2012-10-31 | 2013-01-30 | 昆明理工大学 | 一种芳纶纤维表面金属化处理方法 |
CN103805972A (zh) * | 2014-01-17 | 2014-05-21 | 北京航空航天大学 | 一种采用模板法构筑超轻空心管微点阵金属材料及其制备方法 |
CN104975277A (zh) * | 2015-06-10 | 2015-10-14 | 上海大学 | 一种镀铜/镍铁磷合金双镀层织物的制备方法 |
CN105256291A (zh) * | 2015-06-10 | 2016-01-20 | 上海大学 | 一种芳纶镀镍/铜双镀层复合导电纤维的制备方法 |
CN104928914A (zh) * | 2015-06-26 | 2015-09-23 | 上海大学 | 一种芳纶镀镍/铜双镀层复合导电纤维的制备方法 |
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