CN113605087B - 一种镍金属牢固附着芳香族特种纤维长丝的连续生产工艺 - Google Patents
一种镍金属牢固附着芳香族特种纤维长丝的连续生产工艺 Download PDFInfo
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Abstract
本发明公开了一种使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺,本发明是一种连续24小时生产如芳纶、PBO纤维、聚酰亚胺纤维等芳香族特种纤维镀镍的方法,它首先解决了高强度纤维金属化不能走出实验室,不能生产稳定的参数一致长纤维丝一次生产几千米以上的问题;同时由于生产速度以及各种化学电镀的参数可控性,解决了纤维丝相同长度,要求的导电性能不同以及镀层厚度不同的难题;在解决了量产化问题的同时又兼顾了生产出的芳纶,PBO纤,聚酰亚胺纤维镀镍金属镀层的耐摩擦、耐老化技术难题。
Description
技术领域
本发明属于特种纤维金属化技术领域,尤其是一种使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺。
背景技术
芳香族纤维通常是指在主链上含有芳环的一系列纤维的统称。芳香族纤维主要包括芳香族聚酰胺纤维、芳香族聚酯纤维以及芳香族杂环类纤维等。由于这些纤维大多是刚性链结构,所以具有较高的强度、模量和较好的耐热性能,在军事、航天、航空、阻燃、防火和民用等方面都发挥着重要作用。例如,芳纶1414有极高的强度,是优质钢材的5-6倍,模量是钢材或玻璃纤维的2-3倍,韧性是钢材的2-3倍,而密度不到钢材的1/5,它的连续使用范围极宽,在-196℃到204℃范围内可以长期正常运行,在150℃下的收缩率为0,在560℃的高温下不融化不分解,具有良好的抗腐蚀性,生命周期很长。PBO纤维作为21世纪超性能纤维,具有十分优异的物理机械性能和化学性能,其强力、模量为芳纶1414纤维的2倍并兼有间位芳纶耐热阻燃的性能,而且物理化学性能完全超过迄今在高性能纤维领域处于领先地位的芳纶1414纤维。一根直径为1毫米的PBO细丝可吊起450千克的重量,其强度是钢丝纤维的10倍以上。耐热温度达到600℃,极限氧指数68,在火焰中不燃烧、不收缩,耐热性和难燃性高于其它任何一种有机纤维。聚酰亚胺纤维是醚类均聚纤维强度4~5cN/dtex,伸长率5%~7%,模量10~12GPA在300℃经100h后强度保持率为50%~70%,极限氧指数44,耐射线好;酮类共聚纤维具有近似中空的异形断面,强度3.8cN/dtex,伸长率32%,模量35cN/dtex,密度1.41g/cm,沸水和250℃收缩率各小于0.5%和1%。现有的纤维金属化的各种专利技术方法,都存在很多问题,无法应用到实际量产化阶段,技术条件参数模糊,镀层结合力极差,纤维强度破坏严重或者产出金属化纤维参数无法定制管控等等。例如:中国专利CN106498715A,使用丙酮溶液清洗,10-60min,利用混合有机极性溶剂溶胀1-4小时,硝酸银溶液浸渍1-2小时,然后还原0.5-1小时,制备过程中使用丙酮,易燃易爆,易挥发,会对人的中枢神经系统造成麻醉作用,长期接触会引起皮炎,整个制备时间太长,而且利用银镜反应制备的镀银芳纶,完全没有附着力,不具备实际产出能力;中国专利CN105133301A、CN104894846A、CN104894539A等在上述CN106498715A处理的基础上进行化学镀镍依然解决不了镀层附着力的问题,同时时间太长无法做到连续量产化。中国专利CN101705614B使用二甲基亚砜与氢化钠混合物进行粗化,这两种物质混合极易引发燃烧或爆炸,尤其是在制备镀银芳纶过程中会遇到水,危险性非常高,稍有不慎就会引发火灾爆炸等危险性事故,而且这种粗化方式会极大的破坏芳纶纤维的强度。中国专利CN101705615B使用20%的硫酸进行粗化,完全无法对芳纶纤维造成任何的表面处理,形成不了微孔或裂纹,从而无法达到金属与纤维基材的结合,而且进行的每一步都要停顿较长时间,无法做到连续性生产,而且后续的化学镍与化学铜的上镀在光滑的纤维表面形成不了牢固的复合层,无法达到实际应用要求。天诺光电专利CN103668944B,制备的镀银芳纶纤维的电阻率≤105Ω×cm,电阻率太大无法在实际应用中起到应有的作用。中国专利CN104532553A此种方法制备的镀银芳纶,结合力依然是达不到实际应用要求,且制备时间超过3小时,无法连续生产,形成产量。本领域技术人员亟待开发出一种使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺,满足现有的性能要求和市场需求。
发明内容
针对上述问题,本发明旨在提供一种使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺。
具体生产工艺步骤如下,芳香族纤维包括芳纶1414、PBO纤维、聚酰亚胺纤维中的其中一种所有过程均在自动线上按设定好的子槽长度,设定速度,以及固定参数下进行,纤维经过流程如下:1、碱性清洗:将芳香族特种纤维通质量分数3%-10%过氢氧化钠溶液,附加超声波振荡(时间2分钟,温度40-60℃);2、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;3、粗化:60%-80%的浓硫酸,加40g/L的WN-LL213膨胀剂,(温度30-40℃,时间30秒钟,辅以机械振动,振幅3.5cm,振动频率为30次/min)以达到纤维在不断裂的前提下,每一根纤维丝形成纵向微裂纹;4、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;纤维经过三次溢流冲洗,以保证再进入下一道工序时没有前一道工序的药液残留;5、表面调节:100g/LWN-Pd2020表面调节剂,温度30℃,时间2分钟,辅以超声波,对纤维进行微观的改性;6、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;7、预活化:10-30mL/L盐酸,温度30℃,时间1分钟;8、预钯:30-50ppm胶体钯溶液CoppermerseCatalystAF,氯化亚锡12g/L,盐酸250-300mL/L,温度35℃,时间5分钟,分段超声波,使纤维束中所有纤维均匀的附着上胶体钯;
胶体钯活化,活化稳定、效果较好,提高结合强度,经过活化处理后,使孔壁上形成一个由锡保护的单层或有限多层的钯胶团,后经清洗,除去锡保护层和多余的钯,仅留下单层,或有限多层的钯,并以此作为催化剂,促进了镀层与孔壁表面的紧密结合。
纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;10、解胶:15%硫酸溶液,温度60℃,时间1分钟,附加超声波振荡;11、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;12、化学铜:温度55℃、时间8分钟,附加间断式超声波振荡,防止纤维粘连,形成良好铜镀层;13、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;14、电镀镍:硫酸镍20-35g/L、氯化镍4-5g/L、硼酸35-45g/L、WN-NickelLS湿润剂5-1mL/L,(pH值3.5~4.5,温度55~60℃,电流密度0.3~2A/dm2),时间5分钟;为防止纤维粘连,同时在子槽内,纤维下方开孔,打气,用气流冲散纤维。导电接触以水加铜导电柱进行导电,此种导电方式能够防止纤维在导电过程中由于局部电流过高从而烧断纤维;15、纯水三次溢流洗涤超纯水清洗3次,共1分钟,附加超声波振荡;16、热水洗:70℃热纯水清洗,清洗时间1分钟;17、吹干:冷风去水,吹干纤维中的水分,时间1分钟;18、烘干:120℃烘箱,4分钟;19、收集成品。
进一步的,所述步骤12化学铜Cu2.5~3g/L、WN-ELCopper99开缸剂150mL/L、NaOH4.5g/L甲醛4g/L、WN-ELCopper99稳定剂15ppm、WN-ELCopper99添加剂1mL/L。
进一步的,上述所有步骤涉及的超声波振荡频率为20~24kHz。
进一步的,所述步骤14镍电镀液含硫酸镍20-35g/L、氯化镍4-5g/L、硼酸35-45g/L、WN-NickelLS湿润剂0.5-1mL/L。
进一步的,所述纯水三次溢流洗涤为超纯水清洗3次,共1分钟,附加超声波振荡。
本发明的有益效果:
本发明公开的工艺方法和参数,其中纤维经过三次溢流冲洗,以保证再进入下一道工序时没有前一道工序的药液残留;导电接触以水加铜导电柱进行导电,此种导电方式能够防止纤维在导电过程中由于局部电流过高从而烧断纤维,采用浓硫酸+膨胀剂的方式进行粗化,形成纵向微裂纹,在保证金属附着力的同时最大程度的保持了纤维的原有强度,力学性能损失少,在间断式超声波作用下进行表面处理,纤维表面能够被完全均匀地活化,化学镀铜 层能很好地沉积在纤维表面,镀层平整致密均匀,结合紧密,工艺控制合理,镀镍过程采用的是电镀镍工艺,通过电流密度以及时间的改变可以改变最终纤维的导电性以及纤维的重量实现纤维重量以及电阻率的精准控制,该过程是是连续镀镍工艺,可以实现工业化的连续生产,得到的镍金属牢固附着的芳纶纤维不仅保留了原有材料的强度和质轻、耐火等特性,同时又具有密度小,导电性和柔韧性好,并具有良好的耐热性和耐化学腐蚀性等优点,可以替代传统的铜丝、不锈钢丝、铝丝等作为新的材料应用在航空航天、医疗军工以及特种领域,同时也可以应用于智能化穿戴,医疗等领域。
本发明相对现有技术具有如下优点:
本发明是一种连续24小时生产如芳纶、PBO纤维、聚酰亚胺纤维等芳香族特种纤维镀镍的方法,它首先解决了高强度纤维金属化不能走出实验室,不能生产稳定的参数一致长纤维丝一次生产几千米以上的问题;同时由于生产速度以及各种化学电镀的参数可控性,解决了纤维丝相同长度,要求的导电性能不同以及镀层厚度不同的难题;在解决了量产化问题的同时又兼顾了生产出的芳纶,PBO纤,聚酰亚胺纤维镀镍金属镀层的耐摩擦、耐老化技术难题。
附图说明
下面结合附图对本发明行详细说明,附图1为镍金属牢固附着芳香族特种纤维长丝的连续生产工艺流水线操作图;附图2为以实施例1未处理前处理完成后的纤维原始表面形貌,附图3为以实施例1为基础的粗化处理完成后的纤维表面形貌。
具体实施方式
下面用具体实施例说明本发明,但并不是对本发明的限制。
实施例1
具体生产工艺步骤如下,芳香族纤维为芳纶1414 500d纤维,所有过程均在自动线上按设定好的子槽长度,设定速度,以及固定参数下进行,纤维经过流程如下:1、碱性清洗:将芳纶1414 500d纤维通过质量分数10%氢氧化钠溶液,附加超声波振荡(时间2分钟,温度60℃);2、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;3、粗化:80%的浓硫酸,加40g/L的WN-LL213膨胀剂(温度40℃,时间30秒钟),辅以机械振动,振幅3.5cm,振动频率为200次/min,以达到纤维在不断裂的前提下,每一根纤维丝形成纵向微裂纹;4、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;5、表面调节:100g/LWN-Pd2020表面调节剂(温度30℃,时间2分钟),辅以超声波,对纤维进行微观的改性;6、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;7、预活化:10mL/L盐酸,温度30℃,时间1分钟;8、预钯:30-50ppm胶体钯溶液CoppermerseCatalystAF,氯化亚锡12g/L,盐酸300mL/L,温度35℃,时间5分钟分段超声波,使纤维束中所有纤维均匀的附着上胶体钯;纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;10、解胶:15%硫酸溶液,温度60℃,时间1分钟,附加超声波振荡;11、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;12、化学铜:Cu2.5g/L、WN-ELCopper99开缸剂150mL/L、NaOH4.5g/L甲醛4g/L、WN-ELCopper99稳定剂15ppm、WN-ELCopper99添加剂1mL/L,(温度55℃、时间8分钟),附加间断式超声波振荡,防止纤维粘连,形成良好铜镀层;13、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;14、14、电镀镍:硫酸镍20g/L、氯化镍4g/L、硼酸35g/L、WN-NickelLS湿润剂0.5mL/L,(pH值3.5,温度55℃,电流密度0.3A/dm2,时间5分钟);铜导电柱进行导电;15、纯水三次溢流洗涤超纯水清洗3次,共1分钟,附加超声波振荡;16、热水洗:70℃热纯水清洗,清洗时间1分钟;17、吹干:冷风去水,吹干纤维中的水分,时间1分钟;18、烘干:120℃烘箱,4分钟;19、收集成品,上述所有步骤涉及的超声波振荡频率均为20kHz。芳纶1414500D烟台泰和新材料股份有限公司。
产品性能结果:500d芳纶1414镀镍纤维,断裂强度≥70N,延长率≥14%,电阻阻值≤3Ω/m,耐摩擦测试阻值变化率≤10%,反复弯曲试验阻值变化率小于1%。
实施例2
具体生产工艺步骤如下,芳香族纤维为PBO400d纤维,所有过程均在自动线上按设定好的子槽长度,设定速度,以及固定参数下进行,纤维经过流程如下:1、碱性清洗:将芳香族特种纤维通过质量分数3%氢氧化钠溶液,附加超声波振荡(时间2分钟,温度40℃);2、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;3、粗化:60%的浓硫酸,加40g/L的WN-LL213膨胀剂,温度40℃,时间30秒钟,辅以机械振动,振幅3.5cm,振动频率为30次/min,以达到纤维在不断裂的前提下,每一根纤维丝形成纵向微裂纹;4、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;5、表面调节:100g/LWN-Pd2020表面调节剂(温度30℃,时间2分钟)辅以超声波,对纤维进行微观的改性;6、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;7、预活化:30mL/L盐酸(温度30℃,时间1分钟);8、预钯:50ppm胶体钯溶液CoppermerseCatalystAF,氯化亚锡12g/L,盐酸250mL/L,温度35℃,时间5分钟,分段超声波,使纤维束中所有纤维均匀的附着上胶体钯;纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;10、解胶:15%硫酸溶液,温度60℃,时间1分钟,附加超声波振荡;11、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;12、化学铜:Cu3g/L、WN-ELCopper99开缸剂150mL/L、NaOH4.5g/L甲醛4g/L、WN-ELCopper99稳定剂15ppm、WN-ELCopper99添加剂1mL/L(温度55℃、时间8分钟),附加间断式超声波振荡,防止纤维粘连,形成良好铜镀层;13、纯水三次溢流洗涤:超纯水清洗3次,共1分钟,附加超声波振荡;14、、电镀镍:硫酸镍20g/L、氯化镍4g/L、硼酸45g/L、WN-NickelLS湿润剂1mL/L,(pH值4.5,温度60℃,电流密度2A/dm2,时间5分钟);铜导电柱进行导电;15、纯水三次溢流洗涤超纯水清洗3次,共1分钟,附加超声波振荡;16、热水洗:70℃热纯水清洗,清洗时间1分钟;17、吹干:冷风去水,吹干纤维中的水分,时间1分钟;18、烘干:120℃烘箱,4分钟;19、收集成品,上述所有步骤涉及的超声波振荡频率均为30kHz。PBO纤维为中蓝晨光生产的400dPBO纤维。
产品性能结果:400d PBO镀镍纤维,断裂强度≥80N,延长率≥12%,电阻阻值≤5Ω/m,耐摩擦测试阻值变化率≤10%,反复弯曲试验阻值变化率小于1%。
注:测试方法采用GB/T3291.1-1997纺织纺织材料性能和试验术语第1部分:纤维和纱线;GB/T3291.3-1997纺织纺织材料性能和试验术语第3部分:通则;GB/T6502-2008化学纤维长丝取样方法;GB/T238-2013金属材料线材反复弯曲试验方法1000次;GB/T14343-2008化学纤维长丝线密度试验方法;FZ/T50035-2016合成纤维长丝电阻试验方法;ASTMD3885-2002,5000次,120r/min,100次/圈0.5Lb、0.5Lb;GB/T19975-2005高强化纤长丝拉伸性能试验方法中隔距长度250mm、拉伸速度125mm/min。
Claims (6)
1.一种使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺,它是按照在设定好子槽长度、设定好速度的自动流水线下进行,其特征在于,具体的包括以下步骤:(1)碱性清洗:将纤维通过质量分数3~10%氢氧化钠溶液,附加超声波振荡,其中时间2分钟、温度40~60℃;(2)溢流洗涤;(3)粗化:含有40g/L的膨胀剂的质量分数的60%~80%的浓硫酸溶液,温度30~40℃,时间30秒钟,辅以机械振动,振幅3.5cm,振动频率为30~200次/min;(4)溢流洗涤;(5)表面调节:100g/L的表面调节剂溶液,温度30℃,时间2分钟,辅以超声波;(6)溢流洗涤;(7)预活化:10-30mL/L盐酸,温度30℃,时间1分钟;(8)预钯:30~50ppm胶体钯溶液,氯化亚锡12g/L,盐酸250~300mL/L,温度35℃,时间5分钟,分段超声波,均匀附着胶体钯;(9)纯水三次溢流洗涤;(10)解胶:质量分数15%硫酸溶液,温度60℃,时间1分钟,附加超声波振荡;(11)溢流洗涤;(12)化学铜:温度55℃,时间8分钟,附加间断式超声波振荡,间隔50cm设置20cm超波振荡;(13)溢流洗涤;(14)电镀镍:pH值3.5-4.5、温度55-60℃、电流密度0.3~2A/dm2、时间5分钟、加铜导电柱进行导电;(15)溢流洗涤;(16)热水洗:70℃热纯水清洗,清洗时间1分钟;(17)吹干:冷风去水,吹干纤维中的水分,时间1分钟;(18)烘干:120℃烘箱,4分钟;(19)收集成品。
2.根据权利要求1所述的使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺,其特征在于,所述步骤(14)的镍电镀液为硫酸镍20-35g/L、氯化镍3-5g/L、硼酸35-45g/L、湿润剂0.5-1.0mL/L。
3.根据权利要求1所述的使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺,其特征在于,所述步骤(12)化学铜Cu2.5~3g/L、开缸剂150mL/L、NaOH4.5g/L、甲醛4g/L、稳定剂15ppm、添加剂1mL/L。
4.根据权利要求1所述的使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺,其特征在于,所述溢流洗涤均为超纯水溢流清洗3次,共1分钟,附加超声波振荡。
5.根据权利要求1所述的使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺,其特征在于,所述的超声波振荡频率均为20~30kHz。
6.根据权利要求1所述的使镍金属牢固附着芳香族特种纤维长丝的连续性生产工艺,其特征在于,所述步骤(1)的芳香族纤维包括芳纶1414、PBO纤维、聚酰亚胺纤维中的其中一种。
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KR101604858B1 (ko) * | 2014-07-17 | 2016-03-21 | (주)크린앤사이언스 | 무전해 및 전해 도금의 연속 공정을 이용한 부직포의 도금방법 |
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 |
CN104894539A (zh) * | 2015-06-10 | 2015-09-09 | 上海大学 | 一种镀镍芳香族聚酰胺纤维的制备方法 |
CN108130573A (zh) * | 2018-02-27 | 2018-06-08 | 深圳市深联发科技有限公司 | 一种凯夫拉纤维的电镀系统 |
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