CN115627632A - 一种莱赛尔短纤维的制备方法及莱赛尔短纤维 - Google Patents
一种莱赛尔短纤维的制备方法及莱赛尔短纤维 Download PDFInfo
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Abstract
本发明公开一种莱赛尔短纤维的制备方法及莱赛尔短纤维,制备方法包括:1)制备纤维长丝,并将纤维长丝切断成短纤维;2)将短纤维铺成纤维网;3)在纤维网上进行交联反应后,解网即得莱赛尔短纤维。本发明中,纤维网上形成了弯折点,交联阶段在纤维网上进行,改善了纤维发脆的情况;交联阶段用添加剂能够在纤维网上均匀分布,保证交联纤维抗原纤化性能均匀,改善了纤维的力学性能,且具有较高的交联率;本发明的莱赛尔短纤维的干强度为3.72‑4.40dtex/cN,当莱赛尔短纤维的纤度为1.3dtex时,其湿摩擦值为730‑810次,即本发明莱赛尔短纤维的力学性能优异,抗原纤化性能好。
Description
技术领域
本发明涉及纤维领域,具体地说,涉及一种莱赛尔短纤维的制备方法及莱赛尔短纤维。
背景技术
莱赛尔(Lyocell)纤维是一种以N-甲基吗啉-N-氧化物(NMMO)为溶剂,采用干喷湿纺方法制备的纤维素纤维。莱赛尔(Lyocell)纤维采用木浆、竹浆和棉浆等作为原料,制备过程中,N-甲基吗啉-N-氧化物(NMMO)的回收率达到99.5%以上,具有经济适用性,且生产过程绿色环保,对环境友好无污染。莱赛尔(Lyocell)纤维力学性能优良,吸湿性好,具有真丝般光泽和柔软的手感,被誉为“21世纪最具发展前景的绿色纤维”,在国内外已经广泛生产。
Lyocell纤维具有较高的结晶度和取向度,在湿态环境下易吸水膨胀,使原纤之间的氢键被破坏,横向结合力减弱,所以在机械外力的作用下,原纤与原纤之间会发生分离,从而剥离纤维表面,发生原纤化现象。Lyocell纤维的原纤化倾向,严重限制了Lyocell纤维的应用。
为了改善Lyocell纤维的原纤化问题:
专利CN1119030A中采用聚乙二醇作为交联剂制备非原纤化莱赛尔纤维,其缺点是交联温度高,容易损伤纤维;
专利CN104005225A中采用乙二醛作为交联剂,氯化镁,硫酸铝,酒石酸作为催化剂,在生产过程中乙二醛会挥发到空气中,会污染环境;
专利CN110924153A、CN113265788A中采用TAHT作为交联剂,无机碱作为催化剂,采用交联剂和催化剂混合添加的方法,交联剂在混合溶液中会水解,不利于交联剂的高效利用,固化时间长,不利于产业化生产。
有鉴于此,特提出本发明。
发明内容
本发明要解决的技术问题在于克服现有技术的不足,提供一种莱赛尔短纤维的制备方法,以实现提高交联剂利用率,增强纤维力学性能,避免纤维发脆,降低制备成本的目的。
本发明采用技术方案的基本构思是:一种莱赛尔短纤维的制备方法,包括:
1)制备纤维长丝,并将纤维长丝切断成短纤维;
2)将短纤维铺成纤维网;
3)在纤维网上进行交联反应后,解网即得莱赛尔短纤维。
本发明中,纤维网上形成了弯折点,交联阶段在纤维网上进行,改善了纤维发脆的情况;添加剂和交联剂能够在纤维网上均匀分布,保证交联纤维抗原纤化性能均匀,改善了纤维的力学性能,且具有较高的交联率。
进一步地,所述步骤3)的交联反应包括:在纤维网上施加交联剂、盐剂、碱剂,并在加热条件下进行交联反应。
本发明中,碱剂提供碱性环境,使纤维充分溶胀,增加纤维素纤维中羟基的活性。盐剂可以降低交联剂与纤维之间的电荷阻力,从而提高交联剂的反应效率。
进一步地,施加交联剂、盐剂、碱剂的方法包括:先施加交联剂、盐剂、碱剂中的一种或两种,后施加剩下的一种或两种;或者,同时施加交联剂、盐剂、碱剂;
优选的,施加交联剂、盐剂、碱剂后,向纤维网施加压力,将交联剂、盐剂、碱剂压出;优选,施加压力的范围为0.1MPa-10Mpa。
交联剂或盐剂或碱剂经过一定压力后,能有效均匀地透过纤维网,从而提高纤维的交联率,首次施加的交联剂或盐剂或碱剂能够被压出重复利用,可以有效提高其利用率。
交联剂、碱剂、盐剂不同的添加顺序在本工艺下都可以实现抗原纤莱赛尔纤维的生产。
进一步地,交联剂或盐剂或碱剂循环添加1-3次,使交联剂或盐剂或碱剂在纤维网上分布均匀,能保证交联纤维抗原纤化性能均匀,且具有较高的交联率。
进一步地,施加的交联剂、盐剂、碱剂中的一种或多种的温度控制在10-95℃范围内,优选65-95℃。
本发明中,交联剂、盐剂、碱剂温度控制在65-95℃,在温度大于65℃时,交联剂可以与纤维素纤维发生反应,所以在进入反应室之前就发生部分交联反应,可以降低能耗。
进一步地,所述步骤3)中加热的温度为70-150℃,优选80-120℃;
优选的,所述步骤3)中的加热采用射频加热、微波加热、烘箱加热、蒸汽加热中的一种或多种方式,优选,采用射频加热或蒸汽加热。
优选的,所述步骤3)中加热的时间为0.5-6min。
本发明步骤3)中加热是第一次干燥纤维,也是仅有的一次干燥纤维,之前的所有处理均是在纤维湿态下进行的,
进一步地,所述步骤3)中解网前先利用清洗剂对纤维网进行清洗;
优选的,所述清洗剂包括水、酸性溶液中的一种或两种,优选,酸性溶液;
优选的,所述酸性溶液包括乙酸、盐酸、硫酸、草酸中的一种或多种;
优选的,酸性溶液的浓度为0.005-1.5wt%。
本发明中解网前纤维网采用清洗剂清洗,然后使用纯水将纤维清洗干净。采用清洗剂可以中和纤维上未反应的碱剂,可以快速将纤维清洗干净且排废量少。
进一步地,所述交联剂选用三嗪类交联剂,优选,1,3,5-丙烯酰胺基六氢-1,3,5-三嗪;
优选的,所述交联剂浓度范围为0.3-6wt%,优选0.5-3wt%。
进一步地,所述碱剂包括氨水、氢氧化钠、氢氧化钾、磷酸盐、碳酸氢钠、碳酸钠中的一种或多种;
优选的,所述碱剂pH范围为11-14;优选,pH范围为11.5-13。
进一步地,所述盐剂为包括氯化钠、硫酸钠、氯化钾,氯化镁、磷酸盐中的一种或多种;
优选的,盐剂的浓度范围为0.5-6wt%,优选0.5-3wt%。
本发明还提供一种莱赛尔短纤维,莱赛尔短纤维的干强度为3.97-4.08dtex/cN;
优选的,当莱赛尔短纤维的纤度为1.3dtex时,其湿摩擦值为780-810次;
优选的,所述莱赛尔短纤维采用上述技术方案任一所述的制备方法制备。
采用上述技术方案后,本发明与现有技术相比具有以下有益效果:
本发明中,纤维网上形成了弯折点,交联阶段在纤维网上进行,改善了纤维发脆的情况;交联阶段用添加剂能够在纤维网上均匀分布,保证交联纤维抗原纤化性能均匀,改善了纤维的力学性能,且具有较高的交联率。
本发明中,碱剂提供碱性环境,使纤维充分溶胀,增加纤维素纤维中羟基的活性。盐剂可以降低交联剂与纤维之间的电荷阻力,从而提高交联剂的反应效率。
下面结合附图对本发明的具体实施方式作进一步详细的描述。
附图说明
附图作为本发明的一部分,用来提供对本发明的进一步的理解,本发明的示意性实施例及其说明用于解释本发明,但不构成对本发明的不当限定。显然,下面描述中的附图仅仅是一些实施例,对于本领域普通技术人员来说,在不付出创造性劳动的前提下,还可以根据这些附图获得其他附图。在附图中:
图1是本发明的工艺流程图。
需要说明的是,这些附图和文字描述并不旨在以任何方式限制本发明的构思范围,而是通过参考特定实施例为本领域技术人员说明本发明的概念。
具体实施方式
实施例1
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝切断成38mm的短纤维,
2)将短纤维铺成纤维网;
3)添加温度为80℃浓度2.5wt%的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)溶液,浸轧三次,交联剂溶液循环利用,同时补加交联剂,保持交联剂溶液浓度不变,再添加温度为80℃pH为12的碱剂(氢氧化钠和碳酸钠)以及盐剂(硫酸钠2wt%和氯化钠2wt%),浸轧三次,其中压辊压力为0.2MPa,采用100℃加热纤维网6min,经过浓度为0.01%的盐酸溶液清洗纤维网,再用纯水清洗纤维网至中性,再经过上油、开解、烘干制备出具有抗原纤化效果的莱赛尔纤维。
实施例2
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝切断成38mm的短纤维,
2)将短纤维铺成纤维网;
3)添加温度为85℃pH为13的碱剂(氢氧化钠和磷酸钠)和盐剂(硫酸钠3wt%和氯化钠3wt%),浸轧三次,碱剂和盐剂循环利用,同时补加一定量的碱剂和盐剂,保持碱剂和盐剂浓度不变,再添加温度为85℃浓度为2.5wt%的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)溶液,浸轧三次,其中压辊压力为0.2MPa,采用110℃加热纤维网2min,经过浓度为0.02%草酸溶液清洗纤维,再用纯水清洗纤维网至中性,再经过上油、开解、烘干制备出具有抗原纤化效果的莱赛尔纤维。
实施例3
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝切断成38mm的短纤维,
2)将短纤维铺成纤维网;
3)添加温度85℃pH为11的碱剂(磷酸钠和碳酸钠)、盐剂(氯化钠3wt%)和浓度为2.5wt%的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)的混合溶液,浸轧三次,其中压辊压力为0.5MPa,采用105℃加热纤维网4.5min,经过浓度为0.03%醋酸溶液清洗纤维,再用纯水清洗纤维网至中性,再经过上油、开解、烘干制备出具有抗原纤化效果的莱赛尔纤维。
实施例4
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝切断成38mm的短纤维,
2)将短纤维铺成纤维网;
3)添加温度90℃、浓度为2.5wt%的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)和盐剂(氯化钠2.5wt%),浸轧三次,交联剂和盐剂循环利用,同时补加一定量的交联剂和盐剂,保持交联剂和盐剂浓度不变,再添加温度90℃、pH为11.5的碱剂(磷酸钠),浸轧三次,其中压辊压力为0.5MPa,采用100℃加热纤维网5min,经过浓度为0.015%的硫酸溶液清洗纤维网,再用纯水清洗纤维网至中性,再经过上油、开解、烘干制备出具有抗原纤化效果的莱赛尔纤维。
实施例5
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝切断成38mm的短纤维,
2)将短纤维铺成纤维网;
3)添加温度90℃、pH为13的碱剂(氢氧化钠和磷酸),浸轧三次,碱剂循环利用,同时补加一定量的碱剂,保持溶液pH不变,再添加温度85℃、浓度为2.5wt%的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)和盐剂(硫酸钠3wt%),浸轧三次,其中压辊压力为0.6MPa,采用110℃加热纤维网4min,经过浓度为0.02%草酸溶液清洗纤维网,再用纯水清洗纤维网至中性,再经过上油、开解、烘干制备出具有抗原纤化效果的莱赛尔纤维。
实施例6
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝切断成38mm的短纤维,
2)将短纤维铺成纤维网;
3)添加温度90℃、pH为13的碱剂(氢氧化钠和碳酸钠),浸轧三次,碱剂循环利用,同时补加一定量的碱剂,保持碱剂pH不变,再添加温度90℃、浓度为2.5wt%的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)和盐剂(氯化钠2.5wt%),浸轧三次,其中压辊压力为0.6MPa,采用100℃加热纤维网3min,经过浓度为0.015%的硫酸溶液清洗纤维网,再用纯水清洗纤维网至中性,再经过上油、开解、烘干制备出具有抗原纤化效果的莱赛尔纤维。
实施例7
本实施例与实施例6的区别仅在于:步骤3)中,采用110℃加热纤维网3min。
实施例8
本实施例与实施例6的区别仅在于:步骤3)中,采用120℃加热纤维网3min。
实施例9
本实施例与实施例6的区别仅在于:步骤3)中,采用130℃加热纤维网3min。
实施例10
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝切断成38mm的短纤维,
2)将短纤维铺成纤维网;
3)添加温度为85℃、pH为12.5的碱剂(磷酸钠和碳酸钠),浸轧三次,碱剂循环利用,同时补加一定量碱剂,保持碱剂pH值不变。再添加浓度为2.5wt%、温度为85℃的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)和盐溶液(硫酸钠3wt%),浸轧三次,其中压辊压力为0.5MPa,采用100℃加热纤维网0.5min,经过浓度为0.02%的草酸溶液清洗纤维,再用纯水清洗纤维至中性,再经过上油、开解、烘干制备出具有抗原纤化效果的莱赛尔纤维。
实施例11
本实施例与实施例10的区别仅在于:步骤3)中,采用100℃加热纤维网2min。
实施例12
本实施例与实施例10的区别仅在于:步骤3)中,采用100℃加热纤维网4min。
试验例1
本试验例对实施例1至实施例5得到的莱赛尔纤维的性能进行了检测,其中,线密度采用GB/T14335-2008进行检测;干断裂强度、钩接伸长率采用GB/T14337-2008进行检测;湿摩擦值采用FZ/T52019-2018进行检测;检测结果如下表1:
表1
由表1可见,本发明中由实施例1至实施例5制备得到的莱赛尔纤维干断裂强度为3.97-4.08dtex/cN,钩接伸长率为1.4-2.8%,即由本发明的制备方法得到的莱赛尔纤维力学性格能优异。当莱赛尔短纤维的纤度为1.3dtex时,其湿摩擦值为780-810次,即本发明的制备方法得到的莱赛尔纤维湿摩擦值较高,表明莱赛尔纤维的抗原纤化性能优异。
试验例2
本试验例对实施例6至实施例9得到的莱赛尔纤维的性能进行了检测,其中,线密度采用GB/T14335-2008进行检测;干断裂强度、钩接伸长率采用GB/T14337-2008进行检测;湿摩擦值采用FZ/T52019-2018进行检测;检测结果如下表2:
表2
由表2可见,当加热纤维网的温度处于100-130℃范围内时,湿摩擦值均较大,莱赛尔纤维具有较好的抗原纤化性能。进一步地,温度越高,莱赛尔纤维的力学性能相对会变差,因此,需要控制加热纤维网的温度保持在一定的范围内。
试验例3
本试验例对实施例10至实施例12得到的莱赛尔纤维的性能进行了检测,其中,线密度采用GB/T14335-2008进行检测;干断裂强度、钩接伸长率采用GB/T14337-2008进行检测;湿摩擦值采用FZ/T52019-2018进行检测;检测结果如下表3:
表3
由表3可见,当加热纤维网的在100℃下加热0.5-4min时,湿摩擦值均较大,莱赛尔纤维具有较好的抗原纤化性能。进一步地,加热时间越长,莱赛尔纤维的力学性能和湿摩擦值相对会变差,因此,需要控制加热纤维网的加热时间保持在一定的范围内。
对比例1
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝纤维,
2)添加温度90℃、pH为13的碱剂(氢氧化钠和磷酸),浸轧三次,碱剂循环利用,同时补加一定量的碱剂,保持溶液pH不变,再添加温度85℃、浓度为2wt%的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)和盐剂(硫酸钠3wt%),浸轧三次,其中压辊压力为0.6MPa,采用110℃加热长丝纤维4min,经过浓度为0.02%草酸溶液清洗长丝纤维,再用纯水清洗长丝纤维至中性,再经过上油、烘干、切断制备出具有抗原纤化效果的莱赛尔纤维。
将本对比例得到的莱赛尔纤维的性能进行了检测,其中,线密度采用GB/T14335-2008进行检测;干断裂强度、钩接伸长率采用GB/T14337-2008进行检测;湿摩擦值采用FZ/T52019-2018进行检测;并将检测结果与实施例5进行对比,结果下表4所示:
表4:
由上表可知,通过将长丝切断成短纤维,能够明显提升莱赛尔纤维的湿摩擦值、干断裂强度、钩接伸长率,即通过将长丝切断成短纤维在纤维网上形成了弯折点,交联阶段在纤维网上进行,改善了纤维发脆的情况;交联阶段用添加剂能够在纤维网上均匀分布,保证交联纤维抗原纤化性能均匀,改善了纤维的力学性能。
对比例2
1)将在N-甲基吗啉-N-氧化物(NMMO)中溶解并成型的长丝纤维,
2)添加温度90℃、pH为13的碱剂(氢氧化钠和磷酸),浸轧三次,碱剂循环利用,同时补加一定量的碱剂,保持溶液pH不变,再添加温度85℃、浓度为2wt%的交联剂(1,3,5-丙烯酰胺基六氢-1,3,5-三嗪)和盐剂(硫酸钠3wt%),浸轧三次,其中压辊压力为0.3MPa,采用110℃加热长丝纤维4min,经过浓度为0.02%草酸溶液清洗长丝纤维,再用纯水清洗长丝纤维至中性,再经过上油、烘干、切断制备出具有抗原纤化效果的莱赛尔纤维。
将本对比例得到的莱赛尔纤维的性能进行了检测,其中,线密度采用GB/T14335-2008进行检测;干断裂强度、钩接伸长率采用GB/T14337-2008进行检测;湿摩擦值采用FZ/T52019-2018进行检测;并将检测结果与实施例5进行对比,结果下表5所示:
表5:
由上表可知,在一定的压力范围内,纤维网上施加的压力越大,其对应的莱赛尔纤维的湿摩擦值越大、干断裂强度越高、钩接伸长率越大,即在一定范围内增大在纤维网上施加的压力有利于改善纤维的力学性能。
以上所述仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专利的技术人员在不脱离本发明技术方案范围内,当可利用上述提示的技术内容作出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明方案的范围内。
Claims (10)
1.一种莱赛尔短纤维的制备方法,其特征在于:
1)制备纤维长丝,并将纤维长丝切断成短纤维;
2)将短纤维铺成纤维网;
3)在纤维网上进行交联反应后,解网即得莱赛尔短纤维。
2.根据权利要求1所述的一种莱赛尔短纤维的制备方法,其特征在于:所述步骤3)的交联反应包括:在纤维网上施加交联剂、盐剂、碱剂,并在加热条件下进行交联反应。
3.根据权利要求2所述的一种莱赛尔短纤维的制备方法,其特征在于:施加交联剂、盐剂、碱剂的方法包括:先施加交联剂、盐剂、碱剂中的一种或两种,后施加剩下的一种或两种;或者,同时施加交联剂、盐剂、碱剂;
优选的,施加交联剂、盐剂、碱剂后,向纤维网向施加压力,将交联剂、盐剂、碱剂压出;优选,施加压力的范围为0.1MPa-2Mpa。
4.根据权利要求2或3所述的一种莱赛尔短纤维的制备方法,其特征在于:施加的交联剂、盐剂、碱剂中的一种或多种的温度控制在10-95℃范围内,优选65-95℃。
5.根据权利要求2-4任一所述的一种莱赛尔短纤维的制备方法,其特征在于:所述步骤3)中加热的温度为70-150℃,优选80-120℃;
优选的,加热的温度高于交联剂、盐剂、碱剂的温度;
优选的,所述步骤3)中的加热采用射频加热、微波加热、烘箱加热、蒸汽加热中的一种或多种方式,优选,采用射频加热或蒸汽加热;
优选的,所述步骤3)中加热的时间为0.5-6min。
6.根据权利要求1-5任一所述的一种莱赛尔短纤维的制备方法,其特征在于:所述步骤3)中解网前先利用清洗剂对纤维网进行清洗;
优选的,所述清洗剂包括水、酸性溶液中的一种或两种,优选,酸性溶液;
优选的,所述酸性溶液包括乙酸、盐酸、硫酸、草酸中的一种或多种;
优选的,酸性溶液的浓度为0.005-1.5wt%。
7.根据权利要求2-6任一所述的一种莱赛尔短纤维的制备方法,其特征在于:所述交联剂选用1,3,5-丙烯酰胺基六氢-1,3,5-三嗪、2,4-二丙烯酰胺基苯磺酸、N,N-亚甲基二丙烯酰胺中的一种或几种;优选,1,3,5-丙烯酰胺基六氢-1,3,5-三嗪;
优选的,所述交联剂浓度范围为0.3-6wt%,优选0.5-3wt%。
8.根据权利要求2-7任一所述的一种莱赛尔短纤维的制备方法,其特征在于:所述碱剂包括氨水、氢氧化钠、氢氧化钾、磷酸盐、碳酸氢钠、碳酸钠中的一种或多种;
优选的,所述碱剂pH范围为11-14;优选,pH范围为11.5-13。
9.根据权利要求2-8任一所述的一种莱赛尔短纤维的制备方法,其特征在于:所述盐剂为包括氯化钠、硫酸钠、氯化钾,氯化镁、磷酸盐中的一种或多种;
优选的,盐剂的浓度范围为0.5-6wt%,优选0.5-3wt%。
10.一种莱赛尔短纤维,其特征在于:莱赛尔短纤维的干强度为3.72-4.40dtex/cN;
优选的,当莱赛尔短纤维的纤度为1.3dtex时,其湿摩擦值为730-810次;
优选的,所述莱赛尔短纤维采用上述权利要求1-9任一所述的制备方法制备。
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