CN116676684A - 一种高可纺性舒适氨纶纤维及其制造方法 - Google Patents
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Abstract
本发明公开了一种高可纺性舒适氨纶纤维，所述的氨纶纤维包含以下组分：NCO封端的聚氨酯脲预聚物、乙二胺扩链剂、黏度稳定剂、封端剂、抗静电剂；所述的NCO封端的聚氨酯脲预聚物由一种或多种多元醇与二异氰酸酯反应生成，所述的多元醇包括改性聚四氢呋喃多元醇、聚四氢呋喃多元醇、聚醚多元醇、聚酯多元醇。本发明采用了改进的产品组分，生产出的舒适氨纶纤维具有较高伸长、较低的模量，同时具有较高的生产连续性。
Description
技术领域
本发明涉及氨纶纤维制备技术领域，具体为一种高可纺性舒适氨纶纤维及其制造方法。
背景技术
氨纶丝线的优异延展性和回复性，令其在服装中的使用越来越广泛，曾经的贵族纤维进入了寻常大众衣橱，并且其应用比例逐年提高，从纤维味精走向织物纤维主成分之一，其在泳衣、内衣、运动衣中的添加比例甚至超过30％。一方面，氨纶纤维的解决了衣服容易穿脱问题，另一方面，氨纶所提供的保型美观性，使得其一经使用，无法拒绝。
除了美观，公众对衣物的健康功能更为关注，裹而不勒、包而不垮、休闲质感的新型氨纶成为有技术储备的厂家努力的方向，提高氨纶纱线的舒适性，需要提高氨纶纱线的伸长率同时降低其模量，能有效缓解人体压力，提高人们健康水平。
舒适氨纶生产过程中，一方面纺丝氨纶原液黏度比较难控制，使得氨纶原液的可纺性较差，丝饼满卷率较低，丝线均一性也受到影响。为提高氨纶的纺丝稳定性，专利CN102713033B透露利用环己胺、正庚胺等作为氨纶封端剂可以提高氨纶的可纺性，该封端体系适合低伸长高模量体系，不适用本舒适氨纶体系。美国专利US 6,403,712 B1透露利用聚合N-乙烯基吡咯烷酮(PVP)可以提高体系的可纺性，但是大量使用聚合物PVP,会降低氨纶的回弹和强力。专利CN101849048讲到在氨纶配方中使用部分2，4-MDI代替4，4′-MDI可以提高纱线的可纺性，2，4-MDI在本发明中仅仅以微量的工艺副产物存在于的4，4′-MDI。
CN1301280C提到二亚乙基三胺DETA可以稳定体系黏度，DETA能抑制氨纶原液黏度过快上涨的趋势，提高黏度的稳定性。但是DETA由于当量摩尔质量太低，添加量非常低，很难再短时间内快速与氨纶预聚物的端基NCO基团均匀反应，另外，DETA由于当量分子量太短会限制适氨纶丝线的伸长，降低舒适氨纶的舒适性。
发明内容
本发明的目的在于提供一种高可纺性舒适氨纶纤维及其制造方法，在提高氨纶纱线的伸长率和降低其模量的同时，提高氨纶纺丝的可纺性，提高氨纶丝线满卷率。
为实现上述目的，本发明提供如下技术方案：
一种高可纺性舒适氨纶纤维，所述的氨纶纤维包含以下组分：NCO封端的聚氨酯脲预聚物、黏度稳定剂、乙二胺扩链剂、封端剂、抗静电剂；所述的NCO封端的聚氨酯脲预聚物由一种或多种多元醇与二异氰酸酯反应生成，所述的多元醇包括改性聚四氢呋喃多元醇、聚四氢呋喃多元醇、聚醚多元醇、聚酯多元醇。
本方案采用包括改性聚四氢呋喃、聚四氢呋喃多元醇、聚醚多元醇、聚酯多元醇中一种或多种，和二异氰酸酯一起作为原材料，制备NCO(异氰酸酯基)封端的聚氨酯预聚物；制得的聚氨酯预聚物再利用黏度稳定剂多官聚醚胺、链增长剂(乙二胺扩链剂)、封端剂进行扩链反应形成聚氨酯脲溶液，在聚氨酯脲溶液中添加抗静电剂，经熟化后纺丝制备氨纶纤维，该氨纶纤维具备较好的可纺性；可纺性在化纤工艺学中并无严格定义，所谓“可纺”，一般意味着氨纶溶液在稳定拉伸作用下形成连续均匀细长丝条的能力，好的可纺性可表现为纺丝过程中纺丝流体黏度稳定，丝线断头率低，丝饼满卷率高，丝线均一性高等。采用本方案制备的舒适氨纶纤维产品，具有高伸长、低应力和稳定的可纺性，该氨纶纤维产品既适用于100D以上粗旦舒适氨纶产品，也适用于100D以下细旦舒适氨纶产品。
作为本发明优选的方案，所述的黏度稳定剂为多官聚醚胺，可选结构为下列结构中一种或多种组合，其用量为聚氨酯脲质量100-10000ppm,优选200-8000ppm。
a.BASF T403，(x+y+z)＝～5-6、
b.BASF T5000，(x+y+z)＝～85、
c.
T-403，(x+y+z)＝～5-6
或T-3000，(x+y+z)＝～50
或T-5000，(x+y+z)＝～85。
相较行业通用黏度稳定剂DETA,本发明优选多官聚醚胺，具有当量分子量高，容易均匀的与氨纶预聚物反应；同时，由于当量分子质量高，在有效控制氨纶原液黏度快速上升提高体系黏度稳定性的同时，能保持本体系氨纶丝线的高伸长与低模量。
作为本发明优选的方案，所述的抗静电剂为磺化琥珀酸二异辛醇钠盐、磺化琥珀酸二戊醇钠盐其中一种或两种，其用量为聚氨酯脲质量的100-5000ppm。
作为本发明优选的方案，所述的抗静电剂与黏度稳定剂的相加总量为聚氨酯脲质量的200-10000ppm，优选添加质量范围为500-8000ppm。
作为本发明优选的方案，所述的封端剂为二乙胺、正丁胺、正己胺、环己胺、正庚胺中的一种或几种组合，优选二乙胺。
作为本发明优选的方案，所述的二异氰酸酯为二苯基甲烷二异氰酸酯。本方案的二苯基甲烷二异氰酸酯主要成分为4,4′-二苯基甲烷二异氰酸酯。
作为本发明优选的方案，所述的NCO封端的聚氨酯脲预聚物中NCO的质量百分比为1.3-3.0％，优选1.5-2.5％。
作为本发明优选的方案，所述多元醇包括改性聚四氢呋喃多元醇、聚四氢呋喃多元醇、聚醚多元醇、聚酯多元醇中的一种或多种。多元醇数均分子量为1500-4500g/mol，优选1700-3500g/mol。
一种高可纺性舒适氨纶纤维的制造方法，包括如下步骤：
1)称取多元醇、二异氰酸酯；
2)使所述多元醇和二异氰酸酯反应生成NCO封端的聚氨酯脲预聚物；
3)称取扩链剂、黏度稳定剂、封端剂；
4)使所述NCO封端聚氨酯脲预聚物与扩链剂、黏度稳定剂和封端剂在溶剂中反应，生成聚氨酯脲溶液；
5)将抗静电剂和其它稳定剂/添加剂浆料加入聚氨酯脲溶液混合老化形成纺丝原液；
6)计量推送所述的纺丝原液进入纺丝甬道去除溶剂、加捻、上油形成氨纶纤维。
本发明采用性聚四氢呋喃、聚四氢呋喃多元醇、聚醚多元醇、聚酯多元醇中一种或多种与二苯基甲烷二异氰酸酯MDI反应制备NCO基封端的聚氨酯脲预聚物，然后以特定比例组合的黏度稳定剂、封端剂和抗静电剂控制纺丝稳定性，乙二胺作为扩链剂反应制备聚氨酯脲原液，以该聚氨酯脲原液可制取氨纶纤维；该方法既可以满足常规100D以上粗旦舒适氨纶连续生产，且适用于100D以下细旦舒适氨纶生产；其中50D氨纶模量SS300≤7.0cN，纺丝满卷率≥95％。
与现有技术相比，本发明的有益效果是：采用了改进的产品组分，生产出的舒适氨纶纤维具有较高伸长率，较低的模量，同时还具有较高的纺丝稳定性。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例,基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同,本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明,本文所使用的术语“及/或”包括一个或多个相关的所列项目的任意的和所有的组合。
本发明提供一种技术方案：
一种高可纺性舒适氨纶纤维，氨纶纤维包含以下组分：NCO封端的聚氨酯脲预聚物、乙二胺扩链剂、黏度稳定剂、封端剂、抗静电剂；NCO封端的聚氨酯脲预聚物由一种或多种多元醇与二异氰酸酯反应生成，多元醇包括改性聚四氢呋喃多元醇、聚四氢呋喃多元醇、聚醚多元醇、聚酯多元醇一种或多种。
黏度稳定剂为多官聚醚胺,其结构为下列结构中的一种或两种以上组合聚醚胺，其用量为聚氨酯脲质量的1～15毫摩尔当量/公斤。
a.BASF T403,(x+y+z)＝～5-6、
b.BASF T5000(x+y+z)＝～85、
c.
T-403，(x+y+z)＝～5-6
或T-3000，(x+y+z)＝～50
或T-5000，(x+y+z)＝～85
抗静电剂为磺化琥珀酸二异辛醇钠盐、磺化琥珀酸二戊醇钠盐其中一种或两种，其用量为聚氨酯脲质量的100-5000ppm。
抗静电剂与黏度稳定剂相加的剂量总量为聚氨酯脲质量的2000-10000ppm,抗静电剂与黏度稳定剂总量优选为聚氨酯脲质量的2000-6000ppm。
封端剂为二乙胺、正丁胺、正己胺、环己胺、正庚胺中的一种或几种组合，优选二乙胺。
二异氰酸酯为二苯基甲烷二异氰酸酯,二苯基甲烷二异氰酸酯主要成分为4,4′-二苯基甲烷二异氰酸酯。
NCO封端的聚氨酯脲预聚物中NCO的质量百分比为1.3-3.0％，优选1.5-2.5％。
多元醇包括改性聚四氢呋喃多元醇、聚四氢呋喃多元醇、聚醚多元醇、聚酯多元醇中的一种或多种。多元醇数均分子量为1500-4500g/mol，优选1700-3500g/mol。
一种高可纺性舒适氨纶纤维的制造方法，包括如下步骤：
1)称取多元醇、二异氰酸酯；
2)使所述多元醇和二异氰酸酯反应生成NCO封端的聚氨酯脲预聚物；
3)称取扩链剂、黏度稳定剂、封端剂；
4)使所述NCO封端聚氨酯脲预聚物与扩链剂、黏度稳定剂和封端剂在溶剂中反应，生成聚氨酯脲溶液；
5)将抗静电剂和其它稳定剂/添加剂浆料加入聚氨酯脲溶液混合老化形成纺丝原液；
6)计量推送所述的纺丝原液进入纺丝甬道去除溶剂、加捻、上油形成氨纶纤维。
具体实施过程；
实施例1，将巴斯夫产数均分子量为3000g/mol的m-PTHF 863克和巴斯夫产4，4′-MDI 137克,90℃反应90min,生成NCO％为2.20％预聚物,降温溶解预聚物于冷二甲基乙酰胺DMAC 1000克中得到预聚物DMAC溶液，预聚物溶液加入混合胺DMAC溶液1018克,其中聚醚胺T-5000相对氨纶纤维3800ppm、扩链剂乙二胺15.143克，封端剂二乙胺2.945克，反应结束得到透明聚氨酯脲原液。
将相对聚氨酯脲质量1000ppm的抗静电剂添加到添加剂浆料中，该添加剂浆料为抗氧剂245、抗紫外线剂622和润滑剂硬脂酸镁分散在DMAC中形成，按固体质量计算与聚氨酯脲质量相比分别为，抗氧剂245占1％、抗紫外线剂622占1％、润滑剂硬脂酸镁占0.2％。
将添加剂浆料加入透明聚氨酯脲原液，搅拌熟化，使纺丝黏度达到3000泊，推送纺丝，卷绕成型；测定氨纶丝伸长率、SS 300模量、满卷率。
实施例2，将数均分子量为2000g/mol的PTHF 839克和巴斯夫产4，4′-MDI 160克,90℃反应90min,生成NCO％为1.85％预聚物；降温溶解预聚物于冷二甲基乙酰胺DMAC 1000克中得到预聚物DMAC溶液；预聚物溶液加入混合胺DMAC溶液1005克,其中聚醚胺T-3000相对氨纶纤维2500ppm、扩链剂乙二胺12.510克，封端剂二乙胺3.080克，反应结束得到透明聚氨酯脲原液。
将1000ppm的抗静电与实施例1相同的添加剂浆料加入到透明聚氨酯脲原液，搅拌熟化，使纺丝黏度达到3000泊，推送纺丝，卷绕成型；测定氨纶丝伸长率、SS 300模量、满卷率。
实施例3，将数均分子量为2000g/mol的PTHF 839克和巴斯夫产4，4′-MDI 160克,90℃反应90min,生成NCO％为1.85％预聚物；降温溶解预聚物于冷二甲基乙酰胺DMAC 1000克中得到预聚物DMAC溶液；预聚物溶液加入混合胺DMAC溶液1005克,其中聚醚胺T-403相对氨纶纤维350ppm、扩链剂乙二胺12.510克，封端剂二乙胺3.080克，反应结束得到透明聚氨酯脲原液。
将3000ppm的抗静电与实施例1相同的添加剂浆料加入到透明聚氨酯脲原液，搅拌熟化，使纺丝黏度达到3000泊，推送纺丝，卷绕成型；测定氨纶丝伸长率、SS 300模量、满卷率。
对比例1，将数均分子量为2000g/mol的PTHF 839克和巴斯夫产4，4′-MDI 160克,90℃反应90min,生成NCO％为1.85％预聚物；降温溶解预聚物于冷二甲基乙酰胺DMAC 1000克中得到预聚物DMAC溶液；预聚物溶液加入混合胺DMAC溶液1005克,其中扩链剂乙二胺12.510克，封端剂二乙胺3.080克，反应结束得到透明聚氨酯脲原液。
将1000ppm的抗静电与实施例1相同的添加剂浆料加入到透明聚氨酯脲原液，搅拌熟化，使纺丝黏度达到3000泊，推送纺丝，卷绕成型；测定氨纶丝伸长率、SS 300模量、满卷率。
对比例2，将数均分子量为2000g/mol的PTHF 839克和巴斯夫产4，4′-MDI 160克,90℃反应90min,生成NCO％为1.85％预聚物；降温溶解预聚物于冷二甲基乙酰胺DMAC 1000克中得到预聚物DMAC溶液；预聚物溶液加入混合胺DMAC溶液1005克,其中聚醚胺T-5000相对氨纶纤维11000ppm、扩链剂乙二胺12.510克，封端剂二乙胺3.080克，反应结束得到透明聚氨酯脲原液。
将与实施例1相同的添加剂浆料加入透明聚氨酯脲原液，加入聚氨酯脲原液，搅拌熟化，使纺丝黏度达到3000泊，推送纺丝，卷绕成型；测定氨纶丝伸长率、SS 300模量、满卷率。
对比例3，将巴斯夫产数均分子量为3000g/mol的m-PTHF 3.00公斤和巴斯夫产MDI0.40公斤,90℃反应90min,生成NCO％为1.50％预聚物；降温溶解预聚物于冷二甲基乙酰胺DMAC中得到预聚物DMAC溶液，预聚物溶液入200ppm黏度稳定剂DETA、封端剂二乙胺和扩链剂乙二胺，反应结束得到透明聚氨酯脲原液；将6000ppm的抗静电与实施例1相同的添加剂浆料加入透明聚氨酯脲原液，搅拌熟化，使纺丝黏度达到3000泊，推送纺丝，卷绕成型；测定氨纶丝伸长率、SS 300模量、满卷率。
本发明的具体实施例和对比例产出的产品，其物理性能和满卷率进行如下评价：
1)断裂伸长率和SS300
将5cm样品采用拉伸测试机(由Instron Corp制造)在25℃，65％相对湿度和50cm/min速度下拉伸，测量断裂伸长率和300％伸长应力SS300；
2)满卷率
氨纶丝线在卷绕成型过程中，统计所有纺丝甬道丝线断头的频率，
满卷率＝1-断头丝饼个数/总丝饼个数。
下表为以上实施例和对比例生产获得的舒适氨纶纤维产品可纺性参数：
| 氨纶丝旦数 | 断裂伸长率 | SS300(cN) | 满卷率 | |
| 实施例1 | 50D | 780 | 5.0 | 99 |
| 实施例2 | 50D | 750 | 6.7 | 99 |
| 实施例3 | 50D | 745 | 6.4 | 98 |
| 对比例1 | 50D | 730 | 5.4 | 92 |
| 对比例2 | 50D | 640 | 6.6 | 90 |
| 对比例3 | 50D | 850 | 4.6 | 89 |
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种高可纺性舒适氨纶纤维，其特征在于，所述的氨纶纤维包含以下组分：NCO封端的聚氨酯脲预聚物、黏度稳定剂、乙二胺扩链剂、封端剂、抗静电剂；
所述的NCO封端的聚氨酯脲预聚物由一种或多种多元醇与二异氰酸酯反应生成，所述的多元醇包括改性聚四氢呋喃多元醇、聚四氢呋喃多元醇、聚醚多元醇、聚酯多元醇中的一种或多种。
2.根据权利要求1所述的一种高可纺性舒适氨纶纤维，其特征在于，所述的黏度稳定剂为多官聚醚胺，其结构为下述结构聚醚胺中的一种或多种组合
a.BASF T403，(x+y+z)＝～5-6、
b.BASF T5000，(x+y+z)＝～85、
c.
T-403，(x+y+z)＝～5-6
或T-3000，(x+y+z)＝～50
或T-5000，(x+y+z)＝～85。
3.根据权利要求1所述的一种高可纺性舒适氨纶纤维，其特征在于，所述的多官聚醚胺，其用量为聚氨酯脲质量的100-10000ppm,优选200-8000ppm。
4.根据权利要求1所述的一种高可纺性舒适氨纶纤维，其特征在于：所述的抗静电剂为磺化琥珀酸二异辛醇钠盐、磺化琥珀酸二戊醇钠盐其中一种或两种，其用量为聚氨酯脲质量的100-5000ppm。
5.根据权利要求1所述的一种高可纺性舒适氨纶纤维，其特征在于：所述的抗静电剂与黏度稳定剂总量为聚氨酯脲质量的500-10000ppm,优选500-8000ppm。
6.根据权利要求1所述的封端剂为二乙胺、正丁胺、正己胺、环己胺、正庚胺中的一种或几种组合。
7.根据权利要求1所述的一种高可纺性舒适氨纶纤维，其特征在于：所述的二异氰酸酯为二苯基甲烷二异氰酸酯。
8.根据权利要求1所述的一种高可纺性舒适氨纶纤维，其特征在于：所述的NCO封端的聚氨酯脲预聚物中NCO的质量百分比为1.3-3.0％。
9.根据权利要求1所述的一种高可纺性舒适氨纶纤维，其特征在于：所述的多元醇数均分子量为1500-4500g/mol。
10.权利要求1-9中任一项所述的一种高可纺性舒适氨纶纤维的制造方法，其特征在于，包括如下步骤：
1)称取多元醇、二异氰酸酯；
2)使所述多元醇和二异氰酸酯反应生成NCO封端的聚氨酯脲预聚物；
3)称取扩链剂、黏度稳定剂、封端剂；
4)使所述NCO封端聚氨酯脲预聚物与扩链剂、黏度稳定剂和封端剂在溶剂中反应，生成聚氨酯脲溶液；
5)将抗静电剂和添加剂/稳定剂浆料加入聚氨酯脲溶液混合老化形成纺丝原液；
6)计量推送所述的纺丝原液进入纺丝甬道去除溶剂、加捻、上油形成氨纶纤维。
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