CN106757485B - 一种高伸长氨纶纤维的制备方法 - Google Patents
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Abstract
本发明公开了一种高伸长氨纶纤维的制备方法,属于高分子材料制备技术领域,特别适合于氨纶纤维的高速纺丝,包括如下步骤:(1)在预聚反应阶段,以二异氰酸酯和低聚物二元醇为基本原料,得到异氰酸酯基封端的预聚物;(2)用非质子性极性溶剂溶解步骤1制备的预聚物,获得预聚物溶液;(3)向步骤2获得的预聚物溶液中加入扩链剂和链终止剂组成的混合胺溶液,经聚合反应后得到聚氨酯脲溶液,所述的扩链剂为聚醚胺与脂肪族二元胺的混合物;(4)将步骤3制备的氨纶纺丝液熟化后,采用干法纺丝制备高伸长氨纶。
Description
技术领域
本发明属于高分子材料制备技术领域,具体涉及一种高伸长氨纶纤维的制备方法。本发明制备的氨纶纤维具有优异的伸长性能,特别适合于在高纺丝速度下进行干法纺丝。
背景技术
氨纶是一种软硬段交替的多嵌段共聚物,硬段为氨纶纤维提供强度,软段为氨纶纤维提供弹性。软硬段交替的结构赋予氨纶纤维高断裂强度和弹性,从而使其广泛应用于多种服装用品。
随着氨纶在各种服装面料中的应用,其市场需求量也逐年增大,上游氨纶生产厂家在提高生产效率降低成本的同时,下游纺织厂家也在降低生产成本,以强化市场竞争力。上游氨纶生产厂家降低生产成本的一个有效途径是提高氨纶纤维的纺丝速度,但是纺丝速度提高会带来氨纶物理性能的恶化(如伸长降低、断裂强力下降);下游纺织厂家在使用氨纶织造时,通过提高氨纶纤维在退绕过程中的牵伸倍数来降低氨纶纤维在织物中的含量,从而降低生产成本,若氨纶纤维伸长不足则易造成断丝。
针对上述问题,开发一种高伸长的氨纶,既能满足氨纶生产企业提高纺速降低其生产成本,又能同时达到下游纺织面料低含氨量的目的。中国专利CN101736435A公开了一种软氨纶的生产方法,通过使用分子量大于3000并且带有侧基的聚合多元醇来制备伸长更高、应力更低的氨纶纤维,但其断裂强力明显下降,这样会导致氨纶纤维在后道应用中发生断丝的现象。中国专利CN102154729A公开了一中高伸长高牵伸氨纶纤维的制备方法,通过提高扩链剂中乙二胺相对于丙二胺的用量,从而赋予纤维高伸长高牵伸低应力的特性,但是本专利的纺丝速度低,仅为600-750m/min,生产成本高。
上述研究均涉及了高伸长氨纶的制备方法,但均存在一定的不足,因此如何在高纺速条件下制备一种高伸长氨纶,对上游氨纶生产企业和下游纺织企业均有十分重要的意义。
发明内容
技术问题:本发明的目的在于解决目前现有技术的不足,提供一种高伸长氨纶纤维的制备方法。由该方法制备的聚氨酯弹性纤维既能满足氨纶纤维高纺速的要求,又能同时满足氨纶纤维在使用过程中高牵伸的要求。
技术方案:为实现上述目的,本发明的一种高伸长氨纶纤维的制备方法包括如下几个步骤:
1)在预聚合反应阶段,将二苯基甲烷-4,4’二异氰酸酯和聚四氢呋喃醚二醇混合反应,得到异氰酸酯基封端的聚氨酯预聚物;
2)用非质子性极性溶剂溶解步骤1)所得的聚氨酯预聚物,从而获得预聚物溶液;
3)将步骤2)制备的预聚物溶液冷却后,加入混合胺溶液进行扩链反应和链终止反应,形成聚氨酯脲溶液;
4)向步骤3)制备的聚氨酯脲溶液中加入多种添加剂,充分混合均匀后,制备氨纶纺丝液;
5)将制备的氨纶纺丝液熟化后,采用干法纺丝得到高伸长氨纶纤维。
其中:
步骤3)所述的扩链反应所用的扩链剂为聚醚胺与脂肪族二元胺的混合物。
所述的聚醚胺为EDR-148,其分子量为148;EDR-176,其分子量为176;或EDR-192,其分子量为192,所述的脂肪族二元胺为乙二胺。
所述的聚醚胺与脂肪组二元胺的摩尔比为1:9~1:49。
步骤3)所述的链终止反应所用的链终止剂为二乙胺、二丙胺、乙醇胺或正己胺,或其混合物。
所述的二苯基甲烷-4,4’二异氰酸酯和聚四氢呋喃醚二醇混合反应,其摩尔比列为1.45:1~1.95:1。
所述的非质子性极性溶剂为N,N-二甲基甲酰胺(DMF)或N,N-二甲基乙酰胺(DMAC)。
所述的多种添加剂包括消光剂、防黄变剂、紫外线吸收剂、抗氧化剂和润滑解舒剂。
有益效果:本发明制备的氨纶纤维与常规氨纶纤维在结构和性质上有很大区别,软段部分仍为聚醚二元醇,但是硬段部分引入了部分柔性链段,破坏了硬段的规整性,使得硬段也具有一定的柔顺性,从而使制备的氨纶纤维具有高伸长的特性。
具体实施方式
本发明高伸长氨纶纤维的制备方法采用的技术方案如下,
1)在预聚合反应阶段,将二苯基甲烷-4,4’二异氰酸酯和聚四氢呋喃醚二醇混合反应,得到异氰酸酯基封端的聚氨酯预聚物;
2)用非质子性极性溶剂溶解步骤1)所得的聚氨酯预聚物,从而获得预聚物溶液;
3)将步骤2)制备的预聚物溶液冷却后,加入扩链剂和链终止剂的混合胺溶液进行扩链反应和链终止反应,形成聚氨酯脲溶液;
4)向步骤3)制备的聚氨酯脲溶液中加入多种添加剂,充分混合均匀后,制备氨纶纺丝液;
5)将制备的氨纶纺丝液熟化后,采用干法纺丝得到高伸长的聚氨酯弹性纤维。
其中,
步骤1)中所述的二苯基甲烷-4,4’二异氰酸酯和聚四氢呋喃醚二醇的摩尔比为1.45:1~1.95:1。
步骤2)中所述的非质子性极性溶剂选自N,N-二甲基甲酰胺(DMF)或N,N-二甲基乙酰胺(DMAC)。
步骤3)中所述的扩链剂为聚醚胺与脂肪族二元胺的混合物。
进一步,步骤3)中所述的聚醚胺为EDR-148(分子量为148),EDR-176(分子量为176)或EDR-192(分子量为192),所述的脂肪族二元胺为乙二胺。
进一步,步骤3)中所述的聚醚胺与脂肪组二元胺的摩尔比为1:4~1:49。
步骤3)中所述的链终止剂为二乙胺、二丙胺、乙醇胺或正己胺,或其混合物,优选二乙胺。
步骤4)中所述的添加剂为消光剂、防黄变剂、抗紫外线吸收剂、抗氧化剂和润滑解舒剂的DMAC溶液。
步骤5)中所述的氨纶纺丝液的表观粘度在40℃为4000~6000poise。
下面用实例来详细描述本发明,但这些实例不得理解为任何意义上对本发明的限制。
实施例1:
(1)将聚四氢呋喃醚二醇PTMG(分子量1810)150Kg、和二苯基甲烷-4,4’二异氰酸酯35.03Kg置于反应器中,在86±2℃反应120min,得到异氰酸酯基封端的预聚物,其中二苯基甲烷-4,4’二异氰酸酯和聚四氢呋喃醚二醇的摩尔比1.69:1;
(2)向预聚物中加入242.749Kg的DMAC,使预聚物在DMAC中充分溶解,形成预聚物溶液;
(3)向上述预聚物溶液加入由3.264Kg乙二胺、2.013Kg的EDR-148、0.608Kg二乙胺溶解于111.817Kg DMAC中所形成的胺类混合溶液,进行扩链反应和链终止反应,得到聚氨酯脲原液,其中混合胺溶液的浓度为5%,聚醚胺EDR-148与脂肪族乙二胺的摩尔比为1:4;
(4)向聚氨酯脲原液中加入消光剂、防黄变剂、紫外线吸收剂、抗氧化剂和润滑解舒剂得到聚氨酯纺丝原液;
(5)聚氨酯纺丝原液经熟化后,40℃下表观粘度为4000poise,经干法纺丝得到40D高伸长聚氨酯弹性纤维,其中纺丝速度为1200m/min,喷丝头温度为264℃。
实施例2:
制备方法同实施例1,区别在于步骤(3)的聚醚胺EDR-148与脂肪族乙二胺的摩尔比为1:9,所得产物在40℃下的表观粘度为4200poise。
实施例3:
制备方法同实施例1,区别在于步骤(3)的聚醚胺EDR-148与脂肪族乙二胺的摩尔比为1:19,所得产物在40℃下的表观粘度为4500poise。
实施例4:
制备方法同实施例1,区别在于步骤(3)的聚醚胺EDR-148与脂肪族乙二胺的摩尔比为1:49,所得产物在40℃下的表观粘度为4300poise。
实施例5:
制备方法同实施例1,区别在于步骤(3)中的聚醚胺为EDR-176,同时EDR-176与脂肪族乙二胺的摩尔比为1:9,所得产物在40℃下的表观粘度为4800poise。
对比例1:
制备方法同实施例1,区别在于步骤(3)采用乙二胺作扩链剂,所得产物在40℃下的表观粘度为5000poise。
对比例2:
制备方法同实施例1,区别在于步骤(3)采用乙二胺作扩链剂,所得产物在40℃下的表观粘度为5000poise,步骤(5)中的纺丝速度为800m/min。
通过以上实施例和对比例,得到以下测试数据。
试样 | 纺丝速度/(m·min<sup>-1</sup>) | 断裂强力DS/g | 断裂伸长率/% |
实施例1 | 1200 | 62.8 | 650.3 |
实施例2 | 1200 | 58.5 | 620.8 |
实施例3 | 1200 | 52.4 | 615.4 |
实施例4 | 1200 | 52.2 | 612.1 |
实施例5 | 1200 | 64.5 | 678.8 |
对比例1 | 1200 | 44.3 | 503.9 |
对比例2 | 800 | 53.3 | 545.7 |
备注:力学性能测试方法
采用CMT6101型微机控制电子万能试验仪(深圳市新三思材料检测有限公司)对试样进行拉伸强度测试。测试前试样在25℃,相对湿度65%的恒温恒湿条件下放置4h;测试时拉伸速度为500mm/min,试样长度为50mm,每个试样测试5次取平均值得其断裂强力、断裂伸长率。
Claims (4)
1.一种高伸长氨纶纤维的制备方法,其特征在于该方法包括如下几个步骤:
1)在预聚合反应阶段,将二苯基甲烷-4,4’二异氰酸酯和聚四氢呋喃醚二醇混合反应,得到异氰酸酯基封端的聚氨酯预聚物;
2)用非质子性极性溶剂溶解步骤1)所得的聚氨酯预聚物,从而获得预聚物溶液;
3)将步骤2)制备的预聚物溶液冷却后,加入混合胺溶液进行扩链反应和链终止反应,形成聚氨酯脲溶液;
4)向步骤3)制备的聚氨酯脲溶液中加入多种添加剂,充分混合均匀后,制备氨纶纺丝液;
5)将制备的氨纶纺丝液熟化后,采用干法纺丝得到高伸长氨纶纤维;
其中:
步骤3)所述的扩链反应所用的扩链剂为聚醚胺与脂肪族二元胺的混合物;所述的链终止反应所用的链终止剂为二乙胺、二丙胺、乙醇胺或正己胺,或其混合物;
所述的聚醚胺为EDR-148,其分子量为148;EDR-176,其分子量为176;或EDR-192,其分子量为192,所述的脂肪族二元胺为乙二胺;
所述的聚醚胺与脂肪组二元胺的摩尔比为1:9~1:49。
2.根据权利要求1所述的一种高伸长氨纶纤维的制备方法,其特征在于:所述的二苯基甲烷-4,4’二异氰酸酯和聚四氢呋喃醚二醇混合反应,其摩尔比列为1.45:1~1.95:1。
3.根据权利要求1所述的一种高伸长氨纶纤维的制备方法,其特征在于:所述的非质子性极性溶剂为N,N-二甲基甲酰胺(DMF)或N,N-二甲基乙酰胺(DMAC)。
4.根据权利要求1所述的一种高伸长氨纶纤维的制备方法,其特征在于:所述的多种添加剂包括消光剂、防黄变剂、紫外线吸收剂、抗氧化剂和润滑解舒剂。
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