CN112176724A - 一种聚芳噁二唑短纤维纺丝油剂及其制备方法 - Google Patents

一种聚芳噁二唑短纤维纺丝油剂及其制备方法 Download PDF

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CN112176724A
CN112176724A CN202011149348.9A CN202011149348A CN112176724A CN 112176724 A CN112176724 A CN 112176724A CN 202011149348 A CN202011149348 A CN 202011149348A CN 112176724 A CN112176724 A CN 112176724A
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徐进云
孙玉
刘燕军
吴玲
张朝
周存
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Tianjin Polytechnic University
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Abstract

本发明公开了一种聚芳噁二唑短纤维纺丝油剂及其制备方法。该纺丝油剂的复配原料质量百分比组成为：抗静电剂15～50％、平滑剂8～40％、乳化剂5～10％、调整剂5～10％和集束剂10～25％，各组份质量之和为100％。该制备方法是先将平滑剂和乳化剂加入反应釜中，加热至50～60℃，搅拌均匀，然后再将调整剂、抗静电剂和集束剂加入反应釜中，搅拌均匀后冷却至40～45℃，过滤即得。本发明得到的聚芳噁二唑短纤维纺丝油剂油剂性能优异，适用于POD的纺丝生产，能赋予纤维适宜的抗静电性、耐热性、平滑性、耐磨性、可洗性、抱合性等性能，满足上游生产和下游制造工艺的需求。

Description

一种聚芳噁二唑短纤维纺丝油剂及其制备方法
技术领域
本发明涉及合成纤维加工中的助剂制造领域，具体是一种聚芳噁二唑短纤维纺丝油剂及其制备方法。
背景技术
聚芳噁二唑(POD)纤维是一种高性能合成纤维，具有优良的耐高温性能、阻燃性能和电绝缘性，广泛应用于工业过滤网、特种防护服、航天服、军用特种装备。因此，聚芳噁二唑纤维对于我国多个重要领域具有极高的价值。
聚芳噁二唑短纤维在纺丝过程中采用的是湿法纺丝，这就要求与其相配套的纺织油剂要有非常好的水溶性，而且聚芳噁二唑短纤维所用的是酸性原液，这就要求油剂具有极好的酸稳定性。同时还要求油剂在溶液中具有较快的润湿速度，从而保证聚芳噁二唑短纤维丝束在油剂的酸性溶液中能够快速、均匀的上油。上油后的聚芳噁二唑短纤维还要经过250℃的高温加热，这就要求油剂具有很好的耐热性，不能在加热过程中过度分解失效，也不能由于受热而发生颜色改变导致纤维发黄变色。此外，聚芳噁二唑短纤维在下游加工工程中，要经过梳棉、并条、粗纱、细纱等工序，要油剂具有良好的抗静电性、摩擦特性、温湿度适应性以及较好的含有均匀性等。
发明内容
针对现有技术的不足，本发明拟解决的技术问题是，提供一种聚芳噁二唑短纤维纺丝油剂及其制备方法。
本发明解决所述纺丝油剂技术问题的技术方案是，提供一种聚芳噁二唑短纤维纺丝油剂，其特征在于，该纺丝油剂的复配原料质量百分比组成为：抗静电剂15～50％、平滑剂8～40％、乳化剂5～10％、调整剂5～10％和集束剂10～25％，各组份质量之和为100％。
本发明解决所述制备方法技术问题的技术方案是，提供一种聚芳噁二唑短纤维纺丝油剂的制备方法，其特征在于，先将平滑剂和乳化剂加入反应釜中，加热至50～60℃，搅拌均匀，然后再将调整剂、抗静电剂和集束剂加入反应釜中，搅拌均匀后冷却至40～45℃，过滤即得。
与现有技术相比，本发明的有益效果在于：
1.本发明得到的聚芳噁二唑短纤维纺丝油剂油剂性能优异，适用于POD的纺丝生产，能赋予纤维适宜的抗静电性、耐热性、平滑性、耐磨性、可洗性、抱合性等性能，满足上游生产和下游制造工艺的需求。
2.由于本油剂具有良好的耐热性，在高温纺丝生产过程中，可以充分保证纺丝的顺利进行
3.本油剂良好的可洗性，保证了纺丝在下游用户的印染、染整等工艺中不会出现质量问题
4.本油剂同时在一定程度上也提高了纤维的耐磨性能，使得POD在特殊领域的功能上得到保障。
5.本制备方法简单，便于操作，使用方便，适于工业化推广。
具体实施方式
下面给出本发明的具体实施例。具体实施例仅用于进一步详细说明本发明，不限制本申请权利要求的保护范围。
本发明提供了一种聚芳噁二唑短纤维纺丝油剂(简称纺丝油剂)，其特征在于该纺丝油剂由质量分数为15～50％的抗静电剂、质量分数为8～40％的平滑剂、质量分数为5～10％的乳化剂、质量分数为5～10％的调整剂和质量分数为10～25％的集束剂制成，各组份质量之和为100％。
优选地，该纺丝油剂由质量分数为25～45％的抗静电剂、质量分数为10～30％的平滑剂、质量分数为5～10％的乳化剂、质量分数为5～10％的调整剂和质量分数为15～25％的集束剂制成，各组份质量之和为100％。
所述抗静电剂是C6～C26烷基磷酸脂钾盐、C8～C18烷基苯磺酸盐或C6～C18烷基甜菜碱中的至少一种，组成原料为两种及以上的混合物时，各组成原料的比例不受限定。
所述平滑剂是基础油、动物油、脂肪酸酯或脂肪酸聚氧乙烯醚中的至少一种，组成原料为两种及以上的混合物时，各组成原料的比例不受限定。所述基础油是指石油裂解产物，矿物油就属于基础油的一种。
所述乳化剂是脂肪醇聚氧乙烯醚、脂肪醇聚氧乙烯聚氧丙烯醚、山梨醇单油酸酯、聚氧乙烯去水山梨醇酯或合成酯中的至少一种，组成原料为两种及以上的混合物时，各组成原料的比例不受限定。
所述调整剂是丙酸醇酯、脂肪醇或脂肪胺中的至少一种，组成原料为两种及以上的混合物时，各组成原料的比例不受限定。
所述集束剂是壬基酚聚氧乙烯醚和/或脂肪醇聚氧乙烯聚氧丙烯醚，组成原料为两种混合物时，各组成原料的比例不受限定。
本发明同时提供了一种聚芳噁二唑短纤维纺丝油剂的制备方法(简称制备方法)，其特征在于，该制备方法是将所述纺丝油剂的复配原料质量百分比组成按下述工艺进行制造，先将计量准确的平滑剂和乳化剂加入反应釜中，加热至50～60℃，搅拌时间0.5～1h，搅拌均匀发生乳化反应，然后再将调整剂、抗静电剂和集束剂加入反应釜中，搅拌1～2h后，冷却至40～45℃，过滤，出料，冷却至常温，包装即得。
实施例1
将40％质量分数的双组份平滑剂(20％质量分数的矿物油、20％质量分数的异构八醇脂肪酸酯)与5％的双组份乳化剂(2％质量分数的聚氧乙烯去水山梨醇酯、3％质量分数的C16醇聚氧乙烯醚)混合搅拌至60℃，搅拌1h，然后加入质量分数10％的调整剂C10脂肪醇和30％质量分数的抗静电剂(15％质量分数的C8烷基磷酸脂钾盐、15％质量分数的C18烷基甜菜碱)以及15％质量分数的集束剂(15％质量分数的壬基酚聚氧乙烯醚)，加入反应釜中，搅拌2h，冷却至40℃，过滤、出料，包装即得。
实施例2
将8％质量分数的双组份平滑剂(5％质量分数的60N矿物油、3％质量分数的动物油)与质量分数10％的双组份乳化剂(5％质量分数的山梨醇单油酸酯、5％质量分数的C8脂肪醇聚氧乙烯醚)混合搅拌至50℃，搅拌0.5h，然后加入10％质量分数的调整剂丙酸三醇酯和50％质量分数的抗静电剂(20％质量分数的C8烷基苯磺酸盐、30％质量分数的C14。烷基磷酸脂钾盐)以及22％质量分数的集束剂(10％质量分数的C14脂肪醇聚氧乙烯聚氧丙烯无规聚醚，12％质量分数的C12脂肪醇聚氧乙烯聚氧丙烯无规聚醚)，加入反应釜中，搅拌2h，冷却至40℃，过滤、出料，包装即得。
实施例3
将28％质量分数的双组份平滑剂(14％质量分数的异构十三醇脂肪酸酯、14％质量分数的异构十八醇脂肪酸酯)与质量分数10％的两组份乳化剂(7％质量分数的山梨醇单油酸酯、3％质量分数的C8脂肪醇聚氧乙烯醚)混合搅拌至60℃，搅拌0.5h，然后加入5％质量分数的调整剂C8脂肪胺和40％质量分数的抗静电剂(15％质量分数的C8烷基苯磺酸盐、25％质量分数的C16烷基磷酸脂钾盐)以及17％质量分数的集束剂(8％质量分数的壬基酚聚氧乙烯醚，9％质量分数的C8脂肪醇聚氧乙烯聚氧丙烯无规聚醚)，加入反应釜中，搅拌2h，冷却至45℃，过滤、出料，包装即得。
实施例4
将31％质量分数的双组份平滑剂(20％质量分数的硬脂酸聚氧乙烯醚、11％质量分数的动物油)与质量分数7％的两组份乳化剂(4％质量分数的C20脂肪醇聚氧乙烯醚、3％质量分数的C18脂肪醇聚氧乙烯聚氧丙烯醚)混合搅拌至60℃，搅拌0.5h，然后加入7％质量分数的调整剂C12脂肪醇和45％质量分数的抗静电剂(10％质量分数的C8烷基苯磺酸盐、10％质量分数的C14烷基苯磺酸盐、25％质量分数的C14烷基磷酸脂钾盐)以及10％质量分数的集束剂(5％质量分数的C16脂肪醇聚氧乙烯聚氧丙烯无规聚醚，5％质量分数的C14脂肪醇聚氧乙烯聚氧丙烯无规聚醚)，加入反应釜中，搅拌2h，冷却至50℃，过滤、出料，包装即得。
实施例5
将40％质量分数的双组份平滑剂(25％质量分数的动物油、15％质量分数的60N矿物油)与质量分数10％的两组份乳化剂(5％质量分数的山梨醇单油酸酯、5％质量分数的聚氧乙烯去水山梨醇酯)混合搅拌至60℃，搅拌0.5h，然后加入10％质量分数的调整剂C14脂肪醇和15％质量分数的抗静电剂(5％质量分数的C18烷基苯磺酸盐、5％质量分数的C16烷基苯磺酸盐、5％质量分数的C14烷基甜菜碱)以及25％质量分数的集束剂(15％质量分数的C16脂肪醇聚氧乙烯聚氧丙烯无规聚醚，10％质量分数的壬基酚聚氧乙烯醚)，加入反应釜中，搅拌2h，冷却至50℃，过滤、出料，包装即得。
实施例1～5合成的聚芳噁二唑短纤维油剂具有良好的耐热性、水洗型、抗静电性、平滑性、抱合性，可保证纺丝生产和后加工工序的顺利进行。
实施例6
将实施例1～5得到的纺丝油剂应用于纺丝中，以一条纺丝生产线一天需要1吨10％的纺丝油剂乳液计，先加入900kg的水(水温在25℃)，再加入100kg的本纺丝油剂，边搅拌边加入，搅拌制成均一的纺丝油剂乳液。纺丝时，把丝的原料(POD)熔融，然后挤出拉伸成丝，在这个过程中可采用喷淋或者水浴等方式加入纺丝油剂乳液，让丝上浸满纺丝油剂。另选择未添加任何纺丝油剂的方案作为对比例，各项参数与结果见表1。
表1
Figure BDA0002740702890000041
由表1可以看出，添加纺丝油剂后得到的POD纤维纤度有一定的下降，满足下游工艺使用需要，长度、拉伸强度均有大幅度增加，可见油剂组分对于POD生产有着重要作用，但选用不同组分会对油剂的性质产生影响，使得纤维最终的性能也会有着一定的区别。
断裂伸长率比不添加纺丝油剂时增加了一倍多，原因油剂中抱合剂的成分使得纤维在纺丝过程中，减少了毛丝、断头，从而增加了纤维断裂伸长率，增加了纤维的柔软度。
添加纺丝油剂后得到的POD纤维在300℃热收缩率在1％以下，因为油剂具有良好的耐热性能，从而使得纤维遇热产生的变化较小。
纤维卷曲数是影响纤维性能的一个重要指标，POD纤维在特殊领域有着重要应用，通过添加本油剂生产出的POD纤维，在纤维卷取数上完全达到该纤维的应用要求。
采用本纺丝油剂得到的纤维经一次水洗，采用有机溶剂萃取丝中残留组分，然后挥发检测，可检测的存在浓度均在0.5％以下。
本发明得到的油剂可达到如下质量指标：
外观：25℃透明均一的液体；
PH值(质量1％的25℃水溶液)：6～8；
有效成分含量(质量％)：50％以上，因为本发明的配方使用了大量的抗静电剂，抗静电剂多是水溶性的，因此有效成分无法提高，否则无法生产。同样在成品油剂的生产中，也会根据用料的不同有很大区别，本发明得到的成品油剂水相油剂，类似于矿泉水的状态；
乳液稳定性(质量1％的水溶液，72h25℃)，稳定不分层。
本发明未述及之处适用于现有技术。

Claims (10)

1.一种聚芳噁二唑短纤维纺丝油剂，其特征在于，该纺丝油剂的复配原料质量百分比组成为：抗静电剂15～50％、平滑剂8～40％、乳化剂5～10％、调整剂5～10％和集束剂10～25％，各组份质量之和为100％。
2.根据权利要求1所述的聚芳噁二唑短纤维纺丝油剂，其特征在于，该纺丝油剂由质量分数为25～45％的抗静电剂、质量分数为10～30％的平滑剂、质量分数为5～10％的乳化剂、质量分数为5～10％的调整剂和质量分数为15～25％的集束剂制成，各组份质量之和为100％。
3.根据权利要求1所述的聚芳噁二唑短纤维纺丝油剂，其特征在于，所述抗静电剂是C6～C26烷基磷酸脂钾盐、C8～C18烷基苯磺酸盐或C6～C18烷基甜菜碱中的至少一种。
4.根据权利要求1所述的聚芳噁二唑短纤维纺丝油剂，其特征在于，所述平滑剂是基础油、动物油、脂肪酸酯或脂肪酸聚氧乙烯醚中的至少一种。
5.根据权利要求4所述的聚芳噁二唑短纤维纺丝油剂，其特征在于，所述基础油是指石油裂解产物。
6.根据权利要求1所述的聚芳噁二唑短纤维纺丝油剂，其特征在于，所述乳化剂是脂肪醇聚氧乙烯醚、脂肪醇聚氧乙烯聚氧丙烯醚、山梨醇单油酸酯、聚氧乙烯去水山梨醇酯或合成酯中的至少一种。
7.根据权利要求1所述的聚芳噁二唑短纤维纺丝油剂，其特征在于，所述调整剂是丙酸醇酯、脂肪醇或脂肪胺中的至少一种。
8.根据权利要求1所述的聚芳噁二唑短纤维纺丝油剂，其特征在于，所述集束剂是壬基酚聚氧乙烯醚和/或脂肪醇聚氧乙烯聚氧丙烯醚。
9.一种权利要求1-8任一所述的聚芳噁二唑短纤维纺丝油剂的制备方法，其特征在于，先将平滑剂和乳化剂加入反应釜中，加热至50～60℃，搅拌均匀，然后再将调整剂、抗静电剂和集束剂加入反应釜中，搅拌均匀后冷却至40～45℃，过滤即得。
10.根据权利要求9所述的聚芳噁二唑短纤维纺丝油剂的制备方法，其特征在于，第一次搅拌的时间为0.5～1h至均匀，第二次搅拌的时间为搅拌1～2h至均匀。
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