CN114606613B - 一种抗氧化耐腐蚀氨纶包覆丝及其制备方法 - Google Patents

一种抗氧化耐腐蚀氨纶包覆丝及其制备方法 Download PDF

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CN114606613B
CN114606613B CN202210231385.7A CN202210231385A CN114606613B CN 114606613 B CN114606613 B CN 114606613B CN 202210231385 A CN202210231385 A CN 202210231385A CN 114606613 B CN114606613 B CN 114606613B
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spandex
aramid fiber
corrosion
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CN114606613A (zh
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庞秀英
柏芳军
项良夫
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Hangzhou Huifeng Chemical Fiber Co ltd
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Abstract

本申请涉及包覆丝的技术领域，具体公开了一种抗氧化耐腐蚀氨纶包覆丝及其制备方法。抗氧化耐腐蚀氨纶包覆丝包括氨纶芯丝、单向卷绕包覆于氨纶芯丝外围的改性芳纶纤维，所述改性芳纶纤维包括以下重量份的原料：芳纶纤维50‑60份、含氟聚酰亚胺2‑3份、乳清蛋白8‑12份、硅烷偶联剂1‑2份、聚乙二醇二缩水甘油醚8‑15份、抗氧化剂1‑3份。本申请中制备得到的氨纶包覆丝具有抗氧化、耐腐蚀性能优良的优点。

Description

一种抗氧化耐腐蚀氨纶包覆丝及其制备方法
技术领域
本申请涉及包覆丝的技术领域，更具体地说，它涉及一种抗氧化耐腐蚀氨纶包覆丝及其制备方法。
背景技术
氨纶纤维是聚氨基甲酸酯纤维的简称，是由指聚四氢呋喃与二苯基甲烷-4,4'-二异氰酸酯聚合而成。氨纶纤维是是现代服饰工业中常用的服装面料。氨纶长丝外包覆短纤维纱，即氨纶包覆丝，又称氨纶丝包芯纱，用其织制的弹力织物舒适、合体、弹性强，有人体第二皮肤的美誉。
氨纶包覆丝做成衣服，虽然其舒适度较高，但是其抗氧化性能较差，浅色的氨纶包覆丝衣服容易泛黄；由氨纶包覆丝制成的衣服耐腐蚀性能较差，在酸碱腐蚀下，容易发生破损。因此，开发一种抗氧化、耐腐蚀性能优良的氨纶包覆丝迫在眉睫。
发明内容
为了提高氨纶包覆丝的抗氧化、耐腐蚀性能，本申请提供一种抗氧化耐腐蚀氨纶包覆丝及其制备方法。
第一方面，本申请提供一种抗氧化耐腐蚀氨纶包覆丝，采用如下技术方案：
一种抗氧化耐腐蚀氨纶包覆丝，其包括氨纶芯丝、包覆于氨纶芯丝外围的改性芳纶纤维，所述改性芳纶纤维包括以下重量份的原料：芳纶纤维50-60份、含氟聚酰亚胺8-10份、乳清蛋白8-12份、硅烷偶联剂1-2份、聚乙二醇二缩水甘油醚3-5份、抗氧化剂1-3份。
通过采用上述技术方案，使得本申请中制备得到的抗氧化耐腐蚀氨纶包覆丝具有优良的抗氧化、耐腐蚀性能，抗氧化耐腐蚀氨纶包覆丝的DPPH自由基清除率的范围为91.6-91.8％；经过盐酸浸泡后得到断裂强力的范围为531-533N；经过氢氧化钠溶液浸泡后的断裂强力的范围为541-544N，抗氧化耐腐蚀氨纶包覆丝的DPPH自由基清除率、盐酸浸泡后的断裂强力、氢氧化钠溶液浸泡后的断裂强力均较高，说明抗氧化耐腐蚀的抗氧化性能，并且耐酸碱腐蚀的性能优良，符合市场需求。
在本申请中，以改性芳纶纤维对氨纶芯丝进行包覆，有助于弥补氨纶纤维抗氧化、耐腐蚀性能较差的缺陷；芳纶纤维全称为芳香族聚酰胺纤维，其具有超高强度，并且耐酸耐碱性能优良，然而直接将芳纶纤维包覆于氨纶芯丝外围，制备得到的氨纶包覆丝的抗氧化性能较差，通过将芳纶纤维进行改性，制备成为改性芳纶纤维，显著提高了氨纶包覆丝的抗氧化性能，同时进一步提高了其耐腐蚀性能；改性芳纶纤维的原料中加入了含氟聚酰亚胺，含氟聚酰亚胺为化学结构高度规整的刚性聚合物，同时含有的C-F键键能较高，不易断裂，稳定性优良，改性芳纶纤维的原料中还加入了聚乙二醇二缩水甘油醚，聚乙二醇二缩水甘油醚和含氟聚酰亚胺之间反应，使得制备得到的聚合物韧性提高，同时稳定性优良，在硅烷偶联剂的交联作用下，能够附着于芳纶纤维上；此外，乳清蛋白容易成膜，在乳清蛋白的作用下，有助于提高改性芳纶纤维的抗氧化、耐腐蚀、防水性能。
可选的，所述改性芳纶纤维采用以下方法制备得到：将含氟聚酰亚胺、乳清蛋白、硅烷偶联剂、聚乙二醇二缩水甘油醚、抗氧化剂混合均匀，得到混合液，然后将芳纶纤维加入至混合液中浸渍2-3h，然后取出，摊放晾干1-1.5h，再于55-60℃下烘干1.5-1h，得到改性芳纶纤维。
通过采用上述技术方案，通过浸渍、烘干即可制备得到改性芳纶纤维，制备方法简单，便于操作。并且当各操作条件分别位于上述范围内时，对于性能检测结果的影响在可预期范围内。
可选的，所述含氟聚酰亚胺包括以下重量份的原料：4-氯代苯酐25-30份、3-三氟甲基-4-氯苯胺22-25份、三乙胺12-15份、双(三苯基膦)二溴化镍0.6-1份、锌1-1.5份、N,N-二甲基乙酰胺60-80份。
通过采用上述技术方案，在双(三苯基膦)二溴化镍的催化下，锌的还原作用下，4-氯代苯酐和3-三氟甲基-4-氯苯胺反应得到含氟聚酰亚胺，各原料简单易得，且当各原料含量在上述范围内时，对于性能检测结果的影响在可预期范围内。
可选的，所述含氟聚酰亚胺采用以下方法制备得到：将4-氯代苯酐加入至N,N-二甲基乙酰胺总量的1/2-2/3中，再加入三乙胺，搅拌至混合均匀，然后在搅拌条件下于15-20min内加入3-三氟甲基-4-氯苯胺，反应6-8h，冷却至22±3℃，然后加入剩余量的N,N-二甲基乙酰胺，搅拌条件下加入双(三苯基膦)二溴化镍和锌，升温至80-90℃，反应7-9h，冷却至22±3℃，除溶剂，得到含氟聚酰亚胺。
通过采用上述技术方案，制备方法简单，容易操作，并且当各操作条件位于上述范围内时，对于性能检测结果的影响在可预期范围内。
可选的，抗氧化剂为四(2，4-二叔丁基苯基-4，4’-联苯基)双膦酸酯、双(2，4-二叔丁基苯基)季戊四醇二亚磷酸酯、DL-酒石酸中的一种或几种。
通过采用上述技术方案，能够有效提高氨纶包覆丝的抗氧化性能。
可选的，抗氧化剂为质量比为3-4:1的四(2，4-二叔丁基苯基-4，4’-联苯基)双膦酸酯与DL-酒石酸的混合物。
通过采用上述技术方案，能够进一步提高抗氧化耐腐蚀氨纶包覆丝的抗氧化性能。
可选的，芳纶纤维为芳纶1313。
可选的，硅烷偶联剂为3-氨丙基三乙氧基硅烷、乙烯基-三(2-甲氧基乙氧基)硅烷、乙烯基三甲氧基硅烷中的一种或几种。
第二方面，本申请提供一种抗氧化耐腐蚀氨纶包覆丝的制备方法，采用如下技术方案：一种如上述的抗氧化耐腐蚀氨纶包覆丝的制备方法，包括以下步骤：将改性芳纶纤维包覆于氨纶芯丝外围，得到抗氧化耐腐蚀氨纶包覆丝。
综上所述，本申请至少具有以下有益效果：
第一、通过以改性芳纶纤维对氨纶芯丝进行包覆，使得制备得到的抗氧化耐腐蚀氨纶包覆丝具有优良的抗氧化、耐腐蚀性能，DPPH自由基清除率为91.8％，经过盐酸浸泡后得到断裂强力为533N，经过氢氧化钠溶液浸泡后的断裂强力为544N；
第二、通过以四(2，4-二叔丁基苯基-4，4’-联苯基)双膦酸酯与DL-酒石酸的混合物作为抗氧化剂，进一步提高了抗氧化耐腐蚀氨纶包覆丝的抗氧化性能，使得DPPH自由基清除率升高至93.8％。
具体实施方式
以下结合实施例对本发明作进一步详细说明。
原料
氨纶芯丝，即氨纶单丝，选自南通新帝克单丝科技股份有限公司；芳纶1313货号为KD-101，且选自江苏凯盾新材料有限公司；乳清蛋白选自山东萍聚生物科技有限公司；聚乙二醇二缩水甘油醚选自湖北科沃德化工有限公司。
制备例I
制备例I-1
一种含氟聚酰亚胺，其采用以下方法制备得到：
将25kg4-氯代苯酐加入至40kg N,N-二甲基乙酰胺中，再加入12kg三乙胺，搅拌至混合均匀，然后在搅拌条件下于20min内加入24kg 3-三氟甲基-4-氯苯胺，反应8h，冷却至22℃，然后加入40kgN,N-二甲基乙酰胺，搅拌条件下加入0.8kg双(三苯基膦)二溴化镍和1kg锌，升温至80℃，反应7h，冷却至22℃，旋蒸除溶剂，得到含氟聚酰亚胺。
制备例II
表1制备例II-1～II-4中改性芳纶纤维的各原料含量(kg)
原料 制备例II-1 制备例II-2 制备例II-3 制备例II-4
芳纶纤维 50 53 57 60
含氟聚酰亚胺 3 2.8 2.3 2
乳清蛋白 12 10 9 8
硅烷偶联剂 1 1.4 1.7 2
聚乙二醇二缩水甘油醚 15 12 10 8
抗氧化剂 1 1.8 2.6 3
制备例II-1
一种改性芳纶纤维，其原料含量如表1所示；
其中，芳纶纤维为芳纶1313；
含氟聚酰亚胺由制备例I-1制备得到；
硅烷偶联剂为3-氨丙基三乙氧基硅烷；
抗氧化剂为四(2，4-二叔丁基苯基-4，4’-联苯基)双膦酸酯。
一种改性芳纶纤维，其采用以下方法制备得到：
将含氟聚酰亚胺、乳清蛋白、硅烷偶联剂、聚乙二醇二缩水甘油醚、抗氧化剂混合均匀，得到混合液；然后将芳纶纤维加入至混合液中浸渍3h，然后取出，摊放晾干1.5h，再于真空烘箱中55℃下烘干1h，得到改性芳纶纤维。
制备例II-5
一种改性芳纶纤维，其和制备例II-3的区别之处在于，抗氧化剂为双(2，4-二叔丁基苯基)季戊四醇二亚磷酸酯，其余均和制备例II-3相同。
制备例II-6
一种改性芳纶纤维，其和制备例II-3的区别之处在于，抗氧化剂为DL-酒石酸，其余均和制备例II-3相同。
制备例II-7
一种改性芳纶纤维，其和制备例II-3的区别之处在于，抗氧化剂为质量比为3:1的四(2，4-二叔丁基苯基-4，4’-联苯基)双膦酸酯与DL-酒石酸的混合物，其余均和制备例II-3相同。
实施例
实施例1
一种抗氧化耐腐蚀氨纶包覆丝，其包括氨纶芯丝、单向卷绕包覆于氨纶芯丝外围的由制备例II-1制备得到的改性芳纶纤维。
一种抗氧化耐腐蚀氨纶包覆丝的制备方法，其包括以下步骤：
将制备例II-1制备得到的改性芳纶纤维在细纱机牵伸机构的喇叭口处喂入；
将氨纶芯丝从前罗拉钳口喂入，使得氨纶芯丝与被牵伸的改性芳纶纤维汇合；
将汇合后的氨纶芯丝与改性芳纶纤维复合加捻，得到抗氧化耐腐蚀氨纶包覆丝，捻系数为300。
实施例2-7
实施例2-7的抗氧化耐腐蚀氨纶包覆丝，其和实施例1的区别之处在于，改性芳纶纤维依次分别由制备例II-2～II-7制备得到，其余均和实施例1相同。
对比例
对比例1
一种抗氧化耐腐蚀氨纶包覆丝，其和实施例1的区别之处在于，改性芳纶纤维的原料中未加入含氟聚酰亚胺，其余均和实施例1相同。
对比例2
一种抗氧化耐腐蚀氨纶包覆丝，其和实施例1的区别之处在于，改性芳纶纤维的原料中未加入聚乙二醇二缩水甘油醚，其余均和实施例1相同。
对比例3
一种抗氧化耐腐蚀氨纶包覆丝，其和实施例1的区别之处在于，改性芳纶纤维的原料中未加入含氟聚酰亚胺、聚乙二醇二缩水甘油醚，其余均和实施例1相同。
对比例4
一种抗氧化耐腐蚀氨纶包覆丝，其和实施例1的区别之处在于，以等量的芳纶纤维替换改性芳纶纤维，其与均和实施例1相同。
对比例5
一种抗氧化耐腐蚀氨纶包覆丝，其和实施例1的区别之处在于，抗氧化耐腐蚀氨纶包覆丝为氨纶芯丝，即未以改性芳纶纤维对氨纶芯丝进行包覆，其余均和实施例1相同。
性能检测试验
分别将实施例1-7、对比例1-5中制备得到的12种抗氧化耐腐蚀氨纶包覆丝织成织物，得到12种织物，并对12种织物进行以下性能检测：
抗氧化性能检测：将上述12种织物剪裁为1cm*1cm大小的面料，然后将剪裁后的织物依次分别按照1:30的浴比放置于DPPH的乙醇溶液中，DPPH乙醇溶液的浓度为20μmol/L，然后在恒温水浴振荡器中暗处震荡120分钟，分别取上层清液，于紫外可见吸光光光度计上进行吸光度检测，该吸光度值记为A1；空白的DPPH的乙醇溶液的吸光度值为A0；
另外分别取上述12种织物，并且将其剪裁为1cm*1cm大小，然后将该12种织物剪裁后面料放入乙醇中，然后在恒温水浴振荡器中暗处震荡120分钟，分别取上层清液，于紫外可见吸光光光度计上进行吸光度检测，该吸光度值记为A2；
计算DPPH自由基清除率，DPPH自由基清除率＝[A0-(A1-A2)]/A0*100％，DPPH自由基清除率越高，说明抗氧化耐腐蚀氨纶包覆丝的抗氧化性能越强；
耐腐蚀性能检测：分别取上述12种织物，并且将其剪裁为10cm*10cm大小，然后分别放入30％wt的盐酸中浸泡15min，然后依次检测12种织物的断裂强力I；
分别取上述12种织物，并且将其剪裁为10cm*10cm大小，然后分别放入25％wt的氢氧化钠溶液中浸泡15min，然后依次检测12种织物的断裂强力II，断裂强力I、断裂强力II越大，抗氧化耐腐蚀氨纶包覆丝的耐腐蚀性能越强；
断裂强力依据GB/T3923.1-1997《织物断裂强力和断裂伸长率的测定_条样法》检测得到，检测结果如表2所示。
表2检测结果
检测项目 DPPH自由基清除率/％ 断裂强力I/N 断裂强力II/N
实施例1 91.6 531 542
实施例2 91.6 532 541
实施例3 91.8 533 544
实施例4 91.7 532 543
实施例5 90.6 530 542
实施例6 90.2 532 544
实施例7 93.8 534 546
对比例1 83.1 510 522
对比例2 87.1 523 534
对比例3 81.8 504 516
对比例4 74.2 483 499
对比例5 60.1 310 342
从表2可以看出，本申请中的抗氧化耐腐蚀氨纶包覆丝具有优良的抗氧化、耐腐蚀性能，其DPPH自由基清除率的范围为90.2-93.8％；经过盐酸浸泡后得到断裂强力的范围为530-534N；经过氢氧化钠溶液浸泡后的断裂强力的范围为541-546N。在本申请中，通过改性芳纶纤维各原料之间的相互协同作用、改性芳纶纤维和氨纶芯丝之间的相互协同作用，显著提高了氨纶包覆丝的抗氧化、耐腐蚀性能，符合市场需求。
将对比例1-3和实施例1进行对比，对比例1中的织物的DPPH自由基清除率为83.1％，经过盐酸浸泡后的断裂强力为510N，经过氢氧化钠浸泡后的断裂强力为522N；对比例2中的织物的DPPH自由基清除率为87.1％，经过盐酸浸泡后的断裂强力为523N，经过氢氧化钠浸泡后的断裂强力为534N；对比例3中的织物的DPPH自由基清除率为81.8％，经过盐酸浸泡后的断裂强力为504N，经过氢氧化钠浸泡后的断裂强力为516N；实施例1中的织物的DPPH自由基清除率为91.6％，经过盐酸浸泡后的断裂强力为531N，经过氢氧化钠浸泡后的断裂强力为542N。通过上述数据可以看出，相比于实施例1，对比例1-3中的织物的抗氧化、耐腐蚀性能均下降。且相比于对比例1-2，对比例3中织物的抗氧化、耐腐蚀性能更差。相比于实施例1，对比例1中的改性芳纶纤维的原料中未加入含氟聚酰亚胺；对比例2中的改性芳纶纤维的原料中未加入聚乙二醇二缩水甘油醚；对比例3中的改性芳纶纤维的原料中未加入含氟聚酰亚胺、聚乙二醇二缩水甘油醚。可以看出，含氟聚酰亚胺、聚乙二醇二缩水甘油醚之间存在相互协同作用，两者协同能够进一步提高氨纶包覆丝的抗氧化、耐腐蚀性能。
将对比例4、对比例5和实施例1进行对比，对比例4中的织物的DPPH自由基清除率为74.2％，经过盐酸浸泡后的断裂强力为483N，经过氢氧化钠浸泡后的断裂强力为499N；对比例5中的织物的DPPH自由基清除率为60.1％，经过盐酸浸泡后的断裂强力为310N，经过氢氧化钠浸泡后的断裂强力为342N；实施例1中的织物的DPPH自由基清除率为91.6％，经过盐酸浸泡后的断裂强力为531N，经过氢氧化钠浸泡后的断裂强力为542N。相比于实施例1，对比例4中的以等量的芳纶纤维替换改性芳纶纤维；对比例5中未加入改性芳纶纤维，即以氨纶芯丝作为氨纶包覆丝。从上述对比可以看出，通过以芳纶纤维对氨纶芯丝进行包覆，有助于提高氨纶芯丝的抗氧化、耐腐蚀性能；通过以芳纶纤维制备得到改性芳纶纤维，能够进一步提高氨纶芯丝的抗氧化、耐腐蚀性能。
本具体实施例仅仅是对本发明的解释，其并不是对本发明的限制，本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改，但只要在本发明的权利要求范围内都受到专利法的保护。

Claims (5)

1.一种抗氧化耐腐蚀氨纶包覆丝，其特征在于，抗氧化耐腐蚀氨纶包覆丝包括氨纶芯丝、包覆于氨纶芯丝外围的改性芳纶纤维，所述改性芳纶纤维包括以下重量份的原料：芳纶纤维57份、含氟聚酰亚胺2.3份、乳清蛋白9份、硅烷偶联剂1.7份、聚乙二醇二缩水甘油醚10份、抗氧化剂2.6份；
所述改性芳纶纤维采用以下方法制备得到：将含氟聚酰亚胺、乳清蛋白、硅烷偶联剂、聚乙二醇二缩水甘油醚、抗氧化剂混合均匀，得到混合液，然后将芳纶纤维加入至混合液中浸渍3h，然后取出，摊放晾干1.5h，再于真空烘箱中 55℃下烘干 1h，得到改性芳纶纤维；
所述含氟聚酰亚胺采用以下方法制备得到：将 25kg4-氯代苯酐加入至 40kg N,N-二甲基乙酰胺中，再加入 12kg 三乙胺，搅拌至混合均匀，然后在搅拌条件下于 20min 内加入 24kg 3-三氟甲基-4-氯苯胺，反应 8h，冷却至 22℃，然后加入 40kg N,N-二甲基乙酰胺，搅拌条件下加入 0.8kg 双(三苯基膦)二溴化镍和 1kg 锌，升温至 80℃，反应 7h，冷却至 22℃，旋蒸除溶剂，得到含氟聚酰亚胺。
2.根据权利要求1所述的一种抗氧化耐腐蚀氨纶包覆丝，其特征在于，抗氧化剂为四(2,4-二叔丁基苯基-4,4’-联苯基)双膦酸酯。
3.根据权利要求1所述的一种抗氧化耐腐蚀氨纶包覆丝，其特征在于，芳纶纤维为芳纶1313。
4.根据权利要求1所述的一种抗氧化耐腐蚀氨纶包覆丝，其特征在于，硅烷偶联剂为3-氨丙基三乙氧基硅烷。
5.一种如权利要求1-4任一所述的抗氧化耐腐蚀氨纶包覆丝的制备方法，其特征在于，包括以下步骤：将改性芳纶纤维包覆于氨纶芯丝外围，得到抗氧化耐腐蚀氨纶包覆丝。
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