CN113430813A - 一种阻燃改性涤纶面料的制备方法 - Google Patents
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Abstract
本发明提供了一种阻燃改性涤纶面料的制备方法，包括以下步骤：S1.涤纶面料的改性；S2.低分子量开环透明质酸钠的制备；S3.改性溶液的配置：配制丝肽溶液、透明质酸钠混合溶液，然后加入柠檬酸和次亚磷酸钠，混合均匀；S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，进行浸轧烘焙处理；S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。本发明改良以往含磷阻燃面料的制备方法，通过复合改性的方法得到一种阻燃改性涤纶面料。
Description
技术领域
本发明涉及功能面料领域，具体涉及一种阻燃改性涤纶面料的制备方法。
背景技术
涤纶织物在燃烧时能够形成熔融滴落物，导致火焰的传播和二次伤害。抗熔滴是涤纶织物阻燃的难点之一。涤纶织物的阻燃改性方法主要有涤纶原丝的阻燃改性或者涤纶织物表面处理改性。织物阻燃后整理具有工艺简单、成本较低等优点，是表面处理改性方法之一。其中含磷阻燃剂具有低毒、高效等优点越来越多应用于织物的阻燃后整理，在纺织品阻燃领域有着广阔的发展前景。研究表明，磷元素是PET最有效的阻燃元素之一，目前已得到较多的研究。磷系阻燃剂阻燃涤纶主要是在凝聚相通过促进聚合物炭化起到阻燃作用。膨胀型阻燃剂的主要阻燃元素是磷和氮，在燃烧中起到隔热、隔氧等阻燃作用，并能抑制熔滴现象的产生，具有优良的阻燃特性。经传统膨胀型阻燃剂整理后的聚酯纤维具有优良的阻燃和抗熔滴效果。传统膨胀型阻燃剂在塑料、橡胶以及合成高聚物上得到了大量的研究和广泛的应用，但无磷的阻燃用于PET及其纤维的研究和应用还较少。
发明内容
要解决的技术问题：本发明的目的是提供一种阻燃改性涤纶面料的制备方法，改良以往含磷阻燃面料的制备方法，通过复合改性的方法得到一种阻燃改性涤纶面料。
技术方案：一种阻燃改性涤纶面料的制备方法，包括以下步骤：
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，进行碱胺同浴碱处理，得到表面改性的涤纶面料；
S2.开环透明质酸钠的制备：将透明质酸钠溶解水中，在透明质酸钠溶液中加入高碘酸钠溶液，避光反应，终止反应后截留分子量为10000-14000的透明质酸钠，冷冻干燥得到低分子量透明质酸钠；
S3.改性溶液的配置：配制2-8g/L丝肽溶液、1.5-6.6g/L透明质酸钠溶液，调节pH到2，常温下静置1h，然后加入柠檬酸和次亚磷酸钠，混合均匀；
S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，进行浸轧烘焙处理；
S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
优选的，所述步骤S1中乙二胺中的浓度为1-3wt％，氢氧化钠的浓度为10-20wt％，处理温度为70-80℃。
优选的，所述步骤S2中透明质酸钠的浓度为0.05-0.1wt％，高碘酸钠的浓度为2-4wt％，透明质酸钠溶液和高碘酸钠溶液的体积为5:2，避光反应的时间为15-20h。
优选的，所述步骤S4中浸轧烘焙处理工艺为：两浸两轧-烘干-水洗-烘干。
优选的，所述轧余率为95-100％，烘干温度为90-100℃，水洗温度为40℃。
优选的，所述步骤S5中CaCl2溶液的浓度为1.5-3wt％和SbCl3溶液的浓度为2.5-5.5wt％。
有益效果：本发明的阻燃面料的制备方法具备以下优点：
本发明中利用SbCl3和CaCl2协同阻燃，SbCl3在火焰下分解，分解出Cl游离基，与火焰中的活性H+和OH一等结合，起到抑制火焰的作用。同时SbCl3，蒸气密度大，附着于物料表面，起到隔绝空气的作用，并在火焰上空凝结成液滴或固体颗粒，能量在固体表面被消耗，使燃烧速度减慢或停止，同时利用透明质酸和丝素肽在织物表面的均匀分布，使得SbCl3和CaCl2能够结合在透明质酸的表面，增加阻燃效果。
具体实施方式
实施例1
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，乙二胺中的浓度为1wt％，氢氧化钠的浓度为10wt％，进行碱胺同浴碱处理，处理温度为70℃，得到表面改性的涤纶面料；
S2.开环透明质酸钠的制备：将透明质酸钠溶解水中，透明质酸钠的浓度为0.05wt％，在透明质酸钠溶液中加入高碘酸钠溶液，高碘酸钠的浓度为2wt％，透明质酸钠溶液和高碘酸钠溶液的体积为5:2，避光反应15h，终止反应后截留分子量为10000的透明质酸钠，冷冻干燥得到低分子量透明质酸钠；
S3.改性溶液的配置：配制2g/L丝肽溶液、6.6g/L透明质酸钠溶液，调节pH到2，常温下静置1h，然后加入柠檬酸和次亚磷酸钠，混合均匀；
S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，两浸两轧-烘干-水洗-烘干，轧余率为95％，烘干温度为90℃，水洗温度为40℃；
S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于浓度为1.5wt％CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于浓度2.5wt％SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
实施例2
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，乙二胺中的浓度为3wt％，氢氧化钠的浓度为20wt％，进行碱胺同浴碱处理，处理温度为80℃，得到表面改性的涤纶面料；
S2.开环透明质酸钠的制备：将透明质酸钠溶解水中，透明质酸钠的浓度为0.1wt％，在透明质酸钠溶液中加入高碘酸钠溶液，高碘酸钠的浓度为4wt％，透明质酸钠溶液和高碘酸钠溶液的体积为5:2，避光反应20h，终止反应后截留分子量为14000的透明质酸钠，冷冻干燥得到低分子量透明质酸钠；
S3.改性溶液的配置：配制8g/L丝肽溶液、1.5g/L透明质酸钠溶液，调节pH到2，常温下静置1h，然后加入柠檬酸和次亚磷酸钠，混合均匀；
S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，两浸两轧-烘干-水洗-烘干，轧余率为100％，烘干温度为100℃，水洗温度为40℃；
S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于浓度为3wt％CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于浓度5.5wt％SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
实施例3
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，乙二胺中的浓度为1.5wt％，氢氧化钠的浓度为13wt％，进行碱胺同浴碱处理，处理温度为73℃，得到表面改性的涤纶面料；
S2.开环透明质酸钠的制备：将透明质酸钠溶解水中，透明质酸钠的浓度为0.06wt％，在透明质酸钠溶液中加入高碘酸钠溶液，高碘酸钠的浓度为3wt％，透明质酸钠溶液和高碘酸钠溶液的体积为5:2，避光反应16h，终止反应后截留分子量为12000的透明质酸钠，冷冻干燥得到低分子量透明质酸钠；
S3.改性溶液的配置：配制4g/L丝肽溶液、5.0g/L透明质酸钠溶液，调节pH到2，常温下静置1h，然后加入柠檬酸和次亚磷酸钠，混合均匀；
S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，两浸两轧-烘干-水洗-烘干，轧余率为95％，烘干温度为100℃，水洗温度为40℃；
S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于浓度为2wt％CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于浓度3.5wt％SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
实施例4
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，乙二胺中的浓度为2.4wt％，氢氧化钠的浓度为16wt％，进行碱胺同浴碱处理，处理温度为76℃，得到表面改性的涤纶面料；
S2.开环透明质酸钠的制备：将透明质酸钠溶解水中，透明质酸钠的浓度为0.08wt％，在透明质酸钠溶液中加入高碘酸钠溶液，高碘酸钠的浓度为4wt％，透明质酸钠溶液和高碘酸钠溶液的体积为5:2，避光反应20h，终止反应后截留分子量为13500的透明质酸钠，冷冻干燥得到低分子量透明质酸钠；
S3.改性溶液的配置：配制6g/L丝肽溶液、3.2g/L透明质酸钠溶液，调节pH到2，常温下静置1h，然后加入柠檬酸和次亚磷酸钠，混合均匀；
S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，两浸两轧-烘干-水洗-烘干，轧余率为100％，烘干温度为90℃，水洗温度为40℃；
S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于浓度为2.5wt％CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于浓度4.5wt％SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
实施例5
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，乙二胺中的浓度为2wt％，氢氧化钠的浓度为15wt％，进行碱胺同浴碱处理，处理温度为75℃，得到表面改性的涤纶面料；
S2.开环透明质酸钠的制备：将透明质酸钠溶解水中，透明质酸钠的浓度为0.07wt％，在透明质酸钠溶液中加入高碘酸钠溶液，高碘酸钠的浓度为3.5wt％，透明质酸钠溶液和高碘酸钠溶液的体积为5:2，避光反应18h，终止反应后截留分子量为12500的透明质酸钠，冷冻干燥得到低分子量透明质酸钠；
S3.改性溶液的配置：配制5g/L丝肽溶液、4.5g/L透明质酸钠溶液，调节pH到2，常温下静置1h，然后加入柠檬酸和次亚磷酸钠，混合均匀；
S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，两浸两轧-烘干-水洗-烘干，轧余率为100％，烘干温度为95℃，水洗温度为40℃；
S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于浓度为2.2wt％CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于浓度4wt％SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
对比例1
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，乙二胺中的浓度为2.4wt％，氢氧化钠的浓度为16wt％，进行碱胺同浴碱处理，处理温度为76℃，得到表面改性的涤纶面料；
S2.开环透明质酸钠的制备：将透明质酸钠溶解水中，透明质酸钠的浓度为0.08wt％，在透明质酸钠溶液中加入高碘酸钠溶液，高碘酸钠的浓度为4wt％，透明质酸钠溶液和高碘酸钠溶液的体积为5:2，避光反应20h，终止反应后截留分子量为13500的透明质酸钠，冷冻干燥得到低分子量透明质酸钠；
S3.改性溶液的配置：配制6g/L丝肽溶液、3.2g/L透明质酸钠溶液，调节pH到2，常温下静置1h，然后加入柠檬酸和次亚磷酸钠，混合均匀；
S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，两浸两轧-烘干-水洗-烘干，轧余率为100％，烘干温度为90℃，水洗温度为40℃；
S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于浓度4.5wt％SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
对比例2
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，乙二胺中的浓度为2.4wt％，氢氧化钠的浓度为16wt％，进行碱胺同浴碱处理，处理温度为76℃，得到表面改性的涤纶面料；
S2.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，两浸两轧-烘干-水洗-烘干，轧余率为100％，烘干温度为90℃，水洗温度为40℃；
S3.织物的阻燃改性：将步骤S2处理的织物分别浸渍于浓度为2.2wt％CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于浓度4wt％SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
性能测试：
根据GB/T 5455-1997，采用AG5100A垂直燃烧测试仪进行织物样品的燃烧性能测试
| 点火时间(s) | 续燃时间(s) | 余灼时间(s) | 残余质量(％) | |
| 实施例1 | 10 | 0 | 0 | 98.5 |
| 实施例2 | 10 | 0 | 0 | 99.2 |
| 实施例3 | 10 | 0 | 0 | 98.4 |
| 实施例4 | 10 | 0 | 0 | 98.1 |
| 实施例5 | 10 | 0 | 0 | 99.0 |
| 对比例1 | 5 | 55 | 30 | 54.4 |
| 对比例2 | 2 | 80 | 120 | 23.8 |
Claims (6)
1.一种阻燃改性涤纶面料的制备方法，其特征在于，包括以下步骤：
S1.涤纶面料的改性：将涤纶面料置于乙二胺和氢氧化钠的混合溶液中，进行碱胺同浴碱处理，得到表面改性的涤纶面料；
S2.开环透明质酸钠的制备：将透明质酸钠溶解水中，在透明质酸钠溶液中加入高碘酸钠溶液，避光反应，终止反应后截留分子量为10000-14000的透明质酸钠，冷冻干燥得到低分子量透明质酸钠；
S3.改性溶液的配置：配制2-8g/L丝肽溶液、1.5-6.6g/L透明质酸钠溶液，调节pH到2，常温下静置1h，然后加入柠檬酸和次亚磷酸钠，混合均匀；
S4.织物的浸轧整理：将步骤S1制备的改性涤纶面料加入至改性溶液中，进行浸轧烘焙处理；
S5.织物的阻燃改性：将步骤S4处理的织物分别浸渍于CaCl2溶液中恒温水浴后焙烘，再将上述处理的织物再置于SbCl3溶液恒温水浴，将织物从溶液中取出，焙烘干，得到阻燃改性涤纶面料。
2.根据权利要求1所述的阻燃改性涤纶面料的制备方法，其特征在于：所述步骤S1中乙二胺中的浓度为1-3wt％，氢氧化钠的浓度为10-20wt％，处理温度为70-80℃。
3.根据权利要求1所述的阻燃改性涤纶面料的制备方法，其特征在于：所述步骤S2中透明质酸钠的浓度为0.05-0.1wt％，高碘酸钠的浓度为2-4wt％，透明质酸钠溶液和高碘酸钠溶液的体积为5:2，避光反应的时间为15-20h。
4.根据权利要求1所述的阻燃改性涤纶面料的制备方法，其特征在于：所述步骤S4中浸轧烘焙处理工艺为：两浸两轧-烘干-水洗-烘干。
5.根据权利要求1所述的阻燃改性涤纶面料的制备方法，其特征在于：所述轧余率为95-100％，烘干温度为90-100℃，水洗温度为40℃。
6.根据权利要求1所述的阻燃改性涤纶面料的制备方法，其特征在于：所述步骤S5中CaCl2溶液的浓度为1.5-3wt％和SbCl3溶液的浓度为2.5-5.5wt％。
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