CN112342788A - 一种阻燃吸湿面料及其制备方法 - Google Patents

一种阻燃吸湿面料及其制备方法 Download PDF

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CN112342788A
CN112342788A CN202011314114.5A CN202011314114A CN112342788A CN 112342788 A CN112342788 A CN 112342788A CN 202011314114 A CN202011314114 A CN 202011314114A CN 112342788 A CN112342788 A CN 112342788A
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fabric
flame
metal salt
retardant
moisture
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姚玉元
甄建政
吕维扬
王金辉
孙继安
王燕
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ANZHENG FASHION GROUP
Zhejiang University of Technology ZJUT
Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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ANZHENG FASHION GROUP
Zhejiang University of Technology ZJUT
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Abstract

本发明公开了一种阻燃吸湿面料及其制备方法，具体为：将金属盐和碱性物质在水中充分溶解，然后转移到水热釜中经水热反应得到层状双金属氢氧化物(LDH)；将LDH置于缓冲液中超声得到均匀稳定的悬浮液体系；再将面料以及盐酸多巴胺加入到悬浮液体系中进行振荡处理，最后干燥得到改性织物。本发明中利用多巴胺与LDH配位，使LDH阻燃剂牢固负载在面料表面，并大幅提高改性层的稳定性。同时多巴胺可在常温下自聚，且粘附能力极强，该体现了该方法反应条件温和、简单易行、适用范围广的特点，改性之后的织物在阻燃和吸湿性能方面得到了显著提高。

Description

一种阻燃吸湿面料及其制备方法
技术领域
本发明涉及阻燃吸湿面料的制备领域，具体涉及一种基于层状双金属氢氧化物处理的阻燃吸湿面料。
背景技术
随着人们生活水平和防护意识的提高，阻燃面料的开发已刻不容缓。常用的织物可燃性极强，若不经过阻燃处理，容易引发火灾。据统计，世界上约20％以上的火灾事故都是由织物燃烧所引起，尤其是住宅失火。因此，阻燃面料的开发对消除火灾隐患，降低人民生命财产损失极为重要。现有的织物生产工艺，主要采用含溴、含磷的阻燃剂对织物进行阻燃处理，但是这类阻燃剂在燃烧过程中会释放大量烟雾和有毒气体，使人窒息，并且对环境造成污染，不符合绿色发展的要求。
层状双金属氢氧化物(Layered Double Hydroxides，简写为LDH)是一类层间具有可交换阴离子的水滑石类化合物，其结构类似于水镁石，一般由金属氧化物八面体相互共边形成主体层板，层间则主要分布阴离子以平衡总体电荷。 LDH的主体层板间存在强的共价键，层间是一种弱的相互作用力，主客体之间通过氢键、范德华力、静电力等结合。LDH具有以下性质：(1)可以调换的层间阴离子；(2)组成和结构可控；(3)热稳定性优异；(4)结构记忆效应。其特殊的结构特性和热学特性决定了其可作为阻燃剂用于高分子材料中。LDH层间吸附有大量的水分子，并且层板表面带有大量的羟基。在高温下，附着于聚合物表面的LDH失去层间水和层板表面的羟基，分解释放的水蒸气和CO2 气体能吸收大量热量并且稀释氧气浓度，从而降低聚合物燃烧表面的温度，起到阻燃效果。此外，LDH层板上拥有丰富的羟基，可增大织物的表面能，提高织物的亲水性，赋予其吸湿性能。LDH通常采用混合改性和后处理这两种方法来提高面料的阻燃性能。由于LDH与基体的相容性较差，直接混合纺丝容易导致丝熔体中LDH粒子分布不均匀，令熔体在拉伸过程中出现断裂，不利于纤维成型；后者大都通过物理吸附的方法将LDH附着到纤维表面，得到的改性纤维阻燃稳定性较差。因此，提供一种新型阻燃织物的制备方法是非常有必要的。
发明内容
本发明的目的是提供一种阻燃吸湿面料及其制备方法，利用聚多巴胺的强粘附能力使LDH牢固负载在聚多巴胺包覆的织物上，同时又通过聚多巴胺表面丰富的羟基和氨基与LDH层板的金属元素形成稳定配位，提高功能改性层的稳定性，改善原本面料的吸湿阻燃性能。该方法反应条件温和、简单易行，适用范围广，大大提高了原有面料的性能。
为解决上述技术问题，本发明的目的是这样实现的：
本发明所涉及的一种阻燃吸湿面料的制备方法，包括如下步骤：
(1)分别配制含有可溶性二价金属盐、可溶性三价金属盐的混合溶液和碱性溶液，然后将碱性溶液加入到混合溶液中，将混合溶液经水热处理及真空干燥后得到层状双金属氢氧化物片状物；
(2)将层状双金属氢氧化物加入缓冲液中超声，得到均匀稳定的悬浮液体系；
(3)将清洗干净的织物置于步骤(2)中的悬浮液中，加入盐酸多巴胺，振荡处理6～24h后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
作为优选，所述的可溶性二价金属盐中的二价金属离子为Cu2+、Zn2+、Ni2+、Mg2+、Fe2 +中的一种或两种；
所述的可溶性三价金属盐中的三价金属离子为Al3+、Ni3+、Fe3+、Ti3+中的一种或两种；
所述的可溶性二价金属盐、可溶性三价金属盐的阴离子为Cl-、NO3 -、SO4 2-、 CO3 2-中的一种或两种；
所述的碱性物质为尿素、氨水或氢氧化钠。
作为优选，所述的缓冲液为Tris缓冲液、磷酸盐缓冲液、硼酸盐缓冲液以及碳酸氢盐缓冲液。
作为优选，所述的面料为棉纤维、亚麻、羊毛、蚕丝、粘胶纤维、醋酸纤维、涤纶、锦纶、腈纶、丙纶或氯纶中的一种。
作为优选，所述步骤(1)中可溶性二价金属盐与可溶性三价金属盐的总浓度为0.05～0.5mol/L，可溶性二价金属盐与可溶性三价金属盐的摩尔质量比为 0.5～5:1，可溶性二价金属盐和可溶性三价金属盐总量与碱性物质的摩尔质量比为1:1～10。
作为优选，所述水热反应的温度为95～110℃，时间为6～24h。
作为优选，步骤(2)的超声时间为0.5-6h，LDH浓度为0.5-3g/L。
作为优选，步骤(3)中，所述缓冲物质浓度为0.5～5g/L，盐酸多巴胺加入量为0.2～5g/L；
作为优选，步骤(3)中，所述振荡处理时间为6～24h，振荡温度为20-50℃，振荡速度为100-300r/min。
本发明还涉及一种由上述制备方法所制备的阻燃吸湿面料。
与现有技术相比，本发明具有如下优点：
1、本发明利用聚多巴胺表面丰富的氨基和羟基使LDH和织物两者获得较好的界面结合性能，利于LDH的稳定固载；
2、LDH均匀分布在织物表面，在阻燃和吸湿方面更能发挥作用。LDH分子层间的水分子和层板表面带有的大量羟基在高温下，分解释放出的水蒸气和CO2气体能吸收大量热量，并且可以稀释氧气浓度以降低聚合物燃烧表面的温度，起到阻燃作用；此外，其层板间有大量的水分子并且层板上丰富的羟基，增大了织物的表面能，因此，一些亲水性较差的织物获得了亲水性，提高了织物的吸湿性能。
附图说明
图1为实施例1中未改性涤纶的表面接触角随时间变化的图；
图2为实施例1改性后涤纶的表面接触角随时间变化的图。
具体实施方式
下面结合附图和具体实施例对本发明进一步说明。
实施例1：
在50mL去离子水中，加入0.25g CuSO4、0.7g MgSO4、0.4g Al2(SO4)3和 2.6g尿素，充分溶解后转移到水热釜中，放于烘箱中100℃晶化12h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥12h得到层状双金属氢氧化物。
将2g/L的层状双金属氢氧化物置于浓度为2g/L三羟甲基氨基甲烷(Tris) 缓冲液中超声6h，得到均匀稳定的悬浮液体系。
将清洗干净的涤纶面料置于上述悬浮液中，加入2g/L盐酸多巴胺，在25℃，转速为200r/min下振荡处理12h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例2：
在50mL去离子水中，加入1.05g CuSO4与0.4gAl2(SO4)3和2.6g尿素，充分溶解后转移到水热釜中，放于烘箱中110℃晶化24h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥24h得到层状双金属氢氧化物。
将3g/L的层状双金属氢氧化物置于浓度为1g/L磷酸盐缓冲液中超声3h，得到均匀稳定的悬浮液体系。
将清洗干净的棉布置于上述悬浮液中，加入1g/L盐酸多巴胺，在30℃，转速为100r/min下振荡处理24h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例3：
在50mL去离子水中，1gZnCl2与0.3g FeCl3和5mL氨水(浓度为20％)，充分溶解后转移到水热釜中，放于烘箱中110℃晶化6h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥12h得到层状双金属氢氧化物。
将2g/L的层状双金属氢氧化物置于浓度为0.2g/L硼酸盐缓冲液中超声3h，得到均匀稳定的悬浮液体系。
将清洗干净的黏胶纤维面料置于上述悬浮液中，加入0.5g/L盐酸多巴胺，在50℃，转速为300r/min下振荡处理6h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例4：
在50mL去离子水中，加入2.1g Mg(NO3)2与0.8g Fe(NO3)3和5mL氨水(浓度为20％)，充分溶解后转移到水热釜中，放于烘箱中100℃晶化12h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥12h得到层状双金属氢氧化物。
将0.5g/L的层状双金属氢氧化物置于浓度为3g/L碳酸氢盐缓冲液中超声 6h，得到均匀稳定的悬浮液体系。
将清洗干净的蚕丝面料置于上述悬浮液中，加入1g/L盐酸多巴胺，在35℃，转速为200r/min下振荡处理6h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例5：
在50mL去离子水中，加入0.5g CuSO4与0.375g Fe2(SO4)3和2.7g尿素，充分溶解后转移到水热釜中，放于烘箱中100℃晶化18h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥18h得到层状双金属氢氧化物。
将1g/L的层状双金属氢氧化物置于浓度为1g/L三羟甲基氨基甲烷(Tris) 缓冲液中超声3h，得到均匀稳定的悬浮液体系。
将清洗干净的羊毛面料置于上述悬浮液中，加入2g/L盐酸多巴胺，在35℃，转速为100r/min下振荡处理18h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例6：
在50mL去离子水中，加入0.4gNiSO4与0.1gCr2(SO4)3和1.8g氢氧化钠，充分溶解后转移到水热釜中，放于烘箱中95℃晶化18h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥6h得到层状双金属氢氧化物。
将2g/L的层状双金属氢氧化物置于浓度为1g/L磷酸盐缓冲液中超声2h，得到均匀稳定的悬浮液体系。
将清洗干净的腈纶面料置于上述悬浮液中，加入2g/L盐酸多巴胺，在40℃，转速为300r/min下振荡处理18h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例7：
在50mL去离子水中，加入0.5g MgSO4与0.25gAl2(SO4)3和1.8g氢氧化钠，充分溶解后转移到水热釜中，放于烘箱中100℃晶化24h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥12h得到层状双金属氢氧化物。
将0.5g/L的层状双金属氢氧化物置于浓度为3g/L磷酸盐缓冲液中超声1h，得到均匀稳定的悬浮液体系。
将清洗干净的丙纶面料置于上述悬浮液中，加入2g/L盐酸多巴胺，在30℃，转速为300r/min下振荡处理6h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例8：
在50mL去离子水中，加入0.25gZnSO4、0.7g MgSO4、0.4g Fe2(SO4)3和1.8g 氢氧化钠，充分溶解后转移到水热釜中，放于烘箱中110℃晶化18h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥6h得到层状双金属氢氧化物。
将3g/L的层状双金属氢氧化物置于浓度为1g/L磷酸盐缓冲液中超声6h，得到均匀稳定的悬浮液体系。
将清洗干净的亚麻面料置于上述悬浮液中，加入0.5g/L盐酸多巴胺，在 35℃，转速为200r/min下振荡处理12h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例9：
在50mL去离子水中，加入1.1gFeSO4、0.4g Fe2(SO4)3和1.8g氢氧化钠，充分溶解后转移到水热釜中，放于烘箱中110℃晶化18h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥12h得到层状双金属氢氧化物。
将0.5g/L的层状双金属氢氧化物置于浓度为0.3g/L磷酸盐缓冲液中超声1h，得到均匀稳定的悬浮液体系。
将清洗干净的涤纶面料置于上述悬浮液中，加入0.5g/L盐酸多巴胺，在 35℃，转速为100r/min下振荡处理6h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
实施例10：
在50mL去离子水中，加入1.1gFeSO4、0.5g Ti2(SO4)3和1.8g氢氧化钠，充分溶解后转移到水热釜中，放于烘箱中100℃晶化18h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥6h得到层状双金属氢氧化物。
将1g/L层状双金属氢氧化物置于浓度为3g/L磷酸盐缓冲液中超声6h，得到均匀稳定的悬浮液体系。
将清洗干净的锦纶面料置于上述悬浮液中，加入5g/L盐酸多巴胺，在35℃，转速为300r/min下振荡处理24h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
对比例1：
在50mL去离子水中，加入0.25g CuSO4、0.7g MgSO4、0.4g Al2(SO4)3和 2.6g尿素，充分溶解后转移到水热釜中，放于烘箱中100℃晶化12h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥12h得层状双金属氢氧化物。
将2g/L的层状双金属氢氧化物置于浓度为3g/L磷酸盐缓冲液中超声6h，得到均匀稳定的悬浮液体系。
将清洗干净的涤纶面料置于上述悬浮液中，在25℃，转速为200r/min下振荡处理12h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
对比例2
在50mL去离子水中，加入1.1g MgNO3、0.4gAl(NO3)3和2.6g尿素，充分溶解后转移到水热釜中，放于烘箱中110℃晶化12h。反应结束待其降至室温后取出，用去离子水离心清洗数次，最后真空干燥24h得层状双金属氢氧化物。
将2g/L的层状双金属氢氧化物置于去离子水中超声6h，得到均匀稳定的悬浮液体系。
将清洗干净的涤纶面料置于上述悬浮液中，加入0.2g/L盐酸多巴胺，在 30℃，转速为100r/min下振荡处理24h，然后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
综合描述
(1)阻燃性
阻燃性参照GB/T 5454-1997标准，测定阻燃面料的极限氧指数(LOI)和续燃时间。
(2)吸湿性
吸湿性参照GB/T 16913.6-1997标准，测试其吸湿面料的吸湿率。
根据上述提出的评价标准对所述的实例进行测试，测试结果如表一所示。
Figure BDA0002790775740000101
注：极限氧指数采用GB/T5454，续燃时间采用GB/T5455，接触角表示为： CA0(初始接触角)/CA5(5min后接触角)。
由表一可知，分析实施例1～10的性能评价，可以发现，面料的阻燃性能和吸湿性能随着LDH的负载量和振荡处理时间的增加而显著增强。分析对比例1～2性能差异，可以发现，LDH的牢固负载需要借助多巴胺表面丰富的官能团，结合多巴胺的粘性和LDH可调控的特殊结构和热学性能，才能得到最佳的阻燃吸湿面料。
以上详细描述了本发明的较佳具体实施例。应当理解，本领域的普通技术人员无需创造性劳动就可以根据本发明的构思做出诸多修改和变化。因此，凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案，皆应在由权利要求书所确定的保护范围内。

Claims (10)

1.一种阻燃吸湿面料的制备方法，其特征在于，包括如下步骤：
(1)分别配制含有可溶性二价金属盐、可溶性三价金属盐的混合溶液和碱性溶液，然后将碱性溶液加入到混合溶液中，将混合溶液经水热处理及真空干燥后得到层状双金属氢氧化物片状物；
(2)将层状双金属氢氧化物加入缓冲液中超声，得到均匀稳定的悬浮液体系；
(3)将清洗干净的织物置于步骤(2)中的悬浮液中，加入盐酸多巴胺，振荡处理6～24h后取出织物置于烘箱干燥，得到所述吸湿阻燃的改性面料。
2.根据权利要求1所述的一种阻燃吸湿面料的制备方法，其特征在于，所述的可溶性二价金属盐中的二价金属离子为Cu2+、Zn2+、Ni2+、Mg2+、Fe2+中的一种或两种；
所述的可溶性三价金属盐中的三价金属离子为Al3+、Ni3+、Fe3+、Ti3+中的一种或两种；
所述的可溶性二价金属盐、可溶性三价金属盐的阴离子为Cl-、NO3 -、SO4 2-、CO3 2-中的一种或两种；
所述的碱性物质为尿素、氨水或氢氧化钠。
3.根据权利要求1所述的一种吸湿阻燃面料的制备方法，其特征在于，所述的缓冲液为Tris缓冲液、磷酸盐缓冲液、硼酸盐缓冲液以及碳酸氢盐缓冲液。
4.根据权利要求1所述的一种阻燃吸湿面料及其制备方法，其特征在于，所述的面料为棉纤维、亚麻、羊毛、蚕丝、粘胶纤维、醋酸纤维、涤纶、锦纶、腈纶、丙纶或氯纶中的一种。
5.根据权利要求1所述的一种阻燃吸湿面料的制备方法，其特征在于，所述步骤(1)中可溶性二价金属盐与可溶性三价金属盐的总浓度为0.05～0.5mol/L，可溶性二价金属盐与可溶性三价金属盐的摩尔质量比为0.5～5:1，可溶性二价金属盐和可溶性三价金属盐总量与碱性物质的摩尔质量比为1:1～10。
6.根据权利要求1所述的一种阻燃吸湿面料的制备方法，其特征在于，所述水热反应的温度为95～110℃，时间为6～24h。
7.根据权利要求1所述的一种阻燃吸湿面料的制备方法，其特征在于，步骤(2)的超声时间为0.5-6h，LDH浓度为0.5-3g/L。
8.根据权利要求1所述的一种阻燃吸湿面料的制备方法，其特征在于，步骤(3)中，所述缓冲物质浓度为0.5～5g/L，盐酸多巴胺加入量为0.2～5g/L。
9.根据权利要求1所述的一种阻燃吸湿面料的制备方法，其特征在于，步骤(3)中，所述振荡处理时间为6～24h，振荡温度为20-50℃，振荡速度为100-300r/min。
10.一种根据权利要求1-9任一项所述的制备方法所制备的阻燃吸湿面料。
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