CN116479645A - 一种阻燃混纺织物的制作方法 - Google Patents
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Abstract
本方案公开了纺织物制备技术领域的一种阻燃混纺织物的制作方法，包括以下步骤：步骤一、将混纺织物浸泡于亚铁离子盐溶液中，所述混纺织物的表面含有‑COOH、‑OH和‑NH2基团中的至少一种；步骤二、将浸泡后的混纺织物放置于恒温水浴锅中静置15～35h，然后取出干燥，即得所述阻燃混纺织物。本发明利用混纺织物上的‑COOH、‑OH和‑NH2等基团与金属离子间的强配位作用及氢氧化亚铁与氢氧化铁间稳定性差异，以亚铁盐为前驱体，首先水解生成氢氧化亚铁粒子，再在空气中氧气的缓慢氧化作用下，逐渐转化为稳定性更强的氢氧化铁纳米粒子，从而于混纺织物表面构筑均匀的氢氧化铁纳米阻燃层，制得具有优异阻燃性能的混纺织物。
Description
技术领域
本发明属于纺织物制备技术领域，特别涉及一种阻燃混纺织物的制作方法。
背景技术
羊毛/尼龙混纺织物(W/N)、涤/棉混纺织物等混纺织物具有舒适亲肤性、透水气性以及良好的力学性能被广泛应用。然而，部分混纺织物由于引入了易燃材料，导致混纺织物极容易燃烧。以羊毛/尼龙混纺织物为例，尼龙是一种碳氢链断含量较高的高分子化合物，在空气中极易被点燃，且燃烧时产生大量熔滴、释放有毒烟气。当尼龙与羊毛混纺后，其燃烧时会产生“烛芯效应”，燃烧更加剧烈，引发更大的火灾隐患。因此，提高易燃混纺织物的阻燃性能具有十分重要的现实意义。
混纺织物中，羊毛等表面含有大量的活性基团(-COOH，-OH，-NH2)，是一种两性聚电解质，可与磷元素形成共价键，与金属离子形成配位键。因此常用磷系阻燃剂或金属化合物对W/N进行无卤阻燃处理，实现凝聚相阻燃。例如，杨旭红等人通过沉积的方式将有机植酸和聚乙烯亚胺化合物负载于W/N上，构建了膨胀阻燃体系，有效提高了W/N的阻燃性能[Cheng X W,Tang R C,Yao F,et al.Flame retardant coating of wool fabric withphytic acid/polyethyleneimine polyelectrolyte complex[J].Progress in OrganicCoatings,2019,132:336-342.]。Koparal等人使用含金属锆或钛的化合物与W/N反应，通过形成配位键实现阻燃改性，金属锆或钛在燃烧过程中可催化尼龙/羊毛混纺织物快速成碳，形成保护层[Kaynak E,M E,Koparal AS.Halogen free flame retardantfinishing of wool and wool rich fabrics for aircraft seats[J].MaterialsToday:Proceedings,2020,31:S258-S262]。然而，以上阻燃方法均忽视了混纺织物本体的无毒、亲肤舒适和透水气性，并且降低了其机械强度，影响其使用性能。此外，由于阻燃剂与混纺织物间相互作用力较弱，在使用或洗涤过程中容易脱落，从而失去阻燃性能。
因此，在保持混纺织物优异的亲肤舒适性、透水气性、和较高机械强度的基础上，如何设计环保无毒的阻燃技术以提高其阻燃性能、抑烟性能、较好的耐水洗性能是当前阻燃领域亟待解决的难题之一。
发明内容
本发明意在提供一种阻燃混纺织物的制作方法，在确保混纺织物本身亲肤舒适性、透水气性和较高机械强度的基础上，提高易燃混纺织物的阻燃性能。
本方案中的一种阻燃混纺织物的制作方法，包括以下步骤：
步骤一、将混纺织物浸泡于亚铁离子盐溶液中，所述混纺织物的表面含有-COOH、-OH和-NH2基团中的至少一种；
步骤二、将浸泡后的混纺织物放置于恒温水浴锅中静置15～35h，然后取出干燥，即得所述阻燃混纺织物。
本方案的有益效果：本发明利用混纺织物上的-COOH、-OH和-NH2等基团与金属离子间的强配位作用及氢氧化亚铁与氢氧化铁间稳定性差异，以亚铁盐为前驱体，首先水解生成氢氧化亚铁粒子，再在空气中氧气的缓慢氧化作用下，逐渐转化为稳定性更强的氢氧化铁纳米粒子，从而于混纺织物表面构筑均匀的氢氧化铁纳米阻燃层，制得具有优异阻燃性能的混纺织物。该制备工艺简单、可大规模应用；另外，制备的阻燃混纺织物不但具有优异的阻燃及抑烟性能，其力学性能也有一定的提升。与此同时，由于混纺织物表面构筑的氢氧化铁纳米阻燃层紧密包裹织物纤维，对混纺织物纤维间隙遮挡填充少，其几乎保持了混纺织物本身的亲肤舒适性、透水气性。
进一步，所述混纺织物为羊毛/尼龙混纺织物(W/N)、涤/棉混纺织物、尼龙/棉混纺织物或尼龙/蚕丝混纺织物。
进一步，所述亚铁离子盐溶液为硫酸亚铁(FeSO4)、氯化亚铁(FeCl2)和硝酸亚铁(Fe(NO3)2)中的至少一种。
进一步，步骤一中，所述亚铁离子盐溶液中所含亚铁离子浓度为0.1-1.5mol/L。
进一步，步骤一中，将混纺织物浸泡于亚铁离子盐溶液中后，通过搅动或震荡的方式使得亚铁离子盐溶液将混纺织物完全浸湿。
进一步，步骤二中，所述恒温水浴温度为25～40℃。该温度范围，可以较好的控制氢氧化铁纳米粒子的生长动力学。
进一步，步骤二中，所述干燥的温度为25～90℃。该温度范围有助于防止氢氧化铁纳米粒子发生团聚。
本发明与现有技术相比较，具有以下优点：
(1)采用氧化诱导方式在易燃混纺织物表面原位生长氢氧化铁纳米粒子，可简单且有效控制氢氧化铁纳米粒子生长动力学，制得均匀分布、粒径小的氢氧化铁纳米粒子。
(2)充分利用了混纺织物的-COOH、-OH和-NH2等活性集团与亚铁离子及铁离子键的强配位作用，有效提高纳米阻燃剂与基材间的结合强度，从而获得较好的耐水洗性。
(3)氢氧化铁作为一种高效环保阻燃剂，其制备原料价格便宜，生产成本低；制备的工艺简单，易实现批量生产；
(4)在提高W/N阻燃及抑烟性能的同时，保持W/N原有的优异力学性能。
附图说明
图1为实例1制备的阻燃W/N的表面SEM照片；
图2为实例1制备的阻燃W/N垂直燃烧性能测试后照片；
图3为实例1制备的阻燃W/N与常规W/N锥形量热测试HRR曲线；
图4为实例1制备的阻燃W/N与常规W/N锥形量热测试THR曲线；
图5为实例1制备的阻燃W/N与常规W/N锥形量热测试SPR曲线；
图6为实例1制备的阻燃W/N与常规W/N锥形量热测试TSP曲线；
图7为实例1制备的阻燃W/N经水洗24h后表面SEM照片。
具体实施方式
下面通过具体实施方式进一步详细说明：
下面通过实施例对本发明进行具体的描述，且本发明技术方案不局限于以下所列举的具体实施方式，还包括各具体实施方式之间的任意组合。
有必要在此指出的是本实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，对于本领域的技术人员根据上述发明内容所做的一些非本质的改进与调整，也视为落在本发明的保护范围内。需要强调的是，此处所描述的具体实施例中的基材尺寸仅仅用以详细叙述本发明内容，并不用于限定本发明。
本发明提供的一种阻燃混纺织物的制作方法，该方法的工艺步骤和条件如下(以下实施例所用物料的份数，如无特殊说明，均为重量份)：
实施例1
一种阻燃混纺织物的制作方法，包括以下步骤：
首先，将30×10cm的W/N浸泡于1500mL 0.1mol/L硫酸亚铁溶液中震荡5min；
然后，将充分浸泡后的W/N置于恒温水浴锅中，30℃下保持24h；最后，取出W/N并于90℃烘箱中干燥2h，即得阻燃W/N。
性能测试：
(1)表观形貌测试
采用JEOL JSM-5900LV扫描电子显微镜(SEM)观察W/N织物的表面形貌，测试前对样品表面进行喷金处理。
经测试可见，阻燃处理后，W/N织物表面均匀的附着了大量Fe(OH)3纳米粒子，其粒径约为110nm，如附图1所示。
(2)极限氧指数(LOI)测试
极限氧指数测试是现代测试材料阻燃性能的一种常用测试方法，是指被测材料在氮-氧混合气体中能够平稳燃烧所需的最低氧气浓度。本专利依据《GB/T 5454-1997》使用JF-3氧指数测定仪进行测定，式样规格为125mm×20mm，每组试样平均测试三次，最后结果取平均值，测试结果评定标准如表1所示。
表1极限氧指数等级评定表
经测定，所制阻燃W/N的LOI可高达31.6％，达到难燃材料级别。
(3)垂直燃烧等级测试
本专利采用CZF-3型垂直燃烧仪对样品进行阻燃性能测试，按照UL-94测试标准进行测试，样品尺寸为275mm×75mm，具体判定标准如表2。
表2垂直燃烧测试要求
经测定，所制阻燃W/N通过UL-94测试V-0级，如附图2所示。
(4)锥形量热(Cone Calorimeter,CC)测试
CC为根据氧消耗原理设计的燃烧行为研究仪器，通过测定材料燃烧时的点燃时间(time to ignition,TTI)、热释放速率(heat release rate,HRR)、总热释放量(totalheat release,THR)、烟释放速率(smoke product rate,SPR)、总烟释放量(total smokeproduction,TSP)等燃烧参数对材料的燃烧行为进行表征，是目前公认的最理想的小型燃烧性能测试仪器。本专利中试样的CC测试采用昆山莫帝斯科燃烧技术仪器有限公司的锥形量热仪进行测试，辐照功率为35kW/m2，试样尺寸为100mm×100mm。
经测试，所制阻燃W/N的HRR峰值降低至185.6kW m-2，如附图3所示；THR值降低至6.16MJ m-2，如附图4所示；与未经阻燃处理W/N相比，分别降低了48.5％和15.0％。另外，所制阻燃W/N的SPR峰值与TSP值分别降低至0.006m2 s-1and 0.09m2，分别如附图5和附图6所示；与未经阻燃处理W/N相比，分别降低了76.92％及55.0％。
(5)耐水洗性能测试
将所制阻燃W/N浸泡于600mL水中，磁力搅拌24h后取出烘干，观察其表面Fe(OH)3纳米粒子的变化。
经测试，水洗24h后的阻燃W/N表面仍然附着有大量的Fe(OH)3纳米粒子(如附图7所示)，且其仍然展现出优异的阻燃性能，表明所制阻燃W/N具有较好的耐水洗性。
以上测试结果表明阻燃处理大幅度提升了W/N织物的阻燃及抑烟性能，且所制阻燃W/N具有优异的耐水洗性。
实施例2
一种阻燃混纺织物的制作方法，包括以下步骤：
首先，将30×10cm的W/N浸泡于1500mL 0.8mol/L硫酸亚铁溶液中震荡5min；
然后，将充分浸泡后的W/N置于恒温水浴锅中，30℃下保持24h；最后，取出W/N并于90℃烘箱中干燥2h，即得阻燃W/N。
采用SEM观察所制阻燃W/N表面显示，所制织物表面均匀的附着了大量Fe(OH)3纳米粒子。测试所制阻燃W/N的LOI值为30.0％，通过UL-94测试V-0级，其HRR峰值从360.1降低至221.5kW/m2，THR从7.25降低至6.25MJ/m2，SPR峰值从0.026降低至0.009m2/s，TSP值从0.20降低至0.11m2。
实施例3
一种阻燃混纺织物的制作方法，包括以下步骤：
首先，将30×10cm的W/N浸泡于1500mL 0.6mol/L氯化亚铁溶液中震荡5min；
然后，将充分浸泡后的W/N置于恒温水浴锅中，25℃下保持24h；
最后，取出W/N并于90℃烘箱中干燥2h，即得阻燃W/N。
采用SEM观察所制阻燃W/N表面显示，所制织物表面均匀的附着了大量Fe(OH)3纳米粒子。测试所制阻燃W/N的LOI值为32.1％，通过UL-94测试V-0级，其HRR峰值从360.1降低至242.9kW/m2，THR从7.25降低至6.31MJ/m2，SPR峰值从0.026降低至0.008m2/s，TSP值从0.20降低至0.10m2。
实施例4
一种阻燃混纺织物的制作方法，包括以下步骤：
首先，将30×10cm的W/N浸泡于1500mL 0.4mol/L硫酸亚铁溶液中震荡5min；
然后，将充分浸泡后的W/N置于恒温水浴锅中，40℃下保持24h；
最后，取出W/N并于70℃烘箱中干燥2h，即得阻燃W/N。
采用SEM观察所制阻燃W/N表面显示，所制织物表面均匀的附着了大量Fe(OH)3纳米粒子。测试所制阻燃W/N的LOI值为28.4％，通过UL-94测试V-0级，其HRR峰值从360.1降低至246.2kW/m2，THR从7.25降低至6.36MJ/m2，SPR峰值从0.026降低至0.011m2/s，TSP值从0.20降低至0.12m2。
实施例5
一种阻燃混纺织物的制作方法，包括以下步骤：
首先，将30×10cm的W/N浸泡于1500mL 0.6mol/L硫酸亚铁溶液中震荡5min；
然后，将充分浸泡后的W/N置于恒温水浴锅中，30℃下保持24h；最后，取出W/N并于40℃烘箱中干燥6h，即得阻燃W/N。
采用SEM观察所制阻燃W/N表面显示，所制织物表面均匀的附着了大量Fe(OH)3纳米粒子。测试所制阻燃W/N的LOI值为28.9％，通过UL-94测试V-0级，其HRR峰值从360.1降低至252.8kW/m2，THR从7.25降低至6.43MJ/m2，SPR峰值从0.026降低至0.013m2/s，TSP值从0.20降低至0.14m2。
实施例2～5制备的阻燃W/N的性能检测方法与实施例1相同，在此不再赘述。
Claims (7)
1.一种阻燃混纺织物的制作方法，其特征在于：包括以下步骤：
步骤一、将混纺织物浸泡于亚铁离子盐溶液中，所述混纺织物的表面含有-COOH、-OH和-NH2基团中的至少一种；
步骤二、将浸泡后的混纺织物放置于恒温水浴锅中静置15～35h，然后取出干燥，即得所述阻燃混纺织物。
2.根据权利要求1所述的一种阻燃混纺织物的制作方法，其特征在于：所述混纺织物为羊毛/尼龙混纺织物、涤/棉混纺织物、尼龙/棉混纺织物或尼龙/蚕丝混纺织物。
3.根据权利要求2所述的一种阻燃混纺织物的制作方法，其特征在于：所述亚铁离子盐溶液为硫酸亚铁、氯化亚铁和硝酸亚铁中的至少一种。
4.根据权利要求1～3任一项所述的一种阻燃混纺织物的制作方法，其特征在于：步骤一中，所述亚铁离子盐溶液中所含亚铁离子浓度为0.1-1.5mol/L。
5.根据权利要求4所述的一种阻燃混纺织物的制作方法，其特征在于：步骤一中，将混纺织物浸泡于亚铁离子盐溶液中后，通过搅动或震荡的方式使得亚铁离子盐溶液将混纺织物完全浸湿。
6.根据权利要求5所述的一种阻燃混纺织物的制作方法，其特征在于：步骤二中，所述恒温水浴温度为25～40℃。
7.根据权利要求6所述的一种阻燃混纺织物的制作方法，其特征在于：步骤二中，所述干燥的温度为25～90℃。
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