CN112376271B - 一种超亲水/油下超亲水自清洁阻燃棉布的制备方法 - Google Patents
一种超亲水/油下超亲水自清洁阻燃棉布的制备方法 Download PDFInfo
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Abstract
本发明公开了一种超亲水/油下超亲水自清洁阻燃棉布的制备方法，其特征在于包括有以下步骤：(1)将棉布浸入含有多元酰氯的有机溶剂溶液中，浸泡1～10分钟后，在50～100℃下加热10～30分钟；其中，所述有机溶剂溶液中多元酰氯的浓度0.5～5wt％；(2)将步骤(1)处理后得到的棉布浸入含有四羟甲基氯化磷和胺类化合物的水溶液中，浸泡1～10分钟后，在50～100℃下加热10～30分钟，得到所需的超亲水/油下超亲水自清洁阻燃棉布；其中，所述水溶液中四羟甲基氯化磷的浓度5～10wt％，胺类化合物的浓度5～10wt％。与现有技术相比，本发明的超亲水/油下超亲水自清洁阻燃棉布能对油污进行自清洁且具有阻燃性质。
Description
技术领域
本发明涉及亲水材料技术领域，具体指一种超亲水/油下超亲水自清洁阻燃棉布的制备方法。
背景技术
棉布在日常生活中作为服装和家装饰品被广泛使用，传统的棉布具有超亲水的性质，在穿着和使用过程中容易被油污污染，需要配合洗涤剂进行水洗去除油污，对棉布赋予自清洁能力正被越来越多的研究者关注。
常见的方法是对棉布进行超双疏(疏水疏油)处理，如专利申请号为CN201810576796.3(公布号为CN108951167A)的发明专利《一种棉布表面的双疏处理方法》将棉布先后浸泡于含氢硅油与正己烷的混合溶液及1H,1H,2H-全氟-1-癸烯中，在Kastredt催化剂作用下，最终在棉布表面接枝带有氟原子的长碳链基团，从而赋予棉布优越的疏水性能及一定的疏油性能。但是这种处理会使棉布失去吸湿排汗的功能。
目前最新的技术是对棉布进行超亲水超疏油处理，但是这种方法往往需要使用昂贵的亲水疏油单体，而且制备工艺比较复杂，不利于工业化生产；另外，棉布是高度易燃的，如不幸造成火灾会对人身和财产造成不可估量的损失，限制了其应用，有必要对棉布进行阻燃处理可以有效防止其燃烧。
发明内容
本发明所要解决的技术问题是针对现有技术的现状，提供一种能对油污进行自清洁且具有阻燃性质的超亲水/油下超亲水自清洁阻燃棉布的制备方法。
本发明解决技术问题所采用的技术方案为：一种超亲水/油下超亲水自清洁阻燃棉布的制备方法，其特征在于包括有以下步骤：
(1)将棉布浸入含有多元酰氯的有机溶剂溶液中，浸泡1～10分钟后取出进行烘干；
其中，所述有机溶剂溶液中多元酰氯的浓度0.5～5wt％；
(2)将步骤(1)处理后得到的棉布浸入含有四羟甲基氯化磷和胺类化合物的水溶液中，浸泡1～10分钟后取出进行烘干，得到所需的超亲水/油下超亲水自清洁阻燃棉布；
其中，所述水溶液中四羟甲基氯化磷的浓度5～10wt％，胺类化合物的浓度5～10wt％。
上述棉布为棉纤维构成的各种类型的棉织物，表面具有羟基。
优选地，步骤(1)中所述的多元酰氯为均苯三甲酰氯、丁二酰氯、对苯二甲酰氯、间苯二甲酰氯、邻苯二甲酰氯中的至少一种。
优选地，步骤(1)中所述的有机溶剂为四氢呋喃、二氯甲烷、三氯甲烷、己烷、甲苯中的至少一种。
优选地，步骤(2)中所述的胺类化合物为尿素、丁二胺、己二胺、哌嗪中的至少一种。
优选地，步骤(1)和(2)中所述的烘干温度为50～100℃，烘干时间为10～30分钟。
与现有技术相比，本发明的优点在于：采用两步浸渍涂敷工艺，首先使棉布上的羟基和多元酰氯中的酰氯基团反应，即在棉布纤维表面接枝上酰氯基团；然后使棉布上的酰氯与四羟甲基氯化磷中的羟基反应，同时与胺类化合物中的氨基反应。四羟甲基氯化磷具有极强的水化能力，将其修饰到棉布表面，可以直接得到超亲水/油下超亲水自清洁阻燃棉布，被油渍污染的超亲水/油下超亲水自清洁阻燃棉布浸入到水中时，其亲水性会使水潜入到纤维与油层的界面处，潜入的水层会轻而易举地将油污从纤维表面上剥离，从而达到清洁的目的；同时四羟甲基氯化磷又可以作为棉织物的阻燃剂使用，加入胺类化合物形成P-C-N键的网状结构涂层键接在棉纤维表面，具有磷-氮协同阻燃效应。
附图说明
图1为本发明实施例1制得的超亲水/油下超亲水自清洁阻燃棉布和未处理的棉布垂直燃烧后的形貌比较图；
图2为本发明实施例1制得的超亲水/油下超亲水自清洁阻燃棉布的水下自清洁行为图；
图3为本发明实施例制备超亲水/油下超亲水自清洁阻燃棉布的化学方程式。
具体实施方式
以下结合附图实施例对本发明作进一步详细描述。
实施例1：
(1)将棉布浸入含有均苯三甲酰氯的四氢呋喃溶液中，浸泡1分钟后取出，在50℃下加热10分钟进行烘干，其中，四氢呋喃溶液中均苯三甲酰氯的浓度0.5wt％；
(2)将步骤(1)处理后得到的棉布浸入含有四羟甲基氯化磷和尿素的水溶液中，浸泡1分钟后取出，在50℃下加热10分钟进行烘干，即得到所需的超亲水/油下超亲水自清洁阻燃棉布，其中，水溶液中四羟甲基氯化磷的浓度5wt％，尿素的浓度5wt％。
实施例2：
(1)将棉布浸入含有丁二酰氯的二氯甲烷溶液中，浸泡5分钟后取出，在80℃下加热20分钟进行烘干，其中，二氯甲烷溶液中丁二酰氯的浓度2wt％；
(2)将步骤(1)处理后得到的棉布浸入含有四羟甲基氯化磷和丁二胺的水溶液中，浸泡5分钟后取出，在80℃下加热20分钟进行烘干，即得到所需的超亲水/油下超亲水自清洁阻燃棉布，其中，水溶液中四羟甲基氯化磷的浓度8wt％，丁二胺的浓度8wt％。
实施例3：
(1)将棉布浸入含有对苯二甲酰氯的三氯甲烷溶液中，浸泡10分钟后取出，在100℃下加热30分钟进行烘干，其中，三氯甲烷溶液中对苯二甲酰氯的浓度5wt％；
(2)将步骤(1)处理后得到的棉布浸入含有四羟甲基氯化磷和己二胺的水溶液中，浸泡10分钟后取出，在100℃下加热30分钟进行烘干，即得到所需的超亲水/油下超亲水自清洁阻燃棉布，其中，水溶液中四羟甲基氯化磷的浓度10wt％，己二胺的浓度10wt％。
实施例4：
(1)将棉布浸入含有间苯二甲酰氯的己烷溶液中，浸泡1分钟后取出，在50℃下加热10分钟进行烘干，其中，己烷溶液中间苯二甲酰氯的浓度0.5wt％；
(2)将步骤(1)处理后得到的棉布浸入含有四羟甲基氯化磷和哌嗪的水溶液中，浸泡10分钟后取出，在100℃下加热30分钟进行烘干，即得到所需的超亲水/油下超亲水自清洁阻燃棉布，其中，水溶液中四羟甲基氯化磷的浓度10wt％，哌嗪的浓度10wt％。
实施例5：
(1)将棉布浸入含有邻苯二甲酰氯的甲苯溶液中，浸泡10分钟后取出，在100℃下加热30分钟进行烘干，其中，甲苯溶液中邻苯二甲酰氯的浓度5wt％；
(2)将步骤(1)处理后得到的棉布浸入含有四羟甲基氯化磷和尿素的水溶液中，浸泡1分钟后取出，在50℃下加热10分钟进行烘干，即得到所需的超亲水/油下超亲水自清洁阻燃棉布，其中，水溶液中四羟甲基氯化磷的浓度5wt％，尿素的浓度5wt％。
比较例：
将棉布浸入含有均苯三甲酰氯、四羟甲基氯化磷和尿素的四氢呋喃/水混合溶液中，浸泡1分钟后，在50℃下加热10分钟进行烘干，即得到所需的超亲水/油下超亲水自清洁阻燃棉布，其中，水溶液中均苯三甲酰氯的浓度0.5wt％，四羟甲基氯化磷的浓度5wt％，尿素的浓度5wt％。
实验时发现溶液中会有沉淀析出。
将上述所有实施例制得的超亲水/油下超亲水自清洁阻燃棉布和未处理的棉布进行如下测试：
(1)润湿性质测试：采用接触角设备(Dataphysics Instruments GmbH,OCA15EC-TBU100)进行测试，每滴液滴的体积为5μL。
(2)透气性测试：采用标准BS 5'636进行测试。
(3)阻燃性质测试：垂直燃烧按照ASTM D6413标准进行测试；极限氧指数按照ASTMD 2863-09标准进行测试，测试结果如表2所示；
(4)水下自清洁性能测试：将处理后的棉布沾满油污(以食用油为例)，然后浸入水中，稍微晃动后去除。
上述所有实施例制得的超亲水/油下超亲水自清洁阻燃棉布以及未处理的棉布的润湿性质和透气性测试结果如表1所示，阻燃性质测试结果如表2所示；
上述实施例1制得的超亲水/油下超亲水自清洁阻燃棉布和未处理的棉布垂直燃烧后的形貌比较图如图1所示；
上述实施例1制得的超亲水/油下超亲水自清洁阻燃棉布的水下自清洁行为图如图2所示。
由表1～2和图1～2可以看出：
(1)从表1发现，未处理的棉布具有水下超疏油的性质，但是其油下也是超疏水的，实施例1～5制得的超亲水/油下超亲水自清洁阻燃棉布具有超亲水的性质，其水下是超疏油的，但是其油下是超亲水的，说明其亲水性要比亲油性好，同时处理后的棉布其透气性不受影响；
(2)从表2和图1发现，处理后的棉布具有非常好的阻燃性质，其在空气中无法续燃；
(3)从图2发现，被油渍污染的超亲水/油下超亲水自清洁阻燃棉布浸入到水中时，油污逐渐从纤维表面上剥离，从而达到清洁的目的。
本发明的工作原理如下：如图3所示，采用两步浸渍涂敷工艺，首先使棉布上的羟基和多元酰氯中的酰氯基团反应，即在棉布纤维表面接枝上酰氯基团；然后使棉布上的酰氯与四羟甲基氯化磷中的羟基反应，同时与胺类化合物中的氨基反应，四羟甲基氯化磷具有极强的水化能力，将其修饰到棉布表面，可以直接得到超亲水/油下超亲水自清洁阻燃棉布，被油渍污染的超亲水/油下超亲水自清洁阻燃棉布浸入到水中时，其亲水性会使水潜入到纤维与油层的界面处，潜入的水层会轻而易举地将油污从纤维表面上剥离，从而达到清洁的目的；同时四羟甲基氯化磷又可以作为棉织物的阻燃剂使用，加入胺类化合物形成P-C-N键的网状结构涂层键接在棉纤维表面，具有磷-氮协同阻燃效应。
表1所有实施例制得的超亲水/油下超亲水自清洁阻燃棉布以及未处理的棉布的润湿性质和透气性测试结果
表2所有实施例制得的超亲水/油下超亲水自清洁阻燃棉布以及未处理的棉布的阻燃性质测试结果
| 极限氧指数LOI | 损毁长度 | 续燃时间 | |
| 实施例2 | 39.5％ | 8.5cm | 无续燃 |
| 空白 | 19.3％ | 烧通 | 20s |
Claims (3)
1.一种超亲水自清洁阻燃棉布的制备方法，其特征在于包括有以下步骤：
(1)将棉布浸入含有多元酰氯的有机溶剂溶液中，浸泡1～10分钟后取出进行烘干；
其中，所述有机溶剂溶液中多元酰氯的浓度0.5～5wt％；
(2)将步骤(1)处理后得到的棉布浸入含有四羟甲基氯化磷和胺类化合物的水溶液中，浸泡1～10分钟后取出进行烘干，得到所需的超亲水自清洁阻燃棉布；
其中，所述水溶液中四羟甲基氯化磷的浓度5～10wt％，胺类化合物的浓度5～10wt％；
步骤(1)中所述的多元酰氯为均苯三甲酰氯、丁二酰氯、对苯二甲酰氯、间苯二甲酰氯、邻苯二甲酰氯中的至少一种；
步骤(2)中所述的胺类化合物为尿素、丁二胺、己二胺、哌嗪中的至少一种。
2.根据权利要求1所述的制备方法，其特征在于：步骤(1)中所述的有机溶剂为四氢呋喃、二氯甲烷、三氯甲烷、己烷、甲苯中的至少一种。
3.根据权利要求1所述的制备方法，其特征在于：步骤(1)和(2)中所述的烘干温度为50～100℃，烘干时间为10～30分钟。
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