CN114672990B - 一种阻燃棉织物的制备方法 - Google Patents
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Abstract
本发明公开了一种阻燃棉织物的制备方法，涉及生物质材料阻燃技术领域，包括如下步骤：(1)聚磷酸铵‑氢氧化铝复合物的制备；(2)阻燃剂溶液的配制；(3)棉织物的前处理；(4)棉织物的浸渍阻燃处理。本发明提供了一种阻燃棉织物的制备方法，与现有的技术相比，工艺简便，使用的阻燃抑烟剂种类少、添加量小，处理成本较低，对棉织物的阻燃效率高，并且在提高棉织物阻燃性的同时，对织物其他性能的影响较小，从而提高了棉织物的应用范围，通过本申请方法制备的阻燃棉织物适用于家具、室内建筑装潢装饰等对阻燃要求严格的领域。
Description
技术领域
本发明属于生物质材料阻燃技术领域，具体涉及一种阻燃棉织物的制备方法。
背景技术
棉纤维作为一种常见的天然纤维，已有几千年的应用历史，由其加工生产的纺织品具有手感柔软、透气吸湿以及保暖耐磨等特点，从而广泛受到服装服饰，汽车装饰和室内家居等行业青睐。然而，棉织物的极限氧指数(LOI)仅为18％左右，在空气中遇见明火会发生剧烈燃烧，属于一种常见的易燃材料严重限制了阻燃棉纤维的应用。并且随着人们生活和消费水平的不断提高，消费者对纺织品的要求越来越高，阻燃性能作为纺织品一项重要的安全性指标受到了越来越多的关注。目前用于纤维素的无卤阻燃剂主要包括膦酸盐类阻燃剂、磷-氮阻燃剂、磷-硅阻燃剂及其它阻燃剂。其中，磷-氮阻燃剂因具有较高的阻燃效率和较优的性价比而广泛应用于棉织物的阻燃。制备阻燃棉织物的方法有轧烘固化、溶胶-凝胶、逐层装配及纳米吸附等，其中大多通过物理吸附或形成弱共价键将阻燃剂引入棉织物，制备的阻燃棉织物大多存在耐水洗性能差的缺点。因此，开发具有优良效果的阻燃剂并应用于棉织物整理具有现实意义。
发明内容
本发明的目的是针对现有的问题，提供了一种阻燃棉织物的制备方法。
本发明是通过以下技术方案实现的：
一种阻燃棉织物的制备方法，包括如下步骤：
(1)聚磷酸铵-氢氧化铝复合物的制备：
1)将50g聚磷酸铵加入乙醇中形成悬浮液，转移到装有搅拌磁子和冷凝管的三口烧瓶中；
2)用10mL去离子水溶解2.00g无水氯化铝粉末，缓慢加入烧瓶中，搅拌20min至完全均匀；
3)缓慢加入5mL氨水继续搅拌直至溶液pH值为8，60℃恒温水浴状态下静置沉淀2h；
4)将沉淀产物进行抽滤、洗涤，烘干之后粉碎成粉末；
(2)阻燃剂溶液的配制：
称取相应重量份的步骤(1)制得的聚磷酸铵-氢氧化铝复合物0.1～1.5份、硅溶胶20～50份、磷酸丙基脲0.1～1份、滑石粉0.5～5份混合、搅拌均匀得阻燃剂溶液；
(3)棉织物的前处理：
将棉织物用大量去离子水洗涤3次，室温下晾干，以除去棉织物在加工过程中附着在表面的染料及各种助剂，将棉织物裁剪成10cm×10cm大小，烘干，称量绝干质量；
(4)棉织物的浸渍阻燃处理：
将步骤(3)前处理后的棉织物放入处理盒，向处理盒中倒入步骤(2)所得的阻燃剂溶液直至将棉织物淹没，将棉织物浸泡30分钟后取出，自然风干后放入烘箱，在50℃下烘干至绝干，取出后称量其质量。
进一步地，步骤(2)中所述的硅溶胶质量分数为20％。
本发明相比现有技术具有以下优点：
本发明提供了一种阻燃棉织物的制备方法，与现有的技术相比，工艺简便，使用的阻燃抑烟剂种类少、添加量小，处理成本较低，对棉织物的阻燃效率高，并且在提高棉织物阻燃性的同时，对织物其他性能的影响较小，从而提高了棉织物的应用范围，通过本申请方法制备的阻燃棉织物适用于家具、室内建筑装潢装饰等对阻燃要求严格的领域。
附图说明
图1为具体实施方式部分实施例1电镜图；
图2为具体实施方式部分实施例2电镜图；
图3为具体实施方式部分实施例3电镜图；
图4为具体实施方式部分实施例4电镜图；
图5为具体实施方式部分比较例1电镜图；
图6为具体实施方式部分比较例2电镜图。
具体实施方式
下面结合具体实施例做进一步的说明，本发明的范围不受这些实施例的限制。
实施例1：
一种阻燃棉织物的制备方法，包括如下步骤：
(1)聚磷酸铵-氢氧化铝复合物的制备：
1)将50g聚磷酸铵加入乙醇中形成悬浮液，转移到装有搅拌磁子和冷凝管的三口烧瓶中；
2)用10mL去离子水溶解2.00g无水氯化铝粉末，缓慢加入烧瓶中，搅拌20min至完全均匀；
3)缓慢加入5mL氨水继续搅拌直至溶液pH值为8，60℃恒温水浴状态下静置沉淀2h；
4)将沉淀产物进行抽滤、洗涤，烘干之后粉碎成粉末；
(2)阻燃剂溶液的配制：
称取相应重量份的步骤(1)制得的聚磷酸铵-氢氧化铝复合物0.9份、硅溶胶45份、磷酸丙基脲0.5份、滑石粉2.5份混合、搅拌均匀得阻燃剂溶液；
(3)棉织物的前处理：
将棉织物用大量去离子水洗涤3次，室温下晾干，以除去棉织物在加工过程中附着在表面的染料及各种助剂，将棉织物裁剪成10cm×10cm大小，烘干，称量绝干质量；
(4)棉织物的浸渍阻燃处理：
将步骤(3)前处理后的棉织物放入处理盒，向处理盒中倒入步骤(2)所得的阻燃剂溶液直至将棉织物淹没，将棉织物浸泡30分钟后取出，自然风干后放入烘箱，在50℃下烘干至绝干，取出后称量其质量。
步骤(2)中硅溶胶质量分数为20％。
实施例2：
本实施例2与实施例1不同的是在阻燃剂溶液的配制中添加的聚磷酸铵-氢氧化铝复合物，质量份数为0.675份，本实施例2制备方法如实施例1。
实施例3：
本实施例3与实施例1不同的是在阻燃剂溶液的配制中添加的聚磷酸铵-氢氧化铝复合物，质量份数为0.45份，本实施例3制备方法如实施例1。
实施例4：
本实施例4与实施例1不同的是在阻燃剂溶液的配制中添加的聚磷酸铵-氢氧化铝复合物，质量份数为0.225份，本实施例4制备方法如实施例1。
比较例1：
本比较例1与实施例1不同的是不进行棉织物的浸渍阻燃处理，本比较例1制备方法如实施例1。
比较例2：
本比较例2与实施例1不同的是将阻燃剂溶液替换成硅溶胶，本比较例2制备方法如实施例1。
效果分析：
对上述实施例与比较例制备得到的阻燃棉织物采用性能检测。阻燃性能检测结果如表1。
表1性能检测结果
由表1中的数据结果可以看出，本发明选用的聚磷酸铵-氢氧化铝复合物和硅溶胶为有效的协同阻燃剂，按照合适比例用于阻燃剂溶液的配制，可显著提升棉织物的阻燃效果。
具体的：
1、单一硅溶胶处理棉织物的阻燃效果分析：
从表1可以得出，比较例2与比较例1相比，比较例2中织物点燃时间提高，但是燃烧时间下降，比较例1的残炭率为18％；而比较例2残炭率为40％，并未燃烧充分，说明硅溶胶有一定的阻燃作用。
同比较例1相比，比较例2中织物燃烧速率(即燃烧时每秒消耗的物质的质量)提高，说明硅溶胶对织物的阻燃性主要体现在其可以使织物燃烧后成炭，但并不能显著降低火焰传播速率以及有效阻止织物燃烧，可见硅溶胶的阻燃效果并不显著，且存在一定缺陷。
从微观图中可分析得出，由比较例1电镜图可以清晰地看出，未处理的棉织物纤维根根分离；由比较例2电镜图可看出，由硅溶胶处理过的棉织物纤维通过硅溶胶连接在一起，使硅溶胶处理的棉织物燃烧后成炭。
2、复合阻燃剂处理棉织物的阻燃效果分析：
从表1可以得出，同比较例1相比，实施例1～4中织物点燃时间和燃烧时间均延长，残炭率却提高，通过定性的分析可知，织物的燃烧速率下降，定量的计算后更加能够看出织物燃烧速率下降。同比较例2相比，实施例1～4中织物燃烧时间大大提高，同时也形成了完整的成炭物，残炭率增加，通过定性的分析可知，织物的燃烧速率下降，定量的计算后更加能够看出织物燃烧速率大大下降。因此，可以看出复合阻燃剂的阻燃效果较为显著。
从微观图中可分析得，实施例1～4中的复合阻燃剂大量地附着在棉织物纤维表面及纤维之间，以达到阻燃效果。单一的硅溶胶阻燃剂及无机物阻燃剂都无法达到此种效果，原因是，单一的硅溶胶阻燃剂阻燃效果不强，而单一的无机物阻燃剂无法很好地固着在棉织物纤维上。本发明所制得的复合阻燃剂综合了所含的各种物质成分的优点，各物质间由有协同作用，起到良好的阻燃作用，且能够掩盖单一阻燃剂的不足。
Claims (2)
1.一种阻燃棉织物的制备方法，其特征在于，包括如下步骤：
(1)聚磷酸铵-氢氧化铝复合物的制备：
1)将50g聚磷酸铵加入乙醇中形成悬浮液，转移到装有搅拌磁子和冷凝管的三口烧瓶中；
2)用10mL去离子水溶解2.00g无水氯化铝粉末，缓慢加入烧瓶中，搅拌20min至完全均匀；
3)缓慢加入5mL氨水继续搅拌直至溶液pH值为8，60℃恒温水浴状态下静置沉淀2h；
4)将沉淀产物进行抽滤、洗涤，烘干之后粉碎成粉末；
(2)阻燃剂溶液的配制：
称取相应重量份的步骤(1)制得的聚磷酸铵-氢氧化铝复合物0.1～1.5份、硅溶胶20～50份、磷酸丙基脲0.1～1份、滑石粉0.5～5份混合、搅拌均匀得阻燃剂溶液；
(3)棉织物的前处理：
将棉织物用大量去离子水洗涤3次，室温下晾干，将棉织物裁剪成10cm×10cm大小，烘干，称量绝干质量；
(4)棉织物的浸渍阻燃处理：
将步骤(3)前处理后的棉织物放入处理盒，向处理盒中倒入步骤(2)所得的阻燃剂溶液直至将棉织物淹没，将棉织物浸泡30分钟后取出，自然风干后放入烘箱，在50℃下烘干至绝干，取出后称量其质量。
2.根据权利要求1所述一种阻燃棉织物的制备方法，其特征在于，步骤(2)中所述的硅溶胶质量分数为20％。
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| CN106436285A (zh) * | 2016-07-28 | 2017-02-22 | 东华大学 | 一种膨胀阻燃体系掺杂硅溶胶的制备及其应用 |
| CN113322676A (zh) * | 2021-05-27 | 2021-08-31 | 安徽工程大学 | 一种生物质基环保耐洗阻燃剂pd阻燃整理织物及其制备方法 |
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| CN106436285A (zh) * | 2016-07-28 | 2017-02-22 | 东华大学 | 一种膨胀阻燃体系掺杂硅溶胶的制备及其应用 |
| CN113322676A (zh) * | 2021-05-27 | 2021-08-31 | 安徽工程大学 | 一种生物质基环保耐洗阻燃剂pd阻燃整理织物及其制备方法 |
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