CN114716472A - 一种纺织涂层阻燃剂及其制备方法和应用 - Google Patents

一种纺织涂层阻燃剂及其制备方法和应用 Download PDF

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CN114716472A
CN114716472A CN202210367527.2A CN202210367527A CN114716472A CN 114716472 A CN114716472 A CN 114716472A CN 202210367527 A CN202210367527 A CN 202210367527A CN 114716472 A CN114716472 A CN 114716472A
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piperazine
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韩明序
韩忠山
杨松慧
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Qingdao Changrong Chemical Technology Co ltd
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Abstract

本发明属于阻燃剂技术领域，具体为一种纺织涂层阻燃剂及其制备方法和应用，其特征在于所述的阻燃剂为一种以焦烷基膦酸为基础的膨胀阻燃剂的制备方法。以焦甲基膦酸为原料，与含氮化合物反应成盐，得到含有磷氮及碳源的膨胀型阻燃剂，其结构式为：

Description

一种纺织涂层阻燃剂及其制备方法和应用
技术领域
本发明属于阻燃剂技术领域，具体涉及一种纺织涂层阻燃剂及其制备方法和应用。
背景技术
随着社会经济的发展，降低材料的易燃性越来越收到社会的关注。纺织材料多是由天然纤维、棉、还有涤纶腈纶等有机材料制成，而此等材料都属于易燃品。在可燃性材料上涂阻燃涂层是一种有效的防火保护措施，因此阻燃涂层目前得到了较为广泛的应用。但是涂层本身的材料，例如丙烯酸，聚氨酯，环氧树脂等，均属于易燃材料。而对涂层采取有效的阻燃处理，是当今研究的重点问题之一。
中国专利CN112300695A采取碳化硅与稀土等无机材料研磨成粉末与涂层混拌达到阻燃的功效。中国专利CN105694543A采取无机成膜物质与无机材料填充物制备成膜涂层。此类无机阻燃剂普遍存在添加量大，阻燃效率低等缺点。
目前用于涂层上的液体阻燃剂主要是环状结构的膦酸酯。此阻燃剂磷含量高，水溶性好，并且稳定性佳，通常情况下不会与涂层乳液反正副反应导致破乳等情况的发生。但在一些阻燃要求高的应用领域，过高的添加量会影响涂层的粘接力，影响使用效果。
因此就目前而且还没有一种非常高效的乳液用阻燃剂，可以克服目前所有应用端的问题。在环保要求下的无卤趋势的影响下，磷氮系阻燃体越来越受到关注。磷氮系阻燃剂主要靠三元素即酸元、气元、碳元结合在燃烧时形成致密的碳层，阻断火焰的进一步蔓延并且将可燃物用碳层保护覆盖，阻止进一步的燃烧。最理想的乳液涂层阻燃剂是由磷，氮，碳元，三种元素组成。目前市面上的阻燃成炭剂主要由日本艾迪科公司的焦磷酸哌嗪体系为主导，但由于焦磷酸哌嗪的焦磷酸上含有两个未被成盐的磷羟基。此结构对乳液的影响非常大，例如焦磷酸哌嗪在丙烯酸乳液中，乳液立刻出现破乳的情况，导致无法使用。所以此体系目前只用于工程塑料中。
Figure BDA0003586504930000011
式：焦磷酸哌嗪结构
哌嗪含有氮和丰富的碳元素，非常适合作为气源与碳源同时使用。而本发明通过使用烷基焦磷酸为酸元，烷基焦磷酸只存在两个磷羟基，可以与大部分胺基化合物完全成盐，成为中性物质。与此同时，烷基磷酸结构稳定，耐热性远高于普通的焦磷酸结构。由烷基焦磷酸与有机胺类化合物形成的膦酸盐是一种高效的乳液及涂层阻燃剂。
发明内容
一种纺织涂层阻燃剂及其制备方法和应用具体为一种以焦烷基膦酸为基础的膨胀型阻燃剂，其结构为以下的膦酸盐结构：
Figure BDA0003586504930000021
其中R1为C1–C4的烷基，R2为满足条件的C1–C8的任何集团，R3为氢原子或不存在。R4为氨基官能基团或不存在。
焦烷基膦酸的膦酸盐，其制备方法包括以下步骤：
将烷基膦酸用惰性气体氮气保护，在100–200℃下脱水缩合，形成烷基焦磷酸结构，加入有含氮的氨基化合物，以水为溶剂，将两者混合反应成盐沉淀。沉淀物后经去离子水洗涤烘干，得到含氮的焦烷基酸盐。水溶液可重复利用。
所述的烷基膦酸选自以下合物的一种或多种：甲基膦酸，乙基膦酸，丙基膦酸，丁基膦酸。优选甲基膦酸。
所述的含氮氨基化合物选自但不限于以下合物的一种或多种：乙二胺，二异丙胺，1,2-丙二胺，三聚氰胺，1,3,5三嗪，哌嗪。其中优选哌嗪。
一种阻燃纺织涂层组合物，包含(i)胶黏剂和(ii)根据权利要求1所述的阻燃剂还包括(iii)选自其他阻燃剂、增效剂和阻燃助剂的一种或多种化合物。所述的胶黏剂包括但不限于：丙烯酸乳液，醋丙乳液，水性聚氨酯，水性环氧树脂。
所述的其他阻燃剂、增效剂和阻燃助剂的一种或多种化合物包括但不限于：环状膦酸酯、三聚氰胺、三聚氰胺氰脲酸盐、三聚氰胺聚磷酸盐、聚磷酸铵盐、次磷酸铝、二乙基次磷酸铝、焦磷酸哌嗪、氢氧化铝、氢氧化镁、硼酸锌、氧化锌、氧化铝、蒙脱土、十溴二苯乙烷、十溴二苯醚、溴代三嗪、三氧化二锑、硅氧烷、磷酸镐。
具体实施方式
以下实施例进一步说明。
实施例1：焦甲基膦酸哌嗪
Figure BDA0003586504930000031
使用磁力搅拌导热油锅，500ml的三口瓶中，通入氮气隔绝空气，加入192g甲基膦酸(2 mole)，加热到200度，真空负压使甲基膦酸分子间脱水成焦膦酸状态。大约5小时后得到质量175g 的焦甲基膦酸。将86g的哌嗪(1mole)溶解于300g的水，将哌嗪水溶液缓慢滴加入焦甲基膦酸中，滴加完毕后温至150度保温2小时后冷却降温至室温。过滤出沉淀物257g。用去离子水洗涤两遍即为产物焦甲基膦酸哌嗪。
应用实例：
5份水性涂层试验的成分如下表：
Figure BDA0003586504930000032

Claims (10)

1.一种纺织涂层阻燃剂及其制备方法和应用，其特征在于所述为一种以焦烷基膦酸为基础的膨胀型阻燃剂及其制备方法和应用，其结构为以下的膦酸盐结构：
Figure FDA0003586504920000011
其中R1为C1-C4的烷基，R2为满足条件的C1-C8的任何集团，R3为氢原子或不存在。R4为氨基官能基团或不存在。
2.根据权利要求1所述的焦烷基膦酸的膦酸盐，其制备方法包括以下步骤：
将烷基膦酸用惰性气体氮气保护，在100-200℃下脱水缩合，形成烷基焦磷酸结构，加入有含氮的氨基化合物，以水为溶剂，将两者混合反应成盐沉淀。沉淀物后经去离子水洗涤烘干，得到含氮的焦烷基酸盐。水溶液可重复利用。
3.根据权利要求2所述的制备方法，其特征在于：所述的烷基膦酸选自以下合物的一种或多种：甲基膦酸，乙基膦酸，丙基膦酸，丁基膦酸。
4.根据权利要求2所述的制备方法，其特征在于：优选甲基膦酸。
5.根据权利要求2所述的制备方法，其特征在于：所述的含氮氨基化合物选自但不限于以下合物的一种或多种：乙二胺，二异丙胺，1，2-丙二胺，三聚氰胺，1，3，5三嗪，哌嗪。
6.根据权利要求1或2或5所述的制备方法，其特征在于含氮化合物优选哌嗪。
7.根据权利要求2所述的制备方法，其特征在于：反应在惰性气体保护下进行。
8.一种阻燃纺织涂层组合物，包含(i)胶黏剂和(ii)根据权利要求1所述的阻燃剂还包括(iii)选自其他阻燃剂、增效剂和阻燃助剂的一种或多种化合物。
9.根据权利要求8所述的纺织涂层组合物，所述的胶黏剂包括但不限于：丙烯酸乳液，醋丙乳液，水性聚氨酯，水性环氧树脂。
10.根据权利要求8所述的纺织涂层组合物，所述的其他阻燃剂、增效剂和阻燃助剂的一种或多种化合物包括但不限于：环状膦酸酯、三聚氰胺、三聚氰胺氰脲酸盐、三聚氰胺聚磷酸盐、聚磷酸铵盐、次磷酸铝、二乙基次磷酸铝、焦磷酸哌嗪、氢氧化铝、氢氧化镁、硼酸锌、氧化锌、氧化铝、蒙脱土、十溴二苯乙烷、十溴二苯醚、溴代三嗪、三氧化二锑、硅氧烷、磷酸镐。
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US20160281001A1 (en) * 2013-09-17 2016-09-29 Thor Gmbh Flame retardant composition
CN113166426A (zh) * 2018-12-20 2021-07-23 朗盛公司 含磷阻燃剂的制备方法及其在聚合物组合物中的用途
CN114015115A (zh) * 2021-10-25 2022-02-08 沈阳工业大学 一种基于焦磷酸哌嗪/三聚氰胺氰尿酸盐/聚磷酸铵的膨胀型阻燃剂的制备方法

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US20160281001A1 (en) * 2013-09-17 2016-09-29 Thor Gmbh Flame retardant composition
CN113166426A (zh) * 2018-12-20 2021-07-23 朗盛公司 含磷阻燃剂的制备方法及其在聚合物组合物中的用途
CN114015115A (zh) * 2021-10-25 2022-02-08 沈阳工业大学 一种基于焦磷酸哌嗪/三聚氰胺氰尿酸盐/聚磷酸铵的膨胀型阻燃剂的制备方法

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