CN112267297A - 一种阻燃无纺布及其加工工艺 - Google Patents

一种阻燃无纺布及其加工工艺 Download PDF

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CN112267297A
CN112267297A CN202011110179.8A CN202011110179A CN112267297A CN 112267297 A CN112267297 A CN 112267297A CN 202011110179 A CN202011110179 A CN 202011110179A CN 112267297 A CN112267297 A CN 112267297A
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flame
retardant
parts
woven fabric
finishing liquid
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CN112267297B (zh
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高建奇
施钦胡
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Wenzhou Fuchi Non Woven Packaging Co ltd
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Wenzhou Fuchi Non Woven Packaging Co ltd
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Abstract

本申请涉及无纺布的领域，公开了一种阻燃无纺布及其加工工艺。一种阻燃无纺布，无纺布由阻燃整理液整理，所述阻燃整理液包括如下重量份数的原料：30‑40份磷酸三(异丙基苯)酯；5‑8份甲醚化六羟甲基三聚氰胺树脂；2‑3份三氧化二锑；加工工艺为：S1.阻燃整理液的制备；S2.无纺布的阻燃整理；本申请具有以下优点和效果：磷酸三(异丙基苯)酯可在聚合物燃烧过程中抑制活性较大的HO•的链锁反应，三氧化二锑在阻燃过程中可释放气体达到阻燃目的；甲醚化六羟甲基三聚氰胺树脂作为助剂，和磷酸三(异丙基苯)酯混合得到的产物可提升阻燃效果，并可提升三氧化二锑的分散性，采用该阻燃整理液整理无纺布，获得阻燃性能较好的阻燃无纺布。

Description

一种阻燃无纺布及其加工工艺
技术领域
本申请涉及无纺布的技术领域，尤其是涉及一种阻燃无纺布及其加工工艺。
背景技术
无纺布又称不织布，是由定向的或随机的纤维而构成，因具有布的外观和某些性能而称其为布；无纺布具有防潮、透气、柔韧、质轻、容易分解、无毒无刺激性、色彩丰富、价格低廉、可循环再用等特点；如多采用聚丙烯(pp材质)粒料为原料，经高温熔融、喷丝、铺纲、热压卷取连续一步法生产而成。
而目前市场上的无纺布采用的聚丙烯原料为碳氢类材料，较易于造成燃烧，无法满足安全防火的需要。
发明内容
为了降低无纺布的易燃性，满足安全防火需求，本申请提供一种阻燃无纺布及其加工工艺。
第一方面，本申请提供一种阻燃无纺布，采用如下技术方案：
一种阻燃无纺布，所述无纺布由阻燃整理液整理，所述阻燃整理液包括如下重量份数的原料：
30-40份磷酸三(异丙基苯)酯；
5-8份甲醚化六羟甲基三聚氰胺树脂；
2-3份三氧化二锑。
通过采用上述技术方案，添加具有捕获自由基HO·的作用的磷酸三(异丙基苯)酯，可在聚合物燃烧过程中抑制活性较大的HO·的链锁反应，从而达到阻燃目的；甲醚化六羟甲基三聚氰胺树脂作为助剂，和磷酸三(异丙基苯)酯混合得到的产物可提升阻燃效果；三氧化二锑在阻燃过程中会产生锑的氮氧化物，通过释放气体达到阻燃目的，甲醚化六羟甲基三聚氰胺树脂和三氧化二锑混合，提高三氧化二锑的分散性，使组分间相容性得到提升，提高阻燃性；采用该阻燃整理液整理无纺布，获得阻燃性能较好的阻燃无纺布，满足安全防火需求。
优选的：按重量份数计，所述原料还包括3-4份改性聚亚苯醚树脂。
通过采用上述技术方案，改性聚亚苯醚树脂含有多芳环结构和醚键，成炭指数高并具有良好的阻燃性；且改性聚亚苯醚树脂与磷酸三(异丙基苯)酯之间可产生协同作用，磷酸酯化合物可有效促进的改性聚亚苯醚树脂的成炭作用，从而可使材料表面形成致密炭层，隔绝材料与氧和热的接触，达到更好的阻燃效果。
优选的：按重量份数计，所述原料还包括1-2份液体丁腈橡胶。
通过采用上述技术方案，液体丁腈橡胶具有的腈基基团作为反应性官能团，可与改性聚亚苯醚树脂在80-90℃条件下发生化学反应，从而在聚合物界面上形成起过渡作用的新结构，和阻燃液各组分混合后，可增进阻燃整理液共混组分间的相容性和联结紧密度，由此得到具有更优异的阻燃性能的产物，提升阻燃效果；且液体丁腈橡胶的添加可提升共混物的物理性能，有利于获得阻燃性能更持久的阻燃整理液。
优选的：按重量份数计，所述原料还包括2-3份聚乙烯蜡和1-2份苯甲酸苄酯。
通过采用上述技术方案，聚乙烯蜡和苯甲酸苄酯混合后得到的复合物可提高阻燃剂各组分的相容性，从而辅助提升阻燃剂的阻燃效果。
优选的：按重量份数计，所述原料还包括2-3份聚乙烯醇缩丁醛。
通过采用上述技术方案，通常采用阻燃整理液处理的无纺布的力学性能接近未经处理的无纺布，其原因在于，阻燃整理液通过吸附作用附着于无纺布上，因此不影响无纺布的力学性能，但也无法对此进行提升；而本申请中，通过具有较强附着力的聚乙烯醇缩丁醛的添加，甲醚化六羟甲基三聚氰胺树脂具有交联剂的效果，在甲醚化六羟甲基三聚氰胺树脂的存在下，聚乙烯醇缩丁醛可与磷酸三(异丙基苯)酯产生交联，从而使阻燃整理液吸附于无纺布上的同时还可填充于无纺布的孔隙中，获得更好的阻燃效果的同时，又可在一定程度上提升无纺布的力学性能。
优选的：按重量份数计，所述原料还包括0.6-0.8份乙二胺。
通过采用上述技术方案，乙二胺和聚乙烯醇缩丁醛共混可发生加成反应，得到的加成产物可提升与磷酸三(异丙基苯)酯间的交联反应速率，且混合产物有助于提升阻燃整理液的阻燃性。
第二方面，本申请提供一种阻燃无纺布的加工工艺，采用如下技术方案：
一种阻燃无纺布的加工工艺，包括以下步骤：
S1.阻燃整理液的制备；称取所需组分，将甲醚化六羟甲基三聚氰胺树脂和三氧化二锑混合并搅拌3-5min，再加入磷酸三(异丙基苯)酯，升温至105-115℃，搅拌30-40min，冷却至室温，得到阻燃整理液；
S2.无纺布的阻燃整理；将无纺布浸泡于S1得到的阻燃整理液中静置10-20min；将浸泡过的无纺布置于压辊机的两个橡胶压辊之间，挤压除去多余液体；将阻燃整理后的无纺布在100-110℃下烘干，得到阻燃无纺布。
优选的：所述S1中，将5-8份甲醚化六羟甲基三聚氰胺树脂、2-3份三氧化二锑、2-3份聚乙烯蜡和1-2份苯甲酸苄酯混合并搅拌3-5min；然后添加2-3份聚乙烯醇缩丁醛和0.6-0.8份乙二胺在30-35℃下搅拌反应8-10min后的产物；再继续加入30-40份磷酸三(异丙基苯)酯，升温至105-115℃，搅拌反应30-40min；最后加入3-4份改性聚亚苯醚树脂和1-2份液体丁腈橡胶在80-90℃下搅拌反应40-60min的产物，再继续搅拌0.5-1h，冷却至室温，得到阻燃整理液。
综上所述，本申请具有以下有益效果：
1.磷酸三(异丙基苯)酯可在聚合物燃烧过程中抑制活性较大的HO·的链锁反应，三氧化二锑在阻燃过程中可释放气体达到阻燃目的；甲醚化六羟甲基三聚氰胺树脂作为助剂，和磷酸三(异丙基苯)酯混合得到的产物可提升阻燃效果，并可提升三氧化二锑的分散性，采用该阻燃整理液整理无纺布，获得阻燃性能较好的阻燃无纺布；
2.本申请中优选采用改性聚亚苯醚树脂，可与磷酸三(异丙基苯)酯之间产生协同作用，磷酸酯化合物可有效促进的改性聚亚苯醚树脂的成炭作用，从而可使材料表面形成致密炭层，隔绝材料与氧和热的接触，达到更好的阻燃效果；
3.液体丁腈橡胶具有的腈基基团作为反应性官能团，可与改性聚亚苯醚树脂在80-90℃条件下发生化学反应，从而在聚合物界面上形成起过渡作用的新结构，和阻燃液各组分混合后，可增进阻燃整理液共混组分间的相容性和联结紧密度，由此得到具有更优异的阻燃性能的产物，提升阻燃效果；且液体丁腈橡胶的添加可提升共混物的物理性能，有利于获得阻燃性能更持久的阻燃整理液；
4.聚乙烯蜡和苯甲酸苄酯混合后得到的复合物可提高阻燃剂各组分的相容性，从而辅助提升阻燃剂的阻燃效果；
5.在甲醚化六羟甲基三聚氰胺树脂的存在下，聚乙烯醇缩丁醛可与磷酸三(异丙基苯)酯产生交联，从而使阻燃整理液吸附于无纺布上的同时还可填充于无纺布的孔隙中，获得更好的阻燃效果的同时，又可在一定程度上提升无纺布的力学性能；
6.乙二胺和聚乙烯醇缩丁醛共混可发生加成反应，得到的加成产物可提升与磷酸三(异丙基苯)酯间的交联反应速率。
具体实施方式
以下结合实施例对本申请作进一步详细说明。
本申请中，甲醚化六羟甲基三聚氰胺树脂购于上海慈太龙实业有限公司；改性聚亚苯醚树脂购于上海誉宇新材料科技有限公司；聚乙烯醇缩丁醛购于上海邦成化工有限公司。
以下实施方式中所用原料除特殊说明外均可来源于普通市售。
根据实施例4的反应条件，将乙二胺和聚乙烯醇缩丁醛的加成产物与磷酸三(异丙基苯)酯反应，通过31PNMR核磁共振谱中P-O-P的化学位移证明了交联反应的发生。
实施例
实施例1
本申请公开了一种阻燃无纺布及其加工工艺，无纺布由阻燃整理液整理，阻燃整理液包括如下原料：磷酸三(异丙基苯)酯、甲醚化六羟甲基三聚氰胺树脂和三氧化二锑；加工工艺包括以下步骤：
S1.阻燃整理液的制备；称取所需组分，将甲醚化六羟甲基三聚氰胺树脂和三氧化二锑混合并搅拌3min，再加入磷酸三(异丙基苯)酯，升温至105℃，搅拌30min，冷却至室温，得到阻燃整理液；
S2.无纺布的阻燃整理；将无纺布浸泡于S1得到的阻燃整理液中静置10min；将浸泡过的无纺布置于压辊机的两个橡胶压辊之间，挤压除去多余液体；将阻燃整理后的无纺布在100℃下烘干，得到阻燃无纺布。
各组分含量如下表1所示。
实施例2
本申请公开了一种阻燃无纺布及其加工工艺，无纺布由阻燃整理液整理，阻燃整理液包括如下原料：磷酸三(异丙基苯)酯、甲醚化六羟甲基三聚氰胺树脂和三氧化二锑；加工工艺包括以下步骤：
S1.阻燃整理液的制备；称取所需组分，将甲醚化六羟甲基三聚氰胺树脂和三氧化二锑混合并搅拌5min，再加入磷酸三(异丙基苯)酯，升温至115℃，搅拌40min，冷却至室温，得到阻燃整理液；
S2.无纺布的阻燃整理；将无纺布浸泡于S1得到的阻燃整理液中静置20min；将浸泡过的无纺布置于压辊机的两个橡胶压辊之间，挤压除去多余液体；将阻燃整理后的无纺布在110℃下烘干，得到阻燃无纺布。
各组分含量如下表1所示。
实施例3
本申请公开了一种阻燃无纺布及其加工工艺，无纺布由阻燃整理液整理，阻燃整理液包括如下原料：磷酸三(异丙基苯)酯、甲醚化六羟甲基三聚氰胺树脂和三氧化二锑；加工工艺包括以下步骤：
S1.阻燃整理液的制备；称取所需组分，将甲醚化六羟甲基三聚氰胺树脂和三氧化二锑混合并搅拌4min，再加入磷酸三(异丙基苯)酯，升温至110℃，搅拌35min，冷却至室温，得到阻燃整理液；
S2.无纺布的阻燃整理；将无纺布浸泡于S1得到的阻燃整理液中静置15min；将浸泡过的无纺布置于压辊机的两个橡胶压辊之间，挤压除去多余液体；将阻燃整理后的无纺布在105℃下烘干，得到阻燃无纺布。
各组分含量如下表1所示。
实施例4
本申请公开了一种阻燃无纺布及其加工工艺，无纺布由阻燃整理液整理，阻燃整理液包括如下原料：磷酸三(异丙基苯)酯、甲醚化六羟甲基三聚氰胺树脂、三氧化二锑、改性聚亚苯醚树脂、液体丁腈橡胶、聚乙烯蜡、苯甲酸苄酯、聚乙烯醇缩丁醛和乙二胺；加工工艺包括以下步骤：
S1.阻燃整理液的制备；将甲醚化六羟甲基三聚氰胺树脂、三氧化二锑、聚乙烯蜡和苯甲酸苄酯混合并搅拌3min；然后添加聚乙烯醇缩丁醛和乙二胺在30℃下搅拌反应8min后的产物；再继续加入磷酸三(异丙基苯)酯，升温至105℃，搅拌反应30min；最后加入改性聚亚苯醚树脂和液体丁腈橡胶在80℃下搅拌反应40min的产物，再继续搅拌0.5h，冷却至室温，得到阻燃整理液；
S2.无纺布的阻燃整理；将无纺布浸泡于S1得到的阻燃整理液中静置10min；将浸泡过的无纺布置于压辊机的两个橡胶压辊之间，挤压除去多余液体；将阻燃整理后的无纺布在100℃下烘干，得到阻燃无纺布。
各组分含量如下表2所示。
实施例5
本申请公开了一种阻燃无纺布及其加工工艺，无纺布由阻燃整理液整理，阻燃整理液包括如下原料：磷酸三(异丙基苯)酯、甲醚化六羟甲基三聚氰胺树脂、三氧化二锑、改性聚亚苯醚树脂、液体丁腈橡胶、聚乙烯蜡、苯甲酸苄酯、聚乙烯醇缩丁醛和乙二胺；加工工艺包括以下步骤：
S1.阻燃整理液的制备；将甲醚化六羟甲基三聚氰胺树脂、三氧化二锑、聚乙烯蜡和苯甲酸苄酯混合并搅拌5min；然后添加聚乙烯醇缩丁醛和乙二胺在35℃下搅拌反应10min后的产物；再继续加入磷酸三(异丙基苯)酯，升温至115℃，搅拌反应40min；最后加入改性聚亚苯醚树脂和液体丁腈橡胶在90℃下搅拌反应60min的产物，再继续搅拌1h，冷却至室温，得到阻燃整理液；
S2.无纺布的阻燃整理；将无纺布浸泡于S1得到的阻燃整理液中静置20min；将浸泡过的无纺布置于压辊机的两个橡胶压辊之间，挤压除去多余液体；将阻燃整理后的无纺布在110℃下烘干，得到阻燃无纺布。
各组分含量如下表2所示。
实施例6
本申请公开了一种阻燃无纺布及其加工工艺，无纺布由阻燃整理液整理，阻燃整理液包括如下原料：磷酸三(异丙基苯)酯、甲醚化六羟甲基三聚氰胺树脂、三氧化二锑、改性聚亚苯醚树脂、液体丁腈橡胶、聚乙烯蜡、苯甲酸苄酯、聚乙烯醇缩丁醛和乙二胺；加工工艺包括以下步骤：
S1.阻燃整理液的制备；将甲醚化六羟甲基三聚氰胺树脂、三氧化二锑、聚乙烯蜡和苯甲酸苄酯混合并搅拌4min；然后添加聚乙烯醇缩丁醛和乙二胺在33℃下搅拌反应9min后的产物；再继续加入磷酸三(异丙基苯)酯，升温至110℃，搅拌反应35min；最后加入改性聚亚苯醚树脂和液体丁腈橡胶在85℃下搅拌反应50min的产物，再继续搅拌0.8h，冷却至室温，得到阻燃整理液；
S2.无纺布的阻燃整理；将无纺布浸泡于S1得到的阻燃整理液中静置15min；将浸泡过的无纺布置于压辊机的两个橡胶压辊之间，挤压除去多余液体；将阻燃整理后的无纺布在105℃下烘干，得到阻燃无纺布。
各组分含量如下表2所示。
实施例7
与实施例4的区别在于，将改性聚亚苯醚树脂替换为聚苯醚，各组分含量如下表2所示。
实施例8
与实施例7的区别在于，不添加液体丁腈橡胶，各组分含量如下表2所示。
实施例9
与实施例4的区别在于，将聚乙烯蜡替换为苯乙烯，各组分含量如下表2所示。
实施例10
与实施例9的区别在于，将苯甲酸苄酯替换为苯甲醇，各组分含量如下表2所示。
实施例11
与实施例4的区别在于，将磷酸三(异丙基苯)酯替换为阻燃剂TCPP，各组分含量如下表2所示。
实施例12
与实施例11的区别在于，不添加聚乙烯醇缩丁醛，各组分含量如下表2所示。
实施例13
与实施例12的区别在于，将乙二胺替换为苯甲酸，各组分含量如下表2所示。
对比例
对比例1
与实施例1的区别在于，采用未经本申请的阻燃整理液处理的无纺布作为空白对照组。
对比例2
与实施例1的区别在于，将甲醚化六羟甲基三聚氰胺树脂替换为三聚氰胺共聚树脂，各组分含量如下表1所示。
表1实施例1-3和对比例2的组分含量表
Figure BDA0002728336670000071
表2实施例4-12的组分含量表
Figure BDA0002728336670000072
Figure BDA0002728336670000081
性能检测试验
(1)极限氧指数(LOI)测试：依据纺织品燃烧性能试验(垂直法)GB/5455-1997，在氧指数测试仪上进行测试，试样尺寸80mm×300mm；LOI值越大，阻燃性能越好，测试结果如下表3所示。
(2)依据非织造布断裂强力及断裂伸长的测定标准FZ/T6005-91，使用YG065型电子织物强力试验仪对实施例4和实施例8、12、13的断裂强力进行测定，试样尺寸50mm×200mm；断裂强力越大，力学性能越好，测试结果如下表4所示。
(3)将实施例4和实施例8的试样放置于氙灯老化试验箱中，控制温度为(45±2)℃，湿度为(70±2)％，箱内连续照明36h使试样老化；对老化后的试样再次进行极限氧指数测试，测试结果如下表4所示。
表3各实施例和对比例的性能测试结果表
极限氧指数LOI/％
实施例1 27.2
实施例2 27.8
实施例3 27.5
实施例4 29.1
实施例5 29.6
实施例6 29.3
实施例7 21.4
实施例8 19.5
实施例9 25.6
实施例10 24.7
实施例11 24.4
实施例12 21.8
实施例13 19.3
对比例1 16.1
对比例2 24.2
表4实施例4、8、12和13的性能测试结果表
Figure BDA0002728336670000082
Figure BDA0002728336670000091
综上所述，可以得出以下结论：
1.根据实施例1和对比例1并结合表3可以看出，采用本申请的阻燃整理剂处理过的无纺布具有较好的阻燃性。
2.根据实施例1和对比例2并结合表3可以看出，甲醚化六羟甲基三聚氰胺树脂的添加具有较好的提升阻燃整理液的阻燃性的作用，从而可提升无纺布的阻燃性。
3.根据实施例4和实施例7-8并结合表3可以看出，改性聚亚苯醚树脂的添加有助于提升无纺布的阻燃性；且改性聚亚苯醚树脂和液体丁腈橡胶的共同添加可进一步使阻燃整理液获得更优异的阻燃性能，提升无纺布的阻燃效果。
4.根据实施例4和实施例8并结合表3和表4可以看出，液体丁腈橡胶的添加可提升无纺布的阻燃耐久性，其原因可能是液体丁腈橡胶的添加提升了阻燃整理液共混组分的物理性能。
5.根据实施例4和实施例9-10并结合表3可以看出，聚乙烯蜡和苯甲酸苄酯的复合物可在一定程度上提升阻燃整理液的阻燃性，其原因可能是，较好地提高了阻燃整理液各组分的相容性，从而提升阻燃整理后的无纺布的阻燃性能。
6.根据实施例4和实施例11-13并结合表3可以看出，聚乙烯醇缩丁醛的添加在一定程度上提升阻燃整理液的阻燃性能，提高无纺布的阻燃性；且通过乙二胺的进一步添加，可获得阻燃性能更优异的阻燃整理液，从而提升无纺布的阻燃效果；其原因可能是乙二胺和聚乙烯醇缩丁醛的加成产物与磷酸三(异丙基苯)酯交联，使阻燃整理液吸附于无纺布上的同时还可填充于无纺布的孔隙中，提高无纺布的阻燃效果。
7.根据实施例4和实施例12-13并结合表4可以看出，乙二胺和聚乙烯醇缩丁醛的加成产物的添加有利于提升阻燃整理后的无纺布的断裂强力。
本具体实施方式仅仅是对本申请的解释，其并不是对本申请的限制，本领域技术人员在阅读完本说明书后可以根据需要对本实施方式做出没有创造性贡献的修改，但只要在本申请的权利要求范围内都受到专利法的保护。

Claims (8)

1.一种阻燃无纺布，其特征在于：所述无纺布由阻燃整理液整理，所述阻燃整理液包括如下重量份数的原料：
30-40份磷酸三(异丙基苯)酯；
5-8份甲醚化六羟甲基三聚氰胺树脂；
2-3份三氧化二锑。
2.根据权利要求1所述的一种阻燃无纺布，其特征在于：按重量份数计，所述原料还包括3-4份改性聚亚苯醚树脂。
3.根据权利要求2所述的一种阻燃无纺布，其特征在于：按重量份数计，所述原料还包括1-2份液体丁腈橡胶。
4.根据权利要求3所述的一种阻燃无纺布，其特征在于：按重量份数计，所述原料还包括2-3份聚乙烯蜡和1-2份苯甲酸苄酯。
5.根据权利要求1所述的一种阻燃无纺布，其特征在于：按重量份数计，所述原料还包括2-3份聚乙烯醇缩丁醛。
6.根据权利要求5所述的一种阻燃无纺布，其特征在于：按重量份数计，所述原料还包括0.6-0.8份乙二胺。
7.权利要求1所述的一种阻燃无纺布的加工工艺，其特征在于，包括以下步骤：
S1.阻燃整理液的制备；称取所需组分，将甲醚化六羟甲基三聚氰胺树脂和三氧化二锑混合并搅拌3-5min，再加入磷酸三(异丙基苯)酯，升温至105-115℃，搅拌30-40min，冷却至室温，得到阻燃整理液；
S2.无纺布的阻燃整理；将无纺布浸泡于S1得到的阻燃整理液中静置10-20min；将浸泡过的无纺布置于压辊机的两个橡胶压辊之间，挤压除去多余液体；将阻燃整理后的无纺布在100-110℃下烘干，得到阻燃无纺布。
8.权利要求7所述的一种阻燃无纺布的加工工艺，其特征在于：所述S1中，将5-8份甲醚化六羟甲基三聚氰胺树脂、2-3份三氧化二锑、2-3份聚乙烯蜡和1-2份苯甲酸苄酯混合并搅拌3-5min；然后添加2-3份聚乙烯醇缩丁醛和0.6-0.8份乙二胺在30-35℃下搅拌反应8-10min后的产物；再继续加入30-40份磷酸三(异丙基苯)酯，升温至105-115℃，搅拌反应30-40min；最后加入3-4份改性聚亚苯醚树脂和1-2份液体丁腈橡胶在80-90℃下搅拌反应40-60min的产物，再继续搅拌0.5-1h，冷却至室温，得到阻燃整理液。
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