CN109652984A - 一种织物阻燃涂层整理剂组合物及其制备方法 - Google Patents

一种织物阻燃涂层整理剂组合物及其制备方法 Download PDF

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CN109652984A
CN109652984A CN201811522920.4A CN201811522920A CN109652984A CN 109652984 A CN109652984 A CN 109652984A CN 201811522920 A CN201811522920 A CN 201811522920A CN 109652984 A CN109652984 A CN 109652984A
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党婉蓉
李正雄
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TAICANG BAONI INDUSTRIAL Co.,Ltd.
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Abstract

本发明涉及一种织物阻燃涂层整理剂组合物及其制备方法。该阻燃涂层整理剂组合物包括20‑35重量％水溶性聚合物粘合剂、5‑20重量％阻燃剂，2‑15重量％表面活性剂、1‑5重量％羟基含氟化合物和45‑55重量％水，以阻燃涂层整理剂组合物的总重量为基准。与常规阻燃涂层整理剂组合物相比，本发明的阻燃涂层整理剂组合物的阻燃效果好、耐水性和稳定性优异，且生产简单，易于工业化生产。

Description

一种织物阻燃涂层整理剂组合物及其制备方法
技术领域
本发明涉及一种织物涂层整理剂组合物及其制备方法，特别是一种织物阻燃涂层整理剂及其制备方法。
背景技术
近年来，随着人们对生存环境的安全需求越来越强烈，消防安全自然也成为了社会关注的重点。据统计，在火灾事故中，以床上用品、家具、装饰物和衣着占很大比例，而在火灾造成的死亡中，属于纺织品火灾死亡的占50％，因此纺织品的阻燃处理有着重要意义。纺织品的阻燃处理方法分为原纱改性法和后整理法，以后整理法最为普遍，阻燃涂层即为一种最为常用的后整理法，相对于传统的浸渍或浸轧阻燃后整理，阻燃涂层具有耐洗性好，强力不下降，不需要污水处理等优点，因此在工业用布、室内家纺等领域广泛应用。
目前，织物阻燃涂层所用的阻燃涂层胶是由水性涂层胶和阻燃剂两种组分构成，其制备方法研究和应用最广泛的为物理共混，即在水性涂层胶中添加阻燃剂，简单易行，阻燃效果好，国内外的研究报道也较多，生产及应用工艺已经比较成熟，如申请号为201410686122的中国专利公开，介绍了一种纺织品用阻燃涂层胶，由水性聚氨酯乳液和水性聚丙烯酸酯乳液为涂层胶，添加溴系和磷系阻燃剂、阻燃协效剂、多羟基化合物、增稠剂、水性封端异氰酸酯和手感剂，制备的阻燃涂层胶赋予织物优异的阻燃性能，但由于溴系阻燃剂燃烧时分解出有毒气体对环境和人体造成危害，无溴阻燃体系便应运而生，如2008年全国阻燃学术年会论文“聚磷酸铵/水性丙烯酸酯阻燃胶在织物涂层中的应用研究”，采用水性聚丙烯酸酯为粘合剂，聚磷酸铵和协效剂为阻燃剂，制备的阻燃涂层胶环保，但耐水性能差，且容易渗出、稳定性差。为了解决聚磷酸铵环保阻燃涂层胶的耐水性和稳定性，研究者们采用微胶囊等包覆的方法对聚磷酸铵进行包覆改性，从而使水性涂层胶耐水性能得以改善，如申请号为200810121100.4的中国专利公开“含多重包覆改性聚磷酸铵的水性涂层胶及其在织物整理上的应用”，介绍了将过密胺、单一硅烷或者环氧树脂改性的聚磷酸铵，再进行硅烷偶联剂多层包覆改性，制得阻燃涂层胶，实现了耐水环保阻燃涂层织物，但适用的阻燃涂层胶体系单一，且制备工艺繁杂。还有研究者采用化学改性的方法对水性涂层胶进行接枝改性或将阻燃成分直接键合在水性涂层胶的分子链上，如申请号为201410849087.X的中国专利公开“一种无卤持久型阻燃水基聚氨酯及其制备方法”，介绍了将膨胀型阻燃剂通过化学键嵌段到水基聚氨酯结构单元中，阻燃效果优异，毒性低且稳定性好，但反应步骤多，反应时间长，中间过程难于控制，不利于工业化生产。
目前市场上兼具阻燃效果好、耐水性和稳定性优异，且生产简单，易于工业化生产的阻燃涂层胶还不多见，因此，开发出一种满足上述要求的阻燃涂层整理剂，具有非常重要的现实意义。
发明内容
在一个方面，本发明提供一种织物阻燃涂层整理剂组合物，其包括以下组分：
在另一方面，本发明提供一种织物阻燃涂层整理剂组合物的制备方法，它包括如下步骤：
1)将水溶性聚合物粘合剂、表面活性剂和水搅拌均匀，得到混合物；
2)然后阻燃剂和羟基含氟化合物加入到步骤1)中得到的混合物中，再搅拌均匀。
与现已公开的织物阻燃涂层整理剂及其制备方法相比，本发明独创性表现在如下几个方面：(1)本发明织物阻燃涂层整理剂中引入羟基含氟化合物能在阻燃涂层胶整理到织物时，一方面羟基在高温作用下发生交联，进而有效提升了整理织物的耐水性能，另一方面，由于羟基含氟化合物具有极低的表面张力，使得水和油难以浸润整理织物，使其耐水性能进一步提升。(2)在一个优选的实施方式中，在织物阻燃涂层整理剂中引入有机硅表面活性剂，一方面对阻燃涂层整理剂进行良好的分散作用，另一方面，引入的有机硅表面活性剂具有阻燃作用，与阻燃剂一起协同增效。(3)在另一个优选的实施方式中引入的两性表面活性剂在酸性和碱性条件下均具有优异的分散作用，与阻燃剂也有协同增效作用。
本发明织物阻燃涂层整理剂的阻燃效果好、耐水性和稳定性优异，且生产简单，易于工业化生产。
具体实施方式
在一个优选的实施方式中，本发明织物阻燃涂层整理剂组合物包括以下组分：
在一个优选的实施方式中，所述水溶性聚合物粘合剂包括水性聚氨酯乳液粘合剂、水性丙烯酸聚合物乳液粘合剂、水性丁苯聚合物乳液粘合剂、聚醋酸乙烯酯乳液粘合剂或它们的混合物。
在一个优选的实施方式中，所述阻燃剂是磷系阻燃剂、硅系阻燃剂、硼系阻燃剂或或它们的混合物。
在一个更优选的实施方式中，所述的磷系阻燃剂是聚磷酸胺，优选是聚合度大于500，优选为800-1500的聚磷酸胺。所述的硼系阻燃剂是硼酸锌，优选是水硝酸锌。所述硅系阻燃剂为有机硅阻燃剂，优选是有机倍半硅氧烷阻燃剂。
在一个优选的实施方式中，所述表面活性剂是两性表面活性剂、阴离子表面活性剂或它们的混合物，所述混合物中两性表面活性剂和阴离子表面活性剂的重量比为25-55:45-75，优选为30-50:50-70。
在一个更优选的实施方式中，所述两性表面活性剂优选为磷酯类两性表面活性剂，例如优选为HLB值为8-12，优选为HLB值9－10的羟基化卵磷脂。所述的阴离子表面活性剂为有机硅表面活性剂，特别是如下式I)表示的有机硅羧酸钠：
式I)中：
m为1-50，优选为2-40中的一个整数；
n为1-100，优选为2-70中的一个整数。
在一个更优选的实施方式中，式I)表示的有机硅羧酸钠例如可参照如下文献制备：戴润英,等人的《有机硅羧酸钠表面活性剂的合成及其应用研究》，江西师范大学学报(自然科学版)，2015，39(6)：561-565。
在一个优选的实施方式中，所述羟基含氟化合物是羟基含氟有机化合物，例如包括羟基氟硅油、羟苯基C2-6全氟烷醇、或它们的混合物。
在一个更优选的实施方式中，所述的羟基氟硅油为25℃粘度50-200mPa﹒s，优选为50-150mPa﹒s的羟基氟硅油，所述的羟苯基C2-6全氟烷醇是2-(4-羟基苯基)六氟异丙醇。
在一个优选的实施方式中，所述的水是本领域中常用的水，如去离子水。
在一个优选的实施方式中，本发明织物阻燃涂层整理剂组合物是一种均匀的水分散体。
在一个优选的实施方式中，本发明织物阻燃涂层整理剂组合物的制备方法包括如下步骤：
1)将水溶性聚合物粘合剂、表面活性剂和去离子水加入反应釜中，25-40℃搅拌10-15min；
2)然后将阻燃剂和羟基含氟化合物加入到步骤1)中制得的混合物，升温至40-60℃，继续搅拌1-2h；
3)冷却至室温，制得所述织物阻燃涂层整理剂。
按本发明方法制得的织物阻燃涂层整理剂组合物的阻燃效果好、耐水性和稳定性优异，且生产简单，易于工业化生产。
实施例
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
所制得产品粒径、稳定性测定及其在纺织品上的应用与性能测定：
1)粒径测定：
配制1％的乳液，用Zetasizer Nano S90(Malvern公司)纳米粒度仪测定其平均粒径和多分散指数PDI，多分散指数越小，粒径分布越均匀。
2)稳定性测定：
离心稳定性：使用医用离心机(TDZ5-WS)在3000rpm的转速下离心30分钟、1小时，观察是否出现飘油、分层或沉淀，是则判定为不稳定，否则判定为稳定。
pH稳定性：将制备的产品分别用醋酸和液碱调节pH值到4和9，观察是否出现飘油、分层或沉淀，是则判定为不稳定，否则判定为稳定。
3)在纺织品的阻燃涂层处理应用：
织物：涤纶机织布
配方：阻燃涂层整理剂、十二烷基苯磺酸钠(2％)
工艺：机械发泡→涂饰织物→预烘(80℃，2min)→焙烘(160℃，2min)
4)纺织品性能测定标准：
阻燃性能：
a.按GB/T 5455-1997《纺织品燃烧性能试验垂直法》进行测试，测量续燃时间、阴燃时间、损毁长度等参数。按GB/T 17591-2006《阻燃织物》进行评价，B1级：损毁炭长≤15cm，续燃时间≤5s，阴燃时间≤5s；B2级，损毁炭长≤20cm，续燃时间≤10s，阴燃时间≤10s；
b.水洗方法：
按照GB/T 17595-1998《纺织品织物燃烧试验前的家庭洗涤程序》。
实施例1
在一个500毫升四口烧瓶中加入水性聚氨酯涂层胶乳液AH-1704(固含量40％，粘度180mpa﹒s(25℃)，购自安徽安大华泰新材料有限公司)60g、有机硅羧酸钠(式I中，m为4，n为4)6g、羟基化卵磷脂LLW(HLB值为9-10，购自北京源华美磷脂科技有限公司)3.7g和去离子水13.2g，25℃搅拌10min，然后加入聚磷酸铵Ⅱ型15g(聚合度>1000，购自什邡市长丰化工有限公司)、羟基氟硅油NFS7200(粘度100mPa﹒s(25℃)，购自威海新元化工有限公司)2.1g，升温至40℃，继续搅拌2h，冷却至室温，制得所述阻燃涂层整理剂1，测得平均粒径为162.9nm，多分散指数为0.117。
实施例2
在一个500毫升四口烧瓶中加入水性丙烯酸聚合物涂层胶乳液W-1521(固含量50％，粘度320mpa﹒s(25℃)，购自台湾石梅化学工业有限公司)55g.、有机硅羧酸钠6.5g(式I中，m为16，n为34)、羟基化卵磷脂LLW(HLB值为9-10，购自北京源华美磷脂科技有限公司)4.8g和去离子水21.2g，35℃搅拌15min，然后加入有机硅阻燃剂FR-Si9800(购自东莞市铨盛化工有限公司)10g、2-(4-羟基苯基)六氟异丙醇2.5g，升温至50℃，继续搅拌1.5h，冷却至室温，制得所述阻燃涂层整理剂2，测得平均粒径为168.3nm，多分散指数为0.117。
实施例3
在一个500毫升四口烧瓶中加入丁苯聚合物涂层胶乳液342(固含量50％，粘度67mpa﹒s(25℃)，购自杭州龙驹合成材料有限公.司)33g、聚醋酸乙烯酯涂层胶乳液1501(固含量45％，粘度3510mpa﹒s(25℃)，购自塞拉尼斯化工有限公司)25g、有机硅羧酸钠5.5g(式I中，m为32，n为57)、羟基化卵磷脂LLW(HLB值为9-10，购自北京源华美磷脂科技有限公司)4.8g和去离子水18.9g，40℃搅拌10min，然后加入3.5水硼酸锌10g、羟基氟硅油NFS7200(粘度100mPa﹒s(25℃)，购自威海新元化工有限公司)1.8g和2-(4-羟基苯基)六氟异丙醇1.0g，升温至60℃，继续搅拌1h，冷却至室温，制得所述阻燃涂层整理剂3，测得平均粒径为161.8nm，多分散指数为0.103。
对比例1
在一个500毫升四口烧瓶中加入水性聚氨酯涂层胶乳液AH-1704(固含40％，粘度180mpa﹒s(25℃)，购自安徽安大华泰新材料有限公司)60g、有机硅羧酸钠(式I中m为4，n为4)9.7g和去离子水13.2g，25℃搅拌10min，然后加入聚磷酸铵Ⅱ型17.1g(聚合度>1000，购自什邡市长丰化工有限公司)，升温至40℃，继续搅拌2h，冷却至室温，制得阻燃涂层整理剂4，测得平均粒径为204.6nm，多分散指数为0.219。
各实施例的应用效果与对比例1、市售阻燃涂层整理剂A、市售阻燃涂层胶B稳定性和应用效果对比，如表1、表2所示。
表1稳定性
表2应用效果
综合表1、表2，本发明制备的阻燃涂层整理剂在3000rpm转速下离心1小时，仍然稳定，而对比例1和市售阻燃涂层胶已经出现分层现象，并且本发明制备的阻燃涂层整理剂在pH值为4或者9时均稳定，而对比例1和市售阻燃胶在pH值为4时出现了分层。本发明制备的阻燃涂层整理剂应用在织物上时，阻燃效果明显优于市售阻燃胶，且经12次水洗后，阻燃效果几乎没有下降。

Claims (10)

1.一种织物阻燃涂层整理剂组合物，其包括以下组分：
剂组合物的总重量为基准。
2.如权利要求1所述的阻燃涂层整理剂组合物，其特征在于，它包括以下组分：
剂组合物的总重量为基准。
3.如权利要求1所述的织物阻燃涂层整理剂组合物，其特征在于，所述水溶性聚合物粘合剂包括水性聚氨酯乳液粘合剂、水性丙烯酸聚合物乳液粘合剂、水性丁苯聚合物乳液粘合剂、聚醋酸乙烯酯乳液粘合剂或它们的混合物。
4.如权利要求1所述的织物阻燃涂层整理剂组合物，其特征在于，所述阻燃剂是磷系阻燃剂、硅系阻燃剂、硼系阻燃剂或它们的混合物。
5.如权利要求4所述的织物阻燃涂层整理剂组合物，其特征在于，所述的磷系阻燃剂是聚磷酸胺，所述的硼系阻燃剂是硼酸锌，所述硅系阻燃剂为有机硅阻燃剂。
6.如权利要求1所述的织物阻燃涂层整理剂组合物，其特征在于，所述表面活性剂是两性表面活性剂、阴离子表面活性剂或它们的混合物，所述混合物中两性表面活性剂和阴离子表面活性剂的重量比为25-55:45-75。
7.如权利要求6所述的织物阻燃涂层整理剂组合物，其特征在于，所述两性表面活性剂为HLB值为8-12的羟基化卵磷脂，所述的阴离子表面活性剂为如下式I)表示的有机硅表面活性剂；
式I)中：
m为1-50中的一个整数；
n为1-100中的一个整数。
8.如权利要求1所述的织物阻燃涂层整理剂组合物，其特征在于，所述羟基含氟化合物包括羟基氟硅油、羟苯基C2-6全氟烷醇、或它们的混合物，所述的水是去离子水。
9.如权利要求7所述的织物阻燃涂层整理剂组合物，其特征在于，所述的羟基氟硅油为25℃粘度50-200mPa﹒s的羟基氟硅油，所述的羟苯基C2-6全氟烷醇是2-(4-羟基苯基)六氟异丙醇。
10.如权利要求1－9中任一项所述的阻燃涂层整理剂组合物的制备方法，它包括如下步骤：
1)将水溶性聚合物粘合剂、表面活性剂和水搅拌均匀，得到混合物；
2)然后阻燃剂和羟基含氟化合物加入到步骤1)中得到的混合物中，再搅拌均匀。
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