CN104558488A - 一种有机磷改性水性聚氨酯阻燃涂层剂及其制备方法 - Google Patents
一种有机磷改性水性聚氨酯阻燃涂层剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种有机磷改性水性聚氨酯阻燃涂层剂及其制备方法,属于轻工技术领域。一种有机磷改性水性聚氨酯阻燃涂层剂,其特征在于,所述有机磷改性水性聚氨酯阻燃涂层剂是通过有机磷多元醇代替部分非阻燃多元醇与二异氰酸酯反应,并用亲水性扩链剂扩链,经成盐剂中和后得到,所述非阻燃多元醇为聚酯多元醇或者聚醚多元醇中的任一种或者任意几种的混合物。本发明的有机磷改性水性聚氨酯阻燃涂层剂及其制备方法,其中有机磷多元醇两端含有活泼性氢的羟基,可以部分取代多元醇与异氰酸酯反应生成氨基甲酸酯。在该聚氨酯中大分子链中引入有机磷阻燃中间体,形成了环保、无卤、低毒阻燃大分子。
Description
技术领域
本发明涉及一种有机磷改性水性聚氨酯阻燃涂层剂及其制备方法,属于轻工技术领域。
背景技术
水性聚氨酯主要应用于织物、皮革、建筑材料等等,这些材料都为易燃材料,一般均要求进行阻燃处理。水性聚氨酯以水为介质,具有无毒、环保、生产与应用安全、成本低等优点,有利于有色涂层产品的生产,涂层亲水性好。申请号为200510122057.X的专利,将用量为15%的阻燃单体二溴新戊二醇在聚合前加入体系,使生成的聚氨酯大分子链中带有阻燃卤素原子溴,制备出具有自阻燃性能的水性聚氨酯。申请号为200480043181.0,名称为“阻燃性聚氨酯及其添加剂”的发明专利申请公开了一种包含有氯、溴等卤素的反应型阻燃剂。这些专利所用的阻燃成分均含有卤素,在燃烧时生成较多的烟、腐蚀性气体和有毒气体,会对环境和人体造成危害,达不到无卤的环保要求。随着环保要求越来越高,阻燃剂的无卤化越来越重要。
因此开发出环保无卤阻燃水性聚氨酯是十分必要的。专利申请号为200810204199.4的专利,采用水性聚氨酯分散液与含磷含氮的阻燃剂以复配的方式制备出阻燃涂层浆涂覆在涤纶织物上达到阻燃效果。虽然其燃烧性能能达到国家B1级,但它的阻燃剂是与水性聚氨酯分散液以复配的方式涂覆在的涤纶织物上的,具有不耐水洗,阻燃剂用量大、易迁移等缺点。
发明内容
本发明针对现有含卤阻燃剂释放有毒气体,发烟量大的缺点,提供一种有机磷改性水性聚氨酯阻燃涂层剂,其具有环保、低烟、无毒、阻燃效果好的优点。
本发明还提供该有机磷改性水性聚氨酯阻燃涂层剂的制备方法。
本发明解决其技术问题所采用的技术方案是:
一种有机磷改性水性聚氨酯阻燃涂层剂,其特征在于,所述有机磷改性水性聚氨酯阻燃涂层剂是通过有机磷多元醇代替部分非阻燃多元醇与二异氰酸酯反应,并用亲水性扩链剂扩链,经成盐剂中和后得到,所述非阻燃多元醇为聚酯多元醇或者聚醚多元醇中 的任一种或者任意几种的混合物;
上述原料组分的质量百分比为:
其中,非阻燃多元醇包括聚醚多元醇、聚酯二元醇、聚丁烯二醇、聚丁二烯二醇、聚碳酸酯二醇、丙烯酸酯多元醇。
作为优选,所述二异氰酸酯为甲苯二异氰酸酯TDI,六亚甲基二异氰酸酯HDI,异佛尔酮二异氰酸酯IPDI或二烷基甲烷二异氰酸酯MDI中任一种或任意几种的混合物。
作为优选,所述亲水性扩链剂为含羟基的扩链剂,含氨基的扩链剂,含磺酸盐的扩链剂或阳离子型扩链剂中的任一种或者任意几种的混合物。
作为优选,所述成盐剂为三乙胺、三正丁胺、氢氧化钾或氨水中的任一种或者任意几种的混合物。
作为优选,所述有机磷多元醇选自
一种所述的有机磷改性水性聚氨酯阻燃涂层剂的制备方法,制备过程包括如下步骤:a.在氮气保护和搅拌条件下,将所述有机磷多元醇、非阻燃多元醇、二异氰酸酯 混合,在60-90℃的温度下充分反应得到预聚体;b.将所述的亲水性扩链剂与预聚体混合,60-90℃的温度下反应1-4h;c.向步骤b得到的混合物中加入成盐剂中和,反应时间为5-40min;d.降低反应体系的温度至50℃以下,在搅拌速度500-1500r/min下加入去离子水乳化10-60min,得到所述有机磷改性水性聚氨酯阻燃涂层剂乳液。
作为优选,步骤a的反应时间控制在10-90min。
本发明合成的水性聚氨酯阻燃涂层剂具有环保、低烟、无毒、阻燃效果好,具有较高的应用价值。
本发明的有益效果是:本发明的有机磷改性水性聚氨酯阻燃涂层剂及其制备方法,其中有机磷多元醇两端含有活泼性氢的羟基,可以部分取代多元醇与异氰酸酯反应生成氨基甲酸酯。在该聚氨酯中大分子链中引入有机磷阻燃中间体,形成了环保、无卤、低毒阻燃大分子。经过涂层整理后的织物可通过GB/T5455-1997纺织品燃烧性能实验垂直法中的B1级。高温下无卤素释放,无毒,低烟。
具体实施方式
下面通过具体实施例,对本发明的技术方案作进一步的具体说明。应当理解,本发明的实施并不局限于下面的实施例,对本发明所做的任何形式上的变通和/或改变都将落入本发明保护范围。
在本发明中,若非特指,所有的份、百分比均为重量单位,所采用的设备和原料等均可从市场购得或是本领域常用的。下述实施例中的方法,如无特别说明,均为本领域的常规方法。
实施例1
有机磷改性水性聚氨酯阻燃涂层剂的配方如表1所示:
表1 实施例1环保无卤有机磷阻燃改性水性聚氨酯织物涂层剂的配方
原料 | 用量/g |
异佛尔酮二异氰酸酯 | 22.30 |
聚醚多元醇(羟值112mgKOH/g) | 35.10 |
有机磷多元醇 | 6.19 |
二羟甲基丙酸 | 2.87 |
三乙胺 | 2.05 |
[0027] 在氮气保护氛围和搅拌条件下,将所述22.30g异佛尔酮二异氰酸酯、35.10g羟值为112mgKOH/g聚醚多元醇、6.19g有机磷多元醇置于烧瓶中,在70℃下预聚0.5h。
所述有机磷多元醇的结构式为:
将所述2.87g含羧酸的扩链剂二羟甲基丙酸加入烧瓶,在70℃下扩链2h。将烧瓶内的温度降至50℃以下,加入2.05g成盐剂三乙胺中和20min。在搅拌速度800r/min条件下将160g去离子水加入烧瓶,乳化30min得到所述有机磷改性水性聚氨酯阻燃涂层剂乳液。
阻燃性能测试:以涤纶牛津帐篷布为处理和测试织物,采用GB/T5455-1997垂直燃烧法实验检测,须燃时间0s,阴燃时间0s;损毁炭长11.5cm。
实施例2
有机磷改性水性聚氨酯阻燃涂层剂的配方如表2所示:
表2 实施例2环保无卤有机磷阻燃改性水性聚氨酯织物涂层剂的配方
原料 | 用量/g |
六亚甲基二异氰酸酯 | 25.34 |
聚醚多元醇(羟值95mgKOH/g) | 32.70 |
有机磷多元醇 | 7.26 |
1,4-丁二醇-2-磺酸钠 | 3.45 |
三正丁胺 | 2.87 |
在氮气保护氛围和搅拌条件下,将所述25.34g六亚甲基二异氰酸酯、32.70g羟值 为95mgKOH/g聚醚多元醇、7.26g有机磷多元醇置于烧瓶中,在80℃下预聚1h。
所述有机磷多元醇的结构式为:
将所述3.45g含磺酸盐型扩链剂1,4-丁二醇-2-磺酸钠加入烧瓶,在80℃下扩链3h。将烧瓶内的温度降至50℃以下,加入2.87g成盐剂三正丁胺中和15min。
在搅拌速度900r/min条件下将168g去离子水加入烧瓶,乳化20min得到所述有机磷改性水性聚氨酯阻燃涂层剂乳液。
阻燃性能测试:以涤纶牛津帐篷布为处理和测试织物,采用GB/T5455-1997垂直燃烧法实验检测,须燃时间0s,阴燃时间0s;损毁炭长10.7cm。
实施例3
有机磷改性水性聚氨酯阻燃涂层剂的配方如表3所示:
表3 实施例3环保无卤有机磷阻燃改性水性聚氨酯织物涂层剂的配方
原料 | 用量/g |
甲苯二异氰酸酯 | 27.12 |
聚醚多元醇(羟值112mgKOH/g) | 33.48 |
有机磷多元醇 | 5.71 |
N-甲基二乙醇胺 | 3.54 |
氨水 | 3.02 |
在氮气保护氛围和搅拌条件下,将所述27.12g甲苯二异氰酸酯、33.48g羟值为112mgKOH/g聚醚多元醇、5.71g有机磷多元醇置于烧瓶中,在60℃下预聚0.5h。
所述有机磷多元醇的结构式为:
将所述3.54g阳离子型扩链剂N-甲基二乙醇胺加入烧瓶,在60℃下扩链2.5h。将烧瓶内的温度降至50℃以下,加入3.02g成盐剂氨水中和25min。在搅拌速度1000r/min条件下将181g去离子水加入烧瓶,乳化50min得到所述有机磷改性水性聚氨酯阻燃涂层剂乳液。
阻燃性能测试:以涤纶牛津帐篷布为处理和测试织物,采用GB/T5455-1997垂直燃烧法实验检测,须燃时间0s,阴燃时间0s;损毁炭长11.8cm。
实施例4
有机磷改性水性聚氨酯阻燃涂层剂的配方如表4所示:
表4 实施例4环保无卤有机磷阻燃改性水性聚氨酯织物涂层剂的配方
原料 | 用量/g |
异佛尔酮二异氰酸酯 | 24.12 |
聚酯多元醇(羟值100mgKOH/g) | 28.45 |
有机磷多元醇 | 7.21 |
N-甲基二乙醇胺 | 3.86 |
三乙胺 | 2.07 |
在氮气保护氛围和搅拌条件下,将所述24.12g异佛尔酮二异氰酸酯、28.45g羟值为100mgKOH/g聚醚多元醇、7.21g有机磷多元醇置于烧瓶中,在75℃下预聚1h。
所述有机磷多元醇的结构式为:
将所述3.86g阳离子型扩链剂N-甲基二乙醇胺加入烧瓶,在75℃下扩链2h。将烧瓶内的温度降至50℃以下,加入2.07g成盐剂三乙胺中和20min。在搅拌速度1000r/min条件下将153g去离子水加入烧瓶,乳化20min得到所述有机磷改性水性聚氨酯阻燃涂层剂乳液。
阻燃性能测试:以涤纶牛津帐篷布为处理和测试织物,采用GB/T5455-1997垂直燃烧法实验检测,须燃时间0s,阴燃时间0s;损毁炭长9.7cm。
实施例5
有机磷改性水性聚氨酯阻燃涂层剂的配方如表5所示:
表5 实施例5环保无卤有机磷阻燃改性水性聚氨酯织物涂层剂的配方
原料 | 用量/g |
六亚甲基二异氰酸酯 | 18.62 |
聚醚多元醇(羟值112mgKOH/g) | 27.95 |
有机磷多元醇 | 8.59 |
1,4-丁二醇-2-磺酸钠 | 5.86 |
三乙胺 | 4.12 |
在氮气保护氛围和搅拌条件下,将所述18.62g六亚甲基二异氰酸酯、27.95g羟值为112mgKOH/g聚酯多元醇、8.59g有机磷多元醇置于烧瓶中,在65℃下预聚0.5h。
所述有机磷多元醇的结构式为:
将所述5.86g含磺酸盐型扩链剂1,4-丁二醇-2-磺酸钠加入烧瓶,在65℃下扩链3h。将烧瓶内的温度降至50℃以下,加入4.12g成盐剂三乙胺中和10min。在搅拌速度700r/min条件下将149g去离子水加入烧瓶,乳化20min得到所述有机磷改性水性聚氨酯阻燃涂层剂乳液。
阻燃性能测试:以涤纶牛津帐篷布为处理和测试织物,采用GB/T5455-1997垂直燃烧法实验检测,须燃时间0s,阴燃时间0s;损毁炭长11.0cm。
实施例6
有机磷改性水性聚氨酯阻燃涂层剂的配方如表6所示:
表6 实施例6环保无卤有机磷阻燃改性水性聚氨酯织物涂层剂的配方
原料 | 用量/g |
二烷基甲烷二异氰酸酯 | 21.40 |
聚酯多元醇(羟值100mgKOH/g) | 31.12 |
有机磷多元醇 | 7.21 |
N-甲基二乙醇胺 | 3.86 |
氢氧化钾 | 2.07 |
在氮气保护氛围和搅拌条件下,将所述21.40g二烷基甲烷二异氰酸酯、31.12g羟值为100mgKOH/g聚醚多元醇、7.21g有机磷多元醇置于烧瓶中,在75℃下预聚1h。
所述有机磷多元醇的结构式为:
将所述3.86g阳离子型扩链剂N-甲基二乙醇胺加入烧瓶,在75℃下扩链2h。将烧瓶内的温度降至50℃以下,加入2.07g成盐剂氢氧化钾中和30min。在搅拌速度1000r/min条件下将164g去离子水加入烧瓶,乳化30min得到所述有机磷改性水性聚氨酯阻燃涂层剂乳液。
阻燃性能测试:以涤纶牛津帐篷布为处理和测试织物,采用GB/T5455-1997垂直燃烧法实验检测,须燃时间0s,阴燃时间0s;损毁炭长13.2cm。
以上所述的实施例只是本发明的一种较佳的方案,并非对本发明作任何形式上的限制,在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。
Claims (7)
1.一种有机磷改性水性聚氨酯阻燃涂层剂,其特征在于,所述有机磷改性水性聚氨酯阻燃涂层剂是通过有机磷多元醇代替部分非阻燃多元醇与二异氰酸酯反应,并用亲水性扩链剂扩链,经成盐剂中和后得到;所述非阻燃多元醇为聚酯多元醇或者聚醚多元醇中的任一种或者任意几种的混合物;
上述原料组分的质量百分比为:
2.根据权利要求1所述的有机磷改性水性聚氨酯阻燃涂层剂,其特征在于,所述二异氰酸酯为甲苯二异氰酸酯TDI,六亚甲基二异氰酸酯HDI,异佛尔酮二异氰酸酯IPDI或二烷基甲烷二异氰酸酯MDI中任一种或任意几种的混合物。
3.根据权利要求1所述的有机磷改性水性聚氨酯阻燃涂层剂,其特征在于,所述亲水性扩链剂为含羟基的扩链剂,含氨基的扩链剂,含磺酸盐的扩链剂或阳离子型扩链剂中的任一种或者任意几种的混合物。
4.根据权利要求1所述的有机磷改性水性聚氨酯阻燃涂层剂,其特征在于,所述成盐剂为三乙胺、三正丁胺、氢氧化钾或氨水中的任一种或者任意几种的混合物。
5.根据权利要求1所述的有机磷改性水性聚氨酯阻燃涂层剂,其特征在于,所述有机磷多元醇选自
6.一种权利要求1所述的有机磷改性水性聚氨酯阻燃涂层剂的制备方法,其特征在于,制备过程包括如下步骤:
a.在氮气保护和搅拌条件下,将所述有机磷多元醇、非阻燃多元醇、二异氰酸酯混合,在60-90℃的温度下充分反应得到预聚体;
b.将所述的亲水性扩链剂与预聚体混合,60-90℃的温度下反应1-4h;
c.向步骤b得到的混合物中加入成盐剂中和,反应时间为5-40min;
d.降低反应体系的温度至50℃以下,在搅拌速度500-1500r/min下加入去离子水乳化10-60min,得到所述有机磷改性水性聚氨酯阻燃涂层剂乳液。
7.根据权利要求6所述的有机磷改性水性聚氨酯阻燃涂层剂,其特征在于,步骤a的反应时间控制在10-90min。
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