CN104311781A - 一种高透湿水性聚氨酯材料及其制备方法 - Google Patents
一种高透湿水性聚氨酯材料及其制备方法 Download PDFInfo
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Abstract
本发明的目的是提供一种高透湿、用于棉、涤纶纺织品的干法涂层整理中的高透湿水性聚氨酯材料及其制备方法,该材料由聚氨酯树脂和水组成,聚氨酯树脂由以下重量百分比的各组分制成:40wt%~80wt%的长链多羟基化合物、10wt%~50wt%二异氰酸酯化合物、1wt%~10wt%的阴离子型亲水化合物、0.05wt%~5wt%含羟基的低分子化合物和1wt%~5wt%的乙二胺;保持该水性聚氨酯材料中水的重量百分比为50wt%~75wt%。将本发明的水性聚氨酯材料制成织物涂层剂后采用干法整理到涤纶织物上,所得织物的透湿量均大于5000g/m2·day。
Description
技术领域
本发明涉及一种高透湿水性聚氨酯材料及其制备方法,属于纺织化工技术领域。
背景技术
早在20世纪60年代,聚氨酯(PU)合成革就开始出现在人们的生活中。PU合成革真皮感强,具有和基材粘结力强、抗磨损、耐挠曲、抗老化等优异性能,且加工简便、价格低廉。随着人们生活水平的不断提高,对PU革服装舒适性和功能性的要求也越来越高。早期的PU涂层织物防水效果一般都较好,但透湿能力较差,人体穿着这类服装在剧烈运动时,大量汗液无法以蒸汽的形式排出,在衣服内部形成冷凝水滴,使人感觉粘湿而不舒适。防水透湿聚氨酯的研究因此成为聚氨酯研究领域的热点课题。防水透气(又称防水透湿)是指聚合物材料不允许水滴等液体透过,却能保证水蒸气自由透过。20世纪60年代后期到70年代初,美国、日本、比利时等国开始研制聚氨酯微孔涂层织物和亲水聚氨酯薄膜织物,此后以聚氨酯为主体的防水透湿涂层物的研究开发一直很活跃。
溶剂型聚氨酯织物涂层剂虽然透湿性能较好,但由于其含有大量有机溶剂,严重污染环境,特别是溶剂型双组分聚氨酯中的残留异氰酸酯单体,毒性极高。随着人们环保意识的增强和各国政府环保立法,急需一种可以替代传统有机溶剂型的新型聚氨酯材料。水性聚氨酯是以水替代有机溶剂作为分散介质,具有安全、价廉、节能、环境友好、使用方便等特点,因此备受关注,成为当今聚氨酯织物涂层领域发展的重要方向。中国专利CN102633977A公开了一种防水透湿涂层胶、制备方法及其应用,该聚氨酯涂层剂是利用预聚体法以聚醚二元醇和二异氰酸酯接枝长链饱和脂肪醇改性合成水性聚氨酯,但其透湿量较低。本发明合成的一种高透湿水性聚氨酯材料的透湿量普遍高于5000g/m2·day,且耐水压均能达到防水使用要求。
发明内容
技术问题:本发明的目的是提供一种用于棉、涤纶纺织品等的涂层整理中的防水透湿水性聚氨酯材料及制备方法,使其既能满足环境友好,又能满足高透湿要求的水性聚氨酯织物涂层剂。
技术方案:本发明的一种高透湿水性聚氨酯材料是通过以下技术方案实现的:
该材料由聚氨酯树脂和水组成,聚氨酯树脂由以下重量百分比的各组分制成:40wt%~80wt%的长链多羟基化合物、10wt%~50wt%二异氰酸酯化合物、1wt%~10wt%的阴离子型亲水化合物、0.05wt%~5wt%含羟基的低分子化合物、1wt%~5wt%的乙二胺;由聚氨酯树脂和水组成的水性聚氨酯材料中水的重量百分比为50wt%~75wt%。
本发明的高透湿水性聚氨酯材料的制备方法为:
将长链多羟基化合物、阴离子型亲水化合物和含有羟基的低分子化合物同时加入反应釜中,在70~90℃下搅拌0.5~1h混匀得二醇混合液,将该二醇混合液降温至40~55℃后,加入二异氰酸酯化合物,升温至60~80℃,反应6~8h,得异氰酸基团封端的聚氨酯预聚体;将该预聚体降温至15~40℃,并加入与该预聚体总质量比为0.2:1~0.3:1的丁酮稀释,再加入与阴离子型亲水化合物摩尔比为0.9:1~1.1:1的三乙胺进行中和反应0.5~1h,得中和混合液;高速搅拌下往中和混合液中加入与上述预聚体总质量比为1:1~3:1的去离子水,乳化0.5~1h,再加入乙二胺进行扩链反应0.5~1h,得水性聚氨酯乳液;将该水性聚氨酯乳液在40~50℃下减压蒸馏除去溶剂,保持该水性聚氨酯材料中水的重量百分比为50wt%~75wt%,得固含量为25wt%~50wt%的高透湿水性聚氨酯材料。
所述的长链多羟基化合物由重量百分比为40wt%~80wt%的分子量为1000~3000的聚乙二醇和20wt%~60wt%的分子量为1000~3000的聚四氢呋喃二醇组成。
所述的二异氰酸酯化合物为氢化苯基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯中的一种。
所述的阴离子型亲水化合物为二羟甲基丙酸、二羟甲基丁酸中的一种。
所述的含羟基的低分子化合物为1,4-丁二醇、三羟甲基丙烷、1,6-己二醇、一缩二乙二醇、3-甲基-1,5-戊二醇中的一种或多种的组合。
性能测试:将本发明的一种高透湿水性聚氨酯材料,加入0.2wt%L75N增稠剂和0.1wt%BYK333润湿剂制得水性聚氨酯织物涂层剂,将该涂层剂采用干法整理到涤纶织物上,按照《GB/T12704.1-2009纺织品织物透湿性试验方法第1部分:吸湿法》和《GB/T4744-1997纺织织物抗渗水性测定耐水压试验》测定涂层织物的透湿性能和耐水性能。
有益效果:本发明提供了一种高透湿水性聚氨酯材料及其制备方法,与现有技术相比,具有以下特点:
(1)与传统溶剂型聚氨酯织物涂层剂相比,本发明提供的是一种以水为分散介质的水性聚氨酯织物涂层剂,具有安全、价廉、节能、环境友好、使用方便等特点。
(2)本发明通过使用聚乙二醇和聚四氢呋喃二醇混合聚醚二醇化合物作为聚氨酯的软段,并通过选择两者合适的分子量及比例使得到的聚氨酯材料不仅具有高透湿的性能,而且具有机械强度好、耐水解性能优异的特点,在满足基本材料基本使用性能的同时,可显著提高织物的透湿量。
具体实施方式
本发明的高透湿水性聚氨酯材料所述的长链多羟基化合物由重量百分比为40%~80%的分子量为1000~3000的聚乙二醇(PEG)和20%~60%的分子量为1000~3000的聚四氢呋喃二醇(PTMG)组成;所述的二异氰酸酯为氢化苯基甲烷二异氰酸酯(H12MDI)、异佛尔酮二异氰酸酯(IPDI)、六亚甲基二异氰酸酯(HDI)中的一种;所述的阴离子型亲水化合物为二羟甲基丙酸(DMPA)、二羟甲基丁酸(DMBA)中的一种;所述的含羟基的低分子化合物包括:1,4-丁二醇(BDO)、三羟甲基丙烷(TMP)、1,6-己二醇(HDO)、一缩二乙二醇(DEG)、3-甲基-1,5-戊二醇(MPD)中的一种或多种的组合。
实施例1:
将78.18g分子量为2000的聚乙二醇与52.12g分子量为2000的聚四氢呋喃二醇、8g二羟甲基丁酸、1.68g一缩二乙二醇同时加入反应釜中,70℃下搅拌1h,混匀得二醇混合液,将该二醇混合液降温至40℃,加入60g异佛尔酮二异氰酸酯化合物,升温至60℃,反应8h,得异氰酸基团封端的聚氨酯预聚体;将该预聚体降温至20℃,加入40g的丁酮稀释,再加入5.46g三乙胺,中和反应0.5h得中和混合液,高速搅拌下往中和混合液中加入205g去离子水,乳化0.5h,再加入4.87g乙二胺,继续高速搅拌0.5h,得水性聚氨酯乳液,将该水性聚氨酯乳液在40℃下,减压蒸馏除去溶剂,得到固含量为50%的高透湿水性聚氨酯材料,将该材料制成织物涂层剂后测得织物的透湿量为5000g/m2·day、耐水压为73.5KPa。
实施例2:
将55.8g分子量为2000的聚乙二醇与77.4g分子量为2000的聚四氢呋喃二醇、6g二羟甲基丁酸、2.8g三羟甲基丙烷和2.57g1,4-丁二醇同时加入反应釜中,90℃下搅拌0.5h,混匀得二醇混合液,将该二醇混合液降温至55℃,加入60g异佛尔酮二异氰酸酯化合物,升温至80℃,反应6h,得异氰酸基团封端的聚氨酯预聚体,将该预聚体降温至40℃,加入60g的丁酮稀释,再加入4.10g三乙胺,中和反应0.5h得中和混合液,高速搅拌下往中和混合液中加入600g去离子水,乳化0.5h,再加入2.78g乙二胺,继续高速搅拌0.5h,得水性聚氨酯乳液,将该水性聚氨酯乳液在50℃下,减压蒸馏除去溶剂,得到固含量为25%的高透湿水性聚氨酯材料,将该材料制成织物涂层剂后测得织物的透湿量为5100g/m2·day、耐水压为50.9KPa。
实施例3:
将69g分子量为3000的聚乙二醇与69g分子量为1000的聚四氢呋喃二醇、6g二羟甲基丙酸、5.9g3-甲基-1,5-戊二醇同时加入反应釜中,80℃下搅拌45min,混匀得二醇混合液,将该二醇混合液降温至50℃,加入50g异佛尔酮二异氰酸酯化合物,升温至70℃,反应7h,得异氰酸基团封端的聚氨酯预聚体,将该预聚体降温至30℃,加入50g的丁酮稀释,再加入4.07g三乙胺,中和反应45min得中和混合液,高速搅拌下往中和混合液中加入530g去离子水,乳化0.5h,再加入2.25g乙二胺,继续高速搅拌45min,得水性聚氨酯乳液,将该水性聚氨酯乳液在50℃下,减压蒸馏除去溶剂,得到固含量为27%的高透湿水性聚氨酯材料,将该材料制成织物涂层剂后测得织物的透湿量为5200g/m2·day、耐水压为60.4KPa。
实施例4:
将78.34g分子量为2000的聚乙二醇与52.23g分子量为1000的聚四氢呋喃二醇、8g二羟甲基丙酸、1.44g3-甲基-1,5-戊二醇同时加入反应釜中,75℃下搅拌50min,混匀得二醇混合液,将该二醇混合液降温至45℃,加入60g4,4’-二环己基甲烷二异氰酸酯化合物,升温至65℃,反应7.5h,得异氰酸基团封端的聚氨酯预聚体,将该预聚体降温至35℃,加入60g的丁酮稀释,再加入5.43g三乙胺,中和反应50min得中和混合液,高速搅拌下往中和混合液中加入300g去离子水,乳化0.5h,再加入2.36g乙二胺,继续高速搅拌50min,得水性聚氨酯乳液,将该水性聚氨酯乳液在45℃下,减压蒸馏除去溶剂,得到固含量为40%的高透湿水性聚氨酯材料,将该材料制成织物涂层剂后测得织物的透湿量为5400g/m2·day、耐水压为70.6KPa。
实施例5:
将87.9g分子量为2000的聚乙二醇与58.6g分子量为2000的聚四氢呋喃二醇、6g二羟甲基丁酸、2.43g1,6-己二醇同时加入反应釜中,65℃下搅拌1h,混匀得二醇混合液,将该二醇混合液降温至50℃,加入45g六亚甲基二异氰酸酯化合物,升温至70℃,反应7h,得异氰酸基团封端的聚氨酯预聚体,将该预聚体降温至20℃,加入55g的丁酮稀释,再加入4.09g三乙胺,中和反应0.5h得中和混合液,高速搅拌下往中和混合液中加入466g去离子水,乳化0.5h,再加入6.44g乙二胺,继续高速搅拌1h,得水性聚氨酯乳液,将该水性聚氨酯乳液在42℃下,减压蒸馏除去溶剂,得到固含量为30%的高透湿水性聚氨酯材料,将该材料制成织物涂层剂后测得织物的透湿量为5500g/m2·day、耐水压为74.7KPa。
实施例6:
将58.2g分子量为2000的聚乙二醇与58.2g分子量为3000的聚四氢呋喃二醇、8g二羟甲基丁酸、2g三羟甲基丙烷、8.86g一缩二乙二醇同时加入反应釜中,80℃下搅拌50min,混匀得二醇混合液,将该二醇混合液降温至50℃,加入65g4,4’-二环己基甲烷二异氰酸酯化合物,升温至65℃,反应8h,得异氰酸基团封端的聚氨酯预聚体,将该预聚体降温至35℃,加入60g的丁酮稀释,再加入5.46g三乙胺,中和反应50min得中和混合液,高速搅拌下往中和混合液中加入600g去离子水,乳化50min,再加入1.5g乙二胺,继续高速搅拌50min,得水性聚氨酯乳液,将该水性聚氨酯乳液在44℃下,减压蒸馏除去溶剂,得到固含量为25%的高透湿水性聚氨酯材料,将该材料制成织物涂层剂后测得织物的透湿量为5300g/m2·day、耐水压为64.7KPa。
Claims (6)
1.一种高透湿水性聚氨酯材料,其特征在于该材料由聚氨酯树脂和水组成,聚氨酯树脂由以下重量百分比的各组分制成:40wt%~80wt%的长链多羟基化合物、10wt%~50wt%二异氰酸酯化合物、1wt%~10wt%的阴离子型亲水化合物、0.05wt%~5wt%含羟基的低分子化合物、1wt%~5wt%的乙二胺;由聚氨酯树脂和水组成的水性聚氨酯材料中水的重量百分比为50wt%~75wt%。
2.一种高透湿水性聚氨酯材料的制备方法,其特征在于该制备方法为:
将长链多羟基化合物、阴离子型亲水化合物和含有羟基的低分子化合物同时加入反应釜中,在70~90℃下搅拌0.5~1h混匀得二醇混合液,将该二醇混合液降温至40~55℃后,加入二异氰酸酯化合物,升温至60~80℃,反应6~8h,得异氰酸基团封端的聚氨酯预聚体;将该预聚体降温至15~40℃,并加入与该预聚体总质量比为0.2:1~0.3:1的丁酮稀释,再加入与阴离子型亲水化合物摩尔比为0.9:1~1.1:1的三乙胺进行中和反应0.5~1h,得中和混合液;高速搅拌下往中和混合液中加入与上述预聚体总质量比为1:1~3:1的去离子水,乳化0.5~1h,再加入乙二胺进行扩链反应0.5~1h,得水性聚氨酯乳液;将该水性聚氨酯乳液在40~50℃下减压蒸馏除去溶剂,保持该水性聚氨酯材料中水的重量百分比为50wt%~75wt%,得固含量为25wt%~50wt%的高透湿水性聚氨酯材料。
3.根据权利要求1所述的一种高透湿水性聚氨酯材料,其特征在于所述的长链多羟基化合物由重量百分比为40wt%~80wt%的分子量为1000~3000的聚乙二醇和20wt%~60wt%的分子量为1000~3000的聚四氢呋喃二醇组成。
4.根据权利要求1所述的一种高透湿水性聚氨酯材料,其特征在于所述的二异氰酸酯化合物为氢化苯基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯中的一种。
5.根据权利要求1所述的一种高透湿水性聚氨酯材料,其特征在于所述的阴离子型亲水化合物为二羟甲基丙酸、二羟甲基丁酸中的一种。
6.根据权利要求1所述的一种高透湿水性聚氨酯材料,其特征在于所述的含羟基的低分子化合物为1,4-丁二醇、三羟甲基丙烷、1,6-己二醇、一缩二乙二醇、3-甲基-1,5-戊二醇中的一种或多种的组合。
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