CN113429537A - 一种气凝胶复合聚氨酯及其制备方法 - Google Patents
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Abstract
本发明属于发泡材料技术领域,具体涉及一种气凝胶复合聚氨酯及其制备方法。该方法包括以下步骤:1)采用硅烷处理剂对气凝胶粉体原料进行改性,并包覆成膜,制备得到改性包覆气凝胶颗粒;2)将步骤1)得到的改性包覆气凝胶颗粒与聚氨酯制备A料混合,再与聚氨酯制备B料反应,制备得到所述的气凝胶复合聚氨酯。本发明通过硅烷处理剂对气凝胶粉体原料进行改性包覆,避免制备复合聚氨酯过程中气凝胶结构被其他水相或油相成分破坏。
Description
技术领域
本发明属于发泡材料技术领域,具体涉及一种气凝胶复合聚氨酯及其制备方法。
背景技术
目前人们对保温材料的需求及性能要求愈来愈高,对新型保温材料的研究开发获得了广泛的重视,市场上无机保温材料有很多,主要有岩棉、珍珠岩等,无机保温材料的最大的优势就是不会燃烧、稳定性高,但是其保温效果较差。有机保温材料也有很多种类,包括聚氨酯泡沫、聚苯板、酚醛泡沫等,在早期研究最多,工艺最成熟,应用最也为广泛的是聚氨酯材料,聚氨酯发泡材料目前最主要的问题是使用温度偏低,容易老化、碳化使用寿命短。为了解决以上问题,我们引入二氧化硅气凝胶材料,可以完美解决以上问题。
二氧化硅气凝胶具有防火等级高、使用温度高,导热系数低的特点,是目前公认的最佳的轻质保温材料,近年来也被国家大力推广和使用,市场上目前有亲水和亲油两种二氧化硅气凝胶材料,被广泛应用在各种复合材料中。但二氧化硅气凝胶质脆、易碎等缺点,极大的限制了其应用。另外聚氨酯发泡材料多分为AB料形式,有水相和油相同时存在,气凝胶的多孔结构很容易遭到破坏,从而降低了二氧化硅气凝胶的功效。为了解决气凝胶与聚氨酯的复合问题,同时解决聚氨酯发泡材料的保温效果、碳化问题、老化性能和使用温度低的问题,我们通过将气凝胶进行改性和包覆,并以不同的比例添加到聚氨酯体系中,制备得到气凝胶聚氨酯复合材料。将SiO2气凝胶纳米网络骨架结构引入到聚氨酯基体中,从根本上解决了以上问题,从而拓展气凝胶的应用领域,推动气凝胶产业的发展。
发明内容
为解决现有技术的不足,本发明提供了一种气凝胶复合聚氨酯及其制备方法。本发明将聚氨酯与气凝胶进行复合既能保留聚氨酯的优良性能及气凝胶的隔热性能,又弥补了气凝胶易碎裂及与无机材料复合易脱落的缺陷,具有良好发展前景。
本发明所提供的技术方案如下:
一种气凝胶复合聚氨酯的制备方法,包括以下步骤:
1)采用硅烷处理剂对气凝胶粉体原料进行改性,并通过包覆成膜物质制备得到改性包覆气凝胶颗粒;
2)将步骤1)得到的改性包覆气凝胶颗粒与聚氨酯制备A料混合,再与聚氨酯制备B料反应,制备得到所述的气凝胶复合聚氨酯。
基于上述技术方案,通过硅烷处理剂对气凝胶粉体原料进行改性包覆,避免了制备复合聚氨酯过程中气凝胶结构被其他水相或油相成分破坏。
将亲水气凝胶粉体原料经过硅烷处理剂包覆处理成为疏水气凝胶,然后添加亲水剂再次搅拌,最后与分散剂、乳化剂、水性乳液、聚乙烯醇、聚乙二醇和多元醇,分散到水中形成膏体,然后将膏体喷雾干燥,得到所述的改性包覆气凝胶颗粒。
基于上述技术方案,可以适用于亲水气凝胶粉体原料。
将疏水气凝胶粉体原料与亲水剂研磨改性,然后再与分散剂、乳化剂、水性乳液、聚乙烯醇、聚乙二醇和多元醇,分散到水中形成膏体,然后将膏体喷雾干燥,得到改性包覆气凝胶颗粒。
基于上述技术方案,可以适用于疏水气凝胶粉体原料。
具体的,所述步骤2)包括以下具体步骤:向所述聚氨酯制备A料中加入步骤1)得到的所述改性包覆气凝胶颗粒,然后高速搅拌,直至所述聚氨酯制备A料呈现白色,然后加聚氨酯制备B料,搅拌,发泡,再在室温下熟化,得到所述的气凝胶复合聚氨酯。
基于上述技术方案,可以结合现有的A、B料法,在制备聚氨酯的过程中复合改性包覆气凝胶颗粒,得到改性包覆气凝胶颗粒。
具体的,所述硅烷处理剂选自乙基三氧乙基硅烷,二乙基二氧乙基硅烷、甲基三氧乙基硅烷、多聚硅氧烷、二甲基二氯硅烷、辛基三甲氧基硅烷、辛基三乙氧基硅烷、六甲基二硅氮烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷、十六烷基三甲氧基硅烷、十六烷基三乙氧基硅烷、二甲基聚硅氧烷、缩水甘油氧基丙基三甲氧基硅烷、缩水甘油氧基丙基三乙氧基硅烷、九氟代己基三甲氧基硅烷、十三氟代辛基三甲氧基硅烷、十三氟代辛基三乙氧基硅烷或氨丙基三乙氧基硅烷中的任意一种或多种的组合。
具体的,所述的亲水剂为二甲基二氧乙基硅烷聚二烯丙基二甲基氯化铵、十六烷基三甲基溴化铵。
以二乙基二氧乙基硅烷和亲水气凝胶为例:
其完全水解后,生成乙醇和二硅醇基其中,二硅醇基与自身和气凝胶中的四羟基硅烷缩合,得到网状结构,此时气凝胶不亲水,亲油;
采用十六烷基三甲基溴化铵再进行处理,烷基与上述的网状结构通过弱力结合,亲水的铵根基团暴露在外面,其改性后气凝胶变为亲水的表面。这样就形成一种外亲水内亲油的结构。这种结构可以分散在水性体系中,但水不会破坏气凝胶结构。然后我们加入乳液和分散剂将这种颗粒进行包覆,最后喷雾干燥即可。此时这个结构起着很好的保护内部气凝胶的作用,可以在油性环境或水性环境中使用。在PU的A、B料混合中最大程度的保护了气凝胶的微观结构。
对于疏水气凝胶,则可以直接用亲水剂处理以进行包覆。
具体的,所述的分散剂选自二(2-乙基己基)琥珀酸酯磺酸钠、支化的烷基二甲基氧化胺、辛基苯氧基聚乙氧基乙醇、TWEEN 100表面活性剂、BASF聚氧丙烯表面活性剂、二醇、烷氧基化物聚氧基亚烷基脂肪醚、聚合物型表面活性剂、Renex非离子表面活性剂、醇乙氧基化物、醇烷氧基化物、氧化乙烯、氧化丙烯嵌段共聚物、脱水山梨糖醇酯的聚氧乙烯衍生物中的任意一种或多种的混合。
具体的,乳化剂选自PO-10乳化剂或CA90乳化剂。
具体的,水性乳液选自丙烯酸水性乳液、聚氨酯水性乳液或氟硅水性乳液中的任意一种或多种的混合。
具体的,所述改性包覆气凝胶颗粒的粒径为1~50μm,导热系数小于0.020W/(m·K)。
本发明还提供了上述制备方法制备得到的气凝胶复合聚氨酯。
具体实施方式
以下对本发明的原理和特征进行描述,所举实施例只用于解释本发明,并非用于限定本发明的范围。
实施例1:
采用甲基三氧乙基硅烷、乙醇水溶液和亲水气凝胶在50℃中搅拌反应3h,然后干燥得到疏水改性的气凝胶粉体,然后先加入亲水剂十六烷基三甲基溴化铵的水分散体,进行亲水改性。疏水改性时,甲基三氧乙基硅烷:乙醇水溶液(80%):亲水气凝胶质量比例为,10:50:5。亲水改性时的物料质量比例为:改性的气凝胶粉体:十六烷基三甲基溴化铵:水=5:2:95
在上述的分散体中继续加入PO-10乳化剂、731A分散剂、润湿剂W-1855,SY-3000水性聚氨酯乳液的水相中,分散体:乳化剂:分散剂:润湿剂:聚氨酯乳液含量配比为75:1:2:2:15,高速分散成膏体,再喷雾干燥成为10μm大小的粉体颗粒待用。
1)、A料:聚醚4110,苯酐聚醚多元醇,催化剂,匀泡剂,发泡剂,水;
2)、B料:二苯甲基二异氰酸酯;
3)、步骤:A料中加入上述改性的气凝胶粉体颗粒,高速搅拌2000r/min,直至A料呈现白色,后加入B料,快速搅拌,自由发泡,在室温下熟化,切割成标准样再进行测试。
按照以上方法分别制备了1%~4%气凝胶含量的复合聚氨酯,结果如表1所示。
实施例2
使用AG-D 15μm疏水气凝胶粉体。将粉体分散在含有亲水剂氨丙基三乙氧基硅烷、聚乙烯醇的水相处理液中,高速分散搅拌均匀进行亲水改性,气凝胶、氨丙基三乙氧基硅烷、聚乙烯醇:水的质量比为6:10:5:90。在上述分散体中再加入含有CA90乳化剂、1120分散剂、润湿剂W-1855,SY-3000水性聚氨酯乳液,高速分散成为膏体,其中分散体:乳化剂:分散剂:润湿剂:聚氨酯乳液:质量比为80:1:2:3:20,将膏体喷雾干燥成为5μm大小的粉体颗粒待用。
加入聚氨酯的方法同上:数据如下表2所述
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种气凝胶复合聚氨酯的制备方法,其特征在于,包括以下步骤:
1)采用硅烷处理剂对气凝胶粉体原料进行改性,并包覆成膜,制备得到改性包覆气凝胶颗粒;
2)将步骤1)得到的改性包覆气凝胶颗粒与聚氨酯制备A料混合,再与聚氨酯制备B料反应,制备得到所述的气凝胶复合聚氨酯。
2.根据权利要求1所述的气凝胶复合聚氨酯的制备方法,其特征在于,所述步骤1)包括以下具体步骤:将亲水气凝胶粉体原料经过硅烷处理剂包覆处理成为疏水气凝胶,然后添加亲水剂再次搅拌,最后与分散剂、乳化剂、水性乳液、聚乙烯醇、聚乙二醇和多元醇,分散到水中形成膏体,然后将膏体喷雾干燥,得到所述的改性包覆气凝胶颗粒。
3.根据权利要求1所述的气凝胶复合聚氨酯的制备方法,其特征在于,所述步骤1)包括以下具体步骤:将疏水气凝胶粉体原料与亲水剂研磨改性,然后再与分散剂、乳化剂、水性乳液、聚乙烯醇、聚乙二醇和多元醇,分散到水中形成膏体,然后将膏体喷雾干燥,得到改性包覆气凝胶颗粒。
4.根据权利要求1所述的气凝胶复合聚氨酯的制备方法,其特征在于,所述步骤2)包括以下具体步骤:向所述聚氨酯制备A料中加入步骤1)得到的所述改性包覆气凝胶颗粒,然后高速搅拌,直至所述聚氨酯制备A料呈现白色,然后加聚氨酯制备B料,搅拌,发泡,再在室温下熟化,得到所述的气凝胶复合聚氨酯。
5.根据权利要求2所述的气凝胶复合聚氨酯的制备方法,其特征在于:所述硅烷处理剂选自乙基三氧乙基硅烷,二乙基二氧乙基硅烷、甲基三氧乙基硅烷、多聚硅氧烷、二甲基二氯硅烷、辛基三甲氧基硅烷、辛基三乙氧基硅烷、六甲基二硅氮烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷、十六烷基三甲氧基硅烷、十六烷基三乙氧基硅烷、二甲基聚硅氧烷、缩水甘油氧基丙基三甲氧基硅烷、缩水甘油氧基丙基三乙氧基硅烷、九氟代己基三甲氧基硅烷、十三氟代辛基三甲氧基硅烷、十三氟代辛基三乙氧基硅烷或氨丙基三乙氧基硅烷中的任意一种或多种的组合。
6.根据权利要求3所述的气凝胶复合聚氨酯的制备方法,其特征在于:所述的亲水剂为二甲基二氧乙基硅烷聚二烯丙基二甲基氯化铵、十六烷基三甲基溴化铵。
7.根据权利要求2或3所述的气凝胶复合聚氨酯的制备方法,其特征在于:所述的分散剂选自二(2-乙基己基)琥珀酸酯磺酸钠、支化的烷基二甲基氧化胺、辛基苯氧基聚乙氧基乙醇、TWEEN 100表面活性剂、BASF聚氧丙烯表面活性剂、二醇、烷氧基化物聚氧基亚烷基脂肪醚、聚合物型表面活性剂、Renex非离子表面活性剂、醇乙氧基化物、醇烷氧基化物、氧化乙烯、氧化丙烯嵌段共聚物、脱水山梨糖醇酯的聚氧乙烯衍生物中的任意一种或多种的混合;乳化剂选自PO-10乳化剂或CA90乳化剂;水性乳液选自丙烯酸水性乳液、聚氨酯水性乳液或氟硅水性乳液中的任意一种或多种的混合。
8.根据权利要求1至6任一所述的气凝胶复合聚氨酯的制备方法,其特征在于:所述改性包覆气凝胶颗粒的粒径为1~50微米,导热系数小于0.020W/(m·K)。
9.一种根据权利要求1至7任一所述的制备方法制备得到的气凝胶复合聚氨酯。
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