CN115257087A - 一种气凝胶防水隔热毡及其制作方法 - Google Patents

一种气凝胶防水隔热毡及其制作方法 Download PDF

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CN115257087A
CN115257087A CN202210703952.4A CN202210703952A CN115257087A CN 115257087 A CN115257087 A CN 115257087A CN 202210703952 A CN202210703952 A CN 202210703952A CN 115257087 A CN115257087 A CN 115257087A
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aerogel
felt
fiber
layer
manufacturing
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陈耀森
陈泽清
李文斗
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Xiamen Zhuoshite New Material Technology Co ltd
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Oppson Xiamen Energy Saving New Material Technology Co ltd
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Abstract

本发明公开一种气凝胶防水隔热毡的制作方法，该方法包括以下步骤：(1)先将0.1～1wt％分散剂溶于水或醇水混合物中制成分散剂溶液，再按照分散剂、红外遮光剂、气凝胶粉体的质量比1～5:0.5～2:5～10的比例将分散剂溶液与红外遮光剂、气凝胶粉体均匀混合成气凝胶浆料；(2)将气凝胶浆料通过喷洒、刷涂或浸渍的方式附着在纤维毡的内部和表面；(3)将步骤(2)获得的纤维毡在热辊压机下热压，得到单层气凝胶胚毡；(4)将步骤(3)获得的单层气凝胶胚毡层层铺叠，用针刺机针刺成180～280kg/m3的气凝胶纤维毡；(5)干燥由步骤(4)获得的气凝胶纤维毡；本发明制作的气凝胶毡性能较好，不易掉粉。

Description

一种气凝胶防水隔热毡及其制作方法
技术领域
本发明涉及隔热保温材料领域，尤其是一种气凝胶防水隔热毡及其制作方法。
背景技术
目前市面上的保温材料主要有两大类，一类是有机保温材料，如聚苯板、聚氨酯泡沫板等，这类材料防水性、耐候性好，有一定的保温效果，但这类材料极易燃，燃烧时会释放大量的有害物质，仅能在100℃内的条件下使用；另一类是无机保温材料，如有A级防火性能的岩棉板、硅酸铝针刺毡，这类材料导热系数在0.04W/(m·K)以上，虽然在高温下不燃烧不分解，但是短时间就会被烧穿。
气凝胶是具有三维立体结构的纳米多孔材料，是目前为止导热系数最低的材料，同时具有低密度、高孔隙率、高光透性、高比表面积等性质。但纯气凝胶有骨架脆、机械强度低、韧性差的问题，在实际应用中，往往通过复合增强体来提高气凝胶的力学强度。其中玻璃纤维因具有强度高、韧性好、热稳定性优异及耐高温的性能，成为良好的增强体。因此由玻璃纤维和气凝胶制成的气凝胶毡具有低导热系数、强疏水性和高防火性能的同时，兼具高强度、韧性好的特点。
目前气凝胶毡的制备方法主要包括原位复合法和二次复合法。原位复合法即在气凝胶凝胶时浸入纤维毡，再通过对复合材料进行改性的方法，该方法耗时长，工艺复杂，设备投入高，对企业的生产要求高。二次复合法即先制备气凝胶粉体，再将气凝胶粉体通过一定的技术手段和纤维毡复合，该方法便于施工。但目前为止的二次复合法主要是浸渍法和长纱网抄取法，前者工作效率低，制备的材料性能较差，后者需要对设备投入较高，两种方法的掉粉问题也是目前亟待解决的一大问题。
发明内容
为此，本发明为解决上述问题，提供一种气凝胶防水隔热毡及其制作方法，通过二次复合法解决气凝胶毡易掉粉问题，且制作的气凝胶毡性能较好。
为达到上述目的，本发明的技术方案是：一种气凝胶防水隔热毡的制作方法，该方法包括以下步骤：
(1)先将0.1～1wt％分散剂溶于水或醇水混合物中制成分散剂溶液，再按照分散剂、红外遮光剂(红外遮光剂视产品使用温度、硅源的不同等情况酌情添加)、气凝胶粉体的质量比1～5:0.5～2:5～10的比例将分散剂溶液与红外遮光剂、气凝胶粉体均匀混合成气凝胶浆料；
(2)将气凝胶浆料通过喷洒、刷涂或浸渍的方式附着在纤维毡的内部和表面；
(3)将步骤(2)获得的纤维毡在热辊压机下热压，得到单层气凝胶胚毡；
(4)将步骤(3)获得的单层气凝胶胚毡层层铺叠，用针刺机针刺成180～280kg/m3的气凝胶纤维毡；
(5)干燥由步骤(4)获得的气凝胶纤维毡。
作为优选，再用热压机对步骤(5)中得到的气凝胶纤维毡热压定型，形成厚度一致的气凝胶纤维毡产品。
更优选的，热压机压力大于3t。
进一步改进，所述气凝胶粉体为任意一种疏水的气凝胶粉体，包括氧化铝气凝胶、二氧化硅气凝胶、氧化钛气凝胶中的一种或多种的组合。
所述分散剂包括但不限于2,2-乙基己基硫代琥珀酸钠、异构十醇、异构十三醇、脂肪醇聚氧乙烯醚、十二烷基苯磺酸钠、聚氧乙烯失水山梨醇脂肪酸酯、失水山梨醇脂肪酸酯、丁二酸二异辛酯磺酸钠，也可以是上述中一种或多种的组合。所选用的分散剂优选为可以在干燥或热压的过程中分散，分散剂的用量取决于气凝胶粉体的颗粒大小和水的用量，粒径更小的气凝胶颗粒需要更多的分散剂，含水越多，分散剂用量也越高。
所述红外遮光剂包括但不限于炭黑、二氧化钛、氧化铁、二氧化锆、钛白粉，也可以是上述中的一种或多种的组合。
进一步改进，当使用浸渍或喷洒的方法与纤维毡复合时，需要获得有一定流动性的浆液，可以将水替换为醇水混合物，所述醇水混合物为甲醇或乙醇的一种，其中醇占醇水混合物的10％～70％。
进一步改进，步骤(1)中的原料依次加入分散机中进行搅拌，当上一物质分散均匀后才能加入下一种物质，分散机转速1500r/min，搅拌20-30分钟。另外，所述气凝胶浆料需现配现用，若放置时间过长则浆料会发生分层、气凝胶分散不均匀等情况影响后续气凝胶和纤维毡的结合密度。优选所述分散机为涡轮式搅拌器。
进一步改进，步骤(2)中纤维毡为玻璃纤维毡、陶瓷纤维毡、石棉纤维毡、氧化铝纤维毡、玄武岩纤维毡、陶瓷纤维毡中任意一种。优选纤维毡为多根纤维同向平行等距排列组成，纤维毡中的每根纤维的长度为8～11cm，纤维直径＜10μm，纤维毡总厚度不超过1mm。
进一步改进，为了使纤维毡含有更多的气凝胶，步骤(2)中喷洒或刷涂于纤维毡上的气凝胶浆料厚度要保证足够的前提下尽量薄，使得纤维毡和气凝胶的含量达到合适的比例，经过多次测试，厚度在0.02～0.5mm为佳。优选厚度为0.02～0.2mm。
进一步改进，为了使纤维毡具有足够的保温隔热效果，步骤(4)中针刺后的气凝胶纤维毡厚度不超过10mm。优选厚度为3～10mm。
进一步改进，步骤(5)中的干燥方式为传统的热风循环干燥方式或真空干燥，干燥时间随着温度的上升而降低。
进一步改进，还包括步骤(6)在步骤(5)得到的气凝胶纤维毡一面胶合铝箔，另一面胶合含胶的离型膜，形成可以直接自粘使用的气凝胶纤维毡。
再进一步，所述胶合采用的胶为丙烯酸树脂、苯丙乳液、硅丙乳液、聚氨酯乳液、环氧树脂乳液、白乳胶中一种或多种的组合，所述离型膜为市面上任何一种含有双面胶的离型膜或者在离型膜上涂覆上述胶水。
由于铝箔层的胶水基本没有保温隔热效果，所以胶水的量要保证铝箔层粘合在纤维毡上的前提下尽量薄，为达到使用效果，优选铝箔层的厚度为0.02～0.5mm，胶水层的厚度小于0.04mm。
本发明还提供了由上述方法制作得到的气凝胶防水隔热毡。
通过本发明提供的技术方案，具有如下有益效果：
通过二次复合法，采用一定的技术手段使气凝胶均匀分布在纤维毡的内部和表面，制作出的气凝胶毡不易掉粉；同时，该制作方法对设备要求低，能耗少，制作而成的气凝胶毡防水隔热性能好，柔性好。
具体实施方式
一种气凝胶防水隔热毡的制作方法，该方法包括以下步骤：
(1)先将0.1～1wt％分散剂溶于水或醇水混合物中制成分散剂溶液，再按照分散剂、红外遮光剂、气凝胶粉体的质量比1～5:0.5～2:5～10的比例将分散剂溶液与红外遮光剂、气凝胶粉体均匀混合成气凝胶浆料；
(2)将气凝胶浆料通过喷洒、刷涂或浸渍的方式附着在纤维毡的内部和表面；
(3)将步骤(2)获得的纤维毡在热辊压机下热压，得到单层气凝胶胚毡；
(4)将步骤(3)获得的单层气凝胶胚毡层层铺叠，用针刺机针刺成180～280kg/m3的气凝胶纤维毡；
(5)干燥由步骤(4)获得的气凝胶纤维毡。
作为优选，再用热压机对步骤(5)中得到的气凝胶纤维毡热压定型，形成厚度一致的气凝胶纤维毡产品。
更优选的，热压机压力大于3t。
(6)在步骤(5)得到的气凝胶纤维毡一面胶合铝箔，另一面胶合含胶的离型膜，形成可以直接自粘使用的气凝胶纤维毡。
所述气凝胶粉体为任意一种疏水的气凝胶粉体，包括氧化铝气凝胶、二氧化硅气凝胶、氧化钛气凝胶中的一种或多种的组合。
所述分散剂包括但不限于2,2-乙基己基硫代琥珀酸钠、异构十醇、异构十三醇、脂肪醇聚氧乙烯醚、十二烷基苯磺酸钠、聚氧乙烯失水山梨醇脂肪酸酯、失水山梨醇脂肪酸酯、丁二酸二异辛酯磺酸钠，也可以是上述中一种或多种的组合。
所述红外遮光剂包括但不限于炭黑、二氧化钛、氧化铁、二氧化锆、钛白粉，也可以是上述中的一种或多种的组合。
下面具体的实施方式对本发明作进一步详细说明。
实施例一：将198g水和2g 2,2-乙基己基硫代琥珀酸钠混合均匀制成分散剂溶液，再加入10g氧化铝气凝胶和0.5g钛白粉，当上一物质分散均匀后才能加入下一种物质，混合均匀后获得气凝胶浆料；将玻璃纤维毡平铺，用滚筒刷将气凝胶浆料刷涂在厚度为0.2mm的玻璃纤维毡上，将气凝胶纤维毡置于热辊压机中热压一遍，再将单层气凝胶纤维毡层叠，针刺制成240kg/m3气凝胶毡，将针刺成的气凝胶纤维毡置于150℃的烘箱中2h，即得气凝胶纤维毡，所述气凝胶纤维毡的导热系数为0.025W/(m·K)，使用过程中掉粉较少。
实施例二：396.5g水和2g分散剂，分散剂为异构十三醇、山梨醇酐月桂酸酯和聚氧乙烯山梨醇酐单硬脂酸酯按照2:1:2混合的混合物，混合均匀后，再依次加入1.5g钛白粉、8g二氧化硅气凝胶粉体，混合均匀后获得气凝胶浆料；用喷枪装取所制得的气凝胶浆液，喷洒0.1mm的浆液于平铺的厚度为1mm的玻璃纤维毡上，将单层气凝胶纤维毡置于热辊压机中热压一遍，将单层气凝胶纤维毡层叠，针刺制成230kg/m3气凝胶毡，将针刺成的气凝胶纤维毡置于120℃的烘箱中5h，即得气凝胶纤维毡，所述气凝胶纤维毡的导热系数为0.027W/(m·K)，使用过程中掉粉较少。
实施例三：将乙醇浓度为30％的醇水混合物200克，1.5g丁二酸二异辛酯磺酸钠混合均匀，再依次加入1g氧化铁和5g氧化钛气凝胶，混合均匀后获得气凝胶浆液；将0.05mm纤维毡浸渍于气凝胶浆料中，将单层气凝胶纤维毡置于热辊压机中热压一遍，将单层气凝胶纤维毡层叠，针刺制成210kg/m3气凝胶毡，将针刺成的气凝胶纤维毡置于110℃的烘箱中6h，即得气凝胶纤维毡，所述气凝胶纤维毡的导热系数为0.028W/(m·K)，使用过程中掉粉较少。
对比实施例：按照传统的原位复合法制备气凝胶毡：将正硅酸乙酯：水：乙醇按体积比1:4:8混合，加入0.1mol/L盐酸将pH调至2～3，在水浴锅45℃下搅拌12h，按照正硅酸乙酯:甲酰胺体积比1:0.5加入甲酰胺，将pH调至7～8，在凝胶前浸入纤维毡，凝胶后将整体至于乙醇中老化12h后，至于含正硅酸乙酯的溶液中继续老化12h，后按照乙醇和正己烷1:1、1:3分别浸泡进行12h、正己烷的浸泡12h进行三次溶剂置换，再用三甲基氯硅烷进行表面改性，用正己烷、乙醇和正己烷1:1的溶液分别浸泡12h进行清洗，最后至于烘箱中80℃、100℃、150℃分别干燥2h、5h、2h，即可制得气凝胶纤维毡，所得气凝胶纤维毡的导热系数为0.026W/(m·K)，使用过程中较容易出现掉粉的情况。
上述可得，本发明提供的一种气凝胶防水隔热毡制作方法制得的气凝胶毡与传统方法制得的气凝胶毡导热性能相近，但该方法制作工艺简单，掉粉较少。
尽管结合优选实施例具体展示和介绍了本发明，但所属领域的技术人员应该明白，在不脱离所附权利要求书所限定的本发明的精神和范围内，在形式上和细节上可以对本发明做出各种变化，均为本发明的保护范围。

Claims (10)

1.一种气凝胶防水隔热毡的制作方法，其特征在于：该方法包括以下步骤：
(1)先将0.1～1wt％分散剂溶于水或醇水混合物中制成分散剂溶液，再按照分散剂、红外遮光剂、气凝胶粉体的质量比1～5:0.5～2:5～10的比例将分散剂溶液与红外遮光剂、气凝胶粉体均匀混合成气凝胶浆料；
(2)将气凝胶浆料通过喷洒、刷涂或浸渍的方式附着在纤维毡的内部和表面；
(3)将步骤(2)获得的纤维毡在热辊压机下热压，得到单层气凝胶胚毡；
(4)将步骤(3)获得的单层气凝胶胚毡层层铺叠，用针刺机针刺成180～280kg/m3的气凝胶纤维毡；
(5)干燥由步骤(4)获得的气凝胶纤维毡。
2.根据权利要求1所述的一种气凝胶防水隔热毡的制作方法，其特征在于：所述气凝胶粉体为氧化铝气凝胶、二氧化硅气凝胶、氧化钛气凝胶中的一种或多种的组合；
所述分散剂为2,2-乙基己基硫代琥珀酸钠、异构十醇、异构十三醇、脂肪醇聚氧乙烯醚、十二烷基苯磺酸钠、聚氧乙烯失水山梨醇脂肪酸酯、失水山梨醇脂肪酸酯中的一种或多种的组合；
所述红外遮光剂为炭黑、二氧化钛、氧化铁、二氧化锆、钛白粉中的一种或多种的组合。
3.根据权利要求1所述的一种气凝胶防水隔热毡的制作方法，其特征在于：步骤(1)中的原料依次加入分散机中进行搅拌，当上一物质分散均匀后才能加入下一种物质，分散机转速1500r/min，搅拌20-30分钟。
4.根据权利要求1所述的一种气凝胶防水隔热毡的制作方法，其特征在于：步骤(2)中纤维毡为玻璃纤维毡、陶瓷纤维毡、石棉纤维毡、氧化铝纤维毡、玄武岩纤维毡、陶瓷纤维毡中任意一种；优选纤维毡为多根纤维同向平行等距排列组成，纤维毡中的每根纤维的长度为8～11cm，纤维直径＜10μm，纤维毡总厚度不超过1mm。
5.根据权利要求1所述的一种气凝胶防水隔热毡的制作方法，其特征在于：步骤(2)中喷洒或刷涂于纤维毡上的气凝胶浆料厚度为0.02～0.5mm；优选厚度为0.02～0.2mm。
6.根据权利要求1所述的一种气凝胶防水隔热毡的制作方法，其特征在于：步骤(4)中针刺后的气凝胶纤维毡厚度不超过10mm；优选厚度为3～10mm。
7.根据权利要求1所述的一种气凝胶防水隔热毡的制作方法，其特征在于：步骤(5)中的干燥方式为传统的热风循环干燥方式或真空干燥，干燥时间随着温度的上升而降低。
8.根据权利要求1所述的一种气凝胶防水隔热毡的制作方法，其特征在于：还包括步骤(6)在步骤(5)得到的气凝胶纤维毡一面胶合铝箔，另一面胶合含胶的离型膜，形成可以直接自粘使用的气凝胶纤维毡。
9.根据权利要求8所述的一种气凝胶防水隔热毡的制作方法，其特征在于：所述胶合采用的胶为丙烯酸树脂、苯丙乳液、硅丙乳液、聚氨酯乳液、环氧树脂乳液、白乳胶中一种或多种的组合，所述离型膜为市面上任何一种含有双面胶的离型膜或者在离型膜上涂覆上述胶水；优选铝箔层的厚度为0.02～0.5mm，胶水层的厚度小于0.04mm。
10.由权利要求1～9中任意一项所述的方法制作得到的气凝胶防水隔热毡。
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