CN111703169B - 一种复合隔热板及其制备方法 - Google Patents

一种复合隔热板及其制备方法 Download PDF

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CN111703169B
CN111703169B CN202010670401.3A CN202010670401A CN111703169B CN 111703169 B CN111703169 B CN 111703169B CN 202010670401 A CN202010670401 A CN 202010670401A CN 111703169 B CN111703169 B CN 111703169B
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fiber
heat insulation
panel layer
aerogel
water
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CN111703169A (zh
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姚栋嘉
张东生
董会娜
刘喜宗
张继承
吴恒
余启勇
郭金建
杨红霞
王征
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Gongyi Van Research Yihui Composite Material Co Ltd
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Abstract

本发明属于隔热保温技术领域，公开一种复合隔热板及其制备方法。包括第一面板层和隔热层，第一面板层和隔热层之间一体成型；隔热层包括纤维制成的蜂窝结构，蜂窝内填充有气凝胶，蜂窝在和第一面板层相接触面的对面涂覆有隔热涂层；第一面板层为纤维增强树脂基复合片。将第一面板层平铺放置，然后将蜂窝结构叠加放置在第一面板层的上表面；将气凝胶对应的溶胶注入蜂窝结构中，静置老化；将隔热涂料涂刷在蜂窝和第一面板层相接触面的对面，干燥，热压成型，即可。本发明通过将溶胶浸渍于蜂窝结构中，对气凝胶起到很好的固定作用，由于气凝胶占据大部分，因此具有更好的隔热保温效果。

Description

一种复合隔热板及其制备方法
技术领域
本发明属于隔热保温技术领域，具体涉及一种复合隔热板及其制备方法。
背景技术
气凝胶是一种具有纳米级孔径的多孔洞材料，典型的孔洞大小在1-100nm之间，孔洞率在80%以上，内含大量的空气。气凝胶的纳米孔洞结构使得材料的热导率极低，绝热保温效果好。
气凝胶由于比重低、孔洞壁薄，因此具有一定的脆性，直接使用强度不佳。现在工业化的气凝胶有气凝胶布、气凝胶纸、气凝胶板、气凝胶毡和其他气凝胶异形件。气凝胶复合材料因其独特的隔热保温性能，一般将其用作夹层结构防护材料，夹层结构板材通常包括面板层与夹心层，该结构的最大优点是变形协调性能高、抗冲击能力强、尺寸大、隔热效果好、装配简单，解决了传统外防热材料脆性大、掉粉的缺点，提高了设计余量和安全环保特性，已经在管道、建筑墙体、车辆、箱/柜体保温上实现广泛应用。
发明内容
为克服现有技术中存在的不足之处，本发明的目的旨在提供一种复合隔热板及其制备方法。
为实现上述目的，本发明采取的技术方案如下：
一种复合隔热板，其特征在于：包括第一面板层和隔热层，第一面板层和隔热层之间一体成型；所述隔热层包括纤维制成的蜂窝结构，蜂窝内填充有气凝胶，蜂窝在和第一面板层相接触面的对面涂覆有隔热涂层，所述隔热涂层由水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂按质量比（30-60）∶（10-30）∶（2-5）∶（5-40）∶（0.5-5）∶（1-5）组成；所述第一面板层为纤维增强树脂基复合片。
较好地，所述复合隔热板还包括第二面板层，隔热层位于第一面板层和第二面板层之间，第二面板层和隔热层之间亦一体成型，第二面板层与第一面板层的材质相同。
较好地，所述纤维增强树脂基复合片的中树脂为环氧树脂、酚醛树脂、苯并噁嗪树脂、不饱和聚酯、乙烯基酯树脂、硅树脂、氰酸酯树脂中的一种，所述纤维增强树脂基复合片中的纤维为玻璃纤维、碳纤维、石英纤维、高硅氧纤维、硅酸铝纤维、莫来石纤维、碳化硅纤维、氮化硅纤维、氧化铝纤维、氮化硼纤维、玄武岩纤维、水镁石纤维、凹凸棒石纤维、硼纤维、碳纳米管、芳纶纤维、聚酰亚胺纤维、超高分子量聚乙烯纤维中的一种。
较好地，制成蜂窝结构的纤维为玻璃纤维、碳纤维、石英纤维、高硅氧纤维、硅酸铝纤维、莫来石纤维、碳化硅纤维、氮化硅纤维、氧化铝纤维、氮化硼纤维、玄武岩纤维、水镁石纤维、凹凸棒石纤维、硼纤维、碳纳米管、芳纶纤维、聚酰亚胺纤维、超高分子量聚乙烯纤维中的一种；隔热层的气凝胶为二氧化硅气凝胶、碳气凝胶、氧化铝气凝胶、氧化锆气凝胶、氧化钛气凝胶、氧化铁气凝胶、氧化钴气凝胶、氧化镍气凝胶、氧化铜气凝胶、氧化钇气凝胶、氧化铈气凝胶、氧化钒气凝胶、氧化铋气凝胶、氧化锡气凝胶、苯二酚甲醛气凝胶、石墨烯气凝胶中的一种。
较好地，所述水性弹性涂料为水性乙烯-醋酸乙烯弹性涂料、水性有机硅丙弹性涂料、水性丙烯酸类弹性涂料、水性橡胶乳液中的一种；所述水性树脂为水性环氧树脂、水性聚脲树脂、水性酚醛树脂、水性聚氨酯树脂中的一种；所述阻燃剂为磷氮系阻燃剂、无机阻燃剂、DOPO、十溴二苯醚、十溴二苯乙烷中的一种或几种；所述分散剂为BYK-161、BYK-163、BYK-2000中的一种；所述偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂、硼酸酯偶联剂中的一种。
较好地，所述无机阻燃剂为氢氧化铝、氢氧化镁、磷酸铵或硼酸锌，所述磷氮系阻燃剂为聚磷酸铵、异丙基化磷酸三苯酯、蜜胺磷酸盐、蜜胺焦磷酸盐或三聚氰胺氰尿酸盐。
一种所述复合隔热板的制备方法，步骤如下：
（1）、将第一面板层平铺放置，然后将纤维制成的蜂窝结构叠加放置在第一面板层的上表面；
（2）、将气凝胶对应的溶胶注入蜂窝结构中，并在30-60 ℃下静置老化8-24 h；
（3）、按照隔热涂层的组成，将水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂经搅拌混合后得到隔热涂料，然后将其均匀涂刷在步骤（2）所得蜂窝和第一面板层相接触面的对面，得到复合板材；
（4）、将步骤（3）得到的复合板材进行超临界干燥处理；
（5）、干燥完成后，进行热压成型处理，即得到复合隔热板。
较好地，当所述复合隔热板还包括第二面板层时，对应的步骤（3）为：按照隔热涂层的组成，将水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂经搅拌混合后得到隔热涂料，然后将其均匀涂刷在步骤（2）所得蜂窝和第一面板层相接触面的对面，然后在纤维上表面平铺放置第二面板层，得到复合板材。
较好地，所述热压成型的温度为80-150 ℃，压力为0.5-5 Mpa。
较好地，第一面板层和/或第二面板层采用与其对应的半成品--纤维增强树脂基预浸带代替，这是因为纤维增强树脂基预浸带热压固化后即成为纤维增强树脂基复合片。
本发明中，纤维增强树脂基复合片或纤维增强树脂基预浸带可通过市购或现有技术制备获得。
有益效果：
（1）、本发明通过将溶胶浸渍于纤维蜂窝结构中，对气凝胶起到很好的固定作用，由于气凝胶占据大部分，因此其具有更好的隔热保温效果；
（2）、本发明采用在纤维蜂窝表面涂覆隔热涂料，一来其可以提高隔热层的保温和阻燃效果，其次可以防止蜂窝中气凝胶的掉落，对气凝胶进行很好的封装保护作用，隔热涂层良好的柔性也利于其在后续安装使用过程中的方便程度；
（3）、本发明采用一体化热压成型得到复合隔热板，避免了胶黏剂的使用，具有绿色环保的特性，同时纤维增强树脂基预浸带的热压成型操作简单方便，且面板层与隔热层之间结合性能良好，具备较好的整体性，利于后续整体操作使用。
具体实施方式
以下以二氧化硅气凝胶为例，结合具体实施例，对本发明做进一步说明。应理解，以下实施例仅用于说明本发明而非用于限制本发明的范围。
实施例1
一种复合隔热板，包括第一面板层和隔热层，第一面板层和隔热层之间一体成型；所述隔热层包括玻璃纤维制成的蜂窝结构，蜂窝内填充有二氧化硅气凝胶，蜂窝在和第一面板层相接触面的对面涂覆有隔热涂层，所述隔热涂层由水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂按质量比35∶15∶2∶15∶1∶2组成，所述水性弹性涂料为水性乙烯-醋酸乙烯弹性涂料；所述水性树脂为水性环氧树脂；所述阻燃剂为磷氮系阻燃剂聚磷酸铵；所述分散剂为BYK-161；所述偶联剂为硅烷偶联剂；所述第一面板层为玻璃纤维增强环氧树脂基复合片。
所述复合隔热板的制备方法，步骤如下：
（1）、将与第一面板层对应的玻璃纤维增强环氧树脂基预浸带平铺放置，然后将蜂窝结构叠加放置在玻璃纤维增强环氧树脂基预浸带的上表面；
（2）、取正硅酸乙酯、无水乙醇和水混合均匀，之后依次加入NH4F溶液和氨水搅拌均匀，得到二氧化硅溶胶A；其中，以摩尔比计，正硅酸乙酯∶无水乙醇∶水=1∶8∶2；NH4F溶液的加入量保证以摩尔比计，NH4F∶正硅酸乙酯=0.005∶1；氨水的加入量保证以摩尔比计，NH3∶正硅酸乙酯=0.006∶1；
（3）、将二氧化硅溶胶A注入蜂窝结构中，并在40 ℃下静置老化10 h；
（4）、按照隔热涂层的组成，将水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂经高速搅拌混合后得到隔热涂料，然后将其均匀涂刷在步骤（3）所得蜂窝和玻璃纤维增强环氧树脂基预浸带相接触面的对面，得到复合板材；
（5）、将步骤（4）得到的复合板材进行超临界干燥处理；
（6）、干燥完成后，在100 ℃、0.5 Mpa的条件下进行热压成型处理，即得复合隔热板。
实施例2
一种复合隔热板，包括第一面板层和隔热层，第一面板层和隔热层之间一体成型；所述隔热层包括碳纤维制成的蜂窝结构，蜂窝内填充有二氧化硅气凝胶，蜂窝在和第一面板层相接触面的对面涂覆有隔热涂层，所述隔热涂层由水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂按质量比40∶20∶3∶20∶2∶2组成，所述水性弹性涂料为水性有机硅丙弹性涂料；所述水性树脂为水性聚脲树脂；所述阻燃剂为无机阻燃剂氢氧化铝；所述分散剂为BYK-161；所述偶联剂为钛酸酯偶联剂；所述第一面板层为碳纤维增强酚醛树脂基复合片。
所述复合隔热板的制备方法，步骤如下：
（1）、将与第一面板层对应的碳纤维增强酚醛树脂基预浸带平铺放置，然后将蜂窝结构叠加放置在碳纤维增强酚醛树脂基预浸带的上表面；
（2）、取正硅酸乙酯、无水乙醇和水混合均匀，之后依次加入NH4F溶液和氨水搅拌均匀，得到二氧化硅溶胶A；其中，以摩尔比计，正硅酸乙酯∶无水乙醇∶水=1∶10∶4；NH4F溶液的加入量保证以摩尔比计，NH4F∶正硅酸乙酯=0.008∶1；氨水的加入量保证以摩尔比计，NH3∶正硅酸乙酯=0.01∶1；
（3）、将二氧化硅溶胶A注入蜂窝结构中，并在50 ℃下静置老化12 h；
（4）、按照隔热涂层的组成，将水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂经高速搅拌混合后得到隔热涂料，然后将其均匀涂刷在步骤（3）所得蜂窝和第一面板层相接触面的对面，得到复合板材；
（5）、将步骤（4）得到的复合板材进行超临界干燥处理；
（6）、干燥完成后，在130 ℃、2 Mpa的条件下进行热压成型处理，即得复合隔热板。
实施例3
一种复合隔热板，包括第一面板层、隔热层和第二面板层，隔热层位于第一面板层和第二面板层之间，第一面板层和隔热层之间、第二面板层和隔热层之间一体成型；所述隔热层包括玻璃纤维纤维制成的蜂窝结构，蜂窝内填充有二氧化硅气凝胶，蜂窝在和第一面板层相接触面的对面涂覆有隔热涂层，所述隔热涂层由水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂按质量比55∶25∶4∶35∶3∶4组成，所述水性弹性涂料为水性橡胶乳液；所述水性树脂为水性酚醛树脂；所述阻燃剂为DOPO；所述分散剂为BYK-163；所述偶联剂为铝酸酯偶联剂；所述第一面板层和第二面板层为玻璃纤维增强不饱和聚酯树脂基复合片。
所述复合隔热板的制备方法，步骤如下：
（1）、将与第一面板层对应的玻璃纤维增强不饱和聚酯树脂基预浸带平铺放置，然后将蜂窝结构叠加放置在第一面板层的上表面；
（2）、取正硅酸乙酯、无水乙醇和水混合均匀，之后依次加入NH4F溶液和氨水搅拌均匀，得到二氧化硅溶胶A；其中，以摩尔比计，正硅酸乙酯∶无水乙醇∶水=1∶12∶4；NH4F溶液的加入量保证以摩尔比计，NH4F∶正硅酸乙酯=0.01∶1；氨水的加入量保证以摩尔比计，NH3∶正硅酸乙酯=0.015∶1；
（3）、将二氧化硅溶胶A注入蜂窝结构中，并在60 ℃下静置老化18 h；
（4）、按照隔热涂层的组成，将水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂经高速搅拌混合后得到隔热涂料，然后将其均匀涂刷在步骤（3）所得蜂窝和第一面板层相接触面的对面，然后在纤维上表面平铺放置与第二面板层对应的玻璃纤维增强不饱和聚酯树脂基预浸带，得到复合板材；
（5）、将步骤（4）得到的复合板材进行超临界干燥处理；
（6）、干燥完成后，在120 ℃、3 Mpa的条件下进行热压成型处理，即得复合隔热板。

Claims (8)

1.一种复合隔热板，其特征在于：包括第一面板层和隔热层，第一面板层和隔热层之间一体成型；所述隔热层包括纤维制成的蜂窝结构，蜂窝内填充有气凝胶，蜂窝在和第一面板层相接触面的对面涂覆有隔热涂层，所述隔热涂层由水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂按质量比（30-60）∶（10-30）∶（2-5）∶（5-40）∶（0.5-5）∶（1-5）组成；所述第一面板层为纤维增强树脂基复合片；
所述复合隔热板的制备步骤如下：
（1）、将第一面板层平铺放置，然后将纤维制成的蜂窝结构叠加放置在第一面板层的上表面；
（2）、将与气凝胶对应的溶胶注入蜂窝结构中，并在30-60 ℃下静置老化8-24 h；
（3）、按照隔热涂层的组成，将水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂经搅拌混合后得到隔热涂料，然后将其均匀涂刷在步骤（2）所得蜂窝和第一面板层相接触面的对面，得到复合板材；
（4）、将步骤（3）得到的复合板材进行超临界干燥处理；
（5）、干燥完成后，进行热压成型处理，即得到复合隔热板；
上述制备步骤中，第一面板层为与其对应的纤维增强树脂基预浸带，所述热压成型的温度为80-150 ℃，压力为0.5-5 Mpa。
2.如权利要求1所述的复合隔热板，其特征在于：所述复合隔热板还包括第二面板层，隔热层位于第一面板层和第二面板层之间，第二面板层和隔热层之间亦一体成型，第二面板层与第一面板层的材质相同。
3.如权利要求1或2所述的复合隔热板，其特征在于：所述纤维增强树脂基复合片的中树脂为环氧树脂、酚醛树脂、苯并噁嗪树脂、不饱和聚酯、乙烯基酯树脂、硅树脂、氰酸酯树脂中的一种，所述纤维增强树脂基复合片中的纤维为玻璃纤维、碳纤维、石英纤维、高硅氧纤维、硅酸铝纤维、莫来石纤维、碳化硅纤维、氮化硅纤维、氧化铝纤维、氮化硼纤维、玄武岩纤维、水镁石纤维、凹凸棒石纤维、硼纤维、碳纳米管、芳纶纤维、聚酰亚胺纤维、超高分子量聚乙烯纤维中的一种。
4.如权利要求1或2所述的复合隔热板，其特征在于：制成蜂窝结构的纤维为玻璃纤维、碳纤维、石英纤维、高硅氧纤维、硅酸铝纤维、莫来石纤维、碳化硅纤维、氮化硅纤维、氧化铝纤维、氮化硼纤维、玄武岩纤维、水镁石纤维、凹凸棒石纤维、硼纤维、碳纳米管、芳纶纤维、聚酰亚胺纤维、超高分子量聚乙烯纤维中的一种；隔热层的气凝胶为二氧化硅气凝胶、碳气凝胶、氧化铝气凝胶、氧化锆气凝胶、氧化钛气凝胶、氧化铁气凝胶、氧化钴气凝胶、氧化镍气凝胶、氧化铜气凝胶、氧化钇气凝胶、氧化铈气凝胶、氧化钒气凝胶、氧化铋气凝胶、氧化锡气凝胶、苯二酚甲醛气凝胶、石墨烯气凝胶中的一种。
5.如权利要求1或2所述的复合隔热板，其特征在于：所述水性弹性涂料为水性乙烯-醋酸乙烯弹性涂料、水性有机硅丙弹性涂料、水性丙烯酸类弹性涂料、水性橡胶乳液中的一种；所述水性树脂为水性环氧树脂、水性聚脲树脂、水性酚醛树脂、水性聚氨酯树脂中的一种；所述阻燃剂为磷氮系阻燃剂、无机阻燃剂、DOPO、十溴二苯醚、十溴二苯乙烷中的一种或几种；所述分散剂为BYK-161、BYK-163、BYK-2000中的一种；所述偶联剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂、硼酸酯偶联剂中的一种。
6.如权利要求5所述的复合隔热板，其特征在于：所述无机阻燃剂为氢氧化铝、氢氧化镁、磷酸铵或硼酸锌，所述磷氮系阻燃剂为聚磷酸铵、异丙基化磷酸三苯酯、蜜胺磷酸盐、蜜胺焦磷酸盐或三聚氰胺氰尿酸盐。
7.一种如权利要求1所述的复合隔热板的制备方法，其特征在于，步骤如下：
（1）、将第一面板层平铺放置，然后将纤维制成的蜂窝结构叠加放置在第一面板层的上表面；
（2）、将与气凝胶对应的溶胶注入蜂窝结构中，并在30-60 ℃下静置老化8-24 h；
（3）、按照隔热涂层的组成，将水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂经搅拌混合后得到隔热涂料，然后将其均匀涂刷在步骤（2）所得蜂窝和第一面板层相接触面的对面，得到复合板材；
（4）、将步骤（3）得到的复合板材进行超临界干燥处理；
（5）、干燥完成后，进行热压成型处理，即得到复合隔热板；
上述制备步骤中，第一面板层为与其对应的纤维增强树脂基预浸带，所述热压成型的温度为80-150 ℃，压力为0.5-5 Mpa。
8.如权利要求7所述的复合隔热板的制备方法，其特征在于：当所述复合隔热板还包括第二面板层时，对应的步骤（3）为：按照隔热涂层的组成，将水性弹性涂料、水性树脂、阻燃剂、二氧化硅粉、分散剂、偶联剂经搅拌混合后得到隔热涂料，然后将其均匀涂刷在步骤（2）所得蜂窝和第一面板层相接触面的对面，然后在纤维上表面平铺放置第二面板层，得到复合板材；该步骤中所述的第二面板层为与其对应的纤维增强树脂基预浸带。
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DE19703262A1 (de) * 1997-01-30 1998-08-06 Zae Bayern Mit Pulver oder Granulat gefülltes, transluzentes Wärmeisolationspaneel
CN106007635A (zh) * 2015-03-24 2016-10-12 金承黎 一种表面无尘处理的气凝胶复合材料及制备方法
CN108940139A (zh) * 2017-05-22 2018-12-07 浙江圣润纳米科技有限公司 一种蜂窝基材增强气凝胶复合材料、制品及制备方法

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DE19703262A1 (de) * 1997-01-30 1998-08-06 Zae Bayern Mit Pulver oder Granulat gefülltes, transluzentes Wärmeisolationspaneel
CN106007635A (zh) * 2015-03-24 2016-10-12 金承黎 一种表面无尘处理的气凝胶复合材料及制备方法
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