CN111016332A - 一种隔热保温真空板的制备方法 - Google Patents

一种隔热保温真空板的制备方法 Download PDF

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CN111016332A
CN111016332A CN201911367478.7A CN201911367478A CN111016332A CN 111016332 A CN111016332 A CN 111016332A CN 201911367478 A CN201911367478 A CN 201911367478A CN 111016332 A CN111016332 A CN 111016332A
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fiber
heat
layer
resin
biomass
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姚栋嘉
吕多军
吴恒
董会娜
何凤霞
陈帅
刘喜宗
张东生
张继承
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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板材制备领域，公开一种隔热保温真空板的制备方法。将生物质纤维材料置于二氧化硅溶胶中浸渍，然后静置老化，疏水化处理，接着溶剂置换、干燥，得到生物质/二氧化硅复合气凝胶作为夹芯保温层；对夹心保温层进行封装处理；在封装完成的夹心保温层外部设置覆膜层，通过抽真空的方式在覆膜层内形成真空层；在覆膜层外部粘贴一层预浸带，即得隔热保温真空板。本发明充分发挥气凝胶的隔热保温性能，同时又可以实现资源再利用；本发明在隔热保温真空板外层胶黏预浸带，进一步提高隔热保温真空板的耐久性及外界环境的破坏性。

Description

一种隔热保温真空板的制备方法
技术领域
本发明属于隔热保温板材制备领域，具体涉及一种隔热保温真空板的制备方法。
背景技术
当今，全球保温隔热材料正朝着高效、节能、薄层、隔热、防水的方向发展，目前在我国，岩棉、玻璃棉、膨胀珍珠岩等传统保温材料仍占据主要市场，这些材料尽管价格比较低，但密度大、保温隔热性能差、铺设较厚材料损耗量大、吸湿性高、抗震性能和环保性能较差，使用这些保温材料无法达到节能标准，另外石棉和玻璃棉等建筑保温材料本身就带有大量的有害物质，无法满足人类的健康要求。
与传统隔热保温材料相比，气凝胶是一种具有高比表面积、高孔隙率、低堆积密度、以及比室温空气更低的热导率的多孔纳米材料。由于气凝胶具有独特的纳米结构，将气凝胶用于保温隔热材料，可达到节能、轻质、高效的效果。
真空绝热板（VIP板）是一种超绝热的保温材料，因它的导热系数极低，所以在满足相同保温技术要求时，具有保温层厚度薄、体积小、重量轻的优点，适用于节能要求较高和要求保温材料体积小、重量轻、有较大技术经济意义的场合。将气凝胶用于真空板领域已经得到研究，如中国实用新型专利200420053407.2公开一种真空绝热板，包括外壳和设置在真空外壳中的绝热芯材，所述芯材包括二氧化硅气凝胶和玻璃纤维，所述玻璃纤维交织于二氧化硅气凝胶之间，并在芯材表面设置红外反射层；所述外壳层为层叠袋或硬质金属或玻璃板。但是现有技术中，隔热性能并没有得到改进且使用寿命有限。为了提高板材的隔热性能，目前通过降低芯部密度来改进VIP产品的导热性能已经成为研究的热点。
发明内容
为解决上述问题，本发明的目的在于提供一种隔热保温真空板的制备方法。
为实现上述目的，本发明采取的技术方案如下：
一种隔热保温真空板的制备方法，步骤如下：
（1）、取正硅酸酯、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；其中，以摩尔比计，正硅酸酯∶乙醇∶水=1∶（4~12）∶（2~4）；NH4F溶液的加入量保证以摩尔比计，NH4F∶正硅酸酯=（0.002~0.01）∶1；氨水的加入量保证以摩尔比计，NH3∶正硅酸酯=（0.005~0.015）∶1；
（2）、将生物质纤维材料压结成毡后，置于步骤（1）所得二氧化硅溶胶中浸渍，然后在30~60 ℃下静置老化8~24 h，得到生物质/二氧化硅复合凝胶；
（3）、将步骤（2）所得生物质/二氧化硅复合凝胶置于改性溶液中进行疏水化改性处理，接着进行溶剂置换，再干燥处理，得到生物质/二氧化硅复合气凝胶作为夹芯保温层；
（4）、对步骤（3）所得夹心保温层进行封装处理；
（5）、在步骤（4）封装完成的夹心保温层外部设置覆膜层，通过抽真空的方式在覆膜层内形成真空层；
（6）、在步骤（5）所得夹芯保温层的覆膜层外部粘贴一层纤维增强树脂预浸带，即得隔热保温真空板。
较好地，步骤（1）中，所述正硅酸酯为正硅酸甲酯、正硅酸乙酯、正硅酸丁酯或正硅酸异丙酯。
较好地，步骤（2）中，所述生物质纤维为农作物秸秆纤维、木纤维、竹纤维，生物质纤维的直径≥10cm，长径比≥1000。
较好地，步骤（2）中，浸渍的时间为12~24 h。
较好地，步骤（3）中，所述改性溶液为疏水化改性剂与无水乙醇按摩尔比1∶（2~5）组成的混合液，疏水化处理时间为12~24 h；所述疏水化改性剂为甲基三甲氧基硅烷、甲基三乙氧基硅烷、三甲基甲氧基硅烷、三甲基乙氧基硅烷、二甲基二甲氧基硅烷、二甲基二乙氧基硅烷、二乙基二甲氧基硅烷、四乙氧基硅烷、六甲基二硅氧烷、七甲基三硅氧烷、辛基三乙氧基硅烷、甲基三氯硅烷、三甲基氯硅烷、二甲基二氯硅烷、乙基三氯硅烷或二乙基二氯硅烷。
较好地，步骤（3）中，利用无水乙醇进行溶剂置换，置换次数为2~3次，每次置换的时间为12~36 h。
较好地，步骤（4）中，封装时采用的封装材料为PET膜、PI膜、PE膜、PEEK膜或PTFE膜。
较好地，步骤（5）中，所述覆膜层为内侧设置有热熔胶层的铝塑膜。
较好地，步骤（6）中，采用胶黏剂粘接预浸带，所述胶黏剂为环氧树脂胶、丙烯酸树脂胶黏剂、酚醛树脂胶黏剂、聚氨酯胶胶黏剂、有机硅树脂胶黏剂、光学环氧胶或聚乙烯醇缩醛胶。
较好地，步骤（6）中，所述纤维增强树脂预浸带中的纤维为碳纤维、玻璃纤维、芳族聚酰胺纤维、生物质纤维、莫来石纤维、石英纤维、硅酸铝纤维、陶瓷纤维、氧化铝纤维、岩棉纤维、玄武岩纤维或有机纤维；纤维增强树脂预浸带中的树脂为有机硅树脂、环氧树脂、酚醛树脂、聚酰亚胺树脂、氰酸酯树脂、聚酯树脂、聚酰胺树脂或聚醚醚酮树脂。并且，这些纤维增强树脂预浸带均可通过市购获得或者按现有制备方法制备获得。
有益效果：生物质纤维材料具有可再生性、低污染性、广泛分布性、资源丰富、易于生物降解，有利于资源再利用，而气凝胶是由胶体粒子相互聚积形成的纳米多孔材料，具有大的比表面积、低密度、平均孔径小、高孔隙率、低导热系数的特点，本发明通过将生物质纤维压结成毡，然后在二氧化硅溶胶中浸渍得到夹芯保温层，这样做可以使得夹心保温层充分发挥气凝胶的隔热保温性能，同时又可以实现资源再利用；为了进一步提高本发明隔热保温真空板的耐久性及外界环境的破坏性，本发明在隔热保温真空板外层胶黏预浸带，因其具有耐磨耗性、耐蚀性、耐冲击性、轻量化等特性，防止传统的隔热真空板因其外层覆膜材料破坏造成的真空度的破坏及降低，同时外层预浸带良好的力学性能避免高温时覆膜层发生软化导致板材变形，本发明隔热保温真空板可作为室内装潢、隔间木材的防火、隔热，或在建筑、工业厂房用耐火隔热材上实现广泛应用。
具体实施方式
以下结合具体实施例，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
一种隔热保温真空板的制备方法，步骤如下：
（1）、取正硅酸甲酯、无水乙醇和水混合均匀，之后依次加入2 mol/L的NH4F溶液和0.2moL/L的氨水搅拌均匀，得到二氧化硅溶胶，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=0.008∶1，氨水的加入量保证以摩尔比计，NH3∶正硅酸乙酯=0.01∶1；
（2）、将麦秸秆纤维（直径≥10cm，长径比≥1000）压结成毡后，置于步骤（1）所得二氧化硅溶胶中浸渍24 h后，在30 ℃下静置老化18 h，得到生物质/二氧化硅复合凝胶；
（3）、将步骤（2）所得生物质/二氧化硅复合凝胶置于改性液中疏水改性处理16 h，接着用无水乙醇进行溶剂置换2次，每次置换的时间为30 h，再超临界干燥处理，即得生物质/二氧化硅复合气凝胶，作为夹芯保温层；其中，所述改性液为改性剂与无水乙醇按摩尔比1∶5组成的混合液，所述改性剂为甲基三甲氧基硅烷；
（4）、将步骤（3）所得夹心保温层外覆PTFE膜进行防掉粉封装；
（5）、将步骤（4）封装完成的夹心保温层外覆内侧有热熔胶层的铝塑膜作为覆膜层，通过抽真空的方式在覆膜层内形成真空层；
（6）、在步骤（5）所得夹芯保温层的覆膜层外部通过环氧树脂胶黏剂粘贴一层碳纤维增强环氧树脂预浸带，即得隔热保温真空板。
实施例2
一种隔热保温真空板的制备方法，步骤如下
（1）、取正硅酸乙酯、无水乙醇和水混合均匀，之后依次加入2 mol/L的NH4F溶液和0.2moL/L的氨水搅拌均匀，得到二氧化硅溶胶，其中，以摩尔比计，正硅酸乙酯∶无水乙醇∶水=1∶10∶3；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；
（2）、将木质纤维（直径≥10cm，长径比≥1000）压结成毡后，置于步骤（1）所得二氧化硅溶胶中浸渍12 h后，在60 ℃下静置老化8 h，得到生物质/二氧化硅复合凝胶；
（3）、将步骤（2）所得生物质/二氧化硅复合凝胶置于改性液中疏水改性处理12 h，接着用无水乙醇进行溶剂置换3次，每次置换的时间为18 h，再超临界干燥处理，即得生物质/二氧化硅复合气凝胶，作为夹芯保温层；其中，所述改性液为改性剂与无水乙醇按摩尔比1∶2组成的混合液，所述改性剂为三甲基甲氧基硅烷；
（4）、将步骤（3）所得夹心保温层外覆PE膜进行防掉粉封装；
（5）、将步骤（4）封装完成的夹心保温层外覆内侧有热熔胶层的铝塑膜作为覆膜层，通过抽真空的方式在覆膜层内形成真空层；
（6）、在步骤（5）所得夹芯保温层的覆膜层外部通过丙烯酸树脂胶黏剂粘贴一层木纤维增强聚酯树脂预浸带，即得隔热保温真空板。
实施例3
一种隔热保温真空板的制备方法，步骤如下
（1）、取正硅酸甲酯、无水乙醇和水混合均匀，之后依次加入2 mol/L的NH4F溶液和0.2moL/L的氨水搅拌均匀，得到二氧化硅溶胶，其中，以摩尔比计，正硅酸乙酯∶无水乙醇∶水=1∶9∶3；NH4F溶液的加入量保证以摩尔比计，NH4F∶正硅酸乙酯=0.006∶1，氨水的加入量保证以摩尔比计，NH3∶正硅酸乙酯=0.013∶1；
（2）、将竹纤维（直径≥10cm，长径比≥1000）压结成毡后，置于步骤（1）所得二氧化硅溶胶中浸渍18 h后，在50 ℃下静置老化20 h，得到生物质/二氧化硅复合凝胶；
（3）、将步骤（2）所得生物质/二氧化硅复合凝胶置于改性液中疏水改性处理18h，接着用无水乙醇进行溶剂置换2次，每次置换的时间为24 h，再超临界干燥处理，即得生物质/二氧化硅复合气凝胶，作为夹芯保温层；其中，所述改性液为改性剂与无水乙醇按摩尔比1∶3组成的混合液，所述改性剂为六甲基二硅氧烷；
（4）、将步骤（3）所得夹心保温层外覆PET膜进行防掉粉封装；
（5）、将步骤（4）封装完成的夹心保温层外覆内侧有热熔胶层的铝塑膜作为覆膜层，通过抽真空的方式在覆膜层内形成真空层；
（6）、在步骤（5）所得夹芯保温层的覆膜层外部通过有机硅树脂胶黏剂粘贴一层芳族聚酰胺纤维增强酚醛树脂预浸带，即得隔热保温真空板。
实施例4
一种隔热保温真空板的制备方法，步骤如下：
（1）、取正硅酸甲酯、无水乙醇和水混合均匀，之后依次加入2 mol/L的NH4F溶液和0.2moL/L的氨水搅拌均匀，得到二氧化硅溶胶，其中，以摩尔比计，正硅酸乙酯∶无水乙醇∶水=1∶6∶3；NH4F溶液的加入量保证以摩尔比计，NH4F∶正硅酸乙酯=0.004∶1，氨水的加入量保证以摩尔比计，NH3∶正硅酸乙酯=0.006∶1；
（2）、将木质纤维压结成毡后，置于步骤（1）所得二氧化硅溶胶中浸渍16 h后，在40 ℃下静置老化12 h，得到生物质/二氧化硅复合凝胶；
（3）、将步骤（2）所得生物质/二氧化硅复合凝胶置于改性液中疏水改性处理24h，接着用无水乙醇进行溶剂置换3次，每次置换的时间为16 h，再超临界干燥处理，即得生物质/二氧化硅复合气凝胶，作为夹芯保温层；其中，所述改性液为改性剂与无水乙醇按摩尔比1∶3组成的混合液，所述改性剂为甲基三氯硅烷；
（4）、将步骤（3）所得夹心保温层外覆PET膜进行防掉粉封装；
（5）、将步骤（4）封装完成的夹心保温层外覆内侧有热熔胶层的铝塑膜作为覆膜层，通过抽真空的方式在覆膜层内形成真空层；
（6）、在步骤（5）所得夹芯保温层的覆膜层外部通过有机硅树脂胶黏剂粘贴一层芳族聚酰胺纤维增强聚酰亚胺树脂预浸带，即得隔热保温真空板。

Claims (10)

1.一种隔热保温真空板的制备方法，其特征在于，步骤如下：
（1）、取正硅酸酯、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；其中，以摩尔比计，正硅酸酯∶乙醇∶水=1∶（4~12）∶（2~4）；NH4F溶液的加入量保证以摩尔比计，NH4F∶正硅酸酯=（0.002~0.01）∶1；氨水的加入量保证以摩尔比计，NH3∶正硅酸酯=（0.005~0.015）∶1；
（2）、将生物质纤维材料压结成毡后，置于步骤（1）所得二氧化硅溶胶中浸渍，然后在30~60 ℃下静置老化8~24 h，得到生物质/二氧化硅复合凝胶；
（3）、将步骤（2）所得生物质/二氧化硅复合凝胶置于改性溶液中进行疏水化改性处理，接着进行溶剂置换，再干燥处理，得到生物质/二氧化硅复合气凝胶作为夹芯保温层；
（4）、对步骤（3）所得夹心保温层进行封装处理；
（5）、在步骤（4）封装完成的夹心保温层外部设置覆膜层，通过抽真空的方式在覆膜层内形成真空层；
（6）、在步骤（5）所得夹芯保温层的覆膜层外部粘贴一层纤维增强树脂预浸带，即得隔热保温真空板。
2.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（1）中，所述正硅酸酯为正硅酸甲酯、正硅酸乙酯、正硅酸丁酯或正硅酸异丙酯。
3.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（2）中，所述生物质纤维材料为农作物秸秆纤维、木纤维或竹纤维，生物质纤维的直径≥10 cm，长径比≥1000。
4.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（2）中，浸渍的时间为12~24 h。
5.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（3）中，所述改性溶液为疏水化改性剂与无水乙醇按摩尔比1∶（2~5）组成的混合液，疏水化处理时间为12~24h；所述疏水化改性剂为甲基三甲氧基硅烷、甲基三乙氧基硅烷、三甲基甲氧基硅烷、三甲基乙氧基硅烷、二甲基二甲氧基硅烷、二甲基二乙氧基硅烷、二乙基二甲氧基硅烷、四乙氧基硅烷、六甲基二硅氧烷、七甲基三硅氧烷、辛基三乙氧基硅烷、甲基三氯硅烷、三甲基氯硅烷、二甲基二氯硅烷、乙基三氯硅烷或二乙基二氯硅烷。
6.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（3）中，利用无水乙醇进行溶剂置换，置换次数为2~3次，每次置换的时间为12~36 h。
7.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（4）中，封装时采用的封装材料为PET膜、PI膜、PE膜、PEEK膜或PTFE膜。
8.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（5）中，所述覆膜层为内侧设置有热熔胶层的铝塑膜。
9.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（6）中，采用胶黏剂粘接预浸带，所述胶黏剂为环氧树脂胶、丙烯酸树脂胶黏剂、酚醛树脂胶黏剂、聚氨酯胶胶黏剂、有机硅树脂胶黏剂、光学环氧胶或聚乙烯醇缩醛胶。
10.如权利要求1所述的隔热保温真空板的制备方法，其特征在于：步骤（6）中，所述纤维增强树脂预浸带中的纤维为碳纤维、玻璃纤维、芳族聚酰胺纤维、生物质纤维、莫来石纤维、石英纤维、硅酸铝纤维、陶瓷纤维、氧化铝纤维、岩棉纤维、玄武岩纤维或有机纤维；纤维增强树脂预浸带中的树脂为有机硅树脂、环氧树脂、酚醛树脂、聚酰亚胺树脂、氰酸酯树脂、聚酯树脂、聚酰胺树脂或聚醚醚酮树脂。
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CN106494038A (zh) * 2016-11-24 2017-03-15 西安思卓新材料科技有限公司 一种绝热可固化热固性复合材料及其制备方法与应用
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CN111910911A (zh) * 2020-07-29 2020-11-10 黑龙江琪正高新材料科技有限公司 一种适用于低温混凝土浇筑的施工模板及其制备方法
CN113620643A (zh) * 2021-09-18 2021-11-09 巩义市泛锐熠辉复合材料有限公司 一种防掉粉二氧化硅气凝胶毡的制备方法

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