CN106795993B - 包含多孔铝硅酸盐的用于真空绝热板的芯材以及具有该芯材的真空绝热板 - Google Patents

包含多孔铝硅酸盐的用于真空绝热板的芯材以及具有该芯材的真空绝热板 Download PDF

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CN106795993B
CN106795993B CN201580053781.3A CN201580053781A CN106795993B CN 106795993 B CN106795993 B CN 106795993B CN 201580053781 A CN201580053781 A CN 201580053781A CN 106795993 B CN106795993 B CN 106795993B
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core material
insulating plate
vacuum heat
porous aluminosilicate
surface area
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CN106795993A (zh
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郑相允
朴哲凞
田信姬
卞沅培
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LG Corp
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LG Chemical Co Ltd
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Abstract

本发明提供一种包含多孔铝硅酸盐的用于真空绝热板的芯材，以及具有该芯材的真空绝热板。根据本发明的用于真空绝热板的芯材具有优异的长期耐久性和提高的气体吸附能力(特别是优异的吸水能力)，同时需要较低的原料成本。包括所述芯材的真空绝热板通过在没有额外的吸气剂或吸收剂的情况下使真空度的降低最小化而可以表现出更加提高的绝热性能。

Description

包含多孔铝硅酸盐的用于真空绝热板的芯材以及具有该芯材 的真空绝热板
相关申请的交叉引用
本申请分别以于2014年10月20日提交的韩国专利申请No.10-2014-0142002和于2015年10月12日提交的韩国专利申请No.10-2015-0142296为基础并要求它们的优先权，这两项申请的公开内容通过引用全部并入本文中。
技术领域
本申请涉及一种包含多孔铝硅酸盐的用于真空绝热板的芯材以及具有该芯材的真空绝热板。
背景技术
市售的真空绝热板，例如，在韩国专利特许公开No.2011-0077860(2011.07.07)中所公开的真空绝热板，包括：芯材，用于保持绝热材料的形状，同时支撑绝缘材料的内部压力和外部压力之间的差；外壳材料，用于将绝热材料保持在真空下，同时包覆芯材；以及吸气剂，用于吸附绝热材料中的残留气体和从外部渗入的其它气体以保持长时间的真空。真空绝热板被制备成各种尺寸和形状，并且主要用于建筑和电子领域。
在现有真空绝热板中用作芯材的玻璃纤维棉通过聚集大量的玻璃纤维采用热压缩工艺来制备，用来确保绝热性能为约0.45W/mK。然而，当使用玻璃纤维棉较长时间时，由于气体穿过外壳材料而导致热导率提高，从而产生长期耐久性劣化的问题。为了改善这个问题，已经尝试通过采用玻璃纤维板作为芯材来确保长期耐久性。然而，玻璃纤维板的局限性在于初始绝热性能相对低。
由于使用玻璃纤维作为芯材的真空绝热板具有较差的长期耐久性或初始绝热性能，因此存在难以确保作为建筑材料的较长寿命以及电子产品的可靠性的问题。此外，使用玻璃纤维的真空绝热板具有制造成本高和成型性能差的缺点。
吸气剂也具有许多局限性，在于：需要高成本的原料，并且在使用之前为了活化而需要高温热处理(例如，300℃以上)，或者额外包括吸收水分的吸附剂。
发明内容
技术问题
本公开旨在提供一种用于真空绝热板的芯材，该芯材具有更加提高的气体吸附能力以表现出优异的绝热性能。
此外，本公开旨在提供一种具有所述芯材的真空绝热板。
技术方案
根据本公开，提供一种用于真空绝热板的芯材，该芯材包含多孔铝硅酸盐，该多孔铝硅酸盐的氩吸附Brunauer-Emmett-Teller(BET)表面积为300m2/g以上，外部比表面积(ESA)为150m2/g以上。
根据本公开，所述多孔铝硅酸盐的Barrett-Joyner-Halenda(BJH)解吸平均孔隙宽度可以为5至15nm。
根据本公开，所述多孔铝硅酸盐可以具有满足下面的式1的孔：
[式1]
Vmeso/Vmicro>3.0，
其中，Vmeso表示孔隙尺寸为2nm至300nm的中孔的Barrett-Joyner-Halenda(BJH)累积体积，
Vmicro表示通过t曲线方法，由氩吸附Brunauer-Emmett-Teller(BET)表面积计算的孔隙尺寸小于2nm的微孔的体积。
根据本公开，当在25℃的等温条件下，在80％、90％和95％的相对湿度下加湿时，多孔铝硅酸盐的吸水率分别为18重量％以上、22重量％以上和25重量％以上。
根据本公开，提供一种包括所述芯材以及密封并包覆该芯材的外壳材料的真空绝热板。
下文中，将描述根据本公开的实施方案的用于真空绝热板的芯材和具有该芯材的真空绝热板。
在此之前，除非在本说明书中另外说明，否则本文所使用的术语仅用于描述示例性实施方案的目的，而不意在限制本公开。
除非上下文另外明确说明，否则本文所使用的单数形式也可以指包括复数形式。
还应当理解的是，本说明书中使用的术语“包含”表明存在所述特征、区域、整数、步骤、操作、元件或组分，但不排除还有其它的特征、区域、整数、步骤、操作、元件或组分。
I.用于真空绝热板的芯材
根据本公开的一个方面，提供一种用于真空绝热板的芯材，该芯材包含多孔铝硅酸盐，该多孔铝硅酸盐的氩吸附Brunauer-Emmett-Teller(BET)表面积为300m2/g以上，外部比表面积(ESA)为150m2/g以上。
作为本发明人进行的不断实验的结果，惊奇地证实，满足上述物理性能的多孔铝硅酸盐可以降低在升高的压力下热导率的升高，并且具有对水的化学稳定性，从而适合用作用于真空绝热板的芯材。通常，真空绝热板的热导率随着时间的进行而升高，特别地，当使用包括根据本公开的一个实施方案的芯材的真空绝热材料时，可以表现出最小的热导率升高。
由于根据本公开的一个实施方案的芯材由无机多孔铝硅酸盐组成，因此原料的成本较低，同时表现出优异的长期耐久性。此外，根据本公开的一个实施方案的芯材具有提高的气体吸附能力(特别是优异的吸水能力)。此外，所述芯材具有优异的化学和热稳定性，因此，所述芯材可以基本上不产生气体并且有效地吸附通过外壳材料从外部渗入的其它气体。
即使少量的水渗入由外壳材料密封的空间，也会立刻引起非常高的相对湿度(例如，80％以上的相对湿度)。然而，根据本公开的一个实施方案的芯材具有提高的气体吸附能力(特别是优异的吸水能力)以有效地吸附从外部渗入的气体，从而使真空度的降低最小化。因此，可以得到更加提高的和稳定的绝热性能。
可以通过将根据本公开的一个实施方案的满足上述物理性能的多孔铝硅酸盐应用于芯材来实现这种效果。
也就是说，作为本发明人进行的不断实验的结果，可以证实，根据多孔铝硅酸盐的比表面积、平均孔隙宽度、中孔和微孔的体积等，用于真空绝热板的芯材的物理性能会出现显著的差异。物理性能的显著差异会导致真空绝热板的长期耐久性和绝热性能的巨大差异。此外，通过使用所述芯材，可以在没有附加的吸气剂或吸收剂的情况下使真空度的降低最小化，从而可以简化真空绝热板的结构和制造工艺。
根据本公开的实施方案，用于绝热材料的芯材包含多孔铝硅酸盐，该多孔铝硅酸盐的氩吸附Brunauer-Emmett-Teller(BET)表面积为300m2/g以上，外部比表面积(ESA)为150m2/g以上。
由于用作芯材的多孔铝硅酸盐的氩吸附Brunauer-Emmett-Teller(BET)表面积为300m2/g以上，外部比表面积(ESA)为150m2/g以上，因此，可以确保芯材的结构稳定性和长期耐久性，并且也可以确保最小化的热导率和稳定的绝热性能。
此处，可以由气体吸附实验，将多孔铝硅酸盐的Brunauer-Emmett-Teller(BET)表面积与微孔的比表面积之间的差估算为多孔铝硅酸盐的外部比表面积(ESA)。微孔是孔隙尺寸小于2nm的孔，例如，可以由t曲线方法来估算微孔的比表面积。
优选地，在实现多孔铝硅酸盐的上述效果方面，更有利地，氩吸附Brunauer-Emmett-Teller(BET)表面积可以为300m2/g至700m2/g、300m2/g至650m2/g、350m2/g至650m2/g、350m2/g至600m2/g或350m2/g至550m2/g，外部比表面积(ESA)可以为150m2/g以上、150m2/g至300m2/g、150m2/g至250m2/g或200m2/g至250m2/g。
也就是说，当多孔铝硅酸盐的氩吸附Brunauer-Emmett-Teller(BET)表面积小于300m2/g或者外部比表面积(ESA)小于150m2/g时，在25℃的等温条件和80％以上的相对湿度下会表现出小于20重量％的较差的吸水率，因此，这种多孔铝硅酸盐不适合作为用于真空绝热板的芯材。
根据本公开的一个实施方案，在实现多孔铝硅酸盐的上述效果方面，更有利地，Barrett-Joyner-Halenda(BJH)解吸平均孔隙宽度可以为5nm至15nm、6nm至14nm或6至12nm。
另外，根据本公开的一个实施方案，多孔铝硅酸盐可以具有满足下面的式1的孔：
[式1]
Vmeso/Vmicro>3.0，
其中，Vmeso表示孔隙尺寸为2nm至300nm的中孔的Barrett-Joyner-Halenda(BJH)累积体积，
Vmicro表示通过t曲线方法，由氩吸附Brunauer-Emmett-Teller(BET)表面积计算的孔隙尺寸小于2nm的微孔的体积。
也就是说，Vmeso/Vmicro值大于3，优选地，3.1以上或3.1至5.0、3.1至4.7或3.5至4.7的多孔铝硅酸盐可以表现出更加提高的气体吸附能力。
市售沸石(例如，购自Sigma-Aldrich的沸石13X等)的最大吸水率仅为约20重量％，并且在潮湿和等温环境下变为饱和。
相反，根据本公开的实施方案的具有满足上述条件的结构特性的多孔铝硅酸盐可以表现出超过30重量％的较高的吸收率，特别是在较高的相对湿度下。
例如，当在25℃的等温条件下在80％的相对湿度下加湿时，根据本公开的实施方案的多孔铝硅酸盐可以表现出18重量％以上，优选地18重量％至25重量％的吸水率。
另外，当在25℃的等温条件下在90％的相对湿度下加湿时，根据本公开的实施方案的多孔铝硅酸盐可以表现出22重量％以上，优选地22重量％至27重量％的吸水率。
此外，当在25℃的等温条件下在95％的相对湿度下加湿时，根据本公开的实施方案的多孔铝硅酸盐可以表现出25重量％以上，优选地25重量％至35重量％的吸水率。
因此，包括多孔铝硅酸盐作为芯材的真空绝热板可以有效地吸附绝热材料中的残留气体和通过外壳材料从外部渗入的其它气体，因此，即使长期使用，也可以表现出最小化的真空度的降低以及稳定的绝热性能。
具有满足上述条件的结构特性的多孔铝硅酸盐可以通过多种方法制备，优选地，多孔铝硅酸盐可以通过多孔铝硅酸盐前体在水性介质中的偶合碱介导的溶解(coupledalkali-mediated dissolution)和沉淀反应来制备。
在这一方面，作为硅源，可以使用锻制氧化硅、硅酸盐、铝硅酸盐、粘土、矿物、偏高岭土、活性粘土、粉煤灰、炉渣、火山灰等。作为铝源，可以使用氧化铝、铝酸盐、铝盐、粘土、偏高岭土、活性粘土、粉煤灰、炉渣、火山灰等。
作为一个非限制性实例，根据本公开的实施方案的多孔铝硅酸盐可以通过如下方法制备，该方法包括：i)在搅拌下，通过向碱或碱性溶液(例如，氢氧化钠溶液)中添加硅源、铝源和水，形成满足特定金属原子比例(例如，Na:Al:Si＝3:1:2)的地质聚合物树脂；ii)在大气压下，在较低温度(例如，60℃至80℃)下热处理所述地质聚合物树脂；以及iii)通过洗涤中和热处理后的地质聚合物树脂。
特别地，根据本公开的实施方案，通过在大气压力和较低温度(例如，60℃至80℃，优选地65℃至75℃)的条件下满足特定金属原子比例的地质聚合物树脂的热处理，可以得到具有气体吸附能力(特别是优异的吸水能力)的多孔铝硅酸盐。
II.真空绝热板
根据本公开的另一方面，提供一种包括上述芯材以及密封并包覆该芯材的外壳材料的真空绝热板。
图1是示出根据本公开的一个实施方案的真空绝热板100的示意图。在真空绝热板100中，芯材120包含多孔铝硅酸盐，该多孔铝硅酸盐的氩吸附Brunauer-Emmett-Teller(BET)表面积为300m2/g以上，外部比表面积(ESA)为150m2/g以上。设置外壳材料110以密封和包覆芯材120。
在现有的真空绝热板中，通常在芯材内部设置用于吸附绝热材料中的残留气体和从外部渗入的其它气体的吸气剂或吸收剂。
然而，根据本公开的实施方案的真空绝热板包括上述具有长期耐久性和提高的气体吸附能力的多孔铝硅酸盐作为芯材，从而在没有附加的吸气剂或吸收剂的情况下使真空度的降低最小化。因此，所述真空绝热板即使具有更简化的结构也可以表现出提高的绝热性能。
根据本公开的实施方案，外壳材料110可以是具有气体阻隔性能的层压体。例如，外壳材料110可以是粘合剂层、阻隔层和表面保护层依次层压的层压体。
粘合剂层是通过热密封而熔融的层。作为实例，可以将热熔性树脂，如高密度聚乙烯、低密度聚乙烯、线性低密度聚乙烯、浇铸聚丙烯、定向聚丙烯、聚偏二氯乙烯、聚氯乙烯、乙烯-乙酸乙烯酯共聚物、乙烯-乙烯醇共聚物等应用于粘合剂层。
阻隔层是用于阻隔气体从外部渗入并保护芯材的层，可以是厚度为约5μm至约10μm的薄金属膜。对阻隔层的材料没有特别地限制，并且例示为铝薄膜。
表面保护层是用于防止由金属材料制成的阻隔层破裂的层，可以是厚度为约10μm至约15μm的塑料薄膜。对表面保护层的材料没有特别地限制，并且例示为聚对苯二甲酸乙二醇酯薄膜、聚偏二氯乙烯薄膜、尼龙薄膜、其它乙烯基树脂薄膜等。
同时，根据本公开的实施方案，可以通过将芯材放置在两个外壳材料之间，然后在减压室中进行热压缩来制造真空绝热板。
有益效果
根据本公开的用于真空绝热板的芯材具有优异的长期耐久性和提高的气体吸附能力(特别是优异的吸水能力)，同时需要较低的原料成本。包括所述芯材的真空绝热板可以通过在没有附加的吸气剂或吸收剂的情况下使真空度的降低最小化来表现出更加提高的绝热性能。
附图说明
图1是根据本公开的一个实施方案的真空绝热板的示意性横截面视图。
具体实施方式
下文中，提供优选实施例以便更好地理解本发明。然而，这些实施例仅用于说明的目的，并且本发明不局限于这些实施例。
实施例1
将3.02g的NaOH加入到反应器中，然后向其中添加5.43g的三重蒸馏水并充分混合。向该溶液中添加7.76g的硅酸钠(约10.6％的Na2O，约26.5％的SiO2)，并在室温下在800rpm的搅拌下完全溶解。向该制得的溶液中添加3.8g的偏高岭土，并在室温下以800rpm搅拌40分钟，来得到Na:Al:Si原子比例为约3:1:2的地质聚合物树脂。
在大气压力和70℃的条件下将地质聚合物树脂在烘箱中加热一天，来得到pH约为14的地质聚合物树脂。通过向其中添加足量的三重蒸馏水来洗涤热处理后的地质聚合物树脂，并在10,000rpm下离心5分钟，然后倾析pH约为14的澄清上清液。重复这些洗涤、离心和倾析过程，直到上清液的pH达到7左右。
将中和后的地质聚合物树脂在80℃的真空烘箱中干燥一夜，来得到多孔铝硅酸盐的最终产物。测量最终产物的物理性能，并示于下面的表1和2中。
实施例2
将3.02g的NaOH加入到反应器中，然后向其中添加5.43g的三重蒸馏水并充分混合。向该溶液中添加7.76g的硅酸钠(约10.6％的Na2O，约26.5％的SiO2)，并在室温下在800rpm的搅拌下完全溶解。向该制得的溶液中添加3.8g的偏高岭土，并在室温下以800rpm搅拌40分钟，来得到Na:Al:Si原子比例为约3:1:2的地质聚合物树脂。
在大气压力和70℃的条件下将地质聚合物树脂在烘箱中加热一天，来得到pH约为14的地质聚合物树脂。通过向其中添加足量的7％的硝酸水溶液来洗涤热处理后的地质聚合物树脂，并在10,000rpm下离心5分钟，然后倾析pH约为14的澄清上清液。重复这些洗涤、离心和倾析过程，直到上清液的pH达到7左右。
将中和后的地质聚合物树脂在80℃的真空烘箱中干燥一夜，来得到多孔铝硅酸盐的最终产物。
比较例1
除了在得到地质聚合物树脂的过程中进一步添加4.88g的三重蒸馏水(即，总共添加10.31g的三重蒸馏水)之外，以与实施例1中相同的方式得到多孔铝硅酸盐。
比较例2
得到沸石13X，它是Sigma-Aldrich的产品。
[表1]
实施例1 实施例2 比较例1 比较例2
BET(m<sup>2</sup>/g) 519 371 558 787
ESA(m<sup>2</sup>/g) 210 206 117 12
A<sub>micro</sub>(m<sup>2</sup>/g) 309 165 441 775
孔隙宽度(nm) 8.18 9.29 4.28 2.89
V<sub>total</sub>(cm<sup>3</sup>/g) 0.72 0.61 0.32 0.30
V<sub>meso</sub>(cm<sup>3</sup>/g) 0.59 0.50 0.16 0.02
V<sub>micro</sub>(cm<sup>3</sup>/g) 0.13 0.11 0.16 0.28
V<sub>meso/micro</sub> 4.54 4.55 1.00 0.71
-BET(m2/g)：Brunauer-Emmett-Teller(BET)表面积
-ESA(m2/g)：外部比表面积
-Amicro(m2/g)：孔隙尺寸小于2nm的微孔的表面积
-孔隙宽度(nm)：Barrett-Joyner-Halenda(BJH)解吸平均孔隙宽度
-Vtotal(cm3/g)：总孔体积
-Vmeso(cm3/g)：孔隙尺寸为2nm至300nm的中孔的Barrett-Joyner-Halenda(BJH)累积体积
-Vmicro(cm3/g)：通过t曲线方法，由氩吸附Brunauer-Emmett-Teller(BET)表面积计算的孔隙尺寸小于2nm的微孔的体积。
[表2]
吸水率(重量％) 实施例1 实施例2 比较例1 比较例2
@25℃，70％的相对湿度 17.42 14.67 12.19 19.43
@25℃，80％的相对湿度 21.07 18.80 13.65 19.76
@25℃，90％的相对湿度 25.59 24.56 14.94 20.13
@25℃，95％的相对湿度 30.41 30.69 16.39 20.54
参照表1和2，根据实施例1和2的多孔铝硅酸盐具有较大的外部比表面积(ESA)和BJH解吸平均孔隙宽度，而中孔体积大于微孔体积约4.5倍。因此，可以证实，根据实施例1和2的多孔铝硅酸盐在80％以上的相对湿度下表现出高达30重量％的较高的吸水率，因此适合用作用于真空绝热板的芯材。
相反，根据比较例1和2的多孔铝硅酸盐具有相对较小的外部比表面积、BJH解吸平均孔隙宽度、中孔体积等，因此，具有非常低的吸水率。
[附图标记]
100：真空绝热板
110：外壳材料
120：芯材

Claims (4)

1.一种用于真空绝热板的芯材，该芯材包含多孔铝硅酸盐，该多孔铝硅酸盐的氩吸附Brunauer-Emmett-Teller(BET)表面积为300m2/g以上，外部比表面积(ESA)为150m2/g以上，
其中，所述多孔铝硅酸盐具有满足下面的式1的孔：
[式1]
Vmeso/Vmicro&gt;3.0，
其中，Vmeso表示孔隙尺寸为2nm至300nm的中孔的Barrett-Joyner-Halenda(BJH)累积体积，并且
Vmicro表示通过t曲线方法由氩吸附Brunauer-Emmett-Teller(BET)表面积计算的孔隙尺寸小于2nm的微孔的体积。
2.根据权利要求1所述的用于真空绝热板的芯材，其中，所述多孔铝硅酸盐的Barrett-Joyner-Halenda(BJH)解吸平均孔隙宽度为5nm至15nm。
3.根据权利要求1所述的用于真空绝热板的芯材，其中，当在25℃的等温条件下在80％、90％和95％的相对湿度下加湿时，所述多孔铝硅酸盐的吸水率分别为18重量％以上、22重量％以上和25重量％以上。
4.一种真空绝热板，包括：
权利要求1所述的芯材；以及
密封并包覆所述芯材的外壳材料。
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