CN117945414A - 常压干燥制备二氧化硅气凝胶 - Google Patents
常压干燥制备二氧化硅气凝胶 Download PDFInfo
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- CN117945414A CN117945414A CN202211284343.6A CN202211284343A CN117945414A CN 117945414 A CN117945414 A CN 117945414A CN 202211284343 A CN202211284343 A CN 202211284343A CN 117945414 A CN117945414 A CN 117945414A
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- normal pressure
- silica aerogel
- hydrogel
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- hexamethyldisilazane
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 13
- 238000001035 drying Methods 0.000 title abstract description 8
- 238000002360 preparation method Methods 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 11
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 239000004964 aerogel Substances 0.000 claims abstract description 6
- 239000000017 hydrogel Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011148 porous material Substances 0.000 claims abstract description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 239000000499 gel Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000008346 aqueous phase Substances 0.000 abstract 1
- 238000007385 chemical modification Methods 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
本发明开发了一种简单、经济、快速的水玻璃前驱体常压干燥二氧化硅气凝胶工艺。用极低剂量的六甲基二硅氮烷,用共前驱体方法可以快速地进行水凝胶的表面化学修饰,使这一过程具有相当高的性价比。水相表面改性实质上是使孔隙水置换,同时用正己烷一步溶剂交换,在3h内将水凝胶转化为有机凝胶,使常压干燥法制备气凝胶粉末的总加工时间缩短至5h。
Description
技术领域
本发明属于气凝胶材料的制备
背景技术
由于具有较低的密度(低至0.003g/cm3)以及比表面积大(800~1200m2/g)、孔隙率高(达98%以上)、热导率低[低至0.013W/(m·K)]、介电常数低(1.0-2.0)等性能特征,二氧化硅气凝胶在高效隔热保温、催化剂载体、隔音材质、气-液吸附,油水分离等方面具有广泛的应用价值,且涵盖军工、民用领域,因其优异的隔热性能而被称为超级绝热材料。
然而,目前气凝胶还没有大范围商业应用,其中前驱体高昂的价格和复杂的预处理工艺、凝胶干燥过程是制约气凝胶大规模工业化生产的主要因素。本发明采用廉价的水玻璃为原料,采用工艺简单的常压干燥法制备二氧化硅气凝胶,极具工业化扩大生产的潜力。
发明内容
本发明的目的在于制备二氧化硅气凝胶。
本发明制备的二氧化硅气凝胶,分子式为SiO2.
实验测试结果表明,常压干燥法制备的二氧化硅气凝胶孔径分布均匀,主要集中在40nm左右,组成气凝胶的粒子尺寸均匀。
二氧化硅气凝胶作为一种纳米多孔材料,预期在建筑隔热、催化、储能等领域具有重要的应用价值。
附图说明:
图1.二氧化硅气凝胶在扫描电子显微镜下的形貌图。
图2.二氧化硅气凝胶的孔径分布。
具体实施方式
二氧化硅气凝胶的制备。
水玻璃溶液首先用去离子水稀释,以获得所需的二氧化硅在起始物中的重量百分比。然后采用共前驱体法制备硅烷化水凝胶,即先向硅酸中加入硝酸,然后在恒定搅拌下加入六甲基二硅氮烷由于六甲基二硅氮烷呈碱性,pH值为8.5,因此它加入溶胶即可形成凝胶。随后将共前驱体法制备的水凝胶浸泡在正己烷溶液中,在3h内完成溶剂交换,然后从烧杯中除去置换的孔隙水,在200℃的炉中常压下干燥凝胶30min即可获得二氧化硅气凝胶。
Claims (1)
1.权利要求二氧化硅气凝胶的制备方法,包括如下步骤:
水玻璃溶液首先用去离子水稀释,以获得所需的二氧化硅在起始物中的重量百分比,然后采用共前驱体法制备硅烷化水凝胶,即先向硅酸中加入硝酸,然后在恒定搅拌下加入六甲基二硅氮烷,由于六甲基二硅氮烷呈碱性,pH值为8.5,因此它加入溶胶即可形成凝胶,随后将共前驱体法制备的水凝胶浸泡在正己烷溶液中,在3h内完成溶剂交换,然后从烧杯中除去置换的孔隙水,在200℃的炉中常压下干燥凝胶30min即可获得二氧化硅气凝胶。
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