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CN111099875A - Preparation method of silica aerogel composite light heat insulation tile - Google Patents

Preparation method of silica aerogel composite light heat insulation tile Download PDF

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Publication number
CN111099875A
CN111099875A CN201911328342.5A CN201911328342A CN111099875A CN 111099875 A CN111099875 A CN 111099875A CN 201911328342 A CN201911328342 A CN 201911328342A CN 111099875 A CN111099875 A CN 111099875A
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Prior art keywords
silica aerogel
aerogel composite
preparation
insulation tile
sol
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CN201911328342.5A
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Chinese (zh)
Inventor
张磊
刘瑞祥
王开宇
隋学叶
周长灵
程之强
王重海
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Shandong Industrial Ceramics Research and Design Institute Co Ltd
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Priority to CN201911328342.5A priority Critical patent/CN111099875A/en
Publication of CN111099875A publication Critical patent/CN111099875A/en
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
    • B28B1/265—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor pressure being applied on the slip in the filled mould or on the moulded article in the mould, e.g. pneumatically, by compressing slip in a closed mould
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/40—Porous or lightweight materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention relates to a preparation method of a silica aerogel composite light heat insulation tile. The slurry obtained by mixing the chopped fibers and the sol is placed in a heat insulation tile die for press filtration molding, after gelation, demolding is carried out, and the heat insulation tile is prepared by supercritical drying. The obtained silica aerogel composite light heat insulation tile is free from sintering, high in porosity and small in pore size, and has a good blocking effect on solid heat transfer, air heat transfer and convection.

Description

Preparation method of silica aerogel composite light heat insulation tile
Technical Field
The invention belongs to the field of heat insulation and preservation, and particularly relates to a preparation method of a silica aerogel composite light heat insulation tile.
Background
At present, the aerogel composite heat insulation tile technology is mainly to prepare a ceramic heat insulation tile through high-temperature sintering, and then to compound the aerogel and the ceramic heat insulation tile through a sol-gel process. The preparation technology has the problems of complex process, long preparation period, low production efficiency, high energy consumption and the like, and in order to overcome the defects of the prior art, a method for preparing the aerogel composite heat-insulating tile efficiently, energy-saving and rapidly is urgently needed.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of a silica aerogel composite light heat insulation tile.
According to one aspect of the invention, a preparation method of a silica aerogel composite light heat insulation tile is provided, which comprises the following steps:
and (3) placing the slurry obtained by mixing and dispersing the chopped fibers and the sol into a heat insulation tile die for internal pressure filtration molding, demolding after gelation, and performing supercritical drying to obtain the silica aerogel composite light heat insulation tile.
Wherein the chopped fibers are chopped quartz fibers. The short-cut quartz fiber is obtained by carrying out short-cut treatment on quartz fiber cotton, cleaning with an acidic aqueous solution, filtering and drying. Wherein the average length of the quartz fiber cotton after being chopped is 0.5-5.0mm, and the pH value of the acidic aqueous solution is 2-3.
Further, the sol is obtained by mixing ethyl orthosilicate, ethanol and deionized water and adjusting the pH value by using an acid catalyst.
Further, the molar ratio of ethyl orthosilicate, ethanol and deionized water is 1:4-10:2-12, the acidic catalyst is hydrochloric acid or nitric acid, and the pH value of the sol is 3-4.
Further, the mixture was dispersed so that the ratio of the mass of the chopped fibers to the volume of the sol was 1g:30-60 mL.
Further, the ratio of the mass of the chopped fibers to the volume of the sol in the slurry is 1g:8-15 mL.
Further, after the pH value of the slurry is adjusted to 7-8 by an alkaline catalyst, the slurry is placed in a heat insulation tile die for filter pressing and forming, and the forming pressure is 0.1-0.06 MPa.
Furthermore, the gel is required to be aged in absolute ethyl alcohol after being demoulded, the aging temperature is 50-60 ℃, and the aging time is 1-3 days.
Furthermore, ethanol is used as a medium for supercritical drying, the drying temperature is 270-280 ℃, the drying time is 2-5 hours, and the pressure is controlled to be 7-8 MPa.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the silica aerogel composite light heat insulation tile provided by the invention has the advantages that the slurry obtained by mixing and dispersing the chopped fibers and the sol is placed in a heat insulation tile mould for internal pressure filtration molding, the heat insulation tile is prepared by demoulding after gelation and supercritical drying, the preparation method is scientific, reasonable, simple and easy to implement, and no binder is used, the microstructure characteristics of the aerogel and the fibers form a skeleton structure, so that the material integrally forms a rigid structure, the processing procedure of the silica aerogel composite light heat insulation tile is omitted, any complex irregular part can be prepared, the sintering process of the ceramic heat insulation tile is omitted, the overall process efficiency is improved, and the production energy consumption is greatly reduced. The obtained silica aerogel composite light heat-insulating tile is sintering-free, high in porosity, small in pore size and 0.28-0.33 g/cm in density3The thermal conductivity coefficient at 300 ℃ is less than 0.03W/(mK), the thermal conductivity coefficient at 500 ℃ is less than 0.04W/(mK), the thermal conductivity coefficient at 800 ℃ is less than 0.06W/(mK), the compressive strength is more than or equal to 0.5MPa, the tensile strength is more than or equal to 0.5MPa, and the heat-insulating material has good barrier effect on solid heat transfer and air heat transfer and convection.
Detailed Description
In order to better understand the technical solution of the present invention, the following embodiments are provided to further explain the present invention.
Example one
The preparation method of the silica aerogel composite lightweight heat insulation tile comprises the following steps:
s1, fiber pretreatment: chopping quartz fiber cotton, cleaning with acidic aqueous solution, filtering, and oven drying to obtain the final product, wherein the average length of the chopped quartz fiber cotton is 0.5-5.0mm, and the pH of the acidic aqueous solution is 2-3;
s2, sol: mixing ethyl orthosilicate, ethanol and deionized water according to a molar ratio of 1:4:2, and adjusting the pH value by using an acidic catalyst to obtain sol, wherein the acidic catalyst is hydrochloric acid or nitric acid, and the pH value is adjusted to 3-4;
s3, homogenizing and dispersing: adding the chopped fibers obtained in the step S1 into the sol obtained in the step S2, mixing the chopped fibers and the sol in a ratio of 1g to 30mL, fully stirring, filtering part of the sol in the mixture to obtain homogeneous slurry, wherein the ratio of the mass of the chopped fibers to the volume of the sol in the homogeneous slurry is 1g to 8mL
S4, forming, gelling and aging: adjusting the pH value of the slurry obtained in the step S3 to 7-8 by using an alkaline catalyst ammonia water, adding the slurry into a heat insulation tile die, applying a certain pressure to perform filter pressing forming, wherein the forming pressure is 0.1-0.06MPa, demolding after gelation, and aging a blank body in absolute ethyl alcohol at the aging temperature of 50-60 ℃ for 2 days;
s5, drying: and (5) performing supercritical drying on the aged blank obtained in the step (S4) to obtain the silica aerogel composite light heat insulation tile, wherein ethanol is used as a medium for the supercritical drying, the drying temperature is 280 ℃, the drying time is 2 hours, and the pressure is controlled at 7 MPa.
Example two
The preparation method of the silica aerogel composite lightweight heat insulation tile comprises the following steps:
s1, fiber pretreatment: chopping quartz fiber cotton, cleaning with acidic aqueous solution, filtering, and oven drying to obtain the final product, wherein the average length of the chopped quartz fiber cotton is 0.5-5.0mm, and the pH of the acidic aqueous solution is 2-3;
s2, sol: mixing ethyl orthosilicate, ethanol and deionized water according to a molar ratio of 1:8:10, and adjusting the pH value by using an acidic catalyst to obtain sol, wherein the acidic catalyst is hydrochloric acid or nitric acid, and the pH value is adjusted to 3-4;
s3, homogenizing and dispersing: adding the chopped fibers obtained in the step S1 into the sol obtained in the step S2, mixing the chopped fibers and the sol in a ratio of 1g:60mL, fully stirring, filtering part of sol in the mixture to obtain homogeneous slurry, wherein the ratio of the mass of the chopped fibers to the volume of the sol in the homogeneous slurry is 1g:15 mL;
s4, forming, gelling and aging: adjusting the pH value of the slurry obtained in the step S3 to 7-8 by using an alkaline catalyst ammonia water, adding the slurry into a heat insulation tile die, applying a certain pressure to perform filter pressing forming, wherein the forming pressure is 0.1-0.06MPa, demolding after gelation, and aging a blank body in absolute ethyl alcohol at the aging temperature of 50-60 ℃ for 1 day;
s5, drying: and (5) performing supercritical drying on the aged blank obtained in the step (S4) to obtain the silica aerogel composite light heat insulation tile, wherein ethanol is used as a medium for the supercritical drying, the drying temperature is 270 ℃, the drying time is 5 hours, and the pressure is controlled at 8 MPa.
EXAMPLE III
The preparation method of the silica aerogel composite lightweight heat insulation tile comprises the following steps:
s1, fiber pretreatment: chopping quartz fiber cotton, cleaning with acidic aqueous solution, filtering, and oven drying to obtain the final product, wherein the average length of the chopped quartz fiber cotton is 0.5-5.0mm, and the pH of the acidic aqueous solution is 2-3;
s2, sol: mixing ethyl orthosilicate, ethanol and deionized water according to a molar ratio of 1:10:12, and adjusting the pH value by using an acidic catalyst to obtain sol, wherein the acidic catalyst is hydrochloric acid or nitric acid, and the pH value is adjusted to 3-4;
s3, homogenizing and dispersing: adding the chopped fibers obtained in the step S1 into the sol obtained in the step S2, mixing the chopped fibers and the sol in a ratio of 1g to 40mL, fully stirring, filtering part of sol in the mixture to obtain homogeneous slurry, wherein the ratio of the mass of the chopped fibers to the volume of the sol in the homogeneous slurry is 1g to 9 mL;
s4, forming, gelling and aging: adjusting the pH value of the slurry obtained in the step S3 to 7-8 by using an alkaline catalyst ammonia water, adding the slurry into a heat insulation tile die, applying a certain pressure to perform filter pressing forming, wherein the forming pressure is 0.1-0.06MPa, demolding after gelation, and aging a blank body in absolute ethyl alcohol at the aging temperature of 50-60 ℃ for 3 days;
s5, drying: and (5) performing supercritical drying on the aged blank obtained in the step S4 to obtain the silica aerogel composite light heat insulation tile, wherein the medium used for the supercritical drying is ethanol, the drying temperature is 270-280 ℃, the drying time is 3 hours, and the pressure is controlled to be 7-8 MPa.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.

Claims (10)

1.一种二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，包括以下步骤：1. a preparation method of silica aerogel composite light-weight thermal insulation tile, is characterized in that, comprises the following steps: 短切纤维与溶胶混合分散所得料浆置于隔热瓦模具内压滤成型，待凝胶后脱模、经超临界干燥即得二氧化硅气凝胶复合轻质隔热瓦。The slurry obtained by mixing and dispersing the chopped fibers and the sol is placed in a heat-insulating tile mold for pressure filtration and molding. After gelation, the mold is demolded and supercritically dried to obtain a silica aerogel composite lightweight heat-insulating tile. 2.根据权利要求1所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，所述短切纤维为短切石英纤维。2 . The method for preparing a silica aerogel composite lightweight thermal insulation tile according to claim 1 , wherein the chopped fibers are chopped quartz fibers. 3 . 3.根据权利要求2所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，所述短切石英纤维通过石英纤维棉进行短切处理，并用酸性水溶液清洗后过滤、烘干所得。3. The preparation method of silica aerogel composite light-weight thermal insulation tile according to claim 2, wherein the chopped quartz fiber is subjected to chopped treatment by quartz fiber cotton, and filtered with an acidic aqueous solution after cleaning , obtained from drying. 4.根据权利要求3所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，石英纤维棉短切处理后平均长度为0.5-5.0mm，酸性水溶液的pH＝2-3。4. The method for preparing a silica aerogel composite light-weight heat insulating tile according to claim 3, wherein the average length of the quartz fiber cotton after chopped processing is 0.5-5.0 mm, and the pH of the acidic aqueous solution is 2 -3. 5.根据权利要求1所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，溶胶通过正硅酸乙酯、乙醇、去离子水混合，并使用酸性催化剂调节pH所得。5. The preparation method of silica aerogel composite lightweight heat insulating tile according to claim 1, wherein the sol is mixed with ethyl orthosilicate, ethanol and deionized water, and the pH is adjusted by using an acidic catalyst income. 6.根据权利要求5所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，正硅酸乙酯:乙醇:去离子水的摩尔比＝1:4-10:2-12，所述酸性催化剂选用盐酸或硝酸，溶胶的pH为3-4。6. the preparation method of silica aerogel composite light-weight thermal insulation tile according to claim 5, is characterized in that, the molar ratio of ethyl orthosilicate: ethanol: deionized water=1:4-10: 2-12, the acid catalyst is selected from hydrochloric acid or nitric acid, and the pH of the sol is 3-4. 7.根据权利要求1所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，所述料浆中短切纤维质量与溶胶体积的比为1g:8-15mL。7 . The method for preparing a silica aerogel composite light-weight thermal insulation tile according to claim 1 , wherein the ratio of the quality of the chopped fibers to the volume of the sol in the slurry is 1 g:8-15 mL. 8 . 8.根据权利要求1所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，所述浆料经碱性催化剂调节pH至7-8后，再置于隔热瓦模具内进行压滤成型，成型压力为0.1-0.06MPa。8 . The preparation method of silica aerogel composite lightweight heat insulating tile according to claim 1 , wherein the slurry is adjusted to pH 7-8 by an alkaline catalyst, and then placed in a heat insulating Filter press molding is performed in the tile mold, and the molding pressure is 0.1-0.06MPa. 9.根据权利要求1所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，凝胶脱模后需在无水乙醇中进行老化，老化温度为50-60℃，老化时间为1-3天。9 . The preparation method of silica aerogel composite lightweight heat insulating tile according to claim 1 , wherein the gel needs to be aged in absolute ethanol after demoulding, and the aging temperature is 50-60° C. 10 . , the aging time is 1-3 days. 10.根据权利要求1-9任一所述的二氧化硅气凝胶复合轻质隔热瓦的制备方法，其特征是，超临界干燥所用的介质为乙醇，干燥温度为270-280℃，干燥时间为2-5小时，压力控制在7-8MPa。10. The method for preparing a silica aerogel composite lightweight thermal insulation tile according to any one of claims 1-9, wherein the medium used in the supercritical drying is ethanol, and the drying temperature is 270-280°C, The drying time is 2-5 hours, and the pressure is controlled at 7-8MPa.
CN201911328342.5A 2019-12-20 2019-12-20 Preparation method of silica aerogel composite light heat insulation tile Pending CN111099875A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6068882A (en) * 1995-11-09 2000-05-30 Aspen Systems, Inc. Flexible aerogel superinsulation and its manufacture
CN101450852A (en) * 2008-11-27 2009-06-10 长沙星纳气凝胶有限公司 Nano-pore SiO2 aerogel thermal insulation composite material and preparation method thereof
CN102557577A (en) * 2011-11-01 2012-07-11 厦门纳美特新材料科技有限公司 Preparation and method of silicon dioxide aerogel composite material
CN108503327A (en) * 2018-04-13 2018-09-07 航天特种材料及工艺技术研究所 A kind of low cost aeroge thermal insulation material, preparation method and applications
CN110256101A (en) * 2019-06-12 2019-09-20 中国人民解放军海军工程大学 PI chopped strand enhances flexible silicon dioxide silica aerogel composite material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6068882A (en) * 1995-11-09 2000-05-30 Aspen Systems, Inc. Flexible aerogel superinsulation and its manufacture
CN101450852A (en) * 2008-11-27 2009-06-10 长沙星纳气凝胶有限公司 Nano-pore SiO2 aerogel thermal insulation composite material and preparation method thereof
CN102557577A (en) * 2011-11-01 2012-07-11 厦门纳美特新材料科技有限公司 Preparation and method of silicon dioxide aerogel composite material
CN108503327A (en) * 2018-04-13 2018-09-07 航天特种材料及工艺技术研究所 A kind of low cost aeroge thermal insulation material, preparation method and applications
CN110256101A (en) * 2019-06-12 2019-09-20 中国人民解放军海军工程大学 PI chopped strand enhances flexible silicon dioxide silica aerogel composite material and preparation method thereof

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* Cited by examiner, † Cited by third party
Title
李贺军，齐乐华，张守阳: "《先进复合材料学》", 31 December 2016, 西北工业大学出版社 *

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