CN116874278A - Aerogel sheet, method for producing the same, and heat insulating material - Google Patents
Aerogel sheet, method for producing the same, and heat insulating material Download PDFInfo
- Publication number
- CN116874278A CN116874278A CN202310743173.1A CN202310743173A CN116874278A CN 116874278 A CN116874278 A CN 116874278A CN 202310743173 A CN202310743173 A CN 202310743173A CN 116874278 A CN116874278 A CN 116874278A
- Authority
- CN
- China
- Prior art keywords
- sheet
- aerogel
- fiber
- sol
- sheets
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004964 aerogel Substances 0.000 title claims abstract description 140
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000011810 insulating material Substances 0.000 title claims description 3
- 239000000835 fiber Substances 0.000 claims abstract description 70
- 238000000034 method Methods 0.000 claims abstract description 45
- 239000011268 mixed slurry Substances 0.000 claims abstract description 44
- 239000011240 wet gel Substances 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000001879 gelation Methods 0.000 claims abstract description 22
- 230000032683 aging Effects 0.000 claims abstract description 14
- 238000000352 supercritical drying Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000010438 heat treatment Methods 0.000 claims description 25
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 24
- 230000002209 hydrophobic effect Effects 0.000 claims description 22
- 239000003365 glass fiber Substances 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 230000004048 modification Effects 0.000 claims description 13
- 238000012986 modification Methods 0.000 claims description 13
- 150000001282 organosilanes Chemical class 0.000 claims description 13
- 238000000967 suction filtration Methods 0.000 claims description 10
- 238000002210 supercritical carbon dioxide drying Methods 0.000 claims description 9
- 239000006229 carbon black Substances 0.000 claims description 8
- 239000004642 Polyimide Substances 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003605 opacifier Substances 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 6
- 229920001721 polyimide Polymers 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 4
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000007822 coupling agent Substances 0.000 claims description 4
- 239000003063 flame retardant Substances 0.000 claims description 4
- 229920006277 melamine fiber Polymers 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 229920002972 Acrylic fiber Polymers 0.000 claims description 3
- 229920002748 Basalt fiber Polymers 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 229920006231 aramid fiber Polymers 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052863 mullite Inorganic materials 0.000 claims description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- -1 polypropylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 230000002431 foraging effect Effects 0.000 claims 1
- 238000007493 shaping process Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 14
- 239000000084 colloidal system Substances 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 10
- 239000012774 insulation material Substances 0.000 abstract description 6
- 238000000465 moulding Methods 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 description 19
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 15
- 238000009413 insulation Methods 0.000 description 14
- 238000002156 mixing Methods 0.000 description 13
- 238000003860 storage Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000012796 inorganic flame retardant Substances 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 229910004298 SiO 2 Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 239000011259 mixed solution Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 235000010215 titanium dioxide Nutrition 0.000 description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 238000007171 acid catalysis Methods 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- 238000005815 base catalysis Methods 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000001038 titanium pigment Substances 0.000 description 4
- 229920001410 Microfiber Polymers 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000011094 fiberboard Substances 0.000 description 1
- 239000012767 functional filler Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007652 sheet-forming process Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
- C04B41/4922—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as monomers, i.e. as organosilanes RnSiX4-n, e.g. alkyltrialkoxysilane, dialkyldialkoxysilane
- C04B41/4944—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as monomers, i.e. as organosilanes RnSiX4-n, e.g. alkyltrialkoxysilane, dialkyldialkoxysilane containing atoms other than carbon, hydrogen, oxygen, silicon, alkali metals or halogens, e.g. N-silyldisilazane: Image
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/62—Coating or impregnation with organic materials
- C04B41/64—Compounds having one or more carbon-to-metal of carbon-to-silicon linkages
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to an aerogel sheet, a preparation method thereof and a heat insulation material. The preparation method of the aerogel sheet comprises the following steps: providing a mixed slurry comprising a sol and fibers; forming the mixed slurry sheet to obtain a preformed sheet; carrying out gelation reaction on the preformed sheet to obtain a wet gel sheet; and standing and aging the wet gel sheet, and performing supercritical drying to obtain the aerogel sheet. The preparation method not only ensures that the aerogel sheet is more uniform in molding, higher in flatness and better in colloid wettability, but also combines the two steps of preparing the sheet and impregnating the sol into one step, does not need to additionally customize a die, can freely regulate and control the thickness of the sheet, has simple process and convenient operation, can recycle redundant mixed slurry, and is beneficial to reducing the processing cost.
Description
Technical Field
The invention relates to the technical field of aerogel, in particular to an aerogel sheet, a preparation method thereof and a heat insulation material.
Background
The aerogel is a nanoscale porous net-shaped material, has the characteristics of light weight, low density, high porosity and low heat conductivity, can effectively weaken solid heat conduction, and is a high-quality heat insulation material. The aerogel has lower structural strength and is easy to fracture and crush under the action of external force, so that the aerogel needs to be compounded with fibers to prepare an aerogel composite material which takes the fibers as a bearing framework and takes the aerogel as a functional filler.
The aerogel sheet is a flaky aerogel composite material, can be made into products such as heat insulation sheets, heat insulation pads, building energy-saving heat insulation boards and the like, and has wide application requirements in new energy, building industry and aerospace field. At present, the aerogel sheet is prepared by compounding the fiber after prefabricated molding or compression molding with the aerogel, and the aerogel sheet prepared by the two methods has the problems of low flatness, low colloid wettability and the like of the aerogel sheet with thin thickness, and has adverse effects on the heat insulation performance of the aerogel sheet.
Disclosure of Invention
Based on the above, it is necessary to provide an aerogel sheet, a preparation method thereof and a heat insulation material, so as to solve the problems of low flatness of the aerogel sheet with a thin thickness, poor colloid wettability of the aerogel sheet with a large thickness and the like in the aerogel sheet prepared by the conventional method.
The above object of the present invention is achieved by the following technical solutions:
in a first aspect of the present invention, there is provided a method for preparing an aerogel sheet, comprising the steps of:
providing a mixed slurry comprising a sol and fibers;
forming the mixed slurry sheet to obtain a preformed sheet;
carrying out gelation reaction on the preformed sheet to obtain a wet gel sheet;
and standing and aging the wet gel sheet, and performing supercritical drying to obtain the aerogel sheet.
In one embodiment, forming the mixed slurry sheet comprises the steps of: the step of forming the mixed slurry sheet comprises the following steps: homogenizing the mixed slurry for 1-15 min, and carrying out vacuum suction filtration for 0.5-5 min for sheet making.
In one embodiment, the gelling of the preformed sheet comprises the steps of: heating the preformed sheet at 30-70 ℃ for 1-15 min, vacuumizing, and continuing heating for 1-15 min.
In one embodiment, the method further comprises the step of, prior to the step of aging the wet gel sheet by standing: the wet gel sheet is subjected to hydrophobic modification by placing it in organosilane steam.
In one embodiment, the organosilane includes one or more of hexamethyldisilazane, hexamethyldisiloxane, trimethylmethoxysilane, dimethyldimethoxysilane, and trimethylethoxysilane.
In one embodiment, the aerogel sheets have a thickness of 0.2mm to 20mm.
1) The sol comprises one or more of silica sol, titanium oxide sol, alumina sol, ferric oxide sol, magnesium oxide sol, calcium oxide sol, zirconia sol, polyacrylamide sol, polyacrylate sol, polyurethane sol, polyacrylonitrile sol, polyimide sol and epoxy resin sol;
2) The fiber comprises one or more of carbon fiber, activated carbon fiber, graphene fiber, glass fiber, high silica fiber, quartz fiber, silicon carbide fiber, silicon nitride fiber, aluminum oxide fiber, aluminum silicate fiber, mullite fiber, basalt fiber, melamine fiber, polyester fiber, acrylic fiber, polypropylene fiber, aramid fiber and polyimide fiber;
3) The diameter of the fiber is 0.1-30 mu m;
4) The volume ratio of the sol to the fiber is (1-30): (1-20).
In one embodiment, the mixed slurry further comprises an opacifier and/or adjuvant.
In one embodiment, one or more of the following conditions are met:
1) The opacifier comprises one or more of titanium dioxide, white carbon black, barium sulfate, aluminum oxide, zirconium oxide and carbon black;
2) The auxiliary agent comprises one or more of a coupling agent, a pigment and a flame retardant.
In one embodiment, the supercritical drying is supercritical carbon dioxide drying and/or supercritical ethanol drying.
In a second aspect of the present invention, there is provided an aerogel sheet prepared by the method of preparing an aerogel sheet as described above.
In a third aspect of the present invention, there is provided a thermal insulation material comprising the aerogel sheet described above.
The invention has the following beneficial effects:
the invention directly copies and forms the mixed slurry containing sol and fiber, then makes the sol in the preformed sheet undergo the gelation reaction by an in-situ polymerization method, and carries out supercritical drying to obtain the integrally formed aerogel sheet with uniform structure. The sheet forming is a vacuum filtration forming technology, so that the aerogel sheet can be uniformly formed, has high flatness and good colloid wettability no matter under the condition of thinner thickness or thicker thickness, two steps of preparing the sheet and dipping the sheet into one step are combined, an additional custom die is not needed, the thickness of the sheet can be freely regulated and controlled, the process is simple, the operation is convenient, redundant mixed slurry can be recycled, and the processing cost is reduced. Meanwhile, the sol distribution condition of the sheet can be observed and checked in real time in the sheet making process, and the sheet can be complemented at any time, so that the aerogel sheet has good forming performance and high yield.
Detailed Description
The following detailed description of the present invention will provide further details in order to make the above-mentioned objects, features and advantages of the present invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The present invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit of the invention, whereby the invention is not limited to the specific embodiments disclosed below.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
In the conventional technology, the aerogel sheet is generally prepared by prefabricating or pressing fibers into sheets such as needled felt, pressed felt, fiber board or pressed board, and then compositing the sheets with aerogel to form the aerogel sheet. For example, the glass fiber is needled into a felt, then the felt is compounded with aerogel slices, or the felt is compounded with aerogel after being sliced, the forming method needs a needled felt forming process to support, the density and the thickness of the felt are not easy to control, the thickness is generally thicker, the colloid wettability is poorer, and the content of the compounded aerogel is also not well controlled; for example, the glass fiber and the binder are mixed to form a pressed felt or a pressed plate, the forming process can be used for forming a sheet with a thin thickness, but the flatness is low, the content of the aerogel is influenced by the introduction of the binder to influence the heat insulation performance, and the porous structure of the aerogel is influenced by the decomposition of the binder; in addition, when the aerogel is compounded after the fiber is molded, a special die is needed to control the specification and keep the thickness, the die is needed to be customized in advance according to different thicknesses or specifications, the thickness of the sheet cannot be adjusted at any time, the process is complex and complicated, the repeated processing amount is large, and the processing cost is high.
Therefore, in the aerogel sheet prepared by the method, the aerogel sheet with a small thickness has lower flatness, while the aerogel sheet with a large thickness has poorer colloid wettability, so that the heat insulation performance of the aerogel sheet is adversely affected.
There has been reported a method for producing an aerogel sheet by a sheet-forming method, in which components such as fibers, aerogel powder, a binder, an auxiliary agent and the like are mixed to form a slurry, and then sheet-formed in a sheet-forming machine and dried to obtain the aerogel sheet. In the method, the thickness of the sheet can be controlled by controlling the feeding amount of the slurry, but the pore structure of the aerogel powder is easily damaged in the sheet making process; hydrophilic aerogel powders readily adsorb liquids in the slurry, resulting in a change in thermal conductivity; hydrophobic aerogel powder is difficult to mix with other components uniformly, so that the uniformity of the sheet after molding is poor; in addition, the aerogel powder and the fiber are physically mixed, the structure is loose, and the aerogel powder is easy to fall off, so that the heat insulation performance and the service life are not ideal.
Based on the above, the first aspect of the present invention provides a method for preparing an aerogel sheet, so as to solve the problems of low flatness, poor colloid wettability of the aerogel sheet with high thickness and the like of the aerogel sheet prepared by the conventional method. The preparation method comprises the following steps:
providing a mixed slurry comprising a sol and fibers;
forming the mixed slurry sheet to obtain a preformed sheet;
carrying out gelation reaction on the preformed sheet to obtain a wet gel sheet;
and standing and aging the wet gel sheet, and performing supercritical drying to obtain the aerogel sheet.
The invention directly copies and forms the mixed slurry containing sol and fiber, then makes the sol in the preformed sheet undergo the gelation reaction by an in-situ polymerization method, and carries out supercritical drying to obtain the integrally formed aerogel sheet with uniform structure. The sheet forming is a vacuum filtration forming technology, so that the aerogel sheet can be uniformly formed, has high flatness and good colloid wettability no matter under the condition of thinner thickness or thicker thickness, two steps of preparing the sheet and dipping the sheet into one step are combined, an additional custom die is not needed, the thickness of the sheet can be freely regulated and controlled, the process is simple, the operation is convenient, redundant mixed slurry can be recycled, and the processing cost is reduced. Meanwhile, the sol distribution condition of the sheet can be observed and checked in real time in the sheet making process, and the sheet can be complemented at any time, so that the aerogel sheet has good forming performance and high yield.
In some embodiments, the mixed pulp sheet forming comprises the steps of: homogenizing the mixed slurry for 1-15 min, and carrying out vacuum suction filtration for 0.5-5 min for sheet making.
The components such as sol and fiber are fully and uniformly homogenized before sheet forming, which is beneficial to improving the forming performance of aerogel sheets. According to the types and the contents of different components in the mixed slurry, proper homogenization time and vacuum filtration time are selected, so that aerogel sheets with different thicknesses have good uniformity, flatness and colloid wettability.
Preferably, the mixed pulp sheet forming comprises the following steps: and (3) placing the mixed slurry into a constant-temperature slurry box for homogenizing for 1-15 min, placing the mixed slurry into a slurry storage device of a sheet making device, and carrying out vacuum suction filtration for 0.5-5 min for sheet making.
In some embodiments, the subjecting the preformed sheet to a gelation reaction comprises the steps of: heating the preformed sheet at 30-70 ℃ for 1-15 min, vacuumizing, and continuing heating for 1-15 min.
By heating, the gelation reaction of the preformed sheet can be accelerated, an aerogel structure with certain strength and toughness is formed, and the subsequent operation is facilitated. The vacuum pumping can remove bubbles in the preformed sheet material on one hand, improve the structural uniformity of the preformed sheet material, remove steam released in the gelation reaction on the other hand, reduce the concentration of the steam in the reaction vessel and ensure the production safety. After vacuumizing, the vacuum condition is kept for continuous heating, so that the gelation degree of the sheet material can be further improved.
Preferably, the step of causing the preform sheet to undergo a gelation reaction comprises the steps of: and placing the preformed sheet into a flat plate dryer, heating at 30-70 ℃ for 1-15 min, vacuumizing for 5-60 s, and continuing heating for 1-15 min.
In some embodiments, the wet gel sheet further comprises the step of, prior to the aging by standing: the wet gel sheet is subjected to hydrophobic modification by placing it in organosilane steam.
The aerogel sheet generally retains hydrophilic groups such as unreacted hydroxyl groups, and is liable to adsorb moisture, so that the thermal conductivity of the aerogel sheet is increased, and the pore structure thereof may be destroyed. The organic silane is utilized for hydrophobic modification, so that the hydroxyl content of the aerogel sheet can be reduced, and water vapor is prevented from entering the pores of the aerogel sheet, thereby improving the heat insulation performance and the service life of the aerogel sheet.
The vacuum pumping and heating treatment are carried out in the gelation reaction, so that the speed of vaporizing the organosilane reagent into the organosilane steam and the reaction rate of the organosilane steam and the wet gel sheet can be increased, the tedious operation of opening the container and adding the organosilane reagent for long-time dipping is avoided, and the method has the characteristics of high efficiency and convenience.
Preferably, the hydrophobic modification of the wet gel sheet by placing it in an organosilane steam comprises the steps of: the panel dryer after the vacuum is filled with an organosilane reagent, thereby forming organosilane vapors within the panel dryer.
In some embodiments, the organosilane comprises one or more of hexamethyldisilazane, hexamethyldisiloxane, trimethylmethoxysilane, dimethyldimethoxysilane, and trimethylethoxysilane.
Preferably, the time of standing and aging is 2-36 hours.
By standing and aging for a long time, the wet gel sheet can be subjected to sufficient gelation reaction and hydrophobization modification, and an aerogel sheet with high structural strength and good heat insulation performance can be obtained.
In some embodiments, the aerogel sheets have a thickness of 0.2mm to 20mm.
It is understood that the thickness of the aerogel sheet refers to a single layer thickness.
The aerogel sheet prepared by the sheet forming method has high thickness controllability, not only can be prepared into ultrathin sheets with the thickness as low as 0.2mm, but also can be further laminated into super-thick sheets when in use due to the good flatness of the aerogel sheets with the thickness of 0.2-6 mm, thereby meeting different application requirements.
In some embodiments, one or more of the following conditions are met:
1) The sol comprises one or more of silica sol, titanium oxide sol, alumina sol, ferric oxide sol, magnesium oxide sol, calcium oxide sol, zirconia sol, polyacrylamide sol, polyacrylate sol, polyurethane sol, polyacrylonitrile sol, polyimide sol and epoxy resin sol;
2) The fiber comprises one or more of carbon fiber, activated carbon fiber, graphene fiber, glass fiber, high silica fiber, quartz fiber, silicon carbide fiber, silicon nitride fiber, aluminum oxide fiber, aluminum silicate fiber, mullite fiber, basalt fiber, melamine fiber, polyester fiber, acrylic fiber, polypropylene fiber, aramid fiber and polyimide fiber;
3) The diameter of the fiber is 0.1-30 mu m;
4) The volume ratio of the sol to the fiber is (1-30): (1-20).
The aerogel sheets with different diameters, different types of fibers and different types of sol can be manufactured by using the sheet forming method, on one hand, the fibers do not need to be preformed or pressed in advance, the process is simple, the application range is wide, and on the other hand, an adhesive does not need to be introduced, so that adverse effects on the performance of the aerogel sheets are avoided. In addition, the preparation method is particularly suitable for forming ultrathin sheets, ultrathin sheets and sheets containing ultrafine fibers, and the aerogel content in the sheets can be controlled by controlling the volume ratio of sol to fibers, so that the heat insulation performance and the structural strength of the aerogel sheets are properly adjusted to meet the application requirements of different fields.
Preferably, the sol comprises one or more of a silica sol, a titania sol and an alumina sol.
Further preferably, the sol is a silica sol.
Preferably, the fibers are one or more of glass fibers, aluminum silicate fibers, polyester fibers, and melamine fibers.
In some embodiments, the mixed slurry further comprises an opacifier and/or an auxiliary agent.
According to the application function of the aerogel sheet, various functional materials are directly added into the mixed slurry, so that the aerogel sheet with different performances can be obtained, and the application requirements of different fields are met. The light shielding agent can scatter infrared electromagnetic waves, block infrared radiation heat transfer at high temperature and reduce heat conductivity at high temperature.
In some embodiments, one or more of the following conditions are met:
1) The opacifier comprises one or more of titanium dioxide, white carbon black, barium sulfate, aluminum oxide, zirconium oxide and carbon black;
2) The auxiliary agent comprises one or more of a coupling agent, a pigment and a flame retardant.
Preferably, the coupling agent is a silane coupling agent; the pigment is a high-temperature inorganic pigment; the flame retardant is an inorganic flame retardant.
In some embodiments, the supercritical drying is supercritical carbon dioxide drying and/or supercritical ethanol drying.
Drying by supercritical carbon dioxide or supercritical ethanol is an effective method for ensuring that the pores of the aerogel sheet do not collapse during the drying process and minimizing shrinkage of the aerogel sheet during the drying process.
Preferably, the supercritical drying is supercritical carbon dioxide drying.
In a second aspect of the present invention, there is provided an aerogel sheet prepared by the method of preparing an aerogel sheet described above.
In a third aspect, the present invention provides a thermal insulation material comprising the aerogel sheet described above.
The present invention will be described in further detail with reference to specific examples. The raw materials used in the following examples are all commercially available products unless otherwise specified.
Example 1
The aerogel sheets prepared in this example were ultrathin sheets and were not subjected to lamination treatment and hydrophobic modification.
(1) Preparation of SiO by acid/alkali two-step catalysis method 2 Sol: mixing Tetraethoxysilane (TEOS) and ethanol uniformly, adding mixed solution of hydrochloric acid, water and ethanol for acid catalysis, adding mixed solution of ammonia water, water and ethanol for base catalysis after TEOS is hydrolyzed sufficiently, and obtaining SiO 2 And (3) sol.
(2) SiO is made of 2 After the sol and the glass fiber with the diameter of 12 mu m are uniformly mixed, sequentially adding titanium white and inorganic flame retardant, and continuously uniformly mixing to obtain mixed slurry; wherein SiO is 2 The volume ratio of sol to glass fiber is 1.5:1, the mass of the titanium pigment and the inorganic flame retardant is SiO 2 1% of sol mass.
(3) Placing the mixed slurry into a constant temperature slurry box, and stirring and homogenizing for 2min; and (3) placing 300g of homogenized mixed slurry into a slurry storage device of a sheet machine, and carrying out vacuum suction filtration for 0.5min to carry out sheet making to obtain a preformed sheet.
(4) Opening the pulp storage device, taking out the preformed sheet, placing the preformed sheet in a flat plate dryer, heating for 3min at 50 ℃, vacuumizing for 30s, and continuously heating for 1-5 min to enable the preformed sheet to undergo a gelation reaction to obtain the wet gel sheet.
(5) Standing and aging the wet gel sheet for 24 hours, and then utilizing supercritical CO 2 Drying to obtain SiO with thickness of 2mm 2 Aerogel sheets.
Example 2
The aerogel sheets of this example were prepared in substantially the same manner as in example 1, except that: the aerogel sheets are ultra-thick sheets.
(1) Preparation of SiO by acid/alkali two-step catalysis method 2 Sol: mixing Tetraethoxysilane (TEOS) and ethanol uniformly, adding mixed solution of hydrochloric acid, water and ethanol for acid catalysis, adding mixed solution of ammonia water, water and ethanol for base catalysis after TEOS is hydrolyzed sufficiently, and obtaining SiO 2 And (3) sol.
(2) SiO is made of 2 After the sol and the glass fiber with the diameter of 12 mu m are uniformly mixed, sequentially adding titanium white and inorganic flame retardant, and continuously uniformly mixing to obtain mixed slurry; wherein SiO is 2 The volume ratio of sol to glass fiber is 1.5:1, the mass of the titanium pigment and the inorganic flame retardant is SiO 2 1% of sol mass.
(3) Placing the mixed slurry into a constant temperature slurry box, and stirring and homogenizing for 5min; 2250g of homogenized mixed slurry is placed in a slurry storage device of a sheet making device for vacuum suction filtration for 2min to make sheets, and preformed sheets are obtained.
(4) Opening the pulp storage device, taking out the preformed sheet, placing the preformed sheet in a flat plate dryer, heating for 6min at 50 ℃, vacuumizing for 30s, and continuing heating for 5-10 min to enable the preformed sheet to undergo a gelation reaction to obtain the wet gel sheet.
(5) Standing and aging the wet gel sheet for 24 hours, and then utilizing supercritical CO 2 DryingObtaining SiO with thickness of 15mm 2 Aerogel sheets.
Example 3
The aerogel sheets of this example were prepared in substantially the same manner as in example 1, except that: the aerogel sheet is subjected to a hydrophobic modification treatment.
(1) Preparation of SiO by acid/alkali two-step catalysis method 2 Sol: mixing Tetraethoxysilane (TEOS) and ethanol uniformly, adding mixed solution of hydrochloric acid, water and ethanol for acid catalysis, adding mixed solution of ammonia water, water and ethanol for base catalysis after TEOS is hydrolyzed sufficiently, and obtaining SiO 2 And (3) sol.
(2) SiO is made of 2 After the sol and the glass fiber with the diameter of 12 mu m are uniformly mixed, sequentially adding titanium white and inorganic flame retardant, and continuously uniformly mixing to obtain mixed slurry; wherein SiO is 2 The volume ratio of sol to glass fiber is 1.5:1, the mass of the titanium pigment and the inorganic flame retardant is SiO 2 1% of sol mass.
(3) Placing the mixed slurry into a constant temperature slurry box, and stirring and homogenizing for 2min; and (3) placing 300g of homogenized mixed slurry into a slurry storage device of a sheet machine, and carrying out vacuum suction filtration for 0.5min to carry out sheet making to obtain a preformed sheet.
(4) Opening a pulp storage device, taking out the preformed sheet, placing the preformed sheet in a flat plate dryer, filling 2mL of hexamethyldisilazane in the flat plate dryer, heating for 3min at 50 ℃, vacuumizing for 30s, and continuing heating for 3 min-10 min to enable the preformed sheet to undergo a gelation reaction to obtain a wet gel sheet; in the gelation reaction process, hexamethyldisilazane gradually vaporizes, so that the wet gel sheet can be subjected to hydrophobic modification in hexamethyldisilazane vapor to obtain a hydrophobic wet gel sheet.
(5) Standing and aging the hydrophobic wet gel sheet for 24 hours, and then utilizing supercritical CO 2 Drying to obtain hydrophobic SiO with thickness of 2mm 2 Aerogel sheets.
Example 4
The aerogel sheets of this example were prepared in substantially the same manner as in example 3, except that: the fibers used in this example were ultrafine fibers.
(1) Preparation of SiO by acid/alkali two-step catalysis method 2 Sol: mixing Tetraethoxysilane (TEOS) and ethanol uniformly, adding mixed solution of hydrochloric acid, water and ethanol for acid catalysis, adding mixed solution of ammonia water, water and ethanol for base catalysis after TEOS is hydrolyzed sufficiently, and obtaining SiO 2 And (3) sol.
(2) SiO is made of 2 After the sol and the glass fiber with the diameter of 4 mu m are uniformly mixed, sequentially adding titanium white and inorganic flame retardant, and continuously uniformly mixing to obtain mixed slurry; wherein SiO is 2 The volume ratio of sol to glass fiber is 1.5:1, the mass of the titanium pigment and the inorganic flame retardant is SiO 2 1% of sol mass.
(3) Placing the mixed slurry into a constant temperature slurry box, and stirring and homogenizing for 2min; and (3) placing 300g of homogenized mixed slurry into a slurry storage device of a sheet machine, and carrying out vacuum suction filtration for 0.5min to carry out sheet making to obtain a preformed sheet.
(4) Opening a pulp storage device, taking out the preformed sheet, placing the preformed sheet in a flat plate dryer, filling 2mL of hexamethyldisilazane in the flat plate dryer, heating for 3min at 50 ℃, vacuumizing for 30s, and continuing heating for 3 min-10 min to enable the preformed sheet to undergo a gelation reaction to obtain a wet gel sheet; in the gelation reaction process, hexamethyldisilazane gradually vaporizes, so that the wet gel sheet can be subjected to hydrophobic modification in hexamethyldisilazane vapor to obtain a hydrophobic wet gel sheet.
(6) Standing and aging the hydrophobic wet gel sheet for 24 hours, and then utilizing supercritical CO 2 Drying to obtain hydrophobic SiO with thickness of 2mm 2 Aerogel sheets.
Example 5
The aerogel sheets of this example were prepared in substantially the same manner as in example 3, except that: the sol used in this example was TiO 2 /Al 2 O 3 And (3) sol.
(1) Preparation of TiO 2 /Al 2 O 3 Sol: inorganic aluminum salt, water, ethanol, alkaline catalyst and TiO 2 The TiO is prepared by reaction of propylene oxide as raw material 2 /Al 2 O 3 And (3) sol.
(2) TiO is mixed with 2 /Al 2 O 3 After the sol and the glass fiber with the diameter of 12 mu m are uniformly mixed, sequentially adding the white carbon black and the inorganic flame retardant, and continuously uniformly mixing to obtain mixed slurry; wherein, tiO 2 /Al 2 O 3 The volume ratio of sol to glass fiber is 1.5:1, the mass of the white carbon black and the inorganic flame retardant is TiO 2 /Al 2 O 3 1% of sol mass.
(3) Placing the mixed slurry into a constant temperature slurry box, and stirring and homogenizing for 2min; and (3) placing 300g of homogenized mixed slurry into a slurry storage device of a sheet machine, and carrying out vacuum suction filtration for 0.5min to carry out sheet making to obtain a preformed sheet.
(4) Opening a pulp storage device, taking out the preformed sheet, placing the preformed sheet in a flat plate dryer, filling 2mL of hexamethyldisilazane in the flat plate dryer, heating for 3min at 50 ℃, vacuumizing for 30s, and continuing heating for 3 min-10 min to enable the preformed sheet to undergo a gelation reaction to obtain a wet gel sheet; in the gelation reaction process, hexamethyldisilazane gradually vaporizes, so that the wet gel sheet can be subjected to hydrophobic modification in hexamethyldisilazane vapor to obtain a hydrophobic wet gel sheet.
(5) Standing and aging the hydrophobic wet gel sheet for 24 hours, and then utilizing supercritical CO 2 Drying to obtain hydrophobic TiO with thickness of 2mm 2 /Al 2 O 3 Aerogel sheets.
Comparative example 1
The aerogel sheet of this comparative example was prepared by a compression molding method.
(1) Preparation of SiO by acid/alkali two-step catalysis method 2 Sol: mixing Tetraethoxysilane (TEOS) and ethanol uniformly, adding mixed solution of hydrochloric acid, water and ethanol for acid catalysis, adding mixed solution of ammonia water, water and ethanol for base catalysis after TEOS is hydrolyzed sufficiently, and obtaining SiO 2 And (3) sol.
(2) Needling glass fibers with the diameter of 12 mu m into felt-shaped fibers with the thickness of 3mm, cutting the felt into fiber sheets, and pressing the fiber sheets with the thickness of 3mm into fiber sheets with the thickness of 2mm by using clamping bars and steel plates with the thickness of 2 mm; multiple ones ofStacking the pressed fiber sheets on SiO 2 And (3) immersing the sheet in the sol for 15min under vacuum condition to obtain the preformed sheet.
(3) Taking out the preformed sheet, placing the preformed sheet in a flat plate dryer, heating for 3min at 50 ℃, vacuumizing for 30s, and continuing heating for 3-10 min to obtain the wet gel sheet.
(5) Standing and aging the wet gel sheet for 24 hours, and then utilizing supercritical CO 2 Drying to obtain SiO with thickness of 2mm 2 Aerogel sheets.
Comparative example 2
The aerogel sheet of this comparative example was produced by mixing aerogel powder with fibers and then sheet molding.
(1) SiO is made of 2 After uniformly mixing aerogel powder and glass fiber with the diameter of 12 mu m, sequentially adding a binder, titanium dioxide and an inorganic flame retardant, and continuously uniformly mixing to obtain mixed slurry; wherein SiO is 2 The volume ratio of the aerogel powder to the glass fiber is 1:1.
(2) Placing the mixed slurry into a constant temperature slurry box, and stirring and homogenizing for 5min; 2250g of homogenized mixed slurry is placed in a slurry storage device of a sheet making device for vacuum suction filtration for 0.5min to make sheets, and preformed sheets are obtained.
(3) Opening the slurry storage device, taking out the preformed sheet, placing in a flat plate dryer, heating at 50deg.C for 6min, vacuumizing for 30s, and heating for 15min to obtain SiO with thickness of 2mm 2 Aerogel sheets.
Test case
According to the regulations of GB/T34336-2017 nano-porous aerogel composite heat insulation products, the surface of the aerogel sheet should be flat and no flaws, stains and damages which prevent the use are required; when the waterproof and dampproof requirements exist, the hydrophobicity should be not less than 98.0%; the bending failure load should be not less than 60N. The aerogel sheets described above were tested for appearance, thickness, hydrophobicity, thermal conductivity and flexural failure load according to GB/T34336-2017 nanoporous aerogel composite insulation product, and the results are shown in Table 1.
As can be seen from Table 1, the aerogel sheets of examples 1 to 5 were good in surface flatness, free of cracks and substantially free of residual raised particles, and the aerogel sheets prepared by the sheet forming method were characterized by uniform formation, high flatness and good colloid wettability, and were particularly suitable for preparing ultrathin sheets, ultra-thick sheets and sheets containing ultrafine fibers. The aerogel sheets of examples 1 to 5 had thermal conductivities in the range of 0.0142W/(m.K) to 0.0166W/(m.K) and were each satisfactory in terms of flexural failure load of 60N or more, indicating that the aerogel sheets produced by the sheet-forming method were high in heat insulating property and structural strength. In addition, the aerogel sheets of examples 3 to 5 were subjected to hydrophobic modification treatment, and the hydrophobic rates thereof were 99%, and were excellent in water resistance and moisture resistance.
The aerogel sheet of comparative example 1 had poor surface flatness, no cracks, some residual raised particles, and required additional cleaning; in the preparation of aerogel sheets by the preforming method, a plurality of fiber sheets are generally stacked and then immersed in sol, so that incomplete impregnation is easy to occur, and partial areas of the finally formed sheets are softer; the aerogel sheets of comparative example 1 had higher thermal conductivities than the aerogel sheets of examples 1-5. Accordingly, the aerogel sheets prepared by the conventional preforming method were inferior to those of examples 1 to 5 in terms of molding uniformity, surface smoothness, colloid wettability and heat insulation properties.
The aerogel sheet of comparative example 2 had good surface flatness, but had cracks and grains that affected its normal use; the aerogel sheets of comparative example 2 had a significantly higher thermal conductivity than the aerogel sheets of examples 1 to 5, increased by 73.6% compared to example 1, and had poor thermal insulation properties; after the bending fracture load test, the corners of the sheet are cracked and the surfaces have chipping cracks. This is because the aerogel powder is liable to be destroyed in the pore structure during the sheet forming process, and the undamaged pores are liable to adsorb the slurry of the sheet, and the formed aerogel sheet is relatively loose in structure, resulting in the aerogel sheet of comparative example 2 being relatively poor in both heat insulating property and structural strength.
TABLE 1 test results for aerogel sheets of examples 1-5 and comparative examples 1-2
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. The scope of the invention is, therefore, indicated by the appended claims, and the description may be intended to interpret the contents of the claims.
Claims (12)
1. A method of preparing aerogel sheets comprising the steps of:
providing a mixed slurry comprising a sol and fibers;
forming the mixed slurry sheet to obtain a preformed sheet;
carrying out gelation reaction on the preformed sheet to obtain a wet gel sheet;
and standing and aging the wet gel sheet, and performing supercritical drying to obtain the aerogel sheet.
2. The method of producing aerogel sheets of claim 1, wherein shaping the mixed slurry sheet comprises the steps of: homogenizing the mixed slurry for 1-15 min, and carrying out vacuum suction filtration for 0.5-5 min for sheet making.
3. The method of producing aerogel sheets of claim 2 wherein said subjecting said preformed sheets to a gelation reaction comprises the steps of: heating the preformed sheet at 30-70 ℃ for 1-15 min, vacuumizing, and continuing heating for 1-15 min.
4. The method of producing an aerogel sheet as claimed in claim 3, further comprising the step of, before the wet gel sheet is left to stand for aging: the wet gel sheet is subjected to hydrophobic modification by placing it in organosilane steam.
5. The method of making aerogel sheets of claim 4, wherein the organosilane comprises one or more of hexamethyldisilazane, hexamethyldisiloxane, trimethylmethoxysilane, dimethyldimethoxysilane, and trimethylethoxysilane.
6. The method of producing an aerogel sheet according to any one of claims 1 to 5, wherein the aerogel sheet has a thickness of 0.2mm to 20mm.
7. The method of preparing aerogel sheets according to any one of claims 1 to 5, wherein one or more of the following conditions are satisfied:
1) The sol comprises one or more of silica sol, titanium oxide sol, alumina sol, ferric oxide sol, magnesium oxide sol, calcium oxide sol, zirconia sol, polyacrylamide sol, polyacrylate sol, polyurethane sol, polyacrylonitrile sol, polyimide sol and epoxy resin sol;
2) The fiber comprises one or more of carbon fiber, activated carbon fiber, graphene fiber, glass fiber, high silica fiber, quartz fiber, silicon carbide fiber, silicon nitride fiber, aluminum oxide fiber, aluminum silicate fiber, mullite fiber, basalt fiber, melamine fiber, polyester fiber, acrylic fiber, polypropylene fiber, aramid fiber and polyimide fiber;
3) The diameter of the fiber is 0.1-30 mu m;
4) The volume ratio of the sol to the fiber is (1-30): (1-20).
8. The method of producing aerogel sheets according to any one of claims 1 to 5, wherein the mixed slurry further comprises an opacifier and/or an auxiliary agent.
9. The method of preparing aerogel sheets of claim 8, wherein one or more of the following conditions are satisfied:
1) The opacifier comprises one or more of titanium dioxide, white carbon black, barium sulfate, aluminum oxide, zirconium oxide and carbon black;
2) The auxiliary agent comprises one or more of a coupling agent, a pigment and a flame retardant.
10. The method of producing aerogel sheets according to any of claims 1 to 5, wherein the supercritical drying is supercritical carbon dioxide drying and/or supercritical ethanol drying.
11. An aerogel sheet produced by the method for producing an aerogel sheet according to any one of claims 1 to 10.
12. An insulating material comprising the aerogel sheet according to claim 11.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310743173.1A CN116874278B (en) | 2023-06-21 | 2023-06-21 | Aerogel sheet, method for producing the same, and heat insulating material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310743173.1A CN116874278B (en) | 2023-06-21 | 2023-06-21 | Aerogel sheet, method for producing the same, and heat insulating material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116874278A true CN116874278A (en) | 2023-10-13 |
| CN116874278B CN116874278B (en) | 2024-09-10 |
Family
ID=88255886
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310743173.1A Active CN116874278B (en) | 2023-06-21 | 2023-06-21 | Aerogel sheet, method for producing the same, and heat insulating material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116874278B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105236912A (en) * | 2015-08-31 | 2016-01-13 | 武汉理工大学 | Composite fiber-reinforced hydrophobic SiO2 aerogel and preparation method thereof |
| CN107098354A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method from hydrophobic silicon hydrochlorate aerogel material |
| CN108373316A (en) * | 2018-05-17 | 2018-08-07 | 航天特种材料及工艺技术研究所 | A kind of aerogel heat-proof paper and preparation method thereof |
| CN114804927A (en) * | 2022-05-23 | 2022-07-29 | 谷城钜沣陶瓷有限公司 | Waterproof heat-insulating tile and production process thereof |
-
2023
- 2023-06-21 CN CN202310743173.1A patent/CN116874278B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105236912A (en) * | 2015-08-31 | 2016-01-13 | 武汉理工大学 | Composite fiber-reinforced hydrophobic SiO2 aerogel and preparation method thereof |
| CN107098354A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method from hydrophobic silicon hydrochlorate aerogel material |
| CN108373316A (en) * | 2018-05-17 | 2018-08-07 | 航天特种材料及工艺技术研究所 | A kind of aerogel heat-proof paper and preparation method thereof |
| CN114804927A (en) * | 2022-05-23 | 2022-07-29 | 谷城钜沣陶瓷有限公司 | Waterproof heat-insulating tile and production process thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116874278B (en) | 2024-09-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108778707B (en) | Insulating material | |
| JP4120992B2 (en) | COMPOSITE MATERIAL CONTAINING AIRGEL AND ADHESIVE, ITS MANUFACTURING METHOD, AND USE THEREOF | |
| KR101919121B1 (en) | Aerogel Composite and Preparation Method Thereof | |
| CN107814552B (en) | Silicon dioxide heat insulation composite material and preparation method thereof | |
| CN1085143C (en) | Multilayer composite materials with at least one aerogel-contg. layer and at least one layer contg. polyethylene terephthalate fibres, process for producing same and their use | |
| KR102715882B1 (en) | Insulating composite materials comprising an inorganic aerogel and a melamine foam | |
| KR100366475B1 (en) | Fabrication method of fiber-reinforced xerogel and its use | |
| CN1060749C (en) | Composite material containing aerogel, process for manufacturing said material and use thereof | |
| US10058836B2 (en) | Process for producing aerogels by dielectric heating | |
| CN111607253B (en) | Preparation method of silica aerogel thermal insulation filler | |
| CN109265131A (en) | A kind of preparation method of aerogel vacuum thermal insulation plate and its core material | |
| CN112661477B (en) | Preparation method of modified polystyrene-basic magnesium sulfate cement composite thermal insulation material | |
| CN113402252A (en) | Aerogel modified fiber felt heat insulation composite material and preparation method thereof | |
| CN116874278B (en) | Aerogel sheet, method for producing the same, and heat insulating material | |
| JP4462600B2 (en) | Method for producing calcium silicate material | |
| CN115043408B (en) | Flexible silica aerogel, aerogel felt and preparation method thereof | |
| JP3164291B2 (en) | Manufacturing method of core material for vacuum insulation structure | |
| Gao et al. | Mechanical properties of aerogel-ceramic fiber composites | |
| CN1044881C (en) | Artificial straw board and its manufacturing technology | |
| US20070072761A1 (en) | Manufacturing method of ceramic body with excellent adiabatic capacity | |
| Lü et al. | Structure and characterization of Chinese fir (Cunninghamia lanceolata) wood/MMT intercalation nanocomposite (WMNC) | |
| KR102583742B1 (en) | Manufacturing method of Functional Low-density E-glass fiber with hydrophobicity | |
| KR102693636B1 (en) | Manufacturing method for multi-layered insulation sheet without binder and multi-layered insulation sheet therefrom | |
| CN118145915B (en) | High heat insulation calcium silicate board | |
| CN115464942B (en) | Radiation-resistant high-temperature-resistant heat insulation material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |