CN111018473A - Heat insulation material containing gradient-distributed anti-radiation agent and preparation method and application thereof - Google Patents
Heat insulation material containing gradient-distributed anti-radiation agent and preparation method and application thereof Download PDFInfo
- Publication number
- CN111018473A CN111018473A CN201911314140.5A CN201911314140A CN111018473A CN 111018473 A CN111018473 A CN 111018473A CN 201911314140 A CN201911314140 A CN 201911314140A CN 111018473 A CN111018473 A CN 111018473A
- Authority
- CN
- China
- Prior art keywords
- radiation
- agent
- dispersion liquid
- fiber
- mass
- 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
- 239000000718 radiation-protective agent Substances 0.000 title claims abstract description 40
- 239000012774 insulation material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 85
- 239000006185 dispersion Substances 0.000 claims abstract description 82
- 230000005855 radiation Effects 0.000 claims abstract description 66
- 239000007788 liquid Substances 0.000 claims abstract description 57
- 239000011810 insulating material Substances 0.000 claims abstract description 37
- 239000002131 composite material Substances 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- 230000002787 reinforcement Effects 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 26
- 230000032683 aging Effects 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 24
- 238000009826 distribution Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 77
- 238000011282 treatment Methods 0.000 claims description 40
- 239000000377 silicon dioxide Substances 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 35
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 26
- 235000012239 silicon dioxide Nutrition 0.000 claims description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 238000000352 supercritical drying Methods 0.000 claims description 14
- 238000013329 compounding Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 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 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052863 mullite Inorganic materials 0.000 claims description 7
- 239000010453 quartz Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010574 gas phase reaction Methods 0.000 claims description 6
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 230000002209 hydrophobic effect Effects 0.000 claims description 4
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical group CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 230000009257 reactivity Effects 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 3
- 229920002748 Basalt fiber Polymers 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- -1 more preferably Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 239000003292 glue Substances 0.000 abstract description 7
- 238000001914 filtration Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 83
- 239000000463 material Substances 0.000 description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 22
- 238000005086 pumping Methods 0.000 description 18
- 239000011259 mixed solution Substances 0.000 description 15
- 238000001879 gelation Methods 0.000 description 13
- 230000003471 anti-radiation Effects 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- 230000001105 regulatory effect Effects 0.000 description 8
- 238000009413 insulation Methods 0.000 description 6
- 239000004964 aerogel Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 description 2
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000009828 non-uniform distribution Methods 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000000191 radiation effect Effects 0.000 description 1
- 229940124553 radioprotectant Drugs 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
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
- 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
-
- 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
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic System; Aluminates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- 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
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/0037—Materials containing oriented fillers or elements
- C04B2111/00379—Materials containing oriented fillers or elements the oriented elements being fibres
-
- 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
Abstract
The invention relates to a heat insulation material containing a radiation resistant agent in gradient distribution, and a preparation method and application thereof, wherein the heat insulation material comprises the following components: respectively adjusting the surface group reaction activity and the surface polarity of the fiber reinforcement by utilizing the silicon-aluminum composite sol and the silane coupling agent; preparing a dispersion liquid containing a silica sol precursor, a surfactant, a catalyst and different concentrations of an anti-radiation agent; and adding the dispersion liquid with high concentration of the anti-radiation agent into the dispersion liquid with low concentration to form mixed dispersion liquid, injecting glue, and then gelling, aging and drying. The invention also relates to the heat-insulating material prepared by the method and application thereof. The heat-insulating material has a structure that the radiation-resistant particles are uniformly and discretely distributed in the surface and are in normal gradient and discrete distribution, the radiation-resistant efficiency caused by the same-quality radiation-resistant agent is maximized while the excellent integrity is ensured, the adsorption and filtration effects of the fibers on the radiation-resistant agent particles are eliminated, the random matching of the reinforcement fibers and the radiation-resistant agent is realized, and the agglomeration problem is solved.
Description
Technical Field
The invention relates to a heat insulation material containing a radiation resistant agent in gradient distribution, and a preparation method and application thereof, and belongs to the technical field of thermal protection.
Background
Nanometer heat insulating materials represented by oxide aerogel materials such as silicon dioxide and aluminum oxide have the advantages of high temperature resistance, light weight, excellent heat insulating performance, stable performance and the like, and are widely applied to the fields of aviation, aerospace, deep space exploration and civil heat insulation at home and abroad at present. The nanometer skeleton and nanometer pore structure of the material can inhibit solid phase heat conduction and convection heat conduction greatly, so that the material has excellent heat insulating effect. However, the material has good permeability to infrared radiation in a high-temperature region, and the radiation heat transfer ratio can be rapidly increased along with the increase of the temperature and gradually becomes a main heat transfer mode, so that the thermal conductivity of the material at the corresponding temperature can be greatly increased along with the increase of the use temperature, and the corresponding use thickness can also be greatly increased. Therefore, in order to achieve a better high-temperature heat insulation effect, the materials must be subjected to a heat radiation resistant treatment. However, although the current anti-thermal radiation technology can inhibit the thermal radiation effect to a certain extent, the radiation resistance efficiency, the material integrity, the material weight, the process operability and other aspects are greatly sacrificed, thereby affecting the application range of the material.
In known reports, radiation-resistant treatment of materials is mainly achieved by several means: (1) by inserting the multilayer reflecting screen into the aerogel material matrix, thermal infrared radiation of the material in the using process can be effectively inhibited, (see CN201010148105.3, named as a nanometer multilayer composite heat-insulating material and a preparation method thereof, and CN201811066573.9, named as a multilayer heat-protecting material and a preparation method thereof), so that the high-temperature heat conductivity of the material is effectively reduced. (2) The preparation method comprises the steps of forming a dispersion system in a sol solution by using micron-sized anti-radiation agent powder, compounding the dispersion system with reinforcing fibers, and finishing the introduction of an anti-radiation structure by regulating a rapid gelation method (refer to CN201410206827.8, namely polyimide aerogel with infrared radiation resistance and a preparation method thereof). (3) The reinforcement is radiation resistant. The radiation-resistant reinforcement can be obtained by adopting the radiation-resistant fiber or introducing the radiation-resistant agent on the surface of the fiber, and the introduction of the radiation-resistant structure of the aerogel material can be realized by directly compounding the reinforcement by using the sol (refer to CN107032736A, namely a high-temperature-resistant radiation wave-transparent heat-insulating material and a preparation method thereof). However, although the introduction of the reflective screen can effectively improve the high-temperature heat-insulating property of the material, the integral formability and air permeability of the material are weakened due to the macroscopically formed multilayer structure, and the risk of layering, bulging and the like exists when the material is used in an atmospheric environment; meanwhile, the materials obtained by the latter two modes of introducing the anti-radiation agents have good integrity, but the overall uniformly distributed anti-radiation structure cannot be well matched with the temperature gradient distribution rule of the materials in the thickness direction in the high-temperature use process, and the weight of the redundant anti-radiation agents and the solid-phase heat conduction are increased. In addition, in the process of compounding the precursor with fibers after the radiation-resistant agent is added, local agglomeration caused by adsorption of fiber networks and filtration of radiation-resistant particles also exists. In the scheme of the reinforcing body fiber for resisting heat radiation, the radiation resisting agent is only concentrated on the surface of the fiber, so that the problem of nonuniform distribution of the radiation resisting agent exists. In a word, the heat radiation resistance efficiency of the heat radiation resistant structure is reduced, so that the further improvement of the high-temperature heat insulation efficiency of the high-performance heat insulation material in the application process of a large-scale integrated heat protection system is restricted.
Disclosure of Invention
To overcome the disadvantages of the prior art, the present invention provides in a first aspect a method for preparing a thermal insulation material comprising a graded distribution of radiation resistant agent, the method comprising the steps of:
(1) surface treatment: adjusting the surface group reactivity of a fiber reinforcement by using a composite sol containing silicon dioxide and aluminum oxide, and then adjusting the fiber surface polarity of the fiber reinforcement by using a silane coupling agent;
(2) preparing a precursor dispersion liquid: dispersing an anti-radiation agent into a silica sol precursor to obtain a first dispersion liquid with a first anti-radiation agent concentration and a second dispersion liquid with a second anti-radiation agent concentration, wherein the first anti-radiation agent concentration is lower than the second anti-radiation agent concentration; then adding a surfactant to each of the first dispersion liquid and the second dispersion liquid and uniformly stirring;
(3) gradient compounding: adding a catalyst into the first dispersion liquid and the second dispersion liquid prepared in the step (2) and uniformly mixing; then adding the first dispersion liquid from the first container into a second container containing the second dispersion liquid at a first flow rate and stirring to form a mixed dispersion liquid, and injecting the mixed dispersion liquid into a mold containing the fiber reinforcement prepared in the step (1) at a second flow rate during the stirring and allowing the mixed dispersion liquid to gel to prepare a gel composite;
(4) aging: aging the gel composite to obtain an aged composite;
(5) and (3) drying: and drying the aged composite material to obtain the heat-insulating material.
The present invention provides, in a second aspect, a thermal insulation material produced by the production method according to the first aspect of the present invention.
The present invention provides, in a second aspect, an insulation member comprising the insulation material according to the second aspect of the present invention.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) the heat-resistant radiation structure of the heat-insulating material prepared by the method disclosed by the invention breaks through the problem that the existing heat-insulating material heat-resistant radiation method cannot meet the requirements of integral forming, high-efficiency radiation resistance and adjustable distribution at the same time, and the provided structure with the radiation-resistant particles in the heat-insulating material matrix in uniform and discrete distribution and normal gradient and discrete distribution is formed, so that the excellent integrity of the material is ensured, the maximization of the same-quality heat-resistant radiation agent and the radiation-resistant efficiency is realized, the high-temperature heat-insulating efficiency of the material is effectively improved, and the dosage of the radiation-resistant agent is reduced by about 50%.
(2) The integrated molding preparation of the normal continuous gradient distribution composite material is realized by a specific compounding mode and utilizing a sol-gel reaction, and the distribution gradient is adjustable.
(3) By regulating and controlling the polarity of the surface of the fiber, the adsorption and filtration effects of the fiber network on micron-sized anti-radiation particles are effectively solved, the random matching between different types of fibers and anti-radiation agents is realized, the uniform and discrete distribution can be realized, and the agglomeration problem is solved.
Drawings
Fig. 1 is a schematic view of a gradient radiation-resistant structural composite device.
FIG. 2 is a process flow diagram of one embodiment of the preparation method of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, specific embodiments of the present invention will be described in detail and fully hereinafter with reference to the accompanying drawings. It is to be understood, however, that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments obtained by a person skilled in the art without any inventive step based on the inventive concept of the present invention are within the scope of the present invention.
The present invention provides in a first aspect a method of preparing a thermal insulation material comprising a gradient distribution of radiation resistant agent, the method comprising the steps of:
(1) surface treatment: adjusting the surface group reactivity of a fiber reinforcement by using a composite sol containing silicon dioxide and aluminum oxide, and then adjusting the fiber surface polarity of the fiber reinforcement by using a silane coupling agent;
(2) preparing a precursor dispersion liquid: dispersing an anti-radiation agent into a silica sol precursor to obtain a first dispersion liquid (namely, a dispersion liquid with low anti-radiation agent content) with a first anti-radiation agent concentration and a second dispersion liquid (namely, a dispersion liquid with high anti-radiation agent content) with a second anti-radiation agent concentration, wherein the first anti-radiation agent concentration is lower than the second anti-radiation agent concentration; then adding a surfactant to each of the first dispersion liquid and the second dispersion liquid and uniformly stirring;
(3) gradient compounding: adding a catalyst into the first dispersion liquid and the second dispersion liquid prepared in the step (2) and uniformly mixing; then adding the first dispersion liquid from the first container into a second container containing the second dispersion liquid at a first flow rate and stirring to form a mixed dispersion liquid, and injecting the mixed dispersion liquid into a mold containing the fiber reinforcement prepared in the step (1) at a second flow rate during the stirring and allowing the mixed dispersion liquid to gel to prepare a gel composite;
(4) aging: aging the gel composite to obtain an aged composite;
(5) and (3) drying: and drying the aged composite material to obtain the heat-insulating material.
In some preferred embodiments, the method further comprises the steps of:
(6) moisture-proof treatment: and carrying out moisture-proof treatment on the heat-insulating material by using a hydrophobic treatment agent, preferably, the hydrophobic treatment agent is trimethyl methoxy silane, and more preferably, the moisture-proof treatment is carried out by means of gas phase treatment.
The process flow diagram of the preparation method of the invention is shown in figure 2. Firstly, the surface treatment is carried out on the fiber reinforcement, then the prepared precursor dispersion liquid is utilized for gradient compounding, and then aging and drying are carried out, and when necessary, damp-proof treatment is carried out. The aging, drying, and moisture-proof treatments may be performed by methods well known to those skilled in the art.
In the step (1), the fiber reinforcement can be impregnated with silica/alumina sol and then dried, the reactivity of the surface group of the material is regulated and controlled by adjusting the ratio of silica to alumina on the surface of the fiber, the gas phase reaction treatment is carried out on the surface of the fiber under the condition of vacuum heating by adopting a silane coupling agent, and the surface of the fiber is controlled to have proper surface polarity by the gas phase reaction.
In the step (2), the radiation-resistant particles, for example, particles having a specific particle size, may be dispersed in the silica sol precursor, and if necessary, the pH is adjusted to a range of 5 to 9, and then the surfactant is added to obtain stable precursor dispersion liquid systems having different radiation-resistant agent contents.
In step (3), a sol-gel catalyst, for example, having a certain concentration may be added to the precursor dispersion system having different amounts of the radioprotectant obtained in step (2), and sufficiently mixed. The gradient glue injection mode in the step (3) can be realized by a device shown in fig. 1, and the preparation and structural compounding of a gradient radiation-resistant dispersion system are realized by a pump/stirring/pump mode, wherein a precursor dispersion liquid with low radiation-resistant agent content is added into a dispersion liquid system with high radiation-resistant agent content at a preset flow rate, the system can be quickly stirred to be fully and uniformly mixed, glue injection is carried out in a mould filled with the fiber reinforcement in the step (1) at a preset flow rate in the stirring process until the mould is completely filled, the mould is pressurized to remove gas, and gel is kept still to complete the construction of a radiation-resistant gradient structure, wherein the gradient distribution condition of the radiation-resistant agent can be regulated and controlled by adopting the volume ratio and the glue injection flow rate among different dispersion systems.
In step (4), the composite material after gelling in step (3) may be aged at, for example, 80 ℃ to improve the reaction degree and increase the structural strength of the material.
In the step (5), the solvent in the gel material in the step (4) is removed in a drying mode, and the high-efficiency heat-insulating material with the gradient anti-radiation structure is obtained.
Where necessary, a moisture barrier treatment may be carried out in step (6), for example by subjecting the material to a moisture barrier treatment by means of a gas phase treatment, for example with trimethylmethoxysilane, to obtain the final heat insulating material.
Preferably, in the step (1), the fiber reinforcement is impregnated with the composite sol, then dried, and then the fiber surface of the fiber reinforcement is subjected to gas phase reaction treatment with the silane coupling agent under vacuum heating.
Further preferably, in the step (2), the radiation-resistant agent is a pellet having a particle size of 1 to 10 μm (e.g., 2, 4, 5, or 8 μm). It is also preferred that the pH of the first dispersion and the second dispersion are each independently adjusted to 5 to 9 (e.g., 5, 6, 7, 8, or 9) prior to addition of the surfactant. The adjustment can be carried out using concentrated hydrochloric acid or concentrated ammonia.
It is also preferable that, in the step (3), the mixed dispersion is injected until the mold is completely filled, then deaerated by pressing, and the gel is left to stand.
It is also preferred that in step (4), the aging is carried out at a temperature of 70 ℃ to 90 ℃, for example 80 ℃, for an aging time of 12 to 24 hours (for example 18 hours).
It is also preferred that in step (5), the drying is carried out until the solvent in the aged composite material is completely removed.
Further preferably, the composite sol is obtained by mixing 5 to 20 mass% (e.g., 5%, 10%, 15%, 20%) of a silica sol and 5 to 20 mass% (e.g., 5%, 10%, 15%, 20%) of an alumina sol. More preferably, the mass ratio of silica/alumina in the composite sol is 0:1 to 1:0 (e.g., 0:1, 1:5, 1:10, 1:100, 1:1000, 1:10000, 1: 0). More preferably, the solid content of the composite sol is 1 to 20 mass%.
It is also preferred that the solvent of the composite sol is selected from the group consisting of an alcohol solvent having a boiling point of less than 120 ℃ and water, more preferably water. The alcohol solvent having a boiling point of less than 120 ℃ may be selected from the group consisting of ethanol, n-propanol, isopropanol, butanol, isoamyl alcohol and hexanol, for example.
In the preparation method of the present invention, the kind of the fiber used for the heat insulating material is not limited. Preferably, however, the fibers used for the fiber reinforcement are refractory oxide fibers, more preferably selected from the group consisting of basalt fibers, quartz fibers, mullite fibers, alumina fibers, zirconia fibers.
It is also preferred that the silane coupling agent is of the formula Si (OR)4Wherein R is a non-aromatic carbon chain substituent having 1 to 10 carbons, such as a substituent selected from the group consisting of methyl, ethyl, n-propyl, isopropyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, and decyl. For example, the silane coupling agent is selected from the group consisting of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, and tetraisopropoxysilane, but is not limited thereto.
Preferably, the silane coupling agent is used in an amount of 1% to 20% (e.g. 2, 5, 1 or 15%) of the mass of the fiber reinforcement. More preferably, the heating is carried out at a temperature of 80 ℃ to 200 ℃ (e.g., 100 or 150 ℃), and the treatment time of the gas-phase reaction treatment is 6 to 12 hours (e.g., 8 or 10 hours).
It is also preferable that, in the step (2), the radiation-resistant agent is selected from the group consisting of rutile titanium dioxide, boron nitride, silicon carbide and ferroferric oxide. More preferably, the radiation resistant agent is used in an amount of 5% to 200% (e.g., 5%, 10%, 15%, 20%, 30%, 40%, 50%, 100%, 150%, 200%) by mass of the silica sol precursor. More preferably, the surfactant is polyethylene glycol with a molecular weight of 400-1000 (such as 400, 600, 800, 1000). More preferably, the surfactant is used in an amount of 0.1% to 1% (e.g., 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 1%) by mass of the radiation resistant agent.
It is also preferred that, in step (2), the first concentration of the radiation resistant agent is 1% to 90% (e.g., 1, 10, 20, 30, 40, 50, 60, 70, 80, or 90%) of the second concentration of the radiation resistant agent.
In step (3), the catalyst is preferably a sol-gel catalyst, and may be aqueous ammonia or an aqueous ammonium fluoride solution (e.g., 0.1%, 0.5%, 5%, 10%, 15%, 20%) having a concentration of 0.1 to 20% by mass. More preferably, the catalyst is used in an amount of 0.5 to 5% (e.g., (0.5%, 1%, 1.5%, 2%, 3%, 4%, 5%) of the mass of the dispersion or, in some alternative embodiments, in an amount necessary to control the difference in gel time between the first dispersion and the second dispersion to be 0.5 to 1 h.
It is also preferred that the gradient compounding is achieved by adjusting the volume ratio of the first dispersion and the second dispersion.
Further preferably, in the step (5), the drying is supercritical drying, preferably carbon dioxide supercritical drying.
The inventor finds that the tetraalkoxysilane can selectively react with silicon hydroxyl on the surface of the fiber under gas phase conditions, but not react with aluminum hydroxyl; the regulation of the macroscopic polarity of the fiber surface can be realized by regulating the silicon/aluminum ratio of the fiber surface; by regulating and controlling the polarity of the fiber surface, the adsorption and filtration effects of a fiber network on micron-sized anti-heat radiation particles in the process of compounding a dispersion liquid with a fiber reinforcement can be effectively avoided, the anti-radiation structure is favorably in a discretely distributed state in a composite material, and the influence of the introduction of an anti-radiation agent on solid-phase heat transfer is weakened; after the sol is compounded, the alkoxy carried on the surface of the fiber is gradually hydrolyzed under a catalytic environment, and the surface hydroxyl distribution is recovered, so that the surface of the fiber recovers good wettability with the sol, and the final interface stability of the composite material is not influenced; meanwhile, a gradient distribution heat radiation resistant structure matched with the normal temperature gradient is adopted, so that the utilization efficiency of the radiation resistant agent can be greatly improved, and the high-temperature heat insulation performance of the material is improved.
In some preferred embodiments, the invention can more effectively adjust the type and distribution gradient of the radiation resistant agent of the heat insulating material by adjusting the surface activation procedure, the type of the fiber, the type or the addition amount of the catalyst and the type or the addition amount of the radiation resistant agent, thereby ensuring good stability and overall formability of the material and having excellent high-temperature heat insulating performance.
In some more specific embodiments, the method comprises the steps of:
(1) surface treatment
Mixing commercially available silica sol and alumina hydrosol with a solid content of 20% according to a silica/alumina mass ratio of 0: 1-1: 0 (such as 0:1, 1:5, 1:10, 1:100, 1:1000, 1:10000, 1:0), diluting with deionized water to obtain a sol solution with a solid content of 5% -10% (5%, 6%, 7%, 8%, 9%, 10%), impregnating and drying the reinforcement fiber, and then using a molecular formula of Si (OR)4The silane coupling agent performs polarity regulation and control treatment on the surface of the fiber under the conditions of vacuum and heating. In the present invention, a group consisting of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, and tetraisopropoxysilane is exemplified, but not limited thereto. The heating temperature is 60-150 deg.C (such as 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, 100 deg.C, 150 deg.C), and the gas phase treatment time is 6-12 h (such as 6h, 7h, 8h, 9h, 10h, 11h, 12 h).
(2) Preparing a precursor dispersion liquid: adding an anti-radiation agent (such as 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 10 μm, the type of the anti-radiation agent is a group consisting of rutile titanium dioxide, boron nitride, silicon carbide and ferroferric oxide) with the particle size of 1-10 μm into oxide sol with the solid content of 5-40% which is commercially available or prepared by a method well known by a person skilled in the art, wherein the dosage of the anti-radiation agent accounts for 5-50% (such as 5%, 10%, 15%, 20%, 30%, 40%, 50%) of the mass of the sol, and polyethylene glycol (such as 400, 600, 800, 1000) with the molecular weight of 400-1000, and the dosage of the polyethylene glycol accounts for 0.1-1% (such as 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 1%) of the mass of the anti-radiation agent; the pH value of the system is controlled to be 5-9 (such as 5, 6, 7, 8 and 9) by concentrated hydrochloric acid or ammonia water, and the system is stirred and dispersed for 15-30 min under the stirring of 3000-4000 r/min, so that different stable dispersion systems are obtained.
(3) Gradient compounding: slowly adding 0.5-20% by mass of ammonia water or ammonium fluoride aqueous solution (such as 0.5%, 5%, 10%, 15%, 20%) serving as a catalyst into the different dispersion systems obtained in the step (2) under stirring, wherein the amount of the catalyst accounts for 0.5-5% (0.5%, 1%, 1.5%, 2%, 3%, 4%, 5%) of the total mass of the sol, and fully stirring and mixing. Adding a precursor with low content of the anti-radiation agent into a system with high content at a certain flow rate, quickly stirring to fully and uniformly mix the system, injecting glue into a mould filled with the reinforced fibers in the step (1) at a certain flow rate in the stirring process until the mould is completely filled with the reinforced fibers, pressurizing to remove gas, standing for gelation, and completing the construction of an anti-radiation gradient structure, wherein the gradient distribution condition of the anti-radiation agent is regulated and controlled by adopting the volume ratio and the glue injection flow rate among different dispersion systems.
(4) Aging: aging the composite material after the gelation in the step (3) at 80 ℃ for 1-3 days, improving the reaction degree, naturally cooling to room temperature, replacing the water in the system by using ethanol, and monitoring the water content to be less than or equal to 1%.
(5) And (3) drying: and (4) removing the ethanol solvent in the gel material in the step (4) in a drying mode to obtain the high-efficiency heat-insulating material with the gradient anti-radiation structure.
(6) Moisture-proof treatment: and (3) placing the heat insulating material obtained in the step (5) in a negative pressure heating environment, maintaining the temperature of the system at 80-150 ℃, and absorbing trimethyl methoxy silane accounting for 5-20% of the mass fraction of the heat insulating material into the system to carry out damp-proof treatment on the material to obtain the final heat insulating material.
The present invention provides, in a second aspect, a thermal insulation material produced by the production method according to the first aspect of the present invention.
The heat insulating material of the invention comprises a high-efficiency radiation-resistant structure which is composed of micron-sized heat radiation-resistant particles which are uniformly and discretely distributed in the surface and are discretely distributed in a normal gradient manner.
The heat insulating material of the invention has the following characteristics: (1) the anti-radiation particles form a structure with uniform and discrete distribution in the surface and normal gradient and discrete distribution in the heat-insulating material matrix, the material integrity is excellent, and the dosage of the anti-radiation agent is reduced by about 50 percent under the same anti-radiation efficiency; (2) the polarity of the surface of the fiber can be regulated, different types of fibers and the anti-radiation agent can be matched at will, and the problem of agglomeration is avoided. (3) The surface polarity of the reinforcement fiber is adjustable, and the enrichment and filtration effects of a fiber network on the anti-radiation agent in the composite process can be greatly weakened, so that an anti-radiation structure with uniformly dispersed interior is obtained, and different types of fibers and anti-radiation agents have good compatibility; (4) the radiation-resistant structures uniformly distributed in the horizontal direction keep continuously adjustable gradient distribution in the thickness direction, and the introduction of the gradient structures can maximize the radiation-resistant efficiency of a radiation-resistant system; (5) the anti-radiation agent is distributed discretely in the member, the room temperature thermal conductivity of the material is not obviously changed, and the high temperature thermal conductivity is reduced by more than 40 percent; (6) the thermal stability of the material is obviously improved, and the linear shrinkage rate of the material is reduced by 200% under typical sample and typical examination conditions. (7) The integrated forming property is good, the structure is stable, no obvious interlayer structure exists, and the interface mismatching phenomena such as layering and bulging do not occur under the environment of multiple/long-term use.
The present invention provides, in a third aspect, an insulation member comprising the insulation material of the second aspect of the present invention.
Therefore, the invention provides a more efficient gradient anti-heat radiation structure, and provides a preparation method and application of an integrated heat-insulating material with the gradient anti-radiation structure.
Examples
The present invention is described in detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a commercially available quartz fibrofelt block with the room temperature thermal conductivity of 0.03W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 10% prepared according to the mass ratio of 1:1 of silica to alumina into the container, immersing the fibrofelt for 5-10 minutes, taking out the fibrofelt, drying the fibrofelt, performing heat treatment for 100-1 h/200-1 h/300-1 h, and putting the fibrofelt into a mold shown in the figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Rutile titanium dioxide with the particle size of 4 mu m is added into silicon dioxide hydrosol with the solid content of 20 percent on the market, the dosage is respectively 5 percent and 50 percent of the mass of the sol, and the solution A and the solution B are correspondingly formed. Polyethylene glycol with molecular weight of 1000 is added into the solution A and the solution B respectively, and the dosage is 0.1 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be about 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
A, B adding 5 wt% ammonium fluoride solution into the two systems, the amount of which is 5 wt% of the total sol, pumping 3L of solution A into 6L of solution B by using the device shown in figure 1 at a speed of 0.1L/min, rapidly stirring at a speed of 1000 r/min, pumping the mixed solution into a mould at a flow rate of 0.3L/min until the mixed solution is filled, pressurizing to remove bubbles, and subjecting the systems to gelation, aging, solvent replacement, supercritical drying and damp-proof treatment to obtain the high-performance heat-insulating material. The density of the material is 0.37g/cm3The thermal conductivity at room temperature is less than 0.025W/(mK), and the thermal conductivity at 1000 ℃ is less than 0.06W/(mK).
Example 2
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a commercially available quartz fibrofelt block with the room temperature thermal conductivity of 0.03W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 10% prepared according to the mass ratio of 1:2 of silica to alumina into the container, immersing the fibrofelt for 5-10 minutes, taking out the fibrofelt, drying the fibrofelt, performing heat treatment for 100-1 h/200-1 h/300-1 h, and putting the fibrofelt into a mold shown in the figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Adding silicon carbide with the particle size of 4 mu m into silicon dioxide hydrosol with the solid content of 20 percent sold in the market, wherein the dosage is respectively 5 percent and 40 percent of the mass of the sol, and correspondingly forming solution A and solution B. Polyethylene glycol with molecular weight of 1000 is added into the solution A and the solution B respectively, and the dosage is 0.1 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be about 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
Adding 5 mass percent of ammonium fluoride solution into A, B two systems, wherein the amount of the ammonium fluoride solution is the amount of the ammonium fluoride solution5% of the total mass of the glue, adopting a device shown in figure 1, pumping 3 liters of the A liquid into 6 liters of the B liquid at a speed of 0.1L/min, rapidly stirring at a speed of 1000 revolutions/min, pumping the mixed liquid into a mold at a flow rate of 0.3L/min until the mixed liquid is filled, pressurizing to remove bubbles, and subjecting the system to gelation, aging, solvent replacement, supercritical drying and moisture-proof treatment to obtain the high-performance heat-insulating material. The density of the material is 0.35g/cm3The thermal conductivity at room temperature is less than 0.024W/(m.K), and the thermal conductivity at 1000 ℃ is less than 0.055W/(m.K).
Example 3
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a piece of commercially available mullite fiber felt with the room temperature thermal conductivity of 0.032W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 10% prepared according to the mass ratio of 1:2 of silica to alumina into the container, immersing the fiber felt, keeping for 5-10 minutes, taking out the fiber felt, airing, carrying out heat treatment for 100-1 h/200-1 h/300-1 h, and then putting into a mold shown in the figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Rutile titanium dioxide with the particle size of 3 mu m is added into silicon dioxide hydrosol with the solid content of 20 percent on the market, the dosage is respectively 5 percent and 50 percent of the mass of the sol, and the solution A and the solution B are correspondingly formed. Polyethylene glycol with the molecular weight of 800 is respectively added into the solution A and the solution B, and the dosage is 0.1 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be about 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
A, B adding 5 wt% ammonium fluoride solution into the two systems, the amount of which is 5 wt% of the total sol, pumping 3L of solution A into 6L of solution B by using the device shown in figure 1 at a speed of 0.1L/min, rapidly stirring at a speed of 1000 r/min, pumping the mixed solution into a mould at a flow rate of 0.3L/min until the mixed solution is filled, pressurizing to remove bubbles, and subjecting the systems to gelation, aging, solvent replacement, supercritical drying and damp-proof treatment to obtain the high-performance heat-insulating material. The density of the material is 0.35g/cm3The thermal conductivity at room temperature is less than 0.025W/(mK), and the thermal conductivity at 1000 ℃ is less than 0.06W/(mK).
Example 4
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a commercially available quartz fibrofelt block with the room temperature thermal conductivity of 0.032W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 10% prepared according to the mass ratio of 1:1 of silica to alumina into the container, immersing the fibrofelt, keeping for 5-10 minutes, taking out the fibrofelt, airing, carrying out heat treatment for 100-1 h/200-1 h/300-1 h, and then putting into a mold shown in the figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Rutile titanium dioxide with the particle size of 3 mu m is added into silicon dioxide hydrosol with the solid content of 20 percent on the market, the dosage is respectively 5 percent and 50 percent of the mass of the sol, and the solution A and the solution B are correspondingly formed. Polyethylene glycol with molecular weight of 1000 is added into the solution A and the solution B respectively, and the dosage is 0.1 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be about 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
A, B adding 5 wt% ammonium fluoride solution into the two systems, the amount of which is 5 wt% of the total sol, pumping 6L of solution A into 3L of solution B by using the device shown in figure 1 at a speed of 0.2L/min, rapidly stirring at a speed of 1000 r/min, pumping the mixed solution into a mould at a flow rate of 0.3L/min until the mixed solution is filled, pressurizing to remove bubbles, and subjecting the systems to gelation, aging, solvent replacement, supercritical drying and damp-proof treatment to obtain the high-performance heat-insulating material. The density of the material is 0.34g/cm3The room temperature thermal conductivity is less than 0.022W/(mK), and the 1000 ℃ thermal conductivity is less than 0.065W/(mK).
Example 5
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a piece of commercially available mullite fiber felt with the room temperature thermal conductivity of 0.032W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 10% prepared according to the mass ratio of 1:2 of silica to alumina into the container, immersing the fiber felt, keeping for 5-10 minutes, taking out the fiber felt, airing, carrying out heat treatment for 100-1 h/200-1 h/300-1 h, and then putting into a mold shown in the figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Rutile titanium dioxide with the particle size of 3 mu m is added into silicon dioxide hydrosol with the solid content of 20 percent on the market, the dosage is respectively 50 percent and 50 percent of the mass of the sol, and the solution A and the solution B are correspondingly formed. Polyethylene glycol with the molecular weight of 800 is respectively added into the solution A and the solution B, and the dosage is 0.1 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be about 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
A, B adding 5 wt% ammonium fluoride solution into the two systems, the amount of which is 5 wt% of the total sol, pumping 3L of solution A into 6L of solution B by using the device shown in figure 1 at a speed of 0.1L/min, rapidly stirring at a speed of 1000 r/min, pumping the mixed solution into a mould at a flow rate of 0.3L/min until the mixed solution is filled, pressurizing to remove bubbles, and subjecting the systems to gelation, aging, solvent replacement, supercritical drying and damp-proof treatment to obtain the high-performance heat-insulating material. The density of the material is 0.4g/cm3The thermal conductivity at room temperature is less than 0.028W/(m.K), and the thermal conductivity at 1000 ℃ is less than 0.07W/(m.K).
Example 6
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a piece of commercially available mullite fiber felt with the room temperature thermal conductivity of 0.032W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 10% prepared according to the mass ratio of 1:2 of silica to alumina into the container, immersing the fiber felt, keeping for 5-10 minutes, taking out the fiber felt, airing, carrying out heat treatment for 100-1 h/200-1 h/300-1 h, and then putting into a mold shown in the figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Rutile titanium dioxide with the particle size of 3 mu m is added into silicon dioxide hydrosol with the solid content of 20 percent on the market, the dosage is respectively 100 percent and 100 percent of the mass of the sol, and the solution A and the solution B are correspondingly formed. Polyethylene glycol with the molecular weight of 800 is respectively added into the solution A and the solution B, and the dosage is 0.1 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be about 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
A, B adding 5 wt% ammonium fluoride solution into the two systems, the amount of which is 5 wt% of the total sol, pumping 3L of solution A into 6L of solution B by using the device shown in figure 1 at a speed of 0.1L/min, rapidly stirring at a speed of 1000 r/min, pumping the mixed solution into a mould at a flow rate of 0.3L/min until the mixed solution is filled, pressurizing to remove bubbles, and subjecting the systems to gelation, aging, solvent replacement, supercritical drying and damp-proof treatment to obtain the high-performance heat-insulating material. The density of the material is 0.5g/cm3The thermal conductivity at room temperature is less than 0.029W/(mK), and the thermal conductivity at 1000 ℃ is less than 0.08W/(mK).
Example 7
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a piece of commercially available mullite fiber felt with the room temperature thermal conductivity of 0.032W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 10% prepared according to the mass ratio of 1:2 of silica to alumina into the container, immersing the fiber felt, keeping for 5-10 minutes, taking out the fiber felt, airing, carrying out heat treatment for 100-1 h/200-1 h/300-1 h, and then putting into a mold shown in the figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Rutile titanium dioxide with the particle size of 3 mu m is added into silicon dioxide hydrosol with the solid content of 20 percent sold in the market, the dosage is 0 percent and 0 percent of the mass of the sol respectively, and the solution A and the solution B are correspondingly formed. Polyethylene glycol with the molecular weight of 800 is respectively added into the solution A and the solution B, and the dosage is 0.1 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be about 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
A, B adding 5 wt% ammonium fluoride solution into the two systems, the amount of which is 5 wt% of the total sol, pumping 3L of solution A into 6L of solution B by using the device shown in figure 1 at a speed of 0.1L/min, rapidly stirring at a speed of 1000 r/min, pumping the mixed solution into a mould at a flow rate of 0.3L/min until the mixed solution is filled, pressurizing to remove bubbles, and subjecting the systems to gelation, aging, solvent replacement, supercritical drying and damp-proof treatment to obtain the high-performance heat-insulating material. The density of the material is 0.3g/cm3Room temperature thermal conductivity < 0.022W/((R))m.K), and the thermal conductivity at 1000 ℃ is less than 0.09W/(m.K).
Example 10
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3And placing a commercial mullite fiber felt with the room temperature thermal conductivity of 0.032W/(m.K) into a container, keeping for 5-10 minutes, taking out the fiber felt, carrying out heat treatment for 100-1 h/200-1 h/300-1 h, and then placing into a mold shown in the figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Rutile titanium dioxide with the particle size of 3 mu m is added into silicon dioxide hydrosol with the solid content of 20 percent sold in the market, the dosage is 0 percent and 0 percent of the mass of the sol respectively, and the solution A and the solution B are correspondingly formed. Polyethylene glycol with the molecular weight of 800 is respectively added into the solution A and the solution B, and the dosage is 0 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be about 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
A, B adding 5 wt% ammonium fluoride solution into the two systems, the amount of which is 5 wt% of the total sol, pumping 3L of solution A into 6L of solution B by using the device shown in figure 1 at a speed of 0.1L/min, rapidly stirring at a speed of 1000 r/min, pumping the mixed solution into a mould at a flow rate of 0.3L/min until the mixed solution is filled, pressurizing to remove bubbles, and subjecting the systems to gelation, aging, solvent replacement, supercritical drying and damp-proof treatment to obtain the high-performance heat-insulating material. The density of the material is 0.3g/cm3The room temperature thermal conductivity is less than 0.022W/(mK), and the 1000 ℃ thermal conductivity is less than 0.09W/(mK).
Example 11
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a piece of commercially available quartz fibrofelt with the room temperature thermal conductivity of 0.03W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 0% prepared according to the mass ratio of 1:3 into the container, immersing the fibrofelt for 5-10 minutes, taking out the fibrofelt, drying the fibrofelt, performing heat treatment for 100-1 h/200-1 h/300-1 h, and putting the fibrofelt into a mold shown in figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Adding boron nitride with the particle size of 3 mu m into commercially available silicon dioxide hydrosol with the solid content of 20 percent, wherein the dosage is respectively 5 percent and 50 percent of the mass of the sol, and correspondingly forming solution A and solution B. Polyethylene glycol with the molecular weight of 800 is respectively added into the solution A and the solution B, and the dosage is 0.1 percent of the mass of boron nitride. The pH value of the system is controlled to be about 8 by dropwise adding concentrated ammonia water, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min, so that two different stable dispersion systems A and B are obtained.
Adding ammonia water with the mass fraction of 5% into A, B two systems, wherein the amount of ammonia water accounts for 5% of the total mass of the sol, pumping 4.5 liters of A liquid into 4.5 liters of B liquid at the speed of 0.1L/min by adopting a device shown in figure 1, rapidly stirring at the speed of 1000 r/min, pumping the mixed liquid into a mold at the flow rate of 0.2L/min until the mixed liquid is filled, pressurizing to remove bubbles, and carrying out gelation, aging, solvent replacement, supercritical drying and moisture-proof treatment on the systems to obtain the high-performance heat-insulating material. The density of the material is 0.35g/cm3The thermal conductivity at room temperature is less than 0.03W/(mK), and the thermal conductivity at 1000 ℃ is less than 0.1W/(mK).
Example 12
Taking the sample with the size of 500mm multiplied by 25mm and the density of 0.1g/cm3Putting a piece of commercially available quartz fibrofelt with the room temperature thermal conductivity of 0.032W/(m.K) into a container, adding a silica/alumina sol solution with the mass fraction of 10% prepared according to the mass ratio of 1:1 into the container, immersing the fibrofelt, keeping for 5-10 minutes, taking out the fibrofelt, drying in the air, performing heat treatment for 100-1 h/200-1 h/300-1 h, and then putting into a mold shown in figure 1, wherein the size of the mold is 550mm multiplied by 30 mm.
Rutile titanium dioxide with the particle size of 3 mu m is added into silicon dioxide hydrosol with the solid content of 20 percent on the market, the dosage is respectively 5 percent and 50 percent of the mass of the sol, and the solution A and the solution B are correspondingly formed. Polyethylene glycol with the molecular weight of 1000 is respectively added into the solution A and the solution B, and the dosage is 0 percent of the mass of the rutile titanium dioxide. The pH value of the system is controlled to be less than 6 by dropwise adding concentrated hydrochloric acid, and the two systems are stirred and dispersed for 15min under the stirring of 3000 r/min to obtain two different dispersion systems A and B, but the rapid sedimentation condition occurs in both the two systems A, B.
Adding 5 mass percent of ammonium fluoride solution into A, B two systems, wherein the use amount of the ammonium fluoride solution accounts for 5 percent of the total mass of the sol, and adoptingIn the apparatus shown in FIG. 1, 6L of solution A is pumped into 3L of solution B at a speed of 0.2L/min, and rapidly stirred at a speed of 1000 r/min, and the mixed solution is pumped into a mold at a flow rate of 0.3L/min until the mold is filled, then pressurized to remove air bubbles, and the system is subjected to gelation, aging, solvent displacement, supercritical drying and moisture-proof treatment to obtain the heat-insulating material. The density of the material is 0.34g/cm3The thermal conductivity at room temperature is less than 0.03W/(mK), and the thermal conductivity at 1000 ℃ is less than 0.08W/(mK).
Finally, it should be noted that: the present invention is not described in detail and is known to those skilled in the art, and the above embodiments are only used for illustrating the technical solution of the present invention and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing a thermal insulation material comprising a graded distribution of radiation resistant agent, the method comprising the steps of:
(1) surface treatment: adjusting the surface group reactivity of a fiber reinforcement by using a composite sol containing silicon dioxide and aluminum oxide, and then adjusting the fiber surface polarity of the fiber reinforcement by using a silane coupling agent;
(2) preparing a precursor dispersion liquid: dispersing an anti-radiation agent into a silica sol precursor to obtain a first dispersion liquid with a first anti-radiation agent concentration and a second dispersion liquid with a second anti-radiation agent concentration, wherein the first anti-radiation agent concentration is lower than the second anti-radiation agent concentration; then adding a surfactant to each of the first dispersion liquid and the second dispersion liquid and uniformly stirring;
(3) gradient compounding: adding a catalyst into the first dispersion liquid and the second dispersion liquid prepared in the step (2) and uniformly mixing; then adding the first dispersion liquid from the first container into a second container containing the second dispersion liquid at a first flow rate and stirring to form a mixed dispersion liquid, and injecting the mixed dispersion liquid into a mold containing the fiber reinforcement prepared in the step (1) at a second flow rate during the stirring and allowing the mixed dispersion liquid to gel to prepare a gel composite;
(4) aging: aging the gel composite to obtain an aged composite;
(5) and (3) drying: and drying the aged composite material to obtain the heat-insulating material.
2. The method of manufacturing according to claim 1, further comprising the steps of:
(6) moisture-proof treatment: and carrying out moisture-proof treatment on the heat-insulating material by using a hydrophobic treatment agent, preferably, the hydrophobic treatment agent is trimethyl methoxy silane, and more preferably, the moisture-proof treatment is carried out by means of gas phase treatment.
3. The production method according to claim 1 or 2, characterized in that:
in the step (1), the fiber reinforcement is impregnated by the composite sol, then dried, and then the gas phase reaction treatment is carried out on the fiber surface of the fiber reinforcement by the silane coupling agent under the condition of vacuum heating;
in the step (2), the radiation-resistant agent is a granular material having a particle size of 1 to 10 μm, and it is further preferable that the first dispersion and the second dispersion are each independently adjusted to a pH of 5 to 9 before the surfactant is added;
in the step (3), the mixed dispersion liquid is injected until the mould is completely filled, then the mould is pressed to degas, and the gel is kept still;
in the step (4), the aging is carried out at a temperature of 70 ℃ to 90 ℃, for example, 80 ℃, and the aging time is 12-24 hours; and/or
In step (5), the drying is carried out until the solvent in the aged composite material is completely removed.
4. The production method according to claim 1, wherein in step (1):
the composite sol is obtained by mixing 5-20% by mass of silica sol and 5-20% by mass of alumina sol, preferably, the mass ratio of silica to alumina in the composite sol is 0: 1-1: 0, more preferably, the solid content of the composite sol is 1-20% by mass, and in addition, preferably, the solvent of the composite sol is selected from the group consisting of alcohol solvent with the boiling point of less than 120 ℃ and water, more preferably, water;
the fiber used by the fiber reinforcement body is a high-temperature-resistant oxide fiber, preferably selected from the group consisting of basalt fiber, quartz fiber, mullite fiber, alumina fiber and zirconia fiber; and/or
The silane coupling agent has a molecular formula of Si (OR)4Wherein R is a non-aromatic carbon chain substituent having 1 to 10 carbons; the dosage of the silane coupling agent is 1-20% of the mass of the fiber reinforcement (originally, the heat insulation material), the heating temperature is 80-200 ℃, and the treatment time of the gas phase reaction treatment is 6-12 hours.
5. The production method according to claim 1, wherein in step (2):
the anti-radiation agent is selected from the group consisting of rutile titanium dioxide, boron nitride, silicon carbide and ferroferric oxide;
preferably, the dosage of the anti-radiation agent is 5-200% of the mass of the silica sol precursor;
more preferably, the surfactant is polyethylene glycol with the molecular weight of 400-1000, and the dosage of the surfactant is 0.1-1% of the mass of the anti-radiation agent.
6. The production method according to claim 1, wherein in step (2):
the first concentration of the radiation resistant agent is 1% to 90% of the second concentration of the radiation resistant agent.
7. The production method according to claim 1, wherein in step (3):
the catalyst is ammonia water or ammonium fluoride aqueous solution with the concentration of 0.1 to 20 mass percent;
preferably, the amount of the catalyst is 0.5-5% of the mass of the dispersion, or the amount of the catalyst is an amount required for controlling the difference of the gel time of the first dispersion and the gel time of the second dispersion to be 0.5-1 h;
it is also preferred that the gradient compounding is achieved by adjusting the volume ratio of the first dispersion and the second dispersion.
8. The production method according to claim 1, wherein in step (5):
the drying is supercritical drying, preferably carbon dioxide supercritical drying.
9. An insulating material, characterized in that it is produced by the production method according to any one of claims 1 to 8.
10. An insulating member, characterized in that it comprises the insulating material according to claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911314140.5A CN111018473B (en) | 2019-12-19 | 2019-12-19 | Heat insulation material containing gradient-distributed anti-radiation agent and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911314140.5A CN111018473B (en) | 2019-12-19 | 2019-12-19 | Heat insulation material containing gradient-distributed anti-radiation agent and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111018473A true CN111018473A (en) | 2020-04-17 |
| CN111018473B CN111018473B (en) | 2022-01-28 |
Family
ID=70210681
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911314140.5A Active CN111018473B (en) | 2019-12-19 | 2019-12-19 | Heat insulation material containing gradient-distributed anti-radiation agent and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111018473B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943654A (en) * | 2020-08-18 | 2020-11-17 | 航天特种材料及工艺技术研究所 | High-temperature-resistant and radiation-resistant aerogel composite material and preparation method thereof |
| CN112522852A (en) * | 2020-12-02 | 2021-03-19 | 航天特种材料及工艺技术研究所 | Heat insulation material with controllable structure and preparation method thereof |
| CN116730743A (en) * | 2023-07-03 | 2023-09-12 | 航天特种材料及工艺技术研究所 | Hydrophobic silicon dioxide ceramic composite material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006272660A (en) * | 2005-03-28 | 2006-10-12 | Hiraoka & Co Ltd | Antifouling, nonflammable flexible film material |
| CN103449825A (en) * | 2013-08-19 | 2013-12-18 | 航天特种材料及工艺技术研究所 | Micro-ablation insulating material and preparation method thereof |
| CN107032736A (en) * | 2016-11-16 | 2017-08-11 | 航天特种材料及工艺技术研究所 | A kind of high temperature resistant radiation wave transparent heat-barrier material and preparation method thereof |
| CN109336545A (en) * | 2018-12-10 | 2019-02-15 | 航天特种材料及工艺技术研究所 | A kind of silicon dioxide silica aerogel composite material, preparation method and application |
-
2019
- 2019-12-19 CN CN201911314140.5A patent/CN111018473B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006272660A (en) * | 2005-03-28 | 2006-10-12 | Hiraoka & Co Ltd | Antifouling, nonflammable flexible film material |
| CN103449825A (en) * | 2013-08-19 | 2013-12-18 | 航天特种材料及工艺技术研究所 | Micro-ablation insulating material and preparation method thereof |
| CN107032736A (en) * | 2016-11-16 | 2017-08-11 | 航天特种材料及工艺技术研究所 | A kind of high temperature resistant radiation wave transparent heat-barrier material and preparation method thereof |
| CN109336545A (en) * | 2018-12-10 | 2019-02-15 | 航天特种材料及工艺技术研究所 | A kind of silicon dioxide silica aerogel composite material, preparation method and application |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943654A (en) * | 2020-08-18 | 2020-11-17 | 航天特种材料及工艺技术研究所 | High-temperature-resistant and radiation-resistant aerogel composite material and preparation method thereof |
| CN111943654B (en) * | 2020-08-18 | 2022-04-12 | 航天特种材料及工艺技术研究所 | High-temperature-resistant and radiation-resistant aerogel composite material and preparation method thereof |
| CN112522852A (en) * | 2020-12-02 | 2021-03-19 | 航天特种材料及工艺技术研究所 | Heat insulation material with controllable structure and preparation method thereof |
| CN112522852B (en) * | 2020-12-02 | 2022-05-03 | 航天特种材料及工艺技术研究所 | Heat insulation material with controllable structure and preparation method thereof |
| CN116730743A (en) * | 2023-07-03 | 2023-09-12 | 航天特种材料及工艺技术研究所 | Hydrophobic silicon dioxide ceramic composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111018473B (en) | 2022-01-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111018473B (en) | Heat insulation material containing gradient-distributed anti-radiation agent and preparation method and application thereof | |
| CN101698592B (en) | Silicon-aluminium aerogel composite material and manufacturing method thereof | |
| CN111925194B (en) | High-temperature-resistant high-performance aerogel composite material and preparation method thereof | |
| WO2018133260A1 (en) | Superhydrophobic silicon-aluminum-zirconium composite material and preparation method thereof | |
| CN110282958B (en) | High-temperature-resistant special-shaped nanocrystalline aerogel material and preparation method thereof | |
| CN101792299B (en) | Method for preparing heat-resisting alumina-silox aerogel thermal-protective composite material | |
| CN108636304B (en) | Method for preparing aerogel by supercritical drying method and device for supercritical drying | |
| CN104261798A (en) | High-temperature-resistant SiCOB aerogel heat-insulation composite material and preparation method thereof | |
| CN105536655A (en) | Rapid preparation method for aerogel material | |
| CN101445356A (en) | Nano-hole aerogel heat-insulating composite material and preparation method thereof | |
| CN108793943A (en) | The preparation method for the adjustable aerosil fibre of hydrophilic and hydrophobic that graphene oxide is modified | |
| CN104909729B (en) | Preparation method of lightweight rigid heat insulation material | |
| CN111943654B (en) | High-temperature-resistant and radiation-resistant aerogel composite material and preparation method thereof | |
| CN108116011B (en) | A kind of sandwich thermally protective materials and preparation method thereof of surface Jing Guo protective treatment | |
| CN105036143B (en) | Preparation method of nano silicon dioxide aerogel | |
| CN111848140B (en) | Alumina nanowire aerogel thermal insulation material and preparation method thereof | |
| CN109179428B (en) | Enhanced transparent silicon dioxide aerogel and preparation method thereof | |
| CN104355647B (en) | A kind of Cr2O3Doping silicon dioxide aerogel material and preparation method thereof | |
| CN109336545A (en) | A kind of silicon dioxide silica aerogel composite material, preparation method and application | |
| CN108249901A (en) | A kind of preparation method of high temperature resistant aeroge material | |
| CN114195543B (en) | Mullite whisker/anorthite/SiO 2 Aerogel porous ceramic, preparation method thereof and heat insulation tile | |
| CN113831103A (en) | Preparation method of high-temperature-resistant alumina-silica aerogel composite material | |
| CN110550950A (en) | Preparation process of high-temperature-resistant ceramic aerogel based on nanotechnology | |
| CN106854086A (en) | A kind of resistant to elevated temperatures mullite-type aerogel composite and preparation method thereof | |
| CN113831581A (en) | High-elasticity anti-radiation nanofiber aerogel 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 |