CN108502893A - A kind of preparation method of the elastic silica aerogel block materials with toughness - Google Patents
A kind of preparation method of the elastic silica aerogel block materials with toughness Download PDFInfo
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- CN108502893A CN108502893A CN201810566382.2A CN201810566382A CN108502893A CN 108502893 A CN108502893 A CN 108502893A CN 201810566382 A CN201810566382 A CN 201810566382A CN 108502893 A CN108502893 A CN 108502893A
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- block materials
- toughness
- gel
- elastic silica
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 230000032683 aging Effects 0.000 claims abstract description 12
- 238000009413 insulation Methods 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- 229910002012 Aerosil® Inorganic materials 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 238000007711 solidification Methods 0.000 claims abstract description 3
- 230000008023 solidification Effects 0.000 claims abstract description 3
- 239000003063 flame retardant Substances 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- -1 siloxanes Chemical class 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 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 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- 238000000352 supercritical drying Methods 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 4
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229920000388 Polyphosphate Polymers 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 150000007522 mineralic acids Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 239000001205 polyphosphate Substances 0.000 claims description 3
- 235000011176 polyphosphates Nutrition 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- TZYRSLHNPKPEFV-UHFFFAOYSA-N 2-ethyl-1-butanol Chemical compound CCC(CC)CO TZYRSLHNPKPEFV-UHFFFAOYSA-N 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 125000002029 aromatic hydrocarbon group Chemical group 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims 2
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims 1
- XDEZOLVDJWWXRG-UHFFFAOYSA-N methylenedioxycathinone Chemical compound CC(N)C(=O)C1=CC=C2OCOC2=C1 XDEZOLVDJWWXRG-UHFFFAOYSA-N 0.000 claims 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims 1
- MIBXHGZAARWAGI-UHFFFAOYSA-N phenylmethoxyphosphonoyloxymethylbenzene Chemical class C=1C=CC=CC=1COP(=O)OCC1=CC=CC=C1 MIBXHGZAARWAGI-UHFFFAOYSA-N 0.000 claims 1
- 150000003014 phosphoric acid esters Chemical class 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 230000003321 amplification Effects 0.000 abstract description 5
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 28
- 239000004964 aerogel Substances 0.000 description 18
- 239000000499 gel Substances 0.000 description 18
- 239000000047 product Substances 0.000 description 16
- 239000000843 powder Substances 0.000 description 7
- 239000002131 composite material Substances 0.000 description 4
- 229910052599 brucite Inorganic materials 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 229920006231 aramid fiber Polymers 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 230000010412 perfusion Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- SZWMYRXPLPUQQB-UHFFFAOYSA-N C(#N)NC(=O)N.N1=C(N)N=C(N)N=C1N Chemical compound C(#N)NC(=O)N.N1=C(N)N=C(N)N=C1N SZWMYRXPLPUQQB-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 229910000062 azane Inorganic materials 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl 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])C([H])([H])C([H])([H])* 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SLYCYWCVSGPDFR-UHFFFAOYSA-N octadecyltrimethoxysilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OC)(OC)OC SLYCYWCVSGPDFR-UHFFFAOYSA-N 0.000 description 1
- 125000000913 palmityl 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])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
- 239000002245 particle Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000010410 reperfusion Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of preparation methods of the elastic silica aerogel block materials with toughness, include the following steps：(1) preparation of silicon dioxide gel；(2) preparation of gel：The precursor solution for taking a certain amount of reaction to complete is added dropwise basic catalyst and adjusts pH value, quickly stirs certain time；(3) gel of preparation is slowly injected into mold；(4) a period of time is stood at a certain temperature, aging makes its gel solidification shape；(5) dry：The gel of gained is dried, hydrophobic type aerosil thermal insulation block materials are obtained.Present invention process is simple, cost is relatively low, reaction condition is controllable, excellent product performance, the elastic silica aerogel block materials of preparation have complete block structure, it can adapt to mold and prepare requirement, and very small and shrinkage rates are shunk to stablize, the appropriate amplification by controlling mold be fully able to meet profiled piece product in field of thermal insulation availability.
Description
Technical field
The present invention relates to a kind of elastic aerogel insulating material and preparation method thereof more particularly to a kind of bullets with toughness
The preparation method of property aerosil block materials.
Background technology
SiO2 aeroges are a kind of light nanoporous amorphous solid material that heat release heat-proof quality is very outstanding, hole
Rate is up to 80-99.8%, and the typical sizes of hole are 1-100nm, specific surface area 200-1000m2/g, and density is up to 3Kg/
M3, room temperature thermal coefficient can be down to 0.012W/（m·k）, make aerogel material in calorifics, acoustics, light just because of these features
There is very wide application potential in terms of, microelectronics, particle detection.But due to its specific surface area of SiO2 aeroges and hole
Rate is very big, and density is very low, causes its intensity very low, and intrinsic brittleness and poor mechanical performance greatly limit airsetting glue material
Expect the application in some fields.
The Chinese patent of Publication No. CN 101973752A provides a kind of glass fiber reinforcement aerosil
Composite material and preparation method.But the precursor material used in this method is more complicated, and need to carry out glass fibre
The drying condition of necessary pretreatment and normal temperature and pressure drying needs stringent control, and certain limitation is caused to actual production.
The Chinese patent of Publication No. CN 100386260C discloses a kind of brucite fiber enhancing aerosil
The preparation method of heat-barrier material.This method is to prepare raw material with industrial water glass or Ludox and natural brucite staple fiber.
But dispersion to brucite fiber and comparatively laborious to forming solvent displacement that gel is carried out and hydrophobic treatment process, one
Determine to limit practical application in degree.
The Chinese patent of Publication No. CN 101823867A provides a kind of silica airsetting of aramid fiber doping
The preparation method of glue composite material, but this method requires have good dispersion to aramid fiber, and surfactant is also added,
And it needs to carry out cumbersome solvent displacement before constant pressure and dry.
The application of modern aerosil is mainly reflected in the application in terms of insulation product, existing aerogel heat-insulating
Product is broadly divided into two kinds, the felt or film that composite base material is formed, silica-based aerogel powder.In actual application, different
Insulation of equipment have certain difference for the demand of insulation product.
1. felt class is suitable for pipeline and equipment, it is generally only applicable to the position of not interface, it is existing for there is the position of interface
General using using iron wire or the fixed method of adhesive tape after being cut into specific shape, the shortcomings that this method is that work progress is multiple
Miscellaneous and time-consuming and waste material, and the heat preservation construction of complex surface is cannot achieve, especially mini-plant can not apply airsetting
Glue Related product.
2. material with complex surface heat preservation, it is thus proposed that using the method for perfusion aerogel powder, but due to airsetting rubber powder
Volume density is very low, and pouring construction environment is poor, and the gap after perfusion between powder is bigger, has very big shadow to insulation capacity
It rings.If aerogel powder is made Reperfu- sion after slurry, the problem of can not carrying out redrying will be faced, and in slurry such as
Fruit does not contain base material, and the powder after drying is still highly brittle；Still an alternative is that such as by airsetting rubber powder and other materials
Concrete mixes, and then forms the thermal insulation concrete with certain heat-proof quality, however the thermal coefficient of this material still compares
It is higher, the excellent heat-proof quality of aeroge itself can not be embodied.
3. there is a kind of profiled piece insulating product, first base material is made the shape and size of needs, then with before aeroge
Bluk recombination is driven, then carries out aging, displacement, modification, drying and other steps.Base material makes the process as specific shape in this method
It is cumbersome, in addition lower production efficiency when using the equipment production profiled piece of traditional felt class product, causes product cost non-
Chang Gao.
Invention content
In view of the problems of the existing technology, the purpose of the present invention is to provide a kind of elastic dioxies with toughness
The preparation method of SiClx aerogel block body material, present invention process is simple, cost is relatively low, reaction condition is controllable, properties of product are excellent
Different, the elastic silica aerogel block materials of preparation have complete block structure, can adapt to mold and prepare and receive
Contracting is very small and shrinkage rates are stablized, and the appropriate amplification by controlling mold is fully able to meet leading in heat preservation for profiled piece product
Domain availability；
In order to achieve the above objectives, the present invention is achieved by the following technical solutions：
A kind of preparation method of the elastic silica aerogel block materials with toughness, it is characterised in that including following step
Suddenly：
（1）The preparation of silicon dioxide gel：
Using siloxanes as presoma, a variety of siloxanes are mixed evenly, organic solvent, water is added, stirs evenly, are maintained
Stirring, then acidic catalyst is added dropwise and adjusts solution pH value to 1~7, preferably 1~5；It is mixed again by every 1L silicon dioxide gels
Miscellaneous 1g~100g fire retardants are added in solution, continue to be dispersed with stirring uniformly；At 0 DEG C~70 DEG C, constant temperature 6 hours or more, preferably
It it is 30~70 DEG C, constant temperature 8 hours or more obtains clear silicon dioxide gel；Siloxanes in presoma, organic solvent, water
Molar ratio is 1:3~80:2~40, preferably 1:5~70:2~30.Pass through the molar ratio to siloxanes, organic solvent, water
Optimization, can adjust porosity, specific surface area, density and the content of organics of aeroge, obtain performance more preferably silica
Aeroge.By the optimization to silicon dioxide gel preparation condition, it can make that colloidal sol obtained is more uniform, organic group distribution
Evenly, make intensity and the hydrophobicity of the aerogel composite of preparation more excellent；By adjusting the ratio of fire retardant, can make
Prepared aerogel block body has better flame resistance, to meet different application scenarios.
（2）The preparation of gel：The precursor solution for taking a certain amount of reaction to complete is added dropwise basic catalyst and adjusts pH
Value quickly stirs certain time to 6~7；
（3）By step（2）The gel of preparation is slowly injected into mold；
（4）By step（3）The gel of middle preparation stands a period of time at a certain temperature, and aging makes its gel solidification shape；
（5）It is dry：The gel of gained is dried, hydrophobic type aerosil thermal insulation block materials are obtained.
Further, above-mentioned steps（1）In siloxanes be Si（OR1）4With R2Si（OR3）3、R4 2Si（OR5）2In one kind
Or several mixtures, the R1、R2、R3、R4、R5For identical or different alkane, alkene, aromatic hydrocarbon group, preferably Si（OR1）
4 and R2Si（OR3）3、R32Si（OR4）One or both of 2 mixture；Si（OR1）4 with the siloxanes containing hydrophobic grouping
Molar ratio be 1:0.1~15, preferably 1:0.2~10, by the optimization of each component molar ratio in being mixed to siloxane precursors,
The structure that aerosil can be improved enhances its mechanical performance, controls the content of the organic group in aeroge.
Further, above-mentioned steps（1）In organic solvent be methanol, ethyl alcohol, ethylene glycol, propyl alcohol, n-butanol, isobutyl
One or more of mixtures of alcohol, n-amyl alcohol, isoamyl alcohol, n-hexyl alcohol, isohexyl alcohol or acetone.
Further, above-mentioned steps（1）In catalyst be acidic catalyst, the acidic catalyst is inorganic acid or to have
Machine acid；The inorganic acid is HCl, H2SO4、H3PO4、H2CO3、HF、HBr、HNO3、H2SO3Or HClO4One or more of mixing
Object, the organic acid are CH3COOH、HOOC-COOH、HOOCC2H4COOH or C6H5One or more of mixtures of COOH.
Further, above-mentioned steps（1）In fire retardant be organic halogen-free environment-friendlyflame flame retardant；Organic halogen-free environmental
Fire retardant is polyphosphate, melamine, three (1- oxo -1- phosphas -2,6,7- trioxa-l-phosphabicyclos [2,2,2] octane -4- methylenes
Base) phosphate, N, N- p-phenylenediamine bases（2- hydroxyls）Dibenzyl phosphonic acids tetra-ethyl ester, melamine phosphate or melamine cyanurea
The one or more of acid and the mixing flame retardant products based on listed material.
Further, above-mentioned steps（2）In basic catalyst be sodium bicarbonate solution, sodium hydroxide solution, ammonium hydroxide, silicon
One or more of azane.
Further, above-mentioned steps（4）In dwell temperature be 20~80 DEG C, preferably 30~80 DEG C；Time of repose is
0.2~24 hour, preferably 0.1~6 hour；The temperature of aging be 30~90 DEG C, preferably 30~80 DEG C, ageing time 0
~48 hours, preferably 1~12 hour.
Further, above-mentioned steps（5）The method of middle drying is supercritical drying, constant pressure and dry, subcritical drying, vacuum
One or more of dry or freeze-drying；The supercritical drying, subcritical drying medium be carbon dioxide, methanol,
One kind in ethyl alcohol, normal propyl alcohol, isopropanol, butanol, acetone or acetonitrile；The constant pressure and dry temperature is 20~200 DEG C, and the time is
0.1~120h, preferably drying temperature be 40~200 DEG C, preferably drying time be 0.5~for 24 hours.
A kind of preparation method of the elastic silica aerogel block materials with toughness of the present invention, drives body process before the reaction
In, introduce the siloxanes containing hydrophobic group, and the dredging in control system by controlling reactant content and reaction condition
Surface hydrophobicity group is greatly decreased under conditions of ensureing hydrophobic in the content and distribution of water group；It is adulterated in sol phase
Enter fire retardant, the flame retardant property of aerosil block materials can be substantially improved；The gel prepared is injected into mold
Aging sizing is carried out, it is possible to prevente effectively from due to the improper problem of ratio caused by contraction during traditional dies use, and
Can be met by controlling the appropriate amplification of mold profiled piece product in field of thermal insulation availability.
The present invention has the advantages that compared with traditional handicraft：
1. the present invention has the preparation method of the elastic silica aerogel block materials of toughness, body process is driven before the reaction
In, the long-chain siloxanes containing hydrophobic grouping is introduced, and by controlling reactant content and reaction condition in control system
Hydrophobic group content and distribution aerogel products form is extended so as to improve the brittleness in existing aerogel products
For block, and can guarantee whole hydrophobic；
2. fire retardant is added in the sol-hydrolysis stage, the elastic silica aerogel block materials with toughness are substantially improved
Flame retardant property, and can guarantee the uniform dispersion of fire retardant, ensure the homogeneity of product, makes the elastic dioxy obtained with toughness
SiClx aerogel block body material has complete mass ends, can adapt to mold preparation, it is steady to shrink very small and shrinkage rates
Fixed, the appropriate amplification by controlling mold is fully able to meet the availability of profiled piece product；
3. the elastic silica aerogel block materials produced by the present invention with toughness are with hydrophobic surface group, whole
It is hydrophobic, hydrophobic performance is excellent, phenomena such as not will produce the moisture absorption during storage and use；The toughness that material itself has, to
Realize the rodability of aerogel block body material.
4. the present invention is carried out during preparing the elastic silica aerogel block materials with toughness using mold
Aging is shaped, it is possible to prevente effectively from due to the improper problem of ratio caused by contraction during traditional dies use, and can be with
Appropriate amplification by controlling mold meet profiled piece product in field of thermal insulation availability.
Specific implementation mode
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
The raw material that the present invention uses can be made by means commonly known in the art, can also use commercial product.
Embodiment 1
By methyl orthosilicate, cetyl base trimethoxy silane with molar ratio 1：1 ratio is mixed evenly, then this is mixed
Object is closed with methanol, water with molar ratio 2：10：3 ratio, which is sufficiently mixed, to stir evenly, with the H of 2mol/L2SO4Solution is slowly dropped into
In uniformly mixed solution, side stirring, which becomes, to be added dropwise, and adjusts solution ph to 3,5g poly phosphorus is adulterated by per 1L silicon dioxide gels
Fire retardant is added in solution the ratio of sour ammonium；Prepared solution is persistently stirred to 5 hours obtained presomas at 40 DEG C again
Solution.Quantitative precursor solution is taken, is sufficiently mixed and stirs evenly, then solution is adjusted into pH value to 6 with hexamethyldisilazane,
It adds, is poured into mold that is preprepared, cleaning up and dry while stirring.Then mold is placed in 40 DEG C of water-baths
In, form silica dioxide gel after 2 hours.Change into aging 12 hours in 60 DEG C of water-baths.Mold is taken out, then is removed from the molds
Airsetting blob of viscose, by constant pressure and dry, 120 degrees Celsius, 3 hours obtain hydrophobic type aerogel block body material.It is obtained hydrophobic
Type aerogel block body material has elasticity, and resilience is fine, can bear certain pressure intensity, and hydrophobicity is good, thermal coefficient
0.022w/（m•k）.
Embodiment 2
By ethyl orthosilicate, dodecyl base trimethoxy silane with molar ratio 1：2 ratio is mixed evenly, then this is mixed
Object is closed with ethyl alcohol, water with molar ratio 3：20：4 ratio, which is sufficiently mixed, to stir evenly, and is slowly dropped into the HCl solution of 2mol/L mixed
It closes in uniform solution, side stirring, which becomes, to be added dropwise, and adjusts solution ph to 4,5g melamines are adulterated by per 1L silicon dioxide gels
Fire retardant is added in solution phosphatic ratio；Prepared solution is persistently stirred to 5 hours obtained forerunners at 40 DEG C again
Liquid solution.Quantitative precursor solution is taken, is sufficiently mixed and stirs evenly, then solution is adjusted into pH value to 6 with 10% ammonium hydroxide, side
Side addition is stirred, is poured into mold that is preprepared, cleaning up and dry.Then mold is placed in 50 DEG C of water-baths, 1
Silica dioxide gel is formed after hour.Aging 6 hours in 60 DEG C of water-baths.Mold is taken out, then is removed from the molds aeroge
Block, by supercritical drying, 100 degrees Celsius, 3 hours obtain hydrophobic type aerogel block body material.Hydrophobic type gas obtained
Gel mass material has elasticity, and resilience is fine, can bear certain pressure intensity, and hydrophobicity is good, thermal coefficient 0.025w/
（m•k）.
Embodiment 3
By methyl orthosilicate, octadecyl trimethoxysilane with molar ratio 1：1 ratio is mixed evenly, then this is mixed
Object is with methanol, water with molar ratio 2：20：5 ratio, which is sufficiently mixed, to stir evenly, and is slowly dropped into the HNO3 solution of 2mol/L mixed
It closes in uniform solution, side stirring, which becomes, to be added dropwise, and adjusts solution ph to 3,5g polyphosphates are adulterated by per 1L silicon dioxide gels
Ratio will fire retardant be added solution in；Prepared solution is persistently stirred to 5 hours obtained precursor solutions at 40 DEG C again.
Quantitative precursor solution is taken, is sufficiently mixed and stirs evenly, then pH value is adjusted to 6 with the solution of 0.5Mol/L, is added while stirring
Add, pours into mold that is preprepared, cleaning up and dry.Then mold is placed in 40 DEG C of water-baths, shape after 2 hours
At silica dioxide gel.Aging 12 hours in 60 DEG C of water-baths.Mold is taken out, then is removed from the molds airsetting blob of viscose, is passed through
Vacuum drying, 120 degrees Celsius, 3 hours obtain hydrophobic type aerogel block body material.Hydrophobic type aerogel block body material obtained
Material has elasticity, and resilience is fine, can bear certain pressure intensity, and hydrophobicity is good, thermal coefficient 0.023w/（m•k）.
Claims (9)
1. a kind of preparation method of the elastic silica aerogel block materials with toughness, it is characterised in that：Including following
Step：
（1）The preparation of silicon dioxide gel：Using siloxanes as presoma, a variety of siloxanes are mixed evenly；It has added
Solvent, water, stir evenly, and catalyst is added dropwise while stirring, adjust solution ph to 1~7；It is molten by every 1L silica
1g~100g fire retardants are added in glue；Rapid stirring, is uniformly dispersed；In 10 DEG C~70 DEG C constant temperature 4 hours or more, clear two are obtained
Silica sol；The siloxanes, organic solvent, water molar ratio be 1:3~80:2~40；
（2）The preparation of gel：Take it is a certain amount of reaction complete precursor solution, be added dropwise basic catalyst adjust pH value to
6~7, quickly stir certain time；
（3）By step（2）The gel of preparation is slowly injected into mold；
（4）By step（3）The gel of middle preparation stands a period of time at a certain temperature, and aging makes its gel solidification shape；
（5）It is dry：The gel of gained is dried, hydrophobic type aerosil thermal insulation block materials are obtained.
2. a kind of preparation method of the elastic silica aerogel block materials with toughness as described in claim 1,
It is characterized in that：The step（1）In siloxanes be Si（OR1）4With R2Si（OR3）3、R4 2Si（OR5）2One or more of
Mixture, the R1、R2、R3、R4、R5For identical or different alkane, alkene, aromatic hydrocarbon group.
3. a kind of preparation method of the elastic silica aerogel block materials with toughness as described in claim 1,
It is characterized in that：The step（1）In organic solvent be methanol, ethyl alcohol, ethylene glycol, propyl alcohol, n-butanol, isobutanol, n-amyl alcohol,
One or more of mixtures of isoamyl alcohol, n-hexyl alcohol, isohexyl alcohol or acetone.
4. a kind of preparation method of the elastic silica aerogel block materials with toughness as described in claim 1,
It is characterized in that：The step（1）In catalyst be acidic catalyst, the acidic catalyst be inorganic acid or organic acid；Institute
It is HCl, H to state inorganic acid2SO4、H3PO4、H2CO3、HF、HBr、HNO3、H2SO3Or HClO4One or more of mixtures, it is described
Organic acid is CH3COOH、HOOC-COOH、HOOCC2H4COOH or C6H5One or more of mixtures of COOH.
5. a kind of preparation method of the elastic silica aerogel block materials with toughness as described in claim 1,
It is characterized in that：The step（1）In fire retardant be organic halogen-free environment-friendlyflame flame retardant；Organic halogen-free environment-friendlyflame flame retardant is
Polyphosphate, melamine, three (1- oxo -1- phosphas -2,6,7- trioxa-l-phosphabicyclos [2,2,2] octane -4- methylene) phosphoric acid
Ester, N, N- p-phenylenediamine bases（2- hydroxyls）The one of dibenzyl phosphonic acids tetra-ethyl ester, melamine phosphate or melamine cyanurate
Kind or mixing flame retardant products several and based on listed material.
6. a kind of preparation method of the elastic silica aerogel block materials with toughness as described in claim 1,
It is characterized in that：The step（2）In basic catalyst be sodium bicarbonate solution, sodium hydroxide solution, ammonium hydroxide, in silazane
It is one or more of.
7. a kind of preparation method of the elastic silica aerogel block materials with toughness as described in claim 1,
It is characterized in that：The step（4）In dwell temperature be 20~80 DEG C, time of repose be 0.2~24 hour；The temperature of aging is
30~90 DEG C, the time is 0~48 hour.
8. a kind of preparation method of the elastic silica aerogel block materials with toughness as described in claim 1,
It is characterized in that：The step（5）The method of middle drying is supercritical drying, constant pressure and dry, subcritical drying, vacuum drying or cold
It is lyophilized one or more of dry；The supercritical drying, subcritical drying medium be carbon dioxide, methanol, ethyl alcohol, positive third
One kind in alcohol, isopropanol, butanol, acetone or acetonitrile；The constant pressure and dry temperature be 20~200 DEG C, the time be 0.1~
120h。
9. a kind of elastic silica airsetting with toughness made from claim 1~7 any one of them preparation method
Glue block materials.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110775980A (en) * | 2019-11-27 | 2020-02-11 | 鑫创新材料科技(徐州)有限公司 | Efficient preparation method and application of aerogel |
| CN110817887A (en) * | 2019-11-27 | 2020-02-21 | 鑫创新材料科技(徐州)有限公司 | Efficient production method and application of aerogel |
| CN111072037A (en) * | 2020-02-10 | 2020-04-28 | 洪永建 | Preparation method of silicon dioxide aerogel with good flexibility |
| CN112174144A (en) * | 2020-09-28 | 2021-01-05 | 航天特种材料及工艺技术研究所 | A kind of ultra-high transparency large-size bulk silica aerogel and its preparation method and application |
| CN114163643A (en) * | 2022-01-05 | 2022-03-11 | 航天材料及工艺研究所 | A porous silicone resin and lightweight flexible flame retardant composite material |
| CN116920733A (en) * | 2023-06-30 | 2023-10-24 | 湖北三峡实验室 | Device for continuously producing nano aerogel and application method thereof |
| CN117361544A (en) * | 2023-09-19 | 2024-01-09 | 广州碧天高科技产业有限公司 | Preparation of silica aerogel and application of silica aerogel in heat preservation of clothes |
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| CN104556969A (en) * | 2014-12-30 | 2015-04-29 | 纳诺科技有限公司 | A preparation method of hydrophobic silica airgel thermal insulation composite material |
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Cited By (9)
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| CN110775980A (en) * | 2019-11-27 | 2020-02-11 | 鑫创新材料科技(徐州)有限公司 | Efficient preparation method and application of aerogel |
| CN110817887A (en) * | 2019-11-27 | 2020-02-21 | 鑫创新材料科技(徐州)有限公司 | Efficient production method and application of aerogel |
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| CN111072037A (en) * | 2020-02-10 | 2020-04-28 | 洪永建 | Preparation method of silicon dioxide aerogel with good flexibility |
| CN112174144A (en) * | 2020-09-28 | 2021-01-05 | 航天特种材料及工艺技术研究所 | A kind of ultra-high transparency large-size bulk silica aerogel and its preparation method and application |
| CN114163643A (en) * | 2022-01-05 | 2022-03-11 | 航天材料及工艺研究所 | A porous silicone resin and lightweight flexible flame retardant composite material |
| CN116920733A (en) * | 2023-06-30 | 2023-10-24 | 湖北三峡实验室 | Device for continuously producing nano aerogel and application method thereof |
| CN117361544A (en) * | 2023-09-19 | 2024-01-09 | 广州碧天高科技产业有限公司 | Preparation of silica aerogel and application of silica aerogel in heat preservation of clothes |
| CN117361544B (en) * | 2023-09-19 | 2024-04-12 | 广州碧天高科技产业有限公司 | Preparation of silica aerogel and application of silica aerogel in heat preservation of clothes |
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