CN108249943A - A kind of preparation method of water-fast aerogel material - Google Patents
A kind of preparation method of water-fast aerogel material Download PDFInfo
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- CN108249943A CN108249943A CN201810067687.9A CN201810067687A CN108249943A CN 108249943 A CN108249943 A CN 108249943A CN 201810067687 A CN201810067687 A CN 201810067687A CN 108249943 A CN108249943 A CN 108249943A
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- 239000000463 material Substances 0.000 title claims abstract description 119
- 239000004964 aerogel Substances 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000000835 fiber Substances 0.000 claims abstract description 76
- 238000000034 method Methods 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000002904 solvent Substances 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 230000008569 process Effects 0.000 claims abstract description 27
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 229910052710 silicon Inorganic materials 0.000 claims description 26
- 239000010703 silicon Substances 0.000 claims description 25
- 238000012545 processing Methods 0.000 claims description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 19
- 239000011240 wet gel Substances 0.000 claims description 19
- 239000003960 organic solvent Substances 0.000 claims description 18
- 230000032683 aging Effects 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 239000012445 acidic reagent Substances 0.000 claims description 13
- 239000003153 chemical reaction reagent Substances 0.000 claims description 13
- 238000006073 displacement reaction Methods 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 230000001476 alcoholic effect Effects 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 150000002576 ketones Chemical class 0.000 claims description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 238000000352 supercritical drying Methods 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
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- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 235000021197 fiber intake Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 12
- 238000005728 strengthening Methods 0.000 abstract description 6
- 239000002121 nanofiber Substances 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 32
- 235000012239 silicon dioxide Nutrition 0.000 description 14
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- 239000010453 quartz Substances 0.000 description 12
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- 239000000499 gel Substances 0.000 description 10
- 230000002209 hydrophobic effect Effects 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 8
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- 239000002245 particle Substances 0.000 description 5
- 239000004965 Silica aerogel Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000007863 gel particle Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 235000019994 cava Nutrition 0.000 description 3
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 239000011043 treated quartz Substances 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- GJCOSYZMQJWQCA-UHFFFAOYSA-N 9H-xanthene Chemical compound C1=CC=C2CC3=CC=CC=C3OC2=C1 GJCOSYZMQJWQCA-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- DRUOQOFQRYFQGB-UHFFFAOYSA-N ethoxy(dimethyl)silicon Chemical compound CCO[Si](C)C DRUOQOFQRYFQGB-UHFFFAOYSA-N 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The present invention relates to a kind of preparation methods of water-fast aerogel material, and described method includes following steps：(1) prepared by colloidal sol；(2) powder disperses；(3) prepared by aerogel material；(4) water-fast aerogel material has been made in heat treatment process.The present invention has also carried out surface-active pretreatment, the nanofiber of surface active may be uniformly dispersed in colloidal sol and solvent, enhance the structural strength of material before powder dispersion to fiber described in step (2).The present invention carries out heat treatment process to aerogel material, realize aerogel material microstructure Strengthening and Toughening, nanometer skeleton is more firm, and the structural strength of aerogel material significantly improves, the preparation of water-fast aerogel material is realized, and the water-fast aerogel material can repeatedly use.
Description
Technical field
The present invention relates to aeroge preparing technical field more particularly to a kind of reusable water-fast aerogel materials
Preparation method.
Background technology
Nanoporous aerogel (abbreviation aeroge) material is the gel rubber material that a kind of decentralized medium is gas, is by colloid
Particle or high-polymer molecular mutually build up a kind of nanoporous solid material with network structure of composition, the material mesoporous
The size of gap is in nanometer scale.Its porosity is up to 80~99.8%, and the typical sizes of hole are 1~100nm, specific surface area
For 200~1000m2/ g, and density can be down to 3kg/m3, room temperature thermal conductivity factor can be down to 0.012W/mk.Just because of these
Feature makes aerogel material have very wide application potential in terms of calorifics, acoustics, optics, microelectronics, particle detection.At present,
The prepared and aeroge used and its relevant aerogel composite have good heat-insulated in certain usage time
Effect, but for a long time and repeatedly use and then there are problems that, finally influence heat insulation.Main problem is：First, gas
The nano-porous structure of gel is not sufficiently stable, and is encountering moisture or water environment is easy to recurring structure and caves in.2nd, it is multiple in experience
It caves in after reuse since stress easilys lead to surface micro-structure generation rupture, so as to lose corresponding thermal insulation
Energy.3rd, aeroge occurs moisture absorption and leads to heat-insulated failure in use in order to prevent, at present used in aerogel material it is equal
By special silicic acid anhydride.But the silicic acid anhydride technology used at present is only applicable in primary heat-insulated use, process is heat-insulated
The hydrophobic agents of aeroge surface modification can decompose at high temperature after heating, so as to lose heat insulation.Therefore, repeating makes
Have great importance with the preparation of aerogel material for current repetition thermal insulation applications.
In conclusion preparing reusable aerogel heat-insulating material problem to be solved is one, improves material micro-nano
The stability of rice structure realizes the strong of material microstructure by adjusting complex techniques such as precursor preparation process binding fiber enhancings
Toughening.That the 2nd, carries out aeroge repeats hydrophobic technology, realizes that aeroge is more by the repeatable hydrophobic technology for exploring aeroge
Secondary reuse still has good anti-moisture sorption effect.Entitled " the Orbiter Thermal delivered in 2011
In Protection System Lessons Learned " articles by taking " shuttle Columbia " as an example, for hydrophobic
Problem is mentioned：The technical issues of to prevent moisture from entering inside thermal insulation tile be one important.Since moisture adsorbs thermal protection system meeting
It is abnormal, the water resistance of thermal insulation tile is caused to decline.Initially by spraying treatment, quick special hydrophobization mistake again is carried out
Journey, but waterproof layer can be destroyed when its temperature is more than 1050 ℉ (565 DEG C).Initial spray process is tried using fluoropolymer
Agent provides the film of low-surface-energy in outer surface.This processing procedure of empirical tests cannot provide the barrier of sealing waterproof.
(referring to：Snapp,Cooper,and A.Rodriguez."Orbiter Thermal Protection System Lessons
Learned."AIAA SPACE 2011Conference。)
Then, Kennedy Space Center uses improved hydrophobic agents modified technique, makes hydrophobic more effective, but flight every time
Afterwards, it needs to inject dimethylethoxysilane in the external holes of face coat by the rifle of needle-less, but hydrophobic agents are super
It crosses 1100 ℉ (593 DEG C) and will appear cause thermal damage, water suction behavior can be generated by being exposed to the outer surface of thermal protection system.Therefore, mesh
It is preceding can be with resistance to 600 DEG C or more of high temperature without effective hydrophobic agents, nanostructured is tough to be melted into reusable aeroge
One effective route of material preparation, by the intensity for improving nanostructured prevent material in reuse due to steam and should
The factors such as power cause structure to be destroyed.
Chinese patent application CN201510857626.9 discloses a kind of preparation side of high temperature oxidation resisting Silica Aerogels
Method, this method carry out hydro-thermal process to wet gel, and in hydrothermal treatment process, gel network is further perfect, gel particle grain
Diameter increases to more than 20nm by 10~15nm, is tightly combined between particle, and aeroge temperature tolerance is significantly improved, but the party
Method hydrothermal conditions are long, and are only that the temperature tolerance for improving aerogel material；Prepared aerogel material passes through 1200 DEG C
The time of processing is only 0.5h, and linear shrinkage ratio is minimum also to reach 2%.Chinese patent document CN201310276044.2 is disclosed
A kind of preparation method of high temperature-resistanalumina alumina aerogel material, aerogel material prepared by this method is after 1200 DEG C handle 2h
Linear shrinkage ratio is 5%.Therefore, both methods prepare aerogel material cannot for a long time and repeatedly use.
Chinese patent application CN201610826777.2 discloses a kind of fiber composite aerosil heat-barrier material
And preparation method thereof, this method is compounded with fiber in silica aerogel material, enhances the mechanical property of material, and will
Dried fiber composite silica aerogel material is heat-treated, and the process specifically handled is that material is put into Muffle
In stove, successively adjust temperature and be heat-treated 10~15 minutes respectively for 270~280 DEG C, 295~305 DEG C and 345~355 DEG C, obtained
Hydrophobic angle is 120 °~170 ° of fiber composite silica aerogel material, but according to entitled《Super-hydrophobicity airsetting
The preparation of rubber powder body coating and performance》Article record that " temperature is on aeroge by influencing the Si~CH on its surface3Silylation base
Group influences its hydrophobicity, and aeroge is super-hydrophobicity at less than 250 DEG C, at 350 DEG C or more, because of Si~CH3Group is super by oxidation
Hydrophobicity continuously decreases, at 600 DEG C, Si~CH3Group is all aoxidized, and is changed into hydrophilic aeroge." (referring to：Zhang Ning,
Chen Wei, Lao Lilin, the preparation of field pressure wave super-hydrophobicity aerogel powder coatings and performance [J] functional materials, 2015,46
(13):13091~13094.) therefore, fiber composite aerosil heat-barrier material disclosed in CN201610826777.2
Hydrophobicity may not be presented at high temperature, there are problems that aeroge nanometer skeleton cave in after water is met, heat-insulated failure,
It can not reuse.
At present, it is notable about the raising of the structure Strengthening and Toughening of aerogel material, the structural strength of aerogel material and water resistance
It improves, can realize that the research in terms of aerogel material reusability has not been reported.
Invention content
For overcome the deficiencies in the prior art, the present invention provides a kind of preparation process is simple, materials water-resistant and structure
The preparation method of reusable water-fast aerogel material that intensity significantly improves.
The present invention provides a kind of preparation methods of water-fast aerogel material, and described method includes following steps：
(1) prepared by colloidal sol：Using organo-silicon ester as raw material, acid reagent be catalyst and organic solvent is that dispersant is made
Silica sol；
(2) powder disperses：Oxide powder with fiber is uniformly mixed, obtains the mixing containing oxide powder and fiber
Material, then the mixture is mixed, obtain the first mixed liquor, then add in step into first mixed liquor with organic solvent
(1) silica sol made from, and first time decentralized processing is carried out, the second mixed liquor is obtained, finally into second mixed liquor
Alkaline reagent is added in as catalyst, and carries out second of decentralized processing, aeroge wet gel is made；
(3) prepared by aerogel material：By aeroge wet gel made from step (2) successively by gelling and aging, solvent
Displacement and dry step, are made aerogel material；With
(4) heat treatment process：Aerogel material made from step (3) is heat-treated under conditions of 500 DEG C~1500 DEG C
Water-fast aerogel material is made in 0.1~3h.
Preferably, the method is additionally included in before step (2), and fiber described in step (2) is pre-processed：Use water
Fiber is configured to fiber aqueous solution, surfactant is then added in into the fiber aqueous solution in the fiber aqueous solution
The fiber contained is pre-processed, and obtains pretreated fiber aqueous solution, then the pretreated fiber aqueous solution is dried
It is dry, obtain pretreated fiber.
Preferably, colloidal sol preparation is carried out using two-step method in step (1)：
The first step：Organo-silicon ester, organic solvent and acid reagent are uniformly mixed, and under conditions of stirring reflux 10~
60min obtains the first solution of silica sol presoma；With
Second step：Organo-silicon ester is added in into the first solution of silica sol presoma that the first step obtains, is obtained siliceous molten
The second solution of glue presoma, by second solution of silica sol presoma under conditions of stirring and temperature are 50~120 DEG C
Holding 2~for 24 hours, obtain silica sol.
Preferably, in the first step, a concentration of 0.001~0.1mol/L of the acid reagent, the organo-silicon ester have
The mass ratio of solvent and acid reagent is (50~1000)：(50~1000)：(1~200)；Organo-silicon ester in the first step
Mass ratio with organo-silicon ester in the second step is (50~1000)：(50~1000).
Preferably, a concentration of 0.1wt%~1.0wt% of the fiber aqueous solution；The dosage of the surfactant accounts for
The mass percentage content of the fiber consumption is 1%~2%；The surfactant is neopelex；It is described
Pretreatment carries out under conditions of the fiber aqueous solution is placed in rotating speed as 1000~4000r/min；And/or the drying
Temperature for 50~70 DEG C, the time of the drying is 10~14h.
Preferably, organo-silicon ester described in step (1) is methyl orthosilicate or ethyl orthosilicate；It is sour described in step (1)
Property reagent be selected from the group that is made of hydrochloric acid, hydrofluoric acid and nitric acid；Alkaline reagent described in step (2) is ammonium hydroxide；The alkalinity examination
A concentration of 0.1~1mol/L of agent；And/or step (1) and/or step (2) described organic solvent are selected from by methanol, ethyl alcohol, third
The group of ketone and acetonitrile composition.
Preferably, the quality of oxide powder described in step (2), fiber, silica sol, alkaline reagent and organic solvent
Than for (1~100)：(1~20)：(0.1~60)：(0.1~30)：(10~200)；Oxide powder and fiber in step (2)
Mixing be to be carried out in the dry-mixed machine for being 100~500r/min in rotating speed, time of mixing is 1~3h；Described in step (2)
First time decentralized processing and/or second of decentralized processing are ultrasonic disperse processing；The time of the first time decentralized processing
For 10~60min；The time of second of decentralized processing is 10~30min.
Preferably, it is gelled described in step (3) with the step of aging and is：Aeroge wet gel made from step (2) is quiet
Putting 12~72h makes the aeroge wet gel that gelling reaction occur, and 12~72h carries out old under the conditions of being then placed in 20~80 DEG C again
Change and further gelling reaction.
Preferably, the solvent displacement carries out in alcoholic solvent or ketone solvent；The alcoholic solvent be selected from by methanol, ethyl alcohol,
The group of propyl alcohol and isopropanol composition；The ketone solvent is selected from the group that butanone and acetone form；The time of solvent displacement for 1~
5d。
Preferably, the drying is supercritical drying, and preferably supercritical carbon dioxide is dried.
The present invention at least has the advantages that compared with prior art：
(1) present invention is different by improving high temperature resistant hydrophobic agents from other, it is proposed that passes through microstructure Strengthening and Toughening system
For the aerogel material of standby stable structure for repeating thermal insulation applications, this improved method has more feasibility.
(2) present invention is enhanced using staple in bulk, in order to increase the uniformity, improves fiber dispersion process, this side
Formula can overcome the lamination problem that the reinforcements such as fibrofelt occur in heat treatment process, and the fiber of dispersion can be with oxidate powder
Body is matched in time.
(3) present invention is mixed using pretreated fiber with oxidate nano, obtains the oxidate nano of surface active
As aeroge skeleton unit, great amount of hydroxy group existing for nm-class oxide powder surface can be chemically bonded powder with sol particles,
Nano-particle is made to may be uniformly dispersed in colloidal sol and solvent, do not settle and is reunited, enhances the structure of aerogel material
Intensity.
(4) the powder dispersion in the present invention, when the powder used is oxide nonmetallic powder, there are the mistakes of nanocrystalline assembling
The nano-particle of high temperatures is carried out assembling bonding, realizes oxide by journey, nanocrystalline package technique combination heat treatment process
Nanocrystalline effectively assembles and fixes, and realizes the preparation of nucleocapsid porous network aeroge.Nucleocapsid shape at high temperature
Into network frame, it can effectively inhibit growing up for subscale nanocrystal, improve the intensity of nanostructured, can prevent
Material is in reuse since the factors such as steam and stress cause structure to be destroyed.
(5) present invention is only 0.145g/ since the initial density of preparation is relatively low using low-density Ludox as bonding agent
cm3, the water-fast aerogel material after subsequent heat treatment process is still with relatively low density.
(6) aerogel material prepared by the method for the present invention has excellent water resistance under the premise of keeping durothermic
With mechanical property, can for a long time and repeatedly use.
(7) for the porosity of water-fast aerogel material prepared by the method for the present invention more than 80%, pore size is 5~500nm,
The gel particle grain size of aeroge is 10~400nm, and specific surface area is 50~500m2/ g, heat resisting temperature are 800 DEG C or more.
Description of the drawings
Fig. 1 is preparation flow figure of the present invention.
Fig. 2 is that aerogel material meets water and caves in the schematic diagram of process in the prior art.In figure：(a) it is gas in the prior art
Gel molecular meets the schematic diagram photo before water；(b) be in the prior art airsetting xanthan molecule meet water after schematic diagram photo.
Fig. 3 is the structure Strengthening and Toughening schematic diagram of aerogel material prepared by the present invention.In figure：(a) prepared by the present invention
Schematic diagram before the structure Strengthening and Toughening of aerogel material；(b) it is after the structure Strengthening and Toughening of aerogel material for preparing of the present invention
Schematic diagram.
Fig. 4 is that water-fast aerogel material prepared by the embodiment of the present invention 1 uses photo before and after the soaked 0.5h of room temperature bowssening.
Fig. 5 is that water-fast aerogel material prepared by the embodiment of the present invention 2 uses photo before and after the soaked 0.5h of room temperature bowssening.
Fig. 6 is that water-fast aerogel material prepared by the embodiment of the present invention 3 freezes photo before and after 0.5h in refrigerator.
In fig. 4 to fig. 6：(a) photo for water-fast aerogel material before soaked or before freezing；(b) it is water-fast aeroge material
Photo after parison water or after freezing.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is the part of the embodiment of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of all other embodiments obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of preparation methods of water-fast aerogel material, and described method includes following steps：
(1) prepared by colloidal sol：Using organo-silicon ester as raw material, acid reagent be catalyst and organic solvent is that dispersant is made
Silica sol.The organo-silicon ester can be the organo-silicon ester that can sell on the market, such as methyl orthosilicate or ethyl orthosilicate；Institute
It states acid reagent and is selected from the group being made of hydrochloric acid, hydrofluoric acid and nitric acid, a concentration of 0.001~0.1mol/L of the acid reagent
(such as 0.001,0.005,0.01,0.02,0.03,0.04,0.05,0.06,0.07,0.08,0.09 or 0.1mol/L)；It is described
Organic solvent is selected from the group being made of methanol, ethyl alcohol, acetone and acetonitrile.
(2) powder disperses：Oxide powder with fiber is uniformly mixed, obtains the mixing containing oxide powder and fiber
Material, then the mixture is dissolved, obtain the first mixed liquor, then add in step into first mixed liquor with organic solvent
(1) silica sol made from, and first time decentralized processing is carried out, the second mixed liquor is obtained, finally into second mixed liquor
Alkaline reagent is added in as catalyst, and carries out second of decentralized processing, aeroge wet gel is made.
Heretofore described powder dispersion includes the mixed process of the oxide powder and the fiber, the oxidation
Powder and being mixed into for the fiber are dry-mixed, such as oxide powder and fiber are matched and according to a certain percentage in dry-mixed machine
In be uniformly mixed, the rotating speed of the dry-mixed machine is 100-500r/min (such as 100,150,200,250,300,400 or 500r/
min)。
The oxide powder for example can be nanometer alumina powder or silica nano-powder；Described in step (2)
Organic solvent is selected from the group being made of methanol, ethyl alcohol, acetone and acetonitrile；Alkaline reagent described in step (2) is ammonium hydroxide；The alkali
A concentration of 0.1~1mol/L (such as 0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 or 1mol/L) of property reagent；Step
Suddenly the mass ratio of oxide powder described in (2), fiber, silica sol, alkaline reagent and organic solvent is (1~100)：(1~
20)：(0.1~60)：(0.1~30)：(10~200)；The mixing of oxide powder and fiber is to be in rotating speed in step (2)
Carried out in the dry-mixed machine of 100~500r/min (such as 100,200,300,400 or 500r/min), time of mixing for 1~
3h (such as 1,1.5,2,2.5 or 3h)；First time decentralized processing described in step (2) and/or second of decentralized processing are
Ultrasonic disperse processing；The time of the first time decentralized processing is 10~60min (such as 10,20,30,40,50 or 60min)；
The time of second of decentralized processing is 10~30min (such as 10,15,20,25 or 30min).
(3) prepared by aerogel material：By aeroge wet gel made from step (2) successively by gelling and aging, solvent
Displacement and dry step, are made aerogel material.
(4) heat treatment process：By aerogel material made from step (3) 500 DEG C~1500 DEG C (such as 500 DEG C, 600
DEG C, 700 DEG C, 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C, 1200 DEG C, 1300 DEG C, 1400 DEG C or 1500 DEG C) under conditions of heat at
0.1~3h (such as 0.1,0.2,0.3,0.4,0.5,1.0,1.2,1.5,1.8,2.0,2.3,2.5,2.8 or 3h) is managed, is made resistance to
Aerogel material.
The present invention can react according to silica in aerogel material and oxidate nano crystal grain so that crystal transition
Temperature determine heat treatment temperature, such as aoxidizing silicon nano power, heat treatment temperature is 1000 DEG C~1300 DEG C.
When being heat-treated to aerogel material made from step (3), such as can be by aeroge made from step (3)
Material is warming up to 500 DEG C~1500 DEG C with stove (such as Muffle furnace), heating rate for 1~10 DEG C/min (such as 1,2,3,4,5,
6th, 7,8,9 or 10 DEG C/min), with stove it is cooled to room temperature after keeping the temperature 0.1~3h.
According to some preferred embodiments, gelling described in step (3) is with the step of aging：Step (2) is made
Aeroge wet gel stand 12~72h (such as 12,18,24,30,36,42,48,54,60,66 or 72h) make the aeroge
Gelling reaction occurs for wet gel, is then placed in 20~80 DEG C (such as 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 80 again
DEG C) under the conditions of 12~72h (such as 12,18,24,30,36,42,48,54,60,66 or 72h) carry out aging and further glue
Solidifying reaction.Specifically, such as aeroge wet gel made from step (2) can be placed in mold, stands for 24 hours, be subsequently placed at
48h in 60 DEG C of baking ovens completes the process of gelling and aging.
According to some preferred embodiments, the solvent displacement carries out in alcoholic solvent or ketone solvent；The alcoholic solvent
Selected from the group being made of methanol, ethyl alcohol, propyl alcohol and isopropanol；The ketone solvent is selected from the group that butanone and acetone form；It is described molten
Agent displacement used in solvent volumetric usage be gelling and aging after gel volume 5~30 times (such as 5,10,15,20,
25 or 30 times)；The time of the solvent displacement is 1~5d (1,2,3,4 or 5d), and the process of solvent displacement repeats 1~10
Secondary (such as 1,2,3,4,5,6,7,8,9 or 10 time).Such as will be gelled taken out with the gel after aging after be put into 10 times of volumes
It is replaced 3 days in alcohol solvent, the process of solvent displacement is repeated 3 times.
According to some preferred embodiments, the drying is supercritical drying, and preferably supercritical carbon dioxide is dried.
According to some preferred embodiments, the method is additionally included in before step (2), to fine described in step (2)
Dimension is pre-processed：Fiber is configured to fiber aqueous solution with water, then adds in surfactant into the fiber aqueous solution
The fiber contained in the fiber aqueous solution is pre-processed, obtains pretreated fiber aqueous solution, then by the pre- place
The fiber aqueous solution drying managed, obtains pretreated fiber.Preferably, the fiber aqueous solution is a concentration of
0.1wt%~1.0wt% (such as 0.1wt%, 0.2wt%, 0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%,
0.8wt%, 0.9wt% or 1.0wt%)；The dosage of the surfactant accounts for the mass percentage content of the fiber consumption
For 1%~2% (such as 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9% or
2.0%)；The surfactant is neopelex；The pretreatment is to be placed in rotating speed in the fiber aqueous solution
To be carried out under conditions of 1000~4000r/min (such as 1000,1500,2000,2500,3000,3500 or 4000r/min)
's；And/or the temperature of the drying be 50~70 DEG C (such as 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C or 70 DEG C), the drying when
Between be 10~14h (such as 10,11,12,13 or 14h).
In the present invention, the preprocessing process of the fiber is carried out under conditions of high speed rotation, is realized fully dispersed
Staple in bulk, the present invention using staple in bulk carries out enhancing aerogel material, be in order to increase the uniformity that fiber disperses, can with gram
The lamination problem that the reinforcements such as fibrofelt occur in heat treatment process is taken, the staple in bulk of dispersion can be carried out with oxide powder
Matching in time.The present invention is not particularly limited the fiber, preferably inorfil, such as can be quartz fibre or oxygen
Change aluminum fiber.
According to some preferred embodiments, colloidal sol preparation is carried out using two-step method in step (1)：
The first step：Organo-silicon ester, organic solvent and acid reagent are uniformly mixed, and under conditions of stirring reflux 10~
60min (10,20,30,40,50 or 60min), obtains the first solution of silica sol presoma；With
Second step：Organo-silicon ester is added in into the first solution of silica sol presoma that the first step obtains, is obtained siliceous molten
Second solution of silica sol presoma in stirring and temperature is 50~120 DEG C (such as 50 by the second solution of glue presoma
DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C or 120 DEG C) under conditions of keep 2~for 24 hours, obtain silica sol (example
As 2,4,6,8,10,12,14,16,18,20,22 or for 24 hours).Particularly, the silica sol is diluted, first steamed described
100~500g of solvent (such as 100,200,300,400 or 500g) that silica sol contains, adds 500~1000g of alcoholic solvent
(500,600,700,800,900 or 1000g) is uniformly mixed, and refrigerate spare.
Using two-step method carry out colloidal sol preparation when, it is preferred that in the first step, the organo-silicon ester, organic solvent with
The mass ratio of acid reagent is (50~1000)：(50~1000)：(1~200)；Organo-silicon ester and described the in the first step
The mass ratio of organo-silicon ester is (50~1000) in two steps：(50~1000).The present invention using two-step method prepares colloidal sol, can be to prevent
Only organic silicone grease is hydrolyzed fast, ensures sol particle homoepitaxial.
The porosity of water-fast aerogel material prepared by the present invention more than 80%, pore size be 5~500nm, aeroge
Gel particle grain size for 10~400nm, specific surface area is 50~500m2/ g, heat resisting temperature are 800 DEG C or more.
Embodiment 1
1. prepared by colloidal sol
Methyl orthosilicate 200g and ethyl alcohol 200g are weighed in 1000mL beakers, be sealed against with preservative film and carries out magnetic force
Stir 1min.After mixing, the hydrochloric acid 50g of a concentration of 0.005mol/L is added in as catalyst, which needs slowly to add
Enter, and pass through magnetic agitation 2min；Above-mentioned mixed liquor is added in the there-necked flask of 1000mL, heating and magnetic force under the conditions of 70 DEG C
Stirring, and with reflux 30min, obtain the first solution of silica sol presoma；It is added in into obtained silica sol presoma
The methyl orthosilicate of 200g, continues heating and magnetic agitation under the conditions of 80 DEG C, and reaction for 24 hours, obtains silica sol (silica
Colloidal sol).The silica sol is diluted, steams the solvent 300g that the silica sol contains, ethyl alcohol 1000g is added and mixes
Uniform, the silica sol after being diluted is closed, and the silica sol after the dilution refrigerate spare.
2. powder disperses
It weighs quartz fibre 1g to be dissolved in 1000L water, stir evenly, quartz fibre dosage is added in based on mass percentage
1% neopelex as surfactant, after high speed rotation (rotating speed 4000r/min) dispersion, be placed in 60
12h is dried in DEG C baking oven, obtains pretreated quartz fibre.Then by 10g silica nano-powder and pretreated stone
English fiber 0.1g is mixed, and with the rotating speed mixing 1h of 200r/min in dry-mixed machine, obtains mixing containing silica powder and fiber
Material is closed, the mixture is mixed in 120g ethyl alcohol, is stirred evenly, adds in the silica sol 2g after above-mentioned dilution, ultrasonic disperse
30min adds in a concentration of 0.8mol/L ammonium hydroxide 0.2g as catalyst, continues ultrasound 20min, aeroge wet gel is made.
3. gelling and aging
Aeroge wet gel obtained is placed in mold, is stood for 24 hours, is subsequently placed at 48h in 60 DEG C of baking ovens, completes gelling
With the process of aging.
4. solvent is replaced
Above-mentioned complete is put into progress solvent displacement in the ethyl alcohol of 10 times of volumes after gelling is taken out with the gel after aging,
The time of solvent displacement is 3d, which is repeated 3 times.
5. aerogel material is made in supercritical drying.
6. heat treatment process
Above-mentioned aerogel material be warming up to 1000 DEG C (heat treatment temperatures) with stove, heating rate is 5 DEG C/min, is protected
Room temperature is cooled to stove after warm 2h (heat treatment time), water-fast aerogel material is made.
To water-fast aerogel material progressive energy Indexs measure prepared by embodiment 1, as a result show：Prepared by embodiment 1
The density of water-fast aerogel material is 0.149g/cm3, porosity 88%, pore size be 10~30nm, the grain size of gel particle
For 10~30nm, specific surface area 198m2/ g (heat treated specific surface area)；By airsetting glue material obtained after supercritical drying
Material is tested for the property, and compared with not passing through the aerogel material of 1000 DEG C of heat treatment 2h, the line of water-fast aerogel material is received
Shrinkage is 0.65%, heat resisting temperature be more than 1000 DEG C, special instruction, when under heat treatment temperature after Overheating Treatment, gas
The linear shrinkage ratio of gel rubber material is more than 10%, represents that the heat resisting temperature of the aerogel material is not more than the heat treatment temperature.
The heat resisting temperature of water-fast aerogel material in the present embodiment is high, and linear shrinkage ratio is small after 1000 DEG C of heat treatments, water-fast
Property it is good, can effectively prevent that material meets water or dusting occurs for wet environment and the caused heat-insulated failure that comes off in case of wet.
The water resistance of water-fast aerogel material described in the present embodiment is measured using room temperature bowssening, specifically, often
Warm bowssening is：2/3 area of water-fast aerogel material is made to be immersed in distilled water, is taken out after 0.5h, and dry at room temperature, is examined
It the breakoff phenomenons such as looks into water-fast aerogel material and whether has dusting, slight crack, comes off, and test the specific surface of its soaked front and rear material
Product, using its specific surface area conservation rate as the performance measure standard of water resistance.The specific surface area conservation rate be it is soaked after it is resistance to
The ratio of the specific surface area of aerogel material and its specific surface area before soaked, special instruction, bubble of the present invention
Water-fast aerogel material after water is after carrying out water resistance test using room temperature bowssening, and resistant to moisture after being dried at room temperature for
Gel rubber material.
After water-fast aerogel material manufactured in the present embodiment carries out water resistance test, the surface of water-fast aerogel material is found
There is not phenomena such as dusting and slight crack.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, the difference lies in：In powder dispersion, 10g is aoxidized into silicon nano power
Body is mixed with pretreated quartz fibre 1g, with the rotating speed mixing 1h of 200r/min in dry-mixed machine, is obtained containing silica
The mixture is mixed in 120g ethyl alcohol, stirs evenly by the mixture of powder and fiber, adds in siliceous molten after 1. middle dilution
Glue 3g；In heat treatment process, heat treatment temperature is 1100 DEG C.
Water resistance test is carried out to aerogel material water-fast in embodiment 2, finding the surface of water-fast aerogel material does not have
There is phenomena such as dusting and slight crack, other performance index are as shown in table 1.
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, the difference lies in：In powder dispersion, weigh quartz fibre 2g and be dissolved in
In 1000L water, 10g nanometer alumina powders are mixed with pretreated quartz fibre 2g, in dry-mixed machine (200r/min)
1h is mixed, with the rotating speed mixing 1h of 200r/min in dry-mixed machine, the mixture containing oxide powder and fiber is obtained, by institute
It states mixture to be mixed in 120g alcoholic solvents, stir evenly, add in the silica sol 4g after 1. middle dilution；In heat treatment process,
Heat treatment temperature is 1200 DEG C.
Water resistance test is carried out to aerogel material water-fast in embodiment 3, finding the surface of water-fast aerogel material does not have
There is phenomena such as dusting and slight crack, other performance index are as shown in table 1.
Embodiment 4
Embodiment 4 is substantially the same manner as Example 3, the difference lies in：Aerogel material is carried out to be warming up to 1300 with stove
DEG C (heat treatment temperature), heating rate are 5 DEG C/min, keep the temperature and are cooled to room temperature with stove after 3h, water-fast aerogel material is made.
Water resistance test is carried out to aerogel material water-fast in embodiment 4, finding the surface of water-fast aerogel material does not have
There is phenomena such as dusting and slight crack, other performance index are as shown in table 1.
Embodiment 5
Embodiment 5 is substantially the same manner as Example 1, the difference lies in：In powder dispersion, not using detergent alkylate
Sodium sulfonate is surface-treated quartz fibre as surfactant.
Water resistance test is carried out to aerogel material water-fast in embodiment 5, finding the surface of water-fast aerogel material does not have
There is phenomena such as dusting and slight crack, other performance index are as shown in table 1.
Embodiment 6
Embodiment 6 is substantially the same manner as Example 1, the difference lies in：Quartz fibre is substituted with alumina fibre.
Water resistance test is carried out to aerogel material water-fast in embodiment 6, finding the surface of water-fast aerogel material does not have
There is phenomena such as dusting and slight crack, other performance index are as shown in table 1.
Embodiment 7
Embodiment 7 is substantially the same manner as Example 2, the difference lies in：Quartz fibre is substituted with alumina fibre.
Water resistance test is carried out to aerogel material water-fast in embodiment 7, finding the surface of water-fast aerogel material does not have
There is phenomena such as dusting and slight crack, other performance index are as shown in table 1.
Embodiment 8
Embodiment 8 is substantially the same manner as Example 3, the difference lies in：Quartz fibre is substituted with alumina fibre.
Water resistance test is carried out to aerogel material water-fast in embodiment 8, finding the surface of water-fast aerogel material does not have
There is phenomena such as dusting and slight crack, other performance index are as shown in table 1.
Comparative example 1
Comparative example 1 is substantially the same manner as Example 1, the difference lies in：In powder dispersion, not using detergent alkylate
Sodium sulfonate is surface-treated quartz fibre as surfactant；After gelling with Aging Step, solvent swap step
Before, hydrothermal treatment step, by the wet gel after gel aging in 150 DEG C~250 DEG C deionized waters, hydro-thermal process are carried out
48 hours, room temperature is naturally cooling to, wet gel is totally submerged in deionized water in entire hydrothermal treatment process；And it is heat-treated
Temperature is 1200 DEG C, and the time of heat treatment is 0.5h.
Water resistance test is carried out to water-fast aerogel material in comparative example 1, find aerogel material surface have it is a small amount of
Slight crack occurs, and other performance index are as shown in table 1.
Comparative example 2
Comparative example 2 is substantially the same manner as Example 1, the difference lies in：The heat treatment process of comparative example 2 is：It will be overcritical
Dried aerogel material is heat-treated 15 minutes respectively in 280 DEG C, 300 DEG C and 350 DEG C of Muffle furnace.
Water resistance test is carried out to aerogel material water-fast in comparative example 2, finding the surface of aerogel material has on a small quantity
Slight crack occur, other performance index are as shown in table 1.
Comparative example 3
Comparative example 3 is substantially the same manner as Example 1, the difference lies in：In the dispersion of 2. powder, non-oxidation silicon nano power body
With the dry mixing process of pretreated quartz fibre, directly with 120g ethyl alcohol by 10g silica nano-powder with it is pretreated
Quartz fibre 0.1g is mixed evenly, and adds in silica sol 2g, ultrasonic disperse 30min after dilution, adds in a concentration of
0.8mol/L ammonium hydroxide 0.2g continues ultrasound 20min, aeroge wet gel is made as catalyst.
Water resistance test is carried out to aerogel material in comparative example 3, finding the surface of aerogel material has minimal amount of split
Trace occurs, and other performance index are as shown in table 1.
Symbol-expression is without this performance indicator.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent replacement to which part technical characteristic；
And these modification or replace, various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of water-fast aerogel material, which is characterized in that described method includes following steps：
(1) prepared by colloidal sol：Using organo-silicon ester as raw material, acid reagent be catalyst and organic solvent is that dispersant is made siliceous
Colloidal sol；
(2) powder disperses：Oxide powder with fiber is uniformly mixed, obtains the mixture containing oxide powder and fiber,
Then the mixture is mixed with organic solvent, obtains the first mixed liquor, then step (1) is added in into first mixed liquor
Silica sol obtained, and first time decentralized processing is carried out, the second mixed liquor is obtained, is finally added in into second mixed liquor
Alkaline reagent carries out second of decentralized processing as catalyst, and aeroge wet gel is made；
(3) prepared by aerogel material：Aeroge wet gel made from step (2) is replaced successively by gelling and aging, solvent
With dry step, aerogel material is made；With
(4) heat treatment process：Aerogel material made from step (3) is heat-treated under conditions of 500 DEG C~1500 DEG C to 0.1~
Water-fast aerogel material is made in 3h.
2. preparation method according to claim 1, which is characterized in that the method is additionally included in before step (2), to step
Suddenly fiber described in (2) is pre-processed：Fiber is configured to fiber aqueous solution with water, is then added into the fiber aqueous solution
Enter surfactant to pre-process the fiber contained in the fiber aqueous solution, obtain pretreated fiber aqueous solution,
The pretreated fiber aqueous solution is dried again, obtains pretreated fiber.
3. preparation method according to claim 1 or 2, which is characterized in that colloidal sol is carried out using two-step method in step (1)
It prepares：
The first step：Organo-silicon ester, organic solvent and acid reagent are uniformly mixed, and under conditions of stirring reflux 10~
60min obtains the first solution of silica sol presoma；With
Second step：Organo-silicon ester is added in into the first solution of silica sol presoma that the first step obtains, before obtaining silica sol
The second solution of body is driven, 2 are kept under conditions of being 50~120 DEG C in stirring and temperature by second solution of silica sol presoma
~for 24 hours, obtain silica sol.
4. preparation method according to claim 3, it is characterised in that：
In the first step, a concentration of 0.001~0.1mol/L of the acid reagent, the organo-silicon ester, organic solvent and acid
Property reagent mass ratio be (50~1000)：(50~1000)：(1~200)；
The mass ratio of organo-silicon ester and organo-silicon ester in the second step is (50~1000) in the first step：(50~
1000)。
5. preparation method according to claim 2, it is characterised in that：
A concentration of 0.1wt%~1.0wt% of the fiber aqueous solution；
The mass percentage content that the dosage of the surfactant accounts for the fiber consumption is 1%~2%；
The surfactant is neopelex；
The pretreatment carries out under conditions of the fiber aqueous solution is placed in rotating speed as 1000~4000r/min；And/or
The temperature of the drying is 50~70 DEG C, and the time of the drying is 10~14h.
6. preparation method according to claim 1, it is characterised in that：
Organo-silicon ester described in step (1) is methyl orthosilicate or ethyl orthosilicate；
Acid reagent described in step (1) is selected from the group being made of hydrochloric acid, hydrofluoric acid and nitric acid；
Alkaline reagent described in step (2) is ammonium hydroxide；
A concentration of 0.1~1mol/L of the alkaline reagent；And/or
Step (1) and/or step (2) described organic solvent are selected from the group being made of methanol, ethyl alcohol, acetone and acetonitrile.
7. preparation method according to claim 1, it is characterised in that：
Oxide powder described in step (2), fiber, silica sol, alkaline reagent and organic solvent mass ratio for (1~
100)：(1~20)：(0.1~60)：(0.1~30)：(10~200)；
The mixing of oxide powder and fiber is carried out in the dry-mixed machine for being 100~500r/min in rotating speed in step (2), is mixed
The time of conjunction is 1~3h；
First time decentralized processing described in step (2) and/or second of decentralized processing are ultrasonic disperse processing；
The time of the first time decentralized processing is 10~60min；
The time of second of decentralized processing is 10~30min.
8. preparation method according to claim 1, which is characterized in that being gelled described in step (3) with the step of aging is：
Aeroge wet gel made from step (2) is stood 12~72h makes the aeroge wet gel that gelling reaction occur, and then puts again
12~72h carries out aging and further gelling reaction under the conditions of 20~80 DEG C.
9. preparation method according to claim 1, it is characterised in that：
The solvent displacement carries out in alcoholic solvent or ketone solvent；
The alcoholic solvent is selected from the group being made of methanol, ethyl alcohol, propyl alcohol and isopropanol；
The ketone solvent is selected from the group that butanone and acetone form；
The time of the solvent displacement is 1~5d.
10. preparation method according to claim 1, it is characterised in that：
The drying is supercritical drying, and preferably supercritical carbon dioxide is dried.
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| CN114889252A (en) * | 2022-04-29 | 2022-08-12 | 广东埃力生高新科技有限公司 | Aerogel-bi-component needled fiber felt composite material and preparation method and application thereof |
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