CN101913835B - Foamed ceramic reinforcing fiber aerogel insulating material and preparation method thereof - Google Patents
Foamed ceramic reinforcing fiber aerogel insulating material and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000004964 aerogel Substances 0.000 title claims abstract description 19
- 239000011810 insulating material Substances 0.000 title claims abstract description 16
- 239000012783 reinforcing fiber Substances 0.000 title claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000006260 foam Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 22
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 22
- 238000006073 displacement reaction Methods 0.000 claims description 20
- 239000011159 matrix material Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 8
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052863 mullite Inorganic materials 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- 238000001879 gelation Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 6
- 230000008595 infiltration Effects 0.000 claims description 5
- 238000001764 infiltration Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000012452 mother liquor Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 4
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 8
- 238000009413 insulation Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000008093 supporting effect Effects 0.000 abstract description 2
- 229910052681 coesite Inorganic materials 0.000 abstract 3
- 229910052906 cristobalite Inorganic materials 0.000 abstract 3
- 239000000377 silicon dioxide Substances 0.000 abstract 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract 3
- 229910052682 stishovite Inorganic materials 0.000 abstract 3
- 229910052905 tridymite Inorganic materials 0.000 abstract 3
- 230000003014 reinforcing effect Effects 0.000 abstract 2
- 230000008602 contraction Effects 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract 1
- 238000003980 solgel method Methods 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 23
- 239000000463 material Substances 0.000 description 11
- 230000006835 compression Effects 0.000 description 7
- 238000007906 compression Methods 0.000 description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 239000011240 wet gel Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- -1 silicon alkoxide Chemical class 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
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Abstract
The invention discloses a foamed ceramic reinforcing fiber aerogel insulating material and a preparation method thereof. The method comprises the following steps of: preparing a fiber silicasol-containing foamed ceramic composite material; continuously stirring the composite material by a sol-gel process so as to uniformly disperse chopped fiber in SiO2 sol; filling the composite material consisting of the fiber and the sol in the pores of porous ceramics through vacuum impregnation technology; and preparing the insulating material by processes such as aging, modifying and drying and the like for preparing aerogel. The insulating material has high intensity and low heat conduction coefficient, wherein foamed ceramics are taken as the framework of the composite material to have reinforcing and supporting effects, so that the main intensity of the composite material is borne by the foamed ceramics; the chopped fiber has certain reinforcing effect and can prevent the SiO2 aerogel from great contraction after being dried and falling from the foamed ceramics; and the SiO2 aerogel mainly has heat insulation effect by means of the superior heat-insulating property of the aerogel on the composite material.
Description
Technical field
The present invention relates to a kind of lagging material and preparation method thereof, especially relate to a kind of foamed ceramic reinforcing fiber aerogel insulating material and preparation method thereof.
Background technology
Premium propertiess such as porous foam ceramic has low density, high firmness, thermal conductivity is low, void content is big, high temperature resistant, corrosion-resistant, wear-resistant are widely used in a plurality of fields such as environmental protection, building, kiln furnitures, the energy, chemical industry, smelting.
SiO
2Gas gel has nano-porous structure, and its porosity is up to more than 90%, and density is minimum can be to 0.001g/cm
3, be to know the lightest solid material in the world at present, also be the minimum material of thermal conductivity of generally acknowledging, its thermal conductivity ratio air is also low, so it has the prospect of using very widely.
Premium propertiess such as though porous foam ceramic has low density, high firmness, thermal conductivity is low, void content is big, high temperature resistant, corrosion-resistant, wear-resistant; But its relative thermal conductivity ratio is higher; More than 0.25, restricted its popularization in practical application to a certain extent mostly; SiO
2Gas gel is because its good heat-proof quality; Be considered at present that effect of heat insulation is best in the world; The thermal insulation material that the use prospect is best; But itself have a lot of shortcomings of gas gel inherent as a kind of gas gel, low like intensity, fragility is big, cost is high has restricted its popularization in practical applications.
Existing solution has following several kinds: 1) with inorganic staple fibre and foamed ceramics compound under certain conditions (referring to 101475400A " a kind of floamed ceramic reinforcing fiber porous ceramic "), improved the intensity of foamed ceramics greatly, but its heat-proof quality is relatively poor; 2) gas gel and staple fibre is compound, promptly in the colloidal sol process, add scattered inorganic staple fibre, let fiber follow the process of whole collosol and gel; Final through supercritical fluid drying formation material (referring to No. 97106652.3 " modified nanometer heat insulating material and production technique thereof "); Though its physical strength increases, but still be difficult to satisfy the request for utilization of severe rugged environment, moreover it adopts supercritical fluid drying; Cost height, poor stability, complex equipments, and intensity is also lower; 3) fiber preform and aerogel material is compound, utilizes Infiltration Technics that colloidal sol is infiltrated as in the fiber preform, then through supercritical fluid drying (referring to 200510031952.0 " a kind of aerogel composites and preparation method thereof "); Though physical strength heat conductivility etc. improves a lot; Intensity when fiber preform is done skeleton is compared still much smaller with foamed ceramics, it adopts supercritical fluid drying in addition, complex equipments; Dangerous big, cost is high.
Summary of the invention
The object of the invention is to overcome above-mentioned defective, and foamed ceramic reinforcing fiber aerogel insulating material that a kind of physical strength is high, heat-proof quality is fabulous and preparation method thereof is provided.
The present invention is concrete to adopt following technical scheme to realize:
A kind of foamed ceramic reinforcing fiber aerogel insulating material; Its formation comprises foamed ceramics; Aerosil and fiber; Said foamed ceramics and fiber are not all participated in the reaction of collosol and gel, and foamed ceramics can be that aluminum oxide foam pottery also can be a foam silicon carbide ceramics, and what fiber adopted is mullite fiber, ceramic short fiber or spun glass.Said foamed ceramics has the ceramic foam of communicating aperture for being that precursor is produced with the organic foam, specifically through following method preparation.
The preparation method of a kind of foamed ceramic reinforcing fiber aerogel insulating material provided by the invention is that non-supercritical drying prepares, and concrete steps are following:
(1) preparation of the foamed ceramics matrix material of fibre-bearing silicon sol: with mol ratio is that 1: 4～5: 4～7 tetraethoxy, second alcohol and water mix; Stir according to ratio 1: 1～20 adding blending in of fibers of quality of fiber with the quality that is scaled aerosil according to the tetraethoxy consumption, adding sour adjust pH then is 1.5～4.5; Treating to add after its abundant hydrolysis alkali, to regulate pH be 7.0～8.5 again; Be about to form in the gel in system, foamed ceramics put into also the alcosol that contains fiber of gel not and placed vacuum unit, through the vacuum infiltration technology; Make the inner space of the abundant filled and process pottery of the colloidal sol that contains fiber; And at internal gelation, treat that gelation finishes after, promptly make said matrix material;
(2) matrix material is aging: take out above-mentioned matrix material, put into more than the aging 48h of mother liquor, said mother liquor consist of tetraethoxy: ethanol: the mol ratio of water is 1: 4～5: 4～7;
(3) modification of matrix material: taking out the matrix material after aging, is modification 12～24 hours in 1: 5～10 the modification liquid in trimethylchlorosilane and propyl carbinol volume ratio;
(4) solution displacement: after modification finishes, earlier in the displacement liquid displace of propyl carbinol and normal hexane composition, in the displacement liquid displace of pure hexane, make internal liquid fully replace again in matrix material;
(5) drying: carry out drying after the replacement completion, promptly obtain foamed ceramic reinforcing fiber aerogel insulating material.
Preferably, the mol ratio of the said tetraethoxy of step (1), ethanol, water is 1: 4: 6, and said water is deionized water, and acid is hydrochloric acid, and alkali is ammoniacal liquor.
Preferably, the said system of step (1) is about to form and is meant in the gel when adding alkali in meter 45～90s.
Preferably, the mol ratio of the said tetraethoxy of step (2), ethanol, water is 1: 4: 6.
Preferably, the condition of the said modification of step (3) is at 50 ℃ of following constant temperature 24h, the surface chemical modification that wet gel is carried out.
Preferably, the displacement liquid that said propyl carbinol of step (4) and normal hexane are formed is replaced in two stages, and the fs, 10～15h/ time, subordinate phase was replaced 2～3 times with 1: 1 displacement liquid with 3: 1 displacement liquid of volume ratio displacement 1～2 time; At last with pure hexane displacement 1～3 time, 20～30h/ time.
Preferably, the method drying that step (5) drying process adopts the normal temperature and pressure desiccating method to combine with vacuum drying technique is promptly carried out constant pressure and dry earlier, carries out vacuum-drying again, and the condition of said constant pressure and dry is: temperature 60-80 ℃, time are 6-12h; Vacuum drying condition is: vacuum tightness 52.5～84MPa, 70 ℃～150 ℃ of temperature, time 6～12h.Purpose is in order to get rid of organic liquid as much as possible as far as possible; Because these liquid have very big influence to the sealing property of vacuum dryer; Must try one's best and discharge before the vacuum-drying prerequisite, fully discharge the organic liquid and the micro-surplus water that does not displace of composite inner in the entering vacuum-drying stage for carrying out.
Preferably, the said foamed ceramics of step (1) is alumina porous ceramic or foam silicon carbide ceramics.
Preferably, the said fiber of step (1) is ceramic short fiber, mullite fiber or spun glass.
When the present invention prepared the foamed ceramics matrix material adding acid of fibre-bearing silicon sol, pH helped the abundant hydrolysis of silicon alkoxide between 1.5-4.5; PH is between 7.0-8.5 when adding alkali, and help the carrying out of gelation this moment, if the pH value is too high, it is too fast that the time is carried out in gelation, and the foamed ceramics that has little time fully to infiltrate has just been accomplished gelation.
The present invention has adopted the vacuum infiltration technology in fiber gas gel and foamed ceramics recombination process; So-called vacuum infiltration technology just is meant that fibre-bearing colloidal sol does not also form before the gel, ceramic foam is immersed wherein, because there are a lot of holes ceramic foam inside; Fibrous colloidal sol has certain viscosity; Can not the completely filled ceramic foam inner space, at this moment adopt the method that vacuumizes, make that fibrous colloidal sol was filled its space when ceramic foam internal porosity gas was discharged.
The present invention compared with prior art has following advantage:
(1) matrix material of staple fibre and colloidal sol is filled in the foamed ceramics communicating aperture, and through the compound enhancing of fiber gas gel, the intensity of the lagging material of preparing is higher, and thermal conductivity is lower.
(2) the present invention adds gas gel in foamed ceramics, and wherein foamed ceramics plays the enhancing supporting role as the skeleton of matrix material, and the main intensity of matrix material is born thus; Staple fibre has certain enhancement on the one hand, can prevent SiO on the other hand
2The dry post shrinkage of gas gel is too big, from foamed ceramics, comes off; SiO
2Gas gel relies on its superior heat-proof quality in matrix material, mainly play heat-blocking action, and therefore, the thermal insulation of this lagging material is enhanced.
(3) gas gel drying process of the present invention adopts vacuum drying technique and the method that the Air drying technology combines, and has reduced preparation cost, has shortened time of drying.
Description of drawings
Fig. 1 is preparation technology's schema of the present invention;
Fig. 2 is ceramic foam figure when not adding the fiber gas gel;
Fig. 3 is ceramic foam figure behind the interpolation fiber gas gel;
Embodiment
Below in conjunction with specific embodiment the present invention is done further concrete detailed description the in detail, but embodiment of the present invention is not limited thereto, the processing parameter for not indicating especially can carry out with reference to routine techniques.
Embodiment 1
Tetraethoxy 0.1mol, ethanol 0.4mol, water 0.6mol are mixed stirring, are to add mullite fiber (be 1.04g) at 1: 20 according to the mass ratio of fiber and gas gel, add hydrochloric acid (1mol/L) after stirring 3min; Regulating pH is 3.5, after stirring 30min under 50 ℃ of conditions, adds ammoniacal liquor (10mol/L), and regulating pH is 8.0; After stirring 60s alumina porous ceramic is put into colloidal sol; And put it into (the upward DZF-6020B of Hai'an booth scientific instrument ltd) in the vacuum unit, and vacuum tightness is 73.5Mpa, temperature is 25 ℃; Take out behind the 30min and place tetraethoxy: ethanol: the mixed solution of water; Its mol ratio is 1: 4: 6 (tetraethoxy 0.2mol, ethanol 0.8mol, water 1.2mol), takes out behind the 48h and puts into the modification liquid that contains trimethylchlorosilane and propyl carbinol, at 50 ℃ of following constant temperature 24h; Wet gel is carried out surface chemical modification, and the volume ratio of trimethylchlorosilane and propyl carbinol is 1: 7.Take out afterwards to adopt respectively and replaced with three kinds of displacement liquids of pure hexane in 3: 1,1: 1 with volume ratio; Replacement sequence is: replace 2 times with 3: 1 displacement liquid earlier; Time swap 12h, the displacement liquid that adopted again 1: 1 is replaced 3 times, and each time swap is 12h; Adopt pure hexane displacement 2 times at last, time swap is 24h; After the replacement completion, first dry 50h in 50 ℃ normal temperature and pressure loft drier is transferred to vacuum tightness and is 70 ℃ of dry 6h in the vacuum drying oven of-0.1Pa, 100 ℃ of dry 6h, 150 ℃ of dry 2h when waiting not have obvious liquid.
The intensity of general aluminum oxide foam pottery is less than 3.0MPa, and the intensity of general Mullite Ceramic Fibres is less than 0.5MPa, and the ultimate compression strength of general gas gel is extremely low, be the minimum material of intensity in the world, and the ultimate compression strength of three's matrix material is 3.2MPa.General SiO
2The thermal conductivity of gas gel is 0.013W/Km; The thermal conductivity of Mullite Ceramic Fibres is 0.1W/Km separately; The thermal conductivity of aluminum oxide foam pottery is 0.3W/Km separately, and the thermal conductivity of the aluminum oxide foam pottery fortifying fibre aerogel heat-insulating material of present embodiment preparation is 0.15W/Km.
Embodiment 2
The different of this embodiment and embodiment 1 are: adopt foam silicon carbide ceramics to replace aluminum oxide foam pottery.The ultimate compression strength of the aluminum oxide foam pottery fortifying fibre aerogel heat-insulating material of present embodiment preparation reaches 5.3MPa, and thermal conductivity is 0.13W/Km, and the foam silicon carbide ceramics thermal conductivity is 0.25W/Km separately.
Embodiment 3
The different of this embodiment and embodiment 1 are: the fiber of adding is a mullite fiber; The mass ratio of itself and gas gel is adjusted into 1: 5; The mullite fiber that promptly adds 4.06g, the ultimate compression strength that makes lagging material is 3.8MPa, thermal conductivity is 0.18W/Km.
Embodiment 4
The different of this embodiment and embodiment 3 are: adopt foam silicon carbide ceramics to replace aluminum oxide foam pottery, the ultimate compression strength of the lagging material of system is 6.0MPa, and thermal conductivity is 0.16W/Km.
Embodiment 5
The different of this embodiment and embodiment 1 are: the mol ratio of the tetraethoxy of employing, second alcohol and water is 1: 4: 4, and the ultimate compression strength of the lagging material of system is 3.15MPa, and thermal conductivity is 0.17W/Km.
Embodiment 6
The different of this embodiment and embodiment 1 are: the mol ratio of the tetraethoxy of employing, second alcohol and water is 1: 5: 7, and the ultimate compression strength of the lagging material of system is 3.22MPa, and thermal conductivity is 0.16W/Km.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a foamed ceramic reinforcing fiber aerogel insulating material is characterized in that, concrete steps are following:
(1) preparation of the foamed ceramics matrix material of fibre-bearing silicon sol: with mol ratio is that 1: 4～5: 4～7 tetraethoxy, second alcohol and water mix; Stir according to ratio 1: 1～20 adding blending in of fibers of quality of fiber with the quality that is scaled aerosil according to the tetraethoxy consumption, adding sour adjust pH then is 1.5～4.5; Treating to add after its abundant hydrolysis alkali, to regulate pH be 7.0～8.5 again; Be about to form in the gel in system, foamed ceramics put into also the alcosol that contains fiber of gel not and placed vacuum unit, through the vacuum infiltration technology; Make the inner space of the abundant filled and process pottery of the colloidal sol that contains fiber; And at internal gelation, treat that gelation finishes after, promptly make said matrix material;
(2) matrix material is aging: take out above-mentioned matrix material, put into more than the aging 48h of mother liquor, said mother liquor consist of tetraethoxy: ethanol: the mol ratio of water is 1: 4～5: 4～7;
(3) modification of matrix material: taking out the matrix material after aging, is modification 12～24 hours in 1: 5～10 the modification liquid in trimethylchlorosilane and propyl carbinol volume ratio;
(4) solution displacement: after modification finishes, earlier in the displacement liquid displace of propyl carbinol and normal hexane composition, in the displacement liquid displace of pure hexane, make internal liquid fully replace again in matrix material;
(5) drying: carry out drying after the replacement completion, promptly obtain foamed ceramic reinforcing fiber aerogel insulating material.
2. preparation method according to claim 1 is characterized in that, the mol ratio of the said tetraethoxy of step (1), ethanol, water is 1: 4: 6, and said water is deionized water, and acid is hydrochloric acid, and alkali is ammoniacal liquor.
3. preparation method according to claim 1 is characterized in that, the said system of step (1) is about to form and is meant in the gel when adding alkali in meter 45～90s.
4. preparation method according to claim 1 is characterized in that, the mol ratio of the said tetraethoxy of step (2), ethanol, water is 1: 4: 6.
5. preparation method according to claim 1 is characterized in that, the said modified condition of step (3) is at 50 ℃ of following constant temperature 24h.
6. preparation method according to claim 1; It is characterized in that the displacement liquid that said propyl carbinol of step (4) and normal hexane are formed is replaced in two stages, the fs is with 3: 1 displacement liquid of volume ratio displacement 1～2 time; 10～15h/ time, subordinate phase is replaced 2～3 times with 1: 1 displacement liquid; At last with pure hexane displacement 1～3 time, 20～30h/ time.
7. preparation method according to claim 1 is characterized in that, the said drying process of step (5) is to carry out constant pressure and dry earlier, carries out vacuum-drying again, and the condition of said constant pressure and dry is: temperature 60-80 ℃, time are 6-12h; Vacuum drying condition is: vacuum tightness 52.5～84MPa, 70 ℃～150 ℃ of temperature, time 6～12h.
8. preparation method according to claim 1 is characterized in that, the said foamed ceramics of step (1) is alumina porous ceramic or foam silicon carbide ceramics.
9. preparation method according to claim 1 is characterized in that, the said fiber of step (1) is ceramic short fiber, mullite fiber or spun glass.
10. a foamed ceramic reinforcing fiber aerogel insulating material is characterized in that, it is made by any described preparation method of claim 1～9.
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| CN110078425B (en) * | 2019-05-13 | 2021-07-13 | 天津大学 | Preparation method of light heat-insulating mullite nanofiber aerogel |
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| CN1749214A (en) * | 2005-08-01 | 2006-03-22 | 中国人民解放军国防科学技术大学 | Aerogel heat insulation composite material and its preparing method |
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