CN109225079A - A kind of high temperature resistant aeroge composite material and preparation method - Google Patents
A kind of high temperature resistant aeroge composite material and preparation method Download PDFInfo
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- CN109225079A CN109225079A CN201811361838.8A CN201811361838A CN109225079A CN 109225079 A CN109225079 A CN 109225079A CN 201811361838 A CN201811361838 A CN 201811361838A CN 109225079 A CN109225079 A CN 109225079A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The invention discloses a kind of high temperature resistant aeroge composite material and preparation methods, comprising the following steps: (1) pretreatment of fiber；(2) preparation of silicon-aluminum sol；(3) composite molding；(4) aging is dry, and 1000 DEG C ~ 1300 DEG C of resistance to temperature, 500 DEG C of thermal coefficients are lower than 0.06W/ (mK) to obtained composite material for a long time, and density is 160 ~ 240 kg/m3, 10% strain compression intensity, 0.5 ~ 0.9 MPa.The present invention is by being in advance heat-treated high-temperature fibre; effectively remove the size of fiber surface; convenient for gel complex controll; by controlling the good sial composite aerogel of the available temperature tolerance of sial ratio, by control aeroge and fiber content, available long-term resistance to 1000 DEG C ~ 1300 DEG C of aerogel composite; to meet high-temperature field application demand; the simple process and low cost, is conducive to large-scale production.
Description
Technical field
The invention belongs to high temperature resistant aeroge technical field of composite materials, specially a kind of high temperature resistant aeroge composite material
And preparation method thereof.
Background technique
With the development of aerospace cause, requirement of the aircraft to heat-barrier material is more and more harsher, traditional heat-insulated material
Expect in high temperature section heat insulation or can no longer meet in terms of mechanical property the requirement of practical application, aeroge as it is novel absolutely
Hot material, especially its nanoporous network structure and its mesopore size less than 50nm limit its internal gas
The movement of molecule causes it to can significantly reduce solid phase heat transfer, gaseous heat transfer and thermal convection so that aeroge have it is extremely low thermally conductive
Coefficient, this characteristic make aeroge have very big potentiality in terms of heat-insulation and heat-preservation, are the excellent selections of heat-insulation material.
These excellent performances are but also aeroge is widely used in multiple fields, such as high efficiency heat insulation material, catalysis
Agent and catalyst carrier and aerospace material etc..
Currently, in the aerogel heat-insulating material studied and reported both at home and abroad, most with silica aerogel material research
To be extensive, but its long-term use temperature is generally not more than 650 DEG C.Alumina aerogels not only have the various spies of general aeroge
Property, and have it is higher use temperature, be to prepare the ideal material of high temperature resistant heat insulation material, but with the continuation for using temperature
It increases, series of phase transitions can be generated, the addition of silicon can be such that its thermal stability improves, and sial composite aerogel can overcome pure dioxy
The disadvantage that SiClx aeroge effectively uses temperature low, and the high-temperature stability of alumina aerogels can be improved, and in certain journey
The immersion of colloidal sol is improved on degree.
Although silicon-aluminium binary aeroge temperature tolerance is higher, the disadvantage that pure aeroge intensity is low, brittleness is big makes it difficult to full
It is enough to practical application, in order to preferably meet the market requirement and adapt to some special dimensions, it is necessary to prepare a kind of high temperature resistant
Aerogel composite and preparation method thereof high temperature resistant and the preferable fiber reinforcement silicon-aluminium aerogel composite material of intensity, but
The size different using various types is needed during fiber draw, so that being unable to get effective control in gel recombination process
System, therefore how to prepare high-temperature fibre enhancing aerogel composite and one of have become a hot topic of research.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the existing defects, provide a kind of high temperature resistant aeroge composite material and
Preparation method can effectively solve the problems in background technique.
To achieve the above object, the invention provides the following technical scheme: a kind of high temperature resistant aeroge composite material and its system
Preparation Method, characterized by the following steps:
S1: the pretreatment of fiber:
Fiber is placed at 500 ~ 700 DEG C cooling stand-by after being heat-treated 10 ~ 60min;
S2: the preparation of silicon-aluminum sol:
Using organosilicon as silicon source, according to molar ratio organosilicon: ethyl alcohol: water: acid=1:2 ~ 20:3 ~ 5:1 × 10-5~1×10-3Respectively
It is added in container and stirs 2 hours, obtain clear silica solution；
Using alumina powder as silicon source, the acid prepared is poured into container and is stirred, alumina powder is added while stirring, then by solution
60 ~ 90 DEG C are heated to, stirs after aluminium powder is completely dissolved into solution and forms translucent micro white Aluminum sol;
S3: the compound and molding of fiber and silicon-aluminum sol:
By silica solution and Aluminum sol according to molar ratio silicon: aluminium=1 ~ 8:1 ~ 8 are poured into container and obtain silicon after 10 ~ 30min of mixing
Aluminium complex sol A liquid is stand-by;
By the good concentration of configured in advance be 0.2 ~ 2% ammonium hydroxide ethyl alcohol alkaline solution and A liquid according to volume ratio 1:0.1 ~ 1 through static state
It sprays after mixer onto the fiber blanket being heat-treated, at room temperature gel forming;
S4: aging is dry:
The gel complex material that step S3 is obtained impregnates 6 with ethyl alcohol at room temperature ~ for 24 hours, every 6h replaces an ethyl alcohol, finally uses
Supercritical fluid drying obtains aerogel composite.
As a preferred technical solution of the present invention, the composite material 1000 DEG C ~ 1300 DEG C of resistance to temperature for a long time,
500 DEG C of thermal coefficients are lower than 0.06 W/ (mK), and density is 0.16 ~ 0.24 g/cm3, 10% strain compression intensity 0.5 ~ 0.9
MPa。
As a preferred technical solution of the present invention, the fiber is high silica fiber, and the diameter of fiber is 5 ~ 15 μ
M, fibre length are 1 ~ 5cm.
As a preferred technical solution of the present invention, the silicon source is any of ethyl orthosilicate or methyl orthosilicate
It is a kind of.
As a preferred technical solution of the present invention, described prepares acid used in silicon-aluminum sol, be nitric acid or hydrochloric acid,
It is preferred that the molar ratio of nitric acid, alumina powder and nitric acid is 1:1 ~ 1.5.
As a preferred technical solution of the present invention, the aqueous slkali is the ethanol solution containing ammonia.
As a preferred technical solution of the present invention, supercritical fluid drying is Ethanol supercritical fluid drying or two
Carbonoxide supercritical fluid drying.
Beneficial effects of the present invention: the present invention effectively removes fibre by being heat-treated in advance to high-temperature fibre
The size in dimension table face is convenient for gel complex controll, compound by the control good sial of the available temperature tolerance of sial ratio
Aeroge, by control aeroge and fiber content, available long-term resistance to 1000 DEG C ~ 1300 DEG C of aerogel composite,
To meet high-temperature field application demand, which is conducive to large-scale production.
Specific embodiment
The present invention is further illustrated by the following examples, but these embodiments must not be used to explain to the present invention
The limitation of protection scope.
Embodiment one:
A kind of high temperature resistant aeroge composite material and preparation method, characterized by the following steps:
S1: the pretreatment of fiber:
Alumina silicate fiber felt is placed at 600 DEG C cooling stand-by after being heat-treated 20min；
S2: the preparation of silicon-aluminum sol:
Using ethyl orthosilicate as silicon source, according to molar ratio ethyl orthosilicate: ethyl alcohol: water: hydrochloric acid=1:8:4:8 × 10-5 adds respectively
It is stirred 2 hours into container, obtains clear silica solution；
Using alumina powder as silicon source, the nitric acid solution that the concentration prepared is 1 mol/L is poured into container and is stirred, while stirring plus
Enter alumina powder, solution is then heated to 80 DEG C, stirs after aluminium powder is completely dissolved into solution and form translucent micro white aluminium
Colloidal sol.
S3: the compound and molding of fiber and silicon-aluminum sol:
By silica solution and Aluminum sol according to molar ratio silicon: aluminium=1:4 is poured into container 30min is mixed after to obtain sial compound
Sol A liquid is stand-by:
By the good concentration of configured in advance be 0.4% ammonium hydroxide ethyl alcohol alkaline solution and A liquid according to volume ratio 1:1 through static mixer
It is sprayed in the fiber blanket being heat-treated afterwards, at room temperature gel forming.
S4: aging is dry:
The gel complex material that step S3 is obtained impregnates 12h with ethyl alcohol at room temperature, and every 6h replaces an ethyl alcohol, finally uses second
Alcohol supercritical drying obtains aerogel composite.
Obtained aerogel composite density 186kg/m3,25 DEG C of thermal coefficient 0.020W/ (m.K), 500 DEG C of thermally conductive systems
Number 0.059W/ (m.K), 10% strain compression intensity 0.6MPa.
Preferably, fiber is alumina silicate fibre, and the diameter of fiber is 5 ~ 15 μm, and fibre length is 1 ~ 5cm.
As a preferred technical solution of the present invention, the silicon source is any of ethyl orthosilicate or methyl orthosilicate
It is a kind of.
Preferably, acid used in silicon-aluminum sol is prepared, is nitric acid or hydrochloric acid, preferred nitric acid, alumina powder and nitric acid rub
You are than being 1:1 ~ 1.5.
Preferably, aqueous slkali is the ethanol solution containing ammonia.
Preferably, supercritical fluid drying is that Ethanol supercritical fluid drying or Co 2 supercritical fluid are dry.
Embodiment two:
A kind of high temperature resistant aeroge composite material and preparation method, characterized by the following steps:
S1: the pretreatment of fiber:
Alumina silicate fiber felt is placed at 600 DEG C cooling stand-by after being heat-treated 20min；
S2: the preparation of silicon-aluminum sol:
Using ethyl orthosilicate as silicon source, according to molar ratio ethyl orthosilicate: ethyl alcohol: water: hydrochloric acid=1:10:4:8 × 10-5 adds respectively
It is stirred 2 hours into container, obtains clear silica solution；
Using alumina powder as silicon source, the nitric acid solution that the concentration prepared is 1 mol/L is poured into container and is stirred, while stirring plus
Enter alumina powder, solution is then heated to 80 DEG C, stirs after aluminium powder is completely dissolved into solution and form translucent micro white aluminium
Colloidal sol.
S3: the compound and molding of fiber and silicon-aluminum sol:
By silica solution and Aluminum sol according to molar ratio silicon: aluminium=1:4 is poured into container 30min is mixed after to obtain sial compound
Sol A liquid is stand-by:
By the good concentration of configured in advance be 0.3% ammonium hydroxide ethyl alcohol alkaline solution and A liquid according to volume ratio 1:1 through static mixer
It is sprayed in the fiber blanket being heat-treated afterwards, at room temperature gel forming.
S4: aging is dry:
The gel complex material that step SS03 is obtained impregnates 12h with ethyl alcohol at room temperature, and every 6h replaces an ethyl alcohol, finally uses
Ethanol supercritical drying obtains aerogel composite.
Obtained aerogel composite density 182kg/m3,25 DEG C of thermal coefficient 0.021W/ (m.K), 500 DEG C of thermally conductive systems
Number 0.060W/ (m.K), 10% strain compression intensity 0.7MPa.
Preferably, fiber is alumina silicate fibre, and the diameter of fiber is 5 ~ 15 μm, and fibre length is 1 ~ 5cm.
Preferably, silicon source is any one of ethyl orthosilicate or methyl orthosilicate.
Preferably, acid used in silicon-aluminum sol is prepared, is nitric acid or hydrochloric acid, preferred nitric acid, alumina powder and nitric acid rub
You are than being 1:1 ~ 1.5.
Preferably, aqueous slkali is the ethanol solution containing ammonia.
Preferably, supercritical fluid drying is that Ethanol supercritical fluid drying or Co 2 supercritical fluid are dry.
Embodiment three:
A kind of high temperature resistant aeroge composite material and preparation method, characterized by the following steps:
S1: the pretreatment of fiber:
High silica fiber felt is placed at 700 DEG C cooling stand-by after being heat-treated 10min；
S2: the preparation of silicon-aluminum sol:
Using ethyl orthosilicate as silicon source, according to molar ratio ethyl orthosilicate: ethyl alcohol: water: hydrochloric acid=1:10:4:8 × 10-5 adds respectively
It is stirred 2 hours into container, obtains clear silica solution；
Using alumina powder as silicon source, the nitric acid solution that the concentration prepared is 1 mol/L is poured into container and is stirred, while stirring plus
Enter alumina powder, solution is then heated to 80 DEG C, stirs after aluminium powder is completely dissolved into solution and form translucent micro white aluminium
Colloidal sol.
S3: the compound and molding of fiber and silicon-aluminum sol:
By silica solution and Aluminum sol according to molar ratio silicon: aluminium=4:1 is poured into container 30min is mixed after to obtain sial compound
Sol A liquid is stand-by:
By the good concentration of configured in advance be 0.7% ammonium hydroxide ethyl alcohol alkaline solution and A liquid according to volume ratio 1:1 through static mixer
It is sprayed in the fiber blanket being heat-treated afterwards, at room temperature gel forming.
S4: aging is dry:
The gel complex material that step S3 is obtained impregnates 12h with ethyl alcohol at room temperature, and every 6h replaces an ethyl alcohol, finally uses second
Alcohol supercritical drying obtains aerogel composite.
Obtained aerogel composite density 182kg/m3,25 DEG C of thermal coefficient 0.020W/ (m.K), 500 DEG C of thermally conductive systems
Number 0.059W/ (m.K), 10% strain compression intensity 0.8MPa.
Preferably, fiber is high silica fiber, and the diameter of fiber is 5 ~ 15 μm, and fibre length is 1 ~ 5cm.
Preferably, silicon source is any one of ethyl orthosilicate or methyl orthosilicate.
Preferably, acid used in silicon-aluminum sol is prepared, is nitric acid or hydrochloric acid, preferred nitric acid, alumina powder and nitric acid rub
You are than being 1:1 ~ 1.5.
Preferably, aqueous slkali is the ethanol solution containing ammonia.
Preferably, supercritical fluid drying is that Ethanol supercritical fluid drying or Co 2 supercritical fluid are dry.
Example IV:
A kind of high temperature resistant aeroge composite material and preparation method, characterized by the following steps:
S1: the pretreatment of fiber:
High silica fiber felt is placed at 600 DEG C cooling stand-by after being heat-treated 30min；
S2: the preparation of silicon-aluminum sol:
Using ethyl orthosilicate as silicon source, according to molar ratio ethyl orthosilicate: ethyl alcohol: water: hydrochloric acid=1:10:4:8 × 10-5 adds respectively
It is stirred 2 hours into container, obtains clear silica solution；
Using alumina powder as silicon source, the nitric acid solution that the concentration prepared is 1 mol/L is poured into container and is stirred, while stirring plus
Enter alumina powder, solution is then heated to 80 DEG C, stirs after aluminium powder is completely dissolved into solution and form translucent micro white aluminium
Colloidal sol.
S3: the compound and molding of fiber and silicon-aluminum sol:
By silica solution and Aluminum sol according to molar ratio silicon: aluminium=1:4 is poured into container 30min is mixed after to obtain sial compound
Sol A liquid is stand-by:
By the good concentration of configured in advance be 0.3% ammonium hydroxide ethyl alcohol alkaline solution and A liquid according to volume ratio 1:1 through static mixer
It is sprayed in the fiber blanket being heat-treated afterwards, at room temperature gel forming.
S4: aging is dry:
The gel complex material that step S3 is obtained impregnates 12h with ethyl alcohol at room temperature, and every 6h replaces an ethyl alcohol, finally uses second
Alcohol supercritical drying obtains aerogel composite.
Obtained aerogel composite density 186kg/m3,25 DEG C of thermal coefficient 0.021W/ (m.K), 500 DEG C of thermally conductive systems
Number 0.060W/ (m.K), 10% strain compression intensity 0.6MPa.
Preferably, fiber is high silica fiber, and the diameter of fiber is 5 ~ 15 μm, and fibre length is 1 ~ 5cm.
As a preferred technical solution of the present invention, the silicon source is any of ethyl orthosilicate or methyl orthosilicate
It is a kind of.
Preferably, acid used in silicon-aluminum sol is prepared, is nitric acid or hydrochloric acid, preferred nitric acid, alumina powder and nitric acid rub
You are than being 1:1 ~ 1.5.
Preferably, aqueous slkali is the ethanol solution containing ammonia.
Preferably, supercritical fluid drying is that Ethanol supercritical fluid drying or Co 2 supercritical fluid are dry.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (7)
1. a kind of high temperature resistant aeroge composite material and preparation method, characterized by the following steps:
S1: the pretreatment of fiber:
Fiber is placed at 500 ~ 700 DEG C cooling stand-by after being heat-treated 10 ~ 60min;
S2: the preparation of silicon-aluminum sol:
Using organosilicon as silicon source, according to molar ratio organosilicon: ethyl alcohol: water: acid=1:2 ~ 20:3 ~ 5:1 × 10-5~1×10-3Respectively plus
It is stirred 2 hours into container, obtains clear silica solution；
Using alumina powder as silicon source, the acid prepared is poured into container and is stirred, alumina powder is added while stirring, then by solution
60 ~ 90 DEG C are heated to, stirs after aluminium powder is completely dissolved into solution and forms translucent micro white Aluminum sol;
S3: the compound and molding of fiber and silicon-aluminum sol:
By silica solution and Aluminum sol according to molar ratio silicon: aluminium=1 ~ 8:1 ~ 8 are poured into container and obtain silicon after 10 ~ 30min of mixing
Aluminium complex sol A liquid is stand-by;
By the good concentration of configured in advance be 0.2 ~ 2% ammonium hydroxide ethyl alcohol alkaline solution and A liquid according to volume ratio 1:0.1 ~ 1 through static state
It sprays after mixer onto the fiber blanket being heat-treated, at room temperature gel forming;
S4: aging is dry:
The gel complex material that step S3 is obtained impregnates 6 with ethyl alcohol at room temperature ~ for 24 hours, every 6h replaces an ethyl alcohol, finally uses
Supercritical fluid drying obtains aerogel composite.
2. a kind of high temperature resistant aeroge composite material and preparation method according to claim 1, which is characterized in that institute
The composite material stated 1000 DEG C ~ 1300 DEG C of resistance to temperature for a long time, 500 DEG C of thermal coefficients are lower than 0.06 W/ (mK), and density is 0.16 ~
0.24 g/cm3, 10% strain compression intensity, 0.5 ~ 0.9 MPa.
3. a kind of high temperature resistant aeroge composite material and preparation method according to claim 1, which is characterized in that institute
The fiber stated is high silica fiber, and the diameter of fiber is 5 ~ 15 μm, and fibre length is 1 ~ 5cm.
4. a kind of high temperature resistant aeroge composite material and preparation method according to claim 1, which is characterized in that institute
The silicon source stated is any one of ethyl orthosilicate or methyl orthosilicate.
5. a kind of high temperature resistant aeroge composite material and preparation method according to claim 1, which is characterized in that institute
That states prepares acid used in silicon-aluminum sol, is nitric acid or hydrochloric acid, preferred nitric acid, the molar ratio of alumina powder and nitric acid be 1:1 ~
1.5。
6. a kind of high temperature resistant aeroge composite material and preparation method according to claim 1, which is characterized in that institute
The aqueous slkali stated is the ethanol solution containing ammonia.
7. a kind of high temperature resistant aeroge composite material and preparation method according to claim 1, which is characterized in that super
Supercritical fluid drying is that Ethanol supercritical fluid drying or Co 2 supercritical fluid are dry.
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Cited By (7)
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| CN112174579A (en) * | 2019-07-04 | 2021-01-05 | 福建纳美特材料科技有限公司 | Aerogel composite thermal insulation pipe shell and preparation method thereof |
| CN112778017A (en) * | 2021-01-30 | 2021-05-11 | 山东工业陶瓷研究设计院有限公司 | Ceramic fiber composite aerogel thermal insulation material and preparation method thereof |
| CN113248277A (en) * | 2021-07-01 | 2021-08-13 | 江苏脒诺甫纳米材料有限公司 | Production process of high-temperature-resistant nano porous material |
| CN113402253A (en) * | 2021-07-22 | 2021-09-17 | 浙江圣润纳米科技有限公司 | High-temperature-treated high-tensile-resistance aerogel composite material and preparation method thereof |
| CN113731308A (en) * | 2021-09-02 | 2021-12-03 | 浙江岩谷科技有限公司 | Preparation method of ceramic fiber paper-silica aerogel heat insulation composite material |
| CN115180918A (en) * | 2022-07-31 | 2022-10-14 | 广东省公路建设有限公司湾区特大桥养护技术中心 | Enhanced high-silica fiber composite aerogel fireproof material and preparation method thereof |
| CN115925386A (en) * | 2022-12-28 | 2023-04-07 | 江苏汉信天诚新材料有限公司 | Low-density silicon dioxide aerogel coiled material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112174579A (en) * | 2019-07-04 | 2021-01-05 | 福建纳美特材料科技有限公司 | Aerogel composite thermal insulation pipe shell and preparation method thereof |
| CN112778017A (en) * | 2021-01-30 | 2021-05-11 | 山东工业陶瓷研究设计院有限公司 | Ceramic fiber composite aerogel thermal insulation material and preparation method thereof |
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| CN113402253A (en) * | 2021-07-22 | 2021-09-17 | 浙江圣润纳米科技有限公司 | High-temperature-treated high-tensile-resistance aerogel composite material and preparation method thereof |
| CN113731308A (en) * | 2021-09-02 | 2021-12-03 | 浙江岩谷科技有限公司 | Preparation method of ceramic fiber paper-silica aerogel heat insulation composite material |
| CN115180918A (en) * | 2022-07-31 | 2022-10-14 | 广东省公路建设有限公司湾区特大桥养护技术中心 | Enhanced high-silica fiber composite aerogel fireproof material and preparation method thereof |
| CN115925386A (en) * | 2022-12-28 | 2023-04-07 | 江苏汉信天诚新材料有限公司 | Low-density silicon dioxide aerogel coiled material and preparation method thereof |
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Application publication date: 20190118 |