CN101691293B - Method for preparing heat-insulation materials from nano-silica filled non-graphitized carbon foam - Google Patents
Method for preparing heat-insulation materials from nano-silica filled non-graphitized carbon foam Download PDFInfo
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- CN101691293B CN101691293B CN2009103068715A CN200910306871A CN101691293B CN 101691293 B CN101691293 B CN 101691293B CN 2009103068715 A CN2009103068715 A CN 2009103068715A CN 200910306871 A CN200910306871 A CN 200910306871A CN 101691293 B CN101691293 B CN 101691293B
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- carbon foam
- graphitized carbon
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- silica filled
- lagging material
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Abstract
The invention provides a method for preparing heat-insulation materials from nano-silica filled non-graphitized carbon foam, and relates to a method for applying non-graphitized carbon foam to the preparation of heat-insulation materials. The method solves the problem that the prior aerogel is poor in mechanical properties and cannot be used as independent blocks. The method comprises: allowing mixture of tetraethyl orthosilicate, deionized water and absolute ethanolto react to 10 to 15 minutes under acidic and alkaline conditions respectively; soaking obtained alcogel in tetraethyl ortho-silicate ethanol solution; washing the obtained product with deionized water to obtain SiO2 sol-gel; immersing non-graphitized carbon foam in the SiO2 sol-gel; drying the obtained product; and obtaining nano-silica filled non-graphitized carbon foam heat-insulation composite material. The heat-insulation material obtained by the method can be used as independent blocks, is strong in mechanical properties compared with aerogel, and has the heat-insulation temperature between 1,200 and 1,300 DEG C.
Description
Technical field
The present invention relates to a kind of method that non-graphitized Carbon foam prepares lagging material of using.
Background technology
High hypersonic aircraft is in the process of high speed earth reentry when striding atmospheric layer; Its nose cone big area windward side, positions such as engine jet pipe even tail cone all will suffer violent pneumatic heating, especially sky and space plane inevitably; Also to receive more serious pneumatic heating in the rising cruising flight stage; Because sky and space plane is power with the airbreathing motor, must in dense atmosphere below 50 kilometers, quicken flight, the speed of entering the orbit is more up to 25 Mach numbers.Therefore, anti-/ heat-insulating problem becomes the major issue in the course of new aircraft triturating.Gas gel has excellent heat-proof quality as a kind of superinsulation material, but the non-constant of its mechanical property can't independently become piece to use.Though and the heat insulation temperature of the limit of common high alumina matter heat-insulation blanket is up to 1260 ℃, its density is generally than higher, and its compacting under mechanical load function easily, thereby sharply increases its net heat conductance, influences its heat-proof quality.
Summary of the invention
Technical problem to be solved by this invention is for the problem that solves existing gas gel bad mechanical property, can't independently become piece to use, and provides a kind of nano-silica filled non-graphitized Carbon foam to prepare the method for lagging material.
The method that the nano-silica filled non-graphitized Carbon foam of the present invention prepares lagging material is following: one, tetraethoxy, deionized water and absolute ethyl alcohol and stirring are mixed 10min～15min; Obtain mixture; Then mixture is adopted heating in water bath to 50 ℃～55 ℃; And then to add concentration be that the hydrochloric acid of 0.2mol/L～0.3mol/L continues under 50 ℃～55 ℃ condition, to react 10min～15min, drops to room temperature then, adds volumetric concentration again and be 98% ammoniacal liquor; Reaction 10min～15min obtains alcogel; Two, alcogel was soaked under temperature is 50 ℃～55 ℃ condition in the aged solution 6 hours～10 hours, uses deionized water wash 10min then; Three, the process 3～4 times of repeating step two obtains SiO
2Collosol and gel; Four, non-graphitized Carbon foam is immersed in SiO
2In the collosol and gel 4～6 hours, SiO
2The collosol and gel liquid level did not have non-graphitized Carbon foam 1mm～5mm, was under 150 ℃～200 ℃ the condition dry 72～80 hours at normal pressure, drying temperature then, promptly got nano-silica filled non-graphitized Carbon foam heat-insulation composite material; Tetraethoxy in the step 1 wherein: deionized water: the mol ratio of absolute ethyl alcohol is 1: 6: 13; The mass ratio of hydrochloric acid and mixture is 4～5: 100 in the step 1; The mass ratio of ammoniacal liquor and mixture is 0.1～0.2: 100 in the step 1; Aged solution described in the step 2 is that the tetraethyl orthosilicate volumetric concentration is 70%～75% tetraethyl orthosilicate ethanolic soln.
The nanometer titanium dioxide silica aerogel has filled up the hole of non-graphitized Carbon foam in the lagging material that employing the inventive method obtains; The complicated column ligament of non-graphitized Carbon foam network structure has overcome aerosil fragility defective big, easy to crack as rigid support on the one hand; Making lagging material of the present invention compare mechanical property with gas gel strengthens; Can also absorb and reflect on the other hand through aerosil institute radiating heat; The aerosil filling has weakened the thermal convection effect in the hole of Carbon foam; The column ligament of non-graphitized Carbon foam can improve again aerosil when high temperature to thermal-radiating complete permeability, thereby improved the heat-proof quality of the lagging material of nano-silica filled non-graphitized Carbon foam preparation, and can independently become piece to use.The heat insulation temperature of lagging material of the nano-silica filled non-graphitized Carbon foam preparation of the inventive method gained is 1200 ℃～1300 ℃.
Description of drawings
Fig. 1 is the stereoscan photograph of non-graphitized Carbon foam; Fig. 2 is the stereoscan photograph of nano-silica filled non-graphitized Carbon foam heat-insulation composite material.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method that nano-silica filled non-graphitized Carbon foam prepares lagging material in this embodiment is following: one, tetraethoxy, deionized water and absolute ethyl alcohol and stirring are mixed 10min～15min; Obtain mixture; Then mixture is adopted heating in water bath to 50 ℃～55 ℃; And then to add concentration be that the hydrochloric acid of 0.2mol/L～0.3mol/L continues under 50 ℃～55 ℃ condition, to react 10min～15min, drops to room temperature then, adds volumetric concentration again and be 98% ammoniacal liquor; Reaction 10min～15min obtains alcogel; Two, alcogel was soaked under temperature is 50 ℃～55 ℃ condition in the aged solution 6 hours～10 hours, uses deionized water wash 10min then; Three, the process 3～4 times of repeating step two obtains SiO
2Collosol and gel; Four, non-graphitized Carbon foam is immersed in SiO
2In the collosol and gel 4～6 hours, SiO
2The collosol and gel liquid level did not have non-graphitized Carbon foam 1mm～5mm, was under 150 ℃～200 ℃ the condition dry 72～80 hours at normal pressure, drying temperature then, promptly got nano-silica filled non-graphitized Carbon foam heat-insulation composite material; Tetraethoxy in the step 1 wherein: deionized water: the mol ratio of absolute ethyl alcohol is 1: 6: 13; The mass ratio of hydrochloric acid and mixture is 4～5: 100 in the step 1; The mass ratio of ammoniacal liquor and mixture is 0.1～0.2: 100 in the step 1; Aged solution described in the step 2 is that the tetraethyl orthosilicate volumetric concentration is 70%～75% tetraethyl orthosilicate ethanolic soln.
Can know by Fig. 1 (stereoscan photograph of non-graphitized Carbon foam) and Fig. 2 (stereoscan photograph of nano-silica filled non-graphitized Carbon foam heat-insulation composite material); The nanometer titanium dioxide silica aerogel has filled up the hole of non-graphitized Carbon foam; The complicated column ligament of non-graphitized Carbon foam network structure has overcome aerosil fragility defective big, easy to crack as rigid support on the one hand; Can also absorb and reflect on the other hand through aerosil institute radiating heat; The aerosil filling has weakened the thermal convection effect in the hole of Carbon foam; The column ligament of non-graphitized Carbon foam can improve again aerosil when high temperature to thermal-radiating complete permeability, thereby improved the heat-proof quality of the lagging material of nano-silica filled non-graphitized Carbon foam preparation.
The heat insulation temperature of lagging material of the nano-silica filled non-graphitized Carbon foam preparation of this embodiment gained is 1200 ℃～1300 ℃.
Embodiment two: this embodiment and embodiment one are different is that the mean pore size of the non-graphitized Carbon foam described in the step 3 is 500 μ m～600 μ m.Other is identical with embodiment one.
Embodiment three: this embodiment is different with embodiment one or two is in the step 1 temperature of mixture to be heated to 51 ℃～54 ℃.Other is identical with embodiment one or two.
Embodiment four: this embodiment and embodiment one to three are different is in the step 1 temperature of mixture to be heated to 53.Other is identical with embodiment one to three.
Embodiment five: this embodiment and embodiment one to four are different is that the concentration of hydrochloric acid in the step 1 is 0.25mol/L.Other is identical with embodiment one to four.
Embodiment six: this embodiment and embodiment one to five are different be in the step 2 in the tetraethyl orthosilicate ethanolic soln volumetric concentration of tetraethyl orthosilicate be that 71%～74% other is identical with embodiment one to five.
Embodiment seven: this embodiment and embodiment one to six are different be in the step 2 in the tetraethyl orthosilicate ethanolic soln volumetric concentration of tetraethyl orthosilicate be 73%.Other and embodiment one to six phase are together.
Embodiment eight: what this embodiment and embodiment one to seven were different is that bath temperature is 53 ℃ in the step 2.Other is identical with embodiment one to seven.
Embodiment nine: what this embodiment and embodiment one to eight were different is that drying temperature is 160 ℃～180 ℃ in the step 4.Other is identical with embodiment one to eight.
Embodiment ten: what this embodiment and embodiment one to nine were different is that drying temperature is 170 ℃ in the step 4.Other is identical with embodiment one to nine.
Claims (10)
1. nano-silica filled non-graphitized Carbon foam prepares the method for lagging material; It is characterized in that the method that nano-silica filled non-graphitized Carbon foam prepares lagging material is following: one, tetraethoxy, deionized water and absolute ethyl alcohol and stirring are mixed 10min～15min; Obtain mixture, then mixture is adopted heating in water bath to 50 ℃～55 ℃, and then to add concentration be that the hydrochloric acid of 0.2mol/L～0.3mol/L continues under 50 ℃～55 ℃ condition, to react 10min～15min; Drop to room temperature then; Add volumetric concentration again and be 98% ammoniacal liquor, reaction 10min～15min obtains alcogel; Two, alcogel was soaked under temperature is 50 ℃～55 ℃ condition in the aged solution 6 hours～10 hours, uses deionized water wash 10min then; Three, the process 3～4 times of repeating step two obtains SiO
2Collosol and gel; Four, non-graphitized Carbon foam is immersed in SiO
2In the collosol and gel 4～6 hours, SiO
2The collosol and gel liquid level did not have non-graphitized Carbon foam 1mm～5mm, was under 150 ℃～200 ℃ the condition dry 72～80 hours at normal pressure, drying temperature then, promptly got nano-silica filled non-graphitized Carbon foam heat-insulation composite material; Tetraethoxy in the step 1 wherein: deionized water: the mol ratio of absolute ethyl alcohol is 1: 6: 13; The mass ratio of hydrochloric acid and mixture is 4～5: 100 in the step 1; The mass ratio of ammoniacal liquor and mixture is 0.1～0.2: 100 in the step 1; Aged solution described in the step 2 is that the tetraethyl orthosilicate volumetric concentration is 70%～75% tetraethyl orthosilicate ethanolic soln.
2. nano-silica filled non-graphitized Carbon foam according to claim 1 prepares the method for lagging material, and the mean pore size that it is characterized in that the non-graphitized Carbon foam described in the step 3 is 500 μ m～600 μ m.
3. nano-silica filled non-graphitized Carbon foam according to claim 1 and 2 prepares the method for lagging material, it is characterized in that in the step 1 temperature of mixture is heated to 51 ℃～54 ℃.
4. nano-silica filled non-graphitized Carbon foam according to claim 1 and 2 prepares the method for lagging material, it is characterized in that in the step 1 temperature of mixture is heated to 53 ℃.
5. nano-silica filled non-graphitized Carbon foam according to claim 3 prepares the method for lagging material, and the concentration that it is characterized in that hydrochloric acid in the step 1 is 0.25mol/L.
6. the method for preparing lagging material according to claim 1,2 or 5 described nano-silica filled non-graphitized Carbon foam is characterized in that in the step 2 that the volumetric concentration of tetraethyl orthosilicate is 71%～74% in the tetraethyl orthosilicate ethanolic soln.
7. the method for preparing lagging material according to claim 1,2 or 5 described nano-silica filled non-graphitized Carbon foam is characterized in that in the step 2 that the volumetric concentration of tetraethyl orthosilicate is 73% in the tetraethyl orthosilicate ethanolic soln.
8. nano-silica filled non-graphitized Carbon foam according to claim 6 prepares the method for lagging material, it is characterized in that bath temperature is 53 ℃ in the step 2.
9. prepare the method for lagging material according to claim 1,2,5 or 8 described nano-silica filled non-graphitized Carbon foam, it is characterized in that drying temperature is 160 ℃～180 ℃ in the step 4.
10. prepare the method for lagging material according to claim 1,2,5 or 8 described nano-silica filled non-graphitized Carbon foam, it is characterized in that drying temperature is 170 ℃ in the step 4.
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| CN2009103068715A CN101691293B (en) | 2009-09-11 | 2009-09-11 | Method for preparing heat-insulation materials from nano-silica filled non-graphitized carbon foam |
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| CN2009103068715A CN101691293B (en) | 2009-09-11 | 2009-09-11 | Method for preparing heat-insulation materials from nano-silica filled non-graphitized carbon foam |
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| CN101691293B true CN101691293B (en) | 2012-08-22 |
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| CN102616767A (en) * | 2012-03-28 | 2012-08-01 | 福州大学 | Foam carbon composite material and preparation method thereof |
| CN106747628B (en) * | 2017-02-22 | 2020-02-04 | 南京航空航天大学 | High-temperature-resistant foam-reinforced SiO2Aerogel thermal insulation material and preparation method thereof |
| CN112250472B (en) * | 2020-10-16 | 2021-09-03 | 上海航翼高新技术发展研究院有限公司 | Preparation method of pectin-based aerogel-carbon foam aerospace composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041432A (en) * | 2007-03-20 | 2007-09-26 | 中国科学院山西煤炭化学研究所 | Preparation method of lightweight heat-proof phenolic resin radical foam charcoal |
| CN101182159A (en) * | 2007-11-16 | 2008-05-21 | 烟台鲁航炭材料科技有限公司 | Carbon foam ultrahigh-temperature hard insulating material and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041432A (en) * | 2007-03-20 | 2007-09-26 | 中国科学院山西煤炭化学研究所 | Preparation method of lightweight heat-proof phenolic resin radical foam charcoal |
| CN101182159A (en) * | 2007-11-16 | 2008-05-21 | 烟台鲁航炭材料科技有限公司 | Carbon foam ultrahigh-temperature hard insulating material and production method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 肖正浩等.泡沫炭的研究进展.《化工进展》.2008,第27卷(第4期),1-10. * |
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