Preparation method of mullite-fibrofelt-reinforced SiO2-Al2O3 aerogel composite heat-insulating material

A technology of mullite fiber and composite material is applied in the field of preparation of mullite fiber felt reinforced SiO2-Al2O3 aerogel composite thermal insulation material, which can solve the problems of reduced thermal insulation performance, complicated preparation process, poor temperature resistance and the like , to achieve the effect of increasing operability and controllability, simplifying process steps and reducing production costs

Inactive Publication Date: 2015-08-19
NANJING UNIV OF TECH
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

SiO 2 The room temperature thermal conductivity of airgel is as low as 0.013W m -1 K -1 , but the temperature resistance of this material is poor, and the pore structure will collapse seriously above 800 °C, and the heat insulation performance will drop sharply
al 2 o 3 The temperature resistance of airgel is high, up to 1000 °C, but the material is prone to crystal transformation in high temperature environment, and the high temperature thermal conductivity is high, so through the Al 2 o 3 Aerogels are doped with silicon to prepare SiO 2 -Al 2 o 3 Composite airgel has both high temperature resistance and low high temperature thermal conductivity
Feng Jian and others from the University of National Defense Science and Technology used aluminum sec-butoxide as the aluminum source and tetraethyl orthosilicate as the silicon source to successfully prepare a compound with a specific surface area of ​​116m at 1200°C. 2 / g SiO 2 -Al 2 o 3 composite aerogels, and systematically studied the effect of silicon content on SiO 2 -Al 2 o 3 However, in this method, the aluminum source and the silicon source need to be prepared separately to fully hydrolyze, and the organoaluminum alcohol itself is expensive, and the hydrolysis speed of the organoaluminum alcohol is relatively fast, and the hydrolysis process is easy A colloidal precipitate is produced, and methanol and glacial acetic acid need to be introduced in the subsequent steps, and the preparation process is relatively complicated

Method used

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  • Preparation method of mullite-fibrofelt-reinforced SiO2-Al2O3 aerogel composite heat-insulating material
  • Preparation method of mullite-fibrofelt-reinforced SiO2-Al2O3 aerogel composite heat-insulating material
  • Preparation method of mullite-fibrofelt-reinforced SiO2-Al2O3 aerogel composite heat-insulating material

Examples

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example 1

[0030] The mullite fiber felt was placed in a muffle furnace, raised to 600°C at a rate of 2°C / min and kept for 2 hours, then naturally cooled to room temperature to obtain a surface-pretreated mullite fiber felt. Mix aluminum chloride hexahydrate, tetraethyl orthosilicate, ethanol, and water uniformly at a molar ratio of 1:0.125:15:50, and stir evenly at a temperature of 50°C for 2 hours to hydrolyze the components to obtain silicon aluminum Composite sol. After the silicon-aluminum composite sol is cooled to 25°C, add a certain amount of propylene oxide, wherein the molar ratio of propylene oxide to aluminum chloride is 8, then continue to stir for 10 minutes and then slowly inject it into the mullite fiber mat . The mullite fiber mat reinforced SiO 2 -Al 2 o 3 After the composite wet gel was left at room temperature for 24 hours, ethanol was added to age it, and ethanol was added to replace it in an oven at 30°C for 8 times, 24 hours each time. Finally, the wet gel com...

example 2

[0032] The mullite fiber felt was placed in a muffle furnace, raised to 700°C at a rate of 4°C / min and kept for 2 hours, then naturally cooled to room temperature to obtain a surface-pretreated mullite fiber felt. Mix aluminum chloride hexahydrate, tetraethyl orthosilicate, ethanol, and water uniformly at a molar ratio of 1:0.25:12:40, and stir evenly at a temperature of 60°C for 1 hour to hydrolyze the components to obtain silicon aluminum Composite sol. After the silicon-aluminum composite sol is cooled to 25°C, add a certain amount of cis-2,3 butylene oxide, wherein the molar ratio of cis-2,3 butylene oxide to aluminum chloride is 7, and then continue After stirring for 30 minutes, slowly inject it into the mullite fiber felt. The mullite fiber mat reinforced SiO 2 -Al 2 o 3 After the composite wet gel was left at room temperature for 16 hours, n-hexane was added to age it, and ethanol was added to replace it in an oven at 40°C for 5 times, 24 hours each time. Finally,...

example 3

[0034] The mullite fiber felt was placed in a muffle furnace, raised to 600°C at a rate of 6°C / min and kept for 3 hours, then naturally cooled to room temperature to obtain a surface-pretreated mullite fiber felt. Mix aluminum nitrate nonahydrate, tetraethyl orthosilicate, ethanol, and water uniformly at a molar ratio of 1:0.33:9:45, and then stir evenly at a temperature of 45°C for 3 hours to hydrolyze the components to obtain a silicon-aluminum composite Sol. After the silicon-aluminum composite sol is cooled to 25°C, add a certain amount of glycidol, wherein the molar ratio of glycidol to aluminum nitrate is 10, then continue to stir for 40 minutes and slowly inject it into the mullite fiber mat Inside. The mullite fiber mat reinforced SiO 2 -Al 2 o 3 After the composite wet gel was placed at room temperature for 24 hours, ethanol was added to age it, and ethanol was added to replace it in an oven at 40°C for 5 times, 24 hours each time. Finally, the wet gel composite ...

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Abstract

The invention relates to a preparation method of a mullite-fibrofelt-reinforced SiO2-Al2O3 aerogel composite heat-insulating material, which comprises the following steps: by using surface-pretreated mullite fibrofelt as a reinforcer, tetraethyl orthosilicate as a silicon source, cheap inorganic aluminum salt as an aluminum source and epoxide as a network formation agent, uniformly mixing, and carrying out sol-gel, aging and supercritical drying to obtain the mullite-fibrofelt-reinforced SiO2-Al2O3 aerogel composite heat-insulating material. In the preparation process, no catalyst is needed, and a one-step method is adopted to greatly optimize the preparation technique. Thus, the heat-insulating material has the advantages of low cost, smooth surface and controllable thickness, and can resist the temperature of 1200 DEG C in an air atmosphere. The room temperature thermal conductivity is 0.023-0.027 W.m<-1>K<-1>, and the apparent density is 0.18-0.22 g/cm<3>. The method has the advantages of simple materials, low cost and simple technique, is simple to operate in the technical process, and can easily implement large-scale production.

Description

technical field [0001] The invention belongs to the field of preparation technology of nanoporous materials, and relates to a mullite fiber mat reinforced SiO with high temperature resistance and low thermal conductivity 2 -Al 2 o 3 The invention discloses a preparation method of an airgel composite thermal insulation material. Background technique [0002] With the development of aerospace technology, the flight speed of various aircraft is developing towards a high Mach number, and the severe friction with the atmosphere during the flight will cause a strong aerodynamic heating problem. In order to make it fly faster and for a longer flight time, while ensuring the safety of internal personnel and related equipment, high-efficiency heat insulation materials with high temperature resistance and low thermal conductivity must be used. [0003] Airgel is a nanoporous material formed by the aggregation of nanoparticles. The high porosity of the airgel material can reduce the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B30/02
Inventor 沈晓冬吴晓栋崔升邵高峰
Owner NANJING UNIV OF TECH
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