A rare earth toughened silicon airgel precursor and a preparation process of solid silicon airgel

A silicon airgel and precursor technology, which is applied in the field of airgel, can solve the problems of thermal conductivity decline and achieve the effects of improving heat resistance, shortening the replacement cycle, and compressing the process time

Active Publication Date: 2018-09-25
天津朗华睿博科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The internal structure change of silica airgel above 500°C will lead to a sharp drop in thermal conductivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Below in conjunction with embodiment, content of the present invention is described in detail:

[0041] (1) Prepare a mixed solution of silicon source and solvent

[0042] Take a water glass with a molar number of 3.0 and put it into a reaction kettle, dilute it with 2.5 times the mass of deionized water, stir at 180 rpm for 30 minutes, and filter through a 200-mesh sieve to obtain a water glass solution.

[0043] (2) Sol

[0044] Take 8mol / L sulfuric acid, add zirconium sulfate salt (the zirconium sulfate salt is calculated by its zirconia, and the molar ratio of the silicon oxide of the water glass solution is 5:100), yttrium sulfate salt (the yttrium sulfate salt is calculated by its yttrium oxide, and The molar ratio of aluminum oxide is 1:100); after mixing evenly, spray and add to the water glass solution obtained in step (1), stir rapidly at a speed of 1300 rpm while spraying, and control the pH value to 1.5 Stop spraying, and the spraying time is controlled at...

Embodiment 2

[0056] Below in conjunction with embodiment, content of the present invention is described in detail:

[0057] (1) Prepare a mixed solution of silicon source and solvent

[0058] Take a water glass with a molar number of 3.2 and put it into a reaction kettle, dilute it with deionized water of 3 times the mass, stir at 200 rpm for 30 minutes, and filter through a 200-mesh sieve to obtain a water glass solution.

[0059] (2) Sol

[0060] Get 10mol / L nitric acid, add aluminum hydrochloride (aluminum hydrochloride is calculated as aluminum oxide, and the molar ratio of aluminum oxide and silicon oxide in the water glass solution is 2:100), lanthanum hydrochloride (lanthanum hydrochloride is calculated as lanthanum oxide, and The molar ratio of alumina is 3:100); after mixing evenly, spray and add to the water glass solution obtained in step (1), and stir rapidly at a speed of 1200 rpm while spraying, and control the pH value to 2.5 , the spraying time is controlled at 100 minute...

Embodiment 3

[0072] Below in conjunction with embodiment, content of the present invention is described in detail:

[0073] (1) Prepare a mixed solution of silicon source and solvent

[0074] Take water glass with a molar number of 4.0 and put it into a reaction kettle, dilute it with 3 times the mass of deionized water, stir at 80 rpm for 30 minutes, and filter through a 200-mesh sieve to obtain a water glass solution.

[0075] (2) Sol

[0076] Take 15mol / L nitric acid, add aluminum oxalate salt (calculated as alumina, the molar ratio to silicon oxide in the water glass solution is 3:100), lanthanum oxalate salt (calculated as lanthanum oxide, the molar ratio to alumina is 6: 100); after mixing evenly, spray and join the water glass solution that step (1) obtains, carry out rapid stirring with the speed of 1800 rev / mins while spraying, control pH value till 2.5, spray time is controlled at 100 minutes ; Get the sol.

[0077] (3) Gel

[0078] Add the sodium hydroxide solution with a pH...

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Abstract

The invention discloses a preparation method of a silica aerogel precursor and solid silica aerogel. The preparation method is implemented at normal temperature and normal pressure, and is short in process time, suitable for industrialization and capable of improving the toughness and heat resistance temperature of the silica aerogel. The preparation method of the silica aerogel precursor includes the first step of preparation of a silicon source and solvent mixed solution, the second step of solation, the third step of gelation, the fourth step of ageing, the fifth step of solvent replacement and the sixth step of surface modification. The preparation method of the rare-earth-toughened solid silica aerogel includes the steps that the prepared silica aerogel precursor is put into a drying kettle, nitrogen is introduced into the drying kettle to expel oxygen till the oxygen content in the drying kettle is smaller than 3%, and then materials in the drying kettle are subjected to microwave vacuum drying; after drying, the solid powdery silica aerogel is obtained.

Description

technical field [0001] The invention relates to the technical field of airgel, in particular to a rare earth toughened silicon airgel precursor and a preparation method of solid silicon airgel. Background technique [0002] Silica airgel is a lightweight nanoporous material with controllable structure, which has many excellent properties, such as high porosity, high specific surface area, low density, low thermal conductivity, etc. [0003] The preparation of airgel usually consists of sol, gel process and supercritical drying process. In the process of sol and gel, by controlling the hydrolysis and polycondensation reaction conditions of the solution, nano-clusters of different structures are formed in the solution, and the mutual adhesion between the clusters forms a gel, and around the solid skeleton of the gel It is then filled with the remaining liquid reagent after the chemical reaction. In order to prevent the surface tension in the micropores from causing damage to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/16C01B33/143
CPCC01B33/143C01B33/157C01B33/1585C01B33/16C01P2006/12C01P2006/16C01P2006/21C01P2006/32
Inventor 郑善
Owner 天津朗华睿博科技有限公司
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