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In-situ composite silicon-based multibasic oxide oxide aerogel material and preparation method thereof

An in-situ composite and oxide sol technology, applied in chemical instruments and methods, chemical/physical processes, colloid chemistry, etc., can solve problems such as difficult in-situ composite, few types of metal oxides, damage to the cornea and conjunctiva, etc. To achieve the effect of improving its own performance, improving catalytic performance and improving thermal insulation performance

Inactive Publication Date: 2015-09-30
金承黎
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The above patents all involve the in-situ composite preparation of binary or multi-element airgel materials using silicon airgel technology. The disclosure and implementation of the above-mentioned patents will facilitate the development of high-quality multi-element airgel materials, but there are still obvious problems. One is that the silicon sources used in the prior art are basically organic silicon esters such as tetraethyl orthosilicate, and the price of organic silicon esters is relatively high, which restricts the production cost of airgel; the other is that the reaction environment of the prior art is basically alcohol-containing system, because most metal salts are insoluble in ethanol, and directly produce precipitation, which severely restricts the available types of metal salts and the effect of addition, and it is difficult to achieve ideal in-situ recombination; third, the existing technology is mainly aimed at silicon oxide and Binary or ternary composites of titanium oxide, aluminum oxide, and zirconium oxide involve fewer types of metal oxides, and cannot become a general multi-element airgel preparation method; fourth, the existing technology is to make the added metal Oxide gels generally use propylene oxide, a flammable and explosive toxic substance that is irritating to mucous membranes and skin, can damage the cornea and conjunctiva, cause respiratory pain, skin burns and swelling, and even tissue necrosis

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Weigh 80 g of sodium water glass (sodium silicate) with a modulus of 3.3, add 60 g of pure water and stir evenly to obtain diluted water glass solution 1. Take by weighing 20 g of sulfuric acid with a concentration of 40%wt, then add the diluted water glass solution 1 into the sulfuric acid while stirring to obtain the acidified water glass solution 2. 20 g of solid zirconium sulfate powder and 3 g of titanyl sulfate powder were weighed and dissolved in 50 g of pure water to obtain a water-soluble metal salt mixture solution 3 . Mix the solution 3 with the solution 2, add dropwise 1%wt sodium hydroxide, adjust the pH to 3.2, and obtain the salt-containing multiple oxide sol solution 4. Add 350 g of 95%wt ethanol to solution 4. Use a centrifugal filter to remove the sodium sulfate precipitate in the sol to obtain a multi-component oxide sol. Ammonia water with a concentration of 1%wt was added dropwise to the multi-component oxide sol, and the pH was adjusted to 4.0. A...

Embodiment 2

[0060] Weigh 80 g of potassium water glass (potassium silicate) with a modulus of 3.6, add 80 g of pure water and stir evenly to obtain diluted water glass solution 1. Weigh 12 g of solid zinc sulfate powder and 6 g of manganese sulfate and dissolve them in 80 g of pure water to obtain solution 2. Add the solution 2 dropwise to the solution 1 while stirring, and when the pH is 11, the salt-containing multiple oxide sol solution 3 is obtained. Mix 40% with propanol solution at a mass ratio of 1:10 to obtain 150ml of acidic organic solvent 4. Add the solution 3 dropwise to the organic solvent 4 while stirring. When the pH is 3.3, stop the dropwise addition, filter the resulting potassium sulfate precipitate to obtain the multi-component oxide sol 5, add 1% sodium hydroxide dropwise to adjust the pH value to 4.1, and stand still Gel after 50min. The gel was aged in 500 ml propanol for 1 day. Continue to add 10 g of dimethyldiethoxysilane to the propanol liquid, and carry out h...

Embodiment 3

[0062] Weigh 80g of lithium water glass (lithium silicate) with a modulus of 3.3, 5g of gallium hydroxide powder, 4g of bismuth hydroxide, 3g of tin hydroxide, and 1g of indium hydroxide, and add them to 200g of sodium hydroxide solution with a mass fraction of 50%. , stirred at 65°C for 1 h to obtain solution 1. Nitric acid with a mass fraction of 100% was added dropwise to solution 1 until the pH value was 8.2 to obtain salt-containing multiple oxide sol solution 2. Add 0.3 g of BYC-8440 polyether-modified polyorganosiloxane to solution 2 while stirring to obtain solution 3, add 300 g of ethanol to solution 3, and remove the sodium nitrate precipitate in the sol with a pressurized titanium rod filter to obtain Multiple oxide sols. Add sulfuric acid with a concentration of 5% to the multi-component oxide sol, adjust the pH to 7.5, pour it into a box covered with glass fiber needle felt, gel after 80 minutes, age at 25°C for 7 hours, and then perform supercritical carbon diox...

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Abstract

The invention relates to an in-situ composite silicon-based multibasic oxide oxide aerogel material and its preparation method, especially to a multibasic oxide oxide aerogel material which is prepared by the following steps: using soluble glass as a silicon source, mixing metallic oxide corresponding water-soluble metal salt, adding acid or alkali to adjust pH value of the system so as to form multibasic oxide sol; mixing the multibasic oxide sol with a water-soluble organic solvent, filtering to remove produced precipitate so as to obtain salt-free multibasic oxide sol, carrying out a sol-gel method, aging, modifying and drying. By a mature silica aerogel technology, the multibasic oxide oxide aerogel material is prepared by in-situ polymerization of other oxide components which are not easy to separately prepare aerogel. In addition, the multibasic oxide oxide aerogel material has excellent properties, such as high temperature stability, high activity, magnetic property and the like, none of which are present in single-component silica aerogel. The product is widely applied in fields of high temperature insulation, sound insulation, catalysts, catalytic carriers, battery electrodes, electromagnetism, resistance, gas sensitivity, humidity sensitivity, luminescent materials and the like.

Description

technical field [0001] The invention relates to an airgel material and a preparation method thereof, in particular to an in-situ composite preparation of a silicon-based multi-oxide airgel material and a preparation method thereof. Background technique [0002] Airgel is a new type of nano-insulation material. It was invented by American Kistler.S. in 1931. It is also called "blue smoke" and "frozen smoke". One of the top 10 popular science and technology since then is a military-civilian dual-use technology with great application value. [0003] At present, silica airgel has initially achieved mass production, and other types of oxide airgel, such as alumina airgel, zirconia airgel, titanium oxide airgel, etc. are still at the experimental level, vanadium oxide airgel The preparation of glue and yttrium oxide airgel is even more difficult, and the distance from large-scale industrial production is also farther away. [0004] Patent CN200810033022.2 discloses a preparatio...

Claims

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Application Information

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IPC IPC(8): B01J13/00
Inventor 金承黎
Owner 金承黎
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