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Method for organically modifying nano silicon dioxide aerogel

A nano-silica and aerogel technology, applied in the field of airgel, can solve the problems of limiting the practical application of nano-silica aerogel, poor compatibility of polyester thermal insulation and flame-retardant material matrix, etc.

Active Publication Date: 2021-09-14
安徽瑞联节能科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many hydroxyl groups on the surface of silica airgel, which makes it poorly compatible with the matrix of polyester thermal insulation and flame retardant materials, which limits the practical application of nano silica airgel

Method used

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  • Method for organically modifying nano silicon dioxide aerogel
  • Method for organically modifying nano silicon dioxide aerogel
  • Method for organically modifying nano silicon dioxide aerogel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Prepare the modifier:

[0028] Step S11, mix aniline, p-hydroxybenzaldehyde and 1,4-dioxane, raise the temperature to 85°C under nitrogen protection, and react for 6 hours. After the reaction, carry out post-treatment. The post-treatment process is as follows: The reaction solution was cooled to room temperature, concentrated under reduced pressure to remove the solvent, and then washed with ethanol. After the washing was completed, it was dried to a constant weight at a temperature of 75° C. to obtain intermediate 1;

[0029] Step S12, mixing intermediate 1, tetrahydrofuran and triethylamine, adding phosphorus oxychloride dropwise at a temperature of 20°C, keeping the temperature constant after the addition, stirring for 10 hours, and post-processing after the reaction. The process of treatment is: concentrating the obtained reaction solution under reduced pressure to remove the solvent, and purifying through a column to obtain intermediate 2;

[0030] Step S13, mix 2...

Embodiment 2

[0034] Prepare the modifier:

[0035] Step S11, mix aniline, p-hydroxybenzaldehyde and 1,4-dioxane, raise the temperature to 85°C under nitrogen protection, and react for 6 hours. After the reaction, carry out post-treatment. The post-treatment process is as follows: The reaction solution was cooled to room temperature, concentrated under reduced pressure to remove the solvent, and then washed with ethanol. After the washing was completed, it was dried to a constant weight at a temperature of 75° C. to obtain intermediate 1;

[0036] Step S12, mixing intermediate 1, tetrahydrofuran and triethylamine, adding phosphorus oxychloride dropwise at a temperature of 25°C, keeping the temperature constant after the addition, stirring for 10 hours, and post-processing after the reaction. The process of treatment is: concentrating the obtained reaction solution under reduced pressure to remove the solvent, and purifying through a column to obtain intermediate 2;

[0037] Step S13, mix 2...

Embodiment 3

[0041] Preparation of organically modified nano-silica airgel:

[0042] After mixing tetraethyl orthosilicate, modifier and ethanol, add oxalic acid aqueous solution, stir magnetically for 30 minutes, and let it stand at room temperature for 24 hours; then add ammonia water drop by drop, stir for 30 minutes, and age at room temperature for 2 days to obtain a gel body; then the gel body is dried, and the graded drying method is used to dry at 60°C, 80°C, 100°C and 120°C for 24h, 2h, 1.5h and 1h; to obtain organically modified nano-silica airgel;

[0043] Among them, the concentration of oxalic acid aqueous solution is 1mol / L; the mass fraction of ammonia water is 25%; the mass ratio of ethyl orthosilicate and modifier is 1:0.5; The dosage ratio is 1g: 20mL: 0.6g: 0.5g; the modifier is prepared in Example 2.

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Abstract

The invention discloses a method for organically modifying nano silicon dioxide aerogel, and belongs to the technical field of aerogels, the method comprises the following steps: mixing tetraethoxysilane, a modifier and ethanol, adding an oxalic acid aqueous solution, magnetically stirring for 30 minutes, and standing at room temperature for 24 hours; dropwise adding ammonia water, stirring for 30 minutes, and aging for 2 days at normal temperature to obtain gel; then drying the gel to obtain organic modified nano silicon dioxide aerogel; the prepared modifier contains a flame-retardant element N, and C = N double bonds in the molecular structure of the modifier can be subjected to a cross-linking reaction at high temperature to form a stable carbon layer, so that a thermal protection effect on a polymer material is achieved. Hydroxyl on the surface of silicon dioxide is modified by adopting the modifier, the aerogel with hydrophobic performance is prepared, the compatibility of the aerogel and a matrix is further improved, the interface compatibility problem is solved, and the application of the aerogel in the aspect of thermal insulation flame-retardant materials is improved.

Description

technical field [0001] The invention belongs to the technical field of airgel, and in particular relates to a method for organically modifying nano-silica airgel. Background technique [0002] Nano-silica airgel is a new type of porous amorphous material with low density, low thermal conductivity and high porosity. It has unique thermal, acoustic, optical and electrical properties. Wide range of applications. There are many hydroxyl groups on the surface of silica airgel, which makes it poorly compatible with the matrix of polyester thermal insulation and flame retardant materials, which limits the practical application of nano silica airgel. [0003] The invention improves the interfacial interaction between the silicon dioxide aerogel and the polyester matrix by organically modifying the surface of the silica airgel, solves the interface compatibility problem, and realizes the improvement of the dispersibility of the silicon dioxide airgel in the polyester matrix. Conte...

Claims

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Application Information

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IPC IPC(8): C01B33/141C01B33/158C01B33/157C07F9/12C09C1/30C09C3/12
CPCC01B33/1585C01B33/141C01B33/157C07F9/12C09C1/3081C09C3/12Y02B80/10
Inventor 范伟
Owner 安徽瑞联节能科技股份有限公司
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