A kind of rapid preparation method of silica airgel

A silica and aerogel technology, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve the problems of long preparation cycle, poor product uniformity, and long drying process, and achieve mild and controllable hydrolysis reaction. , The effect of reducing process cost and shortening aging time

Active Publication Date: 2019-06-25
TIANJIN BUILDING MATERIALS SCI RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the surface of the gel has hydroxyl groups after hydrolysis and polycondensation, surface alkylation is required to make it hydrophobic, so the normal pressure drying preparation process usually includes sol-gel, gel aging, solvent replacement, modification, cleaning, drying After several steps, there are many process steps and a long preparation period. The solvent replacement and modification steps need to consume a large amount of chemical reagents, and there are many waste liquids, which will have a certain impact on the environment. In addition, because the common normal pressure drying method is Heating from the outside forms a temperature gradient, often the surface is dry and the interior contains moisture, resulting in a long drying process and poor product uniformity in the large-scale production of airgel

Method used

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  • A kind of rapid preparation method of silica airgel
  • A kind of rapid preparation method of silica airgel

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 1L ethyl orthosilicate to 2L methanol solvent, mix and stir evenly, add 120ml of oxalic acid solution with a concentration of 0.005mol / L, stir well and let stand for 10h; mix 140ml tetramethyldisilazane with Slowly add 0.75ml / min into the above reaction system drop by drop, the total dropping time is 3h, after standing to get the gel, aging at 50℃ for 0.5h, after aging, microwave drying at 600W power for 300s before drying in oven Drying, the oven drying condition is to dry at 120°C for 1.5h, and the obtained product is silica airgel;

[0032] The tested silica airgel product has a density of 57kg / m 3 , specific surface area 920m 2 / g, thermal conductivity 0.016W / (m.K).

Embodiment 2

[0034] Add 1L tetraethyl orthosilicate to 2.5L ethanol solvent, mix and stir evenly, add 220ml of benzoic acid solution with a concentration of 0.002mol / L, stir evenly and let stand for 12h; mix 270ml hexamethyldisilazane with Slowly add dropwise into the above reaction system at a rate of 1ml / min. The total dropping time is 4.5h. After standing still to obtain the gel, age at 50°C for 1h. After aging, microwave dry at 450W for 120s before drying in an oven. , the oven drying condition is to dry at 150°C for 1.5h, and the obtained product is silica airgel;

[0035] The tested silica airgel product has a density of 45kg / m 3 , specific surface area 1050m 2 / g, thermal conductivity 0.013W / (m.K).

Embodiment 3

[0037]Add 1L tetraethyl orthosilicate to 2L ethanol solvent, mix and stir evenly, add 310ml of glacial acetic acid solution with a concentration of 0.001mol / L, stir well and let stand for 3h; mix heptamethyldisilazane with hexamethyl Cyclotrisilazane was mixed at a molar ratio of 1:3 to form a 200ml mixed solution, and the mixed solution was slowly dropped into the reaction system at a rate of 1ml / min. The total reaction time was 3.3 hours. Microwave drying at 200W power for 200s and then oven drying, the condition of oven drying is 2h at 105°C, the obtained product is silica airgel;

[0038] The tested silica airgel product has a density of 60kg / m 3 , specific surface area 865m 2 / g, thermal conductivity 0.018W / (m.K).

[0039] The preparation method of the present invention realizes gel polycondensation reaction and hydrophobic modification in one step by rationally controlling the addition amount, dropping rate and reaction time of nitrogen-containing silane, taking hexame...

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Abstract

The invention provides a fast preparation method of silicon dioxide aerogel. According to the method, tetraethyl orthosilicate is used as a silicon source; low-concentration organic weak acid is added for catalyzed hydrolysis reaction; then, the condensation polymerization reaction and the hydrophobic modification of the gel are completed in one step through reasonably controlling the addition quantity of the nitrogen-containing silane, the dripping speed and the reaction time; the addition of basic catalysts is not needed; the consumption of a great number of replacement solvents in the general post hydrophobic modification method is avoided; waste liquid is not generated; the preparation period is greatly shortened; the process cost is reduced; the industrial production is easy; meanwhile, the prepared silicon dioxide aerogel product has excellent performance.

Description

technical field [0001] The invention belongs to the technical field of silica airgel preparation, and in particular relates to a rapid preparation method of silica airgel. Background technique [0002] Silica airgel has a three-dimensional network skeleton structure and low density (0.03~0.2g / cm 3 ), high porosity (85% ~ 99%), low thermal conductivity (0.01 ~ 0.03W m -1 ·K -1 ), high specific surface area (600~1200m 2 / g) and many other excellent properties, it is often used in aerospace, petroleum and petrochemical, metallurgy and other fields. [0003] Silica airgel was first prepared by Kistler in 1931 through sol-gel method and supercritical drying technology, and this method has become the most commonly used method at present. The sol-gel method usually requires two steps of acid and alkali to catalyze the hydrolysis and polycondensation of the silicon source, respectively. The acid used is generally strong organic acid such as hydrochloric acid, the alkali catalys...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/158
CPCC01B33/1585C01P2004/03C01P2006/10C01P2006/12C01P2006/17C01P2006/32
Inventor 张希王建恒张鹏宇刘栋刘彤王冬梅刘凤东白锡庆赵海波
Owner TIANJIN BUILDING MATERIALS SCI RES INST
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