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A kind of supercritical drying preparation method of silica airgel thermal insulation material

A supercritical drying, silica technology, applied in the polymer field, can solve the problems of increasing aerogel cost, aerogel production cost, weak continuous production capacity, etc. Effect

Active Publication Date: 2020-01-14
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ubiquitous problems are that the preparation cycle is long, the hydrophilic materials cannot be prepared, and the continuous production capacity is weak, which is not conducive to large-scale operation.
However, the temperature of this supercritical drying method is as high as 250 ° C and the pressure is 22 MPa, which consumes a lot of energy and is dangerous to operate. Tetraethyl orthosilicate is used as the silicon source, which greatly increases the cost of airgel and is not conducive to large-scale production. Production; similarly, the Chinese patent (application number 201510911661.4) adopts the supercritical drying method of solvent, the pressure and temperature are relatively high, and the silicon source also uses expensive organic silicon source, which will lead to the production cost of airgel Increase
[0004] To sum up, at present, the supercritical drying technology for preparing silica aerogels uses organosilicon sources as precursors, and the preparation cost is relatively high, which leads to the high price of silica aerogels currently on the market.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Take 70mL of sodium water glass (3.55 mold, 32.16%), dilute it with 70mL of deionized water, and stir evenly to obtain solution A. Finally, slowly pour solution A into 20mL of undiluted concentrated hydrochloric acid (12mol / L), and stir while adding (stirring speed is 300-600r / min), to obtain strongly acidic silica sol solution B, and the obtained strongly acidic The pH value of silica sol is less than 1.5;

[0024] 2) Take 100mL of the acidic silica sol, place it in a rotary evaporator, set the temperature at 50°C, and rotate the evaporation time for 10 minutes to obtain 70mL of silica sol, take out the sol, add 70mL of absolute ethanol to it, and stir it magnetically to make it well mixed. Then add A dropwise thereto, adjust the pH of the solution to 6, and form a gel in ~20min;

[0025] 3) Add absolute ethanol to the formed gel for aging for 4 hours, then place the gel in an autoclave, and perform supercritical CO at 7.4Mpa and 35°C. 2 Extract and dry for 2h. ...

Embodiment 2

[0027] 1) Take 70mL lithium water glass (3.4 mold, 30.64%), dilute it with 70mL deionized water, stir evenly to obtain solution A. Finally, slowly pour the mixed solution into 20mL of undiluted concentrated hydrochloric acid (12mol / L), and stir while adding (stirring speed is 300-600r / min), to obtain a strongly acidic silica sol solution, and the obtained strongly acidic silica The pH value of the sol is less than 1.5;

[0028] 2) Take 100mL of the acidic silica sol, place it in a rotary evaporator, set the temperature at 60°C, and rotate the evaporation time for 5 minutes to obtain 70mL of silica sol, take out the sol, add 70mL of anhydrous methanol to it, and stir it magnetically to make it well mixed. Then add the solution A in step 1) dropwise to it, adjust the pH of the solution to 6, and form a gel in ~15 minutes;

[0029] 3) Add anhydrous methanol to the formed gel for aging for 3 hours, and then place the gel in an autoclave for supercritical CO at 7.6Mpa and 38°C. ...

Embodiment 3

[0031] 1) Take 70mL of potassium silicate (3.2 mold, 29.8%), dilute with 70mL of deionized water, and stir evenly to obtain solution A. Finally, the mixed solution is slowly poured into 20 mL of concentrated hydrochloric acid (10mol / L), and stirred while adding (stirring speed is 300~600r / min), to obtain a strongly acidic silica sol solution, and the pH value of the obtained strongly acidic silica sol is less than 1.5;

[0032] 2) Take 100mL of the acidic silica sol, place it in a rotary evaporator, set the temperature at 70°C, and rotate the evaporation time for 3 minutes to obtain 70mL of silica sol, take out the sol, add 70mL of acetone to it, and stir it magnetically to make it evenly mixed . Then add the solution A in step 1) dropwise to it, adjust the pH of the solution to 6, and form a gel in ~20min;

[0033] 3) Acetone was added to the formed gel to age for 6 hours, and then the gel was placed in an autoclave for supercritical CO at 8Mpa and 45°C. 2 Extraction and d...

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Abstract

The invention relates to a supercritical drying preparation method for a silicon dioxide aerogel heat-insulation material. The method comprises the following steps: 1) diluting a water glass solution by using a certain amount of deionized water; 2) slowly adding the diluted water glass solution into a concentrated hydrochloric acid solution, and performing uniform mixing under continuous stirring, so as to obtain a highly-acidic silica sol; 3) performing rotary evaporation on the acidic silica sol solution to evaporate off partial water, taking out the processed sol, adding a water-soluble polar solvent with a low surface tension, performing uniform mixing with stirring, and then adding the diluted water glass solution to adjust the pH of the formed solution, so as to form a gel; and 4) adding a water-soluble polar solvent into the gel for aging and gelation, then putting the obtained wet gel in an extraction kettle, enabling the kettle to have a high-pressure internal environment and to be sealed, introducing supercritical CO2, contacting CO2 with the wet gel, and performing extraction and drying. The preparation method has the beneficial effects that the technology can be finished within a half day.

Description

technical field [0001] The invention belongs to the technical field of macromolecules, and in particular relates to a method for preparing a silica airgel thermal insulation material by supercritical drying. 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. The preparation of silica airgel at home and abroad usually uses methyl orthosilicate, ethyl orthosilicate or "water glass" as raw materials, adopts sol-gel method, and is often pressed and dried, such as Chinese patents 200810042222.4, 200910042159.5 , 201210123519.X, CN201210121968.0, CN201210114691.9, etc. all prepared mesoporous silica airgel materials using organic or inorganic silicon sources as precursors. The ubiquitous problems are that the preparation cycle is long, the hydrophilic material cannot be prepared, and the cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/158
CPCC01B33/1585
Inventor 何松李乾马力孙国翔陈先锋
Owner WUHAN UNIV OF TECH