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
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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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