Preparation method of vanadium pentoxide sol
A technology of vanadium pentoxide sol and vanadium salt, applied in vanadium oxide and other directions, can solve the problems of unstable product, high cost, and difficulty in obtaining, and achieve the effects of simple and easy operation, mild reaction conditions, and low purity requirements.
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Embodiment 1
[0038] Weigh 0.01mol (2.28g) of vanadyl sulfate and dissolve it in 100ml of deionized water to obtain a 0.1mol / L blue transparent precursor solution. Co-precipitate the precursor solution and the ammonia solution in 100ml of deionized water, adjust the amount of the ammonia solution to keep the pH of the suspension at around 4 after the coprecipitation is completed. The resulting slurry suspension was centrifuged to remove impurities. Add deionized water to the washed precipitate to dilute into a suspension, so that the concentration of vanadium ions is 0.1 mol / L. Use a water bath heating device to keep the temperature of the suspension at about 5°C, and add 1ml of hydrogen peroxide (30%) solution under stirring conditions to carry out peptization reaction. After stirring for 3 h, an orange-red stable and transparent sol was obtained. attached figure 1 It is the photoelectron energy spectrum narrow-range scan diagram of the powder after drying the sol obtained in Example 1...
Embodiment 2
[0040] Weigh 0.04mol (9.12g) of vanadyl sulfate and dissolve it in 100ml of deionized water to obtain a 0.4mol / L blue transparent precursor solution. Co-precipitate the precursor solution and ammonium bicarbonate solution in 100ml of deionized water to adjust the ammonium bicarbonate solution The added amount keeps the pH of the suspension at about 6 after the co-precipitation is completed. The resulting suspension was centrifuged 5 times with deionized water to remove impurities. Add deionized water to the obtained precipitate and dilute to form a suspension, so that the concentration of vanadium ions is 0.2 mol / L. Use a water bath heating device to keep the temperature of the suspension at about 25°C, add 5ml of hydrogen peroxide (30%) solution, 2g of polyvinylpyrrolidone and 0.5g of polyethyleneimine successively under stirring conditions for peptization reaction. After stirring for 3 h, a blood red stable and transparent sol was obtained. attached image 3 It is the XRD...
Embodiment 3
[0042] Weigh 0.06mol (13.68g) of vanadyl sulfate and dissolve it in 100ml of deionized water to obtain a 0.6mol / L blue transparent precursor solution. Co-precipitate the precursor solution with a mixed solution of potassium hydroxide and ammonia water in 100ml of deionized water. The adding amount of the mixed solution of potassium hydroxide and ammonia water keeps the pH of the suspension at about 7 after the co-precipitation is completed. The obtained suspension was centrifuged and washed 5 times with deionized water to remove impurities. Add deionized water to the obtained precipitate to dilute to form a suspension, so that the concentration of vanadium ions is 0.3 mol / L. Heat the suspension in a water bath to 40°C, add 5ml of hydrogen peroxide (30%) solution, 2ml of oxalic acid (0.1mol / L) solution, and 0.5g of polyethylene glycol successively under stirring conditions for peptization reaction, and stir for 30 minutes. A dark red stable transparent sol was obtained.
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