Polyvinyl alcohol/amino silanized graphene oxide macroporous compound spheres as well as preparation method and application of compound spheres
An amino silylation, polyvinyl alcohol technology, applied in chemical instruments and methods, alkali metal compounds, alkali metal oxides/hydroxides, etc., can solve the problems of low mechanical strength, difficult separation and recovery, easy quality loss, etc. Achieve the effect of improving mechanical strength, improving adsorption capacity, and reducing usage
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Embodiment 1
[0027] Embodiment 1: improved Hummers method prepares graphite oxide
[0028] Add 6g of graphite powder into a three-necked flask containing 720mL of concentrated sulfuric acid and 80mL of phosphoric acid solution, and stir evenly in an ice-water bath; keep stirring, and slowly add 36g of potassium permanganate powder (control the temperature of the reaction system ≤ 20°C ); after the addition is complete, put the reaction system into a constant temperature water bath, and keep the constant temperature water bath at 50°C for 12 hours; after the reaction is completed and cooled to room temperature, first pour the mixed solution into 1000mL of ice water, and then transfer To a certain amount of 30% hydrogen peroxide, obtain a bright yellow solution, filter the reaction product; repeatedly wash the above-mentioned solid product with 10% hydrochloric acid solution, detect the filtrate with 10wt% barium chloride solution until no white precipitate; Repeatedly washing with deionized...
Embodiment 2
[0030] (1) Disperse 200 mg of the graphite oxide prepared in Example 1 in 100 mL of deionized water, and stir overnight with a magnetic force to form a graphene oxide colloidal suspension; then ultrasonically treat it in an ultrasonic instrument for 6 hours to peel off the graphite oxide flakes and form a uniform and stable The dispersion liquid, promptly obtains the graphene oxide dispersion liquid of 2mg / mL;
[0031] (2) Under stirring conditions, add 10mL of 3-aminopropyltriethoxysilane into 500mL of deionized water, gradually raise the temperature to 48°C, and react for 6h; then add the graphene oxide dispersion prepared in step (1) into The above reaction system was stirred and reacted for 12 hours to obtain flocculent precipitates; the flocculent precipitates were repeatedly washed with deionized water, centrifuged, and then the solid was placed in a vacuum drying oven to dry to obtain aminosilanized graphene oxide;
[0032] (3) Add 15.0g of polyvinyl alcohol, 3.6g of so...
Embodiment 3
[0034] (1) Disperse 1000 mg of the graphite oxide prepared in Example 1 in 100 mL of deionized water, and stir overnight with a magnetic force to form a graphene oxide colloidal suspension; then ultrasonically treat it in an ultrasonic instrument for 4 hours to peel off the graphite oxide flakes and form a uniform and stable The dispersion liquid, promptly obtains the graphene oxide dispersion liquid of 10mg / mL;
[0035] (2) Under stirring conditions, add 10mL of 3-aminopropyltriethoxysilane into 1000mL of deionized water, gradually raise the temperature to 80°C, and react for 4h; then add the graphene oxide dispersion prepared in step (1) into The above reaction system was stirred and reacted for 24 hours to obtain a flocculent precipitate; the flocculent precipitate was repeatedly washed with deionized water, centrifuged, and then the solid was placed in a vacuum drying oven to dry to obtain aminosilanized graphene oxide;
[0036](3) Add 15.0g of polyvinyl alcohol, 1.5g of s...
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