Thiolated graphene oxide/polyvinyl alcohol macroporous composite spherical adsorbent and its preparation method and application
A technology of polyvinyl alcohol and graphene, which is applied in the preparation of polymer composite materials and the field of environmental engineering, can solve the problems of limited application, difficult separation and recovery, etc., and achieve the effects 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 reaction system temperature ≤ 20 ℃); 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, pour the reaction solution into 1000mL of ice water, and then transfer to Use a certain amount of 30% hydrogen peroxide to obtain a bright yellow solution, and filter the reaction product; wash the above-mentioned filtered product repeatedly with 10% hydrochloric acid solution, and detect it with 10% (W / V) barium chloride solution until there is no white precipitate Then, it was repeatedly w...
Embodiment 2
[0030] (1) Disperse 500 mg of graphite oxide prepared in Example 1 in 100 mL of deionized water, and stir overnight with magnetic force to form a graphene oxide colloidal suspension; then ultrasonically treat it for 4 hours under an ultrasonic instrument to peel off the graphite oxide flakes to form a uniform and stable The dispersion liquid, promptly obtains the graphene oxide dispersion liquid of 5mg / mL.
[0031] (2) Under stirring conditions, add 12mmol of 4-aminothiophenol into 15mL of 1mol / L hydrochloric acid solution, and gradually raise the temperature to 53°C to obtain a 4-aminothiophenol solution; then, dissolve 12mmol of sodium nitrite In 20mL of deionized water, obtain a sodium nitrite solution; slowly add the sodium nitrite solution dropwise to the above-mentioned 4-aminothiophenol solution while stirring in an ice-water bath; finally add the graphene oxide dispersion to the above-mentioned reaction system , stirred for 24 h in an ice-water bath. After the obtaine...
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 magnetic force to form a graphene oxide colloidal suspension; then sonicate for 6 hours under an ultrasonic instrument to peel off the graphite oxide flakes to form a uniform and stable The dispersion liquid, promptly obtains the graphene oxide dispersion liquid of 10mg / mL.
[0035] (2) Under stirring conditions, add 12mmol of 4-aminothiophenol into 18mL of 1mol / L hydrochloric acid solution, and gradually raise the temperature to 35°C to obtain a 4-aminothiophenol solution; then, dissolve 12mmol of sodium nitrite In 20mL of deionized water, obtain a sodium nitrite solution; slowly add the sodium nitrite solution dropwise to the above-mentioned 4-aminothiophenol solution while stirring in an ice-water bath; finally add the graphene oxide dispersion to the above-mentioned reaction system , stirred for 8 h in an ice-water bath. After the obtained mixed so...
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