Preparation method of sulfonated polysulfone polymer doped carboxylic acid sulfonated graphene hybrid membrane as well as product and application thereof
A technology of sulfonated graphene and sulfonated polysulfone, which is applied in the fields of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc. Graphene and other issues, to achieve the effect of favorable adsorption, low cost, and simple film-making conditions
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Embodiment 1
[0044] Preparation of Carboxylic Acid Sulfonated Graphene
[0045] 1) Graphene oxide was prepared by the Hummers' method. Add 300mL of concentrated sulfuric acid with a mass fraction of 98%, 5g of 100-mesh graphite powder and 2.5g of sodium nitrate into a 1L three-necked flask, place the flask in an ice bath and stir, then slowly add potassium permanganate in batches, Reaction in the bath for 1h. Move the flask to a constant temperature water bath at 60°C and react for 12 hours; slowly add 300mL of deionized water at 4°C to the reaction solution, then raise the temperature of the water bath to 95°C and react for 60 minutes; finally add 100mL of deionized water to the reaction solution Dilute it with water, then add 60mL of 30% hydrogen peroxide solution to terminate the reaction; after it cools down, wash it with 5% dilute hydrochloric acid solution for 3 times, then wash it with deionized water until the pH is neutral, and freeze-dry it after ultrasonication for 2h to obtain...
Embodiment 2
[0051] Add 1.05g of the carboxylic acid sulfonated graphene prepared in Example 1 to 68.70g of concentrated sulfuric acid, react at 180°C for 12h, then add 5.25g of PES (polyethersulfone resin), and stir at 60°C for 12h to obtain Uniform casting solution, let it stand overnight for degassing, scrape and coat the treated casting solution on a flat glass plate to form a flat film, then soak it in a coagulation bath for 20 minutes to solidify and form, and finally use deionized water again Soak and wash for 7 days, freeze-dry to obtain a hybrid membrane. The coagulation bath composition is H 2 O: DMAc = 2:1, the temperature of the coagulation bath is 5°C.
[0052] Add 15mg of the dried hybrid membrane adsorbent into a beaker filled with 20mL calcium and magnesium ion solution with a concentration of 1000mg / L, shake it for 24h at room temperature at 25°C, and calculate the adsorption capacity based on the concentration of the test solution. The results are shown in Table 1 .
Embodiment 3
[0054] The preparation method is consistent with Example 2, except that the quality of PES is 1.75g, the quality of concentrated sulfuric acid is 22.2g, and the coagulation bath composition is H 2 O:DMAc=1:1, coagulation bath temperature is 9°C.
[0055] The conditions for testing the adsorption capacity are the same as in Example 2, and the results are shown in Table 1.
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