Sulfonation method of natural zeolite for adsorption and recycling of rare earth ions
A natural zeolite, adsorption and recovery technology, applied in the field of environmental governance and materials, can solve the problems of difficulty in large-scale production, long separation cycle, high production cost, etc., and achieve good separation and enrichment capacity, high specific surface area, and strong adsorption capacity Effect
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Embodiment 1
[0018] (1) First calcinate the natural zeolite at 500°C for 5 hours, then weigh 5g of the calcined natural zeolite, add it into 0.2M sulfuric acid solution under stirring conditions and stir for 3 hours for acidification treatment, and finally separate and dry at 100°C for 6 hours to obtain the acidified natural zeolite.
[0019] (2) Add the acidified natural zeolite into 400ml of anhydrous toluene solution, stir evenly, add 3g of 3-mercaptopropyltrimethoxysilane coupling agent, reflux for 10 hours, separate with 100ml of dichloromethane and The mixed solution of 100ml of ethyl acetate was refluxed and washed to remove the mercaptosilane on the surface of the sample to obtain mercaptolated zeolite.
[0020] (3) Add the thiolated zeolite to the solution containing 15mlH 2 o 2 and 30mlCH 3 OH and 90ml of deionized water, stirred for 15 hours to oxidize the surface groups.
[0021] (4) Add surface oxidized zeolite to 100ml 1M sulfuric acid solution, acidify at room temperatur...
Embodiment 2
[0023] (1) First, calcinate the natural zeolite at 500°C for 5 hours, then weigh 5g of the calcined natural zeolite, add it into 0.2M hydrochloric acid solution under stirring conditions and stir for 8 hours for acidification treatment, and finally separate and dry at 80°C for 9 hours to obtain the acidified natural zeolite.
[0024] (2) Add the acidified natural zeolite into 300ml of anhydrous toluene solution, stir evenly, add 2g of 3-mercaptopropylmethyldimethoxysilane coupling agent, reflux for 15 hours, separate with 100ml dimethoxysilane The mixed solution of methyl chloride and 100ml of ethyl acetate was refluxed and washed to remove mercaptosilane on the surface of the sample to obtain mercaptolated zeolite.
[0025] (3) Add the thiolated zeolite to 200ml of 0.2% acidic potassium permanganate solution, and stir for 8 hours to oxidize the surface groups.
[0026] (4) Add surface oxidized zeolite to 200ml 0.3M sulfuric acid solution, acidify at room temperature for 15 h...
Embodiment 3
[0028] (1) First, calcinate the natural zeolite at 500°C for 5 hours, then weigh 5g of the calcined natural zeolite, add it into a 0.15M nitric acid solution under stirring conditions and stir for 10 hours for acidification treatment, and finally separate and dry at 80°C for 9 hours to obtain the acidified natural zeolite.
[0029] (2) Add the acidified natural zeolite into 200ml of anhydrous toluene solution, stir evenly, add 3g of 3-mercaptopropyltriethoxysilane coupling agent, reflux for 10 hours, separate with 100ml of dichloromethane The mixed solution with 100ml of ethyl acetate was refluxed and washed to remove the mercaptosilane on the surface of the sample to obtain mercaptolated zeolite.
[0030] (3) Add the thiolated zeolite to 200ml of 0.5% acidic potassium permanganate solution, and stir for 5 hours to oxidize the surface groups.
[0031] (4) Add surface oxidized zeolite to 200ml 0.2M nitric acid solution, acidify at room temperature for 10 hours, finally wash an...
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