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

Inactive Publication Date: 2013-08-21
HANGZHOU DIANZI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional ion exchange method has disadvantages such as low separation efficiency, long separation cycle, and high production cost, which also make it difficult to apply to large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention relates to a sulfonation method of natural zeolite for adsorption and recycling of rare earth ions. The method comprises the following steps of firstly, acidizing the natural zeolite, then conducting sulfhydrylation grafting on the surface of the acidized natural zeolite, oxidizing sulfydryl on the surface of the natural zeolite subjected to sulfhydrylation, and finally, acidizing the obtained product in an acidic solution so as to obtain the sulfonated natural zeolite. The sulfonated zeolite not only has the original high specific surface area of the zeolite but also has functional groups with chelation action, and can gather and separate the rare earth ion furthest under the synergistic effect of two different adsorption modes.

Description

technical field [0001] The invention belongs to the field of environmental treatment and materials, in particular to the technical field of metal ion adsorption materials in wastewater, and specifically relates to a surface functionalized sulfonation method of natural zeolite which has the function of enriching and recovering rare earth ions in rare earth production wastewater. Background technique [0002] Due to the similar electronic structure and chemical properties of rare earth elements, and they are always mixed in the form of symbiotic minerals, it is very difficult to separate them. However, most rare earth functional materials require high-purity single elements, and the separation of rare earths has become a bottleneck for their application. Especially for rare earth production wastewater, the concentration of rare earth ions is very low, separation and recovery are particularly difficult, and direct discharge will cause great harm to the environment. [0003] At...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/30B01J20/18C02F1/28C02F1/58
Inventor 殷好勇唐俊红严春杰
Owner HANGZHOU DIANZI UNIV
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