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CN-122006680-A - Micron-sized spherical inorganic composite material, preparation method and application thereof, and adsorption method of Cs+ in solution

CN122006680ACN 122006680 ACN122006680 ACN 122006680ACN-122006680-A

Abstract

The invention provides a micron-sized spherical inorganic composite material, a preparation method and application thereof, and an adsorption method of Cs + in solution, belonging to the technical field of radioactive waste treatment in nuclear fuel circulation. The preparation method comprises the steps of mixing water, absolute ethyl alcohol, hydrochloric acid, a silicon source and ammonium phosphomolybdate, concentrating to obtain a silicic acid solution, mixing benzyl alcohol, a methyl cellulose water solution and a benzyl alcohol solution of an emulsifier to obtain a dispersion system, adding the silicic acid solution into the dispersion system, and heating to obtain the micron-sized spherical inorganic composite material. In the invention, absolute ethyl alcohol is used as a solvent to improve the solubility of a silicon source, hydrochloric acid is used as a catalyst to catalyze the hydrolysis reaction of the silicon source, benzyl alcohol provides a hydrophobic environment, methyl cellulose aqueous solution provides a spherical template to induce a spherical structure, and an emulsifier reduces the surface tension to enable a system to form stable emulsion. The micron-sized spherical inorganic composite material with high adsorption capacity, high selectivity and good stability is prepared by the method.

Inventors

  • HE JIANGANG
  • SHI KELIANG
  • LIU TONGHUAN
  • WANG SHIRONG
  • LI XIANG
  • WANG YINGQI
  • ZHANG ZIHAN

Assignees

  • 兰州大学

Dates

Publication Date
20260512
Application Date
20260326

Claims (10)

  1. 1. The preparation method of the micron-sized spherical inorganic composite material is characterized by comprising the following steps of: Mixing water, absolute ethyl alcohol, hydrochloric acid, a silicon source and ammonium phosphomolybdate, and concentrating to obtain a silicic acid solution; Mixing benzyl alcohol, methyl cellulose water solution and benzyl alcohol solution of an emulsifier to obtain a dispersion system; and adding the silicic acid solution into a dispersion system, and then heating to obtain the micron-sized spherical inorganic composite material.
  2. 2. The preparation method of claim 1, wherein the dosage ratio of water, absolute ethanol, silicon source and ammonium phosphomolybdate is 8.0-12.0 ml, 19-22 g, 4.5-5.5 g, and 0.5-0.8 g.
  3. 3. The method of claim 2, wherein the ratio of water, absolute ethanol, silicon source, and ammonium phosphomolybdate is 10.0ml to 20g to 5.0g to 0.6g.
  4. 4. The method according to claim 1 or 2, wherein the concentration of hydrochloric acid in the mixed solution obtained by mixing water, absolute ethanol, hydrochloric acid, a silicon source and ammonium phosphomolybdate is 0.15mol/L.
  5. 5. The preparation method according to claim 1, wherein the volume ratio of the benzyl alcohol solution to the aqueous solution of methyl cellulose to the benzyl alcohol solution of the emulsifier is 19-21:1.4-1.6:1.4-1.6, the mass concentration of the aqueous solution of methyl cellulose is 1.3-1.5%, and the volume concentration of the benzyl alcohol solution of the emulsifier is 18-20%.
  6. 6. The method according to claim 1 or 5, wherein the emulsifier in the benzyl alcohol solution of the emulsifier comprises dodecylphenol polyoxyethylene ether.
  7. 7. The method according to claim 1, wherein the volume ratio of the silicic acid solution to the dispersion is 1:3.9-4.1.
  8. 8. The micron-sized spherical inorganic composite material prepared by the preparation method of any one of claims 1 to 7.
  9. 9. Use of the micron-sized spherical inorganic composite material according to claim 8 in the cesium removal field.
  10. 10. A method for adsorbing Cs + in a solution, comprising the steps of: the adsorption of Cs + in solution using the micron-sized spherical inorganic composite material of claim 8.

Description

Micron-sized spherical inorganic composite material, preparation method and application thereof, and adsorption method of Cs+ in solution Technical Field The invention relates to the technical field of radioactive waste treatment in nuclear fuel circulation, in particular to a micron-sized spherical inorganic composite material, a preparation method and application thereof, and an adsorption method of Cs + in solution. Background As energy demand continues to grow, nuclear energy is increasingly important as a clean energy source, and its low carbon nature exhibits significant advantages in terms of reduced coal consumption, reduced greenhouse gas emissions, and the like. However, radioactive waste water generated by nuclear fission processes poses serious threats to the ecological environment and human health. Wherein 137 Cs is one of the main radionuclides generated by nuclear reactor uranium fission, has half-life of 30.17 years, and has high-energy gamma-ray radiation characteristic. The nuclide is easy to dissolve in water and has strong migration, and can enter an ecological system through rainwater or soil to cause persistent pollution. Nuclear accidents indicate that large scale release of 137 Cs can lead to serious ecological disasters. In addition, 137 Cs can be enriched in humans through the food chain, causing cell damage and even cancer, severely compromising human health. Therefore, the development of a technology for efficiently and selectively removing 137 Cs in nuclear wastewater has important significance. Methods such as solvent extraction, chemical precipitation and evaporation are widely used for enriching and separating radioactive cesium, but have disadvantages in terms of operation, cost or selectivity, such as high cost and toxicity of extractant, large amount of radioactive sludge produced by precipitation method, and the like. The adsorption method is a common cesium separation method, is particularly suitable for separating cesium with low concentration, has the advantages of simple operation, strong selectivity, high recovery rate, no secondary pollution and the like, and is one of the most industrially applicable methods. The organic-inorganic composite resin material provided in the related art has low cesium ion adsorption capacity (only 0.8 g/L), and is difficult to meet the requirement of efficiently treating high-concentration radioactive wastewater. In addition, the low adsorption capacity results in increased material usage, not only increasing costs, but also producing more radioactive solid waste, increasing the complexity of subsequent processing. Therefore, the cesium ion adsorption material with high adsorption capacity, high selectivity and good stability is developed, and has important significance for improving the radioactive wastewater treatment efficiency, reducing the cost and reducing the secondary pollution. Disclosure of Invention In view of the above, the invention aims to provide a micron-sized spherical inorganic composite material, a preparation method and application thereof, and an adsorption method of Cs + in solution. The micron-sized spherical inorganic composite material prepared by the invention has high adsorption capacity to cesium ions, maintains excellent selectivity and stability, and provides a new solution for efficiently removing 137 Cs in nuclear wastewater. In order to achieve the above object, the present invention provides the following technical solutions: The invention provides a preparation method of a micron-sized spherical inorganic composite material, which comprises the following steps: Mixing water, absolute ethyl alcohol, hydrochloric acid, a silicon source and ammonium phosphomolybdate (AMP) and concentrating to obtain a silicic acid solution; Mixing benzyl alcohol, methyl cellulose water solution and benzyl alcohol solution of an emulsifier to obtain a dispersion system; and adding the silicic acid solution into a dispersion system, and then heating to obtain the micron-sized spherical inorganic composite material. Preferably, the dosage ratio of the water, the absolute ethyl alcohol, the silicon source and the ammonium phosphomolybdate is 8.0-12.0 mL, 19-22 g, 4.5-5.5 g and 0.5-0.8 g. Preferably, the water, absolute ethanol, silicon source and ammonium phosphomolybdate are used in a ratio of 10.0mL to 20g to 5.0g to 0.6g. Preferably, the concentration of hydrochloric acid in the mixed solution obtained by mixing water, absolute ethyl alcohol, hydrochloric acid, a silicon source and ammonium phosphomolybdate is 0.15mol/L. Preferably, the volume ratio of the benzyl alcohol to the aqueous solution of the methyl cellulose to the benzyl alcohol solution of the emulsifier is 19-21:1.4-1.6:1.4-1.6, the mass concentration of the aqueous solution of the methyl cellulose is 1.3-1.5%, and the volume concentration of the benzyl alcohol solution of the emulsifier is 18-20%. Preferably, the emulsifier in the benzyl alcohol solution of