A method for the preparation of a material for the enrichment of cesium

Abstract

The application relates to the technical field of material science, and discloses a preparation method of a material for enriching cesium, which comprises the following steps: (1) adding an eluent X into waste, adding a modifier G under oscillation, uniformly mixing, and reacting for a period of time to obtain a solution or a suspension R; (2) adding a precipitant C into the solution or the suspension R, simultaneously performing ultrasonic treatment, cooling to room temperature after reaction, and performing filtration, washing and drying to obtain a material CST for enriching cesium. The material CST prepared by the method has excellent selective adsorption capacity and high adsorption capacity for cesium ions, and after the CST material is used, the concentration of cesium in wastewater with a cesium content of 200-300 mg / L is reduced to 2-5 mg / L.

Description

Technical Field

[0001] This invention relates to the field of materials science and technology, and more specifically, to a method for preparing materials for enriching cesium. Background Technology

[0002] Cesium is a rare metal, belonging to the alkali metals, and possesses unique physical and chemical properties. Due to its widespread application in numerous high-tech fields, the enrichment and extraction of cesium has become increasingly important. Cesium has significant economic and technological value, but its abundance in nature is extremely low, and it often coexists with other elements, making its separation and enrichment processes complex. Furthermore, existing cesium extraction methods typically involve high energy consumption and high costs, limiting the widespread application of cesium.

[0003] With increasing environmental awareness and the advancement of sustainable development goals, recovering rare elements such as cesium from solid waste has become an effective solution. This not only reduces the exploitation of natural resources but also mitigates the environmental impact of solid waste, achieving resource recycling. Summary of the Invention

[0004] In view of this, the present invention proposes a material preparation method for enriching cesium. By optimizing the extractant and process parameters, the extraction rate of cesium is significantly improved, solving the problem of insufficient extraction efficiency of existing methods. At the same time, the use of environmentally friendly extractants and harmless operation processes reduces the negative impact on the environment and meets the requirements of sustainable development.

[0005] To achieve the above objectives, the present invention proposes a method for preparing materials for enriching cesium, characterized by comprising the following steps: (1) Add eluent X to the waste, add modifier G under shaking conditions, mix evenly and react for a period of time to obtain a solution or suspension R; (2) Add precipitant C to the solution or suspension R and simultaneously perform ultrasonic treatment. After the reaction is complete, cool to room temperature, filter, wash and dry to obtain cesium-enriched material CST.

[0006] Furthermore, the waste mentioned in step (1) is an industrial solid waste containing one or more of the elements iron, potassium, cobalt, nickel, titanium, tin, and zirconium.

[0007] Further, the eluent X mentioned in step (1) is an acidic solvent, selected from one or more of hydrochloric acid, nitric acid, silicic acid, phosphoric acid, ammonium chloride, oxalic acid, and citric acid mixed in proportion to form an aqueous solution.

[0008] Further, in step (1), the solid-liquid ratio of the waste to the eluent X is 1:8 to 1:15 g / mL.

[0009] Furthermore, the modifier G mentioned in step (1) is a solid reagent selected from one or more of compounds containing boron, phosphorus, molybdenum, and aluminum, silicates, phosphates, and carbonates.

[0010] Furthermore, the oscillation conditions in step (1) are: temperature from room temperature to 80°C, oscillation speed of 150-200 rpm, and reaction time of 90-150 minutes.

[0011] Furthermore, the precipitant C mentioned in step (2) is an alkaline or amphoteric reagent, selected from one or more of aluminum hydroxide, titanium dioxide, ammonium carbonate, sodium bicarbonate, sodium silicate, and sodium fluorosilicate.

[0012] Furthermore, in step (2), the ultrasonic treatment power is 300-400W, the treatment time is 45-90 minutes, and the treatment temperature range is room temperature to 80℃.

[0013] Furthermore, the drying conditions described in step (2) are: drying at 60-105℃ for 6-24 hours.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows: The preparation method provided by this invention utilizes widely available and inexpensive raw materials, achieving high-value utilization of solid waste. Furthermore, the preparation process is simple, efficient, and energy-saving, avoiding complex high-temperature calcination processes. The CST material prepared by this invention exhibits excellent selective adsorption capacity and high adsorption capacity for cesium ions. For wastewater solutions with a cesium content of 200-300 mg / L, the cesium concentration in the wastewater decreases to 2-5 mg / L after using CST material. Detailed Implementation

[0015] The present invention will now be described in detail with reference to embodiments.

[0016] This embodiment proposes a method for preparing materials for enriching cesium, including: (1) Add eluent X to the waste, add modifier G under shaking conditions, and mix evenly for a period of time to obtain solution R; (2) Add precipitant C to the solution R obtained in step (1), use ultrasound to treat for a period of time, cool to room temperature after the reaction is complete, filter to obtain solid, and then wash and dry to obtain CST, a material for high-efficiency enrichment of cesium. As a preferred embodiment, the waste in step (1) is waste containing one or more elements from iron, potassium, cobalt, nickel, titanium, tin, and zirconium. As a preferred embodiment, the eluent X in step (1) contains one or more acidic solvents in proportion, such as hydrochloric acid, nitric acid, silanonic acid, phosphoric acid, ammonium chloride, oxalic acid, and citric acid. As a preferred embodiment, the modifier G in step (1) is a solid reagent containing one or more of boron, phosphorus, molybdenum, aluminum, silicate, phosphate, and carbonate; As a preferred embodiment, the precipitant C in step (2) is an alkaline or amphoteric reagent containing one or more of the following: aluminum hydroxide, titanium oxide, ammonium carbonate, sodium bicarbonate, sodium silicate, sodium fluorosilicate, etc.

[0017] Example 1 (1) Eluent X (composed of 6% hydrochloric acid and 0.5% oxalic acid in a volume ratio of 7:3) was added to industrial sludge waste containing iron, nickel and titanium elements, with a solid-liquid ratio of 1:10. Modifier G (a mixture of ammonium molybdate and sodium silicate in a mass ratio of 1:2) was added under shaking conditions of 60℃ and 150 rpm, and after uniform mixing and reaction for 120 minutes, solution R was obtained.

[0018] (2) Add precipitant C dropwise to the solution R obtained in step (1) (precipitant C is a mixture of 10% sodium silicate aqueous solution and saturated ammonium carbonate solution in a volume ratio of 1:1), and treat with an ultrasonic processor with a power of 300W for 60 minutes. After the reaction system cools naturally to room temperature, filter it, and wash the obtained solid three times with deionized water and anhydrous ethanol in sequence. Finally, dry it in a vacuum drying oven at 80℃ for 12 hours to obtain a powdered cesium-enriched material, denoted as CST-1.

[0019] Example 2 (1) Eluent X (eluent X is a mixed aqueous solution of 20% nitric acid and 10% phosphoric acid) was added to the waste catalyst powder containing potassium, cobalt and zirconium elements, with a solid-liquid ratio of 1:15. Modifier G (modifier G is a mixture of diammonium hydrogen phosphate, borax and sodium silicate in a mass ratio of 3:1:3) was added under room temperature and shaking conditions of 200 rpm. After uniform mixing and reaction for 90 minutes, suspension R was obtained.

[0020] (2) The solution R obtained in step (1) was transferred to a reaction vessel, and precipitant C (precipitant C is a mixture of nano-aluminum hydroxide colloid and 5% sodium fluorosilicate aqueous solution) was added. The mixture was then treated at 80°C for 90 minutes using an ultrasonic processor with a power of 400W. After the reaction was completed, the mixture was cooled to room temperature, filtered, and the resulting solid was washed with hot water until the filtrate was neutral. The solid was then dried at 105°C for 6 hours to obtain particulate cesium-enriched material, denoted as CST-2.

[0021] Example 3 (1) Add eluent X (eluent X is a mixed aqueous solution of 40% citric acid and 5% ammonium chloride) to metallurgical slag containing iron and tin elements, with a solid-liquid ratio of 1:8. Under shaking conditions of 75℃ and 180 rpm, add modifier G (modifier G is a solid mixture of phosphomolybdic acid and light magnesium carbonate), and after uniform mixing and reaction for 150 minutes, obtain a clear solution R.

[0022] (2) Slowly add precipitant C (precipitant C is a mixture of titanium dioxide sol and sodium bicarbonate saturated solution) to the solution R obtained in step (1), and treat with an ultrasonic processor with a power of 350W for 45 minutes. After the reaction is complete, allow it to stand and cool, filter, wash the resulting gel-like solid twice with anhydrous ethanol, dry it at 60°C for 24 hours, grind it to obtain a porous cesium-enriched material, denoted as CST-3.

[0023] The adsorption and removal effects of CST-1, CST-2, and CST-3 prepared in Examples 1-3 on wastewater with an initial cesium concentration of 250 mg / L were compared, and the statistical results are shown in Table 1.

[0024] Table 1

[0025] As shown in Table 1, the CST material prepared by this invention efficiently reduces the cesium concentration to 2-5 mg / L under 250 ml / L wastewater conditions, achieving a removal rate of over 98%. Simultaneously, the raw materials are derived from industrial solid waste containing elements such as iron, potassium, cobalt, and nickel, resulting in low cost and high-value resource utilization of solid waste. The preparation process is simple and efficient, requiring no high-temperature calcination, reducing energy consumption through ultrasonic-assisted isothermal conditions, and using environmentally friendly extractants and precipitants, minimizing negative environmental impacts. Therefore, this invention improves cesium enrichment efficiency while being economical, environmentally friendly, and resource-recycling, meeting the requirements of sustainable development.

[0026] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the specific implementation of the present invention. Any modifications or equivalent substitutions that do not depart from the spirit and scope of the present invention should be covered within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing materials for enriching cesium, characterized in that, Includes the following steps: (1) Add eluent X to the waste, add modifier G under shaking conditions, mix evenly and react for a period of time to obtain a solution or suspension R; (2) Add precipitant C to the solution or suspension R and simultaneously perform ultrasonic treatment. After the reaction is complete, cool to room temperature, filter, wash and dry to obtain cesium-enriched material CST.

2. The method according to claim 1, characterized in that, The waste mentioned in step (1) is an industrial solid waste containing one or more of the elements iron, potassium, cobalt, nickel, titanium, tin and zirconium.

3. The method according to claim 1, characterized in that, The eluent X mentioned in step (1) is an acidic solvent, selected from one or more of hydrochloric acid, nitric acid, silicic acid, phosphoric acid, ammonium chloride, oxalic acid, and citric acid in an aqueous solution mixed in proportion.

4. The method according to claim 1, characterized in that, In step (1), the solid-liquid ratio of the waste to the eluent X is 1:8 to 1:15 g / mL.

5. The method according to claim 1, characterized in that, The modifier G mentioned in step (1) is a solid reagent selected from one or more of compounds containing boron, phosphorus, molybdenum, and aluminum, silicates, phosphates, and carbonates.

6. The method according to claim 1, characterized in that, The shaking conditions in step (1) are: temperature from room temperature to 80°C, shaking speed of 150-200 rpm, and reaction time of 90-150 minutes.

7. The method according to claim 1, characterized in that, The precipitant C mentioned in step (2) is an alkaline or amphoteric reagent, selected from one or more of aluminum hydroxide, titanium dioxide, ammonium carbonate, sodium bicarbonate, sodium silicate, and sodium fluorosilicate.

8. The method according to claim 1, characterized in that, The ultrasonic treatment power in step (2) is 300-400W, the treatment time is 45-90 minutes, and the treatment temperature range is room temperature to 80℃.

9. The method according to claim 1, characterized in that, The drying conditions described in step (2) are: drying at 60-105℃ for 6-24 hours.

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