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CN-121988349-A - Nickel/cadmium manganese sulfur modified photocatalytic material and preparation method thereof

CN121988349ACN 121988349 ACN121988349 ACN 121988349ACN-121988349-A

Abstract

The invention relates to the technical field of preparation of photocatalytic materials, in particular to a nickel/cadmium manganese sulfur modified photocatalytic material and a preparation method thereof, wherein the preparation method comprises the following steps of S1, dissolving manganese acetate tetrahydrate, cadmium acetate dihydrate and thioacetamide in a mixed solvent of deionized water and ethylenediamine to obtain a mixed solution; S2, reacting the mixed solution obtained in the step S1 to obtain a primary product, sequentially carrying out acid and heat treatment on the natural zeolite, S4, placing the natural zeolite treated in the step S3 in a nickel chloride hexahydrate aqueous solution to obtain the natural zeolite loaded with nickel ions, and S5, adding the natural zeolite loaded with nickel ions obtained in the step S4 into an ethanol aqueous solution containing sodium chloride, and adding the primary product to react to obtain the photocatalytic material. The photocatalytic material prepared by the invention has uniform load and no agglomeration phenomenon, and effectively improves the catalytic effect of the photocatalytic material.

Inventors

  • QIAO HAIJUN
  • WANG DANJUN
  • WANG MIMI
  • JIA ZHILONG

Assignees

  • 甘肃农业大学

Dates

Publication Date
20260508
Application Date
20260410

Claims (8)

  1. 1. The preparation method of the nickel/cadmium manganese sulfur modified photocatalytic material is characterized by comprising the following steps of: s1, dissolving manganese acetate tetrahydrate, cadmium acetate dihydrate and thioacetamide in a mixed solvent of deionized water and ethylenediamine, and uniformly stirring to obtain a mixed solution; s2, adding the mixed solution obtained in the step S1 into a high-pressure reaction kettle, reacting for 18-28 hours at 180-220 ℃, and obtaining a primary product after centrifugal collection, washing and drying to constant weight; S3, placing the natural zeolite into a hydrochloric acid solution for stirring reaction for 4-8min, and placing the natural zeolite after hydrochloric acid treatment into an oven for treatment at 160-200 ℃ for 30-40min; s4, placing the natural zeolite treated in the step S3 into a nickel chloride hexahydrate aqueous solution for stirring reaction for 3-5 hours, and then centrifugally filtering to obtain the natural zeolite loaded with nickel ions; S5, adding the natural zeolite loaded with nickel ions obtained in the step S4 into an ethanol water solution containing sodium chloride, then adding the primary product obtained in the step S2, continuously reacting for 20-28h at 30-40 ℃, separating out the product, and drying the product at 80-90 ℃ for 2-4h to obtain the photocatalytic material.
  2. 2. The method for preparing the nickel/cadmium manganese sulfur modified photocatalytic material according to claim 1, wherein the molar ratio of manganese acetate tetrahydrate, cadmium acetate dihydrate and thioacetamide in the step S1 is 1 (2-2.4): 4-4.3.
  3. 3. The method for preparing a nickel/cadmium manganese sulfur modified photocatalytic material according to claim 1, wherein the volume ratio between deionized water and ethylenediamine in the step S1 is 1:1.
  4. 4. The method for preparing a nickel/cadmium manganese sulfur modified photocatalytic material according to claim 1, wherein the pH of the hydrochloric acid solution in step S3 is 2 to 3.
  5. 5. The method for preparing a nickel/cadmium manganese sulfur modified photocatalytic material according to claim 1, wherein the concentration of nickel chloride hexahydrate in the aqueous solution of nickel chloride hexahydrate in the step S4 is 0.04-0.08mol/L.
  6. 6. The method for preparing a nickel/cadmium manganese sulfur modified photocatalytic material according to claim 1, wherein the ratio between the mass of the aqueous solution of nickel chloride hexahydrate in step S4 and the mass of the natural zeolite not treated with the hydrochloric acid solution in step S3 is 40:1.
  7. 7. The method for preparing a nickel/cadmium manganese sulfur modified photocatalytic material according to claim 1, wherein the mass ratio between the nickel ion-loaded natural zeolite and the primary product in the step S5 is (12-20): 1.
  8. 8. A nickel/cadmium manganese sulfur modified photocatalytic material prepared by the method for preparing a nickel/cadmium manganese sulfur modified photocatalytic material according to any one of claims 1-7.

Description

Nickel/cadmium manganese sulfur modified photocatalytic material and preparation method thereof Technical Field The invention relates to the technical field of preparation of photocatalytic materials, in particular to a nickel/cadmium manganese sulfur modified photocatalytic material and a preparation method thereof. Background The Transition Metal Chalcogenides (TMCs) have broad prospects in solar-driven Hydrogen Evolution Reactions (HER) due to their unique electronic structure and good light absorption capabilities. Cadmium sulfide (CdS) has a proper band gap (2.4 eV) and conduction band position (about-0.5V vs. NHE), and meets the thermodynamic requirement of water reduction. However, its application is limited by low surface active site density, poor crystal plane reaction efficiency, and rapid charge recombination. To overcome these challenges, elemental doping (e.g., mn) can effectively regulate the electronic structure of CdS. The similar ionic radii of Mn 2+ and Cd 2+ favor the formation of solid solutions. Meanwhile, nickel (Ni) monoatoms have excellent intrinsic HER activity due to their favorable electron configuration. Thus, co-incorporation of Mn and Ni into CdS is expected to synergistically enhance photocatalytic performance. Therefore, according to the characteristic of the material, mn and Ni are jointly introduced into Cds to obtain the photocatalytic material, and meanwhile, when Ni is introduced into the prepared material, nickel ions loaded by the prepared material are desorbed into the solution through the characteristic of natural zeolite, so that the problem of agglomeration caused by overhigh local ion concentration in the solution and the problem of reduced catalytic performance are solved. Disclosure of Invention The invention aims to provide a nickel/cadmium manganese sulfur modified photocatalytic material and a preparation method thereof, which are used for solving the problems in the background technology. In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the nickel/cadmium manganese sulfur modified photocatalytic material comprises the following steps: s1, dissolving manganese acetate tetrahydrate, cadmium acetate dihydrate and thioacetamide in a mixed solvent of deionized water and ethylenediamine, and uniformly stirring to obtain a mixed solution; s2, adding the mixed solution obtained in the step S1 into a high-pressure reaction kettle, reacting for 18-28 hours at 180-220 ℃, and obtaining a primary product after centrifugal collection, washing and drying to constant weight; S3, placing the natural zeolite into a hydrochloric acid solution for stirring reaction for 4-8min, and placing the natural zeolite after hydrochloric acid treatment into an oven for treatment at 160-200 ℃ for 30-40min; s4, placing the natural zeolite treated in the step S3 into a nickel chloride hexahydrate aqueous solution for stirring reaction for 3-5 hours, and then centrifugally filtering to obtain the natural zeolite loaded with nickel ions; S5, adding the natural zeolite loaded with nickel ions obtained in the step S4 into an ethanol water solution containing sodium chloride, then adding the primary product obtained in the step S2, continuously reacting for 20-28h at 30-40 ℃, separating out the product, and drying the product at 80-90 ℃ for 2-4h to obtain the photocatalytic material (Ni/Mn-CdS). Further, in the step S1, the molar ratio of manganese acetate tetrahydrate, cadmium acetate dihydrate and thioacetamide is 1 (2-2.4): 4-4.3. Further, in the step S1, the volume ratio between deionized water and ethylenediamine is 1:1. Further, the pH of the hydrochloric acid solution in the step S3 is 2-3. Further, the concentration of the nickel chloride hexahydrate in the aqueous solution of the nickel chloride hexahydrate in the step S4 is 0.04-0.08mol/L. Further, the ratio of the mass of the aqueous solution of nickel chloride hexahydrate in the step S4 to the mass of the natural zeolite not treated with the hydrochloric acid solution in the step S3 is 40:1. Further, the mass ratio between the nickel ion-loaded natural zeolite and the primary product in the step S5 is (12-20): 1. The nickel/cadmium manganese sulfur modified photocatalytic material is prepared by the preparation method of the nickel/cadmium manganese sulfur modified photocatalytic material. Compared with the prior art, the invention has the following beneficial effects: 1. according to the invention, mn and Ni are jointly introduced into CdS to obtain the composite photocatalytic material, so that the catalytic performance of the material is improved; 2. According to the invention, mn and Cd are synthesized by a one-step hydrothermal method, mn is uniformly doped in CdS, and nickel ions are slowly released into the reaction system through the desorption of natural zeolite on metal ions when Ni is introduced, so that the agglomeration phenomenon caused by