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CN-117753981-B - Controllable preparation method of micro-sized flake silver powder

CN117753981BCN 117753981 BCN117753981 BCN 117753981BCN-117753981-B

Abstract

The invention discloses a controllable preparation method of micro-sized flake silver powder, which comprises the steps of dispersing silver nitrate into deionized water, completely dissolving the silver nitrate, adding a solvent to regulate the PH value to obtain a mixed solution A, mixing a reducing agent and a bio-based dispersing agent, dispersing the mixture into the solvent, completely dissolving the mixture to obtain a mixed solution B, moving the mixed solution A into the mixed solution B, stirring the mixed solution A at room temperature for reacting for a period of time to obtain a mixed solution C, and standing, washing and drying the mixed solution C to finally obtain the micro-sized flake silver powder. The flaky micro-sized silver powder obtained by the method is regular in shape, good in dispersibility and low in cost, the adopted dispersant raw material is the bio-based platform compound 5-hydroxymethylfurfural obtained by hydrolyzing biomass resources, the environment is protected, the concept of green chemistry is met, and no extra dispersant is used in the preparation of the silver powder.

Inventors

  • YANG YU
  • CHEN YONGQIANG
  • Ai Wenying
  • LIU YUAN
  • Hang Silin
  • LI PENGYU
  • ZOU JIAWEI
  • CUI HAITAO
  • YIN LI
  • CAO ZHENFENG

Assignees

  • 中原工学院

Dates

Publication Date
20260512
Application Date
20231120

Claims (10)

  1. 1. A controllable preparation method of micro-sized flake silver powder, which is characterized by comprising the following steps: (1) Dispersing silver nitrate into deionized water, completely dissolving the silver nitrate, and adding a solvent to adjust the PH value to obtain a mixed solution A; (2) Mixing a reducing agent and a bio-based dispersing agent, dispersing the mixture into deionized water, completely dissolving the mixture to obtain a mixed solution B, transferring the mixed solution A into the obtained mixed solution B, and stirring the mixed solution A at room temperature for reacting for a period of time to obtain a mixed solution C; (3) Standing, washing and drying the mixed solution C to finally obtain micro-sized flake silver powder; the bio-based dispersant has a structural formula shown in formula I: wherein the number of carbon atoms of the linear alkyl group R is 3 to 7.
  2. 2. The controllable preparation method of micro-sized plate-like silver powder according to claim 1, wherein the concentration of silver nitrate in the mixed solution A in the step (1) is 0.1-0.2mol/L.
  3. 3. The controllable preparation method of the micro-sized plate-like silver powder according to claim 1, wherein the dissolution in the step (1) is rapid dissolution using ultrasound, the pH-adjusting added solvent is nitric acid, and the pH is adjusted to 1-4.
  4. 4. The controllable preparation method of the micro-sized plate-like silver powder according to claim 1, wherein the reducing agent in the step (2) is selected from ascorbic acid, and the molar ratio of the reducing agent to the silver nitrate is 2:1-3:1.
  5. 5. The controllable preparation method of micro-sized plate-like silver powder according to claim 1, wherein in the step (2), the concentration of the reducing agent in the mixed solution B is 0.2 to 0.3mol/L.
  6. 6. The controllable preparation method of the micro-sized plate-like silver powder according to claim 1, wherein in the step (2), the bio-based dispersant is 4wt% of the mass of the silver nitrate.
  7. 7. The controllable preparation method of the micro-sized plate-like silver powder according to claim 1, wherein the dissolution mode in the step (2) is to use ultrasound to rapidly dissolve the silver powder, the stirring is magnetic stirring, the stirring speed is 200rpm, and the reaction time is20 min.
  8. 8. The controllable preparation method of the micro-sized plate-like silver powder according to claim 1, wherein in the step (3), the washing solvent used in the washing process is selected from one or both of deionized water and ethanol, and the filtering and washing operations are repeated 3 times.
  9. 9. The controllable preparation method of the micro-sized plate-like silver powder according to claim 1, wherein the drying in the step (3) is vacuum drying, the temperature is 60 ℃ and the time is 6h.
  10. 10. The micro-sized plate-like silver powder produced by the controllable preparation method according to any one of claims 1 to 9, wherein the micro-sized plate-like silver powder has a plate-like shape and a size of 3.0 to 5.0 μm.

Description

Controllable preparation method of micro-sized flake silver powder Technical Field The application belongs to the technical field of new application of bio-based products, and particularly relates to micro-sized flake silver powder and a preparation method thereof. Background In the conductive material in the new energy field, the conductivity of the noble metal material silver is highest in metal, the cost is lowest in noble metal, and the silver has the advantages of good oxidation resistance and weldability, good adhesive force and the like. The flaky microsize silver powder has greatly improved surface activity, catalytic performance and antibacterial capability by virtue of the nano effect, and has wide application prospect in a plurality of fields. However, the precise regulation and preparation of the morphology of the flake silver powder is still one of the keys limiting the great development of the field. Based on the above, a biological base dispersing agent which takes a biological base platform compound 5-hydroxymethylfurfural as a raw material is developed through quoted patent a alpha, beta-unsaturated ketone compound, a preparation method and application (CN 114656431A), and after the research of the structure-activity relationship of the biological base dispersing agent, the biological base dispersing agent which can accurately regulate the morphology of silver powder into flaky micro-sized silver powder is obtained, and the prepared flaky silver powder has uniform morphology particle size, good dispersibility and can be accurately controlled to be about 3.0 mu m in size. The preparation method is simple, the raw materials are green and environment-friendly, the sources are wide, and the development concept of green chemistry is fully met. Disclosure of Invention The invention aims to provide a bio-based dispersing agent which is prepared by taking a bio-based platform compound 5-hydroxymethylfurfural as a raw material, wherein the dispersing agent can accurately regulate and control the morphology of silver powder into flaky micro-size silver powder in the preparation of the silver powder. The specific surface area of the flake silver powder is large, and compared with silver powder with other morphologies, the flake silver powder has better conductive performance, and because the contact area of the flake surface is larger than that of the silver powder with other morphologies, the flake silver powder has relatively low resistance value, good conductive performance and stable chemical property, the flake silver powder is the most favorable for promoting innovation and development of metal conductive materials. The micro-sized silver material prepared by the method has high conductivity, can be used as a conductive additive for preparing materials such as solar cell panels, electronic material conductive plates and the like, and can also be used as a high-conductivity material for the field of new energy. In order to solve the technical problems, the invention adopts the following technical scheme: a controllable preparation method of micro-sized flake silver powder, comprising the following steps: (1) Dispersing silver nitrate into deionized water, completely dissolving the silver nitrate, and adding a solvent to adjust the PH value to obtain a mixed solution A; (2) Mixing a reducing agent and a bio-based dispersing agent, dispersing the mixture into deionized water, completely dissolving the mixture to obtain a mixed solution B, transferring the mixed solution A into the obtained mixed solution B, and stirring the mixed solution A at room temperature for reacting for a period of time to obtain a mixed solution C; (3) And (3) standing, washing and drying the mixed solution C to finally obtain the micro-sized flake silver powder. The bio-based dispersant has a structural formula shown in formula I: wherein the number of carbon atoms of the linear alkyl group R is 3 to 7. Further, the concentration of silver nitrate in the mixed solution A in the step (1) is 0.1-0.2mol/L. Further, the dissolution in the step (1) is rapid dissolution using ultrasound, and the pH-adjusting solvent is nitric acid, and the pH is adjusted to 1-4, preferably to 2. Further, the reducing agent in the step (2) is selected from ascorbic acid, and the molar ratio of the reducing agent to the silver nitrate is 2:1-3:1. Further, in the step (2), the concentration of the reducing agent in the mixed solution B is 0.2-0.3mol/L. Further, in the step (2), the bio-based dispersant is 4wt% of the mass of the silver nitrate. Further, the dissolution mode in the step (2) is to use ultrasound to rapidly dissolve, the stirring is magnetic stirring, the stirring speed is 200rpm, and the reaction time is 20min. Further, in the step (3), the washing solvent used in the washing process is selected from one or two of deionized water and ethanol, and the filtering and washing operations are repeated for 3 times. Further, the drying in th