Method for preparing micronano silver particles in aqueous solution system

A technology of micro-nano silver and aqueous solution, which is applied in the field of preparing micro-nano silver particles, can solve problems such as the need for heating or high-temperature hydrothermal reaction, and achieve the effects of high yield, uniform particle size distribution and simple preparation method.

Active Publication Date: 2021-10-26
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the above prior art, the preparation of micro-nano silver particles mostly adopts high molecular polymers such as polyvinylpyrrolidone or polyacrylamide as surface protection agent and dispersant, and what reducing agent used is ascorbic acid, ferrous sulfate, amino acid, o-phthalic acid, etc. Diphenol, hydrogen peroxide, ethylene glycol, polyvinylpyrrolidone, etc., some processes require heating or high-temperature hydrothermal reaction; some reaction processes need to use acid and alkali to adjust the pH value, or use two reducing agents for step-by-step reduction Response and other cumbersome processes
Instead of using high molecular polymer as surface protection agent and dispersant, and using hydrazine hydrate as reducing agent at room temperature to prepare flower-shaped micro-nano silver particles with clean surface, there is no report

Method used

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  • Method for preparing micronano silver particles in aqueous solution system
  • Method for preparing micronano silver particles in aqueous solution system
  • Method for preparing micronano silver particles in aqueous solution system

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Weigh trisodium citrate and dissolve it in deionized water to prepare an aqueous solution of trisodium citrate with a concentration of 0.11 g / mL. Dissolve silver nitrate in deionized water to prepare a silver nitrate aqueous solution with a concentration of 0.5 g / mL. Take 40mL of trisodium citrate aqueous solution and 10mL of silver nitrate aqueous solution and mix first, and stir for 30min to obtain a uniform silver complex solution, which is a silver precursor solution. Hydrazine hydrate was added into deionized water to prepare a hydrazine hydrate reducing agent solution with a concentration of 6%. Then 50mL of reducing agent solution and 50mL of silver precursor solution were added dropwise to 200mL of water with a metering pump for a mixed reaction. The addition time was 15min, and then at a temperature of 10°C, under stirring at 600 rpm, the reaction was continued for 60min. , to obtain a uniform brown-black solution, and to obtain silver particles after post-tre...

Embodiment 2

[0041] Weigh trisodium citrate and dissolve it in deionized water to prepare an aqueous solution of trisodium citrate with a concentration of 0.16 g / mL. Dissolve silver nitrate in deionized water to prepare a silver nitrate aqueous solution with a concentration of 0.1 g / mL. Take 50mL of trisodium citrate aqueous solution and 50mL of silver nitrate aqueous solution and mix first, and stir for 30min to obtain a uniform silver complex solution, which is a silver precursor solution. Hydrazine hydrate was added into deionized water to prepare a 4% hydrazine hydrate reducing agent solution. Then 100mL of reducing agent solution and 100mL of silver precursor solution were added dropwise to 100mL of water with a metering pump for a mixed reaction, the addition time was 25min, and then at a temperature of 20°C, under stirring at 600 rpm, the stirring reaction was continued for 60min. A uniform brown-black solution is obtained, and silver particles are obtained after post-treatment, su...

Embodiment 3

[0043] Weigh disodium edetate and dissolve it in deionized water to prepare a disodium edetate aqueous solution with a concentration of 0.06 g / mL. Dissolve silver nitrate in deionized water to prepare a silver nitrate aqueous solution with a concentration of 0.1 g / mL. Mix 60 mL of disodium edetate aqueous solution with 50 mL of silver nitrate aqueous solution, and stir for 30 minutes to obtain a uniform silver complex solution, which is a silver precursor solution. Hydrazine hydrate was added into deionized water to prepare a hydrazine hydrate reducing agent solution with a concentration of 5%. Then 110mL of reducing agent solution and 110mL of silver precursor solution were added dropwise to 80mL of water with a metering pump for a mixed reaction. The addition time was 30min, and then at a temperature of 15°C, under stirring at 600 rpm, the stirring reaction was continued for 60min. The reaction is over. Then wash 2 times three times with water, and obtain silver particles ...

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Abstract

The invention relates to a method for preparing micro-nano silver particles in an aqueous solution system, comprising the following steps: mixing an aqueous silver salt solution with an aqueous solution of a complexing agent to obtain a silver complex precursor solution, and then adding and mixing the aqueous solution of a reducing agent simultaneously to carry out One-step reduction reaction to obtain micronano silver particles. The invention reacts in aqueous solution under normal temperature and pressure, does not use high molecular polymer as protective agent and dispersant, and uses hydrazine hydrate as reducing agent to reduce silver complex precursor. The preparation method is simple, avoids the residue of the high molecular polymer on the surface of the silver powder, and the prepared flower-shaped micro-nano silver particles have regular appearance, uniform particle size distribution, good dispersibility, controllable size and high yield.

Description

technical field [0001] The invention discloses a method for preparing micronano silver particles in an aqueous solution system, and belongs to the field of preparation of micronano material silver. Background technique [0002] Silver micro-nano materials have unique physical and chemical properties, and have broad application prospects in the fields of electricity, catalysis, magnetism and SERS spectroscopy. The properties of silver micro-nano materials are closely related to factors such as shape, size and structure. In recent years, nanoparticles and nanomaterials have become one of the research hotspots in the field of material science. The research and development of micro-nano silver in my country started in the early 1960s, and entered a stage of rapid development in the 1980s and 1990s. During this period, the government invested heavily, and many units participated in the research of silver powder preparation technology, and produced many series of silver powder. ,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24
CPCB22F9/24
Inventor 陈代荣田尚玲焦秀玲
Owner SHANDONG UNIV
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