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Supercritical hydrothermal synthesis method of nano metal or nano metal oxide particles

An oxide particle, nano metal technology, applied in nanotechnology, metal processing equipment, copper oxide/copper hydroxide, etc., can solve the problems of large particle growth, abnormal particle growth, production pollution, etc., and achieve high purity and dispersibility. Good, small particle size effect

Inactive Publication Date: 2014-07-23
XI AN JIAOTONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Physical methods include mechanical grinding and physical vapor deposition. The disadvantages are complex process equipment, low output, and difficulty in large-scale production.
The microemulsion method and the spray pyrolysis method generally have to undergo high-temperature heat treatment, which causes the particles to easily agglomerate and cause abnormal particle growth.
However, the conventional hydrothermal method has a long reaction cycle, usually requiring several hours or even several days of reaction time, which inevitably leads to the problem of larger particle growth.
The preparation of nano-metal particles by chemical electrolysis is a relatively mature and industrial production method, but the obtained metal powder usually needs to go through ball milling, sieving and other processes to finally obtain ultra-fine metal particles, and the electrolytic waste liquid contains a large amount of metal ions , arbitrary discharge will cause resource waste and environmental pollution, thus restricting the large-scale application of this method
The liquid-phase reduction method is a relatively active method for preparing nanoparticles in recent years, but this method usually requires the use of a large amount of organic solvents or highly toxic additives, which causes serious pollution in production and greatly limits its application.

Method used

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  • Supercritical hydrothermal synthesis method of nano metal or nano metal oxide particles
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  • Supercritical hydrothermal synthesis method of nano metal or nano metal oxide particles

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preparation example Construction

[0028] see figure 1 , the supercritical hydrothermal synthesis method of nanometer metal or nanometer metal oxide particle of the present invention, comprises the steps:

[0029] 1) Use pure water to dissolve the soluble metal salt to obtain a soluble metal salt solution. When preparing the soluble metal salt solution, it can be preheated to increase the solubility of the soluble metal salt.

[0030] 2) pressurize the obtained soluble metal salt solution and lye or the mixture of lye, reducing agent and organic ligand to supercritical pressure, and pre-mix the two at room temperature to obtain a supercritical hydrothermal The reaction precursor of synthetic reaction; Wherein, the addition amount of the mixture of lye or lye, reducing agent and organic ligand should make reaction precursor be neutral, and reducing agent can be hydrogen or formic acid, and it is used for the high valence state Metal ions are reduced, and the molecule of the organic ligand contains a carboxyl gr...

Embodiment 1

[0035] This embodiment takes copper sulfate supercritical hydrothermal synthesis as an example to illustrate the method of the present invention, including the following steps:

[0036] 1) Add CuSO 4 ·5H 2 O crystals (Cu(NO 3 ) 2 Crystal or CuCl 2 Crystals) were dissolved in pure water to obtain a 0.5mol / L copper sulfate (copper nitrate or copper chloride) solution;

[0037] 2) Using NaOH solution to adjust the pH value of the copper sulfate (copper nitrate or copper chloride) solution to be close to neutral, and use the obtained mixture as the reaction precursor of the supercritical hydrothermal synthesis reaction;

[0038] 3) Use a high-pressure pump to directly mix the reaction precursors generated in step 2) with pure water preheated to supercritical temperature into the supercritical hydrothermal synthesis reactor. After a period of reaction time (usually less than 1min), collect and cool , the reaction product of depressurization, using a centrifuge to separate the ...

Embodiment 2

[0042] In this embodiment, taking the preparation of nano-copper by supercritical hydrothermal synthesis of soluble copper salt as an example, the method of the present invention is described, including the following steps:

[0043] 1) Add CuSO 4 ·5H 2O crystals (Cu(NO 3 ) 2 Crystal or CuCl 2 Crystals) were dissolved in pure water to obtain a 0.5mol / L copper sulfate (copper nitrate or copper chloride) solution;

[0044] 2) Thoroughly mix the obtained copper sulfate (copper nitrate or copper chloride) solution with a mixture of NaOH solution, formic acid solution and ethylenediaminetetraacetic acid as a reaction precursor for supercritical hydrothermal synthesis;

[0045] 3) Use a high-pressure pump to directly mix the reaction precursors generated in step 2) with pure water preheated to supercritical temperature, and then enter the supercritical hydrothermal synthesis reactor. After a period of reaction time, collect the The reaction product of the nano-copper product is ...

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Abstract

The invention discloses a supercritical hydrothermal synthesis method of nano metal or nano metal oxide particles. The method includes the following steps that soluble metal salt solution and alkali liquor (or a mixture of alkali liquor, reducing agent solution and organic ligands) are fully mixed to serve as reaction precursors of supercritical hydrothermal synthesis; the reaction precursors and preheated supercritical water are pressurized and pumped into a mixer through a high-pressure pump, after temperature is raised in a direct mixing mode, supercritical hydrothermal synthesis reaction is conducted; after a period of reaction, the obtained product is cooled, centrifuged and dried, and the nano metal or nano metal oxide particles are obtained. The nano metal or nano metal nano metal oxide particles produced through the method have the advantages of being small in particle size, good in dispersibility, high in purity and the like.

Description

【Technical field】 [0001] The invention relates to a method for preparing nanoparticles, in particular to a method for supercritical hydrothermal synthesis of nanometer metal or nanometer metal oxide particles. 【Background technique】 [0002] Nano metal or nano metal oxide particles are important industrial products. Compared with ordinary metal or metal oxide powder, they have superior properties, such as large specific surface area, interface effect, quantum effect and quantum tunnel effect, etc. Endowed with various unique properties different from traditional materials and specific electrical, thermal, magnetic, optical and mechanical properties, it is widely used in various fields, such as being used as a catalyst, with small particle size, large specific surface, and particle surface Features such as large number of active centers, high catalytic efficiency and strong selectivity; in terms of sensors, it can be used as a coating film for sensors, which can greatly impro...

Claims

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Application Information

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IPC IPC(8): B22F9/24C01G3/02B82Y40/00B22F1/054
CPCB22F9/24B82Y40/00C01G3/02C01P2002/72C01P2004/04C01P2004/64B22F2999/00Y02P20/54B22F1/054B22F2202/03
Inventor 王树众周璐郭洋钱黎黎任萌萌李艳辉
Owner XI AN JIAOTONG UNIV
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