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High-pressure hydrothermal method for preparing precious metal nanometer particles and with reaction temperature controllable

A nanoparticle and reaction temperature technology, applied in the field of nanomaterials, can solve the problems of unknown pressure effect and invisible actual reaction temperature of pressure, and achieve the effects of simple steps, diversified control methods, and environmental protection.

Inactive Publication Date: 2019-08-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the value of the pressure in the ordinary hydrothermal reactor and the actual reaction temperature are invisible, and the role of pressure is also unknown

Method used

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  • High-pressure hydrothermal method for preparing precious metal nanometer particles and with reaction temperature controllable
  • High-pressure hydrothermal method for preparing precious metal nanometer particles and with reaction temperature controllable
  • High-pressure hydrothermal method for preparing precious metal nanometer particles and with reaction temperature controllable

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Prepare a gold decahedron nanomaterial, the steps are as follows:

[0032] (1) Add cetyltrimethylammonium chloride and polyvinylpyrrolidone into a glass container, then add chloroauric acid, and finally add water, stir evenly to obtain a reaction solution, and in the reaction solution, cetyl The concentration of trimethylammonium chloride is 0.23mol / L, the concentration of polyvinylpyrrolidone is 1.34 wt%, and the concentration of chloroauric acid is 3 mmol / L;

[0033] (2) Transfer the above reaction liquid into a polytetrafluoroethylene liner, then put the liner into the reaction kettle, seal the reaction kettle and fill it with nitrogen until the pressure inside the kettle is 1.00 MPa;

[0034] (3) Add the reactor to an oil bath at a temperature of 200°C, and react for 2 hours. During the reaction, the pressure gauge shows that the pressure inside the kettle is 2.0MPa (calculated, the boiling point here is 212°C);

[0035] (4) Take out the reaction kettle, take out t...

Embodiment 2

[0037] Prepare a gold decahedron nanomaterial, the steps are as follows:

[0038] (1) Add cetyltrimethylammonium chloride and polyvinylpyrrolidone into a glass container, then add chloroauric acid, then add water, stir evenly to obtain a reaction solution, and in the reaction solution, cetyl trimethyl The concentration of methyl ammonium chloride is 0.23 mol / L, the concentration of polyvinylpyrrolidone is 1.34 wt%, and the concentration of chloroauric acid is 3 mmol / L;

[0039] (2) Transfer the above reaction solution into a polytetrafluoroethylene liner, and then put the liner into the reaction kettle. After sealing the reaction kettle, fill it with nitrogen until the pressure inside the kettle is 0.50 MPa;

[0040] (3) Add the reactor to an oil bath at a temperature of 200°C for 2 hours of reaction. During the reaction, the pressure gauge shows that the pressure inside the kettle is 1.1MPa (calculated, the boiling point here is 184°C);

[0041] (4) Take out the reaction ke...

Embodiment 3

[0043] Prepare a gold decahedron nanomaterial, the steps are as follows:

[0044] (1) Add cetyltrimethylammonium chloride and polyvinylpyrrolidone into a glass container, then add chloroauric acid, then add water, stir evenly to obtain a reaction solution, and in the reaction solution, cetyl trimethyl The concentration of methyl ammonium chloride is 0.23 mol / L, the concentration of polyvinylpyrrolidone is 1.34 wt%, and the concentration of chloroauric acid is 3 mmol / L;

[0045] (2) Transfer the above reaction solution into a polytetrafluoroethylene liner, and then put the liner into the reaction kettle. Close the reactor, the pressure gauge shows a reading of 0.10 MPa;

[0046] (3) Add the reactor to an oil bath at 200 °C for 2 hours of reaction. During the reaction, the pressure gauge shows that the pressure inside the autoclave is 0.15 MPa (calculated, the boiling point here is 78 °C);

[0047] (4) Take out the reaction kettle, take out the reaction solution after cooling wi...

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Abstract

The invention discloses a high-pressure hydrothermal method for preparing precious metal nanometer particles and with the reaction temperature controllable. The method comprises the following steps offirst, mixing and evenly stirring precursors, packaging agents, reducing agents, crystal face selective agents and solvent to obtain a mixed solution; second, feeding the mixed solution into a reaction still; third, inflating the reaction still with gas, and heating the reaction still to carry out reaction; and fourth, carrying out cooling after the reaction ends, taking out the reaction mixture,and then carrying out centrifugal separation and washing to obtain the precious metal nanometer particles. According to the high-pressure hydrothermal method for preparing precious metal nanometer particles and with the reaction temperature controllable, and compared with the common hydrothermal reaction and the normal-pressure backflow reaction, the reaction temperature of an aqueous solution israised while it is achieved that the reaction temperature in a closed container is controllable, the reaction temperature and the form and size of a product can be adjusted by having control over pressure, and a new control way is provided.

Description

technical field [0001] The invention belongs to the field of nanometer materials, in particular to a high-pressure hydrothermal method with controllable reaction temperature for preparing noble metal nanoparticles. Background technique [0002] Water is used as a solvent. For non-airtight reaction devices, due to the limitation of the boiling point of water under normal pressure, the reaction temperature is generally not higher than 100 °C. As a result, many reactions that need to be carried out at higher than 100 °C cannot use water as a solvent. The conventionally used hydrothermal reaction is a closed reaction device, in which there is a certain amount of air in addition to the reaction liquid. When the reactor is in a heated state, the internal air will expand due to heat, which will generate a certain pressure, and this pressure will change with the heating temperature. Since the boiling point of water will increase with the increase of air pressure, the temperature th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/00B82Y30/00B82Y40/00
CPCB22F9/24B82Y30/00B82Y40/00B22F1/054
Inventor 胡建强陈宇宇
Owner SOUTH CHINA UNIV OF TECH