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Hydrothermal reaction device for synthesis of inorganic nanoparticles

A hydrothermal reaction and microparticle technology, applied in chemical/physical/physical chemistry fixed reactors, methods of chemically changing substances by atmospheric pressure, chemical instruments and methods, etc. Reactor blockage, uneven mixing of raw materials, etc.

Active Publication Date: 2015-10-14
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of using the inorganic nanoparticles of the above-mentioned device, because the raw materials are not fully mixed before entering the reactor, and the concentration of the raw materials transported into the reactor by each high-pressure pump is different, it is easy to cause the blockage of the reactor; in addition, because the raw materials Inadequate mixing before entering the reactor, resulting in uneven mixing of raw materials and poor compositional uniformity of the prepared inorganic nanoparticles

Method used

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  • Hydrothermal reaction device for synthesis of inorganic nanoparticles
  • Hydrothermal reaction device for synthesis of inorganic nanoparticles
  • Hydrothermal reaction device for synthesis of inorganic nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] LiMnPO 4 Preparation of microparticles

[0032] With LiOH aqueous solution as lithium source, MnSO 4 As a source of iron, H 3 PO 4 As a phosphorus source, add it to the raw material tank according to Li: Fe: P = 3: 1: 1. At the same time, add 25% (molar ratio) ascorbic acid solution as a reducing protection agent. After fully stirring and mixing in the raw material tank, pass the raw material The conveying pump is transported to the air pressurizer. The compressed air pressure of the air pressurizer is 30MPa, and at the same time, it is uniformly stirred. The pressurized and homogenized raw materials pass through the high-pressure reactor with a temperature of 370°C continuously. The reacted raw materials Inorganic nanoparticles are obtained through a cooling device and a continuous filtering device.

[0033] The inorganic nanoparticles prepared in this example were subjected to XRD test, scanning electron microscope test and particle distribution test respectively....

Embodiment 2

[0035] ZrO 2 Preparation of microparticles

[0036] Prepare 0.4mol of ZnOCl 2 Solution, 1mol NaOH solution;

[0037] Under normal pressure and room temperature, the ZnOCl 2 Add the solution into the raw material tank, add NaOH solution dropwise, and control the pH at 11. After being fully stirred and mixed in the raw material tank, it is then transported to the air booster through the raw material delivery pump. The compressed air pressure of the air booster is 28MPa. Stir uniformly at the same time, the pressurized and homogenized raw materials are continuously passed through a high-pressure reactor with a temperature of 400° C., and the reacted raw materials are passed through a cooling device and a continuous filtering device to obtain inorganic nanoparticles.

[0038] Adopt the method identical with embodiment 1 to test, the result shows, what the present embodiment prepares is good dispersibility 50nm spherical ZrO 2 .

Embodiment 3

[0040] BaTiO 3 Preparation of microparticles

[0041] At normal pressure and room temperature, 0.44 mol of BaNO 3 and 0.4TiCl 4 The solution (according to the ratio of Ba / Ti=1.1) is added to the raw material tank, and the alkali solution NaOH is added to adjust the pH value at 13.2. After being fully stirred and mixed in the raw material tank, it is then transported to the air press by the raw material delivery pump In the process, the compressed air pressure of the air pressurizer is 25MPa, and it is uniformly stirred at the same time. The pressurized and homogenized raw materials pass through the high-pressure reactor with a temperature of 370°C continuously, and the reacted raw materials pass through the cooling device and continuous filtering device. Inorganic nanoparticles are obtained.

[0042] The same method as in Example 1 was used to test, and the results showed that what was prepared in this example was 50nm flake BaTiO with good dispersibility. 3 product.

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Abstract

The invention discloses a hydrothermal reaction system for inorganic nanoparticle synthesis. The hydrothermal reaction system comprises a material mixing and pressurization system, a heating reaction system, a cooler and a filter which are sequentially connected, the material mixing and pressurization system comprises a material tank, a material transfer pump and an air pressurizer with a first agitator which are sequentially connected, and the outlet of the air pressurizer is connected with the inlet of the heating reaction system. Compared with the prior art, the hydrothermal reaction system adopts the air pressurizer with the first agitator, so that materials can be sufficiently mixed in the air pressurizer before entering the heating reaction system, consequently, the blockage of a reactor, which is caused by the ununiform mixing of the materials, is prevented, and meanwhile, the components of prepared inorganic nanoparticles are uniform. An experiment result shows that the components of the inorganic nanoparticles prepared by the hydrothermal reaction system for inorganic nanoparticle synthesis provided by the invention are uniform and that the dispersibility of the inorganic nanoparticles is good.

Description

technical field [0001] The invention relates to the technical field of nanomaterial reactors, and more specifically relates to a hydrothermal reaction device for synthesizing inorganic nanoparticles. Background technique [0002] Inorganic nanoparticles refer to metal, ceramic, semiconductor and other material particles with a size between 1 and 100nm. Compared with bulk solid materials, they have obvious surface effects, small size effects and macroscopic quantum tunneling effects. They have been widely used in ceramics, Semiconductors, pigments and catalysts and other fields. According to different uses, the uniformity, high dispersion and morphology of inorganic nanoparticles become important factors affecting the performance of inorganic nanoparticles. The commonly used preparation methods of inorganic nanomaterials include sol-gel method, conventional hydrothermal method, co-precipitation method, gas phase method and hydrolysis method, etc. Among these synthesis method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J3/02B01J19/18
Inventor 刘兆平夏永高周旭峰
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI