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Method for preparing carbonate thin film under super-gravitational and hydrothermal conditions

A high-gravity and carbonate technology, which is applied in the preparation of carbonate/acid carbonate, nanotechnology, etc., can solve the problems of no literature reports on the high-gravity hydrothermal preparation of carbonate film materials, and achieve the reaction Easy to control, simple equipment effect

Inactive Publication Date: 2011-11-23
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to overcome the above shortcomings, Li Wenjun et al. combined the characteristics of easy preparation of non-equilibrium materials under supergravity and the direct preparation of nanomaterials by hydrothermal reaction technology, and proposed a new preparation technology of thin film materials - supergravity hydrothermal reaction technology, and using this technology to successfully prepare various sulfide nano-ceramic balls, but there is no literature report on the high-gravity hydrothermal preparation of carbonate film materials

Method used

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  • Method for preparing carbonate thin film under super-gravitational and hydrothermal conditions
  • Method for preparing carbonate thin film under super-gravitational and hydrothermal conditions
  • Method for preparing carbonate thin film under super-gravitational and hydrothermal conditions

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Embodiment 1

[0026] figure 1 It is a structural diagram of a high-gravity hydrothermal reaction equipment, wherein: 1. Furnace shell, 2 insulation bricks, 3 heating wire, 4 anti-riot cylinder, 5 autoclave, 6 fixed bracket, 7 cooling water pipe, 8 rotating shaft, 9 motor, 10 wind blade and 11 temperature controller.

[0027] The structure of the equipment includes a centrifugal device, a high-pressure reaction kettle, and a temperature control furnace, wherein the centrifugal device includes a motor and a fixed bracket fixed on the motor shaft; the temperature control furnace includes a temperature controller, an electric heating wire, an insulation material and a furnace shell; Including kettle lid, kettle body and PTFE lining. The fixed bracket of the centrifugal device is located in the cavity of the temperature control furnace, and the high-pressure reaction kettle is installed on the fixed bracket of the centrifugal device.

Embodiment 2

[0029] MnCO 3 Preparation of thin film: its preparation steps are:

[0030] Step 1: add a certain amount of manganese chloride to 5 milliliters of deionized water to form a manganese chloride solution with a concentration of 0.2 mol / l;

[0031] Step 2: Add a certain amount of urea to the solution in step 1, adjust the pH value to dissolve it, and require the molar ratio of manganese chloride and urea to be 1:10;

[0032] Step 3: Add 2 milliliters of dichlorobenzene to the solution in step 2;

[0033] Step 4: Put the mixed solution in step 3 into the autoclave, seal the autoclave, and fix it on figure 1 on a fixed stand in the hypergravity reaction apparatus shown. Then heat up to 120-150°C, keep warm for half an hour, and cool down. After the reaction, the SEM photo of the resulting product is as follows figure 2 shown.

Embodiment 3

[0035] MnCO 3 Preparation of thin film: its preparation steps are:

[0036] Step 1: add a certain amount of manganese nitrate to 5 milliliters of deionized water to make a manganese nitrate solution with a concentration of 0.5 mol / l;

[0037] Step 2: Add a certain amount of urea to the solution in step 1, adjust the pH value to dissolve it, and require the molar ratio of manganese nitrate and urea to be 1:5;

[0038] Step 3: add 2 milliliters of bromobenzene in the solution of step 2;

[0039] Step 4: Put the mixed solution in step 3 into the autoclave, seal the autoclave, and fix it on figure 1 on a fixed stand in the hypergravity reaction apparatus shown. Then heat up to 120-150°C, keep warm for half an hour, and cool down. After the reaction, the SEM photo of the resulting product is as follows image 3 shown.

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Abstract

The invention relates to a method for preparing a carbonate thin film under super-gravitational and hydrothermal conditions, which comprises the specific steps of: adding a metal salt precursor into de-ionized water so as to prepare a metal salt solution with the concentration of 0.1-2 mol / L; adding a chemical reagent capable of correspondingly producing CO3<2-> at a reaction temperature between 50 DEG C and 250 DEG C into the metal salt solution; adding a water-insoluble organic solvent in which the density is more than that of the water or a water-soluble macromolecular compound in which the density is more than that of the water into the prepared solution; loading the mixed solution into a reaction kettle, fixing the sealed reaction kettle on a fixed support in a hearth, and performing hydrothermal reaction at a certain temperature in the presence of super-gravity, wherein the reaction temperature of the hydrothermal reaction is 50 DEG C to 250 DEG C, the reaction time is 0.1-5 h, and the relative centrifugal force is 500-10000 / g; after finishing reaction, filtering, repeatedly washing the filtered solid product through ethanol and water, and vacuum drying at a temperature between 30 DEG C and 100 DEG C to obtain the needed material. The method for preparing the carbonate thin film under the super-gravitational and hydrothermal conditions, disclosed by the invention, has the advantages that: (1) the prepared carbonate thin film has the characteristics of high resistance to pressure and high tenacity; and (2) equipment is simple, the reaction is easy to control, and the industrialization is easily realized.

Description

technical field [0001] The invention belongs to many high-tech fields such as battery materials, ceramics, medicine, catalysis, etc., and specifically relates to a preparation method of a carbonate film under high-gravity hydrothermal conditions. Background technique [0002] Carbonate is one of the important mineral resources, mainly including MnCO 3 , MgCO 3 、NiCO 3 , CaCO 3 They are basic resource materials with large output, mainly used in many high-tech fields such as electronics, ceramics, medicine, and catalysts. In recent years, as countries around the world attach great importance to new energy materials, especially the rapid development of power lithium batteries, the demand for carbonate materials is increasing, and the application fields are constantly expanding. At the same time, the above carbonate materials The quality also puts forward higher requirements. High-quality and refined manganese carbonate products are key manganese source materials for the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/24B82Y40/00C01B32/60
Inventor 李汶军方璐
Owner TONGJI UNIV