Supergravity hydrothermal preparation method of spherical inorganic powder grains

A technology of inorganic powder and supergravity, applied in the direction of inorganic chemistry, chemical instruments and methods, lead sulfide, etc., can solve the problem that it is difficult to prepare spherical powder, and achieve the effect of easy control of reaction and simple equipment

Inactive Publication Date: 2010-09-15
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the fact that the nano-powder prepared by the hydrothermal method is carried out in an unforced state, the formed powder has the characteristics of complete grain crystallization and good dispersion, and it is difficult to obtain a metastable spherical powder.

Method used

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  • Supergravity hydrothermal preparation method of spherical inorganic powder grains
  • Supergravity hydrothermal preparation method of spherical inorganic powder grains
  • Supergravity hydrothermal preparation method of spherical inorganic powder grains

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] figure 1 It is a schematic diagram of the structure of a high-gravity hydrothermal reaction equipment, in which: 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 blades, 11 for

[0047] 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; the autoclave 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

[0049] The preparation of spherical cadmium sulfide particle powder: its preparation steps are:

[0050] Step 1: Add a certain amount of cadmium chloride to 5 ml of deionized water to prepare a cadmium chloride solution with a concentration of 0.1-1mol / l;

[0051] Step 2: add a certain amount of thioacetamide in the solution of step 1, adjust the pH value to make it dissolve, and require the molar ratio of cadmium chloride and sodium thiosulfate to be 1:2;

[0052] Step 3: add 2 milliliters of bromobenzene in the solution of step 2;

[0053] 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 make the relative centrifugal force be 1000 grams, heat up to 120-150 ℃, keep warm for half an hour, and cool down. The product was taken out, washed repeatedly with carbon disulfide, ethanol and distilled water, and then dried in vacuum at 80° C. for 1 h. The morpho...

Embodiment 3

[0055] Preparation of spherical zinc sulfide particle powder: its preparation steps are:

[0056] Step 1: adding a certain amount of zinc chloride to 5 ml of deionized water to form a zinc chloride solution with a concentration of 0.1-1mol / l;

[0057] Step 2: Add a certain amount of sodium thiosulfate to the solution in step 1, adjust the pH value to dissolve it, and require the mol ratio of zinc chloride and thiocaproamide to be 1:1;

[0058] Step 3: Add 1.5 milliliters of o-dichlorobenzene to the solution in step 2;

[0059] 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 make the relative centrifugal force be 1500 grams, heat up to 120-150 ℃, keep warm for half an hour, and cool down.

[0060] The product was taken out, washed repeatedly with carbon disulfide, ethanol and distilled water, and then dried in vacuum at 80° C. for 2 h. The morphology o...

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Abstract

The invention relates to a supergravity hydrothermal preparation method of spherical inorganic powder grains, which comprises the following steps: preparing a metal salt solution at a concentration of 0.001 to 2mol/L; adding a S<2-> chemical reagent into the obtained solution, and adjusting the pH value of the solution to dissolve the S<2-> chemical reagent, wherein the molar ratio of the metal salt ions to the sulfur ions is 1:1 to 1:5; adding an organic solvent or aqueous high polymer compound into the obtained solution, wherein the volume ratio of the organic solvent or aqueous high polymer compound to the metal salt solution is 1:1 to 1:50; pouring the mixed solution into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, fixing the high-pressure reaction kettle on a fixed bracket in a hearth, and performing a hydrothermal reaction in the presence of supergravity at 50 to 250 DEG C for 0.1 to 5 hours under the action of a relative centrifugal force of 100 to 10,000 grams; and filtering the reaction product, washing the reaction product, and drying the reaction product under vacuum to obtain the needed product. The spherical inorganic powder grains prepared by the invention have the characteristics of high roundness, monodispersion and narrow distribution. The inorganic powder prepared by the method of the invention comprises ZnS, CdS, CuS, PbS, and the like. The inorganic powder grains can be used for manufacturing photonic crystals, rare earth luminescent materials, phononic crystals, solar materials, left-handed materials and the like.

Description

technical field [0001] The invention relates to a high-gravity hydrothermal preparation method of spherical inorganic powder particles. Background technique [0002] In recent years, nano or submicron spheres with monodispersity have been used more and more in high-tech fields due to their many characteristics (such as quantum effects and special optical and electrical properties, etc.), such as it can be used for Make storage and release devices in microreactors, loading and release tools for drugs, dyes and cosmetics, protectors and catalysts for bioactive macromolecules, separation of waste, and filling of materials, etc. In addition, monodisperse spheres arranged in three-dimensional order also exhibit special properties such as light and sound, and can be used to make photonic and phononic crystal materials, etc. [1-2] . At present, the research on spherical particles mainly focuses on nanometer or submicron hollow spheres, and the methods used mainly include nozzle r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G11/02C01G9/08C01G21/21C01G45/00C01G51/00C01G53/11
Inventor 李汶军陈静
Owner TONGJI UNIV
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