Process for preparing high-purity ultra-fine metal-oxide by solvent circulation

A technology of solvent circulation and oxide, which is applied in the field of preparation of functional inorganic materials, can solve the problems of particle ultra-fineness, environmental pollution, high carbonate purity, etc., and achieve easy control of product purity, product performance and environmental friendliness.

Inactive Publication Date: 2005-11-23
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The resulting method defect is: 1) carbonate is far less pure than ammonia, and it is easy to introduce impurities, so that the product purity is limited (the reason that ammonia precipitation cannot be used in aqueous solution is that the hydroxides of most metals are dissolved in ammonium salts. solution); 2) the adsorption of water on the surface of the particles causes hard agglomeration of the particles in the drying and calcination process; 3) because the solubility of metal hydroxides in water is much greater than that in organic solvents, it brings difficulties to the ultra-fine particle size; 4 ) produces a large amount of washing sewage, causing environmental pollution; etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take MgCl 2 ·6H 2 Add 10-50 grams of O to 100ml of methanol, stir to dissolve and filter out the insoluble matter; add 10-100ml of benzene to the filtrate and stir to mix evenly; pass into the solution under stirring conditions 100%-300% of stoichiometric ammonia The aeration time is 10-50 minutes; stop stirring after aeration, and filter the formed precipitate after aging for 0.5-3 hours, and recycle the filtrate; put the filter cake into a pressure-resistant airtight container; add 10-200ml of liquid ammonia or its derivatives; stir / shake the container for 10-30 minutes; liquid-solid separation; liquid phase recycling, solid phase at 400-600 ° C, calcined for 1.5-2 hours; the calcined powder can be obtained by crushing and dispersing The spherical magnesia superfine powder has a particle size of 50-150nm, the magnesia purity is 99.9%, and the iron content is less than 5ppm.

Embodiment 2

[0017] In Example 1, methanol was replaced with ethanol, and other processes remained unchanged. An approximately ellipsoidal magnesia superfine powder is obtained, the particle size is 20-60nm, the magnesia purity is 99.9%, and the iron content is less than 5ppm.

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Abstract

The invention relates to a process for preparing high-purity ultra-fine metal-oxide by solvent circulation, more specifically the production of hydroxides and ammonium chloride in organic phase through the reaction between metal chloride and ammonia, and the preparation and segregation method of ammonium chloride through dissolving and isolating by-product with another cheap solvent, the provided method can be applied to control the particle size of the metallic oxide to nano-micron range for control as requirement, the particle shape can be regulated from ball-shaped to fibrous forms.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional inorganic materials, and in particular relates to a method for preparing various metal oxide high-purity ultrafine materials at low cost by a solvent circulation method. Background technique [0002] High-purity ultra-fine metal oxide is one of the important and non-negligible key materials in the field of new materials. It is the basic raw material or precursor of some high-performance ceramic devices; it is the basic component of various luminescent materials such as photoluminescence and electroluminescence; It is also the main body of materials such as information storage, absorbing coatings and photocatalysis. The performance of these functional materials directly depends on the quality of their material components or precursors. Therefore, related preparation technologies have become a hot spot in the research and production fields in recent years. [0003] There are many ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/01
Inventor 宁桂玲王静慧宋奥林源
Owner DALIAN UNIV OF TECH
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