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Method for preparing electronic grade titania ultrafine powder through gas phase oxidation process

A titanium dioxide, gas-phase oxidation technology, applied in the direction of titanium dioxide, preparation with chloride, chemical instruments and methods, etc., can solve the problem of high technical level and process parameter control requirements of titanium dioxide ultrafine powder, affecting product use effect and application range, product The problem of poor dispersion and other problems can improve the market competitiveness of products, high sphericity, and good particle size consistency.

Active Publication Date: 2017-08-04
SANXIANG ADVANCED MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to ultrafine TiO 2 The particles are small, the specific surface area is large, and the surface energy is high. During the drying and calcination process, it is easy to cause agglomeration, especially hard agglomeration, which makes the dispersibility of the product worse and affects the use effect and application range of the product. There are many processes in the liquid phase method. Production The process is complicated and the preparation cost is high; the technical level and process parameter control requirements for the production of titanium dioxide ultrafine powder by gas phase method are high, and the quality of the obtained product is good. The electrical performance still needs to be improved, which limits its further development in the fields of thermistor / varistor, semiconductor capacitor and battery material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. The titanium tetrachloride with a purity of 99.99wt% and the vanadium tetrachloride of 99.9wt% are batched according to the mass percentage 1:0.035, and preheated to 480 ° C in a closed preheating furnace to obtain titanium chloride and chloride Mixed vapor of vanadium;

[0028] 2. Heating oxygen with a purity ≥99.9wt% to 1580°C in an oxygen heating furnace;

[0029] 3. Spray the mixed steam of titanium chloride and vanadium chloride and oxygen into the oxidation reactor through a spray gun to carry out gas-phase oxidation reaction at high temperature, react for 7 minutes, and generate a mixture of titanium dioxide particles containing vanadium oxide and chlorine gas;

[0030] 4. Rapid cooling of the product in the oxidation reactor, so that titanium dioxide particles and chlorine gas and solid are separated;

[0031] 5. The chlorine gas produced is absorbed by liquid alkali to make by-products such as sodium hypochlorite;

[0032] 6. Titanium dioxide particles in ...

Embodiment 2

[0035] 1. The titanium tetrachloride with a purity of 99.99wt% and the vanadium tetrachloride of 99.9wt% are batched according to the mass percentage 1:0.056, and preheated to 500°C in a closed preheating furnace to obtain titanium chloride and chloride Mixed vapor of vanadium;

[0036] 2. Heating oxygen with a purity ≥99.95wt% to 1550°C in an oxygen heating furnace;

[0037] 3. Spray the mixed steam of titanium chloride and vanadium chloride and oxygen into the oxidation reactor through a spray gun to carry out gas-phase oxidation reaction at high temperature, react for 6 minutes, and generate a mixture of titanium dioxide particles containing vanadium oxide and chlorine;

[0038] 4. Rapid cooling of the product in the oxidation reactor, so that titanium dioxide particles and chlorine gas and solid are separated;

[0039] 5. The chlorine gas produced is absorbed by liquid alkali to make by-products such as sodium hypochlorite;

[0040] 6. Titanium dioxide particles in the d...

Embodiment 3

[0043] 1. The titanium tetrachloride with a purity of 99.99wt% and the vanadium tetrachloride of 99.9wt% are batched according to the mass percentage 1: 0.075, and preheated to 520 ° C in a closed preheating furnace to obtain titanium chloride and chloride Mixed vapor of vanadium;

[0044] 2. Heating oxygen with a purity ≥99.9wt% to 1510°C in an oxygen heating furnace;

[0045]3. Spray the mixed steam of titanium chloride and vanadium chloride and oxygen into the oxidation reactor through a spray gun to carry out gas-phase oxidation reaction at high temperature, react for 10 minutes, and generate a mixture of titanium dioxide particles containing vanadium oxide and chlorine;

[0046] 4. Rapid cooling of the product in the oxidation reactor, so that titanium dioxide particles and chlorine gas and solid are separated;

[0047] 5. The chlorine gas produced is absorbed by liquid alkali to make by-products such as sodium hypochlorite;

[0048] 6. Titanium dioxide particles in the...

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Abstract

The invention relates to a method for preparing electronic grade titania ultrafine powder through a gas phase oxidation process. The method comprises the following steps: reacting titanium chloride vapor, vanadium chloride vapor and oxygen under high-temperature conditions at the temperature of 1500 DEG C or higher so as to obtain a mixture of titania particles containing vanadium oxide and chlorine; performing gas-solid separation on the titania particles and the chlorine, thereby obtaining the electronic grade titania ultrafine powder. The method disclosed by the invention is different from the conventional technology and is short in process procedures, low in production cost and less in environmental pollution, and the produced product is low in impurity content, high in rutile content, high in granularity consistency and high in degree of sphericity. Since a certain ratio of vanadium oxide is introduced into the gas phase oxidation reaction process, the dielectric constant, electrical conductivity and other electrical properties of the titania are greatly improved, the stability of an electronic device is improved, and the operating performance and stability of the titania ultrafine powder in the fields of thermal / pressure sensitive resistors, semiconductor capacitors, battery materials and the like are enhanced.

Description

technical field [0001] The invention relates to the technical field of inorganic materials and electronic materials, in particular to a method for preparing electronic-grade titanium dioxide ultrafine powder by gas phase oxidation. Background technique [0002] Titanium dioxide is one of the important metal oxides, widely used in industries such as military, rubber, plastic, paper, ink, chemical fiber and cosmetics. High-purity titanium dioxide ultrafine powder is widely used in the fields of thermistor / varistor, semiconductor capacitor and battery due to its characteristics of semiconductor performance, high dielectric constant and resistivity. At present, the preparation methods of electronic grade titanium dioxide ultrafine powder mainly include liquid phase method and gas phase method. Titanium dioxide nanopowder is prepared by chemical reaction in the liquid phase, and the liquid phase method is also the main method for industrially preparing high-purity titanium dioxi...

Claims

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Application Information

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IPC IPC(8): C01G23/07C01G31/02C01B7/03C01B11/06B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B7/03C01B11/062C01G23/07C01G31/02C01P2004/64C01P2006/80
Inventor 包晓刚叶旦旺颜玉萍范志强张高平
Owner SANXIANG ADVANCED MATERIALS
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