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Hydrolysis method for producing electronic-grade special titanium white by sulfuric acid process

An electronic grade titanium dioxide technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of large half-peak width, unable to control the average particle size of titanium dioxide, unable to meet the requirements of electronic grade special titanium dioxide, etc. Low, narrow particle size distribution, good economic and social benefits

Active Publication Date: 2013-01-16
PANGANG GROUP VANADIUM TITANIUM & RESOURCES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Under the background of this application, the inventor of the present invention intends to achieve the purpose of producing special titanium dioxide products (high-purity titanium dioxide) for electronics by improving the hydrolysis process in the sulfuric acid method, but by adjusting the concentration of the titanium solution, the heating process, and the iron content of the titanium solution Titanium ratio (Fe / TiO 2 ) After investigation, it is found that the average particle size of titanium dioxide cannot be controlled at 800-1200nm, and the half-peak width is also very large, which cannot meet the requirements of electronic grade special titanium dioxide.

Method used

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  • Hydrolysis method for producing electronic-grade special titanium white by sulfuric acid process
  • Hydrolysis method for producing electronic-grade special titanium white by sulfuric acid process
  • Hydrolysis method for producing electronic-grade special titanium white by sulfuric acid process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 245ml of deionized water is added in the hydrolysis pot as the bottom water, and the bottom water is preheated to 95°C, and the concentration is 162g / l (with TiO 2 meter), preheat to 80°C, add 1000ml of titanium ore titanium liquid into the hydrolysis pot at a constant speed within 12 minutes. After the feeding is complete, the hydrolysis system is heated to the first boiling point (about 103° C.), and the heating rate is maintained at 0.8° C. / min, and the heating time is 15 minutes, and the system is kept in a slightly boiling state. When the system turns steel gray (that is, the gray point), keep this state for 5 minutes, stop heating and stirring, and ripen for 25 minutes. After aging, raise the temperature of the system to the second boiling point (about 106.5°C) under stirring, keep the heating rate at 1.0°C / min, and the heating time for 16 minutes, and keep the system in a slightly boiling state, and stop the hydrolysis after 3.0 hours. The obtained hydrolyzed ma...

Embodiment 2

[0063] Add 333.3ml of deionized water into the hydrolysis pot as the bottom water, and preheat the bottom water to 95°C. 2 meter), preheat to 75°C, add 1000ml of titanium slag and titanium solution into the hydrolysis pot at a constant speed within 17.5min. After the feeding is complete, the hydrolysis system is heated to the first boiling point (about 104.5° C.), and the heating rate is maintained at 0.6° C. / min. The heating time is 28 minutes, and the system is kept in a slightly boiling state. When the system turns steel gray (that is, the gray point), keep this state for 12 minutes, stop heating and stirring, and ripen for 30 minutes. After aging, raise the temperature of the system to the second boiling point (about 107°C) under stirring, keep the heating rate at 2.0°C / min, and the heating time for 9 minutes, and keep the system in a slightly boiling state, and stop the hydrolysis after 2.5 hours. The obtained hydrolyzed material is pickled, bleached, washed with water, ...

Embodiment 3

[0066] Add 300ml of deionized water into the hydrolysis pot as the bottom water, and preheat the bottom water to 88°C, and make the concentration 175g / l (with TiO 2 (meter), preheat to 88°C, mix 1000ml of slag ore with titanium solution, and add it into the hydrolysis pot at a constant speed within 20 minutes. After the feeding is complete, the hydrolysis system is heated to the first boiling point (about 104° C.), and the heating rate is maintained at 1.3° C. / min, and the heating time is 10 minutes to maintain the system in a slightly boiling state. When the system turns steel gray (that is, the gray point), keep this state for 25 minutes, stop heating and stirring, and ripen for 20 minutes. After aging, raise the temperature of the system to the second boiling point (about 107°C) under stirring, keep the heating rate at 2.3°C / min, and the heating time for 7 minutes, and keep the system in a slightly boiling state, and stop the hydrolysis after 2.8 hours. The obtained hydrol...

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Abstract

The invention belongs to the field of chemical industry and relates to a hydrolysis method for producing electronic-grade special titanium white by a sulfuric acid process. The technical problem to be solved is that the electronic-grade special titanium white with narrow particle size distribution and low impurity content is prepared by the sulfuric acid process. The method improves the hydrolysis method in the sulfuric acid process, and the improved hydrolysis method comprises the following steps of: A, adding titanium liquid with the concentration of 140 to 190g / L which is preheated to the temperature of between 75 and 95 DEG C into water which is preheated to the temperature of between 80 and 95 DEG C; B, heating the system to boil, and keeping the system boiling; C, when the hydrolysis system becomes steel grey, continuously keeping boiling for 5 to 25 minutes, stopping heating and stirring, and curing; and D, heating the system to boil with stirring, and keeping the system slightly boiling until the hydrolysis is finished. The obtained titanium white has the mean grain size of 800 to 1,200nm, the half-peak width of 70 to 98nm, narrow range of particle size distribution and low impurity content, and can be used as electronic-grade special titanium white.

Description

technical field [0001] The invention relates to a hydrolysis method in the production of special electronic-grade titanium dioxide by a sulfuric acid method, which belongs to the field of chemical industry. Background technique [0002] Electronic-grade special titanium dioxide (high-purity titanium dioxide) is one of the main crystal phase raw materials for new electronic components, and is widely used in PTC thermistors, MLCCs, semiconductor capacitors, semiconductor ceramics and piezoelectric ceramics and other fields. As one of the main raw materials for the manufacture of such electronic materials, high-purity titanium dioxide belongs to electronic chemicals. It not only has chemical characteristics, that is, requirements for purity and impurities, but also requires physical characteristics and practical tests. The chemical properties of high-purity titanium dioxide refer to its purity and impurity element content; while the physical properties mainly include its partic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053
Inventor 罗志强杜剑桥陈新红马维平程晓哲
Owner PANGANG GROUP VANADIUM TITANIUM & RESOURCES
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