Green preparation technology for TiO2

A preparation process and green technology, applied in the preparation of chlorides, nanotechnology for materials and surface science, inorganic chemistry, etc., can solve the problems of poor quality of titanium dioxide, great influence of post-treatment, and long use time. Achieve the effect of easy industrial production, good dispersion and simple operation

Inactive Publication Date: 2016-06-01
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is to add lye to the titanium tetrachloride aqueous solution to produce neutralization seeds, and add oxalic acid as an auxiliary agent to produce titanium dioxide. Due to the influence of many factors such as system temperature and neutralization speed, the quality of the prepared titanium dioxide is not good; the second is Adding different crystal forms of nano-titanium dioxide as seeds to prepare rutile-type nano-titanium dioxide with a large specific surface area, but it takes too long to crystallize for 6 to 12 days
[0004] In the existing preparation of titanium dioxide, the mother liquor contains a large amount of hydrogen chloride, which is very acidic and has a great influence on the crystallization of titanium dioxide or the post-treatment of the mother liquor.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Under the condition of stirring at 200r / min, add 20mL of titanium tetrachloride dropwise to 100mL of water at a rate of 0.5mL / min, and simultaneously raise the temperature of the kettle liquid from room temperature to boiling at a rate of 2°C / min during the dropping process. Finally, react under boiling conditions for 2 hours, and cool to room temperature to obtain titanium oxide crystal slurry. Hydrogen chloride released during the process, after the white suspended particles are removed by the glass spring packed tower, is absorbed with pure water to obtain hydrochloric acid; the liquid crystal slurry in the kettle is filtered for solid-liquid separation, washed with 0.1% hydrochloric acid, and the filtrate during the filtration process is collected. The white filter cake was dried at 115°C for 24h, then calcined in a muffle furnace at 500°C for 2h, taken out and cooled to obtain white titanium dioxide powder.

Embodiment 2

[0025] Under the condition of stirring and cooling at 400r / min, 25mL of titanium tetrachloride was added dropwise to 100mL of the filtrate collected in Example 1 at a rate of 0.8mL / min, and the temperature of the kettle was controlled <40°C during the dropping process to finally obtain a clear Clear solution. Control the temperature rise rate to keep the pressure in the kettle < 5 cm of water column, until the kettle liquid boils, and maintain the boiling condition for 0.5h, and then cool to room temperature to obtain titanium oxide crystal slurry. The hydrogen chloride released during the hydrolysis process is absorbed with pure water to prepare hydrochloric acid; the liquid crystal slurry in the kettle is filtered for solid-liquid separation, washed with pure water, and the filtrate during the filtration process is collected. The white filter cake was dried at 200°C for 0.5h, then calcined in a muffle furnace at 950°C for 2h, taken out for cooling, and ground to obtain nanos...

Embodiment 3

[0027] Under the stirring condition of 300r / min, 30mL of titanium tetrachloride was added dropwise in the filtrate recovered in Example 2 of 100mL, the dripping process controlled the temperature of the kettle <30°C and the rate of addition was controlled to keep the pressure in the kettle <3cm water column . After the dropwise addition, the temperature was raised to boiling, and reacted under boiling conditions for 1 h, and then cooled to room temperature to obtain a titanium oxide crystal slurry. The hydrogen chloride gas released during the dropwise addition of titanium tetrachloride is in the form of white smoke, and the suspended titanium oxide particles are removed by bubbling and washing with two-stage concentrated hydrochloric acid. The hydrogen chloride released during the hydrolysis process is absorbed by milk of lime to prepare a calcium chloride solution. The liquid crystal slurry in the kettle is filtered for solid-liquid separation, and gradient washing with pur...

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PUM

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Abstract

The invention relates to a green preparation technology for TiO2. The green preparation technology for TiO2 takes titanium tetrachloride as the raw material and comprises the steps of titanium tetrachloride hydration, hydrogen chloride gas release/titanium-chlorine oxide hydrolysis and precipitation, titanic oxide solid-liquid separation, titanic oxide purification and calcination and hydrogen chloride gas comprehensive utilization. A mother liquor obtained from solid-liquid separation and a washing liquid in the purification process can be used for titanium tetrachloride hydration, the collected hydrogen chloride gas can be absorbed to be used for preparing hydrochloric acid or producing calcium chloride, and the titanic oxide can be processed to obtain high-purity titanium dioxide powder. The green preparation technology for TiO2 has the characteristics of simple flow, fully green process and good TiO2 product quality.

Description

technical field [0001] The present invention relates to a kind of TiO 2 green preparation process. Background technique [0002] As an important inorganic chemical raw material, titanium dioxide is non-toxic, harmless, good chemical stability, thermal stability, excellent optical, mechanical and electrical properties and excellent dye performance, and has been widely used in many fields. Such as coatings, plastics, papermaking, chemical fiber, ink, rubber, electronics industry, cosmetics, ceramics and catalysts, etc. These applications are closely related to the particle size, crystal form, crystallinity, and morphology of titanium dioxide. [0003] At present, the preparation methods of titanium dioxide mainly include solid-phase method, gas-phase method and liquid-phase method; among them, the liquid-phase method is a common method to realize the controllable size and shape of titanium dioxide nanoparticles. Liquid phase methods mainly include sol-gel method, sol method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053C01B7/03C01F11/28B82Y30/00
CPCC01G23/0536B82Y30/00C01B7/035C01F11/28
Inventor 王岚陈丹萍王龙耀陈群
Owner CHANGZHOU UNIV
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