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Method used for preparing high purity nanoscale titanium sub-oxides at low temperature

A titanium suboxide and nano-scale technology, which is applied in the low-value oxide of titanium, titanium oxide/hydroxide, nanotechnology, etc., can solve the problems of material performance degradation, particle growth, growth, etc., and achieve production efficiency High, short preparation process, the effect of realizing continuous industrial production

Inactive Publication Date: 2018-02-23
JIANGSU UNIV OF SCI & TECH IND TECH RES INST OF ZHANGJIAGANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, titanium dioxide is usually prepared by high-temperature sintering method, and the main reducing agent includes H 2 , NH 3 , C, Ti, Si, Zr, etc., the outstanding problem of the high temperature sintering method is that the material particles grow up and coarsen during the high temperature sintering process, which leads to a great reduction in the performance of the material, because the material particle size, porosity, crystallization The degree directly affects its optical, electromagnetic and electrochemical characteristics.
In order to improve the morphology of materials, researchers have successively developed laser ablation methods, sol-gel-sintering methods, etc., which have achieved control of the morphology and size of materials to a certain extent, and reduced the reduction temperature requirements. It fundamentally solves the problem of particle growth caused by high sintering temperature in the process of material preparation. Table 1 lists some representative titanium dioxide preparation methods

Method used

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  • Method used for preparing high purity nanoscale titanium sub-oxides at low temperature
  • Method used for preparing high purity nanoscale titanium sub-oxides at low temperature
  • Method used for preparing high purity nanoscale titanium sub-oxides at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 8000g of nano-sized rutile titanium dioxide, add 3000g of asparagine and 1000g of asparagine aqueous solution with a concentration of 5%, press into balls after mixing, and dry the balls at 105°C for 3 hours; then dry the dried The pellets are sent into the microwave rotary kiln. The temperature in the heating section of the microwave rotary kiln is set at 850°C, and the heating time is 30 minutes. After the reaction is completed, it is cooled rapidly; the reduced pellets are crushed and then put into a ball mill for grinding. The grinding time for 50min. Finally, the ground nano-scale titanium dioxide is subjected to heat treatment at a heat treatment temperature of 250° C. and a heat treatment time of 3 hours to finally obtain high-purity nano-scale titanium dioxide.

[0027] TiO 2 The recovery mechanism is as follows:

[0028] TiO 2 +C 4 h 8 N 2 o 3 → Ti 4 o 7 +CO 2 +H 2 O+N 2 …...(1)

[0029] The analysis result of high-purity nano-scale titanium ...

Embodiment 2

[0031] Weigh 8000g of nano-sized rutile titanium dioxide, add 3000g of glutamine and 1000g of 5% glutamine aqueous solution, mix well, press into balls, and dry the balls at 105°C for 3 hours; then dry the dried The pellets are sent into the microwave rotary kiln. The temperature in the heating section of the microwave rotary kiln is set at 800°C, and the heating time is 40 minutes. After the reaction is completed, it is cooled rapidly; the reduced pellets are crushed and then put into a ball mill for grinding. The grinding time for 50min. Finally, the ground nano-scale titanium dioxide is subjected to heat treatment at a heat treatment temperature of 250° C. and a heat treatment time of 3 hours to finally obtain high-purity nano-scale titanium dioxide.

[0032] TiO 2 The recovery mechanism is as follows:

[0033] TiO 2 +C 5 h 10 N 2 o 3 → Ti 4 o 7 +CO 2 +H 2 O+N 2 …...(2)

[0034] The analysis result of high-purity nano-scale titanium dioxide is: the content of t...

Embodiment 3

[0036] Weigh 8000g of nano-scale rutile titanium dioxide, add 1500g of asparagine, 1500g of glutamine and 1000g of (2.5% of glutamine+2.5% of asparagine) aqueous solution, mix and press into balls. The pellets were dried at 105°C for 3 hours; then the dried pellets were sent into the microwave rotary kiln, the temperature of the heating section of the microwave rotary kiln was set at 750°C, the heating time was 60 minutes, and the reaction was completed and cooled rapidly; the reduced pellets were passed through After crushing, put it into a ball mill for grinding, and the grinding time is 50 minutes. Finally, the ground nano-scale titanium dioxide is subjected to heat treatment at a heat treatment temperature of 250° C. and a heat treatment time of 3 hours to finally obtain high-purity nano-scale titanium dioxide.

[0037] TiO 2 The recovery mechanism is as follows:

[0038] TiO2 +C 4 h 8 N 2 o 3 +C 5 h 10 N 2 o 3 →Ti 4 o 7 +CO 2 +H 2 O+N 2 ......(3)

[0039] ...

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Abstract

The invention relates to a method used for preparing high purity nanoscale titanium sub-oxides at low temperature. The method comprises following steps: nanoscale rutile titanium dioxide, a reducing agent, and a wetting agent are subjected to uniform mixing and pelletizing so as to obtain pellets; the pellets are dried at 105 DEG C for 2 to 4h; the dried pellets are introduced into a microwave rotary kiln at a non-oxidizing atmosphere, are heated to 700 to 900 DEG C, the temperature is maintained for 20 to 60min, and cooling is carried out under the action of a reducing gas flow; after reduction, the pellets are smashed, and are introduced into a ball mill for 20 to 60min of grinding; after grinding, an obtained powder is subjected to 2 to 4h of heat treatment at 200 to 400 DEG C so as toobtain the high purity nanoscale titanium sub-oxides. According to the method, the high purity nanoscale titanium sub-oxides are prepared from rutile titanium dioxide at a relatively low temperature,the preparation process is short, the production efficiency is high, and the method is convenient for continuous industrialized production.

Description

technical field [0001] The invention relates to a method for preparing titanium oxide, in particular to a method for preparing high-purity nano-scale titanium oxide at low temperature. Background technique [0002] Titanium oxide is a series of non-stoichiometric titanium oxides with the general formula Ti n o 2n-1 (n=4~10). In 1959, X-ray scientist Magnéli first used anatase TiO 2 Based on the systematic research on this kind of substances. Therefore, people collectively refer to these substances as Magnéli phase, or titanium oxide for short. In recent years, the study of Magnéli phase has attracted more and more researchers' attention, especially the Ti in Magnéli phase 4 o 7 Due to its excellent properties such as strong corrosion resistance, electrochemical stability, and high electrical conductivity, it has shown great application prospects in combustion battery catalyst carriers, gas sensors, anti-reflection films, and photoelectric catalysis. [0003] At presen...

Claims

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Application Information

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IPC IPC(8): C01G23/04B82Y30/00B82Y40/00
CPCC01G23/043B82Y30/00B82Y40/00C01P2006/80
Inventor 居殿春邱家用徐敏人白妮陈春钰张荣良周夏芝周磊
Owner JIANGSU UNIV OF SCI & TECH IND TECH RES INST OF ZHANGJIAGANG
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