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Preparation method of copper ion doped anatase titanium dioxide

An anatase-type titanium dioxide and copper ion technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve problems such as difficult to scientifically control the crystal form of titanium dioxide, weaken the catalytic efficiency of titanium dioxide, and not easy to form a film. Stable, easy to operate, low cost effect

Active Publication Date: 2014-09-03
南京宁馨净化工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Titanium dioxide has three crystal forms, which are brookite, anatase and rutile. Titanium dioxide prepared by the usual process is a mixture of various crystal forms, so it is difficult to scientifically control the crystal form of titanium dioxide. Composition, greatly weakened titanium dioxide Therefore, by controlling the reaction conditions and optimizing the parameters, it is of great significance to prepare a single crystal form of titanium dioxide
[0003] At present, there are few methods for preparing anatase titanium dioxide doped with copper ions, and the prepared anatase titanium dioxide doped with copper ions does not have a single crystal form, and is unstable and difficult to form a film

Method used

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  • Preparation method of copper ion doped anatase titanium dioxide

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Experimental program
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Effect test

Embodiment 1

[0024] (1) Preparation of crude product: Wash and dry the 1L beaker, add 0.6ml of concentrated sulfuric acid into it, in a fume hood, add concentrated sulfuric acid to 15mL of titanium tetrachloride aqueous solution; under constant stirring, add 585mL of deionized water , stirred for 0.5h until titanium tetrachloride was hydrolyzed; added oxalic acid solution containing 0.47g copper oxalate, stirred for 0.5h, added 33mL of ammonia water until the pH value of the solution was 7.5, then stirred for 2h to obtain crude product A; Wash with deionized water, test the chloride ion in the solution with 0.02mol / L silver nitrate until no obvious white precipitate occurs; filter with suction, put the obtained filter cake into a blast drying oven, and dry at 100°C for 4 hours; then Put it into a vacuum drying oven to dry, and the vacuum degree is maintained at 10 -1 Pa, the temperature was maintained at 80°C, and dried for 6 hours.

[0025] (2) Grind the dried crude product A into a fine...

Embodiment 2

[0028] (1) Preparation of crude product: Wash and dry the 2L beaker, add 2ml of concentrated sulfuric acid into it, and add concentrated sulfuric acid to 25mL of titanium tetrachloride aqueous solution in a fume hood; add 973mL of deionized water under constant stirring, Stir rapidly for 0.5h until titanium tetrachloride is hydrolyzed, add oxalic acid solution containing 0.7834g of copper oxalate, stir for 0.5h, add 70mL of ammonia water until the pH value of the solution is 7.5, then stir for 2h to obtain crude product A; deionize with 6L Wash with water, and use 0.02mol / L silver nitrate to test the chloride ion in the solution until no obvious white precipitate occurs; filter with suction, put the obtained filter cake into a blast drying oven, and dry it at 100°C for 4 hours; Dry in a vacuum oven with a vacuum of 10 -1 Pa, the temperature was maintained at 80°C, and dried for 6 hours.

[0029] (2) Grind the dried crude product A into a fine powder with a radius of 40-50 μm,...

Embodiment 3

[0032] (1) Preparation of crude product: wash and dry the 3L beaker, add 1.6ml of concentrated sulfuric acid into it, in a fume hood, add concentrated sulfuric acid to 30mL of titanium tetrachloride aqueous solution; under constant stirring, add 2970mL of deionized water , stirred for 0.5h until titanium tetrachloride was hydrolyzed; added oxalic acid solution containing 1.5g of copper oxalate, stirred for 0.5h, added 125mL of ammonia water until the pH of the solution was 7.5, then stirred for 2h to obtain crude product A; Wash with deionized water, test the chloride ion in the solution with 0.02mol / L silver nitrate until no obvious white precipitate occurs; filter with suction, put the obtained filter cake into a blast drying oven, and dry at 100°C for 4 hours; then Put it into a vacuum drying oven to dry, and the vacuum degree is maintained at 10 -1 Pa, the temperature was maintained at 80°C, and dried for 6 hours.

[0033] (2) Grind the dried crude product A into a fine p...

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Abstract

The invention discloses a preparation method of copper ion doped anatase titanium dioxide. The preparation process comprises the following steps: 1, adding concentrated sulfuric acid into a titanium tetrachloride aqueous solution, and then adding deionized water to obtain a first crude product; 2, adding an oxalic acid copper solution into the first crude product obtained in the step 1, adjusting the pH value to 7-8 by using ammonia, and washing with deionized water to obtain a secondary crude product; 3, washing the secondary crude product obtained in the step 2 with deionized water to obtain a third crude product; step 4, conducting pump filtration on the third crude product washed in the step 3 to obtain a filter cake, drying the filter cake in an air blast drying box, and conducting vacuum drying to obtain a fourth crude product; and step 5, grinding the forth crude product obtained in the step 4 get into particles, heating, calcining and cooling to room temperature to obtain copper ion doped anatase titanium dioxide. The preparation method provided by the invention has the advantages of simple operation, high controllability, and easiness for industrial popularization and application.

Description

technical field [0001] The invention relates to anatase titanium dioxide, in particular to a method for preparing anatase titanium dioxide doped with copper ions. Background technique [0002] Titanium dioxide has three crystal forms, which are brookite, anatase and rutile. Titanium dioxide prepared by the usual process is a mixture of various crystal forms, so it is difficult to scientifically control the crystal form of titanium dioxide. Composition, greatly weakened titanium dioxide Therefore, it is of great significance to prepare single-crystal titanium dioxide by controlling the reaction conditions and optimizing parameters. In the last five years, in order to improve the catalytic efficiency of single-crystal titanium dioxide, loading a certain amount of metal ions on a single titanium dioxide lattice can significantly improve the feminization performance of the catalyst. A certain amount of metal ions has great research significance and application prospects. [00...

Claims

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Application Information

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IPC IPC(8): C01G23/053C01G23/08
Inventor 郑凯韩玉华李红艺季仁杰张同超黄国正秦天羽
Owner 南京宁馨净化工程有限公司
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