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A method for recovering exposed (001) crystal plane tio2 from titanium-containing waste liquid

A technology for titanium waste liquid and crystal face, which is applied in the field of recovering exposed crystal face TiO2, can solve problems such as environmental pollution and resource waste, and achieve the effects of low cost, simple process method, easy operation and large-scale realization.

Active Publication Date: 2018-07-24
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of the above-mentioned problems existing in the prior art, the object of the present invention is to provide a method for recovering exposed (001) crystal face TiO from the titanium-containing waste liquid produced by acid etching treatment of titanium sheets 2 method to solve the problems of environmental pollution and resource waste while realizing the reuse of resources

Method used

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  • A method for recovering exposed (001) crystal plane tio2 from titanium-containing waste liquid
  • A method for recovering exposed (001) crystal plane tio2 from titanium-containing waste liquid
  • A method for recovering exposed (001) crystal plane tio2 from titanium-containing waste liquid

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Experimental program
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Effect test

Embodiment 1

[0030] Simulate the pickling titanium waste liquid of a titanium production company, the waste liquid contains Ti 4+ and unreacted HF and HNO 3 : H according to the volume ratio 2 O:HNO 3 (mass fraction is 60%, analytically pure, Quzhou Juhua Reagent Co., Ltd.): HF (mass fraction is 40%, analytically pure, Zhejiang Zhongxing Chemical Reagent Co., Ltd.) = 5:4:1 configuration corrosion solution; 50 × Immerse a 50×1mm titanium sheet in 10ml of corrosive solution for 10-15s to remove oxides on the surface of the titanium sheet; take out the titanium sheet, collect the waste liquid, and obtain the titanium-containing waste liquid required for the test, and measure the Ti in the waste liquid 4+ The concentration is 8g / L, F - The concentration is 45.6g / L, NO 3 - The concentration is 364g / L.

[0031] Collect the titanium-containing waste liquid produced by the mixed acid etching of hydrofluoric acid and nitric acid to treat the metal titanium sheet, and dilute the collected wast...

Embodiment 2

[0033] Collect the titanium-containing waste liquid that the mixed acid acid etching of hydrofluoric acid and nitric acid produces in the embodiment 1, and the waste liquid that collects is diluted with water, until the Ti that contains in the waste liquid 4+ The concentration is 0.55g / L, F - The concentration is 3.0g / L, NO 3 - The concentration was 24g / L; then the diluted titanium-containing waste liquid was transferred to a polytetrafluoroethylene hydrothermal reaction kettle for hydrothermal reaction at 190°C for 24 hours; the reaction was completed, centrifuged, and the separated precipitates were separated by water and ethanol respectively. After washing three times, the product was dried in a drying oven at 80°C for 12 hours; the dried product was calcined in a muffle furnace at 500°C for 2 hours to remove residual fluoride, and the exposed (001) crystal plane was obtained TiO 2 , and the recovery rate was 65%.

Embodiment 3

[0035] Collect the titanium-containing waste liquid that the mixed acid acid etching of hydrofluoric acid and nitric acid produces in the embodiment 1, and the waste liquid that collects is diluted with water, until the Ti that contains in the waste liquid 4+ The concentration is 0.47g / L, F - The concentration is 2.7g / L, NO 3 - The concentration was 21.6 g / L; then the diluted titanium-containing waste liquid was transferred to a polytetrafluoroethylene hydrothermal reaction kettle for a hydrothermal reaction at 200°C for 36 hours; the reaction was completed, centrifuged, and the separated precipitate was separated with water and ethanol Each was washed three times, and then the product was dried in a drying oven at 80°C for 12 hours; the dried product was calcined in a muffle furnace at 500°C for 2 hours to remove residual fluoride, and the exposed (001) crystal was obtained. Surface TiO 2 , the recovery rate was 70%.

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Abstract

The invention discloses a method for recycling exposed (001) crystal face TiO2 from titanium-containing waste liquid. The method comprises the steps that a, collecting titanium-containing waste liquid generated by acid etching of a metallic titanium sheet and diluting the waste liquid with water till the concentration of Ti4+ contained in the waste liquid is 0.4-1.0 g / L, the concentration of F- is 2-5 g / L, and the concentration of NO3- is 18-38 g / L; b, the diluted titanium-containing waste liquid is transferred into a reaction kettle for a hydrothermal reaction; c, after the reaction is ended, centrifugal separation is performed, sediments are washed by water and ethyl alcohol and dried under the temperature of 75-85 DEG C; d, the dried product is calcinated under the temperature of 450-550 DEG C for 1-3 h, and the exposed (001) crystal face TiO2 is obtained. The exposed (001) crystal face TiO2 is recycled from the titanium-containing waste liquid, damage caused by high-concentration hydrofluoric acid and nitric acid to the environment is avoided, meanwhile, a metal titanium source is recycled, and the method is simple and low in cost.

Description

technical field [0001] The invention relates to a method for recovering exposed (001) crystal plane TiO from titanium-containing waste liquid 2 The method, specifically, involves a recovery of exposed (001) crystal plane TiO from the titanium-containing waste liquid produced by acid etching treatment of titanium sheets. 2 Methods. Background technique [0002] Metal titanium sheet is a multipurpose structural metal, and TiO is prepared by platinum plating and anodic oxidation on titanium base. 2 Nanotube films and oral implants have been more and more widely used. However, titanium is very easy to be passivated, and its surface passivation film will make the coating and the substrate unreal, reduce the biological activity and cause TiO 2 The formation of nanotubes is hindered, etc. Therefore, the mixed acid etching method of hydrofluoric acid and nitric acid is often used to remove the oxide film on the surface of the titanium sheet before the application. The waste liqu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/16C30B7/10
CPCC30B7/10C30B29/16
Inventor 孙善富孙明轩方亚林于治水
Owner SHANGHAI UNIV OF ENG SCI