Method for preparing titanium oxide through reducing titanium-containing complexes at normal temperature

A technology of titanium complex and titanium suboxide, applied in the direction of titanium oxide/hydroxide, etc., can solve the problems of high price, small output and high manufacturing cost of titanium suboxide, and achieve the elimination of explosion hazards, low raw material cost, high temperature and the effect of time reduction

Active Publication Date: 2019-06-14
CHENGDU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The properties and functions of titanium dioxide in other phases need to be researched and developed, but the key is to prepare titanium dioxide in a single phase rather than a series of titanium dioxide mixtures that can be afforded by the application, with high purity. The high manufacturing cost and small output of titanium oxide lead to high price of titanium oxide, especially for the preparation of high-purity Ti 4 o 7 It is a technical problem that needs to be solved at present

Method used

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  • Method for preparing titanium oxide through reducing titanium-containing complexes at normal temperature
  • Method for preparing titanium oxide through reducing titanium-containing complexes at normal temperature

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: Get the titanium sulfate solution that measures 1 mole with titanium dioxide, add ammoniacal liquor to observe that precipitation is complete, pH7, obtain orthotitanic acid white precipitation; The above-mentioned orthotitanate Ti(OH) 4 Wash the precipitate with 5 times the volume of deionized water to remove sulfate and ammonium ions to obtain pure orthotitanic acid; add 2.5 moles of oxalic acid and 5 times the volume of deionized water, add pure orthotitanic acid, and stir Slowly dissolve completely; add 1 mole of zinc powder, stir the reaction until no bubbles are generated, and react for 5 hours; obtain a black solution; slowly add ammonia water to adjust the pH value of the solution to 12, and then produce a brown to dark purple-black precipitate , washed 5 times with 5 times deionized water to obtain pure titanium hydroxide precipitate mainly composed of purple trivalent titanium; add oxalic acid and stir until the pH is 0.5; The precipitate was drie...

Embodiment 2

[0032] Embodiment 2: Get the titanium sulfate solution that measures 1 mole with titanium dioxide, add ammoniacal liquor to observe that precipitation is complete, pH8, obtain orthotitanic acid white precipitation; The above-mentioned orthotitanate Ti(OH) 4 Wash the precipitate with 4 times the volume of deionized water to remove sulfate and ammonium ions to obtain pure orthotitanic acid; add 2 moles of oxalic acid and 3.5 times the amount of deionized water, put in pure orthotitanic acid, and stir Slowly dissolve completely; add 0.5 mole of zinc powder, stir the reaction until no bubbles are generated, react for 4 hours; obtain a black solution; slowly add ammonia water to adjust the pH value of the solution to 12, and then produce a brown to dark purple-black precipitate , washed 4 times with 4 times deionized water to obtain pure titanium hydroxide precipitate mainly composed of purple trivalent titanium; add oxalic acid and stir until the pH is 1.0; The precipitate was dri...

Embodiment 3

[0033] Embodiment 3: Get the titanium sulfate solution that measures 1 mole with titanium dioxide, add sodium hydroxide to observe that precipitation is complete, pH9, obtain orthotitanic acid white precipitation; The above-mentioned orthotitanate Ti(OH) 4 Wash the precipitate with 5 times the volume of deionized water to remove sulfate and sodium ions to obtain pure orthotitanic acid; add 2.5 moles of citric acid to 5 times the volume of deionized water, add pure orthotitanic acid, and stir Add 1 mole of zinc powder, stir the reaction until no bubbles are produced, and react for 5 hours; obtain a black solution; slowly add ammonia to adjust the pH value of the solution to 12, and then produce brown to deep purple black Precipitate, washed 5 times with 5 times deionized water to obtain pure titanium hydroxide precipitate mainly composed of purple trivalent titanium; add oxalic acid and stir until the pH is 0.5; The titanium precipitate was dried at 180°C for 3 hours until no o...

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Abstract

The invention discloses a method for preparing titanium oxide through reducing titanium-containing complexes at normal temperature. The method is characterized in that reduction reaction occurs in a normal temperature liquid phase; the potential safety hazards due to mixing of reducing agents and air are eliminated; the reduction is performed in the liquid phase, the microscopic uniformity is high; the firing temperature is low; the time is short. The method has the following principle and steps that titanium sulfate or titanium tetrachloride and ammonium hydroxide or sodium hydroxide take a reaction to obtain titanic acid; the titanic acid reacts with oxalic acid or citric acid to form an oxalate oxytitanate complex-ion or oxytitanate citrate complex-ion solution; next, reaction is performed with zinc powder; the complex ions are reduced into low-valent titanium complex ions; the pH value of the solution is regulated to 12 by ammonium hydroxide; precipitates of dark brown color to dark violet color are generated; washing is performed for 3 to 5 times by 3 to 5 times of deionized water; the zin is washed away in an ion ZnO2<2-> form to obtain pure titanium hydroxide precipitates; oxalic acid is added until the pH is 0.5 to 1.5; drying is performed to 2 to 5 hours at 120 to 180 DEG C; the temperature is raised from room temperature to 820 to 950 DEG C by a muffle furnace; roasting is performed for 2 to 6 hours; titanium oxide spherical powder with the Ti4O7 content being 90 percent or higher is obtained.

Description

technical field [0001] The invention relates to the field of inorganic materials, in particular to a method for preparing inorganic functional materials, in particular to a method for preparing titanium oxide by reducing a titanium-containing complex at normal temperature. Background technique [0002] Titanium oxide refers to a series of non-measured titanium oxides other than titanium dioxide or titanium monoxide, which can be represented by the general formula Ti n o 2n -1 (n=4~10) indicates that this type of compound was discovered by Magnéli through XRD analysis in the 1950s, and is also called Magnéli phase titanium suboxide material, which is different from titanium dioxide and is a black conductive material. [0003] In this series of Magnéli phase titanium oxides, Ti 4 o 7 The properties are the most prominent, its physical and chemical properties are stable, and it has excellent electrical conductivity. At room temperature, its electrical conductivity is even gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/04
Inventor 邓昭平张文焕胡鹏
Owner CHENGDU UNIVERSITY OF TECHNOLOGY
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