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New process for preparing anatase type nano titanium dioxide

A nano-titanium dioxide, anatase technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve problems such as environmental protection work problems, and achieve the effect of economical recycling and uniform particle size distribution

Inactive Publication Date: 2006-03-29
西藏大昭圣泉实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the process, three times of water washing (secondary water washing of metatitanic acid hydrolysis, and water washing of filter cake after solid-liquid separation) resulted in a large amount of sewage discharge, which brought difficulties to environmental protection work

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Weigh 1000 grams of metatitanic acid and place it in a 10L reactor, add 3000 grams of deionized water for beating, then add 3000 ml of sulfuric acid, after the reaction is completed, add 200 grams of hydrogen peroxide and stir evenly (about 10 minutes), and then slowly Add 100 grams of urea, 3000 grams of ammonia water and 1000 grams of sodium hydroxide solution (the amount of sodium hydroxide solution is determined by the pH value of the desired product) and stir for 20 minutes, then set aside for 2 hours, then add 30 grams of absolute ethanol and stir evenly , use the static sedimentation method to remove the metatitanic acid and ammonium sulfate double salt precipitated supernatant in the recovery tank, the metatitanic acid and ammonium sulfate double salt paste obtained by the static sedimentation method is sent to the air dryer at 120 ° C ~ 180 ° C The powder is dried under high temperature to form a powder, and the powder is heated to 600°C in a sealed d...

Embodiment 2

[0019] Embodiment 2: technological process, equipment are the same with embodiment 1, so omit relevant description. With 1000 grams of metatitanic acid as raw material, after adding excess sulfuric acid to react, the weight ratio of various auxiliary materials is: metatitanic acid: hydrogen peroxide: urea: ammonia water: sodium hydroxide solution: absolute ethanol=1: 5%: 08% : 2: 1.5: 5%; the calcination temperature is 450° C., and the temperature is kept constant for 2 hours. Anatase titanium dioxide products have a particle size of 10-30nm and a specific surface area of ​​about 52m 2 / g.

Embodiment 3

[0020] Embodiment 3: technological process, equipment are the same as embodiment 1, omit. With 2000 grams of metatitanic acid as raw material, after adding sulfuric acid to react, the weight ratio of various auxiliary materials is: metatitanic acid: hydrogen peroxide: urea: ammonia water: sodium hydroxide solution: triethanolamine=1: 5%: 1%: 1 : 1.5: 5%; calcination temperature 700°C, constant temperature 1.5 hours. The particle size of anatase titanium dioxide product is 20-30nm, and the specific surface area is about 60m 2 / g.

[0021] The preparation technological process of embodiment 1-3 is summarized as follows:

[0022] Dissolving (dissolving metatitanic acid with deionized water) → reaction (adding excess concentrated sulfuric acid) → synthesis (adding hydrogen peroxide, urea, ammonia water, and 50% sodium hydroxide solution in sequence in proportion, the temperature is controlled at less than 130°C, and the reaction time does not exceed 2 hours, the pH value is con...

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Abstract

The invention relates to a new technics to manufacture nanometer titanium dioxide. Using metatitanic acid as material, the steps are as follows: firstly reacting with enough vitriol to get titanyl sulfate solution, adding hydrogen peroxide and carbamide into the solution, then adding ammonia and sodium hydroxide, separating solid and liquor after free settling, adding absolute ethyl alcohol or triethanolamine into solid-phase separation substance. The weight ratio of above materials is metatitanic acid : hydrogen peroxide : carbamide : ammonia : sodium hydroxide : absolute ethyl alcohol or triethanolamine = 1:0.1%-1:0.1%-1:0.5-3:0.5-2:0.1%-1. Then finished product can be made after pneumatic conveying drying in 120-180deg.C to get powder, calcining the powder in 450-700deg.C and keeping the temperature for 0.5-2 hours. With metatitanic acid as material and firstly producing titanyl sulfate, the technics is reduced. Canceling washing operation resolves the problem of producing plentiful sewage. The invention meets the requirement of environment protection for its no barren liquor and exhaust gas discharge.

Description

1. Technical field [0001] The invention relates to a process for preparing anatase nano titanium dioxide by using metatitanic acid as a raw material and supplemented with other chemical substances. 2. Background technology [0002] There are many methods for preparing nano-titanium dioxide, which are generally divided into gas-phase method and liquid-phase method. The gas-phase method uses titanium tetrachloride or titanium organic ester as raw material, and generates nano-titanium dioxide by gas-phase oxidation under high temperature conditions. This method requires strict control conditions. , The equipment is severely corroded. The liquid phase method can be divided into organic ester method, titanium tetrachloride method, titanium sulfate method, metatitanic acid method and so on according to different raw materials. Generally, different raw materials are used according to the needs of preparing nano-titanium dioxide with different crystal forms. For example, titanium s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047
Inventor 戴允民
Owner 西藏大昭圣泉实业有限公司
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