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Preparation method of low-valence titanium oxide powder

A low-valent titanium oxide and titanium dioxide technology, applied in the direction of titanium oxide/hydroxide, can solve the problems of high environmental damage, easy environmental pollution, application restrictions, etc., and achieve easy popularization and application, good product reproducibility, and physical and chemical properties. great effect

Inactive Publication Date: 2012-04-25
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The powder of carbon black, a traditional black pigment, is easy to float in the air when used, which brings inconvenience to the use and also brings certain harm to the health of users
In addition, the miscibility of carbon black and resin is poor, and there are disadvantages such as uneven dispersion.
Ferroferric oxide can also be used as a black pigment, but its application is limited due to its magnetic properties and poor thermal stability.
[0003] At present, there are mainly methods for preparing low-valent titanium oxide, such as ammonia reduction method, hydrogen reduction method, metal titanium powder reduction method, methylamine reduction method, etc. Among them, the ammonia reduction method is to reduce titanium dioxide to low-valent Titanium oxide, the reduction speed is slow, and ammonia gas is a corrosive and irritating gas, which is harmful to the environment; the hydrogen reduction method is to reduce titanium dioxide to low-valent titanium oxide at a high temperature of 1100 ° C under a hydrogen atmosphere, and the reduction speed is slow , due to the use of hydrogen, the equipment requirements are high, and the risk factor is high during preparation; the metal titanium powder reduction method is to use metal titanium powder to reduce titanium dioxide to low-priced titanium oxide under a nitrogen or argon protective atmosphere, the cost is high, and the reduction speed It is slow, and it also needs a protective atmosphere, which makes the equipment complicated; the methylamine reduction method is to reduce titanium dioxide to low-valent titanium oxide at a temperature of 700 ° C to 1000 ° C in a methylamine atmosphere. The reduction is faster, but methylamine itself is a toxic gas, which is more harmful to humans and easy to pollute the environment
In short, the above methods for preparing low-valent titanium oxide have many limitations, such as high reaction temperature, need to use a protective atmosphere, high requirements for equipment and safety, high energy consumption, and hydrogen, ammonia, etc. Gas, methylamine and other protective atmospheres are also dangerous, and are easy to harm the human body and the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 2g of nano-sized rutile titanium dioxide powder, 1.5g of sodium borohydride and 1.5g of potassium borohydride and mix evenly, then transfer the mixed material to a dry corundum pan for compaction and flattening. Then put the crucible into the muffle furnace for heating, keep it at 500°C for 1 hour, and then cool down with the furnace. Take out the dark black powder in the lower layer of the cooled crucible, wash and filter it repeatedly with distilled water, and dry the filter cake at 50°C to obtain uniform dark black nano-scale low-valent titanium oxide powder.

Embodiment 2

[0017] Weigh 2g of submicron rutile titanium dioxide powder, 1g of sodium borohydride and 1.5g of potassium borohydride and mix evenly, then transfer the mixed material to a dry corundum pan for compaction and flattening. Then put the crucible into the muffle furnace for heating, keep it at 550°C for 20 minutes and then cool down with the furnace. Take out the black powder in the middle and lower layers of the cooled crucible, wash and filter repeatedly with distilled water, and dry the filter cake at 60°C to obtain uniform black submicron low-valent titanium oxide powder.

Embodiment 3

[0019] Weigh 2g of submicron anatase titanium dioxide powder, 0.75g of sodium borohydride and 1.5g of potassium borohydride and mix evenly, then transfer the mixture to a dry corundum pan for compaction and flattening. Then put the crucible into the muffle furnace for heating, keep it at 550°C for half an hour, and then cool down with the furnace. Take out the brown-black powder in the lower layer of the crucible after cooling, wash and filter repeatedly with distilled water, and dry the filter cake at 50°C to obtain uniform brown-black submicron low-valent titanium oxide powder.

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PUM

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Abstract

The invention provides a preparation method of low-valence titanium oxide powder, which comprises the following steps: (1) uniformly mixing titanium dioxide powder, sodium borohydride and potassium borohydride, and then compacting and flattening the mixed materials in a drying corundum crucible; (2) heating the system prepared in step (1) in a muffle furnace, maintaining the temperature, and thencooling in the furnace; and (3) taking out deep-color powder at the lower layer of the crucible after cooling, thoroughly cleaning with distilled water, filtering, and drying the filter cake to obtain the low-valence titanium oxide powder. The low-valence titanium oxide powder prepared by the method maintains the particle diameters of titanium dioxide raw materials, and the color can be changed with the formula. The low-valence titanium oxide powder can be used as a deep-color pigment in the fields of coating, resin, paint, cosmetics and the like. Compared with the traditional low-valence titanium oxide preparation method, the invention has the advantages of low temperature, simple equipment, easy control, stable product quality, low energy consumption and easy popularization and application.

Description

technical field [0001] The invention relates to a method for preparing low-valent titanium oxide powder, which belongs to the field of new material preparation. Background technique [0002] In recent years, titanium dioxide (also known as titanium dioxide, the molecular formula is TiO 2 ) has always been a popular research object in materials and other disciplines, and products related to titanium dioxide are used in many fields. Low-valent titanium oxide is also an oxide of titanium, but because the oxygen content in low-valent titanium oxide is less than that of titanium dioxide, its molecular formula is often written as Ti n o 2n-1 (1≤n≤20), its properties are also quite different from titanium dioxide, especially in terms of color, titanium dioxide is white or light yellow, while low-valent titanium oxide is dark, even dark black. Due to its special properties, low-valent titanium oxide has a wide range of applications. First of all, low-priced titanium oxide produc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/04
Inventor 毛健管东波涂铭旌
Owner SICHUAN UNIV