Preparation method for rutile phase vanadium dioxide superfine nano powder

A technology of vanadium dioxide and ultrafine nanometers, which is applied in the field of preparation of rutile phase vanadium dioxide ultrafine nanometer powders, can solve the problems of organic solvent toxicity and safety, difficult water recycling, large particle uniformity, etc., and achieve relative The effect of low value, high production speed and high particle purity

Inactive Publication Date: 2019-02-12
INST FOR PROCESS MODELING & OPTIMIZATION JITRI
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  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the solvothermal and microemulsion reaction methods need to use certain organic solvents as the reaction medium, the cost is high, and some organic solvents have certain toxicity and other safety hazards
The reaction pressure of the hydrothermal reaction method is high, resulting in a high initial investment in equipment and production safety using this method
The reaction system of the hydrothermal reaction is also relatively complicated, and the water used as a solvent is difficult to recycle and will cause some additional waste water treatment costs
The solid phase reaction method will generate some waste gas in the synthesis of vanadium dioxide nanoparticles, which will lead to some waste gas treatment costs, and the formed particles have greater uniformity and higher production energy consumption

Method used

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  • Preparation method for rutile phase vanadium dioxide superfine nano powder
  • Preparation method for rutile phase vanadium dioxide superfine nano powder
  • Preparation method for rutile phase vanadium dioxide superfine nano powder

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preparation example Construction

[0034] A preparation method of rutile phase vanadium dioxide ultrafine nano-powder, comprising the following steps:

[0035] S1. Add ammonia water to the tetravalent vanadium solution A, and stir to obtain a suspension B; wherein, the concentration of vanadium ions in the tetravalent vanadium solution A is 0.1-2mol / L, which is dissolved in water by tetravalent vanadium salt, And it is obtained by stirring at a rotating speed of 50-2500r / min for 1-60min, preferably 25min. Wherein the tetravalent vanadium salt can be one or more of vanadyl sulfate, vanadyl oxalate, vanadyl chloride, vanadyl ascorbate, vanadyl citrate or vanadyl tartrate, and can also be through other vanadium compounds, such as penta Vanadium oxide, ammonium metavanadate or sodium vanadate is reduced by a reducing agent to form a tetravalent vanadium salt; the water here is pure water, distilled water or deionized water;

[0036] S2. Carry out sealing, heat preservation and stirring treatment on the suspension ...

Embodiment 1

[0049] Preparation of non-doped rutile phase vanadium dioxide ultrafine nanopowder

[0050] 1) Colloidal suspension preparation:

[0051] Take 4g of vanadyl sulfate, add the powder into a 200ml flask, add 60ml of deionized water and keep stirring for 10 minutes. Add 10 ml of 25% ammonia water and continue stirring for 10 minutes to obtain a cloudy precursor solution. Seal the flask containing the turbid precursor solution, heat it to 80° C. and keep it warm for 2 hours to obtain a colloidal suspension.

[0052] 2) Colloid treatment:

[0053] Transfer the colloidal suspension obtained in step 1) to a plastic centrifuge tube, put it into a centrifuge, keep centrifuging at a speed of 6000r / min for 10 minutes, take it out, remove the supernatant, add deionized water, and remove the precipitate Mix well in water and put it into an ultrasonic cleaning machine for ultrasonic treatment for 5 minutes, put it into a centrifuge for centrifugation, repeat the operation three times, tak...

Embodiment 2

[0059] Preparation of 1% tungsten-doped vanadium dioxide ultrafine nano-powder in rutile phase

[0060] 1) Colloidal suspension preparation:

[0061] Take 4g of vanadyl sulfate, put the powder into a 200ml flask, add 60ml of deionized water and keep stirring for 10 minutes, then add 0.07g of ammonium metatungstate. After continuing to stir for 10 minutes, add 10 ml of 25% ammonia water, and continue stirring for 10 minutes to obtain a cloudy precursor solution. Seal the flask containing the turbid precursor solution, heat it to 80° C. and keep it warm for 2 hours to obtain a colloidal suspension.

[0062] 2) Colloid treatment:

[0063] Transfer the colloidal suspension obtained in step 1) to a plastic centrifuge tube, put it into a centrifuge, keep centrifuging at a speed of 6000r / min for 10 minutes, take it out, remove the supernatant, add deionized water, and remove the precipitate Mix well in water and put it into an ultrasonic cleaning machine for ultrasonic treatment f...

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Abstract

The invention discloses a preparation method for rutile phase vanadium dioxide superfine nano powder, which comprises the following steps: S1, enabling ammonium hydroxide to quickly react with an acidic tetravalent vanadium solution to obtain turbid liquid B; S2, performing sealing, heat preservation and stirring treatment on the turbid liquid B to obtain a colloidal suspension C, wherein the temperature for heat preservation is not higher than the boiling point of a solvent in the tetravalent vanadium solution; S3, performing solid-liquid separation and cleaning on the colloidal suspension Cto obtain hydrated vanadium hydroxide colloid D; S4, drying the hydrated vanadium hydroxide colloid D and sintering in the protection atmosphere to obtain the rutile phase vanadium dioxide superfine nano powder. The rutile phase vanadium dioxide particles prepared by the process method disclosed by the invention have the advantages of high purity, smaller and even size and good dispersion and canserve as an excellent raw material for high-quality vanadium dioxide intelligent temperature-control coated windows.

Description

technical field [0001] The invention belongs to the chemical field of metal-insulator phase change materials, and in particular relates to a preparation method of rutile phase vanadium dioxide ultrafine nanometer powder. Background technique [0002] The increasingly serious energy problem and environmental pollution have become a global key issue. The demand for clean energy and new environmentally friendly and energy-saving materials is growing rapidly. Among them, building energy consumption, especially temperature control equipment such as air conditioning and heating, has accounted for about 30% of the total energy consumption according to statistics. Studies have found that coating the glass surface of buildings or automobiles can partially reflect heat radiation (10-50%, depending on the material used) in hot summer, thereby reducing the use of indoor air conditioning systems and energy consumption. However, so far, many energy-saving materials have complex producti...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y40/00
CPCB82Y40/00C01G31/02C01P2002/72C01P2004/04C01P2004/32C01P2004/62C01P2004/64
Inventor 刘闽苏刘礼华范维仁蒋绪川余艾冰郑锐
Owner INST FOR PROCESS MODELING & OPTIMIZATION JITRI
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