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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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 hydrotherm

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

Examples

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Example Embodiment

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

[0035] S1, in tetravalent vanadium solution A, add ammoniacal liquor, stir to obtain suspension B; Wherein, the vanadium ion concentration in described tetravalent vanadium solution A is 0.1-2mol / L, and it is water-soluble by tetravalent vanadium salt, And stirring at a 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, or it can be a compound through other vanadium, such as five The tetravalent vanadium salt obtained by reducing vanadium oxide, ammonium metavanadate or sodium vanadate by reducing agent; the water here is pure water, distilled water or deionized water;

[0036] S2, described suspension B is carried out sealing heat preservation stirring process, obtains colloidal suspension C,...

Example Embodiment

[0048] Example 1

[0049] Preparation of Undoped Rutile Phase Vanadium Dioxide Ultrafine Nano-powders

[0050] 1) Preparation of colloidal suspension:

[0051] Take 4 g of vanadyl sulfate, add the powder to a 200 ml flask, add 60 ml of deionized water and continue stirring for 10 minutes. Add 10 ml of ammonia water with a concentration of 25%, and continue stirring for 10 minutes to obtain a turbid precursor solution. The flask containing the cloudy precursor solution was sealed, heated to 80° C., and then kept for 2 hours to obtain a colloidal suspension.

[0052] 2) Colloid treatment:

[0053] Transfer the colloidal suspension obtained in step 1) into a plastic centrifuge tube, put it into a centrifuge, keep it centrifuged for 10 minutes at a rotating speed of 6000 r / min, take it out, remove the supernatant, add deionized water, and remove the precipitate. Mix well in water, put it into an ultrasonic cleaner for 5 minutes of ultrasonic treatment, put it into a centrifuge...

Example Embodiment

[0058] Example 2

[0059] Preparation of 1% tungsten-doped rutile phase vanadium dioxide ultrafine nanopowders

[0060] 1) Preparation of colloidal suspension:

[0061] Take 4 g of vanadyl sulfate, add the powder into a 200 ml flask, add 60 ml of deionized water and continue stirring for 10 minutes, then add 0.07 g of ammonium metatungstate. After continuing stirring for 10 minutes, 10 ml of ammonia water with a concentration of 25% was added, and the turbid precursor solution was obtained after continuing stirring for 10 minutes. The flask containing the cloudy precursor solution was sealed, heated to 80° C., and then kept for 2 hours to obtain a colloidal suspension.

[0062] 2) Colloid treatment:

[0063] Transfer the colloidal suspension obtained in step 1) into a plastic centrifuge tube, put it into a centrifuge, keep it centrifuged for 10 minutes at a rotating speed of 6000 r / min, take it out, remove the supernatant, add deionized water, and remove the precipitate. M...

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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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