Silicon-vanadium composite oxide and preparation method thereof

A composite oxide and chemical technology, applied in the direction of vanadium oxide, silicon oxide, silicon dioxide, etc., to achieve the effect of high thermal stability, large specific surface area, and simple operation

Active Publication Date: 2018-08-14
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above method can only get disordered stacking structure

Method used

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  • Silicon-vanadium composite oxide and preparation method thereof
  • Silicon-vanadium composite oxide and preparation method thereof
  • Silicon-vanadium composite oxide and preparation method thereof

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preparation example Construction

[0034] In order to obtain the non-metal-metal oxide phase structure with the above-mentioned uniform structure, the present invention adopts a one-step hydrothermal synthesis method in which a complexing agent and a surfactant are combined: a certain amount of ammonium metavanadate powder and ethyl orthosilicate are respectively Dissolve in aqueous solution and mix, then add a certain amount of complexing agent oxalic acid and surface-active ammonium lauryl sulfate, and move it into a reaction kettle (hydrothermal reaction kettle or high-pressure hydrothermal kettle, etc.) for one-time hydrothermal reaction; take out Afterwards, the precursor is obtained by filtering, washing, and drying, and the precursor is placed in a heating furnace (muffle furnace, etc.) and roasted for a certain period of time to obtain a silicon-vanadium composite oxide with a curd layer structure. The specific preparation methods include:

[0035] According to (SiO 2 ) n VO m The preset values ​​of ...

Embodiment 1

[0043] Example 1 is as follows:

[0044](1) Weigh 2.73g of tetraethyl orthosilicate and 4.0g of ammonium metavanadate, and dissolve them in 100mL of distilled water separately under the condition of stirring at 50°C to prepare an aqueous solution of ethyl orthosilicate and ammonium metavanadate . Mix the two aqueous solutions prepared above, stir fully at 50°C, then add 4.3g oxalic acid dihydrate as a complexing agent, and stir for 2 hours; then add 6.2g of 30wt% ammonium lauryl sulfate aqueous solution, The stirring reaction was continued at 50°C for 24 hours.

[0045] (2) The reacted solution was transferred into a high-pressure hydrothermal kettle, aged at 180°C for 24 hours, and then the product was taken out, centrifuged, washed, and dried in an oven at 60°C for 8 hours to obtain a solid precursor. Place the obtained precursor in a muffle furnace, raise the temperature to 450°C at a rate of 2°C / min, bake at 450°C for 6 hours, and cool to obtain the composite with this s...

Embodiment 2

[0049] (1) Weigh 2.73 g of ethyl orthosilicate and 2 g of ammonium metavanadate, and dissolve them in 70 mL of distilled water separately under the condition of stirring at 50° C. to prepare an aqueous solution of ethyl orthosilicate and ammonium metavanadate. Mix the two aqueous solutions prepared above, stir fully at 50°C, then add 2.15g oxalic acid dihydrate as a complexing agent, and stir for 2 hours; then add 4.0g of 30wt% lauryl ammonium sulfate aqueous solution, The stirring reaction was continued at 50°C for 24 hours.

[0050] (2) The reacted solution was transferred into a high-pressure hydrothermal kettle, aged at 160°C for 24 hours, and then the product was taken out, centrifuged, washed, and dried in an oven at 60°C for 12 hours to obtain a solid precursor. Place the obtained precursor in a muffle furnace, raise the temperature to 500°C at a rate of 2°C / min, bake at 500°C for 5 hours, and cool to obtain the composite with this special structure.

[0051] The silic...

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Abstract

The invention discloses a silicon-vanadium composite oxide and a preparation method thereof. A chemical formula of the composite oxide is (SiO2) nVOm, and the composite oxide is of a flower-ball layered nanometer structure. A one-step hydro-thermal synthesis method in which a complexing agent is combined with a surfactant is adopted and includes the steps of separately dissolving a certain amountof ammonium metavanadate powder and a certain amount of ethyl orthosilicate in a water solution, then mixing the solutions above, adding a certain amount of oxalic acid serving as the complexing agentand ammonium lauryl sulfate serving as the surfactant into the mixed solution, and placing the mixture into a reaction still for a one-time hydrothermal reaction; taking the mixture, conducting filtering, washing and drying on the mixture to obtain a precursor, then placing the precursor into a heating oven for calcination for a certain period of time, and obtaining the silicon-vanadium compositeoxide of the flower-ball layered structure. The composite oxide has the advantages of a large specific surface area, high thermal stability and the like; moreover, the preparation method is easy to operate, and a result is stable and reliable.

Description

technical field [0001] The invention relates to a silicon-vanadium composite oxide and a preparation method thereof, belonging to the technical field of inorganic nanometer material preparation. Background technique [0002] Vanadium oxides and their derivatives are a class of functional materials that people are very interested in. Their unique chemical characteristics and photoelectrocatalytic properties make them suitable for selective oxidation catalysis of organic hydrocarbons, electrode materials for charging and discharging lithium-ion batteries, organic gases and humidity. Sensors and smart coatings have important application value. Their nanolayered materials exhibit high catalytic activity, excellent electron transport and redox activity due to their special structure and high specific surface area. The synthesis and performance research of vanadium oxide nanolayer structure materials have aroused great interest; in addition, the chemical doping of silicon can imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12C01G31/02B82Y40/00B82Y30/00
CPCB82Y30/00B82Y40/00C01B33/12C01G31/02C01P2002/72C01P2004/03C01P2004/32C01P2004/61C01P2004/82
Inventor 吴晋沪何涛葛元征韩德志王志奇杨静
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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