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Preparation method for economical, safe and environment-friendly Nb3O7F nanometer material
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A nanomaterial and safe technology, applied in the field of preparation of Nb3O7F nanomaterials, can solve the problems of difficult process control, fast reaction rate, high cost, etc., and achieve the effects of avoiding human and environmental hazards, simple preparation process and increasing safety.
Inactive Publication Date: 2017-12-15
CHINA UNIV OF MINING & TECH
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[0009] The object of the invention is to provide a kind of economical, safe and environment-friendly Nb 3 o 7 The preparation method of F nanomaterials, to solve the problems existing in the prior art, such as the problems such as high cost, complex process and many heterogeneous phases in the preparation process of thermal deposition method; the safety of hydrofluoric acid ubiquitous in the process of wet chemical method Low, unfriendly waste liquid environment, high cost, low degree of nanometerization, difficulty in powder collection, fast reaction rate, difficult process control, uneven shape and particle size distribution, etc.
Method used
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Embodiment 1
[0058] (1) Measure 80mL of deionized water and pour it into a plastic beaker;
[0059] (2) Weigh 0.564g NbF 5 The powder was added to the above beaker, and magnetically stirred for 15 minutes to make the NbF 5 fully dissolved;
[0060] (3) Transfer the above solution to a polytetrafluoroethylene lining, then place the lining in a micro-reactor, seal it well, put the reactor into a blast oven, and conduct a hydrothermal reaction at 180°C for 24 hours, and then furnace cooling;
[0061] (4) Centrifuge the precipitated product, wash it three times with deionized water and once with absolute ethanol, and dry the product in a vacuum oven at 70° C. for 6 hours to obtain the final product.
Embodiment 2
[0063] (1) Measure 60mL of deionized water and 20mL of acetone, and pour them into plastic beakers;
[0064] (2) Weigh 1.692g NbF 5 Add the powder into the above plastic beaker and stir it magnetically for 15min to make the NbF 5 fully dissolved;
[0065] (3) Transfer the above solution to a polytetrafluoroethylene lining, then place the lining in a micro-reactor, seal it well, put the reactor into a blast oven, and conduct a hydrothermal reaction at 180°C for 24 hours, and then furnace cooling;
[0066] (4) Centrifuge the precipitated product, wash it 4 times with deionized water, wash it 2 times with absolute ethanol, and dry the product in a vacuum oven at 70° C. for 6 hours to obtain the final product;
[0067] (5) The above product was heat-treated at 380° C. for 2 hours in an air atmosphere to obtain the final product.
Embodiment 3
[0069] (1) Measure 40mL deionized water and 40mL acetone, and pour them into plastic beakers;
[0070] (2) Weigh 2g of P123 surfactant, add it to the above-mentioned beaker, and magnetically stir for 40min to completely dissolve P123;
[0071] (3) Weigh 0.564g NbF 5 powder, added to the above solution, magnetically stirred for 25min to make NbF 5 fully dissolved;
[0072] (4) Transfer the above solution to a polytetrafluoroethylene lining, then place the lining in a micro-reactor, seal it well, put the reactor into a blast oven, and react hydrothermally at 200°C for 24 hours, and then furnace cooling;
[0073] (5) Centrifuge the precipitated product, wash it 4 times with deionized water and 3 times with absolute ethanol, and dry the product in a vacuum oven at 80° C. for 5 hours;
[0074] (6) The above product was heat-treated at 400° C. for 3 hours in an air atmosphere to obtain the final product.
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Abstract
The invention discloses a preparation method for an economical, safe and environment-friendly Nb3O7F nanometer material. The method comprises the following steps: (1) adding a surfactant into a solvent and fully stirring and dissolving; (2) adding NbF5 powder into a solution acquired in the step (1) and fully stirring and dissolving; (3) adding hydrochloric acid into the solution acquired in the step (2) and continuously uniform stirring; (4) transferring the solution acquired in the step (3) into a polytetrafluoroethylene lining reaction still, sealing and then putting into an oven for hydrothermal reaction; (5) ending reaction, and then centrifugally separating the product, using deionized water and absolute ethyl alcohol for washing and drying in the oven; (6) performing thermal treatment on the product, thereby acquiring the Nb3O7F nanometer material. The method disclosed by the invention is simple in process and is safe and environment-friendly; the operation condition is easily controlled; the preparation of the Nb3O7F nanometer material under the condition of no added hydrofluoric acid is firstly realized; and the method is suitable for less preparation in laboratory and volume production.
Description
technical field [0001] The invention relates to an economical, safe and environment-friendly Nb 3 o 7 The preparation method of F nanometer material, specifically a kind of preparation Nb under the condition that adopts cheap niobium source and does not add hydrofluoric acid 3 o 7 F Nanomaterials Methods. Background technique [0002] Due to traditional TiO 2 There are problems of poor spectral response, carrier separation and low transport efficiency. Although rapid development has been achieved in recent years, it is still difficult to completely solve the above three issues in the short term. In recent years, the research and development of some new photocatalytic materials has attracted the general attention of scholars in the industry. Among them, Nb 3 o 7 F due to TiO 2 It has similar electronic structure and energy band structure, single phase, good crystallinity, strong anti-oxidation ability, high photocatalytic activity and so on, which has aroused people's...
Claims
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Application Information
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