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Preparation method and application of a rare earth fluoride/lithium niobate composite photocatalytic material

A composite photocatalysis and rare earth fluoride technology, which is applied in the preparation/separation of ammonia, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low utilization rate of sunlight, increase catalytic performance, improve Sunlight utilization rate, strong reduction effect

Active Publication Date: 2020-05-26
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem of low utilization rate of sunlight, the invention provides a rare earth fluoride / lithium niobate composite photocatalytic material

Method used

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  • Preparation method and application of a rare earth fluoride/lithium niobate composite photocatalytic material
  • Preparation method and application of a rare earth fluoride/lithium niobate composite photocatalytic material
  • Preparation method and application of a rare earth fluoride/lithium niobate composite photocatalytic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) 0.3g (0.676mmol) of niobium hydroxide (H 5 Nb 3 o 10 ) into 50ml of 0.2mol / L oxalic acid solution, stirred by the rotor, heated in a water bath at 70°C for 20min to form a transparent solution; ensure that the molar ratio of niobium hydroxide to oxalic acid is less than or equal to 2:15;

[0024] (2) Drop ammonia solution into the sample prepared in step (1), until the white precipitate is completely separated out; wherein the amount of ammonia water is slightly excessive;

[0025] (3) Take the suspension in the middle and lower layers of step (2), centrifuge the precipitate, wash with distilled water, and centrifuge twice, each time at 8000r / min, 2min;

[0026] (4) Dissolve the precipitate in step (3) in citric acid solution of 100mL0.04mol / L, and dissolve 0.0851g lithium hydroxide monohydrate (LiOH·H 2 O) and 0.16g of cerium fluoride (CeF 3 ) was added to the solution; among them, the molar ratio [Li + ]:[Nb 5+ ]:[CeF 3 ]=1:1:40%, using the sol-gel method, he...

Embodiment 2

[0035] (1) 0.3g (0.676mmol) of niobium hydroxide (H 5 Nb 3 o 10 ) into 50ml of 0.2mol / L oxalic acid solution, stirred by the rotor, heated in a water bath at 80°C for 25min to form a transparent solution; ensure that the molar ratio of niobium hydroxide to oxalic acid is less than or equal to 2:15;

[0036] (2) Drop ammonia solution into the sample prepared in step (1), until the white precipitate is completely separated out; wherein the amount of ammonia water is slightly excessive;

[0037] (3) Take the suspension in the middle and lower layers of step (2), centrifuge the precipitate, wash with distilled water, and centrifuge twice, each time at 8000r / min, 2min;

[0038] (4) Dissolve the precipitate in step (3) in citric acid solution of 100mL0.04mol / L, and dissolve 0.0851g lithium hydroxide monohydrate (LiOH·H 2 O) and 0.04g of praseodymium fluoride (PrF 3 ) was added to the solution; among them, the molar ratio [Li + ]:[Nb 5+ ]:[PrF 3 ]=1:1:10%, using the sol-gel me...

Embodiment 3

[0043] (1) 0.3g (0.676mmol) of niobium hydroxide (H 5 Nb 3 o 10 ) into 50ml of 0.2mol / L oxalic acid solution, stirred by the rotor, heated in a water bath at 90°C for 30min to form a transparent solution; ensure that the molar ratio of niobium hydroxide to oxalic acid is less than or equal to 2:15;

[0044] (2) Drop ammonia solution into the sample prepared in step (1), until the white precipitate is completely separated out; wherein the amount of ammonia water is slightly excessive;

[0045] (3) Take the suspension in the middle and lower layers of step (2), centrifuge the precipitate, wash with distilled water, and centrifuge twice, each time at 8000r / min, 2min;

[0046] (4) Dissolve the precipitate in step (3) in citric acid solution of 100mL0.04mol / L, and dissolve 0.0851g lithium hydroxide monohydrate (LiOH·H 2 O) and 0.09g of ytterbium fluoride (YbF 3 ) was added to the solution; among them, the molar ratio [Li + ]:[Nb 5+ ]:[YbF 3 ]=1:1:20%, using the sol-gel metho...

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Abstract

The invention belongs to the photocatalyst field and discloses a preparation method and application of a rare earth fluoride / lithium niobate composite photocatalytic material. The preparation method comprises the following steps: dispersing niobium hydroxide into an oxalic acid solution, and stirring the mixture to form a transparent solution; dropwise adding an ammonia water solution until whiteprecipitates are completely separated; carrying out centrifugation so as to obtain precipitates, and washing the precipitates with distilled water; and dissolving the precipitates into a citric acid solution, adding lithium hydrate monohydrate and rare earth fluoride into the solution, heating the solution in a water bath kettle so as to form a transparent solution precursor solution, heating to be dry so as to obtain gel, putting the gel into a muffle furnace, carrying out calcining, and grinding, so as to obtain the rare earth fluoride / lithium niobate composite photocatalytic material. By constructing a Z-shaped heterojunction between REF3 and LiNbO3, the photoinduced electron-hole separation effect is relatively obvious, and the composite photocatalytic material has a relatively negative conduction band and relatively strong reducibility, so that N2 can be relatively easily reduced into NH3, and the catalytic performance of the photocatalyst is improved.

Description

technical field [0001] The invention belongs to the field of photocatalysts, in particular to a preparation method and application of a rare earth fluoride / lithium niobate composite photocatalytic material. Background technique [0002] Nitrogen fixation in nature is mainly through lightning and microbial nitrogen fixation, but the nitrogen fixed in nature is far from meeting the needs of industrial and agricultural production. At present, the artificial nitrogen fixation method widely used in industry is the Haber-Bosch industrial nitrogen fixation method to produce ammonia, but the equipment requirements are high, the energy consumption is large, and the pollution is serious. Therefore, it is of great social significance to develop and develop a green, clean, and low-energy artificial nitrogen fixation process. With the continuous development of heterogeneous photocatalytic technology, photocatalytic nitrogen fixation and ammonia production technology has attracted extens...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/12C01C1/04
CPCY02P20/52
Inventor 李霞章何承溧陈晓凡左士祥姚超李忠玉
Owner CHANGZHOU UNIV