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Preparation method for vanadium sulfide/attapulgite nanocomposite with wide spectral response and application

A nano-composite material and attapulgite technology, which is applied in the wide-spectrum response vanadium tetrasulfide/attapulgite nano-composite material and its preparation, and in the field of photocatalytic nitrogen fixation, can solve the problems of easy recombination of photogenerated electrons and holes, and achieve The effect of prolonging life, improving efficiency, and uniform particle size

Active Publication Date: 2019-07-12
江苏纳欧新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve VS 4 The problem that photogenerated electrons and holes are extremely easy to recombine, the present invention provides a broad-spectrum response vanadium tetrasulfide / attapulgite nanocomposite photocatalytic material

Method used

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  • Preparation method for vanadium sulfide/attapulgite nanocomposite with wide spectral response and application
  • Preparation method for vanadium sulfide/attapulgite nanocomposite with wide spectral response and application
  • Preparation method for vanadium sulfide/attapulgite nanocomposite with wide spectral response and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Add 0.67g of Na 3 VO 4 12H 2 O, 0.50 g of CH 3 CSNH 2 1. Add 0.5g of ATP to an appropriate amount of deionized water, and ultrasonically disperse it to make it evenly mixed. Na 3 VO 4 At the molecular level, it is adsorbed by the oxygen-containing functional groups on the surface of ATP and fixed on the surface of ATP.

[0019] (2) Transfer the solution to a microwave hydrothermal kettle for microwave hydrothermal reaction, set the power to 400W, set the temperature to 150°C, and set the time to 5h;

[0020] (3) Centrifuge the product prepared in step (2) with a centrifuge (10000r / min, 2min), wash it with deionized water for 3 times, and dry it in an oven to obtain 60wt% VS 4 / ATP composite photocatalytic material.

[0021] Scanning electron microscopy (SEM) was performed on the obtained samples ( figure 1 ) and transmission electron microscope TEM observation ( figure 2 ), it can be seen that VS is evenly compounded on the surface of ATP 4 Nanoparticles...

Embodiment 2

[0026] (1) 0.33g of Na 3 VO 4 12H 2 O, 0.25g of CH 3 CSNH 2 1. Add 0.5g of ATP to an appropriate amount of deionized water, and ultrasonically disperse it to make it evenly mixed. Na 3 VO 4 At the molecular level, it is adsorbed by the oxygen-containing functional groups on the surface of ATP and fixed on the surface of ATP.

[0027] (2) Transfer the solution to a microwave hydrothermal kettle for microwave hydrothermal reaction, set the power to 400W, set the temperature to 160°C, and set the time to 4h;

[0028] (3) Centrifuge the product prepared in step (2) with a centrifuge (10000r / min, 2min), wash it with deionized water for 3 times, and dry it in an oven to obtain 30wt% VS 4 / ATP composite photocatalytic material.

[0029] Subsequent detection was as in Example 1.

[0030] After 4h light, 30wt% VS 4 / ATP reached the ammonium ion generation rate of 106.3μmol·g cat –1 h –1 amount of nitrogen fixation.

Embodiment 3

[0032] (1) Add 0.45g of Na 3 VO 4 12H 2 O, 0.34g of CH 3 CSNH 2 1. Add 0.5g of ATP to an appropriate amount of deionized water, and ultrasonically disperse it to make it evenly mixed. Na 3 VO 4 At the molecular level, it is adsorbed by the oxygen-containing functional groups on the surface of ATP and fixed on the surface of ATP.

[0033](2) Transfer the solution to a microwave hydrothermal kettle for microwave hydrothermal reaction, set the power to 400W, set the temperature to 170°C and set the time to 3h;

[0034] (3) Centrifuge the product prepared in step (2) with a centrifuge (10000r / min, 2min), wash it with deionized water for 3 times, and dry it in an oven to obtain 40wt% VS 4 / ATP composite photocatalytic material.

[0035] Subsequent detection was as in Example 1.

[0036] After 4h light, 40wt% VS 4 / ATP reached the ammonium ion generation rate of 121.7μmol·g cat –1 h –1 amount of nitrogen fixation.

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Abstract

The invention belongs to the technical field of chemical new materials and relates to a preparation method for a vanadium sulfide / attapulgite nanocomposite with wide spectral response and an application. The preparation method comprises the steps: (1) adding Na3VO4.12H2O, CH3CSNH2 and attapulgite into deionized water, and carrying out ultrasonic uniform mixing; (2) transferring the solution into amicrowave hydrothermal kettle, and carrying out a microwave hydrothermal reaction; and (3) subjecting a reaction product prepared in the step (2) to centrifugation with a centrifuge, carrying out washing with deionized water, and carrying out baking, thereby obtaining the vanadium tetrasulfide / attapulgite composite photocatalytic material. According to the preparation method and the application,a vanadium tetrasulfide / attapulgite nano-catalyst is synthesized by using a microwave hydrothermal method, and N2 can be converted into NH3 to the maximum under the irradiation of a broad spectrum (ultraviolet to near-infrared), so that the vanadium sulfide / attapulgite nanocomposite has excellent light nitrogen fixing capacity.

Description

technical field [0001] The invention belongs to the field of new chemical materials, and in particular relates to a wide-spectrum response vanadium tetrasulfide / attapulgite nanocomposite material, a preparation method thereof and application of photocatalytic nitrogen fixation. Background technique [0002] Nitrogen makes up the major component of the Earth's atmosphere (∼78 vol%), but is difficult to utilize due to the very large activation barrier (941 kJ / mol) for the cleavage of N≡N bonds. At present, the artificial nitrogen fixation method widely implemented in the industry is the Haber-Bosch process, but its reaction conditions require high temperature and high pressure, and the pollution is serious. Therefore, it is of great social significance to develop an artificial nitrogen fixation process that is more environmentally friendly and consumes less energy. Among them, the photocatalytic nitrogen fixation and ammonia production technology has attracted widespread atte...

Claims

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Application Information

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IPC IPC(8): B01J27/04B01J35/08B01J37/34B01J37/10C01C1/02
CPCB01J27/04B01J37/346B01J37/10C01C1/026B01J35/399B01J35/23B01J35/51B01J35/39Y02P20/52
Inventor 李霞章姚超何承溧吴凤芹张海镧严向玉左士祥刘文杰
Owner 江苏纳欧新材料有限公司