Silicon dioxide microsphere surface loaded ferrous sulfide nanocrystal, and preparation method and application thereof

A technology of silicon dioxide and ferrous sulfide, which is applied in the field of nanomaterials, can solve the problems of insufficient performance improvement, complex raw materials, and cumbersome steps of amorphous structure sulfurized nano-zero-valent iron, and achieve good application prospects, high reactivity, and preparation The effect of simple method

Active Publication Date: 2020-12-01
NORTHEAST GASOLINEEUM UNIV
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Problems solved by technology

Although this method achieves the dispersion of sulfurized nano-zero-valent iron, its raw materials are too complicated, and the steps of polymer template synthesis of silica mesoporous shell and sodium borohydride reduction of iron valence are too cumbersome, which increases the cost. , there is a defect that the catalytic performance of amorphous structure sulfide nano-zero-valent iron is not enough to improve

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  • Silicon dioxide microsphere surface loaded ferrous sulfide nanocrystal, and preparation method and application thereof
  • Silicon dioxide microsphere surface loaded ferrous sulfide nanocrystal, and preparation method and application thereof
  • Silicon dioxide microsphere surface loaded ferrous sulfide nanocrystal, and preparation method and application thereof

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preparation example Construction

[0038] In the second aspect, the present invention provides a method for preparing a ferrous sulfide nanocrystalline composite material supported on the surface of silica microspheres. The preparation method comprises: (1) preparing solid silica microspheres; (2) modifying the surface of the solid silica microspheres with mercapto groups to obtain mercapto-modified silica microspheres; (3) preparing silica microspheres modified with mercapto groups; Ferrous sulfide crystals loaded on the surface of silica microspheres.

[0039] In one embodiment, the preparation method of the silicon dioxide microsphere surface loading ferrous sulfide nanocrystalline composite material of the present invention comprises:

[0040] (1) Prepare silica solid microspheres under the condition of no template

[0041] Mix 5 to 20 parts by volume of absolute ethanol, 3 to 10 parts by volume of deionized water and 0.5 to 2 parts by volume of ammonia water, stir in a constant temperature water bath at 2...

Embodiment 1

[0064] (1) Mix 50mL of absolute ethanol, 15mL of deionized water and 5mL of ammonia water, and stir in a constant temperature water bath at 35°C for 10min to mix all components evenly; Continue to stir at a constant speed in the constant temperature water bath, add 0.5mL 3-(mercaptopropyl)triethoxysilane to the system after 12 hours of reaction, and ultrasonically disperse the surface mercapto-modified silica solid microspheres after continuing the reaction for 12 hours.

[0065] (2) Under the condition of nitrogen protection, disperse the product obtained in step (1) into 60mL water, then mix with 5mL of 15mmol / L ferrous sulfate solution, and drop 5mmol / L of ferrous sulfate solution at a speed of 2mL / min Thioacetamide solution 4.2mL, reacted at 35°C for 2h.

[0066] (3) Centrifuge the obtained dispersion at room temperature at 10,000 r / min for 5 minutes, wash the separated solid with water twice, and dry it in a constant temperature drying oven at 50°C to obtain the vulcanize...

Embodiment 2

[0073] (1) Mix 70mL of absolute ethanol, 25mL of deionized water and 5mL of ammonia water, and stir in a constant temperature water bath at 25°C for 10min to mix all components evenly; Continue stirring at a constant speed in a constant temperature water bath, add 1mL of 3-(mercaptopropyl)triethoxysilane to the system after reacting for 24 hours, and ultrasonically disperse the surface mercapto-modified silica solid microspheres after continuing the reaction for 24 hours.

[0074] (2) Under the condition of nitrogen protection, disperse the product obtained in step (1) into 60mL water, then mix with 5mL of 10mmol / L ferrous sulfate solution, and add 10mmol / L of Thioacetamide solution 3.3mL, reacted at 55°C for 0.5h.

[0075] (3) Centrifuge the obtained dispersion at room temperature at 10,000 r / min for 5 minutes, wash the separated solid with water twice, and dry it in a constant temperature drying oven at 50°C to obtain the vulcanized silica microspheres supported on the surfa...

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Abstract

The invention provides a silicon dioxide microsphere surface loaded ferrous sulfide nanocrystal composite material. The silicon dioxide microsphere surface loaded ferrous sulfide nanocrystal compositematerial comprises a silicon dioxide microsphere carrier and ferrous sulfide crystals loaded on the silicon dioxide microsphere carrier; the silicon dioxide microsphere carrier is a solid sphere, andthe particle size of the silicon dioxide microsphere carrier is 100-500 nm; the ferrous sulfide crystals are uniformly distributed on the surface of the silicon dioxide microsphere carrier, and the particle size of the crystals is 5-15 nm. The invention provides a preparation method of the composite material. The preparation method comprises the following steps: (1) preparing silicon dioxide microspheres; (2) carrying out surface sulfydryl modification on the silicon dioxide microspheres; and (3) loading the ferrous sulfide crystals on the surfaces of the sulfydryl modified silicon dioxide microspheres. The invention also provides application of the composite material. The composite material disclosed by the invention is higher in reaction activity, higher in mechanical strength and higher in stability. The microcosmic sizes of the carrier silicon dioxide solid spheres and ferrous sulfide are controllable, the dispersity of ferrous sulfide nanocrystals on the surface of the carrier isadjustable, the preparation method is simple, the cost is low, and the composite material has good application prospects in multiple fields.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular, the invention relates to a ferrous sulfide nanocrystal supported on the surface of a silica microsphere, a preparation method and application thereof. Background technique [0002] The size and nature of the interaction between nano-metal particles or microcrystalline particles and oxide supports are the key factors that determine the catalytic activity and selectivity. Therefore, it is important to study the heterogeneous catalysis and energy conversion of metal (crystal) particles on oxide supports. Scientific research significance and application value. The metal (crystal) is dispersed on a support carrier with a high specific surface area, and the dispersion and size effect of the metal (crystal) particles will be one of the most critical factors determining the reactivity and specificity of the supported metal catalyst. Due to its good thermal stability, large specific ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/12C01B33/18B82Y40/00B82Y30/00B01J27/043B01J31/02B01J35/08C02F1/00
CPCC01G49/12C01B33/18B82Y40/00B82Y30/00B01J27/043B01J31/0274B01J31/0275C02F1/00C01P2004/62C01P2004/64C01P2004/32C01P2004/80C01P2002/77B01J35/23B01J35/33B01J35/51
Inventor 施伟光付晓飞卿红霞刘飞于学聪闫秀玲孙先达张健许承武王以辰赵万春柳波石颖
Owner NORTHEAST GASOLINEEUM UNIV
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