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Hollow urchin-like phosphide material and preparation method

A sea urchin-like, phosphide technology, applied in the field of synthesis of new catalytic materials, can solve the problems of difficult operation, white phosphorus is highly toxic, flammable and explosive, etc., to reduce the risk, the preparation method is simple and easy, and the conditions are easy to control Effect

Inactive Publication Date: 2017-06-20
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the phosphorus source used in the preparation of phosphides by the hydrothermal method is mainly white phosphorus, which is highly toxic, flammable and explosive in the air, and difficult to handle.

Method used

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  • Hollow urchin-like phosphide material and preparation method
  • Hollow urchin-like phosphide material and preparation method
  • Hollow urchin-like phosphide material and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Hollow sea urchin Ni 2 Preparation of P:

[0038] Step 1, prepare Ni simple substance: 0.713gNiCl 2 ·6H 2 0.0.2g polyvinylpyrrolidone (PVP) and 1mL hydrazine hydrate (mass percentage is 80%) are dissolved in 30mL ethylene glycol, magnetic stirring is until mixed evenly, and the mixed solution obtained is transferred in the hydrothermal reaction kettle, in Treat at 170°C for 6h. The obtained gray precipitate was centrifuged and washed several times with absolute ethanol and distilled water, and dried in a vacuum oven at 60° C. for 6 hours to obtain gray Ni powder with a diameter of 1-5 μm.

[0039] Step 2, preparing hollow sea urchin-like Ni 2 P: Disperse 0.379g of Ni elemental substance prepared in step 1 in a mixed solvent consisting of 20mL of absolute ethanol and 10mL of distilled water, and form a mixed solution under ultrasonic treatment. The resulting mixed solution was transferred to a hydrothermal reaction kettle, and 0.1 g of red phosphorus was added. Wil...

Embodiment 2

[0042] Hollow sea urchin Ni 2 Preparation of P:

[0043] In Example 1, the hydrothermal treatment temperature in step 1 was changed to 100°C, and the hydrothermal treatment time was changed to 2h; the hydrothermal treatment temperature in step 2 was changed to 100°C, and the hydrothermal treatment time was changed to 2h, and the obtained product was a hollow sea urchin with uneven appearance. Ni 2 P, the particle size is 1-5um, and the wall thickness is 0.5-1um.

Embodiment 3

[0045] Hollow sea urchin Ni 2 Preparation of P:

[0046] In Example 1, the hydrothermal treatment temperature in step 1 was changed to 220°C, and the hydrothermal treatment time was changed to 16h; the hydrothermal treatment temperature in step 2 was changed to 220°C, and the hydrothermal treatment time was changed to 20h, and the obtained product was hollow sea urchin-like Ni 2 P, the particle size is 1-5um, and the wall thickness is 0.5-1um.

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Abstract

The invention relates to hollow urchin-like phosphide. The hollow urchin-like phosphide has a hollow urchin-like shape; the grain diameter is 1mum to 5mum and the wall thickness is 0.5mum to 1mum; a structural formula of the phosphide is represented as AxPy, wherein x and y are determined through valence states of metal A and phosphorus; the metal A is selected from one or more of elements including metal nickel, cobalt, iron, molybdenum, tungsten, sodium, calcium, zinc, aluminum and copper. The hollow urchin-like phosphide is prepared through the following steps: uniformly mixing a prepared metal A monomer microsphere with an alcohol water solution by ultrasounds, and adding a mixture and red phosphorus into a high-pressure kettle and carrying out hydrothermal treatment; after reacting, collecting a product and washing to prepare the hollow urchin-like phosphide. According to the hollow urchin-like phosphide provided by the invention, the raw materials are simple and easy to obtain; a phosphorus source adopts the toxin-free red phosphorus instead of toxic flammable and explosive white phosphorus, so that the dangers of experiments are extremely reduced. The synthesized hollow urchin-like phosphide has the advantages of low density and large specific surface area, and can cover more active sites on a relatively large specific surface area, so that the catalytic activity is higher.

Description

technical field [0001] The invention belongs to the technical field of synthesis of novel catalytic materials, and in particular relates to a hollow sea urchin-shaped phosphide material and a preparation method thereof. Background technique [0002] Phosphide catalyst is a kind of catalytic material that has attracted people's attention after nitrides and carbides. It not only has similar physical properties to nitrides and carbides, but also has better sulfur resistance, hydrogenation activity, and Carbon deposition and anti-poisoning ability, compared with platinum group noble metals, phosphide catalysts are cheaper. In recent years, transition metal phosphides, as a new type of catalytic material with high activity, high stability and resistance to sulfur poisoning, have attracted extensive attention due to their applications in many fields. [0003] There are many methods for preparing phosphide catalysts, and the temperature-programmed reduction method is currently a c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J27/19B01J27/188B01J27/14C01B25/08C07G1/00C08H7/00C02F1/30C02F101/30
CPCC01B25/08C02F1/30C07G1/00C08H6/00B01J27/14B01J27/1853B01J27/188B01J27/19C01P2004/03C02F2101/308C01P2004/61B01J35/50B01J35/40B01J35/39
Inventor 纪娜张晴黄艺博王琪琪刁新勇宋春风刘庆岭
Owner TIANJIN UNIV
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