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Controllable synthesis method of nickel phosphide micro-nano material

A synthesis method and technology of nickel phosphide, applied in chemical instruments and methods, phosphide, alkali metal compounds, etc., can solve the problems of toxicity, long hydrothermal time, and high reaction temperature, and achieve easy recovery, simple operation, and reaction conditions. mild effect

Inactive Publication Date: 2015-09-30
LIAONING INST OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above experimental method has successfully prepared nickel phosphide in various phases, the raw materials used, such as sodium phosphide and white phosphorus, have certain toxicity. Therefore, scientific researchers are also trying to use non-toxic phosphorus sources as nickel phosphide
For example, Liu et al. used non-toxic red phosphorus and nickel chloride as starting materials to form a mixed system with solvent ethylenediamine and surfactant polyacrylamide, and reacted in a high-pressure hydrothermal kettle at 180°C for 20 hours to prepare a compound with Ni with good dispersibility 2 P nanocrystalline (Journa of Crystal Growth, 2003, 252(1-3): 297), but the reaction temperature of this method is high, the hydrothermal time is long, and the reaction requires a surfactant

Method used

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  • Controllable synthesis method of nickel phosphide micro-nano material
  • Controllable synthesis method of nickel phosphide micro-nano material

Examples

Experimental program
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Embodiment 1

[0032] Synthesis of Ni by Changing the Phosphorus-Nickel Ratio 2 P or Ni 12 P 5 : select the P / Ni molar ratio to be 1 / / 1, 2 / 1, 4 / 1, 6 / 1, 8 / 1 respectively for hydrothermal synthesis. It is only described when the P / Ni molar ratio is 6. Put 10.9009g (0.0375 moL) of nickel nitrate and 50mL of distilled water into a 100mL beaker, stir well until the solution is clear, then add 6.975g (0.225moL) of fully ground red phosphorus. Put the beaker in a water bath with electromagnetic stirring at 60°C for aging for 2 hours, then transfer the suspension into a 100mL polytetrafluoroethylene-lined autoclave, seal it, and place it in a constant temperature drying oven at 120°C for 12 hours. No surfactant was added in the experiment. After the reaction, the reactor was taken out and cooled to room temperature naturally. The black solid matter in the autoclave was collected, and centrifuged and washed with hot ethanol and distilled water in order to remove unreacted inorganic substances do...

Embodiment 2

[0035] Synthesis of Ni by changing the hydrothermal temperature 12 P 5 : Put 10.9009g of nickel nitrate (0.0375mol) and 50ml of distilled water into a 100ml beaker, stir well until the solution becomes clear, then add 4.65g (0.15mol) of fully ground red phosphorus. The hydrothermal reaction temperature was set at 90 o C. 120 o C. 150 o C and 180 o C, the reaction time is 12h, the solvent is water, and no surfactant is added. All the other operating steps are the same as in Example 1.

[0036] figure 2 X-ray powder diffraction (XRD) spectra of synthesized products at different temperatures when n(P) / n(Ni)=4. It can be seen from the figure that when P / Ni=4, the reaction temperature is 90 o C, at 2θ=32.7 o , 35.8 o , 38.4 o , 41.7 o , 44.4 o , 47.0 o , 49.0 o The series of diffraction peaks that appear are attributed to Ni 12 P 5 (PDF22-1190), showing that the resulting product is mainly Ni 12 P 5 , but there are still many impurity peaks in the resulting spec...

Embodiment 3

[0039] Synthesis of Ni by changing the hydrothermal temperature 12 P 5 or Ni 2 P: Put 10.9009g of nickel nitrate (0.0375mol) and 50ml of distilled water in a 100ml beaker, stir well until the solution becomes clear, then add 9.3g (0.3mol) of fully ground red phosphorus. The hydrothermal reaction temperature was set at 90 o C. 120 o C. 150 o C and 180 o C, the reaction time is 12h, the solvent is water, and no surfactant is added. All the other operating steps are the same as in Example 1.

[0040] Figure 4 X-ray powder diffraction (XRD) spectra of synthesized products at different temperatures when n(P) / n(Ni)=8. It can be seen from the figure that when the reaction temperature is 90 o C, at 2θ=40.8 o , 44.6 o , 47.3 o , 54.4 0 The characteristic diffraction peaks appearing at can be attributed to Ni 2P(PDF03-0953), the peak intensity is larger, but at 2θ=38.4 o , 49.0 o There is also a characteristic diffraction peak with low intensity, which can be attributed...

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Abstract

The invention relates to a controllable synthesis method of a nickel phosphide micro-nano material. The method includes the following steps: dissolving a certain amount of soluble nickel salt into deionized water, adding a proper amount of fully ground red phosphorus to obtain a suspension, placing the suspension into an ultrasonic cleaning machine for 1-3 hours, transferring the suspension into an autoclave, heating to 90-180 DEG C and carrying out a hydrothermal reaction for 6-18 hours. The obtained micro-nano material is Ni2P or Ni12P, and the morphology of Ni2P or Ni12P is densely packed nanoparticles with the particle size of 60-120 nm. Compared with the prior art, the non-toxic red phosphorus is used as a phosphorus source; without the presence of a surfactant, pure Ni2P or Ni12P5 can be obtained through changing the ratio of nickel to phosphorus, the hydrothermal temperature and the hydrothermal time; the method is lower in reaction temperature, shorter in reaction time, environment-friendly and applicable to mass production; the prepared nickel phosphide micro-nano material shows good catalytic performance in aspects of adsorption removal of heavy metals and photocatalytic degradation of organic dyes.

Description

technical field [0001] The invention relates to a nickel phosphide (Ni 2 P and Ni 12 P 5 ) The controllable synthesis method of micro-nano materials, and its application in the photocatalytic degradation of organic dyes and the adsorption and removal of heavy metals. Background technique [0002] In recent years, transition metal phosphide micro-nano materials have always been one of the hot research areas for researchers because of their promising application prospects in the fields of catalysis, optics, electricity, magnetism and semiconductors. Phosphide catalysts were early used in the hydrogenation of unsaturated hydrocarbons and nitro compounds (Journal of Catalysis, 1983, 79(1): 207). Further studies have shown that transition metal phosphides are also a stable anti-sulfur compound. Hydrodesulfurization and hydrodenitrogenation reactions have highly efficient catalytic performance and excellent reaction characteristics, among which nickel phosphide (Ni 2 P) The ov...

Claims

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Application Information

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IPC IPC(8): C01B25/08B01J27/185B01J20/06B01J20/28B01J20/30
Inventor 鄢景森鄂永胜田亚赛张闯张恒
Owner LIAONING INST OF SCI & TECH
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