Nickel phosphide catalyst containing sulphur and application of nickel phosphide catalyst

A catalyst, nickel phosphide technology, used in physical/chemical process catalysts, organic chemistry, hydrogenation to hydrocarbons, etc., can solve the problems of low activity of transition metal phosphides, not attracting attention, etc., and achieve easy quantitative preparation, improved activity, The effect of improving hydrogenation activity

Inactive Publication Date: 2015-09-30
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activity of transition metal phosphides is generally lower than that of corresponding transition metals, so it has not attracted attention

Method used

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  • Nickel phosphide catalyst containing sulphur and application of nickel phosphide catalyst
  • Nickel phosphide catalyst containing sulphur and application of nickel phosphide catalyst
  • Nickel phosphide catalyst containing sulphur and application of nickel phosphide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of Ni by Temperature Programmed Reduction of Phosphate Precursor 2 p.

[0037] 3.90 g of nickel nitrate (Ni(NO 3 ) 2 4H 2 O) and 1.77 grams of diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was added to 20 mL of deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear green solution. Continue heating and stirring to evaporate water to obtain a solid product, dry at 120°C for 12 hours to dry the water, and bake at 500°C for 3 hours to obtain a phosphate precursor with a Ni / P molar ratio of 1.

[0038] The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to 120°C at 5°C / min, and kept at 120°C for 1 hour to drive off the water adsorbed by the catalyst; (2) from 120°C to 5°C / min. to 400°C, ...

Embodiment 2

[0040] After the catalyst was prepared according to the method described in Example 1, the temperature was lowered to 340° C. for sulfidation. The used vulcanization liquid raw material is the dimethyl disulfide / decalin solution of 0.8% (mass fraction), and the vulcanization condition is: H 2 Pressure 4MPa, temperature 340°C, liquid hourly space velocity 54 hours -1 , the sulfidation treatment time is 2 hours, and the prepared catalyst is recorded as Ni 2 P-I. According to the XRD spectrum ( figure 2 ), with Ni 2 P standard spectrum comparison (PDF 74-1385), shows that the obtained solid structure is Ni 2 p. XPS spectrum ( Figure 5 ) indicates that the surface of the catalyst contains sulfur, and according to the position of the characteristic peak, the main sulfur species is S δ- (0<δ≤2). The sulfur content (in atomic percent) was 2.2%.

Embodiment 3

[0042] Preparation of Ni by Reduction of Phosphate Precursors by Hydrogen Cooled Plasma 2 P active phase, then use H under an inert or reducing gas atmosphere 2 S passivated the surface to prepare the catalyst.

[0043] The dielectric barrier discharge (DBD) is used to generate hydrogen non-equilibrium plasma for the reduction of phosphate precursors to prepare transition metal phosphides. Take 0.8 g of the phosphate precursor in Example 1, grind, tablet, pulverize and sieve to obtain 20-40 mesh particles, which are filled in the annulus between the electrodes in the reactor. The discharge frequency is fixed at about 10kHz, and the input voltage is 70V. Atmospheric pressure, H 2 The gas velocity is 150mL / min, and the treatment time is 2 hours, and the Ni 2 p. Then pass through 10% H 2 S / H 2 The gas passivates the surface of the newly synthesized metal phosphide, and the catalyst is denoted as Ni 2 P-II. According to the XRD spectrum ( image 3 ), with Ni 2 P standar...

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Abstract

The invention relates to a nickel phosphide catalyst containing sulphur and application of the nickel phosphide catalyst. For the nickel phosphide catalyst, the molar ratio of nickel to phosphorus is 0.1-5, the content of phosphorus is 25% or below by atomic percentage. The nickel phosphide catalyst containing sulphur disclosed by the invention has high selectivity in selective hydrogenation reaction of unsatured unsaturated hydrocarbon compounds and nitrobenzene compounds, has selectivity equivalent to that of Ni2P prepared by adopting the traditional temperature programmed reduction method of phosphate, but has activity obviously improved. Compared with the viewpoint generally known in the prior art that sulphur has side effects for metal hydrogenation catalysts or metalloid hydrogenation catalysts, i.e., sulphur is a toxicant and can be used for greatly reducing the activity of the catalyst, the nickel phosphide catalyst containing sulphur provided by the invention has the advantage that by introducing an appropriate amount of sulphur into the Ni2P catalyst, the hydrogenation activity of the Ni2P catalyst can be significantly improved under the condition that the selectivity of the Ni2P catalyst is not affected.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysis, and in particular relates to a solid selective hydrogenation catalyst mainly used for selective hydrogenation of unsaturated hydrocarbons and nitro reduction of nitroaromatic compounds. Background technique [0002] Transition metal phosphides are a general term for covalent compounds formed by phosphorus and transition metals (Fe, Co, Ni, Mo, and W, etc.). Transition metal phosphides can be divided into metal-rich phosphides (M / P≥1) and phosphorus-rich phosphides (M / P<1) according to the stoichiometric ratio of phosphorus to metal (M). The latter is unstable, while metal-rich transition metal phosphides are hard and have good thermodynamic and chemical stability, which can be used as catalysts. Although these transition metal phosphides are covalent compounds, most of them have metallic properties and are conductors of electricity and heat. Early studies on transition metal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C07B31/00C07C5/11C07C5/09C07C5/03C07C15/073C07C15/46C07C13/48C07C209/36C07C211/46C07C211/52
Inventor 李翔田松王安杰
Owner DALIAN UNIV OF TECH
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