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Preparation method and application of transition metal phosphide used for hydrogenating dechlorination

A transition metal, hydrodechlorination technology, applied in the direction of chloride preparation, chemical instruments and methods, non-metallic elements, etc., can solve the problems of small catalyst surface area, low catalytic activity, etc., to improve hydrodechlorination activity, Good repeatability and stable catalytic performance

Active Publication Date: 2016-02-24
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] For above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a kind of preparation method of the transition metal phosphide that is used for hydrodechlorination reaction, to solve existing pure phase transition metal phosphide catalyst surface area is very little, catalytic activity not high problem

Method used

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  • Preparation method and application of transition metal phosphide used for hydrogenating dechlorination
  • Preparation method and application of transition metal phosphide used for hydrogenating dechlorination
  • Preparation method and application of transition metal phosphide used for hydrogenating dechlorination

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Weigh 4.0 g of ammonium molybdate tetrahydrate and 3.0 g of diammonium hydrogen phosphate, mix and dissolve in 30 ml of deionized water, and dissolve 5.0 g of polyethylene glycol with a molecular weight of 8000 in the above solution to obtain a mixed aqueous solution. The aqueous solution was stirred at 80° C. for 3 h, evaporated to dryness at 100° C., dried at 120° C. for 12 h, and calcined at 500° C. for 5 h to prepare the catalyst precursor in oxidation state. The precursor is ground, pressed into tablets and sieved to obtain 20-40 mesh particles.

[0022] in H 2 Under the atmosphere, after raising the particle to 350°C in 0.5h, at 1°C min -1 The rate was increased to 650°C and kept at this temperature for 2h. h 2 Under the atmosphere, after the temperature was lowered to room temperature, the catalyst was prepared.

[0023] Under a hydrogen atmosphere, the catalyst is placed in a quartz tube, and trichlorethylene is carried by hydrogen into the quartz tube to ca...

Embodiment 2

[0025] Weigh 4.0 g of ammonium molybdate tetrahydrate and 3.0 g of diammonium hydrogen phosphate, mix and dissolve in 30 ml of deionized water, and dissolve 1.0 g of polyethylene glycol with a molecular weight of 8000 in the above solution to obtain a mixed aqueous solution. Subsequent operations are the same as in Example 1. The catalyst prepared by this method is used in the hydrodechlorination reaction of trichlorethylene, and the hydrogen chloride yield can reach up to 54.2%.

Embodiment 3

[0027] Weigh 4.0 g of ammonium molybdate tetrahydrate and 3.0 g of diammonium hydrogen phosphate, mix and dissolve in 70 ml of deionized water, and dissolve 15.0 g of polyethylene glycol with a molecular weight of 8000 in the above solution to obtain a mixed aqueous solution. Subsequent operations are the same as in Example 1. The catalyst prepared by this method is used in the hydrodechlorination reaction of trichlorethylene, and the hydrogen chloride yield can reach up to 68.2%.

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Abstract

The present invention discloses a preparation method and application of transition metal phosphide used for hydrogenating dechlorination. The preparation method comprises the following steps: 1. dissolving soluble metallic salt and diammonium phosphate in water, and dissolving polyethylene glycol in the solvent; 2. stirring an aqueous solution obtained in the step 1 at a temperature of 80 DEG C for 3 hours, then heating up the stirred aqueous solution to the temperature of 100 DEG C to dry the aqueous solution in a steaming manner, then drying at a temperature of 120 DEG C for 12 hours, and then calcining at a temperature of 500 DEG C for 5 hours to obtain an oxidizing precursor; and 3. grinding and tabletting the oxidizing precursor obtained in the step 2 into pieces, screening to obtain particulate matters with meshes of 20-40, and performing reduction on the particulate matters by a heating reduction method to obtain modified transition metal phosphide. When used as a catalyst, the phosphide performs hydrogenating dechlorination and has an significantly improved catalytic activity compared with an unmodified catalyst. The method is simple and easy to operate, and meanwhile can effectively improve hydrogenating dechlorination catalytic activity of the transition metal phosphide.

Description

technical field [0001] The invention relates to the technical field of catalytic hydrodechlorination, in particular to a method for preparing a transition metal phosphide used in hydrodechlorination reaction, which is used to improve its catalytic activity in hydrodechlorination reaction. Background technique [0002] Trichloroethylene (TCE for short) is a colorless, volatile, insoluble in water, aromatic liquid, and carcinogenic. Trichlorethylene is widely used, such as degreasing of metal surfaces, dry cleaning of clothes, extraction of plant and mineral oils, preparation of medicines, organic synthesis, and dissolution of grease, rubber, resins, alkaloids, waxes, and organic chemicals. Raw materials and raw materials for pesticides and medicines. As a widely used solvent, TCE is one of the most widely distributed pollutants in the current environment. [0003] Trichlorethylene treatment methods mainly include biodegradation, activated carbon adsorption, chemical oxidati...

Claims

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Application Information

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IPC IPC(8): B01J27/19B01J27/185A62D3/37C01B7/03A62D101/22
CPCA62D3/37A62D2101/22B01J27/1853B01J27/19C01B7/035
Inventor 任丽丽刘晓梦
Owner SOUTHEAST UNIV
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