Hydrodechlorination palladium-carbon catalyst and preparation method

A palladium carbon catalyst, hydrodechlorination technology, applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problems of short life, easy loss of active components, poor selectivity, etc., to achieve Long life, stable selectivity, and high selectivity

Inactive Publication Date: 2016-06-22
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the problems of current hydrodechlorination catalysts such as poor selectivity, short service life, and easy loss of active components, and provide a hydrodechlorination catalyst for the production of chloroacetic acid with high activity, high selectivity and long service life. Palladium carbon catalyst and preparation method thereof

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  • Hydrodechlorination palladium-carbon catalyst and preparation method

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Comparison scheme
Effect test

Embodiment 1

[0030] The mass percent composition of the palladium carbon catalyst prepared in this example is: Pd content 0.5%, Re content 0.5%, Cl content 0.5%, and the rest is activated carbon carrier. Among them, Pd is the active component, Re and Cl are additives, and the specific surface area of ​​the carrier activated carbon is 800m 2 / g. The preparation method of this catalyst is as follows:

[0031] (1) Under the water bath condition of 60 ℃, the mass concentration of activated carbon is 10% HNO 3 After treatment, it was washed with desalted water until neutral, and then dried at 110°C for 10 hours for use.

[0032] (2) Add the activated carbon obtained in step (1) to the perrhenic acid aqueous solution, immerse it in a water bath at 30°C for 5h, then dry it at 110°C for 2h, and then calcinate it under a nitrogen atmosphere at 400°C for 4h to obtain the supported Rhenium activated carbon.

[0033] (3) Configure palladium chloride aqueous solution, and adjust the pH of the palla...

Embodiment 2

[0035] The palladium-carbon catalyst prepared in this example has a mass percent composition of 0.8% Pd, 1.0% Re, and 1.5% Cl, and the rest is an activated carbon carrier. Among them, Pd is the active component, Re and Cl are additives, and the specific surface area of ​​the carrier activated carbon is 900m 2 / g. The preparation method of this catalyst is as follows:

[0036] (1) Under the water bath condition of 70 ℃, the mass concentration of activated carbon is 20% HNO 3 Treated in neutral for 12h, washed with desalted water to neutral after treatment, and then dried at 110°C for 10h for use.

[0037] (2) The activated carbon obtained in the step (1) is added to the ammonium perrhenate aqueous solution, immersed in an equal volume in a water bath at 40°C for 8h, then dried at 110°C for 3h, and then calcined for 5h under a nitrogen atmosphere at 500°C to obtain Activated carbon loaded with rhenium.

[0038] (3) Configure palladium chloride aqueous solution, and adjust th...

Embodiment 3

[0040]The mass percent composition of the palladium carbon catalyst prepared in this example is that the Pd content is 1.5%, the Re content is 2%, and the Cl content is 3%, and the carrier is activated carbon. Among them, Pd is the active component, Re and Cl are additives, and the specific surface of the carrier activated carbon is 1000m 2 / g. The preparation method of this catalyst is as follows:

[0041] (1) Under the water bath condition of 80 ℃, the mass concentration of activated carbon is 30% HNO 3 Treated in neutral for 15h, washed with desalted water to neutral after treatment, and then dried at 110°C for 10h for use.

[0042] (2) The activated carbon obtained in step (1) is added to an aqueous solution of potassium perrhenate, immersed in an equal volume in a water bath at 60°C for 10h, then dried at 110°C for 4h, and then calcined for 6h under a nitrogen atmosphere at 600°C to obtain Activated carbon loaded with rhenium.

[0043] (3) Configure palladium chloride...

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Abstract

The invention discloses a hydrodechlorination palladium-carbon catalyst and a preparation method. The catalyst is prepared from, by mass, 0.5-1.5% of Pd, 0.5-2% of Re, 0.5-3% of Cl and the balance an activated carbon carrier. The prepared catalyst is high in activity and selectivity, and long in service life. The preparation method is easy to implement and good in repeatability. The catalyst is mainly used for purifying a chlorination solution in the chloroacetic acid industry, high-purity monochloro acetic acid can be obtained after the chlorination solution is subjected to the hydrodechlorination reaction through the catalyst, and meanwhile mother solution zero release is achieved.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and mainly relates to a hydrogenation dechlorination palladium carbon catalyst, which is mainly used for purifying and purifying chlorinated liquid in the chloroacetic acid industry. Background technique [0002] Chloroacetic acid is an important fine chemical product and organic chemical intermediate, widely used in the production of pesticides, medicines, dyes, carboxymethyl cellulose, etc. At present, the domestic production of chloroacetic acid is mainly prepared by the direct chlorination of acetic acid. Although the method is simple, by-products such as dichloroacetic acid are unavoidable in the generated chlorination solution, and 10-20 % of chlorinated mother liquors, the generation of these mother liquors not only increases production costs, reduces product competitiveness but also pollutes the environment. At present, supported palladium and platinum catalysts are widely u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/13C07C51/487C07C53/16
CPCB01J27/13C07C51/487C07C53/16
Inventor 史文涛杜小宝王志文曹立王绍伟吕睿袁海朋
Owner CHINA TIANCHEN ENG
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