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Mercury-free catalyst applied to stationery bed for preparing chloroethylene and preparation method thereof

A mercury catalyst and fixed bed technology, applied in the field of mercury-free catalysts and their preparation, can solve the problems of high risk of aqua regia, high equipment requirements, increase the difficulty of catalysts, etc., and achieve a simple and efficient preparation method, improve synergy, and improve catalysis. Effects of activity and stability

Active Publication Date: 2014-02-05
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aqua regia plays an important role in improving the activity and stability of catalysts, but the introduction of aqua regia requires higher equipment in the catalyst preparation process, and aqua regia is more dangerous, which increases the difficulty of catalysts in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025](1) Pretreatment of carrier: 0.3g cobalt chloride is dissolved in 50g mass concentration and is in the hydrochloric acid solution of 5%, stirs 1 hour under room temperature, obtains the hydrochloric acid solution (a) containing cobalt chloride; The shell carbon carrier was added to the solution (a); at a temperature of 50°C, it was left to stand and sealed for 24 hours, and then the mixture was suction-filtered and separated, and then the obtained filter cake was dried at 130°C to obtain the pretreated carrier A;

[0026] (2) Uploading of active components: under room temperature stirring condition, 0.01g gold trichloride and 0.05g ferric chloride are dissolved in 20g deionized water, obtain solution (b) after fully dissolving; 20g mass concentration is 5% hydrogen peroxide solution is slowly added to pretreated carrier A, and then solution (b) is slowly added. After the mixed solution stops boiling, it is left to stand in airtight storage for 24 hours, and then the mixtu...

Embodiment 2

[0028] (1) Pretreatment of carrier: adding 9g gac carrier to 50g mass concentration is 5% sodium hydroxide solution to obtain the mixture (a) of carrier and solution; react at 60°C for 2 hours, then the mixture is suction filtered, Separating and washing with water until neutral, then drying the obtained filter cake at 130°C to obtain pretreated carrier A;

[0029] (2) Loading of additives: under stirring conditions at room temperature, dissolve 1 g of copper chloride in 30 g of deionized water, then add concentrated hydrochloric acid dropwise to make the pH of the additive solution 2, and obtain a solution of a certain concentration (b) ; Then add the solution (b) to the pretreated carrier A, let it stand and store it airtight for 24 hours, then filter and separate the mixture, and dry the obtained filter cake at 130°C to obtain the pretreated carrier B;

[0030] (3) Uploading of the active component: under stirring at room temperature, 0.01g gold trichloride and 0.05g ferric...

Embodiment 3

[0032] (1) Pretreatment of the carrier: 0.3 g of ruthenium trichloride was dissolved in 50 g of 5% hydrochloric acid solution, stirred at room temperature for 1 hour to obtain a hydrochloric acid solution (a) containing ruthenium trichloride; Add 9g of coconut shell charcoal carrier to the solution (a); at 50°C, keep it airtight and store for 24 hours, then filter and separate the mixture with suction, and then dry the obtained filter cake at 130°C to obtain the pretreated Carrier A;

[0033] (2) Loading of the active component: under stirring at room temperature, 0.002g of gold trichloride and 0.005g of ferric chloride were dissolved in 20g of deionized water to obtain solution (b); The hydrogen peroxide solution was slowly added to the pretreated carrier A, and then the solution (b) was slowly added. After the mixed solution stopped boiling, it was kept in an airtight place for 48 hours. After drying, the required catalyst is obtained, and the number is Cat-3.

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Abstract

The invention provides a mercury-free catalyst applied to stationery bed for preparing chloroethylene and a preparation method thereof. The catalyst takes activated carbon, pretreated by hydrochloric acid or sodium hydroxide water solution, as a carrier, and gold trichloride and ferric chloride as active components, and compared with the ordinary mercury-free catalyst, according to the preparation method of the catalyst, the gold trichloride is guaranteed not to be reduced and can be uniformly and firmly loaded on the surface of the activated carbon carrier by replacing nitrohydrochloric acid in the preparation of the catalyst with hydrogen peroxide and taking other metal chloride, capable of promoting the decomposition of the hydrogen peroxide, as auxiliaries. The catalyst has high activity and selectivity in the reaction of preparing chloroethylene in the stationery bed through acetylene hydrochlorination, and the preparation method is simple and efficient, and green and environment-friendly, and has important practical significance in the industrial application.

Description

technical field [0001] The invention proposes a mercury-free catalyst for the synthesis of vinyl chloride by fixed-bed acetylene hydrochlorination and a preparation method thereof. The catalyst uses activated carbon pretreated with hydrochloric acid or sodium hydroxide aqueous solution as the carrier, and uses gold trichloride and ferric chloride as the active components. Compared with ordinary mercury-free catalysts, the preparation method of the catalyst uses hydrogen peroxide instead of the catalyst Aqua regia in the preparation, and other metal chlorides that can promote the decomposition of hydrogen peroxide are used as auxiliary agents to ensure that gold trichloride is not reduced as much as possible, and can be evenly and firmly loaded on the surface of the activated carbon carrier. The catalyst has high activity and selectivity in the reaction of preparing vinyl chloride by hydrochlorination of acetylene in a fixed bed, and the preparation method is simple, efficient,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/128B01J27/13C07C21/06C07C17/08
Inventor 李伟晁松林关庆鑫
Owner NANKAI UNIV
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