Anion modified mercury-free catalyst for ethyne hydrochlorination reaction, and preparation method thereof

A technology of acetylene hydrochlorination and anion modification, applied in physical/chemical process catalysts, hydrogen halide addition preparation, chemical instruments and methods, etc., can solve problems such as mercury pollution, achieve high catalytic activity, and solve catalyst deactivation Problems, Harm Reduction Effects

Inactive Publication Date: 2013-09-04
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the deficiencies in the prior art, provide a mercury-free catalyst for acetylene hydrochlorination and a preparation method thereof, improve the catalytic activity and selectivity of this type of catalyst, and improve its reaction stability, in the hope of improving the catalyst in a relatively economical environment. Solving the problem of mercury pollution in the process of producing vinyl chloride by acetylene method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 1.28g CuCl 2 2H 2 O was dissolved in 13.5ml of water to prepare an impregnating solution, which was divided into three impregnations. Each time, 4.5ml of the impregnating solution was added to 4g of acid-washed activated carbon, sealed and impregnated at 70°C for 4h, quickly dried at 140°C for 12h, and the above operation was repeated twice. to obtain the desired catalyst. The reaction conditions are hydrogen chloride activation 30min, acetylene space velocity 150h -1 , the reaction temperature is 180°C, the ratio of raw materials n (C 2 h 2 ) / n(HC1)=1:1.1. The catalyst catalyzes the acetylene hydrochlorination reaction under the above conditions, the conversion rate of the acetylene is 50%, and the selectivity of the vinyl chloride is greater than 99%.

Embodiment 2

[0026] 0.95g Cu 3 (PO4) 2 Dissolve in 13.5ml of water, stir evenly to prepare impregnating solution, and impregnate three times. For the first load, 4.5ml of impregnating solution was added to 4g of acid-washed activated carbon, sealed and impregnated at 70°C for 12h, and quickly dried at 140°C for 6h. Take 4.5ml of impregnating solution for the last two loads and add it to the catalyst after the last load, impregnate and dry under the same conditions as the first load. The reaction conditions are hydrogen chloride activation 30min, acetylene space velocity 180h -1 , the reaction temperature is 140°C, the raw material ratio n (C 2 h 2 ) / n(HC1)=1:1.1. The catalyst catalyzes the hydrochlorination of acetylene under the above conditions, and the conversion rate of acetylene is 53%, and the selectivity of vinyl chloride is greater than 99%.

Embodiment 3

[0028] Weigh 0.937g CuSO 4 2H 2 O was dissolved in 13.5ml of water to prepare the impregnating solution, which was divided into three times, and 4.5ml of the impregnating solution was added to 4g of activated carbon each time, sealed and impregnated at 70°C for 4h, quickly dried at 140°C for 12h, and the above operation was repeated twice to obtain required catalyst. The reaction conditions are hydrogen chloride activation 30min, acetylene space velocity 180h -1 , the reaction temperature is 140°C, the raw material ratio n (C 2 h 2 ) / n(HC1)=1:1.1. The catalyst catalyzes the hydrochlorination of acetylene under the above conditions, and the conversion rate of acetylene is 20.9%, and the selectivity of vinyl chloride is greater than 99%.

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Abstract

The invention discloses an anion modified mercury-free catalyst for an ethyne hydrochlorination reaction, and a preparation method thereof. The catalyst comprises a catalyst carrier and an active component, wherein the catalyst carrier is active carbon, the active component is a sulfate, a chloride, a phosphate or a pyrophosphate of copper or tin, and the carrier is acid-washed active carbon or phosphorus doped active carbon. The preparation method comprises preparing an active component impregnating solution, adding a catalyst carrier to carry out equivalent volume impregnation, drying, baking and other process steps. According to the present invention, acetylene and hydrogen chloride are mixed and then are subjected to a reaction in the catalyst system, wherein the catalysis system of the present invention has characteristics of environmental protection and safety compared with the current mercury catalyst in the industry; and the catalyst prepared by the preparation method has characteristics of high activity, high selectivity, good stability, and longer service life, and is more suitable for ethyne hydrochlorination reactions for producing vinyl chloride through a calcium carbide method compared with the general mercury-free catalyst.

Description

technical field [0001] The invention belongs to industrial catalytic production of vinyl chloride monomer, and more specifically relates to an anion-modified mercury-free catalyst used for acetylene hydrochlorination and a preparation method thereof. Background technique [0002] At present, due to the superior performance and versatility of polyvinyl chloride, its demand is also increasing day by day, making the production of vinyl chloride monomer also increase year by year. The synthesis methods of vinyl chloride monomer mainly include ethylene method and acetylene method. Based on the shortage of petroleum resources and the relative abundance of coal resources in my country, the production of vinyl chloride by acetylene has always occupied a dominant position in the domestic market. This method uses mercuric chloride catalyst as catalyst, but mercuric chloride is easy to volatilize and lose, and the liquid mercury metal reduced in the reaction will also be lost. Accord...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/122B01J27/18B01J27/055B01J27/25B01J27/10B01J27/053C07C21/06C07C17/08
Inventor 王富民张绪立张金利张旭斌王录李航
Owner TIANJIN UNIV
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