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Preparation and application of synthesizing chloroethylene mercury free catalyst through acetylene method

A non-mercury catalyst and vinyl chloride technology, applied in the field of catalysis, can solve the problems of uneven distribution of components, short life, low catalytic activity, etc., and achieve the effects of simple preparation method, prolonged service life and improved reaction activity

Inactive Publication Date: 2012-10-31
DALIAN RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing non-mercury catalyst preparation technology for the synthesis of vinyl chloride by acetylene method, traditional external heat conduction technology is adopted, such as drying in an oven, and the temperature outside the particle is higher than the inside, so the evaporation of water starts from the outside of the particle and the orifice. The humidity gradient causes the solution to migrate from the inside of the particle to the outside, resulting in the redistribution of active components, resulting in uneven distribution of components inside and outside the particle, resulting in low catalytic activity and short life

Method used

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  • Preparation and application of synthesizing chloroethylene mercury free catalyst through acetylene method

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Experimental program
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Effect test

Embodiment 1

[0030] Stir 10 g of activated carbon with 2 mol / L hydrochloric acid in a 70°C water bath for 4 hours, filter, wash with deionized water several times until the filtrate is neutral, and dry at 120°C for 12 hours. Dissolve 0.2654g of chloroplatinic acid and 0.5212g of lanthanum chloride in 15ml of 2mol / L hydrochloric acid, add dropwise into the pretreated activated carbon after clarification, and impregnate at room temperature for 4h; Microwave treatment at 1000W and 2450MHz for 5min under protection to obtain a catalyst with a Pt content of 1% and a La content of 2%.

[0031] Use this catalyst for evaluation: put the catalyst in a stainless steel fixed-bed reactor with an inner diameter of 10mm and a length of 40cm, heat and control the temperature by electric heating, raise the temperature to 180°C, pass in hydrogen chloride for activation for 1 hour, and then pass in acetylene, the ratio of raw gas is V (HCl):V(C 2 h 2 )=1.15, acetylene space velocity 100h -1 , The reactio...

Embodiment 2

[0033] Stir 10 g of activated carbon with 5 mol / L hydrochloric acid in a 70°C water bath for 4 hours, filter, wash with deionized water several times until the filtrate is neutral, and dry at 120°C for 12 hours. Dissolve 0.2091g of chloroauric acid, 0.0265g of chloroplatinic acid, and 0.4050g of nickel chloride in 15ml of aqua regia, add dropwise to the pretreated activated carbon after clarification, impregnate for 4 hours at room temperature, and then place the impregnated catalyst in a microwave reactor , and microwaved at 500W and 2450MHz for 15min under the protection of nitrogen to obtain a catalyst with 1% Au content, 0.1% Pt content and 1% Ni content.

[0034] Evaluate the reaction performance of its acetylene synthesis vinyl chloride by the method of embodiment 1, wherein change reaction temperature control is 160 ℃, raw gas ratio is V (HCl): V (C 2 h 2 ) = 1.2, acetylene space velocity 40h-1 . The results are shown in Table 1.

Embodiment 3

[0036] Stir 10 g of activated carbon with 1 mol / L hydrochloric acid in a 70°C water bath for 4 hours, filter, wash with deionized water several times until the filtrate is neutral, and dry at 120°C for 12 hours. Dissolve 0.1666g of palladium chloride, 0.5369g of copper chloride, and 0.1653g of potassium chloride in 15ml of 1mol / L hydrochloric acid, add dropwise to the pretreated activated carbon after clarification, impregnate at room temperature for 4h, and then place the impregnated catalyst in microwave In the reactor, microwave treatment at 700W and 2450MHz for 10min under the protection of nitrogen to obtain a catalyst with a Pd content of 1%, a Cu content of 2%, and a K content of 1%.

[0037] Evaluate the reaction performance of its acetylene synthesis vinyl chloride by the method of embodiment 1, wherein change reaction temperature control is 170 ℃, raw gas ratio is V (HCl): V (C 2 h 2 ) = 1.2, acetylene space velocity 30h -1 . The results are shown in Table 1.

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Abstract

The invention provides a preparation method of synthesizing chloroethylene mercury free catalyst through an acetylene method. The mercury free catalyst comprises a main active ingredient, a promoter and a carrier, the method comprises the steps of: pre-treating the carrier, preparing impregnation mother liquor, impregnating and microwave radiating, and the like, and the microwave radiating step comprises the steps: processing through microwave with power of 100-1000 W and frequency of 2450+ / -50 MHz under the protection of a shielding gas. The impregnation assisted microwave radiating method of preparing heavy metal loaded type catalyst in the invention has the advantages of energy saving, high efficiency and fastness, and the active ingredients are uniformly loaded on the carrier within a short period to improve the catalytic performance of the catalyst, improve the action activity and prolong the service life.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a method for preparing a non-mercury catalyst for synthesizing vinyl chloride by an acetylene method, and also relates to a method for synthesizing vinyl chloride by reacting hydrogen chloride and acetylene using a non-mercury catalyst. Background technique [0002] Vinyl chloride is an important raw material for organic synthesis, and its main use is to produce polyvinyl chloride. At present, there are two main methods for the synthesis of vinyl chloride: the acetylene method and the ethylene method. At present, more than 95% of the production capacity of vinyl chloride monomer in the world adopts ethylene process. Due to the characteristics of rich coal and little oil in our country, and the high international oil price in recent years, the vinyl chloride monomer in my country is still dominated by the acetylene process of the coal chemical route. [0003] At pr...

Claims

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Application Information

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IPC IPC(8): B01J23/63B01J23/89B01J29/76B01J37/34C07C21/06C07C17/08
Inventor 孟纪文邵玉昌左洪亮吴井龙
Owner DALIAN RES & DESIGN INST OF CHEM IND