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Catalyst for acetylene hydrochlorination and preparation method and application thereof

An acetylene hydrochlorination and catalyst technology, which is applied in physical/chemical process catalysts, chemical instruments and methods, hydrogen halide addition preparation, etc., can solve the problems of strictness, complicated operation process, complicated operation, etc. The effect of large specific surface area, good catalytic activity and selectivity

Pending Publication Date: 2020-07-10
鄂尔多斯市瀚博科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst is applied to the reaction of preparing vinyl chloride by fixed-bed acetylene hydrochlorination, which has certain catalytic activity and selectivity; but the preparation of the catalyst requires multiple solidification, temperature programming, and HF solution etching processes, so the conditions are relatively low. Strict, complex operation
[0006] Patent CN 104549401 B discloses a method for preparing a non-metallic catalyst for acetylene hydrochlorination. A non-metallic compound containing at least one of N, O, S and P is dissolved in a solvent and heated in a water bath at 30°C-100°C and stir to dissolve the impregnating solution; immerse the catalyst carrier in the impregnating solution, seal and stir for impregnation, and filter off the liquid; dry, put it in a tube furnace or a muffle furnace, heat up in a nitrogen atmosphere, and cool to room temperature. The catalyst reduces the pollution caused by the metal catalyst to the environment; the initial conversion rate of acetylene can be significantly improved compared with the activated carbon catalyst that does not support non-metallic components, and the selectivity of generating vinyl chloride is greater than 99.0%; but there are also complicated operation processes The problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] First, weigh 25g of wood-based activated carbon and soak it in 60mL of 5% hydrochloric acid solution for 3 hours at a temperature of 50°C, then wash it with deionized water until the pH of the aqueous solution is close to 5.5, and dry it at 120°C for 12 hours to obtain pickling After the activated carbon; Weigh 2.38g of urea and 2.98g of ammonium hypophosphite and dissolve it in 30mL of deionized water, put the acid-washed activated carbon into the above-mentioned prepared solution, soak it at 40°C for 5h, and use a rotary evaporator to remove The water was evaporated to dryness, and the catalyst A was obtained by calcining at 500° C. for 3 h under a nitrogen atmosphere. Take 10g of Catalyst A, put it into a fixed bed reactor, under normal pressure, 200℃, 20h -1 and HCl / C 2 h 2 The volume ratio is 1.1 under reaction conditions.

Embodiment 2

[0065] First, weigh 25g of wood-based activated carbon and put it into 60mL of hydrochloric acid solution with a mass fraction of 7% and soak for 3h at a temperature of 50°C, then wash with deionized water until the pH of the aqueous solution is close to 5.5, and dry at 120°C for 12h to obtain pickling After the activated carbon; Weigh 2.98g of urea and 2.98g of ammonium hypophosphite and dissolve in 30mL of deionized water, put the acid-washed activated carbon into the above prepared solution, soak it at 40°C for 5h, and use a rotary evaporator to remove The water was evaporated to dryness, and then calcined at 450° C. for 5 h under a nitrogen atmosphere to obtain catalyst B. Take 10g of Catalyst B, put it into a fixed bed reactor, under normal pressure, 200℃, 20h -1 and HCl / C 2 h 2 The volume ratio is 1.1 under reaction conditions.

Embodiment 3

[0067] First, weigh 25g of wood-based activated carbon and soak it in 60mL of 5% hydrochloric acid solution for 3 hours at a temperature of 50°C, then wash it with deionized water until the pH of the aqueous solution is close to 5.5, and dry it at 120°C for 12 hours to obtain pickling After the activated carbon; Weigh 3.58g of urea and 2.98g of ammonium hypophosphite and dissolve it in 30mL of deionized water, put the acid-washed activated carbon into the above-mentioned prepared solution, soak it at 40°C for 5h, and use a rotary evaporator to remove The water was evaporated to dryness, and the catalyst C was obtained by calcining at 500° C. for 5 h under a nitrogen atmosphere. Take 10g of Catalyst C, put it into a fixed bed reactor, under normal pressure, 200℃, 20h -1 and HCl / C 2 h 2 The volume ratio is 1.1 under reaction conditions.

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PUM

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Abstract

The invention discloses a nitrogen-phosphorus co-doped metal-free catalyst for acetylene hydrochlorination reaction and a preparation method and application of thereof, and belongs to the field of material synthesis technology and application. The nitrogen-phosphorus co-doped metal-free catalyst is prepared by blending acid-washed activated carbon with a precursor solution of nitrogen and phosphorus, dipping, drying and roasting and is applied to preparation of vinyl chloride monomers by hydrochlorination of acetylene. The prepared porous activated carbon metal-free catalyst is large in specific surface area and contains nitrogen and phosphorus at the same time and is simple in preparation process and can replace a toxic mercuric chloride catalyst. The metal-free catalyst is applied to fixed bed acetylene hydrochlorination to prepare vinyl chloride and has good catalytic activity and selectivity and good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and relates to a nitrogen-phosphorus co-doped metal-free catalyst for acetylene hydrochlorination, a preparation method and application thereof. Background technique [0002] Polyvinyl chloride (PVC) is widely used in many fields such as building materials, agriculture and national defense, and its output ranks second in the world's polyester output. Since my country has abundant coal resources, polyethylene monomers are mostly produced by acetylene hydrochlorination, and the reaction catalyst is mercuric chloride catalyst supported by activated carbon. Since the mercury catalyst is easily lost during use, it is easy to cause problems such as environmental pollution. Therefore, we are eager to develop a mercury-free catalyst for acetylene hydrochlorination. [0003] In recent years, the research on mercury-free catalysts has made continuous progress, mainly focusing on the following ...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07C17/08B01J35/10C07C21/06
CPCB01J27/24C07C17/08B01J35/618B01J35/617B01J35/615C07C21/06
Inventor 李杰牛强周斌解荣永赵长森
Owner 鄂尔多斯市瀚博科技有限公司
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