Method for preparing vinyl chloride by taking azacyclo-protonic acid ionic liquid as medium through acetylene hydrochlorination

A technology for producing vinyl chloride and ionic liquids by chlorination, which is applied in hydrogen halide addition preparation, organic chemistry, etc., can solve the problems of expensive ionic liquids and unfavorable industrial production, and achieve good industrial application prospects, good solubility, and preparation The effect of simple method

Active Publication Date: 2014-10-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the price of ionic liquids is relatively expensive, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Using N-methylimidazole as a raw material, passing an excess mole of hydrogen chloride into it, and reacting at 80°C, the protonic acid ionic liquid N-methylimidazolium chloride [MIm]Cl can be produced.

[0029] Characterization of the physical properties of protonic acid ionic liquid N-methylimidazolium chloride [MIm]Cl: 1H NMR (500MHz, DMSO-d6, δ / ppm relative to TMS): 3.91(3H, s), 7.69(1H, t;), 7.77(1H, t), 9.24(1H, s), 15.16(1H, s;).

[0030] 268.90mg of copper chloride CuCl 2 The catalyst was dissolved in 20mL of ionic liquid reaction medium, the molar concentration of the catalyst was 0.1mol / L, mixed and heated at a temperature of 120°C, fully dissolved for 40min, and then moved into the reaction device. Before the reaction, pass hydrogen chloride at 120°C to activate the catalytic system for 1 hour, then raise the temperature to 200°C for reaction, the flow rate of acetylene is 5ml / min, and the molar ratio of reactant hydrogen chloride to acetylene is 1:1. The r...

Embodiment 2

[0032] Use N-ethylimidazole as raw material, pass into hydrogen chloride wherein, generate protonic acid ionic liquid N-ethylimidazole chloride [EIm]Cl, the palladium chloride PdCl of 177.33mg 2The catalyst was dissolved in 20 mL of ionic liquid reaction medium, the molar concentration of the catalyst was 0.05 mol / L, mixed and heated at a temperature of 120 ° C, fully dissolved for 40 min, and then moved into the reaction device. Before the reaction, pass hydrogen chloride at 120°C to activate the catalytic system for 1 hour, then raise the temperature to 180°C for reaction, the flow rate of acetylene is 5ml / min, and the molar ratio of reactant hydrogen chloride to acetylene is 1.2:1. The reaction tail gas was deacidified and dried, then passed to gas chromatography for analysis. According to gas chromatography analysis, the conversion rate after stabilization can reach 75%, and the selectivity is greater than 99.5%, and the catalytic system is stable during the reaction proce...

Embodiment 3

[0036] Using N-butylpiperidine as a raw material, hydrogen chloride is passed into it to generate protonic acid ionic liquid N-butylpiperidine chloride [P 4 ]Cl, the chloroauric acid HAuCl of 247.11mg 4 4H 2 The O catalyst was dissolved in 20 mL of ionic liquid reaction medium, the molar concentration of the catalyst was 0.03 mol / L, mixed and heated at a temperature of 120 ° C, fully dissolved for 40 min, and then moved into the reaction device. Before the reaction, pass hydrogen chloride at 140°C to activate the catalytic system for 1 hour, then raise the temperature to 160°C for reaction, the flow rate of acetylene is 5ml / min, and the molar ratio of reactant hydrogen chloride to acetylene is 1.25:1. The reaction tail gas was deacidified and dried, then passed to gas chromatography for analysis. According to gas chromatography analysis, the conversion rate after stabilization can reach 80%, and the selectivity is greater than 99.5%, and the catalytic system is stable during...

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PUM

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Abstract

The invention discloses a method for preparing vinyl chloride by taking an azacyclo-protonic acid ionic liquid as a medium through acetylene hydrochlorination. The method comprises the following steps: by taking the azacyclo-protonic acid ionic liquid which is synthesized by taking an azacycle compound as a raw material as the medium, mixing with a non-mercury catalyst to prepare a catalysis system, feeding the catalysis system into an acetylene hydrochlorination catalysis system firstly, and subsequently feeding acetylene and hydrogen chloride for reaction. The method adopts the ionic liquid as the reaction medium and the non-mercury metal compound as the catalyst, green and environment-friendly liquid phase reaction of acetylene hydrochlorination is achieved, and moreover the azacyclo-protonic acid ionic liquid is simple to prepare, economic and good in application prospect.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing vinyl chloride by hydrochlorination of acetylene using nitrogen heterocyclic protonic acid ionic liquid as a medium. Background technique [0002] Polyvinyl chloride (PVC) is widely used in our lives as a plastic material, which is produced by polymerization of vinyl chloride monomer (VCM). At present, there are two main methods for the preparation of vinyl chloride monomer in industry, one is the acetylene method derived from the coal chemical industry route, and the other is the ethylene method derived from the petrochemical route. In my country, coal resources are abundant and oil resources are relatively scarce, so the acetylene hydrochlorination reaction derived from the coal chemical industry route is the main production process for the synthesis of vinyl chloride monomer in my country, accounting for more than 70% of vinyl chloride producti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/08C07C21/06
Inventor 邢华斌胡静逸杨启炜任其龙苏宝根鲍宗必张志国杨亦文
Owner ZHEJIANG UNIV
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