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A kind of environment-friendly acetylene hydrochlorination catalyst and preparation method thereof

A kind of acetylene hydrochlorination, environment-friendly technology, applied in catalyst activation/preparation, physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, etc., can solve low mass transfer, gas metal dispersion No high problems, achieve high catalytic activity, high stability, and reduce the effect of mass transfer

Active Publication Date: 2022-06-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide an environment-friendly acetylene hydrochlorination catalyst and its preparation method. The present invention fundamentally solves the shortcomings of low gas metal dispersion and low mass transfer in the loaded ionic liquid catalyst system

Method used

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  • A kind of environment-friendly acetylene hydrochlorination catalyst and preparation method thereof
  • A kind of environment-friendly acetylene hydrochlorination catalyst and preparation method thereof
  • A kind of environment-friendly acetylene hydrochlorination catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Preparation of catalyst:

[0077] 1) Select 10 g of zirconium nitride as the carrier, dissolve it in 40 mL of nitrogen nitrogen dimethylformamide, stir for 30 min, and add 0.1 g of dimethyldichlorosilane and 1.0 g of triethylamine. The above mixture was heat treated under nitrogen at 50°C for 5 hours. After filtering, the filter cake was washed with nitrosodimethylformamide and ethanol, dried at 180°C, and the obtained solid sample was used for later use.

[0078] 2) Dissolve 0.04g of 1-octyl-3-methylimidazolium hexafluorophosphate and 0.06g of 1-propyl-3-butylimidazolium tetrafluoroborate ionic liquid in 10mL of nitrogen-nitrogen dimethylformamide , after stirring evenly, the solid sample obtained in step 1) was added, immersed for 10 h, and dried at 180° C. for use. The mass loading of the ionic liquid is 1%.

[0079] 3) Dissolve 0.009g of chloroauric acid and 0.13g of sodium chloride in 0.09mL of nitrogen-nitrogen dimethylformamide, stir evenly, add the sample obt...

Embodiment 2

[0084] Preparation of catalyst:

[0085] 1) Select 10 g of silicon nitride as the carrier, dissolve it in 100 mL of toluene, stir for 30 min, and add 0.1 g of dimethyldichlorosilane and 0.2 g of triethylamine. The above mixture was heat treated under nitrogen at 80°C for 3 hours. After filtering, the filter cake was washed with toluene and ethanol, dried at 180°C, and the obtained solid sample was used for later use.

[0086] 2) Dissolve 0.4 g of 1-hexyl-3-ylimidazolium hexafluorophosphate and 1.6 g of nitrogen methylpyrrolidone hydrochloride ionic liquid in 10 mL of toluene, stir evenly, add the solid sample obtained in step 1), immerse 2h, and dried at 180°C for later use. The mass loading of the ionic liquid is 20%.

[0087] 3) Dissolve 4.23g cupric chloride and 0.03g barium chloride in 2.12mL toluene, stir evenly, add the sample obtained in step 2), immerse it in an external 0.6kV static electric field for 2.5h, and heat it at 180°C Dry under conditions for later use. ...

Embodiment 3

[0092] Preparation of catalyst:

[0093] 1) Select 10 g of titanium nitride as the carrier, dissolve it in 200 mL of nitrogen methyl pyrrolidone, stir for 30 min, and add 0.6 g of dimethyldichlorosilane and 1.0 g of triethylamine. The above mixture was heat treated under nitrogen at 70°C for 4 hours. After filtering, the filter cake was washed with nitrogen methyl pyrrolidone and ethanol, dried at 180°C, and the obtained solid sample was used for later use.

[0094]2) Dissolve 1.0 g of 1-ethyl-2,3-dimethylimidazolium tetrafluorophosphate and 0.5 g of triphenylmethylphosphonium bromide ionic liquid in 30 mL of nitrogen methylpyrrolidone, stir evenly, and add step 1 ), immersed for 8 h, and dried at 180 °C for later use. The mass loading of the ionic liquid is 15%.

[0095] 3) Mix 0.103 g of ruthenium chloride and 0.73 g of ferric chloride and dissolve in 0.5 mL of nitrogen methyl pyrrolidone, stir evenly, add the sample obtained in step 2), immerse it in an external 0.8 kV s...

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Abstract

The invention provides an environment-friendly acetylene hydrochlorination catalyst and a preparation method thereof. The dispersion effect of the metal in the nitrided carrier of the catalyst of the invention is better, the catalytic activity is higher, and the stability is better. The ionic liquid in the invention It is stabilized on the surface of the carrier through the silanol, which is not easy to lose from the surface of the carrier. The metal is stabilized on the outer layer of the catalyst by coordinating with the ionic liquid, which reduces the influence of mass transfer and improves the dispersion of the metal. The present invention For the first time, an external static electric field is introduced into the preparation of metal-based catalysts loaded with ionic liquids, which promotes the enrichment of metal active centers on the surface of ionic liquids. Since the metal active centers of the catalyst of the present invention are distributed on the surface of ionic liquids, the influence of substrate diffusion is reduced. , the induction period of the catalyst disappears under the reaction conditions evaluated.

Description

(1) Technical field [0001] The invention relates to an environment-friendly acetylene hydrochlorination catalyst and a preparation method thereof. (2) Background technology [0002] Vinyl chloride is the monomer of polyvinyl chloride (PVC), one of the five major synthetic resins in the world, and is mainly produced by the calcium carbide acetylene method and the petroleum ethylene method. China's coal-rich, oil-poor, and gas-less energy resources determine that for a long time in the future, the calcium carbide acetylene process will continue to be the main process for the production of vinyl chloride in my country, that is, mercury chloride catalyzes the reaction of acetylene and hydrogen chloride to generate vinyl chloride. However, the disadvantages of high toxicity and volatility of mercuric chloride have greatly polluted the environment and endangered human health. Therefore, the development of non-mercury catalysts is necessary for the sustainable development of vinyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J31/22B01J31/24C07C17/08C07C21/06B01J37/02B01J37/34
CPCB01J31/0295B01J31/0284B01J31/0279B01J31/0282B01J31/0288B01J31/182B01J31/1815B01J31/1805B01J31/24B01J31/183C07C17/08B01J37/342B01J37/0203B01J37/0207B01J37/0205B01J37/0209B01J2231/32B01J2531/16B01J2531/18B01J2531/821B01J2531/822C07C21/06Y02P20/54
Inventor 李小年赵佳卢春山姚楠张群峰赖慧霞王柏林邵淑娟朱文锐
Owner ZHEJIANG UNIV OF TECH
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