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Method for preparing vinylacetylene through acetylene dimerization by utilizing modified nieuwland catalyst

A vinyl acetylene and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as low single-pass conversion rate, reduced catalyst service life, low selectivity of vinyl acetylene, etc., to achieve The catalyst is easy to prepare, the amount of polymer produced is small, and the catalyst cost is low

Inactive Publication Date: 2013-12-25
SHIHEZI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there are still many problems in the acetylene process, such as: (1) the conversion rate per pass is low
(2) Low selectivity of vinyl acetylene
(3) Some tar-like polymers will be generated during the reaction, which greatly reduces the selectivity of vinyl acetylene and reduces the service life of the catalyst
[0003] Obviously, the existing method of acetylene dimerization into vinyl acetylene has problems such as low conversion rate of acetylene per pass and low selectivity of vinyl acetylene; it is necessary to vigorously develop new catalytic systems to solve the above existing problems

Method used

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  • Method for preparing vinylacetylene through acetylene dimerization by utilizing modified nieuwland catalyst
  • Method for preparing vinylacetylene through acetylene dimerization by utilizing modified nieuwland catalyst

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0020] (1) Add 15mL of water into the reactor, then add 0.1049mol of ammonium chloride, at 80°C, under nitrogen for 110h -1 ~155h -1 Stir with air to dissolve it all.

[0021] (2) Keep the reaction temperature at 80°C, add 0.1049mol of cuprous chloride and 0.1mL of 37%-38% concentrated hydrochloric acid to the catalyst, and then continue to feed into the reactor for 110h -1 ~155h -1 Nitrogen for 30 minutes to fully dissolve the cuprous chloride and activate the catalytic system.

[0022] (3) use 206h -1 Acetylene is used instead of nitrogen, and the reaction temperature is maintained at 80°C. Acetylene undergoes dimerization to form vinyl acetylene.

[0023] (4) The gas at the reactor outlet was detected online by Shimadzu GC2014-C gas chromatography, FID detector, and GDX-301 packed column.

specific Embodiment 2

[0024] (1) Add 15mL of water into the reactor, then add 0.1496mol of ammonium chloride, at 80°C, under nitrogen for 110h -1 ~155h -1 Stir with air to dissolve it all.

[0025] (2) Keep the temperature at 80°C, add 0.01496mol strontium dichloride to the ammonium chloride aqueous solution, and keep the nitrogen gas for 110h -1 ~155h -1 Stir with air to dissolve.

[0026] (3) Keeping the reaction temperature at 80°C, add 0.1496mol of cuprous chloride and 0.1mL of 37%-38% concentrated hydrochloric acid to the catalyst, and then continue to feed into the reactor for 110h -1 ~155h -1 Nitrogen for 30 minutes to fully dissolve the cuprous chloride and activate the catalytic system.

[0027] (4) use 206h -1 Acetylene is used instead of nitrogen, and the reaction temperature is maintained at 80°C. Acetylene undergoes dimerization to form vinyl acetylene.

[0028] (5) The gas at the reactor outlet was detected online by Shimadzu GC2014-C gas chromatography, FID detector, and GDX-3...

specific Embodiment 3

[0029] (1) Add 15mL of water into the reactor, then add 0.1144mol of ammonium chloride, at 80°C, under nitrogen for 110h -1 ~155h -1 Stir with air to dissolve it all.

[0030] (2) Keep the temperature at 80°C, add 0.01144mol strontium dichloride to the ammonium chloride aqueous solution, and keep the nitrogen gas for 110h -1 ~155h -1 Stir with air to dissolve.

[0031] (3) Keep the reaction temperature at 80°C, add 0.1144mol of cuprous chloride and 0.1mL of 37%-38% concentrated hydrochloric acid to the catalyst, and then continue to feed into the reactor for 110h -1 ~155h -1 Nitrogen for 30 minutes to fully dissolve the cuprous chloride and activate the catalytic system.

[0032] (4) use 206h -1 Acetylene is used instead of nitrogen, and the reaction temperature is maintained at 80°C. Acetylene undergoes dimerization to form vinyl acetylene.

[0033] (5) The gas at the reactor outlet was detected online by Shimadzu GC2014-C gas chromatography, FID detector, and GDX-301 ...

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Abstract

The invention relates to a method for preparing vinylacetylene through acetylene dimerization by utilizing a strontium chloride modified nieuwland catalyst and an application method. The method is characterized in that a strontium chloride hexahydrate is used as a cocatalyst, cuprous chloride is used as a main catalyst, ammonium chloride is used as a cosolvent, an acid environment is provided by hydrochloric acid, and water is used as a solvent to prepare a copper-strontium-inorganic chloride salt complex to serve as the catalyst. Under the condition, the generation of high polymers in the acetylene dimerization reaction is obviously reduced and the selectivity of vinylacetylene is significantly improved.

Description

technical field [0001] The invention relates to a preparation method and application of a low-carbon alkyne greening catalyst, in particular to a modification method and application of a vinyl acetylene catalyst prepared by acetylene dimerization in a water system. Background technique [0002] In view of the characteristics of my country's rich coal, poor oil and little gas, vigorously developing energy and chemical products that use coal as the source is an inevitable trend in the future development of the energy field. With the direct production of low-carbon alkynes from coal (C 2 ~C 4 ) technology continues to mature, alkyne chemical technology using low-carbon alkynes as raw materials will become an important development direction in the post-petrochemical era. As the "mother of organic synthesis industry", acetylene has a wider range of sources. Vinyl acetylene, as a downstream product of acetylene, is an important fine chemical intermediate. It is produced by dime...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C11/30C07C2/38B01J27/24
Inventor 代斌卢俊龙谢建伟刘平王绪根刘志勇刘海月
Owner SHIHEZI UNIVERSITY
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