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A kind of organic amine catalyst for synthesizing vinylidene chloride and preparation method thereof

A technology of vinylidene chloride and organic amines, applied in the direction of organic compound/hydride/coordination complex catalysts, dehydrohalogenation preparation, chemical instruments and methods, etc., can solve the problem of low reaction conversion rate and reactivity, reaction conversion The problem of low efficiency and VDC selectivity, to achieve the effect of high catalytic performance

Inactive Publication Date: 2015-10-21
ZHEJIANG NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] (2) Reaction conversion rate and reactivity are low: in the document of gas-phase method catalytic cracking TCE synthesis VDC of public report at present, reaction conversion rate and VDC selectivity are all low, as: Mochida etc. (JP05132436,1993; Chem.Lett. , 1992,21:461-464) using 20% ​​cesium nitrate loaded on silica gel as a catalyst, the TCE conversion rate was only 6%, and the VDC selectivity was 50%;
The pulse reaction is only a qualitative investigation of the catalyst effect, and there is a huge gap from the continuous reaction of industrialization

Method used

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  • A kind of organic amine catalyst for synthesizing vinylidene chloride and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0024] (1) According to the proportion that polyethyleneimine accounts for 30% of the mass percentage of ethanol, polyethyleneimine is dissolved in ethanol, stirred and dissolved, and a uniform mixed solution is obtained;

[0025] (2) According to the proportion that polyethyleneimine accounts for 40% of the mass percentage of the carrier, in the uniform mixed solution obtained in the above (1), add activated carbon as a carrier, immerse for 1.5h and then ultrasonically for 0.5h to obtain a particle suspension;

[0026] (3) Stir and reflux the particle suspension obtained in the above (2) at 80° C. for 2 h, and then take a water bath until all the ethanol volatilizes to obtain a solid-supported organic amine catalyst.

[0027] (4) The solid-supported organic amine catalyst obtained in the above (3) is placed in a fixed-bed reactor to carry out the reaction of gas phase cracking of 1,1,2-trichloroethane to synthesize vinylidene chloride. And under 100 DEG C of temperature, the ...

Embodiment 2

[0029] (1) According to the ratio that polyethyleneimine accounts for 50% of the mass percentage of ethanol, polyethyleneimine is dissolved in ethanol, stirred and dissolved to obtain a uniform mixed solution;

[0030] (2) According to the proportion that polyethyleneimine accounts for 70% of the mass percentage of the carrier, in the uniformly mixed solution obtained in the above (1), add activated carbon as a carrier, immerse for 1.5h and then ultrasonicate for 0.5h to obtain a particle suspension;

[0031] (3) Stir and reflux the particle suspension obtained in the above (2) at 80° C. for 2 h, and then take a water bath until all the ethanol volatilizes to obtain a solid-supported organic amine catalyst.

[0032] (4) The solid-supported organic amine catalyst obtained in the above (3) is placed in a fixed-bed reactor to carry out the reaction of gas phase cracking of 1,1,2-trichloroethane to synthesize vinylidene chloride. And under 100 DEG C of temperature, the vinylidene ...

Embodiment 3

[0034] (1) According to the ratio that polyethyleneimine accounts for 30% of the mass percentage of isopropanol, polyethyleneimine is dissolved in isopropanol, stirred and dissolved to obtain a uniform mixed solution;

[0035] (2) According to the proportion that polyethyleneimine accounts for 15% of the mass percentage of the carrier, in the uniform mixed solution obtained in the above (1), add silicon oxide as a carrier, immerse for 1.5h and then ultrasonicate for 0.5h to obtain a particle suspension ;

[0036] (3) Stir and reflux the particle suspension obtained in the above (2) at 80° C. for 2 h, and then take a water bath until the isopropanol is completely volatilized to obtain a solid-supported organic amine catalyst.

[0037] (4) The solid-supported organic amine catalyst obtained in the above (3) is placed in a fixed-bed reactor to carry out the reaction of gas phase cracking of 1,1,2-trichloroethane to synthesize vinylidene chloride. And under 120 ℃ of temperature, ...

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Abstract

The invention discloses an organic amine catalyst for synthesizing vinylidene chloride and a preparation method of the catalyst. The catalyst is composed of a carrier and an active ingredient, wherein the carrier is one of active carbon, silicon oxide and a silicon-aluminum molecular sieve; the active ingredient is chain fatty amine type organic amine; and the chain fatty amine type organic amine accounts for 5%-80% by mass of the carrier, and the organic amine is immobilized on the carrier by virtue of a soaking method. The preparation method of the catalyst comprises the following steps of: dissolving a certain amount of chain fatty amine type organic amine in organic solvent; adding a certain amount of carrier after stirring and dissolving; soaking for 1.5 hours and ultrasonic treating for 0.5 hour to obtain granule suspension liquid; and stirring and refluxing the granule suspension liquid for 2 hours at 80 DEG C, and carrying out water bath until the organic solvent is completely volatilized to obtain the solid carrier type organic amine catalyst. The organic amine catalyst has very high catalytic performances and can be reacted under gentle conditions. Moreover, the product yield reaches 90% or higher.

Description

technical field [0001] The invention relates to a chemical catalyst and an application method thereof, in particular to an organic amine catalyst for synthesizing vinylidene chloride and a preparation method thereof. Background technique [0002] Vinylidene chloride (VDC) polymer (PVDC resin) has the properties of moisture resistance, oxygen resistance, moisture resistance, acid and alkali resistance, oil immersion resistance and resistance to various chemical solvents, and is widely used in the packaging of food, medicine and military products. Without adding any preservatives, PVDC resin has long-term freshness preservation performance than other packaging materials. With the improvement of people's living standards and the emphasis on food safety issues, my country's demand for food packaging materials made of PVDC resin is increasing. Therefore, the market prospect of vinylidene chloride is huge. [0003] However, whether it is international or domestic industrial produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J31/26C07C21/08C07C17/25
Inventor 谢冠群王树华张文革李小年罗孟飞胡庚申冯星星
Owner ZHEJIANG NORMAL UNIVERSITY