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Ethylidene diacetate catalyst and preparation method thereof

A technology of ethylene diacetate and catalyst, applied in chemical instruments and methods, catalysts for physical/chemical processes, carbon monoxide or formate reaction preparation, etc., can solve the problem of low yield and low selectivity of ethylene diacetate , the problem of high selectivity of ethylene diacetate, to achieve the effect of improving activity and stability, improving yield and selectivity

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the technical problems to be solved by this invention is the problem of low yield and low selectivity of diacetate, and a new catalyst for the synthesis of diacetate is provided, which has diacetate The characteristics of high yield and high selectivity to diethylene acetate

Method used

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  • Ethylidene diacetate catalyst and preparation method thereof
  • Ethylidene diacetate catalyst and preparation method thereof
  • Ethylidene diacetate catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of catalyst: Pd(OAc) containing 5.12gPd, containing 2.56gCe and containing 1.39gSb 2 、Ce(OAc) 3 ·5H 2 O and antimony trioxide are fully mixed and dissolved in dilute nitric acid to obtain 500ml of impregnation solution, and 1.0L of spherical SiO with a diameter of 5.6mm 2 The carrier was immersed in the above impregnating solution, and dried at 100°C for 2 hours. 2 The catalyst was obtained by raising the temperature to 500° C. and calcining for 4 h in the atmosphere.

[0024] Synthesis of diethylene acetate: Add 1.5mol acetic acid, 0.05mol catalyst and 0.45mol methyl acetate into a 1.5L titanium reactor, first use argon to exhaust the air in the kettle, then pressurize to 2.0MPa, and then introduce carbon monoxide And hydrogen until the pressure is 8.0MPa, increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 186°C, the molar ratio of carbon monoxide to hydrogen is 2:1, conti...

Embodiment 2

[0047] Preparation of catalyst: PdCl containing 3.05gPd, 1.05gCe and 0.60gSb 2 , Ce(NO 3 ) 3 ·6H 2 O and Cl 5 Sb was fully mixed and dissolved in dilute hydrochloric acid to obtain 500ml of impregnating solution. Immerse 1.0L of activated carbon carrier in the above impregnating solution, let it stand for 2 hours, dry at 80°C, and heat up to 400°C for 4 hours in a He atmosphere to obtain the catalyst.

[0048] Synthesis of diethylene acetate: Add 1.5mol acetic acid, 0.05mol catalyst and 0.45mol methyl acetate into a 1.5L titanium reactor, first use argon to discharge the air in the kettle, then pressurize to 1.0MPa, and then introduce carbon monoxide And hydrogen until the pressure is 2.0MPa, increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 130°C, the molar ratio of carbon monoxide to hydrogen is 1:10, continue the reaction for 3.0h, then stop the reaction.

[0049] Product analysis: The re...

Embodiment 3

[0052] Preparation of catalyst: Pd(NO 3 ) 2 2H 2 O, Ce 2 o 3 and Sb 2 (SO 4 ) 3 Fully mixed and dissolved in dilute nitric acid to obtain 500ml of impregnation solution, 1.0L Al 2 o 3 The carrier was immersed in the impregnating solution, left to stand for 2 hours, dried at 120° C., and then calcined at 600° C. for 4 hours in an Ar atmosphere to obtain the catalyst.

[0053] Synthesis of diethylene acetate: Add 1.5mol acetic acid, 0.05mol catalyst and 0.45mol methyl acetate into a 1.5L titanium reactor, first use argon to exhaust the air in the kettle, then pressurize to 2.0MPa, and then introduce carbon monoxide And hydrogen until the pressure is 10..0MPa, increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 200°C, the molar ratio of carbon monoxide to hydrogen is 10:1, continue the reaction for 10.0h, stop the reaction.

[0054] Product analysis: The reaction mixture obtained from the ab...

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Abstract

The invention relates to a catalyst for synthesizing ethylidene diacetate with methyl acetate and a preparation method of the catalyst, which are mainly used for solving the problems of low activity and poor selectivity of an ethylidene diacetate catalyst in the prior part. The technical problems are well solved through the adoption of the technical scheme that the ethylidene diacetate catalyst comprises a carrier, 3.0-15.0 g / L of palladium, 1.0-5.0 g / L of cerium and 0.5-5.0 g / L of stibium, wherein palladium, cerium and stibium are loaded on the carrier, and the carrier is at least one of activated carbon, silicon oxide, aluminum oxide and silicon carbide. The catalyst can be used in industrial production of vinyl acetate.

Description

technical field [0001] The invention relates to a catalyst for synthesizing diethylene acetate, a preparation method and a synthesis method of diethylene acetate. Background technique [0002] Vinyl acetate, namely vinyl acetate (VAC or VAM for short), is a colorless, transparent, flammable liquid at room temperature with a sweet ether fragrance. It is one of the most productive organic chemical raw materials in the world, widely used in the production of polyvinyl acetate (PVAc), polyvinyl alcohol, coatings, pastes, adhesives, vinylon, films, vinyl copolymer resins, acetal resins A series of chemical and chemical fiber products are widely used in various industries. [0003] The production of vinyl acetate adopts ethylene gas phase method and acetylene gas phase method at home and abroad, which belong to the petrochemical process route. Since the rise of C1 chemistry, in the 1980s, American Halcon (Halcon) company and British Petroleum (BP) company successively A new proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/644B01J27/228C07C69/16C07C67/36
Inventor 查晓钟杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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