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Catalyst used in synthesis of ethylidene diacetate

A technology of ethylene diacetate and catalyst, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, organic chemistry, etc., can solve the problem of low yield of ethylene diacetate, diacetic acid The problems of high selectivity and low selectivity of ethylene ester can achieve the effect of improving yield and selectivity, improving activity and stability

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

AI Technical Summary

Problems solved by technology

[0006] 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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  • Catalyst used in synthesis of ethylidene diacetate

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Embodiment 1

[0027] Synthesis of diethylene acetate: 1.5mol acetic acid, 0.06mol RhCl 8 , 0.15molCH 3 I, 0.045mol structure (II) imidazole type NHC (its synthesis method is according to literature Arduengo A J, Harlow R L, Kline M.J. Am.Chem.Soc., 1991,113:361-363) and 0.45mol methyl acetate add 1.5L titanium In the material reactor, in which, in molar ratio, RhCl 8 :CH 3 I: Accelerator is 1:2.5:0.75 (where iodide is calculated as I atom). First use argon to exhaust the air in the kettle, then pressurize to 2.0MPa, then introduce carbon monoxide and hydrogen until the pressure is 7.5MPa, increase the stirring speed to 1500rpm, and at the same time stir and heat up to the reaction temperature, control the reaction temperature to 184 ° C, carbon monoxide and hydrogen The molar ratio was 2:1, and the reaction was stopped after 6.5 hours of continuous reaction.

[0028] Product analysis: The reaction mixture obtained from the above reaction was cooled, decompressed, and separated, and the ...

Embodiment 2

[0036] Synthesis of diethylene acetate: 1.5mol acetic acid, 0.06mol RhCl 8, 0.15molLiI, 0.045mol structure (III) imidazoline-type NHC (its synthesis method is based on the literature Arduengo A J, Harlow R L, Kline M.J. Am.Chem.Soc., 1991,113: 361-363) and 0.45mol methyl acetate were added In a 1.5L titanium reactor, RhCl is in molar ratio 8 : LiI: Accelerator is 1:2.5:0.75 (where iodide is calculated as I atom). First use argon to exhaust the air in the kettle, then pressurize to 2.0MPa, then introduce carbon monoxide and hydrogen until the pressure is 7.5MPa, increase the stirring speed to 1500rpm, and at the same time stir and heat up to the reaction temperature, control the reaction temperature to 184 ° C, carbon monoxide and hydrogen The molar ratio was 2:1, and the reaction was stopped after 6.5 hours of continuous reaction.

[0037] Product analysis: The reaction mixture obtained from the above reaction was cooled, decompressed, and separated, and the liquid phase was...

Embodiment 3

[0040] The synthesis of diethylene acetate: 1.5mol acetic acid, 0.06mol RhCl8, 0.15molHI, 0.045mol structure (IV) triazole type NHC (its synthetic method is according to literature Arduengo A J, Harlow R L, Kline M.J. Am.Chem.Soc. , 1991,113: 361-363) and 0.45mol methyl acetate were added to a 1.5L titanium reactor, wherein in molar ratio, RhCl 8 : HI: Accelerator is 1:2.5:0.75 (where iodide is calculated as I atom). First use argon to exhaust the air in the kettle, then pressurize to 2.0MPa, then introduce carbon monoxide and hydrogen until the pressure is 7.5MPa, increase the stirring speed to 1500rpm, and at the same time stir and heat up to the reaction temperature, control the reaction temperature to 184 ° C, carbon monoxide and hydrogen The molar ratio was 2:1, and the reaction was stopped after 6.5 hours of continuous reaction.

[0041] Product analysis: The reaction mixture obtained from the above reaction was cooled, decompressed, and separated, and the liquid phase ...

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Abstract

The invention relates to a catalyst used in the synthesis of ethylidene diacetate and a synthesis method of the ethylidene diacetate, and mainly aims at solving the problems that the yield of the ethylidene diacetate is low and the selectivity is low in the prior art. The catalyst used in the synthesis of the ethylidene diacetate comprises a main catalyst, a catalyst promoter and an accelerator, wherein the main catalyst is Rh metal or a compound of the Rh metal; the catalyst promoter is an iodine compound; and the accelerator is N-heterocyclic carbine and derivatives of the N-heterocyclic carbine. By adopting the technical scheme, the problems are relatively well solved, and the catalyst used in the synthesis of the ethylidene diacetate can be applied to the production of the ethylidene diacetate.

Description

technical field [0001] The invention relates to a catalyst for synthesizing diethylene acetate and a synthesis method for 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. Vinyl acetate is widely used in organic synthesis, mainly in textiles, machinery, construction, automobiles, light industry, agriculture and other fields. [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 process for the production of vinyl acetate from methanol and synthesis gas - carbonyl synthesis of vinyl acetate was proposed. The process does not rely on petrochemical raw materials, but through...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/30C07C69/16C07C67/36
Inventor 查晓钟杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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