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Preparation method of ethylidene diacetate

A technology of ethylene diacetate and acetic acid is applied in the field of preparation of synthesizing ethylene diacetate from methyl acetate, and can solve the problem of low yield of ethylene diacetate, low selectivity, low conversion rate of methyl acetate, etc. problem, to achieve the effect of improving conversion rate and improving activity and stability

Active Publication Date: 2015-03-25
CHINA PETROLEUM & CHEM CORP +1
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AI Technical Summary

Problems solved by technology

[0005] The invention relates to a preparation method for synthesizing diethylene acetate from methyl acetate, which mainly solves the problems of low conversion rate of methyl acetate and low yield and low selectivity of diacetate in the prior art using pyridine as an accelerator question

Method used

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  • Preparation method of ethylidene diacetate
  • Preparation method of ethylidene diacetate
  • Preparation method of ethylidene diacetate

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Synthesis of diethylene acetate: 2.5mol acetic acid, 0.02molPd(OAc) 2 , 0.1molCH 3 I. Add 0.063mol N, N', N"-trihydroxyisocyanuric acid (formula II, THICA) and 0.62mol methyl acetate into the titanium reactor, first use argon to discharge the air in the reactor and then pressurize to 2.0MPa, Then feed carbon monoxide and hydrogen until the pressure is 7.5 MPa, increase the stirring speed to 1200rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 178°C, the molar ratio of carbon monoxide to hydrogen is 33:17, continue the reaction for 7 hours, stop the reaction .

[0020] Product analysis: The reaction mixture obtained from the above reaction was cooled, decompressed, and separated, and the liquid phase was analyzed by gas chromatography-mass spectrometry (GC-MASS).

[0021] And calculate the yield and the selectivity of synthesizing ethylene diacetate by following formula:

[0022]

[0023]

[0024] The conversion ra...

Embodiment 2

[0031] Synthesis of diethylene acetate: 2.5mol acetic acid, 0.02molPd(OAc) 2 , 0.1molCH 3 I. Add 0.063mol N, N'-dihydroxypyromellitic acid imide (formula V, NDHPI) and 0.62mol methyl acetate into the titanium reactor, first use argon to discharge the air in the reactor and then pressurize to 2.0MPa , then feed carbon monoxide and hydrogen until the pressure is 7.5 MPa, increase the stirring speed to 1200rpm, at the same time stir and heat up to the reaction temperature, control the reaction temperature to 178°C, the molar ratio of carbon monoxide and hydrogen is 33:17, continue the reaction for 7h, stop reaction.

[0032] Product analysis: The reaction mixture obtained from the above reaction was cooled, decompressed, and separated, and the liquid phase was analyzed by gas chromatography-mass spectrometry (GC-MASS).

[0033] The conversion rate of methyl acetate was calculated to be 70.82%, the yield of ethylene diacetate was 60.09%, and the selectivity was 84.85%. For ease...

Embodiment 3

[0035] Synthesis of diethylene acetate: 2.5mol acetic acid, 0.02molPd(OAc) 2 , 0.1molCH 3 I. Add 0.063mol N-hydroxyphthalimide (Formula III, NHPI) and 0.62mol methyl acetate into the titanium reactor, first use argon to discharge the air in the kettle, then pressurize to 2.0MPa, and then pass Add carbon monoxide and hydrogen until the pressure is 7.5 MPa, increase the stirring speed to 1200rpm, stir and heat to the reaction temperature at the same time, control the reaction temperature to 178°C, the molar ratio of carbon monoxide to hydrogen is 33:17, continue the reaction for 7 hours, then stop the reaction.

[0036] Product analysis: The reaction mixture obtained from the above reaction was cooled, decompressed, and separated, and the liquid phase was analyzed by gas chromatography-mass spectrometry (GC-MASS).

[0037] The conversion rate of methyl acetate was calculated to be 70.54%, the yield of ethylene diacetate was 60.07%, and the selectivity was 85.16%. For ease of d...

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Abstract

The invention relates to a preparation method of ethylidene diacetate, which is mainly used for solving the problems that in the prior art, conversion rate of methyl acetate using pyridine as a promoter is low, yield of ethylidene diacetate is low and selectivity is low. The method is used for synthesizing the ethylidene diacetate with methyl acetate, carbon monoxide and hydrogen as raw materials and acetic acid as a solvent at a reaction temperature of 130-200 DEG C, a reaction pressure of 2-10 MPa and a reaction time of 3-10 hours, the main catalyst is selected from platinum group metals or compounds thereof, the auxiliary catalyst is an iodide, an oxynitride selected from the general formula (I) is used as the promoter, the technical scheme is used for well solving the problem, and the preparation method can be used in the production of vinyl acetate. The formula is described in the specification.

Description

technical field [0001] The invention relates to a preparation method for synthesizing diethylene acetate from methyl acetate. Background technique [0002] Vinyl acetate, namely vinyl acetate, is widely used in organic synthesis, mainly for the synthesis of vinylon, and also for chemical reagents in the adhesive and coating industries. [0003] The production of vinyl acetate adopts ethylene method and acetylene method at home and abroad, which belongs to the petrochemical process route. Since the rise of C1 chemistry, in the 1980s, American Halcon and British Petroleum (BP) successively proposed the A new process for the production of vinyl acetate from methanol and synthesis gas. The process does not rely on petrochemical raw materials, but through the carbonylation reaction of methyl acetate and synthesis gas to synthesize the intermediate diethylene acetate (EDDA), and then produce vinyl acetate and acetic acid through thermal cracking. [0004] The preparation method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/16C07C67/36
CPCC07C67/36C07C69/16
Inventor 查晓钟杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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