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The preparation method of diethylene acetate

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: 2016-05-25
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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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  • The preparation method of diethylene acetate
  • The preparation method of diethylene acetate
  • The preparation method of diethylene acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Synthesis of ethylene diacetate: 2.5mol acetic acid, 0.02molPd(OAc) 2 , 0.1molCH 3 I. 0.063molN,N',N"-trihydroxyisocyanuric acid (formula II, THICA) and 0.62mol methyl acetate are added to the titanium reaction kettle, the air in the kettle is discharged with argon and the pressure is 2.0MPa. Then pass in carbon monoxide and hydrogen until the pressure is 7.5MPa, increase the stirring speed to 1200rpm, while stirring and heating to raise the temperature to the reaction temperature, control the reaction temperature to 178℃, the molar ratio of carbon monoxide to hydrogen is 33:17, continue the reaction for 7 hours, stop the reaction .

[0019] 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).

[0020] And calculate the yield and selectivity of synthetic ethylene diacetate according to the following formula:

[0021]

[0022]

[0023...

Embodiment 2

[0030] Synthesis of ethylene diacetate: 2.5mol acetic acid, 0.02molPd(OAc) 2 , 0.1molCH 3 I. 0.063molN,N'-dihydroxypyromellitic acid imide (formula V, NDHPI) and 0.62mol methyl acetate are added to the titanium reaction kettle, and the air in the kettle is first discharged with argon and then pressurized to 2.0MPa. Then pass in carbon monoxide and hydrogen until the pressure is 7.5MPa, increase the stirring speed to 1200rpm, while stirring and heating to raise the temperature to the reaction temperature, control the reaction temperature to 178℃, the molar ratio of carbon monoxide to hydrogen is 33:17, continue the reaction for 7 hours, stop the reaction .

[0031] 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).

[0032] The calculated conversion rate of methyl acetate is 70.82%, the yield of diethylene acetate is 60.09%, and the selec...

Embodiment 3

[0034] Synthesis of ethylene diacetate: 2.5mol acetic acid, 0.02molPd(OAc) 2 , 0.1molCH 3 I. 0.063molN-hydroxyphthalimide (formula III, NHPI) and 0.62mol methyl acetate are added to the titanium reaction kettle, the air in the kettle is first discharged with argon and then the pressure is increased to 2.0MPa, and then passed The pressure of carbon monoxide and hydrogen is 7.5 MPa, the stirring speed is increased to 1200 rpm, and the temperature is raised to the reaction temperature while stirring and heating. The reaction temperature is controlled to be 178° C. The molar ratio of carbon monoxide and hydrogen is 33:17. After the reaction continues for 7 hours, the reaction is stopped.

[0035] Product analysis: The reaction mixture obtained from the above reaction is cooled, decompressed, and separated, and the liquid phase is analyzed by gas chromatography-mass spectrometry (GC-MASS).

[0036] The calculated conversion rate of methyl acetate is 70.54%, the yield of diethylene acetat...

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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 (vinylacetate), is widely used in organic synthesis, mainly for the synthesis of vinylon, as well as chemical reagents in the adhesive and coating industries. [0003] The production of vinyl acetate at home and abroad adopts the ethylene process and the acetylene process, which belong to the petrochemical process route. Since the rise of C1 chemistry, in the 1980s, the United States Halcon (Halcon) and British Petroleum (BP) successively proposed A new process for preparing vinyl acetate from methanol and syngas. The process does not rely on petrochemical raw materials, but through the carbonylation reaction of methyl acetate and synthesis gas to synthesize the intermediate ethylene diacetate (EDDA), and then undergo thermal cracking to produce vinyl acetate and acetic acid. [0004] The prep...

Claims

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Application Information

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Patent Type & Authority Patents(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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