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Synthetic method of ethylidene diacetate

A technique for the synthesis of diethylene acetate, applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, organic compound/hydride/coordination complex catalyst, etc., can solve the problem of low conversion rate of methyl acetate , low selectivity, low yield of diethylene acetate, etc., to improve activity and stability, increase conversion rate, and reduce loss

Active Publication Date: 2015-05-13
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention relates to a synthetic method of diethylene acetate, which mainly solves the problem of using organic nitrogen or organic phosphorus as a promoter in the prior art, and the carbonylation of methyl acetate to synthesize diethylene acetate in the reaction of methyl acetate is low. , low yield and low selectivity of diacetate

Method used

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  • Synthetic method of ethylidene diacetate
  • Synthetic method of ethylidene diacetate
  • Synthetic method of ethylidene diacetate

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Synthesis of diethylene acetate: 1.8mol acetic acid, 0.07mol Co 2 (CO) 8 , 0.20molCH 3 1, 0.04mol18-crown (ether)-6 and 0.54mol methyl acetate are added in the titanium material reaction kettle, first discharge the air in the kettle with argon and pressurize to 2.0MPa, then feed carbon monoxide and hydrogen until the pressure is 8.7MPa, Increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 183°C, the molar ratio of carbon monoxide and hydrogen to 2:1, continue the reaction for 8.5h, then stop the reaction.

[0017] Product analysis: the reaction mixture obtained by the above reaction is cooled, decompressed, separated, and the liquid phase is analyzed by gas chromatography-mass spectrometry (GC-MASS) to obtain 4.07% ethylene diacetate, 0.72% acetic anhydride, acetaldehyde 0.27%, 85.88% acetic acid.

[0018] The calculated yield of ethylene diacetate is 58.68%, and the selectivity is 85.88%....

Embodiment 2

[0028] 1.8mol acetic acid, 0.015mol Co 2 (CO) 8 , 0.25molCH 3 1, 0.05mol15-crown (ether)-5 and 0.54mol methyl acetate are added in the titanium material reaction kettle, first use argon gas to discharge the air in the kettle and pressurize to 2.0MPa, then feed carbon monoxide and hydrogen until the pressure is 8.7MPa, Increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 183°C, the molar ratio of carbon monoxide and hydrogen to 2:1, continue the reaction for 8.5h, then stop the reaction.

[0029] Product is through analysis and calculation, and for convenience of illustration and comparison, the yield and the selectivity of reaction condition, each material feed amount, and diacetate are listed in table 1 and table 2 respectively.

Embodiment 3

[0031] 2.1mol acetic acid, 0.10mol Co 2 (CO) 8 , 0.23molCH 3 1, 0.046mol15-crown (ether)-5 and 0.63mol methyl acetate are added in the titanium material reaction kettle, first discharge the air in the kettle with argon and pressurize to 2.0MPa, then feed carbon monoxide and hydrogen until the pressure is 8.7MPa, Increase the stirring speed to 1500rpm, while stirring and heating to the reaction temperature, control the reaction temperature to 183°C, the molar ratio of carbon monoxide and hydrogen to 2:1, continue the reaction for 8.5h, then stop the reaction.

[0032] Product is through analysis and calculation, and for convenience of illustration and comparison, the yield and the selectivity of reaction condition, each material feed amount, and diacetate are listed in table 1 and table 2 respectively.

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Abstract

The invention relates to a synthesis method for the carbonylation of methyl acetate to synthesize ethylene diacetate. It mainly solves the problem of using organic nitrogen or organic phosphorus as a promoter in the prior art to react methyl acetate through the carbonylation of methyl acetate to synthesize ethylene diacetate. The problems include low ester conversion rate, low yield of ethylene diacetate and low selectivity. This method uses methyl acetate, carbon monoxide and hydrogen as raw materials, and the solvent is acetic acid. The reaction temperature is 130~200°C, the reaction pressure is 2~10MPa, and the reaction time is 3~10h. The main method is to synthesize ethylene diacetate. The technical solution of using iron-based metals or their compounds as the catalyst, iodide as the cocatalyst and crown ether as the accelerator solves this problem well and can be used in the production of vinyl acetate.

Description

technical field [0001] The present invention relates to the synthetic method of diethylene acetate. Background technique [0002] Vinyl acetate, namely vinyl acetate, is an important organic chemical raw material, a monomer for the manufacture of polyvinyl alcohol, and an important raw material for the manufacture of coatings, adhesives, and paints. The route of manufacturing vinyl acetate has acetylene method and ethylene method, and the production of vinyl acetate adopts ethylene method and acetylene method technology both at home and abroad, belongs to petrochemical process route, since the rise of C1 chemistry, in the 1980s, the United States Halcon (Halcon ) Company and British Petroleum (BP) Company successively proposed a new process for preparing 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 a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/36C07C69/16B01J31/02B01J31/20
CPCC07C67/36B01J31/0204B01J31/0231B01J31/20B01J2531/847B01J2531/845B01J2531/007B01J35/393C07C69/16
Inventor 查晓钟杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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