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Synthesis method of ethylidene diacetate from methyl acetate

A technology of diethylene acetate and its synthesis method, which is applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of low selectivity of diacetate and low conversion rate of methyl acetate, etc., and achieve The effect of increasing the conversion rate

Active Publication Date: 2015-03-25
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0004] The invention relates to a synthesis method of diethylene acetate, which mainly solves the problem of using sulfur-containing sulfones or sulfoxides as solvents in the prior art, and the carbonylation of methyl acetate into diethylene acetate, which has a low conversion rate of methyl acetate. , The selectivity of diethylene acetate is not high

Method used

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  • Synthesis method of ethylidene diacetate from methyl acetate
  • Synthesis method of ethylidene diacetate from methyl acetate

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Experimental program
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Effect test

Embodiment 1

[0013] Synthesis of diethylene acetate: 2.20mol SOCl 2 , 0.003molRhCl 3 .3H 2 O, 0.18molCH 3 1, 0.018mol tributylphosphine and 1.20mol MeOAc add in the 2 liters of titanium reactors that have replaced the air wherein with argon in advance, pass into carbon monoxide and hydrogen then, make solvent: MeOAc:CO:H 2 =1:0.55:0.55:0.28, after reacting at 165° C. for 8 hours under stirring, stop the reaction.

[0014] Product analysis: The reaction mixture obtained from the above reaction was cooled, decompressed, and separated, and the liquid phase was analyzed by chromatography and nuclear magnetic resonance (GLC / NMR).

[0015] The transformation rate of methyl acetate reaches 93.86% through calculation, and the selectivity of diacetate ethylene is 94.31%. The yields and selectivities of ethyl esters are listed in Table 1.

Embodiment 2

[0037] 2.20mol SOCl 2 , 0.003molRhCl 3 .3H 2 O, 0.10molCH 3 1, 0.018mol triphenylphosphine and 1.20mol MeOAc add in the 2 liters of titanium reactors that have replaced the air wherein with argon in advance, pass into carbon monoxide and hydrogen then, make solvent: MeOAc:CO:H 2 =1:0.55:0.55:0.28, after reacting at 165° C. for 8 hours under stirring, stop the reaction.

[0038] Reaction conditions, each material feed amount, product after analysis and calculation, the conversion rate of methyl acetate and the selectivity and yield of diacetate are listed in Table 1.

Embodiment 3

[0040] 2.20mol SOCl 2 , 0.006molRhCl 3 .3H 2 O, 0.20molCH 3 1, 0.018mol triphenylphosphine and 1.20mol MeOAc add in the 2 liters of titanium reactors that have replaced the air wherein with argon in advance, pass into carbon monoxide and hydrogen then, make solvent: MeOAc:CO:H 2 =1:0.55:0.55:0.28, after reacting at 165° C. for 3 hours under stirring, stop the reaction.

[0041] Reaction conditions, each material feed amount, product after analysis and calculation, the conversion rate of methyl acetate and the selectivity and yield of diacetate are listed in Table 1.

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Abstract

The invention relates to a synthesis method of ethylidene diacetate from methyl acetate, which mainly solves the problems of low conversion rate of methyl acetate and low selectivity of ethylidene diacetate in the prior art. MeOAc, CO and H2 used as raw materials react in the presence of a catalyst by mainly using SOCl2 or SOCl2-sulfolane mixture as a solvent to generate the ethylidene diacetate. The catalyst comprises a main catalyst, a cocatalyst and an accelerator, wherein the main catalyst adopts VIII metals or compounds thereof, the cocatalyst is a halogen-containing compound, and the accelerator is a nitrogen oxygen organic matter or phosphorus-containing compound. The technical scheme well solves the problems, and can be used for producing vinyl acetate.

Description

technical field [0001] The invention relates to a synthetic method for synthesizing diethylene acetate from methyl 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 routes for producing vinyl acetate include acetylene method and ethylene method. 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, Halcon (Halcon, USA) ) 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 diethyle...

Claims

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Application Information

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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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