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Method for synthesis of vinyl acetate through hydroformylation of methyl acetate

A technology for the synthesis of vinyl acetate and methyl acetate by hydroformylation, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., and can solve the problems of low selectivity and low yield of vinyl acetate. Achieve the effect of improving yield and selectivity, improving activity and stability

Active Publication Date: 2016-04-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is the problem of low vinyl acetate yield and low selectivity. A new method for the synthesis of vinyl acetate by hydroformylation of methyl acetate is provided. The method has the advantages of high vinyl acetate yield and low selectivity. high feature

Method used

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  • Method for synthesis of vinyl acetate through hydroformylation of methyl acetate
  • Method for synthesis of vinyl acetate through hydroformylation of methyl acetate
  • Method for synthesis of vinyl acetate through hydroformylation of methyl acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Preparation of carbonylation catalyst: CoCl containing 8.60gCo, 3.40gY and 3.10gSn 2 ·6H 2 O, Y (NO 3 ) 3 ·6H 2 O and SnCl 2 2H 2 O is fully mixed and dissolved in hydrochloric acid with a concentration of 8wt%, to obtain 400ml of impregnation solution, and the specific surface of 1.0L is 165m2 / g, spherical SiO with a pore volume of 0.95 and a diameter of 5.6mm 2 The carrier was immersed in the above impregnating solution, left to stand for 2 hours and dried at 100° C. to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Co content was 8.60 g / L, the Y content was 3.40 g / L, and the Sn content was 3.10 g / L.

[0030] Synthesis of vinyl acetate:

[0031] Step (1): Add 1.5 mol of acetic acid, 0.05 mol of carbonylation catalyst, 0.10 mol of methyl iodide and 0.45 mol of methyl acetate into a 500ml titanium reactor, first use argon to discharge the air in the reactor and pressurize to 2.0MPa, then Introduce carbon monoxide and hydrogen until...

Embodiment 2

[0036] Preparation of carbonylation catalyst: CoCl containing 8.60gCo, 3.40gY and 3.10gRb 2 ·6H 2 O, Y (NO 3 ) 3 ·6H 2 O and RbNO 3 Fully mix and dissolve in pure water to obtain 400ml of impregnation solution, and the specific surface of 1.0L is 165m 2 / g, spherical SiO with a pore volume of 0.95 and a diameter of 5.6mm 2 The carrier was immersed in the above impregnating solution, left to stand for 2 hours and dried at 100° C. to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Co content was 8.60 g / L, the Y content was 3.40 g / L, and the Rb content was 3.10 g / L.

[0037] Synthesis of vinyl acetate:

[0038] Step (1): Add 1.5 mol of acetic acid, 0.05 mol of carbonylation catalyst, 0.10 mol of methyl iodide and 0.45 mol of methyl acetate into a 500ml titanium reactor, first use argon to discharge the air in the reactor and pressurize to 2.0MPa, then Introduce carbon monoxide and hydrogen until the pressure is 7.2MPa, increase the stirring sp...

Embodiment 3

[0052] Preparation of carbonylation catalyst: NiCl containing 7.00gNi, 1.00gSc and 1.00gGe 2 ·6H 2 O, Sc(OAc) 3 ·6H 2 O and GeCl 4 Fully mixed and dissolved in hydrochloric acid with a concentration of 8wt%, to obtain 400ml of impregnation solution, and the specific surface of 1.0L was 150m 2 / g, spherical Al with a pore volume of 0.90 and a diameter of 5.6mm 2 o 3 The carrier was immersed in the above impregnating solution, left to stand for 2 hours and dried at 80° C. to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Ni content was 7.00 g / L, the Sc content was 1.00 g / L, and the Ge content was 1.00 g / L.

[0053] Synthesis of vinyl acetate:

[0054] Step (1): Add 1.5 mol of acetic acid, 0.05 mol of carbonylation catalyst, 0.10 mol of methyl iodide and 0.45 mol of methyl acetate into a 500ml titanium reactor, first use argon to discharge the air in the reactor and pressurize to 2.0MPa, then Introduce carbon monoxide and hydrogen until the p...

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Abstract

The invention relates to a method for synthesis of vinyl acetate through hydroformylation of methyl acetate. The method mainly solves the problem that the existing vinyl acetate preparation method utilizing methyl acetate carbonylation and carboxide cracking has a low yield and low selectivity. The method provided through the invention comprises methyl acetate carbonylation for ethylidene diacetate preparation and ethylidene diacetate cracking for vinyl acetate preparation. A carbonylation catalyst utilizes SiO2, Al2O3 or their mixture as a carrier and active ingredients comprise at least one of iron group metal elements, at least one of IIIB elements and at least one of IVA and alkali metals. The method well solves the technical problem and can be used for vinyl acetate industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing vinyl acetate by hydroformylation of methyl acetate. Background technique [0002] Vinyl acetate (vinylacetate, VAC or VAM for short), is a colorless, transparent, flammable liquid at room temperature with a sweet ether fragrance. It is one of the most productive organic chemical raw materials in the world, widely used in the production of polyvinyl acetate (PVAc), polyvinyl alcohol, coatings, pastes, adhesives, vinylon, films, vinyl copolymer resins, acetal resins A series of chemical and chemical fiber products are widely used in various industries. [0003] The production of vinyl acetate adopts ethylene gas-phase method and acetylene gas-phase method both at home and abroad, which belong to the petrochemical process route. Since the rise of C1 chemistry, in the 1980s, the American Halcon (Halcon) company and the British Petroleum (BP) company successively A new process for the production of vinyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/15C07C67/297C07C67/36C07C69/16B01J31/28B01J23/835B01J23/83
Inventor 查晓钟杨运信
Owner CHINA PETROLEUM & CHEM CORP
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