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Preparation method for preparing ethylidene diacetate from methyl acetate

A technology of diethylene acetate and methyl acetate, applied in the direction of carbon monoxide or formate reaction preparation, chemical instruments and methods, organic compound/hydride/coordination complex catalyst, etc., can solve the problem of diacetate Solve the problems of low selectivity and low conversion rate of methyl acetate to achieve the effect of improving selectivity

Active Publication Date: 2015-03-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention relates to a preparation method for preparing diethylene acetate from methyl acetate, which mainly solves the problems of the low conversion rate of methyl acetate and the selection of diethylene acetate in the prior art by carbonylation of methyl acetate to diethylene acetate. low sex problem

Method used

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  • Preparation method for preparing ethylidene diacetate from methyl acetate
  • Preparation method for preparing ethylidene diacetate from methyl acetate
  • Preparation method for preparing ethylidene diacetate from methyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Preparation of core-shell carrier: will contain 4g SiO 2 200ml of acidified sodium silicate solution was evenly added dropwise in 5gAl 2 o 3 After 20 minutes, it was filtered, placed under ventilated conditions for 1 hour, dried at 110°C for 2 hours, and then calcined at 450°C for 4 hours to obtain a core-shell carrier (Y), in which the amorphous silica shell accounted for the weight of the carrier (Y) 44.4% of the total.

[0017] Modification of the carrier: 30g of 2-[methoxy(polyethyleneoxy)propyl]trimethoxysilane (CAS No.65994-07-2, English name 2-[Methoxy(polyethyleneoxy)propyl]- trimethoxy silane) in acetone solution, sprayed on the core-shell carrier (Y), stirred, filtered, washed and dried to obtain the modified core-shell carrier (X).

[0018] Preparation of supported catalyst: weigh 33g carrier X, 0.75gRhCl 3 .3H 2 O, 200mlH 2 O was mixed thoroughly, and then dried at 100 °C to obtain a supported catalyst RhCl containing 0.8% (weight percent) Rh 3 .3H ...

Embodiment 2

[0023] for 【Example 1】 comparative example.

[0024] Preparation of core-shell carrier: will contain 4g SiO 2 200ml of acidified sodium silicate solution was evenly added dropwise in 5gAl 2 o 3 After 20 minutes, it was filtered, placed under ventilated conditions for 1 hour, dried at 110°C for 2 hours, and then calcined at 450°C for 4 hours to obtain a core-shell carrier (X), in which the amorphous silica shell accounted for the weight of the carrier (X) 44.4% of the total.

[0025] Preparation of supported catalyst: weigh 33g X carrier, 0.75gRhCl 3 .3H 2 O, 200mlH 2 O was mixed thoroughly, and then dried at 100 °C to obtain a supported catalyst RhCl containing 0.8% (weight percent) Rh 3 .3H 2 O / X.

[0026] Synthesis of diethylene acetate: 0.006molRhCl 3 .3H 2 O / X, 0.18molCH 3 I. Add 0.018mol tributylphosphine and 1.20mol MeOAc into a 2-liter titanium reactor that has replaced the air with argon in advance, and then feed carbon monoxide and hydrogen so that the mo...

Embodiment 3

[0096] Preparation of core-shell carrier: will contain 5g SiO 2 200ml of acidified sodium silicate solution was evenly added dropwise in 5gAl 2 o 3 After 20 minutes, it was filtered, placed under ventilated conditions for 1 hour, dried at 110°C for 2 hours, and then calcined at 450°C for 4 hours to obtain a core-shell carrier (Y), in which the amorphous silica shell accounted for the weight of the carrier (Y) 50.0% of.

[0097] Modification of the carrier: 30g of 2-[methoxy(polyethyleneoxy)propyl]trimethoxysilane (CAS No.65994-07-2, English name 2-[Methoxy(polyethyleneoxy)propyl]- trimethoxy silane) in acetone solution, sprayed on the core-shell carrier (Y), stirred, filtered, washed and dried to obtain the modified core-shell carrier (X).

[0098] Preparation of supported catalyst: weigh 33g carrier X, 0.75gRhCl 3 .3H 2 O, 200mlH 2 O was mixed thoroughly, and then dried at 100 °C to obtain a supported catalyst RhCl containing 0.8% (weight percent) Rh 3 .3H 2 O / X.

...

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Abstract

The invention relates to a preparation method for preparing ethylidene diacetate from methyl acetate, which mainly solves the problems that the methyl acetate conversion rate is low and the ethylidene diacetate selectivity is low in the prior art. The invention adopts the following technical scheme: the preparation method for preparing ethylidene diacetate from methyl acetate comprises the following step: reacting MeOAc, CO and H2 used as raw materials in the presence of a supported catalyst, a cocatalyst and a promoter, thus generating the ethylidene diacetate, wherein the supported catalyst comprises a core-shell type support and a VIII metal or VIII metal compound supported on the support; the cocatalyst is an iodine-containing compound; the promoter is a nitrogen-oxygen organic substance or phosphorus-containing compound; and the core-shell type support has an amorphous aluminum oxide core and an amorphous silicon oxide shell. Thus, the technical scheme well solves the problems. The invention can be used for production of vinyl acetate.

Description

technical field [0001] The invention relates to a preparation method for preparing 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 diethylen...

Claims

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Application Information

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IPC IPC(8): C07C69/16C07C67/36B01J31/30
CPCC07C67/36C07C69/16
Inventor 查晓钟杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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