Liquid phase reaction process of methyl acetate and CO to produce acetic anhydride and its catalyst preparing process

A carbon monoxide and methyl acetate technology, which is applied to the preparation of carboxylic anhydride, physical/chemical process catalysts, molecular sieve catalysts, etc., can solve the problems of many side reaction products, short catalyst life, high production costs, etc., and achieve conversion rate and acetic anhydride yield High efficiency, high conversion rate and selectivity, easy to adjust and optimize the effect

Active Publication Date: 2007-06-27
山东华鲁恒升集团德化设计研究有限公司 +1
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AI Technical Summary

Problems solved by technology

[0012] Among the above various liquid-phase oxo-synthesis methods for acetic anhydride, although some processes are very mature and industrialized, there are generally the following disadvantages: the catalyst preparation process is complex and the selectivity and activity of the prepared catalyst are poor and the catalyst life is short ; The conversion rate of methyl acetate is low, the side reaction products are more, and the space-time yield of methyl acetate is low so that it brings difficulties to the subsequent separation process of the product, and the process production cost is higher

Method used

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  • Liquid phase reaction process of methyl acetate and CO to produce acetic anhydride and its catalyst preparing process

Examples

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example 1

[0026] In the laboratory, a 500ml titanium pressure reactor is used to carry out the implementation of the above invention, and the logistics composition and operating parameters added to the reactor are:

[0027] Methyl acetate add-on: 1.20mol; The content of active component rhodium-palladium complex A is 2.1%, and its proportioning ratio is 4: 1; Cocatalyst: ethyl iodide or methyl bromide are loaded on ZSM-5 molecular sieve, Its weight percentage is 2.5%; Carrier is ZSM-5 molecular sieve, and its weight percentage is 30.0%, and all the other components are the mixture of kaolin and silicon oxide that mass ratio is 1: 1; The weight ratio of catalyst and methyl acetate, carbon monoxide is 1: 0.65: 0.45; acetic acid dosage: 0.22L; carrier impregnation and burning time: 65.0min, burning temperature: 550.0°C; reaction system is potassium acetate solution, liquid phase solvent content is 70.0% of the total weight of the reaction system; Time: 18.0min; Reaction temperature: 195.0±...

example 2

[0029] In the laboratory, a 500ml titanium pressure reactor is used to carry out the implementation of the above invention, and the logistics composition and operating parameters added to the reactor are:

[0030] The amount of methyl acetate added: 1.21mol; the content of the active component rhodium palladium complex A is 2.1%, and its proportioning ratio is 4.5: 1; the cocatalyst B ethyl iodide or methyl bromide is loaded on the ZSM-5 molecular sieve, Its weight percentage is 2.6%; Carrier is ZSM-5 molecular sieve, and its weight percentage is 35.0%, and all the other components are the mixture of kaolin and silicon oxide that mass ratio is 1: 1.2; The weight ratio of catalyst and methyl acetate, carbon monoxide is 1: 0.68: 0.45; acetic acid dosage: 0.21L; carrier impregnation and burning time: 60.0min, burning temperature: 560.0°C; reaction system is potassium acetate solution, liquid phase solvent content is 75.0% of the total weight of the reaction system; reaction Time:...

example 3

[0032] In the laboratory, a 500ml titanium pressure reactor is used to carry out the implementation of the above invention, and the logistics composition and operating parameters added to the reactor are:

[0033]The amount of methyl acetate added: 1.22mol; the content of the active component rhodium palladium complex A is 2.1%, and its proportioning ratio is 4.4: 1; the cocatalyst B ethyl iodide or methyl bromide is loaded on the ZSM-5 molecular sieve, Its weight percentage is 2.6%; Carrier is ZSM-5 molecular sieve, and its weight percentage is 34.9%, and all the other components are the mixture of kaolin and silicon oxide that mass ratio is 1: 1.2; The weight ratio of catalyst and methyl acetate, carbon monoxide is 1: 0.68: 0.45; Acetic acid dosage: 0.21L; Carrier impregnation and burning time: 58.0min, burning temperature: 550.0°C; Reaction system is potassium acetate solution, liquid phase solvent content is 75.0% of the total weight of the reaction system; Time: 20.0min; ...

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Abstract

The present invention is the preparation process of acetic anhydride through liquid phase reaction of methyl acetate and CO and the preparation process of its catalyst. The catalyst has Rh-Pd complex with Rh / Pd weight ratio of 4-5 as the active component in 2.0-5.0 wt%, ethyl iodide or methyl bromide as co-catalyst in 0.5-9.5 wt%, and carrier of ZSM or MCM molecular sieve in 30.0-40.0 wt%. The catalyst is prepared through dissolving soluble compound of the catalyst and co-catalyst to obtain solution, soaking the carrier inside the solution, high temperature roasting at 500.0-600.0 deg.c for 1.0-1.5. The catalyst is used in preparing acetic anhydride through liquid phase reaction of methyl acetate and CO and can result in high methyl acetate converting rate and acetic anhydride yield. The present invention provides one new industrial production way.

Description

technical field [0001] The invention belongs to the method of chemical reaction. The invention relates to a preparation process for generating acetic anhydride (acetic anhydride) from methyl acetate and carbon monoxide in a liquid phase carbonyl group and a catalyst preparation method thereof. Background technique [0002] Acetic anhydride is the abbreviation of acetic anhydride, and its scientific name is acetic anhydride. It is a colorless and transparent liquid with a pungent smell and strong lachrymatory properties. It is an important organic chemical raw material with very active chemical properties. It is widely used in the production of cellulose acetate and as a medicine, dye, Acetylation agent in fragrance and organic synthesis. The production of acetic anhydride was initially by the ketene process based on acetic acid and acetone, and then by the oxidation cogeneration of acetaldehyde. Although the ketene method is a mature technology, its process is complex and...

Claims

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Application Information

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IPC IPC(8): B01J29/068C07C51/56C07C53/12
Inventor 杨世东张力明陈庆忠华超贾飞刘素英高岚张帆
Owner 山东华鲁恒升集团德化设计研究有限公司
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