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Catalyst for methanol or dimethyl ether carbonylation synthesis of methyl acetate, preparation method and application thereof

A technology of methyl acetate and catalyst, applied in the field of synthesis of methyl acetate, can solve the problems of low catalyst activity, poor catalyst stability and the like, and achieve the effects of high selectivity, good stability and mild reaction conditions

Active Publication Date: 2014-03-26
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acidity of the transition metal catalyst supported on silica-alumina zeolite is too strong, and a large amount of dehydration / hydrolysis products are generated; the acidity of the transition metal sulfurized catalyst is too weak, the catalyst activity is low, and the catalyst stability is poor

Method used

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  • Catalyst for methanol or dimethyl ether carbonylation synthesis of methyl acetate, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Mix 33.6ml TEOS, 46.2ml TPAOH (0.68M) aqueous solution and 3.9ml deionized water, stir at room temperature for 2h until complete hydrolysis, and obtain solution A. Dissolve 1.02g TBOT in 11.4ml IPA, add 19.3ml TPAOH (0.68M) aqueous solution and 16.6ml deionized water, stir at room temperature for 40min to obtain a clear light yellow hydrolyzate B. Mix and stir the two hydrolyzates A and B evenly, then stir at 50°C for 3 hours to remove the alcohol in the system, and at the same time replenish deionized water to keep the volume of the glue constant, and then put it into a stainless steel crystallizer with a polytetrafluoroethylene liner In the kettle, it was aged at 80°C for 27 hours to obtain Sol 1. Take 6.0g of DDA and dissolve it in a mixed solution composed of 60ml of absolute ethanol and 60ml of deionized water, add the sol 1 prepared in the first step, and adjust the pH of the system to 10 with hydrochloric acid. The resulting mixture was continuously stirred at r...

Embodiment 2

[0025] Mix 20ml TEOS, 25.2ml TPAOH (0.68M) aqueous solution and 3.5ml deionized water, stir at room temperature for 1 hour until complete hydrolysis, and obtain solution A. Dissolve 1.25g TBOT in 9.8ml IPA, add 17ml TPAOH (0.68M) aqueous solution and 9.5ml deionized water, stir at room temperature for 30min to obtain clear light yellow hydrolyzate B. Mix and stir the two hydrolyzates A and B evenly, then stir at 40°C for 3 hours to remove the alcohol in the system, and at the same time replenish deionized water to maintain a constant volume of the glue, and then put it into a stainless steel crystallizer with a polytetrafluoroethylene liner In the kettle, it was aged at 80°C for 30 hours to obtain Sol 1.

[0026] Dissolve 3.3g of DDA in a mixed solution of 30ml of absolute ethanol and 32ml of deionized water, add the sol 1 prepared in the first step, and adjust the pH of the system to 11 with hydrochloric acid. The resulting mixture was continuously stirred at room temperatur...

Embodiment 3

[0030]Mix 20ml TEOS, 25.2ml TPAOH (0.68M) aqueous solution and 9ml deionized water, stir at room temperature for 1 hour until complete hydrolysis, and obtain solution A. Dissolve 0.5g TBOT in 5.6ml IPA, add 9.5ml TPAOH (0.68M) aqueous solution and 8.5ml deionized water, stir at room temperature for 30min to obtain a clear light yellow hydrolyzate B. Mix and stir the two hydrolyzates A and B evenly, then stir at 45°C for 2 hours to remove the alcohol in the system, and supplement deionized water at the same time to keep the volume of the glue constant, and then put it into a stainless steel crystallizer with a polytetrafluoroethylene liner In the kettle, it was aged at 140°C for 6 hours to obtain Sol 1.

[0031] Dissolve 3.5g of DDA in a mixed solution of 35ml of absolute ethanol and 34ml of deionized water, add the sol 1 prepared in the first step, and adjust the pH of the system to 9.5 with hydrochloric acid. The resulting mixture was continuously stirred at room temperature...

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Abstract

A catalyst for methanol or dimethyl ether carbonylation synthesis of methyl acetate is composed of copper oxide, titanium silicalite molecular sieves and transition metal oxides. The copper oxide accounts for 5-30 wt% calculated by pure copper, transition metal oxides account for 0.2-5.0 wt% calculated by elementary transition metal, and the titanium silicalite molecular sieves account for 94.8-65 wt%. The invention has the advantages of mild reaction conditions, high selectivity of methyl acetate, and good stability and long service life of the catalyst.

Description

technical field [0001] The invention relates to a method for synthesizing methyl acetate, in particular to a catalyst for carbonylation of methanol or dimethyl ether to synthesize methyl acetate, a preparation method and application thereof. technical background [0002] Methyl acetate is an important chemical product, which is widely used in many industries such as textile, fragrance and medicine, and has considerable potential utilization value in leather and polyester industries. At the same time, as an important platform compound, methyl acetate is widely used in the synthesis of scarce products such as vinyl acetate and methyl acrylate, especially the technical route of producing acetic anhydride through carbonylation of methyl acetate has become the mainstay of acetic anhydride synthesis technology. Development Direction The existing methyl acetate synthesis processes are mainly acetic acid-methanol esterification and methanol liquid-phase carbonylation. The acetic ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C07C69/14C07C67/37C07C67/36
Inventor 李德宝郭荷芹肖勇陈从标
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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