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Methyl methoxyacetate preparation method

A technology of methyl methoxyacetate and methylal, applied in the directions of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of less research on ethylene glycol precursors, etc., and is conducive to large-scale industrial production, Ease of separation and mild reaction conditions

Inactive Publication Date: 2013-06-26
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few studies on the production of ethylene glycol precursors by gas-phase carbonylation of formaldehyde and its derivatives [see: Angew.Chem.Int.Ed.2009,48,4813-4815; J.Catal.2010,274,150-162 ]

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Fill 0.5g of 33%H in a fixed bed reactor with an inner diameter of 6mm 3 PW 12 o 40 / SiO 2 , the reaction pressure is 1.5MPa, the reaction temperature is 110°C, the space velocity of the gaseous medium containing CO is 100ml / min, the volume percentage of CO in the gaseous medium is 60%, and the other gas in the gaseous medium containing CO is hydrogen, CO / The DMM molar ratio was 150. After the reaction was stable, the reaction raw materials and products were analyzed by online chromatography, and the yield of methyl methoxyacetate was 36.8%. The results are shown in Table 1.

Embodiment 2

[0040] Except for using the solid acid catalyst in Table 1, other conditions were the same as in Example 1, and performance evaluation of gas phase carbonylation reaction of methylal was performed, and the reaction effluent was analyzed by online chromatography. The results are shown in Table 1.

[0041] Table 1

[0042] catalyst

Embodiment 3

[0044]In addition to filling 1g33%H in the fluidized bed reactor and the moving bed reactor with an inner diameter of 10mm 3 PW 12 o 40 / SiO 2 Except that other conditions are the same as in Example 1, performance evaluation of gas-phase carbonylation reaction of methylal was carried out, and the reaction effluent was analyzed by online chromatography. The results are shown in Table 2.

[0045] Table 2

[0046] Reactor type

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PUM

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Abstract

The invention discloses a methyl methoxyacetate preparation method by gaseous carbonylation. The method comprises the step of reacting methylal and a CO-containing gas phase medium under the action of heteropolyacid and supported heteropolyacid catalyst to generate the methyl methoxyacetate, wherein the reaction temperature is 50-300 DEG C and the reaction pressure is 0.1-4MPa. Compared with the traditional ethylene glycol precursor preparation method by liquid phase carbonylation reaction synthesis, the method provided by the invention has the advantages of mild reaction conditions and high catalytic efficiency. Furthermore, the product is easily separated from the catalyst as no solvent is used in the reaction, which is conductive to large-scale industrial production.

Description

technical field [0001] The invention relates to a method for continuously producing ethylene glycol precursor methyl methoxyacetate under gas-solid phase conditions. Specifically, under the action of a solid acid catalyst, methylal and CO or a gas phase medium containing CO react in a fixed-bed reactor to generate methyl methoxyacetate. Background technique [0002] Ethylene glycol is an important organic chemical raw material, widely used in the synthesis of polyester monomers, surfactants, antifreeze and explosives. At present, the industrial production method of ethylene glycol mainly uses ethylene oxidation to ethylene oxide, ethylene oxide is hydrolyzed to obtain ethylene glycol aqueous solution, and ethylene glycol is obtained through rectification. Ethylene mainly comes from petroleum, and due to the increasing shortage of petroleum resources and rising prices, the production cost of ethylene glycol has been high. Simultaneously, this route also has the disadvantage...

Claims

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Application Information

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IPC IPC(8): C07C69/708C07C67/37
Inventor 刘红超朱文良刘勇刘中民孟霜鹤李利娜刘世平周慧
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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