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Method for producing methyl methoxyacetate by methylal vapor-phase carbonylation by using supported heteropoly acid catalyst

A technology of methyl methoxyacetate and gas-phase carbonylation, 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 beneficial to large-scale industrial production, catalysis High efficiency and easy separation effect

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

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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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  • Method for producing methyl methoxyacetate by methylal vapor-phase carbonylation by using supported heteropoly acid catalyst
  • Method for producing methyl methoxyacetate by methylal vapor-phase carbonylation by using supported heteropoly acid catalyst

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Embodiment 1

[0044] 5%H 3 PW 12 o 40 / SiO 2 Catalyst preparation process is as follows: with concentration is the phosphotungstic acid aqueous solution of 6% by weight, with SiO 2 As a carrier, the volume of the impregnation solution is the same as the pore volume of the carrier, the carrier is mixed with the impregnation solution, and after mixing uniformly, it is left at room temperature for 10 hours to obtain the carrier impregnated with the heteropolyacid as a sample, and the sample Dry at 120°C and bake at 350°C for 4 hours to prepare catalyst samples. The catalyst number is 1.

[0045] 5%H 3 PW 12 o 40 / SiO 2 Catalyst preparation process is as follows: with concentration is the phosphotungstic acid aqueous solution of 6% by weight, with SiO 2 As a carrier, the volume of the impregnation solution is the same as the pore volume of the carrier, the carrier is mixed with the impregnation solution, and after mixing uniformly, it is left at room temperature for 20 hours to obtain ...

Embodiment 2

[0053] Experiments on Vapor Phase Carbonylation of Methylal over Various Catalysts

[0054] A fixed-bed reactor with an inner diameter of 6mm is filled with 0.5g of one of the catalysts 1 to 30, the reaction pressure is 1.5MPa, the reaction temperature is 110°C, the space velocity of the gas phase medium containing CO is 100ml / min, and the CO in the gas phase medium The ratio is 60%, the additional gas of the CO-containing gas phase is hydrogen, and the CO / DMM molar ratio is 150. After the reaction was stable, the reaction raw materials and products were analyzed by online chromatography. The results are shown in Table 3.

[0055] Table 3: Experiments on gas phase carbonylation of methylal over various catalysts

[0056]

Embodiment 3

[0058] 33%H at different temperatures 3 PW 12 o 40 / SiO 2 Vapor Phase Carbonylation of Methylal over Catalyst

[0059] A fixed bed reactor with an inner diameter of 6 mm is filled with 0.5 g of catalyst, the reaction pressure is 1.5 MPa, the space velocity of the gas phase medium containing CO is 100 ml / min, the proportion of CO in the gas phase medium is 60%, and the other gas containing CO gas phase is Hydrogen with a CO / DMM molar ratio of 150. After the reaction was stable, the reaction raw materials and products were analyzed by online chromatography. The results are shown in Table 4.

[0060] Table 4

[0061] temperature(℃) Yield of methyl methoxyacetate (%) 80 32.9 100 35.2 130 38.7 180 35.8

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Abstract

The invention relates to application of a supported heteropoly acid catalyst in production of methyl methoxyacetate by methylal vapor-phase carbonylation. The catalyst is prepared by an isometric impregnation method, and uses at least one of activated carbon, TiO2, Al2O3, SiO2, SBA-15, MCM-41 and zeolite molecular sieve as a supporter, wherein the heteropoly acid accounts for 0.1-50 wt% of the supported heteropoly acid catalyst. When being used for the reaction for producing methyl methoxyacetate by methylal vapor-phase carbonylation, the catalyst has the characteristics of mild reaction conditions and high catalytic efficiency; and since no solvent is used in the reaction, the product and catalyst can be easily separated, thereby being beneficial to large-scale industrial production.

Description

technical field [0001] The invention relates to a method for producing methyl methoxyacetate through gas-phase carbonylation of methylal with a supported heteropolyacid catalyst. 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 disadvantages of large consumption of raw materials and high energy consumption. [0003] The carbonylation of formaldehyde and its derivatives to ethylene glycol is an imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/708C07C67/36
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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