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Method for preparing polyoxymethylene dimethyl ether carboxylate and methyl methoxy acetate

A technology of polyoxymethylene dimethyl ether and carbonylate, which is applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problem of unsatisfactory conversion rate of methylal to methyl methoxyacetate, methylation Low aldehyde concentration, short catalyst life, etc., to achieve high selectivity, long catalyst life, and high conversion

Active Publication Date: 2015-06-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

However, the catalyst life is short, the concentration of methylal in the feed gas is low, the conversion rate of methylal and the selectivity of methyl methoxyacetate are not ideal enough, and there is still a considerable distance from industrialization [Angew.Chem.Iht.Ed., 2009, 48, 4813-4815; J.Catal., 2010, 270, 185-195; J.Catal., 2010, 274, 150-162; WO2010 / 048300A1]

Method used

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  • Method for preparing polyoxymethylene dimethyl ether carboxylate and methyl methoxy acetate
  • Method for preparing polyoxymethylene dimethyl ether carboxylate and methyl methoxy acetate
  • Method for preparing polyoxymethylene dimethyl ether carboxylate and methyl methoxy acetate

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Embodiment 1

[0050] Dry 50g of acidic Nafion-117 resin in a blast drying oven at 105°C for 12 hours in an air atmosphere. After cooling, weigh 10g and put it into a stainless steel reaction tube with an inner diameter of 8.5mm for activity testing. Activation with nitrogen for 1 hour, then lowered to reaction temperature (T) = 90 ° C, introduced carbon monoxide: dimethyl methoxy dimethyl ether: hydrogen (CO: DMM 2 :H 2 )=7:1:1, slowly increase the pressure to the reaction pressure (P)=10MPa, the mass space velocity of dipolyoxymethoxydimethyl ether (WHSV)=0.2h -1 , Analyze the product with gas chromatography, after the reaction is basically stable, calculate the conversion rate of dipolyoxymethoxydimethyl ether and the selectivity of polymethoxydimethyl ether carbonylate, the reaction results are shown in Table 1.

Embodiment 2

[0052] The catalyst in embodiment 1 is changed into acidic Nafion-115 resin, T=60 ℃, CO: DMM 2 :H 2 =13:1:3, P=4MPa, WHSV=1.5h -1 , all the other experimental procedures are consistent with Example 1, and the reaction results are shown in Table 1.

Embodiment 3

[0054] The catalyst in embodiment 1 is changed into acidic Nafion-112 resin, T=140 ℃, CO:DMM 2 :H 2 =2:1:5, P=6.5MPa, WHSV=3.0h -1 , all the other experimental procedures are consistent with Example 1, and the reaction results are shown in Table 1.

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Abstract

The invention provides a method for preparing polyoxymethylene dimethyl ether carboxylate and / or methyl methoxy acetate which serves as an intermediate for producing ethylene glycol. The method comprises the step of enabling a raw material, namely polyoxymethylene dimethyl ether or methylal, together with carbon monoxide and hydrogen gas to react in an acidic resin catalyst loaded reactor under appropriate reaction conditions without adding other solvents, so as to prepare corresponding products, wherein a reaction process is of gas-liquid-solid three-phase reaction. According to the method provided by the invention, the conversion ratio of the raw material polyoxymethylene dimethyl ether or methylal is high, the selectivity of each product is high, the service life of a catalyst is long, external solvents are not required to be used, reaction conditions are relatively mild, and continuous production can be carried out, so that the method has industrial application potential. Furthermore, the obtained products can be used for producing ethylene glycol through hydrolyzing after hydrogenating or hydrogenating after hydrolyzing.

Description

technical field [0001] The invention relates to a method for preparing polymethoxy dimethyl ether carbonylate and methyl methoxyacetate as intermediates for producing ethylene glycol. Background technique [0002] Ethylene glycol is an important chemical raw material and strategic material in the country. It is used in the manufacture of polyester (which can further produce polyester, PET bottles, films), explosives, glyoxal, and can be used as antifreeze, plasticizer, hydraulic fluid and solvent Wait. In 2009, China's ethylene glycol imports exceeded 5.8 million tons. It is estimated that my country's ethylene glycol demand will reach 11.2 million tons in 2015, with a production capacity of about 5 million tons, and a supply-demand gap of 6.2 million tons. Therefore, my country's ethylene glycol production The development and application of new technologies has a good market prospect. Internationally, ethylene oxide from petroleum cracking is mainly oxidized to obtain ethy...

Claims

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Application Information

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IPC IPC(8): C07C67/37C07C69/708
CPCC07C67/37C07C69/708
Inventor 倪友明朱文良刘红超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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