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Method for preparing polyoxymethylene dimethyl ether carboxylate and methyl methoxy acetate

A technology of polyoxymethylene dimethyl ether and carbonyl, which is applied in the direction of chemical instruments and methods, chemical/physical processes, carbon monoxide or formate reaction preparation, etc., and can solve the conversion rate of methylal to methyl methoxyacetate Unsatisfactory selectivity, low methylal 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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  • Application Information

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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, 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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preparation example Construction

[0037] The preparation method of the acidic molecular sieve catalyst of described desiliconization modification comprises putting molecular sieve into optional 0.05~6.0mol / L, preferably 0.2~1.5mol / L sodium hydroxide, potassium hydroxide, lithium hydroxide, hydroxide In one or several mixed solutions of magnesium, calcium hydroxide, sodium carbonate or sodium bicarbonate, react at 15-95°C, preferably 50-85°C for 0.5-24h, and filter the filter cake with 0.01-0.5mol / Wash with L of hydrochloric acid, nitric acid, sulfuric acid or acetic acid solution to neutralize the acidity of the filter cake, then wash and neutralize the salt solution with deionized water, and then undergo the conventional ammonium ion exchange, filtration, drying, and calcination procedures to obtain desiliconization. Acidic molecular sieve catalyst.

[0038] The structural type of the acidic molecular sieve catalyst is MWW, FER, MFI, MOR, FAU or BEA. Preferably, the acidic molecular sieve catalyst is any on...

Embodiment 1

[0051] 50 g of MCM-22 molecular sieves with a sodium-type silicon-aluminum ratio of 40:1 were converted into acidic molecular sieves using standard operating procedures, which were recorded as catalyst A, as shown in Table 1.

Embodiment 2

[0053] Add 100g of MCM-22 molecular sieve with a sodium-type silicon-aluminum ratio of 40:1 to 500ml of calcium hydroxide solution with a concentration of 1.5mol / L, stir and react at 75°C for 10h, and filter the cake with 0.08ml / L The nitric acid solution was washed until the pH was 6, filtered and washed repeatedly with deionized water until neutral, dried at 100°C and converted into an acidic molecular sieve through standard operating procedures, which was recorded as catalyst B, see 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 a desiliconisation modified acidic molecular sieve 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): C07C69/708C07C67/37B01J29/70B01J29/65B01J29/40B01J29/08
Inventor 倪友明朱文良刘勇刘红超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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