Method for preparing methyl glycollate and byproduct methyl methoxy acetate by molecular sieve catalyst

A technology for by-producing methyl methoxyacetate and methyl glycolate is applied in the directions of carbon monoxide or formate reaction preparation, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of polluted environment, low product selectivity, Problems such as low conversion rate of raw materials, to achieve the effect of increasing the ratio of CO and aldehyde groups

Active Publication Date: 2017-12-08
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A.T.Bell et al. used methyl formate instead of gaseous CO and formaldehyde for carbonylation reaction, but since the decomposition of methyl formate and release of CO is a rate-controlling step, it affects the performance of the catalytic reac

Method used

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  • Method for preparing methyl glycollate and byproduct methyl methoxy acetate by molecular sieve catalyst
  • Method for preparing methyl glycollate and byproduct methyl methoxy acetate by molecular sieve catalyst
  • Method for preparing methyl glycollate and byproduct methyl methoxy acetate by molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Embodiment 1: catalyst preparation example

[0071] H-Y catalyst

[0072] Exchange 100 grams of calcined Na-Y (Si / Al=6.5) molecular sieves with 0.5mol / L ammonium nitrate three times, each time for 2 hours, wash with deionized water, dry, calcinate at 550°C for 4 hours, and extrude 1# catalysts of 20-40 mesh were prepared respectively.

[0073] Supported M / Y catalyst

[0074] The supported 5% M / Y catalyst was prepared by isometric impregnation method. 4.32 g Cu(NO 3 ) 2 ·3H 2 O, 3.04 gAgNO 3 ·3H 2 O, 4.32gFe(NO 3 ) 3 , 5.21g Co(NO 3 ) 2 ·6H 2 O , 5.21 g Ni(NO 3 ) 2 ·6H 2 O and 4.58 g Ga(NO 3 ) 3 Dissolve in 18 mL deionized water to make the corresponding nitrate aqueous solution. Add 20g of 1# H-Y molecular sieve catalyst to the above-mentioned nitrate aqueous solution respectively, let it stand for 24 hours, then separate it, wash it with deionized water, dry the obtained sample in an oven at 120°C for 12 hours, and place the dried sample in a muffle f...

Embodiment 2

[0085] Embodiment 2: the reactivity performance of catalyst

[0086] The catalyst powder obtained in Example 1 was tabletted, crushed, and sieved to obtain a 40-60 mesh sample for the synthesis of methyl glycolate and the determination of the reaction performance of the by-product methyl methoxyacetate. Weigh 20 kg of methylal (DMM), 3.9 kg of paraformaldehyde, 4 kg of water, and 300 g of various catalysts prepared in Example 1 and put them into the reaction kettle, and then feed 1.0 MPa of carbon monoxide gas. After emptying the gas in the reactor, repeat the above operation 2 times (replacing the air in the reactor). Introduce a certain amount of gas (6.0 MPa) again to test for leaks, and let it stand for 15 minutes. If the pressure indicator does not drop, it means that there is no air leakage in the device. Then empty the gas in the kettle and fill the kettle with 6.0 MPa CO gas again. , heated up, the stirring speed of the reactor was 500 rpm, the reaction pressure was 6...

Embodiment 3

[0092] Respectively with hydrogen type Y molecular sieve, hydrogen type MCM-22 molecular sieve, hydrogen type ZSM-35 molecular sieve, hydrogen type ZSM-5 molecular sieve, hydrogen type mordenite, hydrogen type Beta molecular sieve as the metal modified catalyst carrier, with 6 in embodiment 1 The preparation method of #catalyst prepares metal-modified catalyst, respectively marked as 6#, 6# MCM-22, 6# ZSM-35, 6# ZSM-5, 6# MOR, 6#β catalyst, and gained catalyst powder is through tabletting The 40-60 mesh samples obtained by grinding, crushing and sieving were used for the synthesis of methyl glycolate and the determination of the reaction performance of the by-product methyl methoxyacetate. Weigh 20 kg of methylal (DMM), 3.9 kg of paraformaldehyde, 4 kg of water, and 300 g of the above-mentioned catalysts into the reaction kettle, and then feed 1.0 MPa of carbon monoxide gas, and empty the gas in the kettle if there is no leakage After that, repeat the above operation 2 times (...

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Abstract

The invention provides a method for preparing methyl glycollate and a byproduct methyl methoxy acetate by a molecular sieve catalyst and relates to methods for preparing chemical raw materials. According to the method, methylal serves as a solvent, tripoly-, tetrapoly-or paraformaldehyde serves as a formaldehyde source, metal element doped modified molecular sieves of different topological structures serve as a catalyst, and methyl glycollate (MG) is synthesized in one step in a high conversion ratio and high selectivity manner on the premise that a proper volume of water is present in a system. The two kinds of products, i.e., the methyl glycollate (MG) and the methyl methoxy acetate (MMAc) are relatively large in boiling point difference and can be separated subsequently through simple distillation. According to the one-step synthesis method for the methyl glycollate and the byproduct methyl methoxy acetate, under the reaction conditions that the reaction temperature is 130 DEG C, the reaction pressure is 6.0MPa and the reaction time is 6h, 5% Ni/Y prepared by an isometric dipping method serves as a catalyst, the conversion ratio of DMM can reach 89.59%, the selectivity of MG can reach 80.40%, and the catalyst is not deactivated in 2,000h of stable use.

Description

technical field [0001] The invention relates to a method for preparing chemical raw materials, in particular to a method for preparing methyl glycolate with a molecular sieve catalyst and producing methyl methoxyacetate by-product. Background technique [0002] Methyl glycolate (HOCH 2 COOCH 3 ), abbreviated as MG, is a colorless liquid with a pleasant smell, with a melting point of 74°C, a boiling point of 150°C, and a density of 1.168g / cm 3 , soluble in water, and soluble in alcohol and ether in any proportion. Methyl glycolate has α-H, hydroxyl and ester functional groups, so it has both the chemical properties of alcohols and esters, and can undergo carbonylation reactions, hydrolysis reactions, ammoniation reactions, oxidation reactions, etc. Methyl glycolate itself is an excellent solvent for many celluloses, resins and rubbers, and is easily soluble in nitrocellulose, cellulose acetate, polyvinyl acetate, etc. Methyl glycolate is also an important intermediate in ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/675C07C67/37C07C69/708
Inventor 石磊姚杰陈飞
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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