Method for preparation of methyl glycolate and by-product methyl methoxyacetate with catalyst

A by-product technology of methyl methoxyacetate and methyl glycolate, which is applied in the direction of carbon monoxide or formate reaction preparation, chemical instruments and methods, and the preparation of organic compounds, can solve the problem of low conversion rate of raw materials and product selectivity Low cost, environmental pollution and other problems, to achieve the effect of high conversion rate of raw materials, high product selectivity, and short synthetic route

Active Publication Date: 2017-12-22
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 preparation of methyl glycolate and by-product methyl methoxyacetate with catalyst
  • Method for preparation of methyl glycolate and by-product methyl methoxyacetate with catalyst
  • Method for preparation of methyl glycolate and by-product methyl methoxyacetate with catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Weigh 20 kg of methylal (DMM), 3.9 kg of paraformaldehyde (the molar ratio of DMM to aldehyde group is 2:1), 300 g of catalyst, and 4 kg of water and put them into the reactor. The catalyst types are liquid acid (H 2 SO 4 , HCl), cation exchange resins (NKC-9, Amberlyst-15, DA330, KAD302, KC107, D072H), heteropoly acids (phosphotungstic acid, molybdenum tungstic acid, silicotungstic acid), solid super acid (SO 4 2 - / ZrO 2 , WO 3 / ZrO 2 , MoO 3 / ZrO 2 , B 2 o 3 / ZrO 2 ), impregnated solid acid (SO 4 2 - / SiO 2 ), and then introduce 1.0 MPa carbon monoxide gas, if there is no leakage, after emptying the gas in the kettle, 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 g...

Embodiment 2

[0065] Weigh 20 kg of methylal (DMM), 3.9 kg of paraformaldehyde (the molar ratio of DMM to aldehyde group is 2:1), 4 kg of water, and 300 g of NKC-9 resin catalyst into the reaction kettle, and then pass it into the reaction vessel at 1.0 MPa Carbon monoxide gas, if there is no leakage, after emptying the gas in the kettle, repeat the above operation twice (replace 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 6.0 MPa, the reaction temperatures were 90°C, 100°C, 110°C, 130°C, 150°C, and the reaction time was 6 h. The reaction results are shown in Table 2.

[0066]

[0067] Reaction conditions: 20 kg methylal, 3.9 kg paraformaldehyde, 4 kg...

Embodiment 3

[0070] Weigh 20 kg of methylal (DMM), 3.9 kg of paraformaldehyde (the molar ratio of DMM to aldehyde group is 2:1), 4 kg of water, and 300 g of NKC-9 resin catalyst into the reaction kettle, and then pass it into the reaction vessel at 1.0 MPa Carbon monoxide gas, if there is no leakage, after emptying the gas in the kettle, repeat the above operation twice (replace 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 pressures were 2.0 MPa, 3.0 MPa, 4.0 MPa, 5.0 MPa, 6.0 MPa, 8.0 MPa, 10.0 MPa, 15.0 MPa, the reaction temperature was 130°C, and the reaction time was 6 h , and the reaction results are shown in Table 3.

[0071]

[0072] Reaction conditions: 2...

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Abstract

Relating to a preparation method of chemical raw materials, the invention provides a method for preparation of methyl glycolate and by-product methyl methoxyacetate with a catalyst. The method adopts methylal as the solvent, s-trioxane, tetrameric or paraformaldehyde and methylal are taken as the source of formaldehyde, H2SO4, HCl and other liquid acids or cation exchange resin, heteropoly acid, impregnation solid acid, solid super acid and other solid acids are employed as the catalyst, one-step synthesis with high conversion rate and high selectivity is carried out to obtain methyl glycolate and the by-product methyl methoxyacetate. In a fixed bed reactor, 300g of an NKC-9 sulfonic acid resin catalyst is used, the raw materials include: 20kg of methylal, 4kg of water and 2.9kg of s-trioxane, the mass space velocity of the raw materials is 30h<-1>, reaction is carried out under a reaction temperature of 130DEG C and a reaction pressure of 6.0MPa, the catalyst is stable without inactivation for 2000h, the methylal conversion rate is 89.83%, the product methyl glycolate has mass selectivity of 28.88%, the methyl methoxyacetate has mass selectivity of 67.68%. The method provided by the invention has the advantages of short synthetic route, high raw material conversion rate or high product selectivity, and the synthesis process has no pollution to the environment.

Description

technical field [0001] The invention relates to a method for preparing methyl glycolate, in particular to a method for preparing methyl glycolate with a 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 organic synthesis and ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/675C07C67/36C07C69/708
Inventor 石磊陈飞姚杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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