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Method for synthesizing methyl methoxyacetate through carbonylation of formaldehyde

A technology of methyl methoxyacetate and carbonylation, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve problems such as difficulty in product separation, corrosion of devices by sulfuric acid, and achieve product yield High, no corrosion reaction equipment, the effect of saving production costs

Pending Publication Date: 2022-05-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction conditions are relatively mild, but there are still problems such as corrosion of sulfuric acid to the device and difficulty in product separation.

Method used

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  • Method for synthesizing methyl methoxyacetate through carbonylation of formaldehyde
  • Method for synthesizing methyl methoxyacetate through carbonylation of formaldehyde
  • Method for synthesizing methyl methoxyacetate through carbonylation of formaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Catalyst treatment

[0030] Weigh 0.459 g (0.5 mmol) of tris(triphenylphosphine)rhodium carbonyl hydride and add it into 44 g of methyl tert-butyl ether, and ultrasonically disperse for 1 hour to obtain a uniform light yellow liquid.

[0031] 2. Carbonylation reaction

[0032] Put the above homogeneous mixture in a 100mL stainless steel autoclave, add 7.5g of acetic acid, 6.1g of water, and 7.5g of paraformaldehyde (0.25mol, CAT / HCHO=0.2mol%) in sequence, seal the reactor, and replace the reactor with CO Air was injected 3 times, high-pressure CO was introduced to 8MPa, and the reaction was carried out at 110°C for 3 hours under vigorous stirring. After the reaction, the reactor was cooled to room temperature, all the reaction solution was taken out and placed in a separatory funnel, and allowed to stand until layers were separated. Such as figure 1 As shown, the liquid is divided into upper and lower layers, and the lower layer liquid is filtered through a microp...

Embodiment 2

[0037] 1. Catalyst recovery

[0038] The upper layer of the liquid after the carbonylation reaction in Example 1 was taken out to obtain a homogeneous mixture of catalyst and solvent, which was sealed and set aside.

[0039] 2. Carbonylation reaction

[0040] Put the above homogeneous mixture in a 100mL stainless steel autoclave, add 7.5g of acetic acid, 6.1g of water, and 7.5g of paraformaldehyde (0.25mol, CAT / HCHO=0.2mol%) in sequence, seal the reactor, and replace the reactor with CO Air was injected 3 times, high-pressure CO was introduced to 8MPa, and the reaction was carried out at 110°C for 3 hours under vigorous stirring. After the reaction, the reactor was cooled to room temperature, all the reaction solution was taken out and placed in a separatory funnel, and allowed to stand until layers were separated. Such as figure 2 As shown, the liquid is divided into upper and lower layers, and the lower layer liquid is filtered through a microporous membrane to obtain a ...

Embodiment 3

[0046] 1. Catalyst treatment

[0047] Weigh 0.131 g (0.5 mmol) of rhodium dicarbonyl acetylacetonate and add it into 82 g of ethyl tert-butyl ether, and ultrasonically disperse for 1 hour to obtain a uniform light yellow liquid.

[0048] 2. Carbonylation reaction

[0049] Put the above homogeneous mixture in a 100mL stainless steel autoclave, add 7.4g of propionic acid, 6.1g of water, and 9.0g of paraformaldehyde (0.1mol, CAT / HCHO=0.5mol%) in sequence, seal the autoclave, and replace the autoclave with CO Insulate the air three times, pass high-pressure CO to 6MPa, and react at 100°C for 5h under vigorous stirring. After the reaction, the reactor was cooled to room temperature, all the reaction solution was taken out and placed in a separatory funnel, and allowed to stand until layers were separated. The liquid is divided into upper and lower layers, and the lower layer liquid is filtered through a microporous membrane to obtain a light yellow, transparent and clear carbonyl...

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Abstract

The invention relates to a method for synthesizing methyl methoxyacetate through carbonylation of formaldehyde, which adopts a carbonyl rhodium catalyst and comprises the following steps: (1) uniformly mixing the carbonyl rhodium catalyst with a solvent methyl tert-butyl ether and / or ethyl tert-butyl ether to obtain a mixture; (2) fully contacting a formaldehyde monomer source substance, CO, organic carboxylic acid and the mixture obtained in the step (1) for carbonylation reaction; after the reaction is finished, separating the solvent and the catalyst to obtain a carbonylation product; and (3) adding methanol into the carbonylation product for esterification reaction to generate methyl methoxyacetate. The method has the characteristics that the catalyst is non-corrosive to reaction equipment, the direct separation of the product and the catalyst and the direct recycling of the catalyst and the solvent are realized, and the energy consumption of the separation process and the production cost are effectively reduced.

Description

technical field [0001] The invention relates to the field of petrochemical industry, in particular to a method for synthesizing methyl methoxyacetate by carbonylation of formaldehyde. Background technique [0002] The carbonylation of formaldehyde and its derivatives is an important research direction of C1 chemistry. This route uses formaldehyde and its derivatives from coal, natural gas or biomass as raw materials to produce ethylene glycol, which is one of the important alternatives to the existing ethylene glycol process. Methyl methoxyacetate, one of the carbonylation products, is a very valuable intermediate, which can be used for the dynamic resolution of chiral amine compounds, the synthesis of vitamin B6 and sulfa-5-pyrimidine, etc., and as a catalyst for polymerization reactions Among them, ethylene glycol can also be produced through hydrogenation and hydrolysis. [0003] At present, there are two routes for carbonylation reaction, homogeneous catalysis and hete...

Claims

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Application Information

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IPC IPC(8): C07C69/708C07C67/31C07C67/08C07C67/00
CPCC07C67/31C07C67/08C07C67/00C07C51/145C07C69/708C07C59/06
Inventor 王迪吕建刚刘波周海春金萍
Owner CHINA PETROLEUM & CHEM CORP
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