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Synthesis method of methyl glycolate

A technology for the synthesis of methyl glycolate and methyl glycolate, which is applied in the field of carbonylation of formaldehyde to synthesize methyl glycolate, can solve the problems of poor stability of organophosphorus ligands, high cost, difficulty in large-scale promotion and application, and achieve non-corrosive reaction equipment , high product yield, and the effect of solvent recycling

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

On the one hand, formaldehyde is prone to reduction reaction to generate methanol during the reaction process; on the other hand, the catalyst uses Rh as the catalytic active center, and the organophosphorus ligand has poor stability, resulting in high cost of the process and difficulty in large-scale promotion and application

Method used

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  • Synthesis method of methyl glycolate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Carbonylation reaction

[0026] Weigh 0.171 g (0.5 mmol) of dicobalt octacarbonyl and add it into 42 g (0.25 mol) of cyclohexane. The above homogeneous mixture was placed in a stainless steel autoclave, 0.25 g (3 mmol) of 1-methylimidazole, 18.5 g (0.25 mol) of propionic acid, and 0.25 mol of paraformaldehyde were added in sequence, and the autoclave was sealed. All the above operations were carried out in a vacuum glove box. The reactor is taken out through the transition chamber and installed on the base. The air in the kettle was replaced with CO 3 times, high-pressure CO was introduced to 8 MPa, and the reaction was carried out at 110° C. for 3 h. After the reaction, the reactor was cooled to room temperature, all the reaction solution was taken out, and the layers were separated. Filter the dark liquid in the lower layer through a microporous membrane to obtain the carbonylation product, which is set aside.

[0027] 2. Esterification reaction

[0028] Put t...

Embodiment 2

[0031] 1. Reaction solvent recovery

[0032] The upper layer of the liquid after the carbonylation reaction in Example 1 was taken out, filtered through a microporous membrane, and set aside.

[0033] 2. Carbonylation reaction

[0034] Put the filtered upper solvent into a stainless steel autoclave. Add 0.5 mmol of dicobalt octacarbonyl, 0.25 g (3 mmol) of 1-methylimidazole, 18.5 g (0.25 mol) of propionic acid, and 0.25 mol of paraformaldehyde in sequence, and seal the reaction vessel. All the above operations were carried out in a vacuum glove box. The reactor is taken out through the transition chamber and installed on the base. Add CO to replace the air in the kettle for 3 times, pass high-pressure CO to 8MPa, and react at 110°C for 3h. 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. Filter the dark liquid in the lower layer throu...

Embodiment 3

[0039] 1. Carbonylation reaction

[0040]Weigh 0.684 g (2.0 mmol) of dicobalt octacarbonyl and add it into 101 g (1.4 mol) of n-pentane. The above homogeneous mixture was placed in a stainless steel autoclave, 1.54 g (16 mmol) of ethylimidazole, 10.2 g (0.17 mol) of acetic acid, and 0.25 mol of paraformaldehyde were added in sequence, and the autoclave was sealed. All the above operations were carried out in a vacuum glove box. The reactor is taken out through the transition chamber and installed on the base. The air in the kettle was replaced with CO for 3 times, high-pressure CO was introduced to 6MPa, and the reaction was carried out at 90°C for 5h. After the reaction, the reactor was cooled to room temperature, all the reaction solution was taken out, and the layers were separated. Filter the dark liquid in the lower layer through a microporous membrane to obtain the carbonylation product, which is set aside.

[0041] 2. Esterification reaction

[0042] Put the filter...

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Abstract

The invention relates to a synthesis method of methyl glycolate, which comprises the following steps: under the condition of water insulation and oxygen insulation, contacting polyformaldehyde, a solvent, organic carboxylic acid, a stabilizer and a cobalt carbonyl catalyst, and introducing CO to carry out carbonylation reaction to generate glycollic acid; and separating the carbonylation product from the solvent, and carrying out esterification reaction on the carbonylation product and methanol to generate methyl glycolate. The method has the characteristics that the catalyst is non-corrosive to reaction equipment, the direct separation of the product and the solvent and the direct recycling of 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 glycolate by carbonylation of formaldehyde. Background technique [0002] Methyl glycolate is an important organic chemical raw material, which can be widely used in the fields of chemical industry, polymer materials, pesticides, medicine, spices, feed and dyes. At the same time, methyl glycolate is also an important intermediate for coal to ethylene glycol In recent years, due to the rise of coal-based routes, it has received extensive attention. [0003] Traditional homogeneous synthesis methods mainly use inorganic liquid acids as catalysts, such as concentrated sulfuric acid, hydrofluoric acid, fluorine-containing sulfonic acid, etc. DuPont disclosed in USP2152852 and USP2285448 that sulfuric acid was used as a catalyst to catalyze the carbonylation reaction of formaldehyde and CO under the conditions of 200 ° C and 90 MPa, and it was us...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/08
CPCC07C67/08C07C51/12C07C69/675C07C59/06
Inventor 王迪吕建刚刘波周海春金萍邵益
Owner CHINA PETROLEUM & CHEM CORP
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