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Method for preparing methyl glyoxylate/glyoxylic acid through continuous oxidation of methyl glycolate

A technology of methyl glycolate and methyl glyoxylate, which is applied to the preparation of carboxylate, carboxylate/lactone, chemical instruments and methods, etc., and can solve problems such as adverse effects, difficult separation, and harsh catalyst conditions , to stabilize the reaction process, improve reaction efficiency, and reduce excessive oxidation decomposition

Pending Publication Date: 2022-06-24
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the catalyst condition of this reaction is comparatively harsh, and the separation of raw material methyl glycolate and product glyoxylate methyl ester is comparatively difficult, and the prepared glyoxylate methyl ester has adverse effect on hydrolysis preparation glyoxylic acid

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: a kind of method utilizing methyl glycolate continuous oxidation to prepare methyl glyoxylate / glyoxylic acid

[0042] The method provided by this embodiment specifically includes the following operation steps:

[0043] S1, take 8 mL of catalyst 1 and 2 mL of silica carrier and fill it in a fixed-bed reactor, and heat the fixed-bed to 280°C under the condition of introducing air;

[0044] S2, after the temperature is stable, feed the raw material into the vaporization furnace, and control the liquid hourly space velocity of methyl glycolate to be 1.2h -1 , the control oxygen airspeed is 697h -1 , the molar ratio of oxygen to methyl glycolate is 2:1;

[0045] S3. The effluent steam is collected after cooling and gas-liquid separation, and the collected product is quantitatively analyzed. The conversion rate of the raw material is 99.8%, and the total selectivity of methyl glyoxylate and glyoxylic acid is 85.4%.

[0046] In this embodiment, the preparation m...

Embodiment 2

[0048] Embodiment 2: a kind of method utilizing methyl glycolate continuous oxidation to prepare methyl glyoxylate / glyoxylic acid

[0049] The method provided by this embodiment specifically includes the following operation steps:

[0050] S1, take 8mL of catalyst 2 and 2mL of zirconia carrier and fill it in a fixed-bed reactor, and heat the fixed-bed to 290°C under the condition of introducing air;

[0051] S2, after the temperature is stable, feed the raw material into the vaporization furnace, and control the liquid hourly space velocity of methyl glycolate to be 0.2h -1 , using a mixture of oxygen and nitrogen as the oxidant, the volume ratio of oxygen and nitrogen is 1:1, and the air velocity of the mixed gas is controlled to be 465h -1 , the molar ratio of oxygen to methyl glycolate is 4:1;

[0052] S3. The effluent steam is collected after cooling and gas-liquid separation, and the collected product is quantitatively analyzed. The conversion rate of the raw material i...

Embodiment 3

[0055] Embodiment 3: a kind of method utilizing methyl glycolate continuous oxidation to prepare methyl glyoxylate / glyoxylic acid

[0056] The method provided by this embodiment specifically includes the following operation steps:

[0057] S1, take 5mL of catalyst 3 and 5mL of silica carrier and fill it in a fixed-bed reactor, and heat the fixed-bed to 400°C under the condition of introducing air;

[0058] S2, after the temperature is stable, feed the raw material into the vaporization furnace, and control the liquid hourly space velocity of methyl glycolate to be 2h -1 , using air as the oxidant, and controlling the air space velocity to 4353 h -1 , the molar ratio of oxygen in the air to methyl glycolate is 1.5:1;

[0059] S3. The effluent steam is collected after cooling and gas-liquid separation, and the collected product is quantitatively analyzed. The conversion rate of the raw material is 99.4%, and the total selectivity of methyl glyoxylate and glyoxylic acid is 75.3...

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Abstract

The invention relates to the technical field of organic synthesis, in particular to a method for preparing methyl glyoxylate / glyoxylic acid through continuous oxidation of methyl glycolate. According to the technical key points, the method specifically comprises the following operation steps: S1, gasifying methyl glycolate; s2, the gasified methyl glycolate and an oxidizing agent are jointly and continuously introduced into a reactor for a reaction; s3, cooling the gas flowing out of the reactor, and carrying out gas-liquid separation to obtain a methyl glyoxylate solution; wherein the reactor is filled with a catalyst and a catalyst carrier; the catalyst is a supported composite oxide, the general formula is NixMyPzO, and M is any one or more of copper, manganese, cobalt, iron or vanadium. According to the method for preparing methyl glyoxylate / glyoxylic acid through continuous oxidation, the ratio of x to y is 0.6-1.5; the ratio of x to z is 2-8, the conversion rate of methyl glycolate is stabilized at 99% or above, the selectivity of methyl glyoxylate can reach 85.4%, the separation process of methyl glycolate and the product can be avoided, and convenience is provided for subsequent preparation of glyoxylic acid.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing methyl glyoxylate / glyoxylic acid by continuous oxidation of methyl glycolate. Background technique [0002] Glyoxylic acid is the simplest aldehyde acid with both aldehyde and carboxylic acid properties. It is widely used in chemical production processes. Its downstream products mainly involve fine chemical products with high added value and high demand, such as the field of pharmaceutical synthesis. , perfume synthesis, pesticide synthesis, etc. At the same time, glyoxylic acid can also be used as an intermediate for industrial chemicals such as dyes and plastics. [0003] There are many preparation methods of glyoxylic acid, which can be divided into glyoxal oxidation method, maleic anhydride ozone oxidation method, halogenated acid hydrolysis method and oxalic acid electrolytic reduction method according to different raw materials. Among them,...

Claims

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Application Information

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IPC IPC(8): C07C67/313C07C69/716C07C51/09C07C59/147B01J27/185B01J27/187B01J27/198B01J29/76B01J29/78
CPCC07C67/313B01J27/1853B01J27/198B01J27/187B01J29/7607B01J29/7807C07C51/09C07C69/716C07C59/147
Inventor 周维友王祥何明阳钱俊峰吴中
Owner CHANGZHOU UNIV
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