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Catalyst for preparing glyoxylic acid from methyl glycolate, preparation method and application

A technology of methyl glycolate and glyoxylic acid is applied in the preparation of carboxylate, the preparation of carboxylate/lactone, and the preparation of oxygenated compounds, and can solve the problems of harsh reaction conditions, difficult product separation, environmental pollution and the like, To achieve the effects of mild reaction conditions, simple and convenient preparation process and high conversion rate

Active Publication Date: 2018-04-06
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention can solve the disadvantages of difficult product separation, certain pollution to the environment, harsh reaction conditions and high energy consumption in the prior art.

Method used

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  • Catalyst for preparing glyoxylic acid from methyl glycolate, preparation method and application
  • Catalyst for preparing glyoxylic acid from methyl glycolate, preparation method and application
  • Catalyst for preparing glyoxylic acid from methyl glycolate, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 4.65g of cobalt nitrate hexahydrate, 0.81g of ferric nitrate nonahydrate and 2.00g of oxalate dihydrate in a mortar, mix well; add 1mL of ethylene glycol to it, grind for 30min; transfer it to a beaker, Dry in an oven at 110° C. for 12 hours; then bake in a muffle furnace at 300° C. for 4 hours to obtain catalyst A. Its XRD diagram is shown in figure 1 . It includes the composite oxide formed by ferric oxide and tricobalt tetroxide; among them, ferric oxide is amorphous and in an amorphous state.

Embodiment 2

[0024] Weigh 4.65g of cobalt nitrate hexahydrate, 9.70g of ferric nitrate nonahydrate and 2.00g of oxalate dihydrate in a mortar, mix well; add 1mL of ethylene glycol to it, and grind for 30min; Dry in an oven at 110°C for 12h; then bake in a muffle furnace at 300°C for 4h to obtain Catalyst B, whose XRD pattern is shown in figure 1 , in the catalyst, the crystallization effect of ferric oxide and cobalt tetraoxide may not be very good or there are few samples to be tested, so the characteristic peaks are not obvious.

Embodiment 3

[0026] Weigh 4.65g of cobalt nitrate hexahydrate, 12.93g of ferric nitrate nonahydrate and 2.00g of oxalate dihydrate in a mortar, mix well; add 1mL of ethylene glycol to it, grind for 30min; transfer it to a beaker, Dry in an oven at 110°C for 12h; then bake in a muffle furnace at 300°C for 4h to obtain catalyst C, whose XRD pattern is shown in figure 1 , the results show that catalyst C includes ferric oxide and tricobalt oxide composite oxide, and cobalt ferrite.

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Abstract

The invention belongs to the technical field of organic chemical industry and particularly relates to a catalyst for preparing glyoxylic acid from methyl glycolate, a preparation method and an application. The catalyst is a composite oxide formed of ferric oxide and osmium tetroxide, or a mixture of one or two of cobalt ferrite, wherein the molar ratio of Fe to Co is between 1:8 and 2:1. The catalyst is prepared by a solid phase grinding method, that is, iron nitrate nonahydrate, cobalt nitrate hexahydrate, oxalic acid dihydrate and ethylene glycol are mixed and then ground, dried and baked. The method is simple and easy to implement. The catalyst is used in the preparation of the glyoxylic acid from the methyl glycolate, a fixed bed reactor is used, the reaction is performed under the conditions of the reaction temperature of 200 to 260 DEG C and the space velocity of gaseous methyl glycolate of 1740 ml / (h.g), the conversion rate of the methyl glycolate is 67% to 99%, and the selectivity of the glyoxylic acid is 55% to 100%.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, in particular to a catalyst for preparing glyoxylic acid from methyl glycolate, a preparation method and application. Background technique [0002] Glyoxylic acid is an important intermediate in organic synthesis. It is widely used in the fields of spices, food additives, medicine, pesticides, anti-corrosion and corrosion inhibition. It can be used to produce vanillin, ethyl vanillin, oral penicillin, Raw material of mandelic acid, phenylglycine and other products. [0003] The current industrial methods for preparing glyoxylic acid can be divided into two categories: chemical synthesis and electrochemical synthesis . Chemical synthesis methods mainly include glyoxal oxidation and maleic acid ozone oxidation. The glyoxal oxidation method is to prepare glyoxylic acid by oxidizing glyoxal with nitric acid, peroxide and other oxidants. This method is the most mature preparation ...

Claims

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Application Information

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IPC IPC(8): B01J23/75C07C27/02C07C59/147
CPCB01J23/002B01J23/75C07C51/09C07C67/313C07C59/147C07C69/716
Inventor 刘芳芳郭晓明毛东森俞俊毛海舫徐新良
Owner SHANGHAI INST OF TECH
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