Catalyst for synthesizing methyl glycolate through hydrogenation by dimethyl oxalate and preparation method thereof

A technology of methyl glycolate and dimethyl oxalate, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of low concentration of methyl glycolate, ethyl Dialdehyde is expensive, waste water is difficult to treat and other problems, to achieve the effect of low price, low cost and easy control

Active Publication Date: 2010-05-05
JIANGSU JINJU ALLOY MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production of methyl glycolate at home and abroad mainly adopts the chloroacetic acid method, that is, mixing chloroacetic acid with caustic soda, then removing the sodium chloride generated by the reaction to obtain glycolic acid, and then adding methanol and concentrated sulfuric acid to react to generate methyl glycolate. The production pollution is serious, the wastewater is difficult to treat, and the produced methyl glycolate has a low concentration and high chloride ion content, which seriously affects the use as an intermediate in the fields o

Method used

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Examples

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Effect test

Embodiment 1

[0015] A preparation method of a catalyst for synthesizing methyl glycolate by hydrogenation of dimethyl oxalate, comprising the steps of: (1) taking by weighing 30gAl(OH) 3 Powder, fineness is 300 mesh, add 1000ml distilled water and mix and stir, and be heated up to 65 ℃, constant temperature 15min; 2 CO 3 Aqueous solution, add dropwise for 20min, then keep the temperature at 65°C and stir for 20min; (3) Weigh 160g Cu(NO 3 ) 2 ·6H 2 O, 18g Mn(NO 3 ) 2 4H 2 O and 5g AgNO 3 Dissolve in 600g of distilled water to make a mixed aqueous solution, and drop the mixed aqueous solution evenly into the solution obtained in step 2. The time for adding is 40min, and the temperature for adding is 70°C. 2 CO 3 The pH value of the aqueous solution adjustment system = 9; (4) the mixed system prepared in the above steps was stirred at 75 ° C for 40 minutes and then suction filtered, and the filter cake was washed with distilled water repeatedly and then suction filtered until the filt...

Embodiment 2

[0017] A preparation method of a catalyst for synthesizing methyl glycolate by hydrogenation of dimethyl oxalate, comprising the steps of: (1) taking by weighing 30gAl(OH) 3 Powder, fineness is 400 mesh, add 1000ml distilled water and mix and stir, and be warmed up to 50 ℃, constant temperature 18min; 2 CO 3 Aqueous solution, add dropwise for 25min, then keep the temperature at 80°C and stir for 30min; (3) Weigh 180g Cu(NO 3 ) 2 ·6H 2 O, 8g Mn(NO 3 ) 2 4H 2 O and 8g AgNO 3 Dissolve in 700g distilled water to make a mixed aqueous solution, and drop the mixed aqueous solution evenly into the solution obtained in step 2, the time for adding is 60min, and the temperature for adding is 60°C. 2 CO 3 The aqueous solution adjusts the pH value of the system to 10; (4) the mixed system prepared in the above steps is stirred at 80°C for 60 minutes and then suction filtered, and the filter cake is washed with distilled water repeatedly and then suction filtered until the filtrate ...

Embodiment 3

[0019] A preparation method of a catalyst for synthesizing methyl glycolate by hydrogenation of dimethyl oxalate, comprising the steps of: (1) taking by weighing 30gAl(OH) 3 Powder, fineness is 400 mesh, add 1000ml distilled water and mix and stir, and be heated up to 80 ℃, constant temperature 20min; 2 CO 3 Aqueous solution, add dropwise for 30min, then keep the temperature at 60°C and stir for 25min; (3) Weigh 170g Cu(NO 3 ) 2 ·6H 2 O, 12g Mn(NO 3 ) 2 4H 2 O and 6g AgNO 3 Dissolve in 650g distilled water to make a mixed aqueous solution, and drop the mixed aqueous solution evenly into the solution obtained in step 2. The time for adding is 50min, and the temperature for adding is 80°C. 2 CO 3 The aqueous solution adjusts the pH value of the system to 9.5; (4) the mixed system prepared in the above steps is stirred at 70°C for 50 minutes and then suction-filtered, and the filter cake is washed with distilled water repeatedly and then suction-filtered until the filtrat...

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PUM

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Abstract

The invention discloses a catalyst for synthesizing methyl glycolate through hydrogenation by dimethyl oxalate and a preparation method thereof. The catalyst takes metal copper as a main active component, silver and manganese as auxiliary components and Al2O3 as a carrier, wherein the content of metal copper accounts for 25-50% of the mass of the catalyst, the content of metal silver accounts for 5-15% of the mass of the catalyst, the content of metal manganese accounts for 8-20%, and the content of Al2O3 accounts for 15-40% of the mass of the catalyst. In the reaction for synthesizing methyl glycolate through hydrogenation by dimethyl oxalate, the catalyst of the invention has the advantages of high reaction activity, simple preparation method, easily obtained raw material resource, low price, lower cost and longer service life, the methyl glycolate has high selectivity, stable reaction performance and easy controllability.

Description

technical field [0001] The invention belongs to the field of catalyst chemistry, in particular to a catalyst for hydrogenating dimethyl oxalate to synthesize methyl glycolate and a preparation method thereof. Background technique [0002] Methyl glycolate is a compound with α-H, hydroxyl and ester functional groups. Therefore, it can undergo carbonylation reactions, hydrolysis reactions, and oxidation reactions. It is widely used in organic synthesis and drug synthesis, as an important chemical reaction intermediate Body: a. Hydrogenation reduction to produce ethylene glycol, a bulk chemical product, to solve the shortage of raw materials for the production of ethylene glycol from petroleum routes; b. Hydrolysis to produce glycolic acid, which is widely used as a fungicide and chemical cleaning agent; c. Oxidative deoxidation Hydrogenation of methyl glyoxylate, the hydrolysis product of glyoxylate, glyoxylic acid is the main raw material for the synthesis of vanillin spices,...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C69/675C07C67/31
Inventor 吴晓金刘志刚许叶飞魏超汤涛
Owner JIANGSU JINJU ALLOY MATERIAL
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