Catalyst for preparing methyl glycolate through dimethyl oxalate hydrogenation and synthetic method of catalyst

A technology of dimethyl oxalate and methyl glycolate is applied in the preparation of carboxylate, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc., and can solve the problem of increasing catalyst production cost and corrosion reaction pressure. , Hydrocyanic acid has problems such as high toxicity, and achieves the effect of high catalyst activity and stability, simple preparation process and good repeatability.

Active Publication Date: 2014-05-14
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are many traditional synthesis methods of methyl glycolate, and most of these traditional processes have deficiencies, such as the one-step synthesis of glyoxal and methanol to prepare MG, the glyoxal in the raw material is too toxic and expensive, and is not suitable for industrialization Production; the addition method of formaldehyde and hydrocyanic acid, the raw material hydrocyanic acid is highly toxic, and it is not suitable for large-scale production even if the yield is high; the coupling method is mostly catalyzed by liquid and solid strong acids, and

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A catalyst synthesis method for preparing methyl glycolate by hydrogenating dimethyl oxalate: comprising the following steps: (1) weighing about 11.40g Cu(NO 3 ) 2 .3H 2 O and 6.25g mass fraction of 50% Mn(NO 3 ) 2 .6H 2 O, and dissolve it with 200mL deionized water; (2) Weigh 4.65g of NaOH that can completely precipitate metal ions as a precipitant, and dissolve it with deionized water to make a concentration of 2mol / L; (3) Stir and the temperature of the water bath is At 80°C, slowly drop the nitrate solution prepared in step 1) into the NaOH solution prepared in step 2) until the pH is about 8.0, and the process is about 1 hour; (4) Speed ​​up the stirring, and at the same temperature, put Alkaline silica sol was added to the solution obtained in step 3), and stirred at this temperature for 4 hours, and then aged at the above temperature for 12 hours. (5) Suction filter the aged catalyst, wash it several times with deionized water until the pH of the filtrate is...

Embodiment 2

[0020] A catalyst synthesis method for preparing methyl glycolate by hydrogenating dimethyl oxalate: comprising the following steps: (1) weighing about 11.40g Cu(NO 3 ) 2 .3H 2 O and 2.73g of Zn(NO 3 ) 2 .3H 2 O, and dissolve it with 200mL deionized water; (2) Weigh 4.51g of NaOH that can completely precipitate metal ions as a precipitant, and dissolve it with deionized water to make a concentration of 2mol / L; (3) Stir and water bath temperature is At 80°C, slowly drop the nitrate solution prepared in step 1) into the NaOH solution prepared in step 2) until the pH is about 8.0, and the process is about 1 hour; (4) Speed ​​up the stirring, and at the same temperature, put Alkaline silica sol was added to the solution obtained in step 3), and stirred at this temperature for 4 hours, and then aged at the above temperature for 12 hours. (5) Suction filter the aged catalyst, wash it several times with deionized water until the pH of the filtrate is 7.0; then dry the filter cak...

Embodiment 3

[0023] A catalyst synthesis method for preparing methyl glycolate by hydrogenating dimethyl oxalate: comprising the following steps: (1) weighing about 11.40g Cu(NO 3 ) 2 .3H 2 O and 2.12 g of ZrOCl 2 .8H 2 O, and dissolve it with 200mL deionized water; (2) Weigh 4.83g of NaOH that can completely precipitate metal ions as a precipitant, and dissolve it with deionized water to make a concentration of 2mol / L; (3) Stir and water bath temperature is At 80°C, slowly drop the nitrate solution prepared in step 1) into the NaOH solution prepared in step 2) until the pH is about 8.0, and the process is about 1 hour; (4) Speed ​​up the stirring, and at the same temperature, put Alkaline silica sol was added to the solution obtained in step 3), and stirred at this temperature for 4 hours, and then aged at the above temperature for 12 hours. (5) Suction filter the aged catalyst, wash it several times with deionized water until the pH of the filtrate is 7.0; then dry the filter cake fo...

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Abstract

The invention discloses a catalyst for preparing methyl glycolate through dimethyl oxalate hydrogenation and a synthetic method of the catalyst, belonging to the technical field of preparation of methyl glycolate catalysts. The catalyst is prepared by taking NaOH as a precipitator, wherein Cu is a main active ingredient of the catalyst, alkaline silica sol serves as a carrier, one or more base metals in Mn, Zr and Zn serve as aids, the mass content of metal copper is 10-40 percent, the content of the other base metal aids is 5-10 percent, and the carrier content is 60-80 percent. According to the catalyst, the preparation method is simple, raw materials are readily available, preparation repeatability is high, high reaction activity is achieved in a methyl glycolate preparation reaction through the dimethyl oxalate hydrogenation, and the catalyst stability and the selectivity of the methyl glycolate are high.

Description

technical field [0001] The invention relates to a catalyst synthesis method for preparing methyl glycolate by hydrogenating dimethyl oxalate, and belongs to the technical field of methyl glycolate catalyst preparation. technical background [0002] Methyl glycolate (MG) is the simplest type of alkyd ester. It is an urgently needed chemical in the fields of high-end pesticides, medicines, and chemical environmental protection. Anti-carrier additive raw material for oil extreme pressure and wear resistance. In addition, methyl glycolate is a compound with hydroxyl, carbonyl and α-H functional groups at the same time. As an intermediate, a series of important downstream products can be prepared, such as hydrolysis to prepare glycolic acid, hydrogenation to prepare ethylene glycol, carbonylation to prepare propane Dimethyl diacid and ethyl acetoacetate, ammonia solution to prepare DL-glycine, oxidative dehydrogenation to prepare glyoxylate, etc. [0003] There are many traditi...

Claims

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Application Information

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IPC IPC(8): B01J23/889B01J23/80B01J23/72C07C69/675C07C67/31
Inventor 何明阳陈群杨秋慧钱俊峰
Owner CHANGZHOU UNIV
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