Catalyst for use in synthesis methylglycollate and glycol and preparation method thereof

A technology of methyl glycolate and silver silicon oxide, applied in the field of chemical industry, to achieve the effects of high selectivity, high activity and selectivity

Inactive Publication Date: 2010-09-01
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] What the present invention solves is the technical problem that methyl glycolate and ethylene glycol cannot be directly obtained from dimethyl oxalate through a continuous catalytic hydrogenation one-step method at present, and a method for directly obtaining methyl glycolate through catalytic hydrogenation of dimethyl oxalate is provided Novel catalysts for esters and ethylene glycol and methods for their preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Ag / SiO 2 -1# Catalyst

[0022] 0.096g silver acetylacetonate (C 5 h 7 AgO 2 ) was dissolved in 100ml of deionized water, and ammonia water was slowly added dropwise to pH = 10 to form a silver ammonia solution, 0.57g of PVP was added as a protective agent and a structure-directing agent, vigorously stirred for 0.5h, and 50ml containing 0.1635g aqueous solution of hexamethylenetetramine, continue to stir for 12 hours after the dropwise addition, add 17.19g tetraethyl orthosilicate dropwise at a constant speed, continue to stir for 1 hour after the dropwise addition, heat up to 90°C to evaporate part of the excess ammonia water to pH=8, cooled to room temperature. Wash 3 times with deionized water, wash once with ethanol, bake at 150°C for 16h, and raise the temperature to 200°C at 1°C / min in a muffle furnace for 24h. The catalyst powder was granulated into 40-60 mesh, and the activity evaluation was carried out. The results of selective hydrogenation are ...

Embodiment 2

[0023] Example 2: Ag / SiO 2 -2# Catalyst

[0024] 0.48g C 5 h 7 AgO 2 Dissolve in 100ml of deionized water, slowly add ammonia water dropwise to pH = 8 to form a silver ammonia solution, add 1.14g of PVP as a protective agent and structure-directing agent and stir vigorously for 1 hour, in a water bath at 20°C, slowly add 50ml containing 0.8265g six For the aqueous solution of methylenetetramine, continue to stir for 2 hours after the dropwise addition, add 16.49 g of tetraethyl orthosilicate dropwise at a constant speed, continue to stir for 2 hours after the dropwise addition, and raise the temperature to 70°C to evaporate part of the excess ammonia water to pH = 7 , cooled to room temperature. Wash 3 times with deionized water and once with ethanol, bake at 180°C for 2h, raise the temperature to 400°C at 2°C / min in a muffle furnace and keep for 4h. The catalyst powder was granulated into 40-60 mesh, and the activity evaluation was carried out. The results of selective h...

Embodiment 3

[0025] Example 3: Ag / SiO 2 -3# Catalyst

[0026] 0.96g C 5 h 7 AgO 2 Dissolve in 100ml of deionized water, slowly add ammonia water dropwise to pH = 9 to form a silver ammonia solution, add 5.7g of PVP as a protective agent and a structure-directing agent and stir vigorously for 2 hours, in a water bath at 60°C, slowly dropwise add 50ml containing 1.653g of six For the aqueous solution of methylenetetramine, continue to stir for 6 hours after the dropwise addition, add 15.62 g of tetraethyl orthosilicate dropwise at a constant speed, continue to stir for 4 hours after the dropwise addition, and raise the temperature to 60°C to evaporate part of the excess ammonia water to pH = 9 , cooled to room temperature, washed three times with deionized water, washed once with ethanol, baked at 100°C for 12h, and heated to 600°C at 5°C / min in a muffle furnace for 6h. The catalyst powder was granulated into 40-60 mesh, and the activity evaluation was carried out. The results of selecti...

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Abstract

The invention belongs to the field of chemical techniques, in particular to a catalyst for continuously catalyzing the hydrogenation of gas-phase dimethyloxalate for preparing methylglycollate and glycol, and preparation method thereof. The catalyst of the invention is prepared by the following steps of: preparing ammonia solution of silver by using a soluble silver salt and adding polyvinylpyrrolidone, which serves as a protective agent and structure-directing agent, into the solution; stirring the solution, adding a reducer into the solution and keeping the reaction temperature between 20 and 90 DEG C; adding tetraethoxysilane, stirring the reaction solution for 1 to 24 hours, raising temperature to 60 to 90 DEG C, and keeping the pH value of the reaction solution at the end of the reaction between 6 and 10; and finally, washing and drying the resulting product, and roasting the reaction product at 100 to 900 DEG C for 1 to 24 hours. The prepared catalyst is used for continuously catalyzing the hydrogenation of gas-phase dimethyloxalate for preparing the methylglycollate and the glycol, can well solve existing problems, and can be used in the industrial production of the methylglycollate and the glycol.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a high-efficiency catalyst for preparing methyl glycolate and ethylene glycol by gas-phase continuous catalytic hydrogenation of dimethyl oxalate and a preparation method thereof. Background technique [0002] Methyl glycolate is a multi-purpose chemical raw material, which can be widely used in the fields of chemical industry, medicine, pesticide, feed, spices and dyes. Methyl glycolate is readily soluble in nitrocellulose, cellulose acetate, cellulose acetate propionate, and polyvinyl acetate. It is also an excellent solvent for many celluloses, resins and rubbers. At the same time, different esters can be obtained by alcoholysis of methyl glycolate with other alcohols. In addition, methyl glycolate is an important intermediate in the synthesis of isoharringtonine and its analogs with anticancer activity, and it is also a raw material for the synthesis o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/50C07C69/675C07C67/32C07C31/20C07C29/149C07C27/04
CPCY02P20/52
Inventor 戴维林尹安远范康年
Owner FUDAN UNIV
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