Preparation method of fluid catalyst for production of hydroxyacetic acid ester by oxalate through hydrogenation

A fluidized bed catalyst and glycolate technology, which is applied in the preparation of carboxylate, the preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problems of low selectivity of glycolate in hydrogenation products

Inactive Publication Date: 2012-08-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is the low technica...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Using silicon oxide as a carrier, prepare the catalyst according to the active component of 20wt% Cu+5wt% Mg+1wt% Mo and the auxiliary dosage based on the total weight of the catalyst. The steps are as follows: (a) configure the copper, magnesium and molybdenum of the required concentration Mixed nitrate solution and sodium carbonate solution; (b) the above solution was co-precipitated at 70°C, stirring continuously during the precipitation process, and PH=6 when the precipitation was terminated; (c) the above precipitation slurry was washed repeatedly with deionized water until No Na + After adding silicon oxide carrier (specific surface area 150 square meters / gram) and concentration are 10% silica sol binding agent beating; Spherical shape; (e) Dry at 120°C for 6 hours and bake at 450°C for 4 hours. That is, the fluidized bed catalyst A was obtained.

[0018] Using a fluidized bed reactor, using dimethyl oxalate as a raw material, the reaction temperature is 200 ° C...

Embodiment 2

[0020] Using alumina as a carrier, prepare the catalyst according to the active components of 40wt% Cu+3wt%Ca+15wt%V and the auxiliary amount based on the total weight of the catalyst. The steps are as follows: (a) configure the required concentration of copper, calcium and vanadium Mixed nitrate solution and sodium carbonate solution; (b) the above solution was co-precipitated at 65°C, stirring continuously during the precipitation process, and PH=7 when the precipitation was terminated; (c) the above precipitation slurry was washed repeatedly with deionized water until No Na + After adding alumina carrier (specific surface area 300 square meters / gram) and concentration are 15% silica sol binding agent beating; Spherical shape; (e) Dry at 120°C for 6 hours and bake at 450°C for 4 hours. That is, the fluidized bed catalyst B was obtained.

[0021] Using a fluidized bed reactor, using dimethyl oxalate as a raw material, the reaction temperature is 170 ° C, and the weight spac...

Embodiment 3

[0023] With ZSM-5 molecular sieve as the carrier, prepare the catalyst according to the active components of 45wt% Cu+8wt% Zn+0.5wt% Re and the auxiliary dosage, the steps are as follows: (a) configure the mixture of copper, zinc and rhenium of required concentration Nitrate solution and sodium carbonate solution; (b) the above solution is co-precipitated at 65°C, stirring continuously during the precipitation process, and the pH = 5 when the precipitation is terminated; (c) repeatedly washing the above precipitation slurry with deionized water until there is no Na + Finally, add ZSM-5 molecular sieve carrier (specific surface area 450 square meters / gram) for beating; (d) spray molding with a pressure spray dryer, control the average diameter of catalyst particles to be 140 microns, and the particles are spherical; (e) 120 ° C Dry for 6 hours and bake at 450°C for 4 hours. That is, a fluidized bed catalyst C is obtained.

[0024] Using a fluidized bed reactor, using dimethy...

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Abstract

The invention relates to a preparation method of fluid catalyst for production of hydroxyacetic acid ester by oxalate through hydrogenation, which mainly solves the problem of low hydroxyacetic acid ester selectivity in hydrogenated products in the prior art. The preparation method comprises following steps: (a), preparing required mixed nitrate solution and sodium carbonate solution of copper element and auxiliary agent element; (b), performing coprecipitation to the required mixed nitrate solution and sodium carbonate solution at the temperature of 50 to 90 DEG C, continuously stirring during coprecipitation, and ensuring that the PH value ranges from 5 to 9 when the coprecipitation is ended; (c), washing the precipitated slurry with deionized water repeatedly, and adding a carrier and an adhesion agent for pulping until no Na<+> ion is caused; (d), performing spray forming as per required particle size: the average diameter of catalyst particles is 50 to 300 micrometers, and the catalyst particulars are spheroidal; (e), drying for 4 to 20 hours at the temperature of 80 to 120 DEG C, and roasting for 2 to 8 hours at the temperature of 300 to 550 DEG C. The preparation method solves the problem better and can be used for industrial production of hydroxyacetic acid ester.

Description

technical field [0001] The invention relates to a preparation method of a fluidized bed catalyst for hydrogenation of oxalate to glycolate, in particular to a preparation method of a fluidized bed catalyst for catalytic hydrogenation of dimethyl oxalate or diethyl oxalate into glycolate. Background technique [0002] With its unique molecular structure: it has a-H, hydroxyl and ester functional groups at the same time, which makes it have the chemical properties of alcohol and ester, and can undergo carbonylation reaction, hydrolysis reaction, oxidation reaction, etc., and has become an important chemical raw material . Glycolate is an excellent solvent for many celluloses, resins, and rubbers. Its downstream products such as glycolic acid, glycine, dimethyl malonate and glyoxylic acid also have extensive application value. [0003] At present, there is no mature production process of environmentally friendly glycolic acid ester in China. It is still produced by the chlor...

Claims

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Application Information

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IPC IPC(8): B01J23/887B01J23/847B01J29/48B01J23/89B01J35/08C07C69/675C07C67/31
Inventor 刘俊涛李斯琴蒯骏
Owner CHINA PETROLEUM & CHEM CORP
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