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
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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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