Preparation method of composite catalyst and alcohol ether carboxylate
A composite catalyst and alcohol ether carboxylate technology, which is applied in the preparation of carboxylate, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of high catalyst cost, difficult removal of chloroacetic acid, and high viscosity of material systems. Achieve large-scale industrial production, improve metal utilization, and improve catalytic activity
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[0022] The present embodiment provides a kind of preparation method of composite catalyst, comprises the following steps:
[0023] (1) Pretreatment of activated carbon: the aqueous solution of activated carbon and activating reagent is reacted under heating conditions to obtain pretreated activated carbon;
[0024] (2) Mix divalent palladium, divalent non-noble metal, hydrochloric acid and the pretreated active carbon obtained, and react; adjust the pH to alkaline, add a reducing agent, and separate after the reaction to obtain a composite catalyst;
[0025] The activation reagent described in step (1) includes at least one of hydrochloric acid, nitric acid and hydrogen peroxide;
[0026] The divalent non-noble metal in step (2) includes at least one of divalent nickel, divalent tin and divalent cobalt.
[0027] Specifically, the preparation method of described composite catalyst comprises the following steps:
[0028] (1) Pretreatment of activated carbon: react the aqueous ...
Embodiment 1
[0050] (1) Pretreatment of activated carbon: Weigh 5.0 g of activated carbon with a particle size of 200 mesh in a three-necked flask, add 60 mL of 10% hydrochloric acid aqueous solution, and stir and reflux at 90° C. for 5 h. Filter and wash the activated carbon until the pH of the filtrate is neutral, and dry in vacuum at 80°C for 12 hours to obtain pretreated activated carbon.
[0051] (2) Preparation of composite catalyst: get 32mg palladium chloride and 41mg cobalt chloride hexahydrate and be dissolved in 4ml concentrated hydrochloric acid (37wt%), dilute with 35ml water, add the active carbon after the 0.5g pretreatment after the solution is stirred, continue Stir for 3h, add Na 2 CO 3 Adjust the pH of the system to 8-9 with the aqueous solution, continue to stir for 1h, and dissolve 200mg of NaBH 4Dissolve in 2ml of water, add dropwise to the solution, react for 3 hours, centrifuge the solution, wash with water until the pH is neutral.
[0052] (3) Preparation of alc...
Embodiment 2
[0056] (1) Pretreatment of activated carbon: Weigh 5.0 g of activated carbon with a particle size of 200 mesh in a three-necked flask, add 80 mL of aqueous hydrogen peroxide solution with a mass concentration of 8%, and stir and reflux at 90° C. for 5 h. Filter and wash the activated carbon until the pH of the filtrate is neutral, and dry in vacuum at 80°C for 12 hours to obtain pretreated activated carbon.
[0057] (2) Preparation of composite catalyst: get 41mg palladium chloride and 23mg tin chloride dihydrate and be dissolved in 4ml concentrated hydrochloric acid (37wt%), dilute with 30ml water, add the active carbon after the 0.5g pretreatment after the solution is stirred, continue Stir for 3h, add Na 2 CO 3 Adjust the pH of the system to 8-9 with aqueous solution, continue to stir for 1h, and dissolve 200mg NaBH 4 Dissolve in 2ml of water, add dropwise to the solution, react for 3 hours, centrifuge the solution, wash with water until the pH is neutral.
[0058] (3) P...
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