Decarbonylation chlorination catalyst as well as preparation method and application thereof
A decarbonylation and chlorination catalyst, a catalyst technology, applied in physical/chemical process catalysts, chemical instruments and methods, preparation of organic compounds, etc., can solve the difficulty of synthesizing and separating chlorinated aromatic compounds, and the product quality is difficult to guarantee , increase the difficulty of separation, etc., to achieve the effect of reducing temperature, good adaptability, and reducing the amount of precious metals
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Embodiment 1
[0042] Preparation of catalyst: at room temperature, the specific surface area is 200m 2 / g of activated aluminum oxide 10g, added to 15mL containing 1.67g of palladium chloride and 0.50g of gallium trichloride prepared by hydrochloric acid acid (pH <1) In the aqueous solution, slowly heat to boiling and maintain for 2h, then cool to below 40°C, collect the solid by filtration, wash with deionized water until the mother liquor is neutral, and then dry in an oven at 80°C to obtain the catalyst precursor About 12g. Take 5g of the prepared catalyst precursor and put it into a fixed-bed reactor, first purge the adsorbed moisture with nitrogen to a temperature of 200°C, maintain it for 2h and then further increase the temperature to 450°C, maintain it for 3h, and then slowly decrease the temperature to 80°C. Into a hydrogen-nitrogen mixture with a volume content of 10% (the volume fraction of hydrogen is 10%), keep the reduction until anhydrous gas is generated, then heat up to 200°C...
Embodiment 2
[0048] Catalyst preparation: at room temperature, the specific surface area is 200m 2 / g of activated aluminum oxide 10g, added to 15mL containing 1.67g palladium chloride, chloroplatinic acid 0.20g and gallium trichloride 0.50g prepared by hydrochloric acid acid (pH <1) In the aqueous solution, slowly heat to boiling and maintain for 2h, then cool to below 40°C, collect the solid by filtration, wash with deionized water until the mother liquor is neutral, and then dry in an oven at 80°C to obtain the catalyst precursor About 12g. Take 5g of the prepared catalyst precursor and put it into a fixed-bed reactor, first purge the adsorbed moisture with nitrogen to a temperature of 200°C, maintain it for 2h and then further increase the temperature to 450°C, maintain it for 3h, and then slowly decrease the temperature to 80°C. Into a hydrogen-nitrogen mixture with a volume content of 10% (the volume fraction of hydrogen is 10%), keep the reduction until anhydrous gas is generated, the...
Embodiment 3
[0053] Catalyst preparation: at room temperature, take the specific surface as 50m 2 / g of magnesium fluoride 10g, added to 15mL containing 0.83g palladium chloride, 0.10g chloroplatinic acid and 0.20g titanium tetrachloride prepared by hydrochloric acid acid (pH <1) In the aqueous solution, slowly heat to boiling, and further evaporate the solvent to obtain about 11.2 g of solid. Take 5g of the prepared catalyst precursor and put it into a fixed-bed reactor, first purge the adsorbed moisture with nitrogen to a temperature of 200°C, maintain it for 2h and then further increase the temperature to 450°C, maintain it for 3h, and then slowly decrease the temperature to 80°C. Fill in the hydrogen-nitrogen mixture with a volume content of 10%, keep the reduction until anhydrous gas is generated, then heat up to 200°C to reduce for 5 hours, then cool to room temperature in a nitrogen atmosphere, and then transfer the catalyst to the reagent bottle under nitrogen protection and seal it ...
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