Carbon loaded type noble metal catalyst and preparation method thereof
A precious metal catalyst and catalyst technology, applied in the direction of metal/metal oxide/metal hydroxide catalyst, chemical instrument and method, ozone oxidation to prepare carboxylic acid, etc., can solve the problems of shortened service life, palladium catalyst poisoning, etc. Effects of replenishment speed, increased activity and stability, improved operational stability and productivity
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Embodiment 1
[0032] Get 50 grams of powdered activated carbon (product of Shanghai Activated Carbon Co., Ltd., analytically pure, specific surface area 860m 2 / g, moisture content 10%, pH value is 3.5, particle size is that 40-60 micron accounts for 50%, all the other are 60-160 micron, the same below), after following pretreatment as the carrier of palladium-ruthenium catalyst:
[0033] (1) The hydrochloric acid aqueous solution of 10% by weight with 500ml concentration of activated carbon is covered and boiled on a water bath for 6 hours, removes soluble impurities, ash and orifice blockages on the surface, rinses with deionized water until the filtrate is neutral, after filtering Dry at 110°C;
[0034] (2) The activated carbon after removing impurities was oxidized with 150ml of 20% by weight nitric acid solution at room temperature for 6 hours, then rinsed with deionized water until the filtrate was neutral, and dried at 110°C. Add 100 mL of deionized water to make an activated carbon...
Embodiment 2
[0039] (1) 50 grams of powdered activated carbon are 10% by weight hydrochloric acid aqueous solution with a concentration of 500ml, adding a cover and boiling for 6 hours on a water bath, removing soluble impurities, ash and orifice blockages on the surface, and washing with deionized water into the filtrate properties, dried at 110°C after filtration;
[0040] (2) The activated carbon after the impurity removal is heated up to 425° C. in a mixed gas atmosphere of 50 ml / min of 5% O2+95% N2 at a gas flow rate and constant for 11 hours for oxidation treatment, and then cooled to room temperature after treatment. Add 100 mL of deionized water to make an activated carbon suspension.
[0041] (3) Under the condition of stirring, add 100ml of aqueous solutions of palladium chloride and ruthenium chloride with concentrations of 20g / l and 5g / l to the above-mentioned activated carbon suspension, and adsorb 2-48 After 1 hour, 18 mL of NaOH solution with a concentration of 5 (weight) %...
Embodiment 3
[0045] (1) 50 grams of powdered activated carbon are 10% by weight hydrochloric acid aqueous solution with a concentration of 500ml, adding a cover and boiling for 6 hours on a water bath, removing soluble impurities, ash and orifice blockages on the surface, and washing with deionized water into the filtrate properties, dried at 110°C after filtration;
[0046] (2) The activated carbon after removing impurities was oxidized with 150ml of 20% by weight nitric acid solution at room temperature for 6 hours, then rinsed with deionized water until the filtrate was neutral, and dried at 110°C. Add 100 mL of deionized water to make an activated carbon suspension.
[0047] (3) Under the condition of stirring, add 100ml concentration to the above-mentioned active carbon suspension and be respectively the aqueous solution of the palladium chloride of 17.5g / l, 7.5g / l and the aqueous solution of ruthenium chloride, under 30 ℃ and strong stirring, constant temperature adsorption 2 After ...
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