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Carbon loaded type noble metal catalyst and preparation method thereof

A precious metal catalyst, catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, preparation of carboxylic acid by ozone oxidation, etc., can solve the problems of palladium catalyst poisoning, shortening service life, etc. and stability, reduce replenishment speed, and reduce the effect of palladium metal loss

Active Publication Date: 2012-05-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the same way, in the process of preparing isopropyl cyclohexane carboxylic acid and ethyl cyclohexane carboxylic acid by hydrogenation of isopropyl benzoic acid and ethyl benzoic acid, the carbon monoxide produced by the side reaction can poison the palladium catalyst and shorten its reaction time. service life

Method used

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  • Carbon loaded type noble metal catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

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 -4 Aft...

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Abstract

The invention relates to a carbon loaded noble metal catalyst, which is characterized in that the catalyst consists of a carrier and palladium and ruthenium which are loaded on the carrier, wherein the carrier is powdery fruit shell active carbon and is between 85 and 99.7 percent by weight; the palladium is between 0.2 and 10 percent by weight; and the ruthenium is between 0.1 and 10 percent by weight. The catalyst is obtained by performing acid treatment, ash removal and oxidation treatment on the carrier, namely the active carbon for removing surface reduction functional groups first, using a solution of the palladium and the ruthenium to perform soakage treatment, and using one or more among hydrogen, potassium borohydride or hydrazine hydrate to perform reduction treatment. The catalyst has high activity and selectivity and good stability in hydrogenation reaction of organic compounds containing carbonyl.

Description

technical field [0001] The invention relates to a carbon-supported noble metal catalyst and a preparation method thereof, more specifically to a carbon-supported palladium-ruthenium two-component noble metal catalyst and a preparation method thereof. Background technique [0002] Catalysts supported by noble metals of group VIII in the periodic table on substrate materials have high activity and can be used in various reactions. Palladium, platinum, and ruthenium supported catalysts are widely used in various organic compounds, such as hydrogenation of alkynes to olefins, hydrogenation of aromatics, hydrogenation of aldehydes to alcohols, alkylation, etc., especially in the preparation of caprolactam in the chemical fiber industry In the SNIA process, the terephthalic acid process in the polyester industry, and the preparation of hydrogen peroxide, the amount of precious metal catalysts is large. [0003] At present, the preparation technology of Pd / C catalyst still mainly ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/46B01J23/44B01J21/18C07C51/36C07C61/08
Inventor 张晓昕孟祥堃王宣宗保宁慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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