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A kind of metal catalyst and preparation method and application

A technology for the preparation of metal catalysts and hydrogen, which is applied in the direction of metal/metal oxide/metal hydroxide catalysts, carbon-based compound preparation, chemical instruments and methods, etc., to achieve the effects of mild preparation conditions, good catalytic performance, and uniform distribution

Active Publication Date: 2016-05-04
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the direct selective hydrogenation of phenol to cyclohexanone under mild conditions remains a challenge.

Method used

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  • A kind of metal catalyst and preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1) Activated carbon pretreatment: put the coconut shell activated carbon that has been washed and boiled 2 to 3 times in a nitric acid solution with a mass fraction of 10.94%, heat and reflux in a water bath at ~60°C for 4 hours, filter with deionized water, and wash to pH It is neutral, and dried at 110°C for 12 hours to obtain oxidized modified activated carbon;

[0058] 2) TiO loaded by sol-gel method 2 : Configure solution A and solution B, under the condition of magnetic stirring, slowly add B to solution A drop by drop to form mixed solution C sol, disperse 12.03g of modified activated carbon obtained in step 1) into solution C, add concentrated HNO 3 (66-68% by mass) to adjust the pH to 3, stir for 5-10 minutes, and then ultrasonically oscillate for 10 minutes to make the sol enter the AC channel, stop stirring and let stand to form a gel, dry at 80°C for 12h, and calcinate at 500°C for 2h to obtain TiO 2 Composite carrier material TiO with a loading of 9.95% ...

Embodiment 2

[0062] TiO by sol-gel method 2 Loaded on the modified activated carbon to obtain the composite carrier TiO 2 / AC. Then use the method of photocatalytic reduction to load metal palladium onto the composite carrier TiO 2 / AC, after subsequent filtration, washing, and drying processes, PdTiO 2 / AC.

[0063] The specific implementation process is the same as in Example 1, except that HNO 3 The concentration is 11.13% by mass, the composite carrier TiO 2 TiO in / AC 2 The content is 9.89% by mass, the catalyst PdTiO 2 The content of palladium in / AC was 0.5% by mass.

[0064] 4) Photocatalytic reduction of loaded Au: take the PdTiO prepared in step 3) 2 / AC Catalyst TiO 2 / AC composite carrier material 5.316g, stirring and dispersing in 300ml ultrapure water, adding 10ml of methanol, stirring in the dark for 10min, then adding 2.21ml of the prepared chloroauric acid solution, the content of chloroauric acid is 20g / L, and the content of chloroauric acid is 37 Mass% concentr...

Embodiment 3

[0066] With embodiment 1, different is that composite carrier TiO 2 TiO in / AC 2 The mass content is 15%, the catalyst PdTiO 2 The mass content of Pd in ​​ / AC is 0.916%.

[0067] 4) Photocatalytic reduction of loaded Au: take the PdTiO prepared in step 3) 2 / AC Catalyst TiO 2 / AC composite carrier material 5.316g, stirred and dispersed in 300ml ultrapure water, added 10ml of methanol, stirred in the dark for 10min, then added 1.21ml of prepared chloroauric acid solution, the content of chloroauric acid was 20g / L, with 37% Adjust the pH to 3-5 with concentrated hydrochloric acid, stir rapidly in the dark for 1h, then place under 15w ultraviolet light for 5h, filter and wash until the filtrate is neutral, and dry at 90°C for 12h to obtain Au-PdTiO 2 / AC catalyst, the mass fraction of palladium is 0.916%, and the mass fraction of Au is 0.5%.

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Abstract

The invention relates to a metal catalyst which comprises: 1) a nano TiO2 modified porous material as a composite carrier, and 2) a nano particle of at least one out of Pd and other transition metals as an active component, wherein the active component and TiO2 in the composite carrier have strong metal-carrier interaction to form a Pd@TiO2 structure or a Pd-M@TiO2 structure, thereby forming the Pd-M@TiO2 / porous carrier catalyst, and M is at least one out of the transition metals except Pd. The invention further relates to a preparation method of the catalyst, and an application of the catalyst in preparing cyclohexanone through selective phenol hydrogenation.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a metal catalyst and its preparation method and application, in particular to the application of the catalyst in the selective hydrogenation of phenol to prepare cyclohexanone. Background technique [0002] The supported nano-noble metal catalyst has good hydrogenation performance, and is used in the catalytic hydrogenation of various unsaturated organic compounds in petrochemical, pharmaceutical, dye, pesticide and other industries. As a hydrogenation catalyst with excellent performance, nano-palladium catalyst is often used in the selective hydrogenation of alkenes, nitro groups, nitroso groups, ketones, aldehydes, etc., and occupies an extremely important position in the chemical industry. It is generally believed that a supported nano-palladium catalyst with excellent performance should have the following characteristics in structure: 1) The palladium microcrystalline particles of th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/52C07C45/00C07C49/403
Inventor 周继承司家奇欧阳文兵
Owner XIANGTAN UNIV
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