Catalyst for one-step preparing cyclohexanone by hydrogenation of water phase phenol, and its preparation method

A technology of phase phenol and catalyst is applied in the field of one-step preparation of cyclohexanone by hydrogenation of aqueous phenol, and achieves the effects of simple separation, high activity and high specific surface area

Inactive Publication Date: 2013-07-24
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above results show that it is still a challenge to achieve high conversion of phenol while obtaining high selectivity to cyclohexanone in an environmentally friendly medium under the condition of easy operation at low temperature and atmospheric pressure.

Method used

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  • Catalyst for one-step preparing cyclohexanone by hydrogenation of water phase phenol, and its preparation method
  • Catalyst for one-step preparing cyclohexanone by hydrogenation of water phase phenol, and its preparation method
  • Catalyst for one-step preparing cyclohexanone by hydrogenation of water phase phenol, and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1-4

[0030] The metal-organic framework (MOF) used in the following examples can be prepared according to the following examples 1-4:

Embodiment 1

[0032] Cr(NO 3 ) 3 9H 2 O, HF and terephthalic acid were added to deionized water at a molar ratio of 1:1:1, and the aqueous solution was transferred to a polytetrafluoroethylene-lined hydrothermal reactor, and reacted at 220 °C for 8 h. Cool to room temperature at a cooling rate of 0.16°C / min and then filter to obtain a green powder. Then soak the powder in 95% by mass ethanol, place it at 80° C. for 24 hours, and finally vacuum-dry it at 150° C. for 10 hours to obtain an activated metal-organic framework (MOF). After testing, the MOF material has a very high comparison area (S BET ≈3000m 2 / g) and a large pore structure with a large number of Lewis acid sites (about 2000 μmol g -1 ), and has good thermal stability and good chemical stability.

Embodiment 2

[0034] Cr(NO 3 ) 3 9H 2 O, HF and terephthalic acid were added to deionized water at a molar ratio of 1:1:0.75, and the aqueous solution was transferred to a polytetrafluoroethylene-lined hydrothermal reactor, and reacted at 210°C for 9h. Cool to room temperature at a cooling rate of 0.2°C / min and then filter to obtain a green powder. Then soak the powder in 95% by mass ethanol, place it at 80° C. for 24 hours, and finally vacuum-dry it at 150° C. for 10 hours to obtain an activated metal-organic framework (MOF).

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Abstract

The invention discloses a catalyst for one-step preparing cyclohexanone by hydrogenation of water phase phenol, and its preparation method. The preparation method comprises the following steps: adding Cr(NO3)3.9H2O, HF and terephthalic acid into deionized water, then adding into a hydrothermal reaction vessel to react for 7-9 hours at the temperature of 210 DEG C-230 DEG C; cooling to the room temperature and filtering, vacuum drying to obtain an activated organometallic framework structure material; taking the framework structure as a carrier, loading the reduction state metal Pd nano particles to obtain a catalyst for one-step preparing cyclohexanone by hydrogenation of water phase phenol; the catalyst possesses two functions of Lewis acid sites and hydrogenation active sites. The preparation method of the invention has the characteristics of environmental protection, mild reaction condition, high activity and selectivity, good stability, simple products separation and the like. Thepreparation method for the catalyst is simple, and a reaction solution and the catalyst are easy to separate.

Description

technical field [0001] The invention relates to the field of metal catalyst preparation and the technical field of liquid-phase hydrogenation, in particular to a method for preparing cyclohexanone in one step by hydrogenating phenol in water phase and a catalyst thereof. Background technique [0002] Cyclohexanone is a widely used chemical raw material, mainly used to prepare synthetic fibers nylon 6, nylon 66 and caprolactam, and can also be used as an important intermediate of fine chemicals such as medicine, coatings and dyes. The current industrial preparation method of cyclohexanone generally involves cyclohexane oxidation (Y.Wang, J.S.Zhang, X.C.Wang, M.Antonietti, H.R.Li, "Boron-and Fluorine-Containing Mesoporous Carbon Nitride Polymers: Metal-Free Catalysts for Cyclohexane Oxidation", Angew.Chem., Int.Ed.2010, 49, 3356) and phenol hydrogenation (P.Claus, H.Berndt, C.Mohr, J.Radnik, E.Shin, M.A.Keane, "Pd / MgO: Catalyst Characterization and Phenol Hydrogenation Activ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J35/10C07C49/403C07C45/00
Inventor 李映伟刘宏利
Owner SOUTH CHINA UNIV OF TECH
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