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Method for selective hydrogenation of phenol on Na-modified NiCo catalyst

A technology for selective hydrogenation and catalyst, applied in the field of catalysis, which can solve the problems of low conversion rate and long reaction time.

Active Publication Date: 2021-09-07
NORTHEAST GASOLINEEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for the selective hydrogenation of phenol on a Na-modified NiCo catalyst. This Na-modified NiCo catalyst and its catalytic reaction system provide a method for the efficient hydrogenation of phenol to cyclohexanol, which is used to solve the problem Problems of low conversion rate and long reaction time of phenol hydrogenation to cyclohexanol catalyst in prior art

Method used

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  • Method for selective hydrogenation of phenol on Na-modified NiCo catalyst
  • Method for selective hydrogenation of phenol on Na-modified NiCo catalyst
  • Method for selective hydrogenation of phenol on Na-modified NiCo catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0036] This Na-modified NiCo catalyst was prepared by the following method:

[0037] 1) Preparation of catalyst precursor Na-NiCo@C:

[0038] The synthetic route of Na-NiCo@C-Surf catalyst is as follows figure 1 As shown, the catalyst precursor Na-NiCo@C was first synthesized as follows:

[0039] Soak Na-NiCo-MOF-74 in ethanol solution at room temperature for 8 hours to remove surface residues, filter with suction, wash alternately with ethanol and water for 6 times, and dry in vacuum at 60°C for 18 hours to obtain pure Na-NiCo-MOF -74. Put pure Na-NiCo-MOF-74 in a tube furnace and pyrolyze it in an argon atmosphere. The temperature is raised from room temperature to 500 °C at a rate of 3 °C / min, kept at this temperature for 2 hours, and then dropped to room temperature , to obtain the carbon-coated nanoscale metal catalyst precursor Na-NiCo@C.

[0040] Wherein the preparation of Na-NiCo-MOF-74:

[0041] Add nickel acetate and cobalt acetate to distilled water to prepare ...

Embodiment 2

[0049] This Na-modified NiCo catalyst was prepared by the following method:

[0050] 1) Preparation of catalyst precursor Na-NiCo@C:

[0051] Soak Na-NiCo-MOF-74 in ethanol solution at room temperature for 24 hours to remove surface residues, filter with suction, wash with ethanol and water alternately 4 times, and dry in vacuum at 120°C for 8 hours to obtain pure Na-NiCo-MOF -74. Put pure Na-NiCo-MOF-74 in a tube furnace and pyrolyze it in an argon atmosphere. The temperature is raised from room temperature to 400 °C at a rate of 3 °C / min, kept at this temperature for 3 hours, and then dropped to room temperature , to obtain the carbon-coated nanoscale metal catalyst precursor Na-NiCo@C.

[0052] Wherein the preparation of Na-NiCo-MOF-74:

[0053] Add nickel acetate and cobalt acetate to distilled water to prepare a solution with a total metal salt concentration of 0.10 mol / L, wherein the molar ratio of nickel acetate and cobalt acetate is 1:4; add 2,5-dihydroxyterephthali...

Embodiment 3

[0059] This Na-modified NiCo catalyst was prepared by the following method:

[0060] 1) Preparation of catalyst precursor Na-NiCo@C:

[0061]At room temperature, the molar ratio of nickel and cobalt is 1:1.5, and the ratio of the molar weight of 2-hydroxypropane-1,2,3-tricarboxylic acid sodium to the total molar weight of the two metal salts is 1.5:7. -MOF-74 was soaked in ethanol solution for 16 hours to remove surface residues, filtered with suction, washed alternately with ethanol and water for 3 times, and dried in vacuum at 120°C for 8 hours to obtain pure Na-NiCo-MOF-74. Pure Na-NiCo-MOF-74 was placed in a tube furnace and pyrolyzed in an argon atmosphere. The temperature was raised from room temperature to 450 °C at a rate of 3 °C / min, kept at this temperature for 3 hours, and then dropped to room temperature , to obtain the carbon-coated nanoscale metal catalyst precursor Na-NiCo@C.

[0062] 2) Preparation of Na-NiCo@C-Surf catalyst:

[0063] Soak the obtained Na-Ni...

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Abstract

The invention relates to a method for selective hydrogenation of phenol on a Na-modified NiCo catalyst, which comprises the following steps: (1) by taking Na-NiCo-MOF-74 as a precursor, carrying out alcoholysis, and adjusting and controlling a pyrolysis process at 400-500 DEG C to obtain a carbon-coated nanoscale catalyst precursor Na-NiCo @C; (2) soaking the Na-NiCo@ C in an alcoholic solution, and then treating the Na-NiCo@ C in an NH3 atmosphere to obtain a high-activity surface modified Na-NiCo@ C-Surf catalyst; (3) establishing a catalytic reaction system taking a mixed hydrogen-donor solvent system as a solvent; and (4) completely converting phenol into cyclohexanol at the temperature of 80-120 DEG C under the hydrogen partial pressure of 2-3 MPa for 2-3 hours, and recycling the separated catalyst. On the premise that the phenol conversion rate and the cyclohexanol selectivity are both 100%, the method also has the characteristic of short reaction time.

Description

Technical field: [0001] The invention belongs to the technical field of catalysis, and in particular relates to a method for selective hydrogenation of phenol on a Na-modified NiCo catalyst. Background technique: [0002] Cyclohexanol is an important raw material in the polymerization industry and one of the raw materials for the production of nylon and plasticizers. Cyclohexanol can also be used in the manufacture of plasticizers, surfactants, detergents and emulsion stabilizers, etc., with a wide range of applications. At present, the production processes of cyclohexanol mainly include cyclohexane oxidation and phenol hydrogenation. Among them, although the cost of cyclohexane oxidation is relatively low, the reaction conditions are harsh, the yield is low, and the separation steps are complicated. Compared with the cyclohexane oxidation method, the phenol hydrogenation method has many advantages such as high operational safety, low energy consumption, short process flow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/20C07C35/08B01J23/78
CPCC07C29/20B01J23/78C07C2601/14B01J35/33C07C35/08Y02P20/584
Inventor 宋华王帅李锋陈彦广蒋博龙张春雷
Owner NORTHEAST GASOLINEEUM UNIV
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