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Method for preparing o-phenylphenol by direct catalytic hydrogenation of dibenzofuran

A technology for the catalytic hydrogenation of o-phenylphenol, applied in the direction of catalyst activation/preparation, chemical instruments and methods, and the preparation of organic compounds, can solve the large-scale preparation of o-phenylphenol, which cannot be recycled repeatedly, and the utilization of raw materials Insufficient problems, to achieve the effect of improving activity and service life, easy separation and reuse, and high selectivity

Inactive Publication Date: 2020-05-15
RONGCHENG QINGMU CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing synthetic techniques for preparing o-phenylphenol from oxyfluorene as a raw material all have non-continuous and large-scale preparation of o-phenylphenol, and in the production process of o-phenylphenol, raw materials are not fully utilized and cannot be recycled repeatedly. underutilized

Method used

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  • Method for preparing o-phenylphenol by direct catalytic hydrogenation of dibenzofuran
  • Method for preparing o-phenylphenol by direct catalytic hydrogenation of dibenzofuran
  • Method for preparing o-phenylphenol by direct catalytic hydrogenation of dibenzofuran

Examples

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Effect test

Embodiment 1

[0027] Example 1 A preparation method of a modified catalyst for preparing o-phenylphenol by direct catalytic hydrogenation of oxyfluorene

[0028] A method for preparing a modified catalyst for o-phenylphenol by direct catalytic hydrogenation of oxyfluorene, comprising the steps of:

[0029] (1) Catalyst carrier pretreatment: make the specific surface area 200m 2 50g of spherical γ-alumina / g was dried in a constant temperature blast drying oven at 120°C for 4 hours, and then cooled to room temperature;

[0030] (2) Equal volume impregnation: Dissolve 1 g of citric acid and 0.66 g of chloroplatinic acid in 45 g of deionized water to prepare an impregnation solution, slowly pour the impregnation solution into the catalyst carrier that has been dried and cooled to room temperature for equal volume impregnation, and stir After uniformity, put it in the air for 3 hours, put the soaked carrier in a constant temperature blast drying oven at 120°C for 8 hours, and then take it out; ...

Embodiment 2

[0034] Example 2 A preparation method of a modified catalyst for preparing o-phenylphenol by direct catalytic hydrogenation of oxyfluorene

[0035]A method for preparing a modified catalyst for o-phenylphenol by direct catalytic hydrogenation of oxyfluorene, comprising the steps of:

[0036] (1) Catalyst carrier pretreatment: set the specific surface area to 200m 2 50g of spherical γ-alumina / g was dried in a constant temperature blast drying oven at 120°C for 4 hours and then cooled to room temperature;

[0037] (2) Equal-volume impregnation: Dissolve 2.3g of oxalic acid and 1.97g of chloroplatinic acid in 45g of deionized water to prepare an impregnation solution, slowly pour the impregnation solution into the catalyst carrier that has been dried and cooled to room temperature for equal-volume impregnation, and stir evenly After immersing in the air for 2 hours, put the impregnated catalyst carrier in a constant temperature blast drying oven at 120°C for 9 hours and then tak...

Embodiment 3

[0041] Example 3 A preparation method of a modified catalyst for preparing o-phenylphenol by direct catalytic hydrogenation of oxyfluorene

[0042] A method for preparing a modified catalyst for o-phenylphenol by direct catalytic hydrogenation of oxyfluorene, comprising the steps of:

[0043] (1) Catalyst carrier pretreatment: set the specific surface area to 280m 2 50g spherical magnesium oxide / g was placed in a constant temperature blast drying oven at 120°C for 4 hours, then cooled to room temperature;

[0044] (2) Equal-volume impregnation: Dissolve 1.5g of nitric acid and 1.02g of palladium nitrate in 54g of deionized water to prepare an impregnation solution, slowly pour the impregnation solution into the catalyst carrier that has been dried and cooled to room temperature for equal-volume impregnation, and stir evenly Immerse in air for 2 hours, put the impregnated catalyst carrier in a constant temperature blast drying oven at 120°C for 8.5 hours and then take it out; ...

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Abstract

The invention relates to the technical field of compound synthesis, and in particular, relates to a method for preparing o-phenylphenol through direct catalytic hydrogenation of dibenzofuran. The method comprises the steps: filling a fixed bed reactor with a modified catalyst, heating, preheating and evaporating dibenzofuran, uniformly mixing a gas phase with hydrogen, continuously introducing themixture from the upper end of a fixed bed, and continuously receiving a mixed gas which contains a product o-phenylphenol and flows out of the reactor; adding an alkaline aqueous solution into the received mixed gas containing the product o-phenylphenol, and carrying out sufficient stirring, suction filtration and separation, wherein the separated solid is unreacted dibenzofuran, and the separated filtrate is salt containing o-phenylphenol; and adding an acid solution into the separated filtrate, adjusting the pH value to 5-7 to generate a precipitate, carrying out suction filtration, separation and washing on the precipitate, and recrystallizing with a recrystallization solvent to obtain o-phenylphenol. According to the invention, o-phenylphenol can be continuously synthesized, and the method is suitable for large-scale production; the purity of the prepared o-phenylphenol reaches 99.5% or above, and the highest purity can reach 99.73%.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a method for preparing o-phenylphenol by direct catalytic hydrogenation of oxyfluorene. Background technique [0002] O-phenylphenol is an important fine chemical intermediate, which is widely used in the fields of sterilization and anticorrosion, printing and dyeing auxiliaries and surfactants, stabilizers and flame retardants for the synthesis of new plastics, resins and polymer materials. The preparation method of o-phenylphenol is divided into two kinds: separation method and synthesis method. The separation method is mainly separated from the distillation residue of phenol produced by the sulfonation method. The process route of this method is complicated, the operating environment is harsh, and limited by resources, the output of o-phenylphenol produced is limited. This process has been gradually eliminated. There are many processes for preparing o-phenylphenol ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/055C07C39/15B01J23/42B01J23/44B01J23/58B01J37/02B01J37/08B01J37/18
CPCC07C37/055B01J37/0207B01J37/0213B01J37/024B01J37/18B01J37/08B01J23/42B01J23/58B01J23/44
Inventor 刘学松宋丽丽李晓明孙朋波聂孟言
Owner RONGCHENG QINGMU CHEM MATERIALS