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Method for preparing o-phenylphenol through dibenzofuran reduction

A technology of o-phenylphenol and oxyfluorene, which is applied in the field of preparation of o-phenylphenol by reduction of oxyfluorene, can solve the problems of low catalyst service life, high investment, and poor economy

Pending Publication Date: 2022-07-29
中化国际新材料(河北)有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above-mentioned processes all use solvents and the concentration of oxyfluorene is low, which requires large energy consumption and high investment, or the service life of the catalyst is relatively low, and the economy is poor, which affects the prospect of industrialization
In the prior art, acid-base treatment is often used to separate OPP products, but the separation efficiency of the technology used is low and the amount of wastewater generated is large

Method used

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  • Method for preparing o-phenylphenol through dibenzofuran reduction
  • Method for preparing o-phenylphenol through dibenzofuran reduction

Examples

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Effect test

preparation example Construction

[0048] The method for preparing o-phenylphenol of the present invention comprises hydrogenating oxyfluorene in the presence of a catalyst, the catalyst comprises a carrier and an active component, and the carrier comprises α-Al 2 O 3 and MgO, the active components include one or more of platinum, palladium and rhodium.

[0049] In the present invention, the carrier has the conventional meaning in the art, and is the support of the active components in the catalyst. The present invention uses alumina of specific crystal form—α-Al 2 O 3 for the carrier core, in α-Al 2 O 3 The surface is coated with alkaline oxide to form an alkaline composite carrier with low specific surface area, and then the active metal is supported on this composite carrier. The utilization efficiency of the catalyst reduces the loading of precious metal components, is also conducive to the diffusion of reaction products, improves the OPP selectivity, and reduces the catalyst cost. The catalyst used i...

preparation example 1

[0081] Preparation Example 1: Catalyst Preparation

[0082] Take 100g of strip α-Al with a diameter of 3mm 2 O 3 Put it into the sugar-coating machine, the speed of the sugar-coating machine is 30r / min, and slowly spray 110g of magnesium nitrate aqueous solution with a magnesium nitrate mass fraction of 32% onto the surface of the carrier. During the whole spraying process, the sugar-coating machine is blasted and kept at 50 ℃ air temperature , after the spraying of the magnesium nitrate solution is completed, take out the carrier, dry it at 100 °C for 5 h, put the dried sample into the muffle furnace for calcination, and raise the temperature from room temperature to 600 °C at a heating rate of 5 °C / min, and then put it in a muffle furnace. Roast at 600°C for 5 hours, take out the carrier, put the carrier into the sugar coating machine, the sugar coating machine rotates at 30r / min, and spray 110g of magnesium nitrate aqueous solution with a mass fraction of 32% on the carrie...

Embodiment 1-5

[0085] Activation of the catalyst: 100 g of the catalyst prepared in Preparation Example 1 was filled into the fixed bed, and hydrogen was introduced into it. The hydrogen flow rate was 8 L / min, and the set pressure was 1.2 MPa, and the catalyst was raised to 400 ° C at a heating rate of 5 ° C / min. , at 400 °C for 4 hours to activate the catalyst.

[0086] Reaction process: as figure 2 As shown in the schematic flow chart of , the oxyfluorene toluene solution (Example 1-4) or pure oxyfluorene (Example 5) with different oxyfluorene concentrations (20%-80%) is pumped into the preheater for gasification by the liquid feed pump, It is mixed with hydrogen, and after heating, it enters the fixed-bed reactor for catalytic reaction. The reaction conditions are: the mass space velocity of oxyfluorene (the mass flow rate of oxyfluorene / catalyst mass) is 0.8h -1 , the hydrogen flow rate satisfies that the ratio of hydrogen mass to oxygen fluorene mass is 0.4, the fixed bed catalytic re...

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Abstract

The present invention provides a method for preparing o-phenylphenol, the method comprises that dibenzofuran is subjected to a hydrogenation reaction in the presence of a catalyst, the catalyst comprises a carrier and an active component playing a catalytic role, the carrier comprises alpha-Al2O3 and MgO, and the active component comprises one or more of a platinum element, a palladium element and a rhodium element. According to the method disclosed by the invention, high-concentration dibenzofuran can be used as a raw material, so that the energy consumption is greatly reduced, and the reaction conversion rate of dibenzofuran and the selectivity of o-phenylphenol are not reduced. The catalyst used in the method disclosed by the invention can stably run for more than 4000 hours, has industrial conditions and is high in economic value.

Description

technical field [0001] The invention belongs to the field of preparation of o-phenylphenol, and in particular relates to a method for preparing o-phenylphenol by reduction of oxyfluorene. Background technique [0002] Ortho-phenylphenol (OPP) is a widely used fine chemical. In recent years, a new type of OPP production method, the oxyfluorene reduction method, has been reported. Although this method has no industrial production practice, it has broad application prospects. Oxyfluorene is an important component in the washing oil, accounting for about 5%-10% of the quality of the washing oil. The washing oil comes from the coal tar 230℃-300℃ distillation section, which accounts for about 4.5%-10% of the coal tar quality. my country is rich in coal resources, and the supply of washing oil is large, and there is a large space for OPP production with oxygen fluorene as raw material. [0003] CN108947775A discloses an oxyfluorene hydrogenation process using a reactive distilla...

Claims

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Application Information

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IPC IPC(8): C07C37/055C07C39/15B01J23/42
CPCC07C37/055B01J23/42B01J23/002C07C39/15
Inventor 谢志强相东商建胡帅珂李永刚吴鹏罗致远
Owner 中化国际新材料(河北)有限公司
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