Method for refining biphenyl by hydrogenating industry fluorene oxide in normal pressure hydrogen

An industrial oxygen fluorene and hydrorefining technology, applied in chemical instruments and methods, hydrocarbons, hydrocarbons, etc., can solve the problems of increasing equipment costs and product separation difficulties, achieving simple process, reducing equipment costs and operation. cost effect

Inactive Publication Date: 2019-03-08
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although in order to achieve a better reaction effect, there are still a small amount of by-products and unconverted

Method used

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  • Method for refining biphenyl by hydrogenating industry fluorene oxide in normal pressure hydrogen
  • Method for refining biphenyl by hydrogenating industry fluorene oxide in normal pressure hydrogen
  • Method for refining biphenyl by hydrogenating industry fluorene oxide in normal pressure hydrogen

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1: MoO 3 Synthesis method: Mix a certain amount of ammonium molybdate aqueous solution with melamine aqueous solution, the solution becomes turbid, and then filter, and the obtained filter cake is heated up to 500°C at 2°C / min in the air, kept at constant temperature for 4 hours, cooled naturally, and set aside. Mo 2 N synthesis method: a certain amount of MoO 3 in N 2 / H 2 Nitriding is carried out under the atmosphere, the specific ammoniation process: 1 ℃ / min from room temperature to 800 ℃, constant temperature for 6 hours, natural cooling to room temperature, passivation treatment. Pt / MoO 3 , Pt / Mo 2 N. Co / MoO 3 、Co / Mo 2 N. Ni / MoO 3 and Ni / Mo 2 Synthesis method of N catalyst: the obtained catalyst is dried, calcined, and then reduced for later use by using a common impregnation method.

Embodiment 2

[0023] Example two: 3Co / MoO prepared in Example 1 3 It is a fixed bed hydrogenation catalyst. Investigate the effect of temperature on the reaction results. Biphenyl (BP), see reaction result in table 1 below.

[0024]

[0025] It can be known from Table 1 that the increase of temperature is beneficial to the conversion of DBF, and the selectivity of BP remains 100% regardless of temperature.

Embodiment 3

[0026] Embodiment three: 3Ni / MoO prepared with embodiment 1 3 It is a fixed bed hydrogenation catalyst. Investigate the effect of temperature on the reaction results. Biphenyl (BP), cyclohexylbenzene (CHB) see the reaction results in Table 2 below.

[0027]

[0028] It is known from Table 2 that the increase of temperature is beneficial to the conversion of DBF, and the selectivity of BP increases with the increase of temperature. Therefore, high temperature is beneficial to increase the yield of BP.

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Abstract

The invention discloses a method for refining biphenyl by hydrogenating industry fluorene oxide in normal pressure hydrogen, and belongs to the technical field of fine chemical synthesis. The used catalyst has high activity to fluorene oxide hydrogenation and high selectivity to biphenyl; the fluorene oxide conversion rate reaches 100 percent; the biphenyl selectivity reaches 100 percent; and purebiphenyl is obtained by a one-step method. The heated raw material liquid enters a circulating catalyst bed under the driving of the normal pressure hydrogen. The catalyst is fully mixed with the hydrogen in a pre-raising section, and is partially reduced. After the reaction of the raw materials is completed in a raising pipe, a reaction product and a solvent enter an evaporator; and the separated solvent continues circulating, and the biphenyl is obtained at the bottom of a tower. The catalyst enters a regenerator from a precipitator under the action of gravity, and is regenerated through air or ammonia gas; and the regenerated catalyst enters a reaction device to achieve catalyst circulating. The catalyst provided by the invention has the characteristics of high activity to the fluoreneoxide, high selectivity to the biphenyl, easiness in regeneration and the like; the process is simple; the equipment and operation cost is greatly reduced; and the method has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a method for refining biphenyl by hydrogenation of industrial fluorene under atmospheric pressure hydrogen. Background technique [0002] Biphenyl (BP) is a very important compound widely used in medicine, pesticides, dyes, and preservatives. Plasticizers and other fields, has a very broad prospects for development. With the continuous development of the biphenyl synthesis process in the direction of cleanliness, low cost and high yield, the demand for biphenyl in the international and domestic markets is increasing year by year, especially the domestic biphenyl market is far short of supply, and most of the biphenyl relies on imports . The gap in the domestic market is large and has a good market prospect, which brings opportunities for the development of the biphenyl industry. Dibenzofuran, also known as dibenzofuran (DBF), is a basic coal tar sep...

Claims

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Application Information

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IPC IPC(8): C07C1/247C07C15/14
CPCC07C1/247C07C2523/652C07C2523/882C07C2523/883C07C2527/24C07C15/14Y02P20/584
Inventor 梁长海张洁李闯殷冬冬关伟翔
Owner DALIAN UNIV OF TECH
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