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A kind of method for preparing cyclohexylbenzene by selective hydrogenation of biphenyl

A technology of cyclohexylbenzene and selectivity, which is applied in the field of preparation of cyclohexylbenzene, can solve the problems of cumbersome production process, difficult industrial operation, expensive catalyst, etc., and achieve the effect of low equipment requirements and mild reaction conditions

Active Publication Date: 2020-06-16
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The biphenyl selective hydrogenation method has a higher yield than the first two methods, but still faces the disadvantages of expensive catalyst, cumbersome production process, and difficult industrial operation.

Method used

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  • A kind of method for preparing cyclohexylbenzene by selective hydrogenation of biphenyl

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Experimental program
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Embodiment 1

[0026] Take 17.65g of ammonium molybdate (0.1molMo), 58.162g of nickel nitrate (0.2molNi), 12.08g of copper nitrate (0.05molCu), and 100ml of ammonia water into the high-pressure hydrothermal reactor, react at 150°C for 5h, turn on the high-pressure hydrothermal Reactor, take out the product, filter, wash with water, and dry in an oven at 120°C for 12 hours. Calcination was carried out under a nitrogen atmosphere, the temperature was raised at a rate of 10°C / min, and calcined at 350°C to obtain a Ni-Mo-Cu composite oxide. Take a certain amount of Ni-Mo-Cu composite oxide and mix it with aluminum sol, and the metal content is 90% based on the metal oxide, and make a paste, knead and extrude to make a strip with a diameter of 1.6mm. After drying for 5 hours under the infrared lamp, put it in an oven and dry it at 120°C for 5 hours, then bake it in a muffle furnace at 400°C for 5 hours to prepare the Ni-Mo-Cu oxidation state catalyst, and put the oxidation state metal catalyst in...

Embodiment 2

[0028]Get the ammonium molybdate (0.1molMo) of 17.65g, 58.16g nickel nitrate (0.2molNi), 12.08g copper nitrate (0.05molCu), 4.29g zirconium nitrate (0.01molZr), 100ml ammoniacal liquor joins in the high pressure hydrothermal reaction kettle, React at 150°C for 5 hours, open the high-pressure hydrothermal reaction kettle, take out the product, filter it, wash it with water, and dry it in an oven at 120°C for 12 hours. Calcination was carried out under a nitrogen atmosphere, the temperature was raised at a rate of 10°C / min, and calcined at 350°C to obtain a Ni-Mo-Cu composite oxide. Take a certain amount of Ni-Mo-Cu composite oxide and mix it with aluminum sol, and the metal content is 90% based on the metal oxide, and make a paste, knead and extrude to make a strip with a diameter of 1.6mm. After drying under the infrared lamp for 5 hours, put it in an oven and dry it at 120°C for 5 hours, and then bake it in a muffle furnace at 400°C for 5 hours to prepare the Ni-Mo-Cu-Zr oxid...

Embodiment 3

[0030] Take 35.3g of ammonium molybdate (0.2molMo), 87.24g of nickel nitrate (0.3molNi), 12.08g of copper nitrate (0.05molCu), and 120ml of ammonia water into the high-pressure hydrothermal reactor, react at 150°C for 5h, turn on the high-pressure hydrothermal Reactor, take out the product, filter, wash with water, and dry in an oven at 120°C for 12 hours. Calcination was carried out under a nitrogen atmosphere, the temperature was raised at a rate of 10°C / min, and calcined at 350°C to obtain a Ni-Mo-Cu composite oxide. Take a certain amount of Ni-Mo-Cu composite oxide and mix it with aluminum sol, and the metal content is 90% based on the metal oxide, and make a paste, knead and extrude to make a strip with a diameter of 1.6mm. After drying for 5 hours under the infrared lamp, put it in an oven and dry it at 120°C for 5 hours, then bake it in a muffle furnace at 400°C for 5 hours to prepare the Ni-Mo-Cu oxidation state catalyst, and put the oxidation state metal catalyst in t...

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Abstract

The invention relates to a catalyst and a method for preparing cyclohexyl benzene by means of biphenyl selective hydrogenation. The method comprises the steps of firstly, preparing a molybdenum-containing compound, a nickel-containing compound, a copper-containing compound, deionized water, ammonia water and auxiliary agents into a mixed solution; synthesizing a nickel-copper-ammonium molybdate oxidation state metal catalyst in a high pressure kettle, partly reducing the obtained catalyst into a reduced catalyst in a steady state fixed bed continuous reactor, and carrying out biphenyl selective hydrogenation under the conditions that the temperature is 50-90 DEG C, the pressure is 1-4MPa and the liquid hourly volume space velocity is 1-10h<-1> so as to obtain the cyclohexyl benzene. After the method is adopted, the conversion rate of biphenyl reaches up to 98% or above, and the selectivity of the cyclohexyl benzene reaches 97% or above; the catalyst prepared by the method is high in activity, mild in reaction conditions and high in cyclohexyl benzene selectivity, can resist sulfur poisoning, and has long running life, thus being very suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of cyclohexylbenzene, in particular to a catalyst and a method for preparing cyclohexylbenzene by selective hydrogenation of biphenyl. Background technique [0002] Cyclohexylbenzene is an important chemical intermediate, a high-boiling solvent for the preparation of coatings, plastics and adhesives, and has special physical and chemical properties. Cyclohexylbenzene can be oxidized to produce phenol and cyclohexanone. Phenol is an important chemical raw material, and cyclohexanone is an intermediate for the production of caprolactam and nylon. Cyclohexylbenzene can also be used as a raw material for synthesizing TFT liquid crystal materials and as an additive for the electrolyte of lithium-ion secondary batteries, and has anti-overcharge performance. [0003] There are currently three synthesis routes for cyclohexylbenzene: benzene hydroalkylation method; benzene and styrene alkylation method; biphenyl se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/885B01J23/887B01J23/889B01J37/03B01J37/08C07C5/10C07C13/28
CPCB01J23/002B01J23/885B01J23/8873B01J23/8898B01J37/031B01J37/088B01J2523/00C07C5/10C07C13/28B01J2523/17B01J2523/68B01J2523/847B01J2523/48B01J2523/27Y02P20/52
Inventor 殷长龙程思雨刘晨光赵会吉刘宾刘东柴永明柳云骐赵瑞玉张孔远
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)