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Catalyst for synthesizing fluorenone and preparation method and application thereof

A technology for synthesizing fluorenones and catalysts, which is applied in the field of catalysts for synthesizing fluorenones and its preparation, can solve the problems of difficult separation of catalysts, increased operational complexity, and high cost of catalysts, and achieve remarkable economic efficiency, easy operation, and simple reaction process Effect

Active Publication Date: 2019-05-21
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of catalyst is a homogeneous catalyst, and it is difficult to separate the catalyst after the reaction, which increases the complexity of the operation.
In addition, there are reaction systems using noble metal active component catalysts. For example, Majumdar et al. prepared Au nanoparticles-polydopamine (Pda)-reduced graphene oxide (rGO) ternary nanocomposites, using 1 mmol fluorene as raw material, Au-Pda - The amount of rGO catalyst (Au loading is 2wt%) is 0.02g, and 10mol% of N-hydroxyphthalimide is added at the same time, 5mL of acetonitrile is used as solvent, O 2 The pressure is 10bar, the stirring rate is 1000rpm, and the reaction is carried out at 60°C for 15h. The conversion rate of fluorene is 89.4%, and the selectivity of fluorenone reaches 97.6%. Although noble metals have high catalytic activity as active components, their price Expensive, resulting in higher catalyst costs, which is not conducive to the control of production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Prepare 60wt% cobalt nitrate ethanol solution, slowly add 5wt% citric acid ethanol solution (volume ratio to cobalt nitrate ethanol solution is 5) at 60°C, keep stirring during the process, and continue stirring at 60°C after the dropwise addition 24h, then the solution was stirred at 90°C, the solvent was evaporated to dryness, the obtained product was dried at 150°C for 24h, and calcined at 800°C for 10h to obtain a tricobalt tetroxide catalyst.

[0025] The fluorene oxidation reaction was carried out in a stainless steel reactor, and the reaction conditions were as follows: Dissolve fluorene in cyclohexane (50wt% mass fraction), add a certain amount of catalyst (0.5 mass ratio to fluorenone), and fill the reactor with Inject oxygen, the initial pressure is 6MPa, and react at 180°C for 24h. After the reaction, centrifugation was carried out, and the composition of the product was analyzed by gas chromatography, and the yield of fluorenone was 76%.

Embodiment 2

[0027] Prepare 5wt% copper nitrate ethanol solution, slowly add 5wt% citric acid ethanol solution (volume ratio to copper nitrate ethanol solution is 0.5) at 10°C, keep stirring during the process, continue stirring at 10°C after dropping 2h, then the solution was stirred at 50°C, the solvent was evaporated to dryness, the obtained product was dried at 50°C for 2h, and calcined at 300°C for 1h to obtain a copper oxide catalyst.

[0028] The fluorene oxidation reaction is carried out in a stainless steel reactor, and the reaction conditions are as follows: fluorene is dissolved in cyclohexane (0.01wt% by mass fraction), a certain amount of catalyst is added (the mass ratio to fluorenone is 0.001), and Inflate with oxygen, the initial pressure is 0.1MPa, and react at 60°C for 0.5h. After the reaction, centrifugation was carried out, and the composition of the product was analyzed by gas chromatography, and the yield of fluorenone was 37%.

Embodiment 3

[0030] Prepare 30wt% ethanol solution of cobalt nitrate and copper nitrate, the molar ratio of cobalt to copper is 1:1, and slowly add 30wt% ethanol solution of citric acid (volume ratio to cobalt nitrate and copper nitrate ethanol solution is 2.5) at 35°C Add, keep stirring during the process, continue to stir at 35°C for 12h after the dropwise addition, then stir the solution at 70°C, evaporate the solvent to dryness, dry the obtained product at 100°C for 12h, and calcinate at 550°C for 6h to obtain cobalt copper composite oxide catalyst.

[0031]The fluorene oxidation reaction is carried out in a stainless steel reactor, and the reaction conditions are as follows: fluorene is dissolved in cyclohexane (mass fraction is 25wt%), a certain amount of catalyst is added (the mass ratio of fluorenone is 0.3), and the reactor is filled with Oxygen was introduced, the initial pressure was 3MPa, and the reaction was carried out at 120°C for 12h. After the reaction, centrifugation was...

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Abstract

The invention relates to a catalyst for synthesizing fluorenone and a preparation method and application thereof, and belongs to the technical field of catalysts. The catalyst is prepared from, by mass, 0-100% of tri-cobalt trioxide and 0-100% of copper oxide, and the sum of the mass percentages of the tri-cobalt trioxide and the copper oxide is 100%; the catalyst for synthesizing the fluorenone is prepared by a sol-gel method or a gel method. The catalyst has the advantages of low cost, high conversion rate, high selectivity, mild reaction condition, good stability and easy separation of reactants.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for synthesizing fluorenone, a preparation method and application thereof. Background technique [0002] Fluorenone, molecular formula C 13 h 8 O, with a molecular weight of 180.20, is a yellow orthorhombic crystal, with a melting point of 81-85°C and a boiling point of 341°C. It is insoluble in water but soluble in organic solvents such as alcohol and ether. It is an important fine chemical raw material. As an intermediate, it has extremely important applications in the fields of polymers, dyes, medicines, pesticides, and optical materials. In the field of polymers, fluorenone can be condensed with phenol to form bisphenol fluorene. The structure of bisphenol fluorene has high thermal stability and is widely used in heat-resistant materials, separation membrane materials, etc. Oxygen resin, polycarbonate, polymethyl methacrylate (plexiglass) and other...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/75B01J37/08B01J37/03C07C45/36C07C49/675
Inventor 肖福魁赵宁雒京宣铿蒲彦锋王峰李枫李磊
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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