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Preparation method and application of tetrakis(pentafluorophenyl)iron porphyrin immobilized on zinc oxide

A technology of pentafluorophenyl and iron porphyrin, which is applied in the field of preparation of zinc oxide immobilized tetrairon porphyrin, can solve the problems of low conversion rate and low recycling efficiency of metal porphyrin per unit mass, and achieve good catalytic activity Effect

Inactive Publication Date: 2011-12-28
GUANGXI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of zinc oxide immobilized tetrakis(pentafluorophenyl)iron porphyrin and its application. This immobilized catalyst has the ability of efficiently reusing catalytic molecular oxygen to oxidize cyclohexane, and has high The conversion rate of cyclohexane overcomes the problems of low conversion rate and low recycling efficiency per unit mass of metalloporphyrin in the current process of catalytic molecular oxygen oxidation of cyclohexane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A preparation method for zinc oxide immobilized tetrakis(pentafluorophenyl)iron porphyrin: take 35g ZnSO 4 ·7H 2 O was dissolved in 100mL deionized water, adjusted to pH=8 with 0.2M sodium hydroxide solution, and the newly prepared Zn(OH) 2 precipitation. Then the precipitate was transferred to a three-necked bottle with 200 mL of organic solvent, and under electric stirring at 600 rpm, 10 mg of tetrakis(pentafluorophenyl)iron porphyrin dissolved in 25 mL of organic solvent was added, kept at 65 to 75° C. Stir continuously for 5-7 hours, remove the organic solvent by distillation under reduced pressure, wash with deionized water and suction filter, and dry the filter cake in vacuum at 120-170°C for 5-8 hours to obtain zinc oxide immobilized tetrakis(pentafluorophenyl ) iron porphyrin catalyst.

Embodiment 2

[0016] The method of using zinc oxide immobilized tetrakis(pentafluorophenyl)iron porphyrin: put 1.0mg tetrakis(pentafluorophenyl)iron porphyrin equivalent zinc oxide immobilized catalyst into a 500ml reaction kettle, add 200ml cyclohexane , the stirring speed is 200 rpm, the reaction time is 4.0h, the reaction pressure is 0.8MPa, and the reaction temperature is 150°C, a sample is taken every half an hour, and the qualitative and GC gas chromatography standard method, combined with chemical titration method to quantitatively measure the molar percentage of each product, the conversion rate of cyclohexane is 44.3%, the ketone alcohol selectivity is 46.2%, and the catalyst conversion number is 8.8×10 5 , the yield of alcohol and ketone was 20.5%.

[0017] When the reaction temperature was 145°C, the conversion rate of cyclohexane was 37.5%, the ketone alcohol selectivity was 47.3%, and the catalyst conversion number was 7.6×10 5 , The yield of alcohol and ketone was 17.7%.

[...

Embodiment 3

[0021] The method of using zinc oxide immobilized tetrakis(pentafluorophenyl)iron porphyrin: put 1.0mg tetrakis(pentafluorophenyl)iron porphyrin equivalent zinc oxide immobilized catalyst into a 500ml reaction kettle, add 200ml cyclohexane , the stirring speed is 200 rpm, the reaction time is 4.0h, the reaction temperature is 150°C, and the reaction pressure is 0.9MPa, the conversion rate of cyclohexane is 31.1%, the ketone alcohol selectivity is 50.8%, and the conversion number is 6.3 ×10 5 , the yield of alcohol and ketone was 15.8%.

[0022] When the reaction pressure was 0.7MPa, the conversion rate of cyclohexane was 37.9%, the selectivity of ketone alcohol was 57.8%, and the catalyst conversion number was 7.8×10 5 , the yield of alcohol and ketone was 21.9%.

[0023] When the reaction pressure was 0.6MPa, the conversion rate of cyclohexane was 33.2%, the ketone alcohol selectivity was 60.3%, and the catalyst conversion number was 6.9×10 5 , the yield of alcohol and ket...

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Abstract

A preparation method of zinc oxide solid borne tetra (pentafiuorophenyl) ferriporphyrin. The method comprises steps of: carrying out mechanical stirring on newly prepared Zn(OH)2 to disperse in a certain amount of organic solvent; adding organic solvent dissolved tetra (pentafiuorophenyl) ferriporphyrin, maintaining at 65-75DEG C, and stirring for 5-7h; depriving the organic solvent by a reduced pressure distillation; carrying out a pumping filtration and washing; drying a filter cake in 120-170 DEG C vacuum for 5-8h to obtain the zinc oxide solid borne tetra (pentafiuorophenyl) ferriporphyrin. 1.0mg tetra (pentafiuorophenyl) ferriporphyrin equivalent weight of zinc oxide solid borne tetra (pentafiuorophenyl) ferriporphyrin catalyses oxygen to oxidize cyclohexane under a pressure of 0.7MPa, a reaction temperature of 150 DEG C for 4h; and an average cyclohexane conversion rate is 34.2%; an average selectivity is 57.5%; and an average yield of a main oxidized product is 19.7%. Besides, the catalyst can be repeatedly use for more than 10 times.

Description

technical field [0001] The invention relates to a method for preparing zinc oxide-immobilized tetrakis(pentafluorophenyl)iron porphyrin, which is prepared by using zinc oxide-immobilized tetrakis(pentafluorophenyl)iron porphyrin as a catalyst to catalyze the oxidation of cyclohexane with oxygen Process for cyclohexanone and cyclohexanol. Background technique [0002] In today's industry, cyclohexanone and cyclohexanol, commonly known as K / A oil, are the main intermediates for the preparation of caprolactam and adipic acid, which can then be used to synthesize nylon-6 and nylon-66, and are also important organic chemical raw materials. The oxidation of cyclohexane to prepare cyclohexanol and cyclohexanone is an important organic synthesis reaction. There are many methods for catalyzing the oxidation of cyclohexane, some of which are also very effective. However, in the past 50 years, countries have mainly competed to improve the method of DuPont of the United States, formin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26C07C27/12C07C35/08C07C29/50C07C49/403C07C45/33
Inventor 黄冠曹轩沈莉郭勇安周红
Owner GUANGXI UNIV
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