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Continuous production method for preparing cyclohexene oxide through cyclohexene oxidation with hydrogen peroxide under normal pressure

A technology for preparing epoxy ring and epoxy cyclohexane from cyclohexene, which is applied in the direction of organic chemistry and the like, can solve the problem of low work efficiency, inability to simplify production processes, save production costs, and realize continuous production, reaction and separation process. and other problems, to achieve the effect of easy operation, mild reaction conditions and simple process

Inactive Publication Date: 2014-06-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0004] The CN1161346C patent of reaction-controlled phase-transfer catalytic cyclohexene oxidation to epoxycyclohexane invented by our research group has been used in the industrial production process, but the production process is a batch reaction with low work efficiency, lengthy reaction and separation process, and cannot meet the requirements Simplify production process, save production cost and realize continuous production

Method used

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  • Continuous production method for preparing cyclohexene oxide through cyclohexene oxidation with hydrogen peroxide under normal pressure
  • Continuous production method for preparing cyclohexene oxide through cyclohexene oxidation with hydrogen peroxide under normal pressure

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Embodiment 1

[0023] Such as figure 1 Shown, 35% hydrogen peroxide feed flow rate is 2kg / h. The feed rate of cyclohexene, solvent and catalyst mixed slurry is 20.5kg / h, the feed flow rate of cyclohexene in the mixed slurry is 5kg / h, the feed flow rate of solvent toluene is 15kg / h, and the feed rate of catalyst is 0.5kg / h;

[0024] The addition amount of polymerization inhibitor 2,6-di-tert-butyl-p-cresol is one hundred thousandth of the addition amount of cyclohexene;

[0025] The volume ratio of the first-stage reactor R1 and the second-stage reactor R2 is 1:2, the volume ratio of the second-stage reactor R2 and the third-stage reactor R3 is 1:1.5, and the volume of the two third-stage reactors The ratio is 1:1;

[0026] After the material enters the first-stage reactor R1 for reaction, the material overflows into the second-stage reactor R2 to continue the reaction, and forms a homogeneous reaction in the second-stage reactor R2. The material overflows into the third-stage reactor R3....

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Abstract

The present invention discloses a continuous production method for preparing cyclohexene oxide through cyclohexene oxidation with hydrogen peroxide under a normal pressure. According to the continuous production method, a reaction part and a separation part are provided, wherein the reaction part reactor comprises two continuous reactors connected in series and two switchable batch reactors connected in parallel, a quaternary ammonium heteropolyphosphatotungstate is adopted as a catalyst, hydrogen peroxide is adopted as an oxidant, preparation of cyclohexene oxide through cyclohexene oxidation is performed under a normal pressure condition, and the separation part is separating an oil phase and a water catalyst mixture through a separator after completing the reaction, wherein the oil phase is subjected to rectification so as to respectively separate the solvent, cyclohexene and cyclohexene oxide, the water catalyst mixture is filtered through a filter to obtain the catalyst, and the water phase is subjected to rectification to separate cyclohexene and cyclohexene oxide contained in the water phase. With the process, the continuous production of cyclohexene oxide through cyclohexene oxidation with phase transfer catalyst catalysis is achieved, and the whole process has characteristics of simpleness, easy operation and mild reaction condition.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and in particular relates to a continuous production process for preparing epoxycyclohexane with hydrogen peroxide as an oxygen source and phosphotungstic heteropolyacid quaternary ammonium salt as a catalyst cyclohexene under normal pressure conditions. technical background [0002] Epoxycyclohexane is an important chemical raw material and intermediate, which has a wide range of uses and can be used in the synthesis of epoxy resins, active agents, pesticides, adhesives, and polymer materials. [0003] Xi Zuwei and others have developed a reaction-controlled phase transfer catalyst, [Reaction-Controlledphase-Transfer Catalysis for Propylene Epoxidation to Propylene Oxide.Science, 2001,292(5519):1139~1141.], which is dissolved in the reaction system during the reaction The characteristics of a homogeneous catalyst, after the end of the reaction, it returns to the initial structure and is pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/04C07D301/12
CPCC07D301/12C07D303/04
Inventor 高爽张毅张恒耘吕迎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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