Method for preparing epoxy cyclohexane through catalytic epoxidation of cyclohexene

Abstract

The invention relates to a method for preparing a fine chemical intermediate, in particular to a method for preparing epoxy cyclohexane through catalytic epoxidation of cyclohexene, which comprises the steps of: taking a synthetic Ti-Si molecular sieve as a catalyst, using an alkaline assistant, controlling the reaction temperature, stirring to react, reacting hydrogen peroxide and the cyclohexene in an organic solvent to obtain epoxy cyclohexane, and then carrying out separation and purification to obtain the epoxy cyclohexane. The reaction time of the invention is between 1 and 48 hours, the single pass conversion rate of the cyclohexene can reach over 40 percent, the selectivity of the epoxy cyclohexane can reach 96 percent, and the utilization rate of the hydrogen peroxide can reach 98 percent. The catalyst can be recovered for repeated use.

Description

technical field [0001] The invention relates to a preparation method of a fine chemical intermediate, in particular to a method for preparing epoxycyclohexane by catalytic epoxidation of cyclohexene. Background technique [0002] Epoxycyclohexane is an important fine chemical intermediate, which has broad application prospects in the fields of pesticides, medicines, and materials. [0003] For example, epoxy cyclohexane reacts with p-tert-butylphenol to generate 2-(4-tert-butylphenoxy)cyclohexanol, and then reacts with thionyl chloride and propynyl alcohol to synthesize high-efficiency, low-toxicity , broad-spectrum, long-lasting, non-teratogenic and carcinogenic organosulfur acaricide clofenac. [0004] Epoxycyclohexane reacts with p-tert-butylphenol, and then hydrogenates to generate 2-(4-tert-butylphenoxy)cyclohexanol, and then reacts with phosphorous trichloride to produce phosphoric acid esters in the It has plasticizing and flame retardant effects in plastic processi...

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Problems solved by technology

[0008] Taking cyclohexane as a raw material to produce epoxy cyclohexane is also proposed [CN1724 524], the method first oxidizes cyclohexane to cyclohexyl hydroperoxide, and then adds cyclohexene to carry out epoxidation reaction to generate Epoxycyclohexane and cyclohexanol, while cyclohexanol is dehydrated to generate cyclohexene, which is used as one of the raw materials for the epoxidation reaction, due to the diversity of cyclohexane oxidation, the raw material consumption of this method is high

Recently, someone proposed a solvent-free method [CN101020 669] for preparing cyclohexene by using transition metal salt and phase transfer agent to catalyze the epoxidation of cyclohexene with hydrogen peroxide [CN101020 669], but there are problems such as low selectivity and cumbersome post-treatment.

[0009] The classic chlorohydrin method and organic peroxide oxidation method related to the synthesis of epoxy compounds can synthesize epoxycyclohexane from cyclohexene, but there are disadvantages of low atom economy and large consumption

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