Method for preparing epoxy cyclohexane through catalytic epoxidation of cyclohexene

A cyclohexene catalytic ring, epoxy cyclohexane technology, applied in organic chemistry and other directions, can solve the problems of low selectivity, low atom economy, and high raw material consumption

Inactive Publication Date: 2010-04-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
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Method used

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  • Method for preparing epoxy cyclohexane through catalytic epoxidation of cyclohexene

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Experimental program
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Embodiment 1

[0023] Mix 800 milliliters of acetone and 1 mole of cyclohexene with 10 grams of titanium-silicon molecular sieve in a reaction flask, add 2 grams of disodium hydrogen phosphate, raise the temperature to 60°C, and add 1 mole of hydrogen peroxide dropwise in 2 hours. 6 hours.

Embodiment 2

[0025] Mix 1200 milliliters of acetone and 1.5 moles of cyclohexene with 15 grams of titanium-silicon molecular sieve in a reaction flask, add 2 grams of sodium carbonate, raise the temperature to 50°C, and add 1.5 moles of hydrogen peroxide dropwise in 2 hours, and react for 25 hours .

Embodiment 3

[0027] Mix 1200 milliliters of acetone and 3.0 moles of cyclohexene with 15 grams of titanium-silicon molecular sieves in a reaction flask, add 3 grams of sodium bicarbonate, raise the temperature to 50°C, and add 1.5 moles of hydrogen peroxide dropwise in 2 hours. Reaction 8 Hour.

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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...

Claims

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Application Information

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IPC IPC(8): C07D303/04C07D301/12
Inventor 朱华元尹笃林沈刚曾厚旭蒋绍阳殷喜平刘志坚郑建坡
Owner CHINA PETROLEUM & CHEM CORP
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