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Method for preparing epoxypropane

A technology of propylene oxide and epoxidation, which is applied in the direction of organic chemistry, can solve the problems of no breakthrough progress, and achieve the effects of high production efficiency, high reaction selectivity, and high peroxide concentration

Inactive Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The direct oxidation of propylene with molecular oxygen to prepare propylene oxide is an ideal method that has been pursued in the field of propylene oxide research. Many researchers have been exploring this process, but there has been no breakthrough.

Method used

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  • Method for preparing epoxypropane
  • Method for preparing epoxypropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] The first step, the oxidation reaction:

[0080]In a 500ml stainless steel reaction kettle equipped with a stirring and condensing reflux device, add 200ml of methylcyclohexane as the reaction raw material, seal the reaction kettle, heat up to and keep the temperature at the reaction temperature of 135°C under a nitrogen atmosphere, and adjust the reaction pressure to a gauge pressure of 0.4MPa , oxidize by feeding air at a speed of 400ml / min, and stir at a speed of 500rmp. When the reaction time was 10 h, the collected reaction solution was used as the raw material for the second step reaction.

[0081] During the experiment, the liquid material samples in the reactor were taken through the sampling port every 1 h, and the concentration of methylcyclohexyl hydroperoxide in the samples was analyzed by traditional iodometric method. At the initial stage of the reaction, the concentration of methylcyclohexyl hydroperoxide increases with the prolongation of the reaction t...

Embodiment 2

[0086] Embodiment 2: the first step oxidation reaction

[0087] Add 200ml of methylcyclohexane to a 500ml stainless steel reaction kettle equipped with a stirring and condensing reflux device, seal it, heat up to and keep the temperature at a reaction temperature of 100°C under a nitrogen atmosphere, adjust the reaction pressure to a gauge pressure of 0.3MPa, and use 400ml / The gas with an oxygen content of 30%, that is, oxygen-enriched air, is passed through at a speed of min for oxidation, and the stirring speed is 500rmp. When the reaction time was 12 hours, the concentration of methylcyclohexyl hydroperoxide in the reaction liquid reached the highest, which was 12.5%. Collect the reaction liquid as the raw material of the second step epoxidation reaction.

Embodiment 3

[0088] Embodiment 3: the first step oxidation reaction

[0089] Add 200ml of methylcyclohexane to a 500ml stainless steel reaction kettle equipped with a stirring and condensing reflux device, seal it, heat up to and keep the temperature at a reaction temperature of 145°C under a nitrogen atmosphere, adjust the reaction pressure to a gauge pressure of 1.0MPa, and use 400ml / The gas with an oxygen content of 15%, that is, oxygen-depleted air, is passed through at a speed of min for oxidation, and the stirring speed is 500rmp. When the reaction time was 8 hours, the concentration of methylcyclohexyl hydroperoxide in the reaction liquid reached the highest, which was 22.4%. Collect the reaction liquid as the raw material of the second step epoxidation reaction.

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Abstract

The invention relates to a method for producing epoxypropane, in particular to a process for preparing epoxypropane by an organic peroxide method, with methylcyclohexane as an initial hydrocarbon. The method comprises the following three steps: 1. oxidizing methylcyclohexane in a liquid phase to obtain methyl cyclohexyl hydrogen peroxide; 2. subjecting the methyl cyclohexyl hydrogen peroxide to react with propylene to obtain epoxypropane and methylcyclohexanol; and 3. dehydrating and hydro-converting the methylcyclohexanol to methylcyclohexane, and returning to the first oxidation reaction step for recycling.

Description

technical field [0001] The present invention relates to the production method of petrochemical raw materials, more specifically to the production method of propylene oxide. Background technique [0002] Propylene oxide is the third largest derivative of propylene after polypropylene and acrylonitrile. Because of its highly tense oxygen-containing three-membered ring, its chemical properties are very active and it has a wide range of uses. It is mainly used for the production of propylene glycol, polypropylene Ether etc. [0003] Traditional propylene oxide production processes mainly include chlorohydrin method and organic peroxide oxidation method. [0004] Chlorohydrin method: The chlorohydrin method is the earliest process for producing propylene oxide on an industrial scale, and it is still in use today. The process is to use hypochlorous acid (chlorine aqueous solution) to react with propylene to generate chloropropanol, and then dehydrochloride under the action of ca...

Claims

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Application Information

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IPC IPC(8): C07D303/04C07D301/19
Inventor 张明森柯丽赵清锐刘红梅
Owner CHINA PETROLEUM & CHEM CORP
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