Method for preparing cyclohexanol and epoxide

A technology for epoxide and cyclohexyl hydrogen peroxide, which is applied in the field of preparing cyclohexanol and epoxide, can solve the problems of large amount of catalyst, catalyst recovery, catalyst loss and the like, and achieves fast reaction speed, improved selectivity and low cost Effect

Inactive Publication Date: 2008-03-12
YUEYANG CHANGDE CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it has problems such as large amount of catalyst used, wate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] This example is an illustration of the cyclohexane oxidation process providing the starting material for the epoxidation of the present invention. Take 60 mol of cyclohexane and put it into a 10-liter reactor with stirring and thermometer, raise the temperature to 145°C, blow in compressed air, keep the pressure at 1.5MPa, and the reaction time is 30min. Get reaction liquid and analyze, and its component comprises (mass percentage): cyclohexyl hydroperoxide is 3.51%, and cyclohexanol is 0.85%, and cyclohexanone is 0.57%, and cyclohexane is 95.03% (other by-products are 0.22%) %, such as epoxy cyclohexane, n-pentanol, cyclopentanol, adipic acid, glutaric acid, succinic acid and their various esters, etc.).

Embodiment 2

[0022] This example is an illustration of the enrichment of the cyclohexane oxidation process to provide the feedstock for the epoxidation of the present invention. Cyclohexane oxidation requires the same embodiment 1. After this oxidizing liquid is cooled and depressurized, carry out negative pressure distillation, steam about 80% of total amount, in remaining 20% ​​still liquid, sampling analysis, its main component (mass percentage): cyclohexyl hydroperoxide is 14.67 %, cyclohexanol is 4.70%, cyclohexanone is 2.82%, and cyclohexane is 76.69%.

Embodiment 3

[0024] Get the 500g oxidation solution prepared in Example 1 and join in the experimental autoclave of 1 liter (containing cyclohexyl hydroperoxide 0.151mol in the oxidation solution), and add the 20ppm catalyst [(C 18 h 37 ) 4 N] 3 PO 4 W 4 o 20 , start stirring, feed propylene to a pressure of 0.8 MPa (with nitrogen), heat to about 150°C, and maintain the pressure for 80 minutes. Sampling analysis: cyclohexyl hydroperoxide is 0.06%, and the conversion rate is 98.3%; propylene oxide is 1.67%, and the selectivity is 95.2%.

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PUM

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Abstract

The present invention relates to a method of preparing the cyclohexyl alcohol epoxide. The method is characterized in that the amount of the organic compound catalyst containing the transition metal is only 5 to 500 ppm of the total weight of materials; the olefin is added in the cyclohexyl oxide compound containing the cyclohexyl hydrogen peroxide; the molar ratio between the olefin and the cyclohexyl hydrogen peroxide is between 0.2 and 20 to 1; under the pressure of 0.1MPa to 6.0MPa and at the temperature between 0 and 200 DEG C, the epoxidation reaction is done for 10 to 20 minutes to prepare the cyclohexyl alcohol and epoxide. The present invention uses the oxygen decomposed from the cyclohexyl hydrogen peroxide for the epoxidation; thus the present invention not only saves the cost of the oxidant of the epoxidation of olefin, but also obviously improves the collection rate of the cyclohexanol and cyclohexanone decomposed from the cyclohexyl hydrogen peroxide. In particular, the dosage of the selected catalyst is minimal so as not to be recycled; the process is simple and the cost is low.

Description

field of invention [0001] The present invention relates to a method for preparing cyclohexanol and epoxides. Background technique [0002] Using cumene hydroperoxide as an oxygen source and using a transition metal-containing molecular sieve catalyst to catalyze the oxidation of olefins to prepare epoxides is a typical Halcon method, and this process has been disclosed in Czech Patent No. CS140743. In order to better realize industrialization, some patents have proposed constructive methods, such as CN1252059, WO2001 / 070710, WO2003 / 027087, WO2005 / 030744, etc. However, the by-product alcohol is difficult to deal with, and if it is recycled, there are problems of long process and high cost. [0003] The production of cyclohexanol and cyclohexanone by oxidation of cyclohexane is well known. And there are many reports on how to improve the selectivity of oxidation products decomposed into cyclohexanol and cyclohexanone, such as CN1447742 and CN1721383. However, they did not f...

Claims

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Application Information

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IPC IPC(8): C07D301/19C07C35/08
Inventor 蒋卫和李浩袁年武屈铠甲肖海军郑宏翠
Owner YUEYANG CHANGDE CHEM IND
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