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
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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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