Method for producing cyclohexylbenzene hydroperoxide by catalytic oxidation of cyclohexylbenzene and oxidative decomposition of cyclohexylbenzene to prepare cyclohexanone and phenol
A technology of cyclohexylbenzene hydroperoxide and cyclohexylbenzene, which is applied in the field of oxidative decomposition of cyclohexylbenzene to prepare cyclohexanone and phenol, can solve the problems of cumbersome separation process of catalyst NHPI, difficulty in recovery and recycling, and high price. Achieve the effect of controllable synthesis process, high selectivity and simple preparation
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[0025] According to the present invention, the preparation method of the copper oxide of described rod shape comprises:
[0026] Mixing a monohydric alcohol solution containing a water-soluble copper salt with an aqueous inorganic alkali solution, and performing a hydrothermal reaction in a closed environment; the water-soluble copper salt is selected from one or more of copper nitrate, copper sulfate and copper chloride , preferably copper nitrate; the monohydric alcohol is selected from one or more of methanol, ethanol and propanol, preferably ethanol; the inorganic base is selected from sodium hydroxide and / or potassium hydroxide, preferably hydroxide Sodium; the molar ratio of the water-soluble copper salt to the inorganic base is 1:18-22; the conditions of the hydrothermal reaction include: the temperature is 100-120°C, and the time is 10-15 hours. In addition, the concentration of the water-soluble copper salt in the monohydric alcohol solution may generally be 0.45-0.55...
Embodiment 1-4
[0060] This example is used to illustrate the method for producing cyclohexylbenzene hydroperoxide by catalytic oxidation of cyclohexylbenzene provided by the present invention.
[0061] Mix 50mL cyclohexylbenzene (density 0.94g / mL) and 0.01g catalyst flower-shaped copper oxide (morphology as figure 1 shown), the weight ratio of catalyst to cyclohexylbenzene was 0.0021:1, was added into a 250mL three-necked flask, and was ultrasonically treated for 2min to form a suspension. Then under magnetic stirring again, after the mixed solution was heated to a predetermined reaction temperature (see Table 1) in an oil bath, under normal pressure at 25mL / min (in terms of per milliliter of cyclohexylbenzene, the feed rate of oxygen was 0.5mL / min). min) Oxygen was introduced, and the reaction was carried out for 9 hours. After the reaction is finished, the obtained mixed solution is filtered to obtain the copper oxide catalyst and the liquid mixture containing CHBHP. The liquid mixture w...
Embodiment 5-8
[0066] This example is used to illustrate the method for producing cyclohexylbenzene hydroperoxide by catalytic oxidation of cyclohexylbenzene provided by the present invention.
[0067] Mix 50mL cyclohexylbenzene (density 0.94g / mL) and 0.01g catalyst flower-shaped copper oxide (morphology as figure 1 shown), the weight ratio of catalyst to cyclohexylbenzene was 0.0021:1, was added into a 250mL three-necked flask, and was ultrasonically treated for 2min to form a suspension. Then under magnetic stirring, after heating the mixed solution to 100° C. in an oil bath (see Table 2), under normal pressure at 25 mL / min (in terms of per milliliter of cyclohexylbenzene, the oxygen feed rate is 0.5 mL / min) ) into oxygen and react for a certain period of time. After the reaction is finished, the obtained mixed solution is filtered to obtain the copper oxide catalyst and the liquid mixture containing CHBHP. The liquid mixture was analyzed to measure the conversion rate of cyclohexylbenze...
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Abstract
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