Hydrogenolysis method of cyclohexyl hydroperoxide

Abstract

The invention discloses a hydrogenolysis method of cyclohexyl hydroperoxide and belongs to the technical field of organic chemistry. The method comprises the following specific steps: washing a cyclohexane oxidation solution containing cyclohexyl hydroperoxide, isolating an organic phase, adding a Pd / Al catalyst into the organic phase, introducing hydrogen, reacting at the temperature of 50-120 DEG C and at the pressure of 0.1-1.5 MPa for 0.1-3h, filtering the catalyst, carrying out alkali cleaning by adding 5-30 wt% of alkali lye into the reaction liquid with introduced hydrogen, washing with water after alkali cleaning, carrying out liquid separation after water washing, and collecting the organic phase, wherein mass ratio of the catalyst to the organic phase is 1:10-10000 and diameter of the catalyst is 0.01-10mm. The Pd / Al catalyst is used to catalyze hydrogenolysis of cyclohexyl hydroperoxide; reaction condition is mild; selectivity is high; treatment after the reaction is convenient; dosage of the catalyst is low and the catalyst can be recycled; and conversion rate and selectivity are high.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a method for hydrolysis of cyclohexyl hydroperoxide. Background technique [0002] At present, most of the KA oil used in the industrial production of adipic acid is prepared by the non-catalytic air oxidation of cyclohexane. The preparation of KA oil by cyclohexane oxidation includes the following steps: 1) Cyclohexane is heated at 160-180°C , the cyclohexane oxidation liquid whose main product is cyclohexyl hydroperoxide is obtained through air non-catalytic oxidation, and contains about 0.5-0.8% acids and esters; 2) cyclohexyl peroxide in the cyclohexane oxidation liquid Hydrogen oxide decomposes into cyclohexanone and cyclohexanol at a certain alkalinity; 3) Distillation to obtain a mixture of cyclohexanone and cyclohexanol, namely KA oil. At present, the following problems exist in the decomposition process of cyclohexyl hydroperoxide: high production energy consu...

AI Technical Summary

Problems solved by technology

At present, the following problems exist in the decomposition process of cyclohexyl hydroperoxide: high production energy consumption, low selectivity of cyclohexyl hydroperoxide decomposition, obvious polycondensation of cyclohexanone, and adding a large amount of alkali in the production, generating a large amount of alkaline wastewater and polluting surroundings

The reaction condition requirement of this method is higher, and the requirement to equipment is also higher; The by-product in the cyclohexane oxidation preparation cyclohexyl hydroperoxide process is easy to be attached on the hydrogenation catalyst surface, causes the activity of catalyst to reduce; Alcohol and ketone The total yield is not high at 92%