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Method for separating cyclohexanol and cyclohexanone from KA oil

A technology for cyclohexanone and cyclohexanol, which is applied in the field of separating cyclohexanol and cyclohexanone, can solve the problems of high cost, high energy consumption, complicated operation and the like, and achieves reduction of energy consumption and production cost, high separation efficiency and simplification The effect of the process steps

Active Publication Date: 2015-11-04
新疆普禾粟新型环保材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the defects of complex operation, high energy consumption and high cost in the separation of KA in the prior art, the purpose of the present invention is to provide a method with simple operation, low energy consumption and effective separation of cyclohexanol and cyclohexanone in KA oil , the method is low in cost and meets industrial production

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  • Method for separating cyclohexanol and cyclohexanone from KA oil

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Experimental program
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Effect test

Embodiment 1

[0024] In the stirred reactor equipped with KA oil, slowly add 55% hydrogen peroxide to carry out the stirring reaction, keep the temperature of the stirred reactor at 15°C, the reaction will continue to precipitate cyclohexanone peroxide precipitation, until the reaction proceeds to no precipitation, stop reaction, filtration and separation to obtain cyclohexanone peroxide, and the filtrate obtained by filtration and separation was left to cool in a cold water bath at 5°C, and the upper layer solid was collected to obtain cyclohexanol; the separated cyclohexanone peroxide was placed in a large amount of water and heated to 60 ℃ for hydrolysis reaction, after the completion of the hydrolysis reaction, cooling, collecting the upper layer of oily liquid, that is, cyclohexanone. The cyclohexanone and cyclohexanol products collected are carried out chromatographic analysis, and cyclohexanol purity is 97.5%, and cyclohexanone purity is 98%; And calculate according to raw material co...

Embodiment 2

[0026]In the stirred reactor equipped with KA oil, slowly add 35% hydrogen peroxide to carry out the stirring reaction, keep the temperature of the stirred reactor at 30°C, the reaction will continue to precipitate cyclohexanone peroxide precipitation, until the reaction proceeds to no precipitation, stop reaction, filtration and separation to obtain cyclohexanone peroxide, and the filtrate obtained by filtration and separation was left to cool in an ice-water bath, and the upper layer solid was collected to obtain cyclohexanol; the obtained cyclohexanone peroxide was placed in a large amount of water and heated to 70°C for Hydrolysis reaction, after the completion of the hydrolysis reaction, cool down, collect the oily liquid in the upper layer, and obtain cyclohexanone. The cyclohexanone and cyclohexanol products collected are carried out chromatographic analysis, and cyclohexanol purity is 96.1%, and cyclohexanone purity is 97%; And calculate according to raw material compos...

Embodiment 3

[0028] by figure 1 The device realizes the separation of KA oil. First open the valve between the settling tower and the stirring reaction tower to connect the two, inject KA oil from the KA oil inlet until the KA oil covers the stirring bar at the bottom of the agitator, add 45% hydrogen peroxide from the hydrogen peroxide inlet, and control The temperature in the stirred reaction tower is 40°C. Under the stirring condition, the hydrogen peroxide and the cyclohexanone in the KA oil fully contact and react in the stirred reaction tower. It settles into the settling tower under its own gravity, and the KA oil in the settling tower is pushed up by the settled cyclohexanone peroxide and rises into the stirring reaction tower, and the reaction continues until the settling tower is filled with cyclohexanone peroxide. When oxidation occurs, close the valve between the settling tower and the stirring reaction tower, open the discharge branch pipe to recover a small amount of reactio...

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Abstract

The invention discloses a method for separating cyclohexanol and cyclohexanone from KA oil. Hydrogen peroxide and cyclohexanone undergo a reaction at a low temperature to produce cyclohexanone peroxide precipitates and the cyclohexanone peroxide can be hydrolyzed and reduced into cyclohexanone at a high temperature, and according to the above characteristic, the method realizes separation of cyclohexanol and cyclohexanone from KA oil. The method has simple processes and low energy consumption and effectively realizes KA oil separation. The method can further utilize a reaction separation synchronous reactor to separate KA oil. The reaction separation synchronous reactor comprises a stirring reaction tower and a settling tower communicated with the bottom of the stirring reaction tower. Cyclohexanone in KA oil and hydrogen peroxide undergo a reaction in the stirring reaction tower to produce cyclohexanone peroxide, and the cyclohexanone peroxide settles in the settling tower by gravity so that timely separation of the cyclohexanone peroxide and a reaction solution is realized. The method prevents cyclohexanone peroxide hydrolysis side reaction, further improves cyclohexanol and cyclohexanone separation efficiency and further improves cyclohexanol and cyclohexanone purity.

Description

technical field [0001] The invention relates to a method for separating cyclohexanol and cyclohexanone from KA oil, belonging to the technical field of petrochemical industry. Background technique [0002] KA oil is a mixture of cyclohexanol and cyclohexanone, which is the basic chemical raw material for the production of Nylon 6 and Nylon 66. At present, in the industry, cyclohexane liquid-phase air oxidation is the main method for preparing KA oil, such as the non-catalyzed oxidation method of the Netherlands Stamika Company, which is mainly prepared by cyclohexane liquid-phase air oxidation under high temperature and high pressure conditions get. At present, the best conversion rate of cyclohexane that can be achieved in industry is 4%, and the yield of KA oil is 82%. The patent (publication number CN 1191218 A) discloses a method for preparing KA oil by air oxidation of cyclohexane under metalloporphyrin catalysis. According to this method, Sinopec used 2ppm tetrapheny...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/26C07C45/85C07C49/403C07C29/88C07C35/08
CPCC07C29/88C07C45/85C07C49/403C07C35/08
Inventor 郭灿城郭欣
Owner 新疆普禾粟新型环保材料有限公司
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