Method for preparing epsilon-caprolactone from cyclohexanone

A technology of cyclohexanone and caprolactone, applied in the field of electrochemical preparation of ε-caprolactone, to achieve enhanced oxidation reaction effect, simple process flow and mild reaction conditions

Active Publication Date: 2022-05-06
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Documents such as Li Shaofeng disclose that the peroxyacid oxidation method is the method for industrialized production of ε-caprolactone adopted in large quantities so far, and the remaining methods are still in the stage of laboratory research and development, and need to be further explored [peroxyacetic acid synthesis and its role in ε -Application in the preparation of caprolactone[J].Chemical Propellants and Polymer Materials, 2016,14(1):36-54.]

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  • Method for preparing epsilon-caprolactone from cyclohexanone
  • Method for preparing epsilon-caprolactone from cyclohexanone

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preparation example

[0044] The initial peracetic acid solution of the present invention is prepared with reference to the method of patent document CN106349140B, and its specific preparation process is:

[0045] 200 g of bissulfonic acid-based polystyrene resin was charged into a reactor with a volume of 4 L, and 1200 g of acetic acid and 880 g of ethyl acetate were added into the reactor.

[0046] The reactor has a packed distillation column and a reflux condenser with a settling tank. Stir this solution at about 20kPa (absolute pressure), heat it to about 40° C. with an oil bath, and add a total amount of 440 g of 50 wt % hydrogen peroxide solution into the reactor. Control the temperature of the reactor at about 40-45°C, introduce the organic phase in the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser into the adsorption tower, which is equipped with molecular sieves, and the organic phase passes through the molecular sieves Adsorption dehydration, the...

Embodiment 1

[0049] Weigh 224.1g of the initial peracetic acid solution and 375.9g of ethyl acetate into the flask, mix evenly and prepare an 8wt% peracetic acid solution.

[0050] Transfer all the above peracetic acid solution to the electrolytic cell, weigh 0.50 g of lead tetraacetate and 2.50 g of lithium chloride and add them to the electrolytic cell, start stirring to mix the materials in the electrolytic cell evenly. Then, the anode (lead electrode, 2.5×6cm 2 ) and cathode (lead electrode, 2.5×6cm 2 ) into the reaction system, turn on magnetic stirring and energize, and keep the current constant at 4.8A (current density 3200A / m 2 ), control the temperature at 35°C, add cyclohexanone dropwise to the electrolytic cell by an advection pump, carry out the electrolysis reaction, and control the reaction time of dropwise adding cyclohexanone (74.3g) at 3h, continue after the dropwise addition of cyclohexanone solution ends Insulation reaction 3h. Collect 675.7 g of the reaction solution...

Embodiment 2

[0052] Weigh 140.1g of the initial peracetic acid solution and 9.9g of ethyl acetate into the flask, mix well and prepare a 20wt% peracetic acid solution.

[0053] Transfer all the above peracetic acid solution to the electrolytic cell, weigh 0.75g of copper acetate and 0.75g of cobalt chloride and add them to the electrolytic cell, start stirring to mix the materials in the electrolytic cell evenly. Then, the anode (platinum electrode, 2.5×6cm 2 ) and cathode (platinum electrode, 2.5×6cm 2 ) into the reaction system, turn on magnetic stirring and energize, and keep the current constant at 18A (current density 12000A / m 2 ), control the temperature at 65°C, drop cyclohexanone in the electrolytic cell by an advection pump, carry out the electrolysis reaction, and drop the reaction time of cyclohexanone solution (185.8g cyclohexanone and 433.6g butyl butyrate) at 1h, after the dropwise addition of the cyclohexanone solution was completed, the insulation reaction was continued f...

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Abstract

The invention provides a method for preparing epsilon-caprolactone from cyclohexanone, which comprises the following steps: taking a cyclohexanone solution as a raw material, adding the cyclohexanone solution into a peracetic acid solution containing a catalyst a and a catalyst b, and carrying out electrolytic oxidation reaction to obtain epsilon-caprolactone. According to the method for preparing epsilon-caprolactone through electro-catalytic oxidation of cyclohexanone, the blank of an electro-catalytic oxidation technology in the aspect of preparing epsilon-caprolactone through a peroxy acid oxidation method is filled, and the method is mild in reaction condition and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of electrochemical synthesis, in particular to a method for preparing ε-caprolactone by using cyclohexanone as a raw material by an electrochemical method. Background technique [0002] ε-caprolactone is a synthetic monomer of polycaprolactone, a biodegradable material, and it is also a research hotspot in the field of polymer material development. However, my country has been in a relatively backward situation in the industrial production of ε-caprolactone for a long time, mainly relying on imports, high prices, and unstable supply, which also restricts the development and promotion of downstream products to a large extent. [0003] The production technology of ε-caprolactone is currently monopolized by a few foreign companies, such as DAICEL Co., Ltd. of Japan and Ingevity Corporation of the United States, etc., while there is only one industrial production of ε-caprolactone in China. device. [0004] Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/05C25B3/07C25B3/23
CPCC25B3/05C25B3/07C25B3/23
Inventor 林龙黄真真翟文超张涛张永振黎源
Owner WANHUA CHEM GRP CO LTD
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