A kind of method that improves caprolactone yield

A technology of caprolactone and cyclohexanone, which is applied in the field of improving caprolactone yield, can solve the problems of high processing difficulty, increased waste amount, and rising production cost, so as to reduce production cost, improve yield, and reduce self-consumption. The effect of agglomeration

Active Publication Date: 2019-01-22
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polycaprolactone polyol is one of the starting materials of high-grade polyurethane materials. Since caprolactone is a temperature-sensitive substance, it is easy to self-polymerize into 2-10 molecular oligomers at high temperature, while in ε-caprolactone In the process of ester production, the temperature in the rectification process is high, and ε-caprolactone produces a certain degree of self-polymerization, resulting in an increase in the amount of waste and an increase in production costs, and the high-boiling point waste produced is a sludge-like fluid at room temperature, and it is placed for a period of time After turning into a solid, it is difficult to deal with, and it is a difficult environmental protection problem
However, the current method of azeotropic distillation cannot solve the above problems well.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] React anhydrous peroxypropionic acid and cyclohexanone at 40-80°C for 1-10 hours to prepare a mixture containing caprolactone.

[0022] Put 200g of the above-mentioned mixture containing caprolactone into a 500mL glass three-necked bottle, add 2g of acetic anhydride, seal the three-necked bottle, put it on the heating oil bath, connect the gas phase condenser, turn on the cooling water and stir, and keep the temperature at 120°C React for 5 hours, then distill at 1.0-1.5kPa, cool the gas phase, stop the distillation after no distillate flows out, remove the vacuum, and weigh the residual liquid (mainly oligomers of caprolactone, the same below) in the three-necked flask It was 9.0 g, and the yield of caprolactone was 82.0%.

Embodiment 2

[0024] Put 200g of the above-mentioned mixture containing caprolactone into a 500mL glass three-necked bottle, add 5g of acetic anhydride, seal the three-necked bottle, put it on the heating oil bath, connect the gas phase condenser, turn on the cooling water and stir, and keep the temperature at 120°C React for 5 hours, then distill at 1.0-1.5kPa, cool the gas phase, stop the distillation after no distillate flows out, unload the vacuum, weigh the residual liquid in the there-necked flask to be 8.9g, and the yield of caprolactone is 82.2%.

Embodiment 3

[0026] Put 200g of the above-mentioned mixture containing caprolactone into a 500mL glass three-necked bottle, add 10g of succinic anhydride, seal the three-necked bottle, put it on a heating oil bath, connect the gas phase condenser, turn on the cooling water and stir, at 120°C React at constant temperature for 5 hours, then distill at 1.0-1.5kPa, cool the gas phase, stop the distillation after no distillate flows out, unload the vacuum, weigh the residual liquid in the there-necked flask to be 8.9g, and the yield of caprolactone is 82.2%.

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Abstract

The present invention discloses a method for improving the yield of caprolactone, and anhydride substances such as acetic anhydride, propionic anhydride, butyric anhydride, valeric anhydride, hexanoic anhydride, succinic anhydride, glutaric anhydride, adipic anhydride, phthalic anhydride and the like are added in the last phase of the reaction for production of caprolactone from cyclohexanone and a peracid to improve the yield of caprolactone. The method is simple and easy to implement and suitable for industrial application, can greatly reduce the production cost of the caprolactone, and brings huge economic benefits.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for increasing the yield of caprolactone. Background technique [0002] ε-caprolactone (ε-CL) is an important intermediate in organic synthesis, for example, it can be used to synthesize polycaprolactone and polycaprolactone polyol, and it can also be copolymerized or blended with other esters for modification. Caprolactone and its modified polymers have been widely used in degradable plastics and biomedicine because of their good biocompatibility, non-toxicity, biodegradability and good drug penetration. Polycaprolactone polyol is one of the starting materials of high-grade polyurethane materials. Since caprolactone is a temperature-sensitive substance, it is easy to self-polymerize into 2-10 molecular oligomers at high temperature, while in ε-caprolactone In the process of ester production, the temperature in the rectification process is high, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D313/04
Inventor 刘洪武黎树根周小文
Owner CHINA PETROLEUM & CHEM CORP
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