Method for recycling epsilon-caprolactone byproduct

A technology of by-product and caprolactone, which is applied in the field of recycling of ε-caprolactone by-product, can solve the problems such as by-product in the production process of ε-caprolactone, achieve economic benefits of turning waste into treasure, and solve environmental problems , The effect of environmental protection benefits is obvious

Active Publication Date: 2019-07-16
湖南东为化工新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention provides a method for recycling caprolactone by-products, which

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0032] 2000.00g caprolactone by-product (acid value 128.02mg KOH / g, hydroxyl value 10.31mg KOH / g, ε-caprolactone content 17%, caprolactone oligomer 81%) was added to 5L stainless steel for reaction In the still, add 148.61g ethylene glycol, 2.15g antioxidant 1010, 4.30g antioxidant triphenyl phosphite, 80ppm catalyst monobutyltin oxide. Raise the temperature to 140°C under stirring conditions for reaction, then raise the temperature at a heating rate of 5°C / h, and react for 1 hour at each temperature point after the temperature rise; then keep warm at 215°C for 1 hour, and the acid value of the measurement system is 28.33 mg KOH / g.

[0033] Add 40ppm catalyst tetrabutyl titanate, vacuumize and control the absolute vacuum to 60KPa, and gradually increase the vacuum degree. After adjustment, the absolute pressure of the system is 40KPa, 20KPa, 10KPa, 5KPa, 2KPa, 1KPa, 0.5KPa. The acid value of the system was continuously monitored during the process, and the final acid value wa...

example 2

[0036] Add 2000.00g caprolactone by-product (acid value 128.02mg KOH / g, hydroxyl value 10.31mg KOH / g, ε-caprolactone content 17%, caprolactone oligomer 81%) to 5L stainless steel for reaction In the still, add 155.69g ethylene glycol, 2.16g antioxidant 1010, 4.31g antioxidant triphenyl phosphite, 80ppm catalyst dialkyltin dimaleate. Raise the temperature to 140°C under stirring conditions for 1 hour, then increase the temperature at a rate of 10°C / h, and react for 1 hour at each temperature point after the temperature rise; then keep it at 220°C for 1 hour, and measure the acid value of the system 27.45 mg KOH / g.

[0037] Add 40ppm catalyst tetraisopropyl titanate, vacuumize and control the absolute vacuum to 60KPa, and gradually increase the vacuum degree. After adjustment, the absolute pressure of the system is 40KPa, 20KPa, 10KPa, 5KPa, 2KPa, 1KPa, 0.5KPa. The acid value of the system was continuously monitored during the process, and the final acid value of the system was...

example 3

[0040]2000.00g caprolactone by-product (acid value 128.02mg KOH / g, hydroxyl value 10.31mg KOH / g, ε-caprolactone content 17%, caprolactone oligomer 81%) was added to 5L stainless steel for reaction In the still, add 147.11g glycerin, 2.15g antioxidant 1010, 4.29g antioxidant triphenyl phosphite, add 80ppm catalyst monobutyltin oxide. Raise the temperature to 140°C under stirring conditions for 1 hour, then increase the temperature at a rate of 5°C / h, and react for 1 hour at each temperature point after the temperature rise; then keep it at 215°C for 1 hour, and measure the acid value of the system 29.36 mg KOH / g.

[0041] Add 40ppm catalyst tetrabutyl titanate, vacuumize and control the absolute vacuum to 60KPa, and gradually increase the vacuum degree. After adjustment, the absolute pressure of the system is 40KPa, 20KPa, 10KPa, 5KPa, 2KPa, 1KPa, 0.5KPa. The acid value of the system was continuously monitored during the process, and the final acid value of the system was 1.94...

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Abstract

The invention discloses a method for recycling an epsilon-caprolactone byproduct. The method comprises the steps: preparing a caprolactone byproduct and micromolecular polyol according to a certain ratio, adding an antioxidant and a catalyst, carrying out a reaction at a temperature of 140 DEG C to 200 DEG C, then, carrying out heat preservation for 1 to 3 hours at a temperature of 205 DEG C to 240 DEG C, adding the catalyst to gradually lower pressure intensity to finally enable an acid number of a system to be not higher than 2.0 mg KOH/g; and subjecting the product to decoloring treatment.The method can be used for solving the problem in recycling of caprolactone oligomers and is an environment-friendly and efficient treatment method.

Description

technical field [0001] The invention relates to a method for recycling by-products produced by chemical products, in particular to a method for recycling ε-caprolactone by-products. Background technique [0002] ε-caprolactone (ε-CL) is an important intermediate in organic synthesis, mainly used for the synthesis of polycaprolactone polyols, the copolymerization and modification of polycaprolactone and other ester polymers, because polycaprolactone Lactone has good non-toxicity, biodegradability, compatibility, and drug penetration, so it has been widely used in degradable plastics and biomedicine. [0003] The synthesis of ε-caprolactone is generally generated by Bayer-Villiger reaction of cyclohexanone, peroxyacetic acid or peroxypropionic acid under certain conditions. ε-caprolactone is a temperature-sensitive substance, which is easy to self-polymerize into oligomers with a degree of polymerization of 2-10 at high temperature. In the production process of ε-caprolactone...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/78C08G63/88
CPCC08G63/08C08G63/78C08G63/88
Inventor 方文拓陶丹陈卫星
Owner 湖南东为化工新材料有限公司
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