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Preparation method for caprolactone

A technology of caprolactone and cyclohexanone, applied in the field of preparation of caprolactone, can solve the problems of high cost, low yield, unstable quality of caprolactone, etc., and achieve the effect of low loss and simple operation

Inactive Publication Date: 2014-11-05
NANJING RED SUN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the quality of caprolactone obtained by the current method is unstable, the yield is low, and the cost is high, so it is difficult to carry out industrialized continuous production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Mix 220 grams of butyric acid, 100 grams of hydrogen peroxide (concentration is 30-50%), and 1 gram of concentrated phosphoric acid with a concentration of 85% into a 1000ml four-neck flask, heat to 60°C for 5 hours, and obtain peroxygen after rectification and dehydration. butyric acid.

[0019] A mixed solution containing 130 grams of peroxybutyric acid, 200 grams of acetone, and 50 grams of butyric acid (as a catalyst) is put into a 1000 ml four-necked round-bottomed flask, 105 grams of cyclohexanone is added dropwise to the solution, and the reaction is stirred at 50°C After 2 hours, the crude caprolactone solution was obtained, and the solvents acetone, butyric acid and perbutyric acid were evaporated under negative pressure at a temperature of 65°C, and the remaining solution was cooled to -10°C, stirred for 2 hours, crystallized, and then separated by filtration The caprolactone product is obtained, the caprolactone content is 99.5%, and the separation yield is 9...

Embodiment 2

[0021] 280 grams of valeric acid, 100 grams of hydrogen peroxide (concentration is 30 to 50%), and 1 gram of concentrated phosphoric acid with a concentration of 85% are mixed into a 1000ml four-neck flask, heated to 60°C for 5 hours, and obtained after rectification and dehydration. Valeric acid.

[0022] A mixed solution containing 140 grams of peroxyvaleric acid, 220 grams of acetone, and 40 grams of valeric acid (as a catalyst) is put into a 1000 ml four-necked round-bottomed flask, 100 grams of cyclohexanone is added dropwise to the solution, and the reaction is stirred at 50°C After 2 hours, the crude caprolactone solution was obtained, and the solvents acetone, valeric acid and peroxyvaleric acid were evaporated under negative pressure at a temperature of 65°C, and the remaining solution was cooled to -20°C, stirred for 2 hours, crystallized, and then separated by filtration The caprolactone product is obtained, the caprolactone content is 99.3%, and the separation yiel...

Embodiment 3

[0024] 250 grams of acetic acid, 200 grams of hydrogen peroxide (concentration 30-50%) and 1 gram of concentration are 85% concentrated phosphoric acid and are mixed into a 1000ml four-neck flask, heated to 60°C for 5 hours, and obtained peracetic acid after rectification and dehydration.

[0025] A mixed solution containing 300 grams of peracetic acid and 100 grams of acetone was put into a 1000 ml four-necked round-bottomed flask, 95 grams of cyclohexanone was added dropwise to the solution, and stirred and reacted at 40° C. for 2 hours to obtain a thick caprolactone solution. Distill the solvent acetone and peracetic acid under negative pressure at a temperature of 65°C, cool the remaining solution to -20°C, stir for 2 hours, crystallize, and then filter and separate to obtain the caprolactone product with a caprolactone content of 99.1%. Yield 91%.

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PUM

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Abstract

The invention discloses a preparation method for caprolactone. The method comprises the following steps: with supersaturated aliphatic acid and cyclohexanone as reaction raw materials, carrying out a reaction at 40 to 50 DEG C for 1 to 2 h so as to obtain a crude caprolactone solution; then carrying out negative pressure distillation so as to remove a solvent and incompletely reacted raw materials; and cooling the residual solution and carrying out crystallization, filtering and separation so as to obtain caprolactone. The method has the advantages of simple operation, high separation yield of caprolactone, small loss, capacity of realizing continuous feeding in the whole separation process from the crude caprolactone solution to the caprolactone product and applicability to industrial production.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for preparing caprolactone. Background technique [0002] Caprolactone is an important organic raw material, mainly used in the synthesis of polycaprolactone. Due to its superior biodegradability and memory, polycaprolactone has been used in many fields, especially in medical treatment, such as tapes, bandages, orthotics, sutures, drug release agents, etc. However, the quality of caprolactone obtained by the current method is unstable, the yield is low, and the cost is high, so it is difficult to carry out industrialized continuous production. Contents of the invention [0003] The purpose of the present invention is to provide a kind of stable product quality, high yield, low cost, suitable for the preparation method of industrialized continuous caprolactone. [0004] The purpose of the present invention is achieved in the following manner: [0005] A p...

Claims

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Application Information

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IPC IPC(8): C07D313/04
CPCC07D313/04
Inventor 葛九敢芮桂生李健薛谊陶峻
Owner NANJING RED SUN NEW MATERIAL
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