Production method for preparing epsilon-caprolactone solution by using novel dehydrating agent

A production method and dehydrating agent technology, applied in the direction of preparation of peroxide compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of unstable performance, low degree of polymerization, low degree of polymerization, etc., and achieve good social benefits and Economic benefits, the effect of increasing productivity

Inactive Publication Date: 2016-08-31
WUHAN UNIV OF TECH
View PDF7 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Commonly used H at home and abroad 2 o 2 Two-step method to synthesize ε-caprolactone. In this production process, the by-product water cannot be completely removed, which in turn triggers the self-polymerization reaction of ε-caprolactone to generate PCL with a low degree of polymerization, and its content accounts for 10% of the total output of ε-caprolactone. About 30%, however, its polymerization is too low, its shape is irregular, its performance is unstable, and its commercial value is not high, so it is of great significance to choose a suitable dehydrating agent

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Production method for preparing epsilon-caprolactone solution by using novel dehydrating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Preparation of peracetic acid solution:

[0024] First put 2gMg / Sn / W composite oxide catalyst, 96g analytical pure acetic acid, 100g analytical pure butyl acetate, and 8 drops of analytical pure 2-methylpyridine into a three-necked flask with magnetic stirring and a reflux condenser. Stir this solution at 10-20kPa (absolute pressure), then heat it to about 56°C with a water bath, and slowly drop 54.4g of 50% (weight) hydrogen peroxide aqueous solution through a constant pressure funnel into the three-necked flask . Control the temperature of the mixed solution to 50-60°C, reflux the organic phase of the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser to the three-necked flask, and drain the water phase continuously from the water separator. Acetic acid and hydrogen peroxide reacted until the water phase was basically no longer separated in the water trap, and then the second step of the reaction was started. From the time of add...

Embodiment 2

[0031] 1. Preparation of peracetic acid solution:

[0032] First put 2gMg / Sn / W composite oxide catalyst, 96g acetic acid, 100g cyclohexane, 8 drops of 2-methylpyridine into a three-necked flask with magnetic stirring and a reflux condenser. The temperature is about 10-20kPa ( (Absolute pressure) Stir this solution, and then heat it to about 56°C with a water bath, and slowly drop 54.4 g of 50% (weight) hydrogen peroxide aqueous solution through a constant pressure funnel into the three-necked flask. The temperature of the mixed solution is controlled to be about 50-60°C, the organic phase of the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser is refluxed to the three-necked flask, and the water phase is continuously drained from the water separator. Acetic acid and hydrogen peroxide reacted until the water phase was basically no longer separated in the water trap, and then the second step of the reaction was started. From the time of addin...

Embodiment 3

[0038] 1. Preparation of peracetic acid solution:

[0039] First put 2gMg / Sn / W composite oxide catalyst, 96g acetic acid, 100g ethyl propionate, 8 drops of 2-methylpyridine into a three-necked flask with magnetic stirring and a reflux condenser, at about 10-20kPa (Absolute pressure) Stir this solution, and then heat it to about 56°C with a water bath, and slowly drop a 50% (weight) hydrogen peroxide aqueous solution with a total amount of 54.4 g into the three-necked flask through a constant pressure funnel. The temperature of the mixed solution is controlled to be about 50-60°C, the organic phase of the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser is refluxed to the three-necked flask, and the water phase is continuously drained from the water separator. Acetic acid and hydrogen peroxide reacted until the water phase was basically no longer separated in the water trap, and then the second step of the reaction was started. From the time...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
particle size (mesh)aaaaaaaaaa
Login to view more

Abstract

The invention relates to a production method for preparing an epsilon-caprolactone solution by using a novel dehydrating agent; the production method comprises the specific steps: taking one of organic solvents butyl acetate, cyclohexane and ethyl propionate as a dehydrating agent, taking a Mg / Sn / W composite oxide as a catalyst, and oxidizing acetic acid by using hydrogen peroxide to obtain a peracetic acid solution; then adding cyclohexanone to the peracetic acid solution; and after completion of the reaction, cooling the reaction to room temperature, and thus obtaining the epsilon-caprolactone solution. The method provided by the invention can reduce water as far as possible before caprolactone is produced, so as to avoid the polymerization of caprolactone and improve the yield.

Description

Technical field [0001] The present invention uses a new type of dehydrating agent to prepare caprolactone. The method uses butyl acetate as the dehydrating agent, Mg / Sn / W composite oxide as the catalyst, and the peroxyacetic acid solution is prepared by oxidizing acetic acid with hydrogen peroxide. Caprolactone is prepared by adding hexanone to the peroxyacetic acid solution. Background technique [0002] At present, the global production capacity and demand for ε-caprolactone are growing rapidly at an average annual rate of about 6%. In 2011 alone, the global market demand for ε-caprolactone has exceeded 50,000 tons. According to customs statistics, In 2010, the domestic import growth rate of ε-caprolactone reached 41.9%, compared with 53.2% in 2011. At the same time, the domestic price of ε-caprolactone has been rising continuously with the tight supply and demand relationship. [0003] Commonly used at home and abroad H 2 O 2 Two-step synthesis of ε-caprolactone. In this produ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D313/04C07C409/26C07C407/00
CPCC07D313/04C07C407/00
Inventor 张光旭李胜楠李莹
Owner WUHAN UNIV OF TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap