Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for synthesizing gamma lactone

A synthesis method and lactone technology, applied in the direction of organic chemistry, can solve the problems of reduced reaction efficiency, complicated reaction device, and influence on product purity, and achieve the effect of improving product yield

Inactive Publication Date: 2011-02-16
ANHUI HYEA AROMAS
View PDF1 Cites 15 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many domestic research institutions have conducted research on this process, and found that the optimum temperature for the addition reaction of acrylic acid or acrylate and alcohol is between 165 and 185°C, which is affected by the boiling point of the starting material. When the system reaches such a temperature, it can only be pressurized or a large amount of high-boiling-point substrate (such as lactone) can be added as a solvent in the system, resulting in a decrease in reaction efficiency. Increasing the pressure will cause the complexity of the reaction device, increase equipment investment and operation Inconvenient, while the reaction system is heated for a long time, resulting in an increase in by-products and affecting the purity of the final product

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
  • Method for synthesizing gamma lactone
  • Method for synthesizing gamma lactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1 (gamma undecalactone)

[0016] a ingredient

[0017] 172g (2.0mol) of methyl acrylate; 2000g (15.4mol) of octanol; 30g (0.2mol) of di-tert-butyl peroxide; 1.7g of SL-90 polymerization inhibitor was added to stirring pot 1, and the temperature dropped to -5°C , stirring for 10 minutes;

[0018] b reaction

[0019] The above-mentioned ingredients are continuously added into the 1L autoclave 2 through the pump 3 through the feeding device, and the flow rate is controlled at 160g / hour; the nitrogen is pressurized to 0.25Mpa, and the temperature is raised and controlled at 190°C; Product methanol, tert-butanol and other by-products; unreacted octanol is recovered to the reflux tank 8 at the bottom of the tower; the reaction product is continuously extracted from the pump 4, and the flow rate of the extracted reactant is controlled to maintain the liquid level of the reactor; after 10 hours, the reaction The content of the crude product reaches and stabilizes ...

Embodiment 2

[0021] Embodiment 2 (gamma nonalactone)

[0022] a ingredient

[0023] 200g of methyl acrylate; 1900g of hexanol; 40g of di-tert-butyl peroxide; 1.7g of SL-90 polymerization inhibitor was added to the stirring pot 1, the temperature dropped to -5°C, and stirred for 10 minutes;

[0024] b reaction

[0025] The above-mentioned ingredients are continuously added into the 1L autoclave 2 through the pump 3 through the feeding device, and the flow rate is controlled at 160g / hour; the nitrogen is pressurized to 0.25Mpa, and the temperature is raised and controlled at 190°C; Product methanol, tert-butanol and other by-products; unreacted hexanol is recovered to the reflux tank 8 at the bottom of the tower; the reaction product is continuously extracted from the pump 4, and the flow rate of the extracted reactant is controlled to maintain the liquid level of the reactor; after 10 hours, the reaction The content of the crude product reaches and stabilizes at 20%. After high-vacuum pre...

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

No PUM Login to View More

Abstract

The invention discloses a method for synthesizing gamma lactone. The method comprises the following steps of: putting acrylic acid or acrylic ester as well as alcohol and a ditertiary butyl peroxide or benzoyl peroxide into a stirring pot by a molar ratio of 1:(3-30); uniformly mixing at -20-30 DEG C; adding accessories to a kettle type reactor from a fractionating column which is filled with a cy700 stainless steel ripple filler and has 5-30 theoretical plates; controlling the flow rate to 50-200g / hour and the reaction temperature between 165 DEG C and 280 DEG C and pressurizing nitrogen to 0.05-1.25MPa; after 5 hours, fractionating out tertiary butanol and low-carbon ester which are byproducts under normal pressure through the fractionating column, and recovering unacted alcohol; after 10 hours, under vacuum pressure of 133-1,000Pa, extracting a crude reaction product from the reactor; and fractionating the crude product in a rectifying column to obtain a product. The method effectively improves the product yield, and the product quality conforms to the requirement on food blending.

Description

1. Technical field [0001] The invention relates to a method for synthesizing gamma lactone. 2. Background technology [0002] Gamma-lactone is a series of synthetic fragrances, including ga-caprolactone, ga-enantholactone, ga-caprolactone, ga-nonanolide, ga-decalactone, ga-undecalactone, ga-deca Dilactone. In the early days, heptanal and malonic acid were condensed and decarboxylated to synthesize gamma-nonanolide, and undecylenic acid sulfuric acid was used to synthesize gamma-undecalactone, both of which were replaced due to high cost. Japanese Patent No. 04-054177 describes the synthesis method of gamma-lactone series products. Using di-tert-butyl peroxide as a catalyst, acrylic acid or methyl acrylate and alcohol undergo free radical addition reaction in a high-pressure reactor. One-step synthesis Gamma lactone, changing different raw material alcohols to obtain lactone series products. Many domestic research institutions have conducted research on this process, and f...

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
IPC IPC(8): C07D307/33
Inventor 范一义
Owner ANHUI HYEA AROMAS
Features
  • Generate Ideas
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com