Method for preparing high-quality epoxidized fatty acid ester with micro-reaction device

Patent metadata

Field	Value
Publication number	US-9546143-B2
Application number	US-201615201274-A
Country	US
Kind code	B2
Filing date	Jul 1, 2016
Priority date	Apr 7, 2016
Publication date	Jan 17, 2017
Grant date	Jan 17, 2017

Abstract

A method for preparing a high-quality epoxidized fatty acid ester with a micro-reaction device, including: respectively pumping an aqueous hydrogen peroxide solution and a carboxylic acid at the same time into a first micro-mixer; after the reaction in the first micro-reactor, respectively pumping the output material and an unsaturated fatty acid ester into a second micro-mixer;
completely mixing them and then introducing the mixture into a second micro-reactor; and after a complete reaction, water-rinsing the organic phase part of the resultant reaction liquid and drying the same to obtain the epoxidized fatty acid ester.

First claim

What is claimed is:

1. A method for preparing a high-quality epoxidized fatty acid ester with a micro-reaction device, comprising the following steps:
(1) respectively pumping an aqueous hydrogen peroxide solution and a carboxylic acid at the same time into a first micro-mixer of the micro-reaction device, completely mixing them and then introducing the mixture into a first micro-reactor of the micro-reaction device to react; and
(2) respectively pumping the output material of the first micro-reactor and an unsaturated fatty acid ester at the same time into a second micro-mixer of the micro-reaction device, completely mixing them and then introducing the mixture into a second micro-reactor of the micro-reaction device to react completely, water-rinsing the organic phase part of the resultant reaction liquid and drying to obtain the epoxidized fatty acid ester.

2. The method of claim 1 , wherein in step (1), the mass fraction of the solute, hydrogen peroxide, comprised in the aqueous hydrogen peroxide solution is 50-70%.

3. The method of claim 1 , wherein in step (1), the carboxylic acid is formic acid, acetic acid, propanoic acid or butyric acid.

4. The method of claim 1 , wherein in step (1), the molar ratio of hydrogen peroxide to carboxylic acid is 1:1-5.

5. The method of claim 1 , wherein in step (1), in the first micro-reactor the reaction temperature is 35-85° C. and the residence time is 1-8 min.

6. The method of claim 1 , wherein in step (2), the unsaturated fatty acid ester is an unsaturated fatty acid methyl ester, an unsaturated fatty acid ethyl ester, an unsaturated fatty acid propyl ester or an unsaturated fatty acid butyl ester.

7. The method of claim 1 , wherein in step (2), in the second micro-reactor the reaction temperature is 65-115° C. and the residence time is 4-8 min.

8. The method of claim 1 , wherein the molar ratio of hydrogen peroxide to double bonds of the unsaturated fatty acid ester is 5-20:1.

9. The method of claim 1 , wherein the micro-reaction device comprises the first micro-mixer, the first micro-reactor, the second micro-mixer and the second micro-reactor sequentially connected in series via connecting tubes, wherein the feed inlet of the first micro-mixer is connected to a first liquor inlet and a second liquor inlet respectively, and the feed inlet of the second micro-mixer is connected to the outlet of the first micro-reactor and a third liquor inlet respectively.

Assignees

• Nanjing Tech Univ (Cn)
• Nanjing University Of Technology

Inventors

• Guo Kai
• Fang Zheng
• Li Xin
• Zhu Ning
• Wan Li
• He Wei
• Zhang Kai
• Ouyang Pingkai

Classifications

• B01J2219/00795

  Spiral-shaped · CPC title

• C07D301/16 Primary

  formed in situ, e.g. from carboxylic acids and hydrogen peroxide · CPC title

• B01J19/0093

  Microreactors, e.g. miniaturised or microfabricated reactors (laboratory containers with capillary fluid transport in microfabricated channels or chambers B01L3/5027) · CPC title

• B01J2219/00873

  Heat exchange · CPC title

• B01J2219/00889

  Mixing · CPC title