Unlock instant, AI-driven research and patent intelligence for your innovation.

Technique for synthesizing ester amine and quaternary ammonium salt thereof

A technology of quaternary ammonium salts and ester amines, which is applied in the technical field of synthesizing ester amines and quaternary ammonium salts to achieve the effects of ensuring product color, improving product quality, and enhancing mass transfer

Active Publication Date: 2010-05-19
SHANGHAI FINE CHEM CO LTD
View PDF2 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For adopting loop reactor technique to prepare ester amine and the method for quaternary ammonium salt thereof, there is no report

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
  • Technique for synthesizing ester amine and quaternary ammonium salt thereof
  • Technique for synthesizing ester amine and quaternary ammonium salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Ester amination reaction: Weigh 57Kg of molten stearic acid, 14.9Kg of triethanolamine and 200g of alkylbenzenesulfonic acid into a 200L loop reactor 2, replace with nitrogen, and keep the entire loop system at a reaction pressure of 0.2MPa Nitrogen pressure, start the external circulation pump 1, use the external circulation heat exchanger 8 and the loop reactor 2 to raise the temperature of the material to the reaction temperature of 180 ° C, and start the reaction. After 6 hours of reaction time, when the acid value of the esteramine product was measured to be 2.8 mgKOH / g, the reaction was terminated to obtain the esteramine.

[0022] Quaternization reaction: Use the external circulation heat exchanger 8 and the loop reactor 2 to lower the temperature of the esteramine to the reaction temperature of 70°C, and the system pressure to normal pressure, and add 10Kg of isopropanol to the loop reactor through the material inlet 4 In, then make the loop reaction system airt...

Embodiment 2

[0024] Ester amination reaction: molten stearic acid 100Kg, methyldiethanolamine 20.9Kg, phosphorous acid 100g, reaction pressure 0.5MPa, reaction temperature 170°C, reaction time 5 hours, product acid value 3mgKOH / g.

[0025] Quaternization reaction: the reaction temperature is 60°C, the amount of isopropanol is 14.2Kg, the amount of dimethyl sulfate is 22Kg, the feeding time is 2 hours, and after 6 hours of reaction time, the free amine content in the product is 0.016mmol / g. Other conditions are with embodiment 1.

Embodiment 3

[0027] Ester amination reaction: 56.4Kg of oleic acid, 14Kg of triethanolamine, 200g of alkylbenzenesulfonic acid, reaction pressure 0.4MPa, reaction temperature 200°C, reaction time 4 hours, product acid value 2.5mgKOH / g.

[0028] Quaternization reaction: the reaction temperature is 80°C, the amount of isopropanol is 10Kg, the amount of methyl chloride is 5.3Kg, the feeding time is 1 hour, and after 5 hours of reaction time, the free amine content in the product is 0.015mmol / g. Other conditions are with embodiment 1.

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 relates to a technology for the synthetic ester amine and the quaternary ammonium salt; in the technology, fatty acid, ethanolamine and acidic catalyst are added into a loop reactor; thesystem carries out the nitrogen replacement under the 0.01 to 1.0 Mpa nitrogen pressure; the material begins to react when the temperature of the material is up to150 to 210 Celsius system and laststo react for five to ten hours; when the acid value of the ester amine of the reaction products is less than 5 milligrams of potassium hydroxide in one gram, the reaction is stopped to get the ester amine; after lowering the temperature of the ester amine in the loop reactor to 50 to 90 Celsius system, the pressure of the loop reaction system is lowered to the normal pressure; the isopropanol is added in the loop reactor and the loop system is closed; uniformly the quaternary ammonium reagent is added into the loop reactor within 0.5 to 2 hours; the reaction is kept for 4 to 6 hours; when thecontent of the free amine in the products is less than 0.025 mmol per gram, the reaction is stopped and the quaternary ammonium salt is obtained. The invention has the advantages of the reduced reaction time, the guarantee of the color of the product, the improvement of the product quality, and the reduction of the production cost.

Description

technical field [0001] The invention belongs to a preparation process of esteramine and quaternary ammonium salt compound thereof. Background technique [0002] At present, the main producers of esteramines and their quaternary ammonium salts in the world are Stepan Company and P&G Company in the United States, Henkel Company in Germany and AkzoNobel in the Netherlands. The main method of their production of ester quaternary ammonium salt is to adopt fatty acid and ethanolamine to synthesize ester amine under the condition of taking acid as a catalyst, and then carry out quaternization reaction. From the existing patents on the synthesis of esteramines and their quaternary ammonium salts, such as CN 1419006A, EP0295385, WO 91 / 01295, etc., it can be seen that their synthetic process routes are all carried out using a tank-type stirring reaction process. There is no report on the method for preparing esteramines and quaternary ammonium salts thereof by adopting loop reactor t...

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 Patents(China)
IPC IPC(8): C07C219/06C07C213/00
Inventor 耿涛李秋小王伟
Owner SHANGHAI FINE CHEM CO LTD