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 reduce production costs, reduce nitrogen consumption, and ensure product color.

Active Publication Date: 2008-02-13
SHANGHAI FINE CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For adopting loop reactor technique to prepare ester amine and th

Method used

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  • Technique for synthesizing ester amine and quaternary ammonium salt thereof

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Embodiment 1

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

[0022] Quaternization reaction: use the external circulation heat exchanger 8 and the loop reactor 2 to reduce the temperature of the ester amine to 70°C of the reaction temperature, the system pressure to normal pressure, and add 10Kg of isopropanol to the loop reactor through the material inlet 4 Then, ...

Embodiment 2

[0024] Ester amination reaction: melted 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 the reaction time is 6 hours, the free amine content in the product is 0.016mmol / g. Other conditions are the same as in Example 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℃, 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 the reaction time is 5 hours, the free amine content in the product is 0.015mmol / g. Other conditions are the same as in Example 1.

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Abstract

A process for synthesizing esteramine and its quaternary ammonium salt is to add fatty acid, ethanolamine and acidic catalyst into a loop reactor, the system is replaced by nitrogen, the pressure is 0.01-1.0Mpa nitrogen pressure, and the temperature of the material is raised to 150-210°C for reaction , react for 5-10 hours, when the acid value of the reaction product ester amine is lower than 5mgKOH/g, stop the reaction to obtain ester amine; after the temperature of ester amine in the loop reactor is reduced to 50-90°C, the loop reaction system Reduce to normal pressure, add isopropanol into the loop reactor and seal the loop system, add the quaternizing agent into the loop reactor at a uniform speed within 0.5 to 2 hours, react for 4 to 6 hours, when When the free amine content in the product is less than 0.025mmol/g, the reaction is stopped to obtain quaternary ammonium salt; the present invention has the advantages of shortening the reaction time, ensuring product color, improving product quality and reducing production cost.

Description

technical field [0001] The invention belongs to a preparation process of esteramine and its quaternary ammonium salt compound. Background technique [0002] At present, the main producers of esteramines and their quaternary ammonium salts in the world are Stepan Company, P&G Company of the United States, Henkel Company of Germany and Akzo Nobel of the Netherlands. Their main method for producing ester quaternary ammonium salt is to use fatty acid and ethanolamine to synthesize ester amine under the condition of acid as catalyst, and then carry out quaternization reaction. It can be seen from the existing patents on the synthesis of ester amines and their quaternary ammonium salts such as CN1419006A, EP0295385, WO91 / 01295, etc., that their synthesis process routes are all carried out by using the tank-type stirring reaction process. There is no report on the method for preparing esteramine and its quaternary ammonium salt by using a loop reactor process. SUMMARY OF THE INV...

Claims

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Application Information

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