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Method for synthesizing erucamide propyl betaine

An erucic acid amidopropyl sugar beet, a technology for a synthesis method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., to achieve the effects of simple process, short reaction time, and improved performance

Active Publication Date: 2012-07-25
SICHUAN SIPO CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Since water is used as the reaction medium in the traditional synthesis, short-chain fatty acid-derived betaines are no problem, but long-chain fatty acid-derived betaines cannot proceed.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preheat erucic acid and add it to the reaction kettle, add potassium hydroxide, and then replace it with nitrogen for 3 times, add dimethylaminopropylamine dropwise for reaction, wherein the molar ratio of erucic acid and dimethylaminopropylamine is 1:1.05, the reaction temperature Control at 180°C, keep the kettle temperature at 180°C to continue the dehydration condensation reaction, the reaction time is 8 hours, measure the acid value during the reaction, the acid value is 3.2mgKOH / g, keep the temperature, and then vacuumize to remove water and unreacted Dimethylaminopropylamine, the vacuum degree is 600-650mHg, the time is 45 minutes, then the temperature is lowered to 60°C, and washed three times with 5% sodium hydrogen sodium chloride aqueous solution until the acid value of the intermediate is nearly neutral, and the intermediate product N, N -Dimethyl-N'-docosylacylpropyl tertiary amine.

[0023] Weigh a certain amount of the above-mentioned N,N-dimethyl-N'-dode...

Embodiment 2

[0025] Preheat the erucic acid and put it into the reaction kettle, add sodium hydroxide, then replace it with nitrogen for 3 times, add dimethylaminopropylamine dropwise to react, wherein the molar ratio of erucic acid and dimethylaminopropylamine is 1:1.1, the reaction temperature Control at 140°C, keep the kettle temperature at 140°C to continue the dehydration condensation reaction, the reaction time is 6 hours, measure the acid value during the reaction, the acid value is 3.1mgKOH / g, keep the temperature, and then vacuumize to remove water and unreacted Dimethylaminopropylamine, the vacuum degree is 600-650mHg, the time is 30 minutes, then the temperature is lowered to 60°C, and washed three times with 5% sodium hydrogen sodium chloride aqueous solution until the acid value of the intermediate is nearly neutral, and the intermediate product N, N -Dimethyl-N'-docosylacylpropyl tertiary amine.

[0026] Weigh a certain amount of the above-mentioned N,N-dimethyl-N'-dodecenyl ...

Embodiment 3

[0028] Preheat erucic acid and add it to the reaction kettle, add potassium carbonate, then replace it with nitrogen gas for 3 times, add dimethylaminopropylamine dropwise for reaction, wherein the molar ratio of erucic acid and dimethylaminopropylamine is 1:1.15, and the reaction temperature is controlled At 200°C, keep the kettle temperature at 200°C to continue the dehydration condensation reaction. The reaction time is 10 hours. During the reaction, the acid value is measured. The acid value is 3.2mgKOH / g. Keep the temperature, then vacuumize to remove water and unreacted di Methaminopropylamine, the vacuum degree is 600-650mHg, the time is 60 minutes, then the temperature is lowered to 60°C, and washed three times with 5% sodium hydrogen sodium chloride aqueous solution until the acid value of the intermediate is nearly neutral, and the intermediate product N,N— Dimethyl-N'-dodecenyl propyl tertiary amine.

[0029] Weigh a certain amount of the above-mentioned N,N-dimethy...

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PUM

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Abstract

The invention discloses a method for synthesizing erucamide propyl betaine, relating to a method for manufacturing viscoelastic surfactants. The method for synthesizing the erucamide propyl betaine comprises the steps of carrying out a condensation reaction, a reduced pressure distillation reaction and a quaternary amination reaction and comprises the concrete steps of firstly putting erucic acid, dimethylamino propylamine and a catalyst in a reaction kettle and reacting for 6-10 hours at a temperature of 140-200 DEG C; keeping the temperature and carrying out reduced pressure distillation for 30-60 minutes and vacuumizing to 600-650mHg; neutralizing the erucic acid by using dilute alkaline water and rinsing till to be neutral; and adding a sodium chloroacetate aqueous solution into a mixed solvent of intermediate tertiary amine and carrying out the quaternary amination reaction for 4-8 hours at a temperature of 60-90 DEG C, wherein, finally, the tertiary amine conversion rate is up to more than 98% and the content of active matters is up to more than 30%. The method for synthesizing the erucamide propyl betaine has the advantages that the conversion rate of the erucic acid can be increased; by-products can be reduced; the mixed solvent is added in the quaternary amination reaction to ensure that the reaction is easy to carry out and conversion of the tertiary amine is benefited; and the content of the active matters in the product is effectively increased.

Description

technical field [0001] The invention relates to a preparation method of a viscoelastic surfactant, in particular to a synthesis method for producing erucamidopropyl betaine. Background technique [0002] The unique molecular structure of long-chain alkylpropyl betaine endows it with excellent surface activity, and can be used as detergent, wetting agent, antistatic agent, bactericide, thickener, etc. Especially when used in shampoos, it has ideal thickening, softening and antistatic effects. As erucic acid with 22 carbons, it is the longest fatty acid currently used. The erucamide propyl betaine derived from it is easy to entangle in the system due to its long carbon chain, and it is easy to form worm-like micelles. Therefore, it has good viscoelasticity, and is widely used in cleaning acidification and fracturing, as described in patents WO2006059257, US6399546, and CN1836090, but none of them mention their synthesis methods. [0003] At present, there is no industrial...

Claims

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Application Information

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IPC IPC(8): C07C229/12C07C227/08
Inventor 何祖慧冯明科刘勇朱进冯自伟
Owner SICHUAN SIPO CHEMICAL CO LTD
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