Process of preparing alcohol ether glucoside citrate monoester salts
A technology of citric acid glycosides and alcohol ether glycosides, which is applied in the field of preparing alcohol ether glycoside citric acid monoester salts, can solve the problems of difficult separation, low surface activity, etc. Effect
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Embodiment 1
[0027] In a 250ml four-neck flask equipped with a thermometer, agitator, and condenser, add 0.2mol of anhydrous citric acid and 0.6mol of propionic anhydride to mix, then heat at 40°C, react for 90min, and add 1 times the volume of the reaction product. Squalane, control the pressure at 30mmHg, react for 1h to remove volatiles in the system. Add 0.25 mol of alcohol ether glycosides into the reactor, and react for 3 hours at 60°C and 10mmHg.
[0028] After the product was cooled, it was placed in a separatory funnel to separate layers, and the squalane was removed. Neutralize with 50% sodium hydroxide aqueous solution until the pH value is 9 to obtain alcohol ether glycoside citrate monoester disodium salt with a product yield of 95% and a monoester salt content of 90%.
Embodiment 2
[0030] In a 500ml four-necked flask equipped with a thermometer, a stirrer and a condenser, add 0.3mol of anhydrous citric acid, 0.3mol of butyric acid and 0.6mol of butyric anhydride, heat to 90°C, and react for 15min. Add squalane 2 times the volume of the reaction product, control the pressure at 5 mmHg, react for 1 h to remove volatiles in the system. Add 0.3mol of alcohol ether glycosides into the reactor, and react for 2 hours at 100°C and 15mmHg.
[0031] After the product was cooled, it was placed in a separatory funnel to separate layers, and the squalane was removed. Neutralize with 40% potassium hydroxide aqueous solution until the pH value is 7 to obtain alcohol ether glycoside citrate monoester dipotassium salt with a product yield of 90% and a monoester salt content of 92%.
Embodiment 3
[0033] Add 0.6 mol of anhydrous citric acid, 1.2 mol of valeric acid and 1.2 mol of valeric anhydride into a 1000ml four-necked flask equipped with a thermometer, a stirrer, and a condenser, heat to 50°C, and react for 60 minutes. Add squalane 3 times the volume of the reaction product, control the pressure at 20 mmHg, react for 2 hours to remove volatiles in the system. Add 0.6 mol of alcohol ether glycoside into the reactor, react at 90°C and 20mmHg for 2h.
[0034] After the product was cooled, it was placed in a separatory funnel to separate layers, and the squalane was removed. Neutralize with ammonia solution until the pH value is 8 to obtain alcohol ether glycoside citrate monoester diammonium salt with a product yield of 95% and a monoester salt content of 93%.
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