Preparation method of environment-friendly glycine betaine
A betaine and environment-friendly technology, applied in the field of preparation of environment-friendly betaine, can solve the problems of difficult control, poor fluidity, large investment and the like
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Embodiment 1
[0030] In a 2000ml four-necked flask equipped with a condensing reflux device, stirring, and a thermometer, add 1000 grams of ethanol, heat to 65°C in a water bath, and while adding dropwise 30% ammonium chloroacetate ethanol solution (372 grams), simultaneously A 30% trimethylamine solution (197 g) was added dropwise, and the temperature was controlled between 60°C and 70°C. The dropwise reaction time was 60 minutes. After the reaction was completed, the reaction was incubated for 60 minutes. The temperature was lowered to 50°C, solid ammonium chloride was separated by suction filtration, and 45.3 g of ammonium chloride was obtained after drying.
[0031] The ethanol filtrate was evaporated and concentrated by a rotary evaporator, and 672 grams of ethanol was recovered by distillation. The temperature of the remaining liquid was cooled to 20° C., and after suction filtration and drying, 62.5 grams of crude betaine was obtained. After analysis, the content of betaine was 93....
Embodiment 2
[0033] Add 100 grams of methanol and 0.5 grams of 4-dimethylaminopyridine (DMAP) into a 2000ml four-necked flask equipped with a condensing reflux device, stirring and a thermometer, heat to 50°C in a water bath, and add chloroacetic acid in batches 111.5 grams of ammonium solids were added dropwise with a 30% methanol solution of trimethylamine (197 grams), and the temperature was controlled between 50°C and 60°C. The dropwise reaction time was 60 minutes. After the reaction was completed, the reaction was incubated for 30 minutes. The temperature was lowered to 40°C, solid ammonium chloride was separated by suction filtration, and 45.9 g of ammonium chloride was obtained after drying.
[0034] The methanol filtrate was evaporated and concentrated by a rotary evaporator, and 119 grams of methanol was recovered by distillation. The temperature of the remaining liquid was cooled to 20° C., and after suction filtration and drying, 55.36 grams of crude betaine was obtained. Aft...
Embodiment 3
[0036] Take the methanol solvent that filtered out the crude betaine in Example 2, add 75 grams of methanol, heat it to 50 ° C in a water bath, add 111.5 grams of ammonium chloroacetate solids in batches, and simultaneously add 30% trimethylamine dropwise Methanol solution (197 grams), the temperature is controlled between 50°C-60°C. The dropwise reaction time was 60 minutes. After the reaction was completed, the reaction was incubated for 30 minutes. The temperature was lowered to 10°C, solid ammonium chloride was separated by suction filtration, and 49.3 g of ammonium chloride was obtained after drying.
[0037] The methanol filtrate was evaporated and concentrated by a rotary evaporator, and 213 grams of methanol was recovered by distillation. The temperature of the remaining liquid was cooled to 20° C., and after suction filtration and drying, 121.5 grams of crude betaine was obtained. After analysis, the content of betaine was 96.4%.
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