Method for preparing betaine hydrochloride
A technology of hydrochloride and betaine, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, etc. It can solve the problems of difficult to remove salt, impurities in products, and consume large energy, so as to save raw materials , short production cycle, and the effect of reducing energy consumption
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Embodiment 1
[0022] Before the reaction, the content of water in chloroacetic acid and trimethylamine was determined. It is determined that the water content of chloroacetic acid is 0.5 wt%, and the water content of trimethylamine is 0.5 wt%.
[0023] Put 232ml of chloroform into the reaction kettle, start stirring, then add 94.5g of solid chloroacetic acid into the reaction kettle, control the temperature at 30°C and slowly feed 59.1g of gaseous trimethylamine, and keep the gauge pressure of the reaction kettle after passing through 0.1MPa, stirring and heat preservation reaction for 6 hours, after the reaction, cool down to 25°C, stand still for crystallization, and then centrifuge, the centrifuged product is then crystallized in water, washed with chloroform after crystallization, and dried to obtain 90.4g Betaine hydrochloride with perfect crystal form, organic solvent and raw materials are recycled.
Embodiment 2
[0025] Put 346ml of DMF into the reactor, start stirring, then add 141.7g of chloroacetic acid with a water content of 1wt% into the reactor, control the temperature at 40°C and slowly feed 88.6g of trimethylamine with a water content of 1wt%, and Finally, keep the gauge pressure of the reactor at 0.2MPa, stir and heat-preserve for 8 hours, cool to 25°C after the reaction, let it stand for crystallization, then centrifuge, wash with DMF, and dry to obtain 92g of betaine hydrochloride, organic solvent and raw materials Cycle through.
Embodiment 3
[0027] Before the reaction, the water content of chloroacetic acid and trimethylamine was determined to be 1 wt%, respectively, and the amount of raw materials required for the reaction was obtained according to the molar ratio of chloroacetic acid to trimethylamine and the molar ratio of water content to water removal agent. The operation steps are as follows:
[0028] Put 308ml of toluene into the reactor, start stirring, then add 80g of chloroacetic acid with a water content of 1wt% in the reactor, then add 15.9g of chloroacetic anhydride, control the temperature at 45°C and slowly feed 59.1g of chloroacetic acid with a water content of 1wt% trimethylamine, keep the gauge pressure of the reactor at 0.1MPa after passing through, stir and heat-preserve for 5 hours, cool down to room temperature after the reaction, stand for crystallization, then centrifuge, crystallize in water, wash with toluene, and dry to obtain 120.2 g betaine hydrochloride, organic solvents and raw mater...
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