Green synthesis process of betaine hydrochloride
A green synthesis, hydrochloride technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of complex separation process, environmental pollution, environmental pollution, etc., achieve short process flow and lower reaction temperature , the effect of shortening the reaction time
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Embodiment 1
[0015] At room temperature, put calcium chloroacetate into a reaction flask equipped with a stirring and reflux condenser, add water at a weight ratio of 3.5 times, and slowly add 30% trimethylamine dropwise at a molar ratio of calcium chloroacetate to trimethylamine of 1:2.2 Aqueous solution, the temperature of the control system does not exceed 40°C. After the feeding is completed, keep it warm at 40°C for 1.5 hours; the reaction solution is acidified with sulfuric acid to make the pH = 1, until there is no white precipitate, filter, and the filter cake is dried to obtain the by-product calcium sulfate ; The filtrate was evaporated and concentrated until a large number of solid crystals were precipitated, and dried under normal pressure at 100 ° C to obtain betaine hydrochloride.
Embodiment 2
[0017] At room temperature, put chloroacetic acid into a reaction flask equipped with stirring and reflux condenser, add 4.5 times the weight ratio of water to dissolve, put into calcium hydroxide for neutralization according to the molar ratio of chloroacetic acid and calcium hydroxide at 2:1.05, and then press The molar ratio of chloroacetic acid and trimethylamine is 1: 2.0 and slowly add 30% trimethylamine aqueous solution dropwise, and the temperature of the control system does not exceed 40°C. After the addition is completed, it is kept at 40°C for 3 hours; the reaction solution is acidified with sulfuric acid to make pH = 1.5, until there is no white precipitate, filter, and dry the filter cake to obtain calcium sulfate as a by-product; the filtrate is evaporated and concentrated until a large amount of solid crystals are precipitated, and then vacuum-dried to obtain betaine hydrochloride.
Embodiment 3
[0019] At room temperature, put chloroacetic acid into a reaction flask equipped with stirring and reflux condenser, add water with a weight ratio of 4.5 times, and put in calcium carbonate for neutralization according to the molar ratio of chloroacetic acid and calcium carbonate at 2:11, then press chloroacetic acid and calcium carbonate The molar ratio of trimethylamine is 1:2.1, slowly add 30% trimethylamine aqueous solution dropwise, and the temperature of the control system does not exceed 40°C. After the addition is completed, keep the temperature at 40°C for 2 hours; the reaction solution is acidified with sulfuric acid to make pH=1.0 , until there is no white precipitate, filter, and dry the filter cake to obtain the by-product calcium sulfate; the filtrate is evaporated and concentrated until a large amount of solid crystals are precipitated, and dried under normal pressure at 105°C to obtain betaine hydrochloride. Example 4
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