Preparation method of betaine preparation with low sodium chloride content and low hygroscopicity
A low hygroscopicity, betaine technology, applied in the preparation of organic compounds, chemical instruments and methods, cyanide reaction preparation and other directions, can solve the problem of lack of low-cost and high-efficiency separation and purification methods, and achieve broad promotion prospects and market value, The separation method is simple and the effect of improving the stability
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Embodiment 1
[0051] Betaine purification and preparation
[0052] (1) After betaine is prepared as main raw material with chloroacetic acid, sodium hydroxide, trimethylamine, 1.25kg of the product mixed solution that will contain betaine, sodium chloride evaporates and concentrates at 110 ℃ in the falling film concentrator, concentrates to Stop concentrating when feed liquid begins to separate out solid, feed liquid is transferred in the vacuum distillation crystallization still and regulate pH to be 8, when distilling to water content at 105 ℃, be cooled to 60 ℃, add 45ml methyl alcohol (about 100% of water) Weight 15wt%) as a betaine co-solvent, stir and mix evenly, filter, collect the precipitated solid 1 (mainly sodium chloride component), and move the filtrate to a vacuum rotary evaporator.
[0053] (2) Under the vacuum condition of -0.06Mpa and the temperature of 100°C, the filtrate was evaporated until the water content was 15%, the evaporation was stopped, the temperature was lower...
Embodiment 2
[0060] (1) After preparing betaine with chloroacetic acid, sodium carbonate and trimethylamine as the main raw materials, 116.8kg of the product mixed solution was evaporated and concentrated at 110°C until the feed liquid precipitated solids, and the feed liquid was transferred to a vacuum distillation crystallization kettle and adjusted When the pH is 7.5, vacuum distill at 105°C until the water content is 35.8%, cool down to 60°C, add 5.6L of methanol as betaine co-solvent, stir and mix evenly, filter, collect the precipitated solid 1, and move the filtrate to vacuum in a rotary evaporator.
[0061] (2) Under the vacuum condition of -0.06Mpa and the temperature of 105°C, evaporate the filtrate until the water content is 15%, stop evaporation, cool down to 70°C, filter and separate the precipitated solid to obtain crystalline solid 2; filter the mother liquor in the crystallizer Slowly and uniformly cool in the medium, cooling crystallization, in the whole cooling crystalliz...
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