A kind of preparation method of agmatine hydrochloride
A technology of agmatine hydrochloride and agmatine sulfate, which is applied in the field of preparation of agmatine hydrochloride or waste liquid treatment, and can solve problems such as large safety hazards, many side reactions, and cumbersome operations , to achieve the effect of reducing carbon emissions and increasing social benefits
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Embodiment 1
[0024] Take agmatine sulfate crystallization mother liquor with a content of 10g / L for a total of 5L, concentrate under reduced pressure at a vacuum degree of -0.09mpa, and a temperature of 70±5°C to remove the solvent in the mother liquor, collect and distill under reduced pressure to concentrate 3.5L of solvent, and the remaining Feed liquid passes through anion resin 717 with a flow rate of 25-30ml / min. When 1.5L of the lower column liquid is collected, there is turbidity in spotting with barium chloride at the outlet. Concentrate to 150ml under vacuum conditions, adjust the pH to 3.8 with 20% hydrochloric acid solution, add 2.25g of activated carbon, stir at room temperature for 40min, filter, remove carbon, and pass the filtrate through a fiber resin water-based membrane again with a pore size of 0.45μm. Add ethanol with a concentration of 95% to the 25°C crystallization liquid while stirring. When the feed liquid becomes cloudy, stop adding ethanol dropwise. After growing...
Embodiment 2
[0027] Take agmatine sulfate crystallization mother liquor 15g / L content to be 4L altogether, in vacuum degree be-0.09MPa, temperature is 70 DEG C and concentrates under reduced pressure to remove the solvent in the mother liquor, collects and distills under reduced pressure and concentrates out solvent 3L, and the remaining material liquid is passed through Anion resin 717, the flow rate is 25-30ml / min, when 1.2L of the lower column liquid is collected, there is turbidity in spotting with barium chloride at the outlet, stop the collection, and continue to vacuum the collected lower column liquid at a temperature of 70±5°C Concentrate to 170ml, adjust the pH to 4.2 with hydrochloric acid solution, add 2.55g of activated carbon, stir at room temperature for 40min, filter, remove carbon, and pass the filtrate through a fiber resin water-based membrane again with a pore size of 0.45μm. Add ethanol with a concentration of 95% to the crystallization liquid at 20°C while stirring. Wh...
Embodiment 3
[0030] Take agmatine sulfate crystallization mother liquor with 10g / L content of 4L in total, concentrate under reduced pressure at a vacuum degree of -0.009MPa and a temperature of 68°C to remove the solvent in the mother liquor, collect and distill and concentrate under reduced pressure 2.8L of solvent, and remove the remaining material The liquid passes through anion resin 717 with a flow rate of 25-30ml / min. When 1.5L of the lower column liquid is collected, the barium chloride spotting sample at the outlet is turbid. Stop the collection and continue to concentrate the collected lower column liquid in vacuum at a temperature of 68°C. to 120ml, adjust the pH to 3.8 with hydrochloric acid solution, add 1.8g of activated carbon, stir at room temperature for 40min, filter, remove carbon, and pass the filtrate through a fiber resin water-based membrane to pass 0.45μm again. Add ethanol to the crystallization liquid at 30°C while stirring. When the feed liquid becomes cloudy, sto...
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