A kind of preparation method of magnesium L-ascorbic acid-2-monophosphate
A technology of ascorbic acid and monophosphate, which is applied in the field of preparation of L-ascorbic acid-2-monophosphate magnesium, can solve the problem of high purity of L-ascorbic acid-2-monophosphate magnesium, and achieve the effect of simple post-processing
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Embodiment 1
[0015] In a 500L reactor, add 200 kg of water, cool to -5 degrees Celsius, add 100 kg of Vc and 20 kg of calcium chloride, stir for 2 hours, then slowly add 40% calcium hydroxide aqueous solution, adjust Ph to 7.5, add 100 kg of sodium trimetaphosphate , keep the temperature at 25 degrees Celsius, and react for 2.5 hours. Wash the above reaction product with water, then adjust the pH value to 1.8 with hydrochloric acid, filter, pass the filtrate through a weakly basic anion exchange column, and elute with 0.02M hydrochloric acid and 0.5M hydrochloric acid in sequence, collect the eluted part and oxidize it under constant stirring. Adjust the pH to 9 with magnesium, remove the precipitate by filtration, concentrate the filtrate under reduced pressure at 40°C to 1 / 5 of the original volume, add 3 times 95% ethanol, crystallize, collect by centrifugation, break after washing, and dry in a fluidized bed to obtain white 72.48 kg of magnesium L-ascorbyl-2-phosphate, the content of ma...
Embodiment 2
[0017] In a 1000L reactor, add 300 kg of water, cool to 2 degrees Celsius, add 100 kg of Vc and 30 kg of calcium chloride, stir for 1.5 hours, then slowly add 20% calcium hydroxide aqueous solution, adjust Ph to 6, add sodium trimetaphosphate 80 kg, keep the temperature at 35 degrees Celsius, and react for 4 hours. Wash the above reaction product with water, then adjust the pH value to 0.5 with sulfuric acid, filter, pass the filtrate through a weakly basic anion exchange resin, and successively elute with 0.02M hydrochloric acid and 0.2M hydrochloric acid, collect the eluted part and oxidize it with constant stirring Adjust the pH to 10 with magnesium, remove the precipitate by filtration, concentrate under reduced pressure, add 2 times of 95% ethanol, crystallize, centrifuge, wash, and dry in a fluidized bed to obtain 69.67 kg of white magnesium L-ascorbic acid-2-phosphate, L- Magnesium ascorbyl-2-monophosphate content 98.20%.
Embodiment 3
[0019] In a 500L reactor, add 100 kg of water, cool to 10 degrees Celsius, add 100 kg of Vc and 5 kg of calcium chloride, stir for 1 hour, then slowly add 60% calcium hydroxide aqueous solution, adjust Ph to 9.5, add 150 kg of sodium trimetaphosphate , keep the temperature at 15 degrees Celsius, and react for 1 hour. Wash the above reaction product with water, then adjust the pH value to 3 with oxalic acid, filter, pass the filtrate through a weakly basic anion exchange resin, and successively elute with 0.02M hydrochloric acid and 0.8M hydrochloric acid, collect the eluted part, and wash with Adjust the pH to 8.0 with magnesium oxide, remove the precipitate by filtration, concentrate under reduced pressure, add 4 times of 95% ethanol, crystallize, centrifuge, wash, and dry in a fluidized bed to obtain 71.45 kg of white magnesium L-ascorbic acid-2-phosphate, L - Magnesium ascorbyl-2-monophosphate content 96.70%.
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