A preparation method for Ascorbyl Magnesium Phosphate, comprising the following processing steps:
(1) Add 110Kg vitamin C, 8.8Kg anhydrous calcium chloride, and 110Kg deionized water into a 500L reaction kettle at -10°C, stir for 2 hours, then add dropwise a 30% sodium hydroxide aqueous solution to adjust the pH 5, then add 110Kg of sodium trimetaphosphate, keep the temperature at 25°C, and react for 2 hours, and the obtained reactant is vitamin C ester calcium;
(2) Ascorbic acid ester calcium is added in the 500L bucket cleaner and washed with water, and then the pH is adjusted to 1.5 with sulfuric acid, and the reactant obtained is ascorbic acid phosphate;
(3) Carry out nanofiltration membrane filtration with Ascorbyl Magnesium Phosphate through the roll-type nanofiltration membrane filter, the temperature at the roll-type nanofiltration membrane filter inlet is 120°C, and the temperature at the roll-type nanofiltration membrane filter outlet is 30°C; The filter membrane has a nano-scale pore size, and the molecular weight cut-off of the nanofiltration membrane is 500. The roll-type nanofiltration membrane filter has a high removal rate of inorganic salts, and the removal rate is 90%;
(4) Add the filtrate obtained by filtering in step (3) into a 500L reaction kettle, and elute with 0.05M hydrochloric acid and 0.5M hydrochloric acid successively through a weakly basic anion exchange resin, collect the eluted part, and the eluted part is continuously stirred Regulating pH with magnesium oxide is 7, and the reactant obtained is vitamin C phosphate magnesium;
(5) Ascorbyl Magnesium Phosphate is filtered through an activated carbon filter to remove the precipitate, and the filtrate is concentrated under reduced pressure at 30°C to one-fifth of the original volume, and the volume is 3 times that of the concentrated filtrate. Ethanol with a content of 95% is added, and then passed through a spray dryer Drying, the drying temperature is 140 DEG C, and the drying time is 30 minutes, to obtain 79.85 kg of white magnesium ascorbic acid phosphate, and the content of magnesium ascorbic acid phosphate is 97.75%.
The production method of Ascorbyl Magnesium Phosphate, Ascorbyl Magnesium Phosphate is made up of vitamin C, sodium trimetaphosphate, calcium hydroxide, calcium chloride, is characterized in that: 50% vitamin C, 30% sodium trimetaphosphate, 20% The calcium hydroxide is added into the esterification pot for chemical reaction, fully stirred; then an appropriate amount of calcium chloride is added to generate vitamin C phosphate; the generated vitamin C phosphate is added with an appropriate amount of magnesium oxide, refined and dried , drying, crushing, testing, and packaging into Ascorbyl Magnesium Phosphate products. During specific implementation, esterification: drop 70-80kg of solid alkali into the alkali-dissolving tank and start the agitator for 10-15 minutes to dissolve, drop into 130-150kg of vitamin C in the esterification pot and fully stir and dissolve for 10-20 minutes, Slowly add lye into the reaction pot, control the reaction temperature within 20-35°C, and constantly test the ph value, when the ph value reaches 6-8, put 90-120kg of sodium trimetaphosphate into the pot, and continue to add alkali , When the pH value reaches 11-13, stop adding alkali, and keep stirring for about 2 hours. Drying and granulation: put the esterification material into the centrifuge, the filling capacity is two-thirds of the capacity of the centrifuge, and discharge the material after drying for 2 hours. The dry material discharged from the centrifuge is granulated and dried by the granule shaking mechanism. Drying and crushing: Add 150kg-200kg of granules to the hopper each time, control the inlet air temperature at 110-135°C during drying, and discharge the material when the outlet air temperature reaches 70-80°C. Delivery: Each batch is accurately weighed 20kg and acidified with an appropriate amount of anion resin. After acidification, it is put into a reaction tank with 500L of soft water, and the agitator is turned on. After stirring for 2 hours, 400L is accurately measured and poured into the reaction tank. Neutralization: prepare 50% magnesium oxide aqueous solution with soft water for later use, start stirring, slowly add magnesium oxide aqueous solution into the reaction tank, and finally adjust the pH value between 8-9, and control the entire magnesium addition time at about 2 hours. The feed liquid reacts fully with magnesium oxide for about 5 hours, starts to filter the magnesium slag, heats it for decolorization for 40 minutes and pumps charcoal, and sends the feed liquid to the crystallization tank to be crystallized. Crystallization: Control the temperature in the crystallization tank at 50-60°C, start to add alcohol slowly and uniformly, the process of adding alcohol is 1.5-2 hours, keep the crystal for 2 hours, turn on the cooling water to cool down, when the temperature drops to 30-40°C , start centrifuging to dry. Refining: each batch weighs 40kg of crystallized dry material and pumps it into a melting material tank with 400L of soft water, stirs and dissolves it for 24 hours, pumps the clarified liquid into the crystallization tank, opens the steam valve and raises the temperature to 50-60°C, and slowly adds 80-120L alcohol, after clarification, take out the clarified liquid, keep warm and grow the crystal for 2 hours, start to cool down, when the temperature drops to 30-40°C, start centrifugal drying, and discharge the material for drying. Drying, crushing, sieving, packaging: Put the same amount of refined semi-dry material into the drying bag and put it into the drying box, open the vacuum and heating valve, control the drying temperature to 38-55°C, and the vacuum degree to be above 0.8Mpa , drying for 20-24 hours, the dried material is crushed, sieved, and packaged after laboratory inspection.