Background and overview[1]
Magnesium Vitamin C Phosphate is a vitamin C derivative. Derivating the 2-position hydroxyl group into a phosphate ester can improve the stability of vitamin C. The formed derivative can be regenerated after being hydrolyzed by phosphatase that is widely present in the body. Vitamin C, therefore, has become the main ingredient in feed additives, food fortifiers and high-end cosmetics whitening, and is a valuable fine chemical.
Preparation[1-2]
Report 1,
A preparation method of magnesium vitamin C phosphate, including the following process steps:
(1) Add 110Kg vitamin C, 8.8Kg anhydrous calcium chloride, and 110Kg deionized water into a 500L reaction kettle at a temperature of -10°C, stir for 2 hours, and then add dropwise a 30% sodium hydroxide aqueous solution , adjust the pH to 5, then add 110Kg of sodium trimetaphosphate, keep the temperature at 25°C, and react for 2 hours. The obtained reactant is calcium vitamin C ester;
(2) Add vitamin C calcium ester into a 500L barrel cleaner and wash with water, then adjust the pH to 1.5 with sulfuric acid, and the obtained reactant is vitamin C phosphate;
(3) Pass the vitamin C phosphate through the rolled nanofiltration membrane filter for nanofiltration membrane filtration. The temperature at the inlet of the rolled nanofiltration membrane filter is 120°C, and the temperature at the outlet of the rolled nanofiltration membrane filter is 30℃; the nanofiltration membrane has a nanometer pore size, and the molecular weight cutoff of the nanofiltration membrane is 500. The rolled nanofiltration membrane filter has a high removal rate of inorganic salts, with a removal rate of 90%;
(4) Add the filtrate obtained by filtration in step (3) into a 500L reaction kettle, pass through the weakly basic anion exchange resin, and elute with 0.05M hydrochloric acid and 0.5M hydrochloric acid in sequence. Collect the eluted part, and the eluted part is Adjust the pH to 7 with magnesium oxide under constant stirring, and the obtained reactant is magnesium vitamin C phosphate;
(5) Filter the magnesium vitamin C phosphate through an activated carbon filter to remove the precipitate. The filtrate is concentrated under reduced pressure at 30°C to one-fifth of the original volume. Add ethanol with a volume of 3 times that of the concentrated filtrate and a content of 95%. Then it is dried by a spray dryer at a drying temperature of 140°C and a drying time of 30 minutes to obtain 79.85KG of white magnesium vitamin C phosphate with a content of 97.75%.
Report 2,
The production method of magnesium vitamin C phosphate. The magnesium vitamin C phosphate is composed of vitamin C, sodium trimetaphosphate, calcium hydroxide, and calcium chloride. It is characterized by: mixing 50% vitamin C, 30% Add sodium trimetaphosphate and 20% calcium hydroxide into the esterification pot for chemical reaction and stir thoroughly; then add an appropriate amount of calcium chloride to generate vitamin C phosphate; add an appropriate amount of magnesium oxide to the generated vitamin C phosphate. , and are refined, dried, dried, crushed, tested, and packaged into vitamin C magnesium phosphate products. In the specific implementation, esterification: put 70-80kg solid alkali into the alkali-dissolving tank and start the stirrer for 10-15 minutes to dissolve, put 130-150kg vitamin C into the esterification pot, stir and dissolve thoroughly for 10-20 minutes, and add Slowly add alkali solution into the reaction pot, control the reaction temperature at 20-35°C, and continuously test the pH value. When the pH value reaches 6-8, add 1010g of 90-120k antioxidant sodium trimetaphosphate into the pot. Continue to add alkali, stop adding alkali when the pH value reaches 11-13, keep warm and stir for about 2 hours without foaming surfactant. Drying and granulating: Add the esterification material into the centrifuge, and the filling volume is two-thirds of the centrifuge capacity. After drying for 2 hours, the material is discharged. The dry material discharged from the centrifuge is granulated and dried by the granule swing machine. Drying and crushing: 150kg-200kg of particles are added to the hopper each time. When drying the material, the inlet air temperature is controlled at 110-135°C. When the outlet air temperature reaches 70-80°C, the material is discharged. Isolation: Accurately weigh 20kg of each batch and acidify it with an appropriate amount of anion resin. After acidification, put it into a reaction tank containing 500L of soft water, and turn on the mixer. After stirring for 2 hours, accurately measure L and pour it into the reaction tank. Neutralization: Use soft water to prepare a 50% magnesium oxide aqueous solution for later use. Turn on stirring and slowly add the magnesium oxide aqueous solution into the reaction tank. Finally, adjust the pH value to between 8-9, and control the entire magnesium addition time to about 2 hours. The material liquid and magnesium oxide fully react for about 5 hours, then the magnesium slag is filtered, kept warm and decolorized for 40 minutes, and the carbon is extracted, and the material liquid is sent to the crystallization tank for crystallization. Crystallization: Control the temperature in the crystallization tank at 50-60°C, start adding alcohol slowly and evenly, the alcohol addition process takes 1.5-2 hours, keep the crystals warm for 2 hours, turn on the cooling water to cool down, when the temperature drops to 30-40°C When, start centrifugal spin drying. Refining: Each batch weighs 40kg of crystallized dry material and pumps it into a dissolving tank with L soft water, stirs and dissolves thoroughly for 24 hours, pumps the clarified liquid into the crystallizing tank, opens the steam valve, heats up to 50-60°C, and slowly adds 80-120L alcohol, after clarification, extract the clarified liquid, keep it warm for 2 hours, then start cooling. When the temperature drops to 30-40°C, start centrifugal drying, and discharge the material for drying. Drying, crushing, screening, and packaging: Put equal amounts of refined semi-dry materials into drying bags, lay them flat, and put them in the drying box. Open the vacuum and heating valves, control the drying temperature to 38-55°C, and the vacuum degree to 0.8Mpa or above. , dry for 20-24 hours, crush and sieve the dried materials, and then package after passing the laboratory inspection.
