The item of the present innovation is to get rid of the shortages existing in the prior art, give a kind of prep work method of Magnesium Ascorbyl Phosphate with basic technique, practical operation, low cost and also high yield, this technique does not make use of organic solvent in the preparation procedure, aftertreatment It is straightforward, does not trigger environmental pollution, as well as the ready item has high purity.
According to technical plan given by the innovation, a kind of preparation approach of Magnesium Ascorbyl Phosphate, is characterized because, consists of the complying with processing steps:
( 1) including vitamin C, anhydrous calcium chloride, deionized water according to the mass ratio of 1: (0.08 ~ 0.4): (1 ~ 5) temperature is in the activator of -10 ~ 20 DEG C, mixes 2 ~ For 3 hrs, include the sodium hydroxide liquid remedy with a focus of 30 ~ 70% dropwise, readjust the pH to 5 ~ 10.5, then add sodium trimetaphosphate with 1 ~ 2.5 times the quantity of vitamin C, keep the temperature level at 25 ~ 45 ° C, and respond 2 ~ 6 hrs, the obtained reactant is vitamin C ester calcium;
( 2) adding vitamin C ester calcium into the container cleaner to wash with water, and afterwards readjusting the pH with sulfuric acid to be 1.5 to 3.5, as well as the gotten reactant is vitamin C phosphate;
( 3) execute nanofiltration membrane purification with vitamin C phosphate via the roll kind nanofiltration membrane layer filter, the temperature level of the roll kind nanofiltration membrane filter inlet is 120 ～ 140 ℃, and the temperature level of the roll type nanofiltration membrane layer filter electrical outlet is 30 ～ 50 ℃; Nanofiltration membrane has nanometer pore dimension, the molecular weight cut-off of nanofiltration membrane layer is 500 ～ 1500, and also the roll type nanofiltration membrane filter has greater removal price to not natural salt, as well as removal rate is 90 ～ 98 %;
( 4) adding the filtrate acquired by the action (3) purification into the activator, through weakly standard anion exchange resin, eluting with 0.05 M hydrochloric acid and also 0.5 M ～ 1.5 M hydrochloric acid together, gathering the elution component, as well as the elution component is continuously Adjusting pH with magnesium oxide under mixing is 7 ～ 11, as well as the reactant that gets is vitamin C magnesium phosphate;
( 5) Magnesium Ascorbyl Phosphate is filtered to eliminate rainfall through gac filter, filtrate is concentrated to one-fifth of original volume at 30 DEG C under minimized pressure, adding quantity is that 3 ～ 6 times of focused filtrate content is 95% ethanol, then by Spray clothes dryer drying out, drying out temperature level is 140 ～ 160 ℃, and also drying out time is 30 ～ 40min, promptly obtains explained Magnesium Ascorbyl Phosphate completed product.
Compared with the previous art, the present development has the complying with benefits:
The phosphoric acid esterification response of today development is performed in an aqueous solvent, does not make use of an organic solvent, and also the whole process is straightforward, not only accelerates the phosphoric acid esterification response rate, reduces the response time, simplifies the operation treatment, yet also is eco secure; a new sort of nanofiltration membrane is used. process, the elimination efficiency of contaminations is high, and the pureness of the ended up Magnesium Ascorbyl Phosphate is greater than 95%, and the security is excellent.
