CN1221559C - Novel method for preparing VC magnesium phosphate ester - Google Patents
Novel method for preparing VC magnesium phosphate ester Download PDFInfo
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- CN1221559C CN1221559C CN 03133674 CN03133674A CN1221559C CN 1221559 C CN1221559 C CN 1221559C CN 03133674 CN03133674 CN 03133674 CN 03133674 A CN03133674 A CN 03133674A CN 1221559 C CN1221559 C CN 1221559C
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 229960002261 magnesium phosphate Drugs 0.000 title abstract 3
- 229910000157 magnesium phosphate Inorganic materials 0.000 title abstract 3
- 239000004137 magnesium phosphate Substances 0.000 title abstract 3
- -1 magnesium phosphate ester Chemical class 0.000 title abstract 3
- 235000010994 magnesium phosphates Nutrition 0.000 title abstract 3
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical group ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 3
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 claims description 51
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 33
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000000395 magnesium oxide Substances 0.000 claims description 11
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 11
- 239000012043 crude product Substances 0.000 claims description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003456 ion exchange resin Substances 0.000 claims description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 4
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- RLOWWWKZYUNIDI-UHFFFAOYSA-N phosphinic chloride Chemical compound ClP=O RLOWWWKZYUNIDI-UHFFFAOYSA-N 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005886 esterification reaction Methods 0.000 abstract description 3
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 abstract 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- 239000007791 liquid phase Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 238000001914 filtration Methods 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000010812 external standard method Methods 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- MIJPAVRNWPDMOR-ZAFYKAAXSA-N L-ascorbic acid 2-phosphate Chemical compound OC[C@H](O)[C@H]1OC(=O)C(OP(O)(O)=O)=C1O MIJPAVRNWPDMOR-ZAFYKAAXSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910019213 POCl3 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000026731 phosphorylation Effects 0.000 description 1
- 238000006366 phosphorylation reaction Methods 0.000 description 1
- 210000002381 plasma Anatomy 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
- PBSRSWFGYPZDAU-FFIPNUABSA-H trimagnesium;[(2r)-2-[(1s)-1,2-dihydroxyethyl]-3-oxido-5-oxo-2h-furan-4-yl] phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].OC[C@H](O)[C@H]1OC(=O)C(OP([O-])([O-])=O)=C1[O-].OC[C@H](O)[C@H]1OC(=O)C(OP([O-])([O-])=O)=C1[O-] PBSRSWFGYPZDAU-FFIPNUABSA-H 0.000 description 1
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- Cosmetics (AREA)
Abstract
The present invention relates to a novel method for preparing VC magnesium phosphate ester by taking VC as raw material. When VC prepares 5, 6-O-isopropylidene VC, the used catalyst is phosphorus oxychloride which is the same with the raw material used in the phosphonic acid esterification reaction in the next step. In this way, the purchase and the management of one material are reduced. Moreover, the produced 5, 6-O-isopropylidene VC can be directly used for the phosphonic acid esterification reaction in the next step without being filtered and separated. The method saves time, labor and energy. The produced VC magnesium phosphate ester has high purity and accords with the cosmetic-stage standard requirements.
Description
(1) technical field
The invention belongs to the synthetic field of medicine, be specifically related to a kind of novel method for preparing VC phosphate magnesium.
(2) background technology
VC phosphate magnesium (Ascorbyl Phosphate Magnesium, be called for short AP-Mg) is one of the most stable VC derivative of chemical property, and entering behind the human body rapidly, enzymolysis become VC.Its stability shows and is difficult for oxidation, is not afraid of alkali, is not subjected to that metal ion influences etc., as at ambient temperature, in the environment of 75% relative humidity, stores 24 months, and serviceability rate is still more than 95%; And for example 218 ℃ of bakings 25 minutes, structure was constant.Its these advantages have overcome the unstable easily oxygenolysis of VC itself, and the deficiency that application conditions is limited has enlarged the range of application of VC indirectly.VC phosphate magnesium has been widely used in the product that needs such as food, feed, makeup, washing composition, blood plasma add VC at present, and the VC multipath is played a role.
VC phosphate magnesium molecular formula and molecular weight: C6H6O9PMg1.5.5H2O=379.61
Structural formula:
VC phosphate magnesium preparation method reports more, as:
(1) VC direct esterification method (Japanese Patent 43-218,52-18191, United States Patent (USP) 3,671,549), the product that makes is a mixture, is difficult to by the VC phosphate magnesium that separates, purifying obtains higher degree.
(2) earlier with VC 5, hydroxyl on 6 makes 5 through ketal reaction, 6-O-isopropylidene VC, carry out the phosphating reaction method again, as United States Patent (USP) 4,999, the preparation method of the 437 VC phosphate magnesium of introducing is such: 24% oleum is added in the acetone, slowly add VC, 0 ℃ was reacted 6 hours, be cooled to-15 ℃, filter filter cake 5,6-O-isopropylidene VC changes in the aqueous solution that adds pyridine in advance after can pressing dry without washing, transfer PH 12-13 with KOH, slowly add POCL3 with this understanding, after adding, 0 ℃ is incubated 30 minutes, and then add MgCl2.6H2O (being made into 30% aqueous solution in advance), stirred crystallization 1 hour, filter, remove inorganic salt K.Mg.PO4.6H2O, filtrate adds methyl alcohol after being concentrated into certain volume, stirs 1 hour, crystallization, filter, remove inorganic salt KCl once more, after the filtrate behind twice desalination is concentrated into certain volume, exchange with strong acid ion exchange resin, collect exchange liquid and elutriant (PH 1.2-0.8), add the oxidation reactive magnesium, excessively behind a small amount of insolubles of filtering, filtrate adds methyl alcohol after being concentrated into certain volume, stir, crystallization filters, washing is dry, (throw VC120g, get VC phosphate magnesium 190～210g, wherein impurity 2 to get VC phosphate magnesium, the content 3%-7% of 2-2-VC magnesium phosphorate, VC content 42～46%).
The operation steps of the above-mentioned method (2) for preparing VC phosphate magnesium is more loaded down with trivial details, wherein not only increased by twice operating process except that inorganic salt, and the first step make 5,6-O-isopropylidene VC must filtering separation come out from reaction solution, so be difficult to make qualified 5 at wet season, 6-O-isopropylidene VC, reason is 5,6-O-isopropylidene VC filters ingress of air and resolves into VC very soon under acidic conditions.A large amount of use oleums (1: 0.3～0.4) are arranged again, severe corrosion equipment not only, and cause environmental pollution.The purity of the VC phosphate magnesium that makes of method (2) is relatively poor in addition, makes with extra care with solvent, even if refining rate is low by 40% o'clock, purity does not still reach the requirement of cosmetics-stage.Food grade standard VC phosphate magnesium, content 〉=85%, and cosmetics-stage standard VC phosphate magnesium, content 〉=95%.
(3) CN1025858C (Granted publication day: on September 7th, 1994) disclose a kind of method of the 2-of production Ascorbic acid 2-phosphate.This method is to make to choose on 5-position and 6-position protected xitix wantonly and carry out phosphorylation simultaneously, maintains in the reaction mixture arbitrarily selectively the concentration of protected xitix less than 0.3M, and removes any blocking group when needed.The contriver says, adopts its inventive method, but high yield and produce the 2-Ascorbic acid 2-phosphate with industrially scalable.17 of examples are disclosed in the patent specification, 3 of comparison example, 1 of reference example.VC-2-magnesium phosphorate output that preceding two kinds of examples provide and yield are measured to come from reaction solution by the high-pressure liquid phase external standard method, are not the yield of the VC-2-magnesium phosphorate finished product taken.To from reaction solution, take finished product and also need pass through ion-exchange, salify, refining three steps.Thus, can not simply VC-2-magnesium phosphorate yield in the reaction solution of measuring with the high-pressure liquid phase external standard method be compared with the finished product VC phosphate magnesium yield of taking.Press the finished product that the embodiment method obtains and measure with the used high-pressure liquid phase method of the present invention, content only about 85% only meets the food grade standard.Reference example has provided the method for taking VC phosphate magnesium from reactant, but product yield remains and calculate from reaction solution, and content measures out with the high-pressure liquid phase area percent.And do not have comparability with high-pressure liquid phase area percent method and the content of measuring with the high-pressure liquid phase external standard method.So the method for preparing VC phosphate magnesium that method (3) provides is not only loaded down with trivial details, and quality product does not meet the cosmetics-stage requirement.
(3) summary of the invention
The technical problem to be solved in the present invention provides a kind of new method for preparing VC phosphate magnesium, to make the VC-magnesium phosphorate that meets the cosmetics-stage standard.
The technical scheme that adopts is:
The novel method of preparation VC phosphate magnesium comprises following reactions steps:
(1), with acetone, phosphorus oxychloride, VC, in VC: the ratio of acetone: phosphorus oxychloride=1g: 4.2ml: 0.1-0.2ml adds in the reaction flask 0-50 ℃ successively, stirs after 1-10 hour, is directly used in down the step phosphating reaction.
(2), water, sodium hydroxide are added in the reaction flask, reaction solution with above-mentioned (1) changes over to wherein again, acetone is reclaimed in underpressure distillation, last solution adds quantitative pyridine, stirring is cooled to 0-10 ℃, transfers reaction solution PH 12-13 with sodium hydroxide solution, drips phosphorus oxychloride, maintain the temperature at 0-10 ℃ simultaneously, PH 12-13.Drip off, continue reaction 30 minutes.VC: water: sodium hydroxide: pyridine: phosphorus oxychloride=1g: 25-26ml: 0.5-0.8g: 1.02ml: 0.67ml;
(3), the pyridine in the reclaim under reduced pressure reaction solution 2, the raffinate thin up is doubly measured to the 37-38 of Vc input amount, promptly corresponding to 1g VC, thin up is to 37-38ml, again through the exchange of 732# ion exchange resin, wash-out is collected exchange liquid and elutriant about PH2.5.
(4), in above-mentioned exchange liquid, add magnesium oxide, magnesium oxide add-on and VC are than being VC: magnesium oxide=1g: 1.60-1.73g.In 30-35 ℃ of stirring, reacted 1-2 hour, to filter, filtrate is concentrated into VC: concentrated solution=1g: behind the 8-10ml, add methyl alcohol, making the concentrated solution and the ratio of methyl alcohol is concentrated solution: methyl alcohol=1ml: 2ml, stirs, and crystallization filters, and drying gets VC phosphate magnesium crude product.
(5), above-mentioned VC phosphate magnesium crude product added a certain amount of water dissolution after, add activated carbon decolorizing, add methyl alcohol, stirring and crystallizing is filtered, washing, drying promptly gets VC phosphate magnesium elaboration.Refining rate 73%-75%, the VC phosphate Mg content can reach 95%-98%, wherein impurity 2,2 '-content＜0.5% of 2-VC magnesium phosphorate, adding the water yield is VC phosphate magnesium: water=1g: 5-10ml.
Wherein, step (1) reaction times is 2-4 hour, and temperature of reaction is 20-30 ℃.
Preparing VC phosphate magnesium according to technical scheme of the present invention has the following advantages:
1, because in preparation 5, adopt POCl3 to make catalyzer during 6-O-isopropylidene VC, raw materials used consistent with back step Phosphation, this has not only reduced the kind of raw material, and make 5,6-O-isopropylidene VC can be without filtering separation, directly change over to down in the step material and carry out phosphating reaction, prescinded for three steps with the documents ratio and filtered, saved time, laborsaving, energy-conservation, especially 5,6-O-isopropylidene VC is without filtering separation, then can avoid or reduce it and meet air resolve into VC in filtration procedure, and the purity of product provides guarantee to the back step.
2, the VC phosphate magnesium crude product that makes of method thus only just can make the VC phosphate magnesium of cosmetics-stage standard through an one-step refining, increase substantially the added value of VC.
(4) description of drawings
Fig. 1 is the reaction process that a kind of documents prepares VC phosphate magnesium.
Fig. 2 is the reaction process of a kind of embodiment of the present invention.
(5) embodiment
Embodiment one
The novel method of preparation VC phosphate magnesium may further comprise the steps:
1, be equipped with at exsiccant and add 57.2ml acetone in the 100ml four-necked bottle of mechanical stirring, thermometer, drying tube, the 2.7ml phosphorus oxychloride stirs and adds 13.5gVC down, and 20 ℃, stirred 4 hours, stand-by.
2, in the 1000ml four-necked bottle that mechanical stirring, thermometer, PH meter, addition funnel are housed, add 342ml water, add sodium hydroxide 10.3g, stir down, stand-by reaction solution 1 is changed over to wherein, underpressure distillation removes acetone, add the 13.8ml pyridine, be cooled to 0-10 ℃, transfer reaction solution PH12-13, drip phosphorus oxychloride 9ml with aqueous sodium hydroxide solution, keep temperature 0-10 ℃ simultaneously, PH12-13 after dropwising, continues reaction 30 minutes.
3, heating in water bath, the reclaim under reduced pressure pyridine, last solution thin up is to 500ml, through the exchange of 732# ion exchange resin, collect exchange liquid and the elutriant of PH2.5, add magnesium oxide 23.4g, 30-35 ℃ was reacted 1 hour, and placement is spent the night, and filter next day, filtrate is concentrated into 120ml, adds 240ml methyl alcohol, separates out precipitation, placement is spent the night, and filter next day, washing, drying gets VC phosphate magnesium crude product 17.5g, yield 60.1%.
4, VC phosphate magnesium crude product adds the dissolving of 5 times of water gagings, add carbon decoloring after, drip methyl alcohol, crystallization, place, filter, washing is dry, gets elaboration 12.97g, refining rate 74.1%, content 96.2% (high-pressure liquid phase method mensuration), wherein impurity 2,2 '-content＜0.5% of 2-VC magnesium phosphorate.
Embodiment two
Embodiment two and embodiment one are basic identical, and its difference is:
Phosphorus oxychloride consumption in the step (1) is 2.0ml, 25 ℃ of temperature of reaction, 4 hours reaction times;
Sodium hydroxide concentration is 7.7g in the step (2);
The magnesium oxide consumption is 22.5g in the step (3);
Adding the water yield in the step (4) is 10 times that VC measures;
Crude product VC phosphate magnesium must be measured 18.1g, yield 62.1%;
Elaboration VC phosphate magnesium must be measured 13.4g, yield 74%;
Content 97.1% (high-pressure liquid phase method mensuration); Wherein impurity 2,2 '-content＜0.5% of 2-VC magnesium phosphorate.
Embodiment three
Embodiment three and embodiment one are basic identical, and its difference is:
Phosphorus oxychloride consumption in the step (1) is 1.35ml, 30 ℃ of temperature of reaction, 2 hours reaction times;
Sodium hydroxide concentration is 6.8g in the step (2);
The magnesium oxide consumption is 22.5g in the step (3);
Crude product VC phosphate magnesium must be measured 17.3g, yield 59.5%;
Elaboration VC phosphate magnesium must be measured 12.8g, yield 73.7%;
Content 95.9% (high-pressure liquid phase method mensuration), wherein impurity 2,2 '-content＜0.5% of 2-VC magnesium phosphorate.
Embodiment four
Embodiment four and embodiment one are basic identical, and its difference is:
Phosphorus oxychloride consumption in the step (1) is 2.7ml, 30 ℃ of temperature of reaction, 2 hours reaction times;
Sodium hydroxide concentration is 10.8g in the step (2);
The magnesium oxide consumption is 23.4g in the step (3);
Crude product VC phosphate magnesium must be measured 17.8g, yield 61.2%;
Elaboration VC phosphate magnesium must be measured 13.3g, yield 74.7%.
Content 96.6% (high-pressure liquid phase method mensuration), wherein impurity 2,2 '-content＜0.5% of 2-VC magnesium phosphorate.
Claims (4)
1, the novel method of preparation VC phosphate magnesium comprises following reactions steps, it is characterized in that:
(1), with acetone, phosphorus oxychloride, VC, in VC: the ratio of acetone: phosphorus oxychloride=1g: 4.2ml: 0.1-0.2ml adds in the reaction flask 0-50 ℃ successively, stirs after 1-10 hour, is directly used in down the step phosphating reaction;
(2), water, sodium hydroxide are added in the reaction flask, reaction solution with above-mentioned (1) changes over to wherein again, acetone is reclaimed in underpressure distillation, last solution adds quantitative pyridine, stirring is cooled to 0-10 ℃, transfers reaction solution PH12-13 with sodium hydroxide solution, drips phosphorus oxychloride, maintain the temperature at 0-10 ℃ simultaneously, PH12-13; Drip off, continue reaction 30 minutes, VC: water: sodium hydroxide: pyridine: phosphorus oxychloride=1g: 25-26ml: 0.5-0.8g: 1.02ml: 0.67ml;
(3), the pyridine in the reclaim under reduced pressure reaction solution 2, the raffinate thin up is doubly measured to the 37-38 of Vc input amount, promptly corresponding to 1g VC, thin up is to 37-38ml, again through the exchange of 732# ion exchange resin, wash-out is collected exchange liquid and the elutriant of PH2-3;
(4), in above-mentioned exchange liquid, add magnesium oxide, magnesium oxide add-on and VC are than being VC: magnesium oxide=1g: 1.60g-1.73g; In 30-35 ℃ of stirring, reacted 1-2 hour, to filter, filtrate is concentrated into VC: concentrated solution=1g: behind the 8-10ml, add methyl alcohol, making the concentrated solution and the ratio of methyl alcohol is concentrated solution: methyl alcohol=1ml: 2ml, stirs, and crystallization filters, and drying gets VC phosphate magnesium crude product;
(5), above-mentioned VC phosphate magnesium crude product added a certain amount of water dissolution after, add activated carbon decolorizing, add methyl alcohol, stirring and crystallizing is filtered, washing, drying promptly gets VC phosphate magnesium elaboration; Refining rate 73%-75%, the VC phosphate Mg content can reach 95%98%, wherein impurity 2,2 '-content＜0.5% of 2-VC magnesium phosphorate, adding the water yield is VC phosphate magnesium: water=1g: 5-10ml.
2, the novel method of VC phosphate magnesium preparation according to claim 1 is characterized in that the reaction times in the step (1) is 2-4 hour, and temperature of reaction is 20-30 ℃.
3, the novel method of VC phosphate magnesium preparation according to claim 1 is characterized in that each ratio is VC in the step (2): NaOH: pyridine: POCl
3: water=1g: 0.76g: 1.02ml: 0.67ml: 25.3ml.
4, the novel method of VC phosphate magnesium preparation according to claim 1 is characterized in that, the material ratio is VC in the step (4): MgO=1g: 1.73g.
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| CN 03133674 CN1221559C (en) | 2003-08-13 | 2003-08-13 | Novel method for preparing VC magnesium phosphate ester |
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| CN108285470B (en) * | 2018-03-28 | 2019-10-01 | 安徽泰格生物技术股份有限公司 | A method of synthesis L-Ascorbic Acid L-O-Phosphate |
| CN108703901A (en) * | 2018-05-18 | 2018-10-26 | 吕莉 | A kind of preparation method of acne eliminating cream |
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