CN108003191B - Preparation method of vitamin C phosphate - Google Patents
Preparation method of vitamin C phosphate Download PDFInfo
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- CN108003191B CN108003191B CN201711399805.8A CN201711399805A CN108003191B CN 108003191 B CN108003191 B CN 108003191B CN 201711399805 A CN201711399805 A CN 201711399805A CN 108003191 B CN108003191 B CN 108003191B
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- MIJPAVRNWPDMOR-UHFFFAOYSA-N [2-(1,2-dihydroxyethyl)-3-hydroxy-5-oxo-2h-furan-4-yl] dihydrogen phosphate Chemical compound OCC(O)C1OC(=O)C(OP(O)(O)=O)=C1O MIJPAVRNWPDMOR-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 30
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- UGTZMIPZNRIWHX-UHFFFAOYSA-K sodium trimetaphosphate Chemical compound [Na+].[Na+].[Na+].[O-]P1(=O)OP([O-])(=O)OP([O-])(=O)O1 UGTZMIPZNRIWHX-UHFFFAOYSA-K 0.000 claims abstract description 12
- 239000011575 calcium Substances 0.000 claims abstract description 11
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 10
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 9
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229930003268 Vitamin C Natural products 0.000 claims abstract description 8
- 239000011718 vitamin C Substances 0.000 claims abstract description 8
- 235000019154 vitamin C Nutrition 0.000 claims abstract description 8
- 238000001694 spray drying Methods 0.000 claims abstract description 4
- 239000000725 suspension Substances 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 229910019142 PO4 Inorganic materials 0.000 description 20
- 239000010452 phosphate Substances 0.000 description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 19
- 239000000047 product Substances 0.000 description 8
- 239000002211 L-ascorbic acid Substances 0.000 description 7
- 229960005070 ascorbic acid Drugs 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 235000000069 L-ascorbic acid Nutrition 0.000 description 6
- 229910052791 calcium Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 230000026731 phosphorylation Effects 0.000 description 5
- 238000006366 phosphorylation reaction Methods 0.000 description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 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 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- SUQVNMZSSKXYRH-ZAFYKAAXSA-N [(2r)-2-[(1s)-1,2-dihydroxyethyl]-3-hydroxy-5-oxo-2h-furan-4-yl] [hydroxy(phosphonooxy)phosphoryl] hydrogen phosphate Chemical group OC[C@H](O)[C@H]1OC(=O)C(OP(O)(=O)OP(O)(=O)OP(O)(O)=O)=C1O SUQVNMZSSKXYRH-ZAFYKAAXSA-N 0.000 description 1
- POXJXWXPDYFTJM-ZAFYKAAXSA-N [(2r)-2-[(1s)-1,2-dihydroxyethyl]-4-hydroxy-5-oxo-2h-furan-3-yl] dihydrogen phosphate Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1OP(O)(O)=O POXJXWXPDYFTJM-ZAFYKAAXSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- NFDFQCUYFHCNBW-SCGPFSFSSA-N dienestrol Chemical compound C=1C=C(O)C=CC=1\C(=C/C)\C(=C\C)\C1=CC=C(O)C=C1 NFDFQCUYFHCNBW-SCGPFSFSSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 150000004712 monophosphates Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/655—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms
- C07F9/65515—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms the oxygen atom being part of a five-membered ring
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a preparation method of vitamin C phosphate, which is characterized by comprising the following process steps: adding vitamin C, anhydrous calcium chloride and deionized water into a reaction kettle at 0-5 ℃, stirring until the feed liquid is in a suspension state, and then slowly dropwise adding Ca (OH)2Solution to pH is 4.5-6.5, sodium trimetaphosphate is added, the calcium hydroxide solution is continuously dripped until the pH value is 8-10.5, the mixture is stirred until the mixture is viscous, the NaOH solution is directly dripped at the feed liquid temperature of 10-25 ℃ to adjust the pH value to 10-13, the mixture is stirred for reaction for 5-30 min, and spray drying is carried out. The invention adopts the direct dropwise addition of the sodium hydroxide solution for degradation reaction, water is not added in the whole degradation process, and the temperature is not increased.
Description
Technical Field
The invention relates to the technical field of drug synthesis, in particular to a preparation method of vitamin C phosphate.
Background
Vitamin C (Vc), an acidic polyol containing six carbon atoms of formula C6H8O6Molecular weight 176.1. The structure of the dienol of the L-ascorbic acid ensures that the L-ascorbic acid has strong antioxidation, and is widely applied to the fields of medicine and health care, food additives, cosmetics, feed additives and the like. However, L-ascorbic acid is unstable and is easily destroyed by light, heat and oxygen to rapidly undergo irreversible decomposition reaction, thereby losing its reducing ability, especially in aquatic feeds such as fish and shrimp.
The vitamin C phosphate is one of Vc derivatives, has strong oxidation resistance and thermal stability compared with Vc, and can be decomposed into free L-ascorbic acid in vivo by phosphate hydrolase to play a role, so that the requirements of feed processing and production can be met.
So far, there are mainly two methods for Vc phosphorylation: firstly, phosphorylation of phosphorus oxychloride takes L-ascorbic acid as a raw material, and the L-ascorbic acid and acetone are subjected to ketal reaction to generate 5, 6-oxo-isopropylidene-L-ascorbic acid, and hydroxyl groups on 5 and 6 positions are protected; dissolving with pyridine, regulating pH value with potassium hydroxide, dropping phosphorus oxychloride for reaction, evaporating to remove pyridine, desalting several times, concentrating, cationic resin exchange, collecting eluent, adding magnesium hydroxide for reaction, crystallizing with low-carbon alcohol, filtering and drying. The product is mainly L-ascorbic acid-2-monophosphate, the byproducts are mainly L-ascorbic acid-3-phosphate and 2-pyrophosphate, the whole process is relatively complex, and the added organic solvent is more, so that the environment is polluted. The second method is to use phosphate for phosphorylation to obtain the main product L-ascorbic acid-2-polyphosphate. When sodium trimetaphosphate is used, the product is L-ascorbic acid-2-triphosphate, but also contains L-ascorbic acid-2-monophosphate in a certain proportion, and the former can be degraded into monophosphate by excessive alkali. The method has short synthetic route, but has more byproducts, high product separation difficulty and low total product yield.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the preparation method of the vitamin C phosphate, which effectively improves the product yield, has simple process, simple operation, low cost, environmental protection and high efficiency.
The technical scheme adopted for realizing the aim of the invention is as follows:
The preparation method of the vitamin C phosphate is characterized by comprising the following process steps: adding vitamin C, anhydrous calcium chloride and deionized water into a reaction kettle at 0-5 ℃, stirring until the feed liquid is in a suspension state, and then slowly dropwise adding Ca (OH)2And adding sodium trimetaphosphate into the solution until the pH value of the solution is 4.5-6.5, continuously dropwise adding a calcium hydroxide solution until the pH value is 8-10.5, stirring the solution until the solution is viscous, directly dropwise adding a NaOH solution until the pH value is 10-13 at the temperature of 10-25 ℃ of the feed liquid, stirring the solution for reaction for 5-30 min, and spray-drying the reaction product.
The dosage ratio of the vitamin C, the anhydrous calcium chloride and the deionized water is 1: 0.01-0.2: 0.8 to 3 in terms of mass ratio.
The amount of the sodium trimetaphosphate is 0.5-2 times of the mass of the vitamin C.
The Ca (OH)2The mass concentration of the solution is 10-50%.
The mass concentration of the NaOH solution is 10-40%.
The method adopts the direct dropwise addition of the sodium hydroxide solution for degradation reaction, does not add water or raise the temperature in the whole degradation process, and has the following technical advantages compared with the prior art:
1. By the process measures of the invention, the content of the Vc phosphate is improved by 2 percent, the product quality of the Vc phosphate is obviously improved, and the market competitiveness of the Vc phosphate is enhanced.
2. In the whole process, steam consumption is changed from the existence to the nonexistence, the yield is improved by 1.5 times, the synthesis time of each batch is shortened by 66.7 percent, the usage amount of deionized water is reduced by 66.7 percent, and the drying time is shortened by 50 percent. Therefore, the method is a green, environment-friendly, energy-saving and consumption-reducing Vc phosphate production process.
3. compared with the conventional process, the method has the advantages of greatly shortening the production time, reducing the material consumption and the energy consumption, obviously improving the utilization rate of personnel and equipment and obviously reducing the production cost.
The following are comparative tests of the present invention with conventional processes:
(1) the synthesis process of the conventional phosphate phosphorylation Vc phosphate comprises the following steps:
the method comprises the following steps of (1): 0.01-0.2: 0.8-3, stirring in a reaction kettle at 0-5 ℃, and slowly dripping 10-50% of Ca (OH)2The pH value of the solution is 4.5-6.5, and the temperature is 10-20 ℃;
Adding 0.5-2 times of coarse Vc weight of sodium trimetaphosphate, continuously dropwise adding a calcium hydroxide solution to adjust the pH value to 8-10.5, adjusting the temperature to 10-25 ℃, and stirring until the mixture is viscous;
Thirdly, after the feed liquid is viscous, adding deionized water with the weight 2-10 times of that of the crude Vc, controlling the temperature of the reaction kettle at 50-70 ℃, finally slowly dropwise adding 10-40% of NaOH solution to adjust the pH value to 10-13, and stirring for 2-5 hours while keeping the temperature;
Fourthly, after the reaction is finished, the feed liquid is dried by a spray dryer to obtain the faint yellow vitamin C phosphate.
(2) The invention relates to a new phosphate phosphorylation Vc phosphate synthesis process
The second step is the same as the conventional process;
Thirdly, after the feed liquid is viscous, directly and slowly dripping 10-40% NaOH solution into the feed liquid at 10-25 ℃ to adjust the pH value to 10-13, and stirring for 5-30 min to finish the reaction;
Fourthly, after the reaction is finished, the feed liquid is dried by a spray dryer to obtain the faint yellow vitamin C phosphate.
The content of Vc phosphate products obtained by the method and the conventional method is shown in tables 1 and 2.
TABLE 1 comparison of Vc phosphate contents obtained by different Vc phosphate synthesis processes
| Process batch | 1 | 2 | 3 | 4 | 5 | Average |
| conventional process | 35.6% | 36.0% | 35.8% | 35.4% | 35.5% | 35.7% |
| New process | 38.0% | 38.4% | 37.2% | 37.8% | 37.3% | 37.7% |
TABLE 2 comparison of energy consumption and material consumption in different Vc phosphate synthesis processes
| parameter(s) | Yield t/month | Steam consumption | Synthesis time h/batch | Dosage L/batch of deionized water | spray drying time length h/batch |
| Conventional process | 80 | Is provided with | 3 | 1200 | 3 |
| New process | 200 | Is free of | 1 | 400 | 1.5 |
| Rate of change% | 150 | ～ | ～66.7 | ～66.7 | 50 |
the data fully show that the Vc phosphate content is improved, the yield is greatly improved, the production time is shortened, and the energy consumption is reduced by applying the method.
Detailed Description
The invention is illustrated below by way of examples, which are to be understood as being illustrative and not limiting. The scope and core content of the invention are to be determined by the claims.
Example 1:
(1) Cooling 1000L reaction kettle interlayer to 0 deg.C, adding 300L deionized water into the reaction kettle, stirring, adding 101Kg crude Vc (content 99.0%) and 20Kg anhydrous calcium chloride, slowly adding 50% Ca (OH) dropwise2The solution was brought to pH 4.5 and the temperature was maintained at 20 ℃.
(2) After 50Kg of sodium trimetaphosphate was added, the calcium hydroxide solution was continuously added dropwise to adjust the pH to 10.5 at 25 ℃ and stirred until viscous.
(3) Slowly dropwise adding 10% NaOH solution to adjust the pH value to 13, keeping the temperature at 10 ℃ and stirring for 5min to finish the reaction.
(4) After the reaction is finished, the feed liquid is dried by a spray dryer to obtain 225.5 Kg of light yellow Vc phosphate with the content of 38.0 percent and the total production time of 2.6 h.
Example 2:
(1) Cooling 1000L reaction kettle interlayer to 5 deg.C, adding 200L deionized water into the reaction kettle, stirring, adding 100.5Kg crude Vc (content 99.5%) and 10Kg anhydrous calcium chloride, slowly adding 30% Ca (OH) dropwise2the solution was brought to pH 6.5 and the temperature was maintained at 10 ℃.
(2) After 100Kg of sodium trimetaphosphate is added, the calcium hydroxide solution is continuously added dropwise to adjust the pH value to 8, the temperature is 15 ℃, and the mixture is stirred until the mixture is viscous.
(3) Slowly dropwise adding 40% NaOH solution to adjust the pH value to 13, keeping the temperature at 15 ℃ and stirring for 15min to finish the reaction.
(4) After the reaction is finished, the feed liquid is dried by a spray dryer to obtain 260.3 Kg of light yellow Vc phosphate with the content of 38.4 percent and the total production time of 2.3 h.
Example 3:
（1）Cooling 1000L reaction kettle interlayer to 2 deg.C, adding 80L deionized water into the reaction kettle, stirring, adding 100.7Kg crude Vc (content 99.3%) and 1Kg anhydrous calcium chloride, slowly adding 10% Ca (OH) dropwise2The solution was brought to pH 5 and the temperature was maintained at 15 ℃.
(2) After 200Kg of sodium trimetaphosphate was added, the calcium hydroxide solution was continuously added dropwise to adjust the pH to 9 at 10 ℃ and stirred until viscous.
(3) slowly dropwise adding 25% NaOH solution to adjust the pH value to 10, keeping the temperature at 25 ℃ and stirring for 30min to finish the reaction.
(4) After the reaction is finished, the feed liquid is dried by a spray dryer to obtain 382.6 Kg of light yellow Vc phosphate with the content of 37.2 percent and the total production time of 2.5 h.
Example 4:
(1) cooling 1000L reaction kettle interlayer to 1 deg.C, adding 150L deionized water into the reaction kettle, stirring, adding 100.3Kg crude Vc (content 99.7%) and 6Kg anhydrous calcium chloride, slowly adding 40% Ca (OH) dropwise2The solution was brought to pH 5.5 and the temperature was maintained at 15 ℃.
(2) After 90Kg of sodium trimetaphosphate is added, the calcium hydroxide solution is continuously added dropwise to adjust the pH value to 10 at the temperature of 23 ℃, and the mixture is stirred until the mixture is viscous.
(3) Slowly dripping 35% NaOH solution to adjust the pH value to 12, keeping the temperature at 23 ℃, stirring for 20min and finishing the reaction.
(4) After the reaction is finished, the feed liquid is dried by a spray dryer to obtain 245.8 Kg of light yellow Vc phosphate with the content of 37.8 percent and the total production time of 2.7 hours.
Example 5:
(1) Cooling 1000L reaction kettle interlayer to 1 deg.C, adding 180L deionized water into the reaction kettle, stirring, adding 100.3Kg Vc (content 99.7%) and 12Kg anhydrous calcium chloride, slowly adding 30% Ca (OH) dropwise2the solution was brought to pH 6.0 and the temperature was maintained at 18 ℃.
(2) After 145Kg of sodium trimetaphosphate was added, the calcium hydroxide solution was continuously added dropwise to adjust the pH to 8.9 at 20 ℃ and stirred until viscous.
(3) Slowly dripping 35% NaOH solution to adjust the pH value to 12.5, keeping the temperature at 18 ℃ and stirring for 10min to finish the reaction.
(4) After the reaction is finished, the feed liquid is dried by a spray dryer to obtain 300.3 Kg of light yellow Vc phosphate with the content of 37.3 percent and the total production time of 2.5 h.
Claims (5)
1. the preparation method of the vitamin C phosphate is characterized by comprising the following process steps: adding vitamin C, anhydrous calcium chloride and deionized water into a reaction kettle at 0-5 ℃, stirring until the feed liquid is in a suspension state, and then slowly dropwise adding Ca (OH)2And adding sodium trimetaphosphate into the solution until the pH value of the solution is 4.5-6.5, continuously dropwise adding a calcium hydroxide solution until the pH value is 8-10.5, stirring the solution until the solution is viscous, directly dropwise adding a NaOH solution until the pH value is 10-13 at the temperature of 10-25 ℃ of the feed liquid, stirring the solution for reaction for 5-30 min, and spray-drying the reaction product.
2. The process for preparing vitamin C phosphate according to claim 1, wherein the amount ratio of the vitamin C, the anhydrous calcium chloride and the deionized water is 1: 0.01-0.2: 0.8 to 3 in terms of mass ratio.
3. The method for preparing vitamin C phosphate according to claim 1, wherein the amount of the sodium trimetaphosphate is 0.5 to 2 times the mass of the vitamin C.
4. The process for preparing vitamin C phosphate according to claim 1, wherein the Ca (OH)2The mass concentration of the solution is 10-50%.
5. The process for producing vitamin C phosphate according to claim 1, wherein the NaOH solution has a concentration of 10 to 40% by mass.
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| CN109081851A (en) * | 2018-08-17 | 2018-12-25 | 北京英惠尔生物技术有限公司 | The preparation method of feeding L-AA -2- tripolyphosphate |
| CN115594717A (en) * | 2020-05-14 | 2023-01-13 | 靖江市宏杰干燥机械制造有限公司（Cn） | Preparation method of L-ascorbic acid-2-phosphate |
| CN114369118A (en) * | 2021-12-14 | 2022-04-19 | 安徽泰格生物技术股份有限公司 | Preparation method of L-ascorbic acid-2-phosphate |
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| US5110950A (en) * | 1991-06-12 | 1992-05-05 | Kansas State University Research Foundation | Method of preparing 2-phosphorylated compounds of ascorbic acid |
| JP4418995B2 (en) * | 1999-03-18 | 2010-02-24 | 昭和電工株式会社 | Method for producing ascorbic acid 2-monophosphate salt |
| CN104974186A (en) * | 2012-11-14 | 2015-10-14 | 帝斯曼江山制药（江苏）有限公司 | Production technology of optimal L-ascorbic acid-2- phosphate ester |
| CN106317113A (en) * | 2016-08-22 | 2017-01-11 | 宁夏启元药业有限公司 | Synthesis method of L-ascorbic acid-2-monophosphate |
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