CN108690076A - The preparation method of the remaining Magnesium L-Ascorbyl Phosphate of organic solvent-free - Google Patents
The preparation method of the remaining Magnesium L-Ascorbyl Phosphate of organic solvent-free Download PDFInfo
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- CN108690076A CN108690076A CN201810353856.5A CN201810353856A CN108690076A CN 108690076 A CN108690076 A CN 108690076A CN 201810353856 A CN201810353856 A CN 201810353856A CN 108690076 A CN108690076 A CN 108690076A
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- organic solvent
- ascorbyl phosphate
- free
- magnesium
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000011777 magnesium Substances 0.000 title claims abstract description 22
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 22
- KIENGQUGHPTFGC-JLAZNSOCSA-N L-ascorbic acid 6-phosphate Chemical compound OP(=O)(O)OC[C@H](O)[C@H]1OC(=O)C(O)=C1O KIENGQUGHPTFGC-JLAZNSOCSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000889 atomisation Methods 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 19
- 150000001768 cations Chemical class 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 238000003860 storage Methods 0.000 claims abstract description 7
- 125000000129 anionic group Chemical group 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 5
- 238000004806 packaging method and process Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 19
- 229910019142 PO4 Inorganic materials 0.000 claims description 16
- 239000010452 phosphate Substances 0.000 claims description 16
- 239000011347 resin Substances 0.000 claims description 16
- 229920005989 resin Polymers 0.000 claims description 16
- 150000001450 anions Chemical class 0.000 claims description 15
- 238000002425 crystallisation Methods 0.000 claims description 15
- 230000008025 crystallization Effects 0.000 claims description 14
- 150000007524 organic acids Chemical class 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 11
- 230000032050 esterification Effects 0.000 claims description 10
- 238000005886 esterification reaction Methods 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000011574 phosphorus Substances 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 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 6
- 239000002253 acid Substances 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 238000005342 ion exchange Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 239000003729 cation exchange resin Substances 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 239000003960 organic solvent Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 24
- 239000000047 product Substances 0.000 description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 12
- 235000006408 oxalic acid Nutrition 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 239000003957 anion exchange resin Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 150000003014 phosphoric acid esters Chemical class 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 229940088594 vitamin Drugs 0.000 description 3
- 229930003231 vitamin Natural products 0.000 description 3
- 235000013343 vitamin Nutrition 0.000 description 3
- 239000011782 vitamin Substances 0.000 description 3
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 2
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- DBSABEYSGXPBTA-RXSVEWSESA-N (2r)-2-[(1s)-1,2-dihydroxyethyl]-3,4-dihydroxy-2h-furan-5-one;phosphoric acid Chemical class OP(O)(O)=O.OC[C@H](O)[C@H]1OC(=O)C(O)=C1O DBSABEYSGXPBTA-RXSVEWSESA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229940093915 gynecological organic acid Drugs 0.000 description 1
- 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 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001308 synthesis method 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation methods of the remaining Magnesium L-Ascorbyl Phosphate of organic solvent-free, include the following steps:1) decationized Y sieve;2) cation impurity is removed;3) anionic impurity is removed;4) atomization drying crystallizes;5) rewinding, detection, packaging, storage.The method that the application uses directly is crystallized by atomization drying without using organic solvent, reduces production cost, and rate of dissolution improves, the residual without any organic solvent.
Description
Technical field
The present invention relates to field of biological pharmacy, more particularly to a kind of remaining L-AA phosphoric acid of organic solvent-free
The preparation method of ester magnesium.
Background technology
It mostly uses two methods greatly currently on the market and prepares Magnesium L-Ascorbyl Phosphate, one is " phosphorus oxychloride " synthesis
Method prepares Magnesium L-Ascorbyl Phosphate, and one kind is " phosphate " synthetic method.It is anti-bad that L- is prepared using " phosphorus oxychloride " synthetic method
Hematic acid phosphate magnesium can cause seriously to pollute, not advocate use at home and abroad to environment;It is prepared using " phosphate " synthetic method
Magnesium L-Ascorbyl Phosphate, although this method is the appropriate method that domestic production producer uses, but organic solvent is used when crystallization
Crystallization is precipitated, residual fraction organic solvent can not be removed in the product after drying;The residual of organic solvent frequently can lead to product
Water-soluble difficulty, the product of some producer's production are up to more than tens of hours since Determination of Residual Organic Solvents is exceeded in dissolving,
Product quality is directly affected, very big difficulty is caused to user.
Invention content
The present invention provides a kind of preparation method of the remaining Magnesium L-Ascorbyl Phosphate of organic solvent-free, organic solvent-free
Residual, product quality is high, and production cost is low.
To achieve the goals above, the present invention uses following technical scheme:A kind of remaining L- Vitamin Cs of organic solvent-free
The preparation method of acid phosphoric acid ester magnesium, includes the following steps:
1) decationized Y sieve:Organic acid is added in the crude product of the Magnesium L-Ascorbyl Phosphate after synthesizing esterification, often
Temperature stirring 1-3H, is put into jar special quiescent settling 1-10H, filters supernatant;The dosage that VC is put into when by synthesis esterification, to
It synthesizes and organic acid is added in the crude product of the Magnesium L-Ascorbyl Phosphate after esterification, the mass ratio of VC and organic acid is 1:
0.1-0.8.Organic acid used in this application can be the conventional use of one or more organic acids of the art, in this step
The amount of acid can not be excessive, otherwise then introduces extra impurity, the step for calcium ion mainly in removal filtrate, according to reaction
The suitable addition deionized water of concentration, make the control of the feed concentration after decalcification in 1.0-20.0%, acylate precipitation is available
Make the raw material of industry or is used as agriculture and forestry fertilizer.
2) secondary removal cation impurity:Filtered supernatant is filtered with pumping to cation exchange resin column, with every
The flow velocity of minute 0.1-10m carries out ion exchange by cationic resin column, removes extra cation;Removal cation is miscellaneous
Matter avoids the quality for influencing finished product.
3) anionic impurity is removed:The content of free phosphate radical and sulfate radical, is adjusted in feed liquid after detection removal cation
Whole PH is 7~12, by filtrate pump to resin anion (R.A.) exchange column, passes through resin anion (R.A.) column with the flow velocity of 0.1-10m per minute
Ion exchange is carried out, extra cation is removed;
Before carrying out resin anion (R.A.) exchange, the content that special equipment measures phosphate radical and sulfate radical can be used, it is necessary to tight
Lattice measure the content of dissociate in feed liquid phosphate radical and sulfate radical, control the dosage of resin anion (R.A.), can effectively remove in filtrate
Existing anionic impurity.The free anionic impurity of titration precipitation method removal can also be used in this step, when selecting titration, protects
Equivalent titration is demonstrate,proved, so that free phosphorus acid group or sulfate radical is formed new compound equivalent precipitation, anion is effectively removed to reach
The purpose of impurity.
4) atomization drying crystallizes:Filtrate after refined filtration is pumped into reaction kettle, PH5.5~7.5 is adjusted, is transported to cleaning shop
Carry out atomization heated drying crystallization;
5) rewinding, detection, packaging, storage.
Further, the atomization steps in step 4) are as follows:Atomization crystallizer is opened, 165-185 DEG C of inlet air temperature goes out
Air temperature will be controlled at 85-90 DEG C °, and air inlet fan temperature is maintained at 50 DEG C, and air-introduced machine temperature is maintained at 40-43 DEG C, and pressure gauge is protected
It holds in -0.1~-0.5atm, starts to feed when leaving air temp reaches 140 DEG C, temperature slowly declines at this time, 85- to be dropped to
95 DEG C of steady timing determination inlet amounies constantly adjust inlet valve, ensure that the moisture content of crystallization material and aridity meet the survey of product requirement
Test-object is accurate.The temperature stablized in atomisation tower preferably must be held between 85-95 DEG C, it is ensured that moisture content and the drying of material are crystallized, it is only warm
Degree is maintained between 85-95 DEG C, can just meet the testing standard of product requirement.
Preferably, the PH of atomization drying crystallization is 6-7.
Compared with prior art, the product ultraviolet specrophotometer prepared by atomization drying crystallisation surveys L- Vitamin Cs
For acid phosphoric acid ester content of magnesium up to 99% or more, free phosphorus hydrochlorate≤0.3% is lower 0.7%, PH7.0-8.0 than national regulations index
It takes 3g to be dissolved in the observation of 100ml aqueous solutions in range, is dissolved in 1 minute and as clear as crystal.It is tied relative to being precipitated with organic solvent
Brilliant method, the method that the application uses directly are crystallized by atomization drying without using organic solvent, reduce and be produced into
This, and rate of dissolution improves, the residual without any organic solvent, and the acylate precipitation after decationized Y sieve can be used as industrial original
Material is used as agriculture and forestry fertilizer.
Description of the drawings
Fig. 1 is the flow chart of the present invention.
Specific implementation mode
With reference to Fig. 1 and specific embodiment, the present invention is described in detail.
Embodiment 1:The dosage that VC is put into when by synthesis esterification, to the L-AA phosphate after synthetic reaction
Oxalic acid is added in crude product, weighs with VC as 1 mass parts, oxalic acid is 0.1-0.25 mass parts, carries out decalcification, can be anti-bad according to L-
The suitable addition deionized water of concentration of hematic acid phosphate crude product makes after organic acid decalcification feed concentration control 1.0%, decalcification
Ion exchange resin exchange column is pumped into feed liquid afterwards, rotating speed 0.1m is per minute, exchanges and removes cation therein;
Feed liquid that treated carries out anion-content measurement, determines the quantity of resin anion (R.A.), then uses D008 macropores
The acrylic acid type anion exchange resin of highly basic is handled, and free phosphate and sulfate are removed, this process needs strictly true
Determine anion-content, to determine the dosage of resin anion (R.A.), ensures Magnesium L-Ascorbyl Phosphate feed liquid before atomization drying crystallization
Quality.
Feed liquid adjustment PH after refined filtration enters atomization heated drying crystallization procedure after being 5.5, opens atomization crystallizer, air inlet
165 DEG C of temperature, leaving air temp will be controlled at 85 DEG C, and air inlet fan temperature is maintained at 50 DEG C, and air-introduced machine temperature is maintained at 40 DEG C, pressure
Table is maintained at -0.1atm, starts to feed when leaving air temp reaches 140 DEG C, and temperature slowly declines at this time, when dropping to 85 DEG C
Equilibrium temperature determines inlet amount, constantly adjusts inlet valve.
With this condition, product obtained with ultraviolet specrophotometer survey content it is reachable >=96%, free phosphorus hydrochlorate <
0.5%, lower than national regulations index 0.5%, it takes in 100ml aqueous solutions of the 3g within the scope of PH7.0-8.0 and observes, in 1 minute
Dissolving, color are as clear as crystal.
It finally collects, pack, storage.
Example 2:
The dosage that VC is put into when by synthesis esterification, is added into the L-AA phosphate crude product after synthetic reaction
Oxalic acid is weighed with VC as 1 mass parts, and oxalic acid is 0.25-0.45 mass parts, carries out decalcification, can be according to L-AA phosphate
The suitable addition deionized water of concentration of crude product, feed concentration control is in the feed liquid after 15%, decalcification after making organic acid decalcification
It is pumped into ion exchange resin exchange column, rotating speed 5m is per minute, exchanges and removes cation therein;
Feed liquid that treated carries out anion-content measurement, determines the quantity of resin anion (R.A.), then uses D008 macropores
The acrylic acid type anion exchange resin of highly basic is handled, and free phosphate and sulfate are removed, this process needs strictly true
Determine anion-content, to determine the dosage of resin anion (R.A.), ensures Magnesium L-Ascorbyl Phosphate feed liquid before atomization drying crystallization
Quality.
Feed liquid adjustment PH after refined filtration is 6, conveys into atomization heated drying crystallization procedure, opens atomization crystallizer, air inlet
170 DEG C of temperature, leaving air temp will be controlled at 87 DEG C, and air inlet fan temperature is maintained at 50 DEG C, and air-introduced machine temperature is maintained at 42 DEG C, pressure
Table is maintained at -0.3atm, starts to feed when leaving air temp reaches 140 DEG C, and temperature slowly declines at this time, when dropping to 85 DEG C
Equilibrium temperature determines inlet amount, constantly adjusts inlet valve.
With this condition, product obtained with ultraviolet specrophotometer survey content it is reachable >=99%, free phosphorus hydrochlorate <
0.3%, lower than national regulations index 0.7%, it takes in 100ml aqueous solutions of the 3g within the scope of PH7.0-8.0 and observes, in 1 minute
It dissolves and as clear as crystal.
It finally collects, pack, storage.
Example 3:The dosage of VC is put into when by synthesis esterification, it is thick to the L- ascorbic acid phosphoric acid esters after synthetic reaction
Oxalic acid is added in product, weighs with VC as 1 mass parts, oxalic acid is 0.6-0.8 mass parts, carries out decalcification, can be according to L-AA
The suitable addition deionized water of concentration of phosphate crude product, feed concentration control is after 20%, decalcification after making organic acid decalcification
Ion exchange resin exchange column is pumped into feed liquid, rotating speed 10m is per minute, exchanges and removes cation therein;
Feed liquid that treated carries out anion-content measurement, determines the quantity of resin anion (R.A.), then uses D008 macropores
The acrylic acid type anion exchange resin of highly basic is handled, and free phosphate and sulfate are removed, this process needs strictly true
Determine anion-content, to determine the dosage of resin anion (R.A.), ensures Magnesium L-Ascorbyl Phosphate feed liquid before atomization drying crystallization
Quality.
Feed liquid adjustment PH after refined filtration is 7, delivers into atomization heated drying crystallization procedure, opens atomization crystallizer, into
185 DEG C of air temperature, leaving air temp will be controlled at 90 DEG C, and air inlet fan temperature is maintained at 50 DEG C, and air-introduced machine temperature is maintained at 43 DEG C, pressure
Power table is maintained at -0.5atm, starts to feed when leaving air temp reaches 140 DEG C, and temperature slowly declines at this time, waits dropping to 95 DEG C
When equilibrium temperature, determine inlet amount, constantly adjust inlet valve.
With this condition, product obtained with ultraviolet specrophotometer survey content it is reachable >=99%, free phosphorus hydrochlorate <
0.3%, lower than national regulations index 0.7%, it takes in 100ml aqueous solutions of the 3g within the scope of PH7.0-8.0 and observes, in 1 minute
It dissolves and as clear as crystal.
It finally collects, pack, storage.
Reference examples 4:The dosage that VC is put into when by synthesis esterification, to the L-AA phosphate after synthetic reaction
Oxalic acid is added in crude product, weighs with VC as 1 mass parts, oxalic acid is 0.6-0.8 mass parts, carries out decalcification, can be according to L- Vitamin Cs
The suitable addition deionized water of concentration of acid phosphoric acid ester crude product, feed concentration control is after 20%, decalcification after making organic acid decalcification
Feed liquid in be pumped into ion exchange resin exchange column, rotating speed 10m is per minute, exchanges and removes cation therein;
Feed liquid that treated carries out anion-content measurement, determines the quantity of resin anion (R.A.), then uses D008 macropores
The acrylic acid type anion exchange resin of highly basic is handled, and free phosphate and sulfate are removed, this process needs strictly true
Determine anion-content, to determine the dosage of resin anion (R.A.), ensures Magnesium L-Ascorbyl Phosphate feed liquid before atomization drying crystallization
Quality.
Feed liquid adjustment PH after refined filtration is 7, delivers into atomization heated drying crystallization procedure, opens atomization crystallizer, into
185 DEG C of air temperature, leaving air temp will be controlled at 90 DEG C, and air inlet fan temperature is maintained at 50 DEG C, and air-introduced machine temperature is maintained at 43 DEG C, pressure
Power table is maintained at -0.5atm, starts to feed when leaving air temp reaches 140 DEG C, and temperature slowly declines at this time, waits dropping to 80 DEG C
When equilibrium temperature, determine inlet amount, constantly adjust inlet valve.
With this condition, product obtained surveys content up to 95.8% with ultraviolet specrophotometer, free phosphorus hydrochlorate <
0.3%, it is lower 0.7%, PH7.0-8.0 than national standard than the world within the scope of, take 3g to be dissolved in the observation of 100ml aqueous solutions, solution it is micro- it is yellow thoroughly
It is bright.
It finally collects, pack, storage.
According to example 3 and the comparison of embodiment 4 it is found that temperature when crystallizing influences the quality of finished product.Embodiment described above
Several preparation methods of the present invention are only described, description is more specific, and preparation method must strictly be operated by technique in detail,
Otherwise final finished product can be variant in individual indexs.Therefore this detailed statement cannot be interpreted as to patent of invention range
Limitation, it should be pointed out that be for those skilled in the art, without departing from the inventive concept of the premise, can be with
Several modifications and improvements are made, these are all within the scope of protection of the present invention.
Claims (4)
1. a kind of preparation method of the remaining Magnesium L-Ascorbyl Phosphate of organic solvent-free, it is characterised in that:Including following step
Suddenly:
1) decationized Y sieve:Organic acid is added in the crude product of the Magnesium L-Ascorbyl Phosphate after synthesizing esterification, room temperature stirs
1-3H is mixed, jar special quiescent settling 1-10H is put into, filters supernatant;
2) cation impurity is removed:Filtered supernatant is filtered with pumping to cation exchange resin column, with 0.1-10m/min
Flow velocity by cationic resin column carry out ion exchange, remove extra cation;
3) anionic impurity is removed:The content of free phosphate radical and sulfate radical, adjusts PH in feed liquid after detection removal cation
It is 7~12, filtrate pump to resin anion (R.A.) exchange column is carried out with the flow velocity of 0.1-10m per minute by resin anion (R.A.) column
Ion exchange removes extra cation;
4) atomization drying crystallizes:Filtrate after refined filtration is pumped into reaction kettle, adjusts PH5.5~7.5, is transported to cleaning shop progress
It is atomized heated drying crystallization;
5) rewinding, detection, packaging, storage.
2. a kind of preparation method of the remaining Magnesium L-Ascorbyl Phosphate of organic solvent-free according to claim 1,
It is characterized in that:Atomization steps in step 4) are as follows:Atomization crystallizer is opened, 165-185 DEG C of inlet air temperature, leaving air temp is wanted
Control is at 85-90 DEG C, and air inlet fan temperature is maintained at 50 DEG C, and air-introduced machine temperature is maintained at 40-43 DEG C, and pressure gauge is maintained at -0.1
~-0.5atm starts to feed when leaving air temp reaches 140 DEG C, and temperature slowly declines at this time, 85-95 DEG C of stabilization to be dropped to
When determine inlet amount, constantly adjust inlet valve.
3. a kind of preparation method of the remaining Magnesium L-Ascorbyl Phosphate of organic solvent-free according to claim 2,
It is characterized in that:The dosage of VC, the L-AA phosphorus after synthesizing esterification are put into when in step 1) by synthesis esterification
It is added organic acid in the crude product of acid esters magnesium, the mass ratio of VC and organic acid is 1:0.1-0.8.
4. a kind of preparation method of the remaining Magnesium L-Ascorbyl Phosphate of organic solvent-free according to claim 2,
It is characterized in that:PH is 6-7 in step 4).
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| CN113582913A (en) * | 2021-08-18 | 2021-11-02 | 河北广祥制药有限公司 | Method for continuously refining nifedipine |
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| CN1494547A (en) * | 2001-03-02 | 2004-05-05 | 昭和电工株式会社 | Ascorbic acid 2-phosphate metal salt with low calcium content |
| CN101307075A (en) * | 2008-05-15 | 2008-11-19 | 无锡市跨克微营养素有限公司 | Method for preparing L-ascorbate-2-phosplate magnesium |
| CN106478722A (en) * | 2016-08-31 | 2017-03-08 | 安徽天寅生物技术有限公司 | High-purity L ascorbic acid 2 magnesium phosphorate salt production process |
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2018
- 2018-04-19 CN CN201810353856.5A patent/CN108690076A/en active Pending
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