CN114130097A - Purification method and device for preparing L-5-methyl tetrahydrocalcium folate - Google Patents
Purification method and device for preparing L-5-methyl tetrahydrocalcium folate Download PDFInfo
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- CN114130097A CN114130097A CN202111499980.0A CN202111499980A CN114130097A CN 114130097 A CN114130097 A CN 114130097A CN 202111499980 A CN202111499980 A CN 202111499980A CN 114130097 A CN114130097 A CN 114130097A
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- suction filtration
- folate
- methyl
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- tetrahydrocalcium
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- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 title claims abstract description 46
- 235000019152 folic acid Nutrition 0.000 title claims abstract description 41
- 239000011724 folic acid Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000000746 purification Methods 0.000 title claims abstract description 38
- 229940014144 folate Drugs 0.000 title claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 46
- 238000000967 suction filtration Methods 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 235000005934 calcium-L-methylfolate Nutrition 0.000 claims description 9
- 239000011681 calcium-L-methylfolate Substances 0.000 claims description 9
- VWBBRFHSPXRJQD-ZEDZUCNESA-L calcium-L-methylfolate Chemical compound [Ca+2].C1NC=2NC(N)=NC(=O)C=2N(C)C1CNC1=CC=C(C(=O)N[C@@H](CCC([O-])=O)C([O-])=O)C=C1 VWBBRFHSPXRJQD-ZEDZUCNESA-L 0.000 claims description 9
- 239000013058 crude material Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- BGJXXVMOQCHQBO-ZEDZUCNESA-N (2s)-2-[[4-[(2-amino-5-methyl-4-oxo-1,6,7,8-tetrahydropteridin-6-yl)methylamino]benzoyl]amino]pentanedioic acid;calcium Chemical compound [Ca].C1NC=2N=C(N)NC(=O)C=2N(C)C1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 BGJXXVMOQCHQBO-ZEDZUCNESA-N 0.000 claims description 3
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- 238000003780 insertion Methods 0.000 description 8
- 230000037431 insertion Effects 0.000 description 8
- 238000003825 pressing Methods 0.000 description 6
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 description 5
- 230000009471 action Effects 0.000 description 5
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- 238000006243 chemical reaction Methods 0.000 description 5
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- 230000003014 reinforcing effect Effects 0.000 description 5
- MSTNYGQPCMXVAQ-KIYNQFGBSA-N 5,6,7,8-tetrahydrofolic acid Chemical compound N1C=2C(=O)NC(N)=NC=2NCC1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 MSTNYGQPCMXVAQ-KIYNQFGBSA-N 0.000 description 4
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- 239000007924 injection Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- ZNOVTXRBGFNYRX-ABLWVSNPSA-N levomefolic acid Chemical compound C1NC=2NC(N)=NC(=O)C=2N(C)C1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 ZNOVTXRBGFNYRX-ABLWVSNPSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- MSTNYGQPCMXVAQ-RYUDHWBXSA-N (6S)-5,6,7,8-tetrahydrofolic acid Chemical compound C([C@H]1CNC=2N=C(NC(=O)C=2N1)N)NC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 MSTNYGQPCMXVAQ-RYUDHWBXSA-N 0.000 description 2
- ZNOVTXRBGFNYRX-STQMWFEESA-N (6S)-5-methyltetrahydrofolic acid Chemical compound C([C@@H]1N(C=2C(=O)N=C(N)NC=2NC1)C)NC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 ZNOVTXRBGFNYRX-STQMWFEESA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- XJLXINKUBYWONI-DQQFMEOOSA-N [[(2r,3r,4r,5r)-5-(6-aminopurin-9-yl)-3-hydroxy-4-phosphonooxyoxolan-2-yl]methoxy-hydroxyphosphoryl] [(2s,3r,4s,5s)-5-(3-carbamoylpyridin-1-ium-1-yl)-3,4-dihydroxyoxolan-2-yl]methyl phosphate Chemical compound NC(=O)C1=CC=C[N+]([C@@H]2[C@H]([C@@H](O)[C@H](COP([O-])(=O)OP(O)(=O)OC[C@@H]3[C@H]([C@@H](OP(O)(O)=O)[C@@H](O3)N3C4=NC=NC(N)=C4N=C3)O)O2)O)=C1 XJLXINKUBYWONI-DQQFMEOOSA-N 0.000 description 2
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- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- VVIAGPKUTFNRDU-STQMWFEESA-N (6S)-5-formyltetrahydrofolic acid Chemical compound C([C@H]1CNC=2N=C(NC(=O)C=2N1C=O)N)NC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 VVIAGPKUTFNRDU-STQMWFEESA-N 0.000 description 1
- AVFZOVWCLRSYKC-UHFFFAOYSA-N 1-methylpyrrolidine Chemical compound CN1CCCC1 AVFZOVWCLRSYKC-UHFFFAOYSA-N 0.000 description 1
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- 206010002065 Anaemia megaloblastic Diseases 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 208000000682 Megaloblastic Anemia Diseases 0.000 description 1
- AHVYPIQETPWLSZ-UHFFFAOYSA-N N-methyl-pyrrolidine Natural products CN1CC=CC1 AHVYPIQETPWLSZ-UHFFFAOYSA-N 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108010022394 Threonine synthase Proteins 0.000 description 1
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- 150000001638 boron Chemical class 0.000 description 1
- JMNIIIQOMSQWJN-ZEXVLMPOSA-L calcium;(2s)-2-[[4-[[(6s)-2-amino-5-methyl-4-oxo-1,6,7,8-tetrahydropteridin-6-yl]methylamino]benzoyl]amino]-5-hydroxy-5-oxopentanoate Chemical compound [Ca+2].C([C@@H]1N(C=2C(=O)NC(N)=NC=2NC1)C)NC1=CC=C(C(=O)N[C@@H](CCC([O-])=O)C(O)=O)C=C1.C([C@@H]1N(C=2C(=O)NC(N)=NC=2NC1)C)NC1=CC=C(C(=O)N[C@@H](CCC([O-])=O)C(O)=O)C=C1 JMNIIIQOMSQWJN-ZEXVLMPOSA-L 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000005515 coenzyme Substances 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
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- 238000012938 design process Methods 0.000 description 1
- 102000004419 dihydrofolate reductase Human genes 0.000 description 1
- OZRNSSUDZOLUSN-LBPRGKRZSA-N dihydrofolic acid Chemical compound N=1C=2C(=O)NC(N)=NC=2NCC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OZRNSSUDZOLUSN-LBPRGKRZSA-N 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
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- 229940075961 levoleucovorin calcium pentahydrate Drugs 0.000 description 1
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- 239000011782 vitamin Substances 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/96—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor in which the filtering elements are moved between filtering operations; Particular measures for removing or replacing the filtering elements; Transport systems for filters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/62—Regenerating the filter material in the filter
- B01D29/64—Regenerating the filter material in the filter by scrapers, brushes, nozzles, or the like, acting on the cake side of the filtering element
- B01D29/6469—Regenerating the filter material in the filter by scrapers, brushes, nozzles, or the like, acting on the cake side of the filtering element scrapers
- B01D29/6476—Regenerating the filter material in the filter by scrapers, brushes, nozzles, or the like, acting on the cake side of the filtering element scrapers with a rotary movement with respect to the filtering element
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D475/00—Heterocyclic compounds containing pteridine ring systems
- C07D475/02—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4
- C07D475/04—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4 with a nitrogen atom directly attached in position 2
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Filtration Of Liquid (AREA)
Abstract
The invention relates to the technical field of L-5-methyl tetrahydrocalcium folate preparation, and particularly discloses a purification method and a purification device for preparing L-5-methyl tetrahydrocalcium folate, wherein the purification method comprises the steps of heating and mixing crude L-5-methyl tetrahydrocalcium folate and ionized water, and carrying out ultrasonic treatment; heating the mixed solution after the ultrasonic treatment to reflux; then putting the mixed solution after heating and refluxing into a suction filtration device for suction filtration; finally, drying the crystals after suction filtration to obtain the crystal; the device comprises a case, a solution tank, a suction filtration assembly, a filter paper switching device and a liquid receiving tank; the method disclosed by the invention is simple, the purification efficiency is high, the industrial preparation and the industrial purification of the L-5-methyl tetrahydrocalcium folate can be realized, the structural design of the device disclosed by the invention is novel, the automation degree is high, the efficient industrial purification processing of the L-5-methyl tetrahydrocalcium folate can be realized, and the actual use effect is very excellent.
Description
Technical Field
The invention relates to the technical field of preparation of L-5-methyl tetrahydrocalcium folate, and particularly discloses a purification method and a purification device for preparation of L-5-methyl tetrahydrocalcium folate.
Background
Calcium L-5-methyltetrahydrofolate, also known as calcium (6S) -5-methyltetrahydrofolate. The (6S) -5-methyltetrahydrofolic acid is the main form of tissue and blood folic acid, and can directly participate in a plurality of important biochemical reactions in human bodies without complicated enzymatic steps in human bodies. L-5-methyltetrahydrofolic acid can be used as a medicine and a food additive, is used as a vitamin preparation, prevents neural tube defects, treats depression, treats megaloblastic anemia and the like, and researches show that L-5-methyltetrahydrofolic acid is the only drug which can penetrate through a blood brain barrier in folic acid drugs and has the effect of preventing and treating Alzheimer disease, so that the L-5-methyltetrahydrofolic acid has incomparable superiority with other folic acid drugs and has huge market prospect.
At present, tetrahydrofolic acid is mainly obtained by reducing folic acid, and the following methods are frequently used: chemical reduction, dihydrofolate reductase, catalytic hydrogenation, and the like. The catalytic hydrogenation method is divided into a normal pressure catalytic hydrogenation method and a pressure catalytic hydrogenation method, and is a main method for preparing tetrahydrofolic acid in the early stage, but the catalytic hydrogenation method has the defects of large catalyst consumption, long reaction time and low yield and purity of synthesized tetrahydrofolic acid. The hydroffolate reductase method adopts a biological enzyme method for reduction, the enzyme method has the greatest advantage of specificity, the dihydrofolic acid can be directly reduced into (6S) -tetrahydrofolic acid with physiological activity, and the synthesized (6S) -tetrahydrofolic acid can be used for synthesizing levofolinic acid and (6S) -5-methyltetrahydrofolic acid, so that the method is an ideal method, but a large amount of coenzyme NADPH is required in the production process, and a matched NADPH regeneration system is required to be constructed, so that the method is only suitable for laboratory implementation at present.
The invention patent with the patent number of CN2018105003466 discloses a preparation process of L-5-methyl calcium tetrahydrofolate, which comprises the steps of adding sodium borohydride in an alkaline environment, dripping a mixture of folic acid and water at normal temperature, and heating for reaction to generate tetrahydrofolic acid; dripping formaldehyde and sodium borohydride aqueous solution in sequence for reaction, cooling and standing for a period of time after the reaction is finished, and then carrying out suction filtration to remove boron salt; dropwise adding a calcium chloride solution into the filtrate, stirring, crystallizing, and carrying out suction filtration to obtain L-5-methyltetrahydrofolic acid calcium; mixing the obtained crystal with water, adding EDTA and methylpyrrolidine to carry out a resolution reaction, cooling after the reaction to precipitate an R-type enantiomer and an S-type enantiomer, continuously dropwise adding a calcium chloride solution into the obtained S-type enantiomer, stirring for crystallization, and carrying out suction filtration to obtain the L-5-methyl tetrahydrocalcium folate. However, the purity of the L-5-methyltetrahydrocalcium folate prepared by the method is still not ideal, so that the method and the device for purifying the L-5-methyltetrahydrocalcium folate are provided for aiming at the defect that the existing preparation process of the L-5-methyltetrahydrocalcium folate is low in purity and needs industrial purification.
Disclosure of Invention
The invention aims to provide a purification method and a purification device capable of realizing industrial purification of L-5-methyl tetrahydrocalcium folate aiming at the problems that the purity of L-5-methyl tetrahydrocalcium folate prepared by the prior art is not ideal and needs extraction treatment.
The invention is realized by the following technical scheme:
a purification method for preparing L-5-methyl tetrahydrocalcium folate comprises the following steps:
1) taking a proper amount of L-5-methyl tetrahydrocalcium folate crude material, putting the crude material into deionized water, heating and stirring the crude material until the crude material is uniformly mixed with the deionized water, and then carrying out ultrasonic treatment;
2) heating the mixed solution after ultrasonic treatment to reflux;
3) putting the mixed solution after heating and refluxing into a suction filtration device for suction filtration;
4) and drying the crystal after suction filtration to obtain the refined L-5-methyl tetrahydrofolic acid calcium.
Preferably, the mass ratio of the L-5-methyltetrahydrocalcium folate crude material to the deionized water in the step 1 is 1: 10-20.
Preferably, the temperature of the heated and refluxed mixed solution is not lower than 50 ℃ during suction filtration.
A purification device for preparing the L-5-methyl calcium tetrahydrofolate is a suction filtration device in step 3 and comprises a case, a solution tank, a suction filtration component, a filter paper switching device and a liquid receiving tank;
the liquid receiving tank is fixedly arranged on the bottom wall of the inner cavity of the case, a tank body neck pipe is arranged at the upper end of the liquid receiving tank, a rubber pipe opening plug is arranged in the tank body neck pipe, the lower end of the liquid receiving tank is connected with a liquid discharge pipe extending out of the case, a sealing valve is arranged on the liquid discharge pipe, the upper end of the liquid receiving tank is connected with an air suction pipe, and the lower end of the air suction pipe extending out of the case is connected with a vacuum pump;
the front side surface of the case is provided with a control cabinet, the upper surface of the case positioned right above the liquid receiving tank is provided with a circular opening, the solution tank is movably arranged in the circular opening, the outer circular surface of the solution tank is attached to the circular opening, the upper end opening of the solution tank is arranged, the open end of the solution tank is provided with a sealing cover, the sealing cover is connected with a liquid injection pipe, the outer circular surface of the solution tank positioned in the inner cavity of the case is symmetrically welded with two fixing lugs, the upper surface of the case positioned right above each fixing lug is provided with a telescopic device, the lower end of each telescopic device extends into the inner cavity of the case to be connected with the corresponding fixing lug, the lower end of the solution tank is connected with a suction filtration through pipe, the lower end of the suction filtration through pipe is connected with a pressing ring, the lower surface of the pressing ring is provided with an annular groove, and a rubber sealing ring is arranged in the annular groove, the upper surface of the rubber sealing ring is provided with a plurality of springs in an annular array shape, and the upper ends of the springs are connected with the top wall of the annular groove;
the suction filtration assembly comprises an insertion pipe penetrating through a rubber pipe orifice plug and extending into the liquid receiving tank, the upper end of the insertion pipe is connected with a bearing plate aligned with the compression ring, a metal filter disc is arranged on the upper surface of the bearing plate, and the inner cavity of the bearing plate is communicated with the insertion pipe;
the filter paper switching device comprises a filter paper winding roller and a filter paper unwinding roller which are respectively arranged on the left side surface and the right side surface of the machine box, a filter paper roll is wound on the filter paper unwinding roller, and the outer end of the filter paper roll passes through the strip-shaped openings on the left and right side surfaces of the case to be connected with the filter paper winding roll, the filter paper roll is positioned in the inner cavity of the case and is jointed with the bearing tray, round filter discs with the diameter larger than that of the metal filter disc are arranged on the filter paper roll at equal intervals, the left side surface of the case is provided with a winding frame, the filter paper winding roller is rotatably arranged at the outer end part of the winding frame, a winding motor for driving the filter paper winding roller to rotate is arranged on the winding rack, a scraping plate is rotatably arranged in the winding rack below the filter paper winding roller, and the movable end of the scraping plate is abutted against the filter paper winding roller, the convex shafts at the two ends of the scraping plate are sleeved with torsional springs, and the two ends of each torsional spring are respectively connected with the scraping plate and the winding rack.
As a further arrangement of the scheme, a heating jacket is arranged on the outer surface of the solution tank in the inner cavity of the case, heat conduction oil is arranged in the heating jacket, and a temperature sensor is arranged in the solution tank.
As a further arrangement of the scheme, a first liquid level sensor and a second liquid level sensor are respectively arranged in the solution tank and the liquid receiving tank.
As a specific arrangement of the above scheme, the telescopic device is one of a hydraulic cylinder and an air cylinder.
As a further arrangement of the above scheme, a triangular reinforcing rib plate is welded to the lower surface of the fixing lug, and the inner end of the triangular reinforcing rib plate is welded to the outer circular surface of the solution tank.
As a further arrangement of the above scheme, the height of the strip-shaped opening formed on the left side surface of the case is greater than the height of the strip-shaped opening formed on the right side surface.
As a further arrangement of the above scheme, a fine material receiving groove is arranged right below the scraper plate.
Has the advantages that:
1) the purification method for preparing the L-5-methyl tetrahydrocalcium folate disclosed by the invention can ensure that the purity of the L-5-methyl tetrahydrocalcium folate obtained by purification reaches more than 98%, and the whole purification method is simple and high in purification efficiency, can realize industrial preparation and industrial purification of the L-5-methyl tetrahydrocalcium folate, and has extremely high prospects.
2) The suction filtration device disclosed by the invention takes the suction filtration device in the existing laboratory as a design model, the solution tank is lifted up and down through the telescopic device, the filter paper is arranged on the filter paper and is pulled through the winding motor, after a certain amount of suction filtration is finished each time, the solution tank is lifted upwards to separate the pressing ring from the bearing tray, then the filter paper roll is extended out from the strip-shaped opening under the action of the winding motor, at the moment, the circular filter disc of the upper station and the lower station of the filter paper roll is just positioned between the pressing ring and the bearing tray, when the suction filtration operation is carried out again, the expansion device is directly controlled to press down the solution tank, the structural design of the whole filter paper switching device and the solution tank realizes the automatic replacement of the filter paper without manual replacement of operators, in addition, the switched filter paper roll is also directly scraped by a scraper plate when being wound on the roller body, so that the automatic blanking process is realized; the whole suction filtration device is novel in structural design and high in automation degree, can realize high-efficiency industrial purification and processing of the L-5-methyl tetrahydrocalcium folate, and has very excellent actual use effect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the steps of the purification method of the present invention;
FIG. 2 is a schematic view of a first angular perspective of the overall device of the present invention;
FIG. 3 is a schematic view of a second angular perspective of the overall apparatus of the present invention;
FIG. 4 is a schematic perspective view of the case, the filter paper switching device, and the like of the present invention;
FIG. 5 is a schematic perspective view of the liquid receiving tank, rubber tube plug, etc. of the present invention;
FIG. 6 is a schematic view of a three-dimensional structure of a solution tank, a suction filtration through pipe and the like in the invention;
FIG. 7 is a schematic perspective view of a suction filtration module according to the present invention;
FIG. 8 is a schematic perspective view of a filter paper switching device according to the present invention;
FIG. 9 is a schematic perspective view of the scraper plate and the torsion spring according to the present invention;
FIG. 10 is a schematic view of the inner plane structure of the solution tank, the liquid receiving tank, etc. in the present invention;
fig. 11 is an enlarged view of a portion a of fig. 10 according to the present invention.
Wherein:
100-cabinet, 101-control cabinet, 102-round port, 103-strip port;
200-a solution tank, 201-a sealing cover, 202-a liquid injection pipe, 203-a fixing lug, 2031-a triangular reinforcing rib plate, 204-a telescopic device, 205-a suction filtration through pipe, 206-a compression ring, 2061-an annular groove, 207-a rubber sealing ring, 208-a spring, 209-a heating jacket, 210-heat conduction oil, 211-a temperature sensor and 212-a first liquid level sensor;
300-a suction filtration assembly, 301-an insertion pipe, 302-a bearing tray and 303-a metal filter disc;
400-a filter paper switching device, 401-a filter paper winding roller, 402-a filter paper unwinding roller, 403-a filter paper roll, 404-a circular filter disc, 405-a winding rack, 406-a winding motor, 407-a scraper plate, 408-a torsion spring and 409-a fine material receiving groove;
500-liquid receiving tank, 501-tank neck pipe, 502-rubber pipe opening plug, 503-liquid discharge pipe, 504-sealing valve, 505-air suction pipe, 506-vacuum pump, 507-second liquid level sensor.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It should be understood that the data so used may be interchanged under appropriate circumstances such that embodiments of the application described herein may be used. Furthermore, the terms "comprises," "comprising," and any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The following will describe a purification method and apparatus for preparing L-5-methyltetrahydrocalcium folate disclosed in the present application in detail with reference to the accompanying drawings 1-11 and examples.
Firstly, the crude calcium L-5-methyltetrahydrofolate used in the embodiment of the invention is prepared by the preparation method disclosed in the invention with the patent number of CN 2018105003466.
Example 1
Embodiment 1 discloses a purification method for preparing L-5-methyltetrahydrocalcium folate, comprising the following steps:
1) taking a proper amount of 10kg of crude L-5-methyltetrahydrocalcium folate, putting the crude L-5-methyltetrahydrocalcium folate into 120kg of ionized water, heating and stirring the mixture until the mixture is uniformly mixed with the deionized water, and then carrying out ultrasonic treatment for 15 min;
2) heating the mixed solution after ultrasonic treatment to reflux;
3) and (3) putting the heated and refluxed mixed solution into a suction filtration device for suction filtration, and ensuring that the temperature of the mixed solution is 55 ℃ during suction filtration.
4) And drying the filtered crystal under hot air at 60 ℃ to obtain the refined L-5-methyltetrahydrocalcium folate, and detecting to obtain the purified refined L-5-methyltetrahydrocalcium folate with the purity of 98.6%.
Example 2
Embodiment 2 discloses a purification method for preparing L-5-methyltetrahydrocalcium folate, comprising the following steps:
1) taking a proper amount of 12kg of crude L-5-methyltetrahydrocalcium folate, putting the crude L-5-methyltetrahydrocalcium folate into 180kg of deionized water, heating and stirring the mixture until the mixture is uniformly mixed with the deionized water, and then carrying out ultrasonic treatment for 20 min;
2) heating the mixed solution after ultrasonic treatment to reflux;
3) and (3) putting the heated and refluxed mixed solution into a suction filtration device for suction filtration, and ensuring the temperature of the mixed solution to be 58 ℃ during suction filtration.
4) And drying the filtered crystal at 62 ℃ in hot air to obtain the purified L-5-methyltetrahydrocalcium folate, wherein the purity of the purified L-5-methyltetrahydrocalcium folate is up to 99.1 percent.
In summary, the purification methods disclosed in this embodiment 1 and embodiment 2 can ensure that the purity of the purified calcium L-5-methyltetrahydrofolate reaches more than 98%, and the whole purification method is simple and has high purification efficiency, and can realize industrial preparation and industrial purification of calcium L-5-methyltetrahydrofolate.
Example 3
Embodiment 3 discloses a purification device for preparing calcium L-5-methyltetrahydrofolate used in embodiments 1 and 2, and referring to fig. 2 and 3, the purification device comprises a cabinet 100, a solution tank 200, a suction filtration assembly 300, a filter paper switching device 400, and a liquid receiving tank 500.
In the specific design process, the liquid receiving tank 500 is fixedly disposed on the bottom wall of the inner cavity of the chassis 100 through a fixing clamp block (not shown in the figure). Referring to fig. 5, a tank neck 501 is opened at the upper end of the liquid receiving tank 500, and a rubber pipe opening plug 502 is arranged in the tank neck 501. A drain pipe 503 extending from the casing 100 is connected to the lower end of the liquid receiving tank 500, and a sealing valve 504 is provided on the drain pipe 503, and the sealing valve 504 can be a manual valve or an electromagnetic valve, and can seal the drain pipe 503 manually or electrically. Meanwhile, the upper end of the liquid receiving tank 500 is connected with an exhaust pipe 505, the lower end of the exhaust pipe 505 extending out of the case 100 is connected with a vacuum pump 506, the interior of the liquid receiving tank 500 can be pumped to a negative pressure state under the action of the vacuum pump 506, and the specific negative pressure value can be adjusted according to the running power of the vacuum pump 506.
Referring to fig. 4 and 6, a control cabinet 101 is disposed on the front side of the cabinet 100, a circular opening 102 is disposed on the upper surface of the cabinet 100 directly above the liquid receiving tank 500, the solution tank 200 is movably disposed in the circular opening 102, and the outer circumferential surface of the solution tank 200 is attached to the circular opening 102. Wherein, the upper end opening of the solution tank 200 is arranged, a sealing cover 201 is arranged at the opening end of the solution tank 200, a liquid injection pipe 202 is connected on the sealing cover 201, the sealing cover 201 seals the opening end of the solution tank 200 when the suction filtration operation is carried out, the liquid injection pipe 202 is connected with the solution tank after the heating and the reflux, and the mixed liquid can be continuously added into the solution tank 200 under the action of the infusion pump. Meanwhile, two fixing lugs 203 are symmetrically welded on the outer circumferential surface of the solution tank 200 in the inner cavity of the cabinet 100, in order to ensure the connection stability between the fixing lugs 203 and the solution tank 200, triangular reinforcing ribs 2031 are also welded on the lower surfaces of the fixing lugs 203, and the inner ends of the triangular reinforcing ribs 2031 are welded with the outer circumferential surface of the solution tank 200. The upper surface of the case 100 right above each fixing lug 203 is provided with a telescopic device 204, when the telescopic device 204 is specifically arranged, one of a hydraulic cylinder and an air cylinder can be selected, the lower end of a piston rod of the hydraulic cylinder or the air cylinder extends into the inner cavity of the case 100 to be connected with the corresponding fixing lug 203, and the whole solution tank 200 can move up and down along the circular opening 102 through the extension or contraction action of the piston rod of the telescopic device 204.
Referring to fig. 6 or 11, a suction filtration through pipe 205 is connected to the lower end of the solution tank 200, a compression ring 206 is connected to the lower end of the suction filtration through pipe 205, an annular groove 2061 is formed in the lower surface of the compression ring 206, a rubber seal 207 is disposed in the annular groove 2061, a plurality of springs 208 are disposed on the upper surface of the rubber seal 207 in an annular array, and the upper ends of the springs 208 are connected to the top wall of the annular groove 2061.
Referring to fig. 7 and 11, the suction filtration assembly 300 includes an insertion tube 301 extending into the access tank 500 through a rubber orifice plug 502, and the insertion tube 301 is sealingly connected to the rubber orifice plug 502 when passing through the plug. A support plate 302 aligned with the clamp ring 206 is connected to the upper end of the insertion tube 301, a metal filter disc 303 is provided on the upper surface of the support plate 302, and the inner cavity of the support plate 302 communicates with the insertion tube 301.
Referring to fig. 8 and 9, the filter paper switching device 400 includes a filter paper winding roller 401 and a filter paper unwinding roller 402 respectively disposed on the left and right sides of the chassis 100, a filter paper roll 403 wound on the filter paper unwinding roller 402, and an outer end of the filter paper roll 403 connected to the filter paper winding roller 401 through the strip-shaped openings 103 on the left and right sides of the chassis 100, wherein the filter paper roll 403 is attached to the support tray 302 in the inner cavity of the chassis 100. A plurality of circular filter pieces 404 are provided at equal intervals on the filter paper roll 403, and the circular filter pieces 404 are provided to have a diameter larger than that of the metal filter disc 303. A winding frame 405 is arranged on the left side surface of the case 100, the filter paper winding roller 401 is rotatably arranged at the outer end part of the winding frame 405, and a winding motor 406 for driving the filter paper winding roller 401 to rotate is arranged on the winding frame 405. The filter paper switching device 400 drives the filter paper roll 403 to move through the winding motor 405, when the circular filter disc 404 is aligned with the bearing tray 302, the whole solution tank 200 is pushed downwards through the effect of the telescopic device 204, so that the rubber sealing ring 207 at the lower end of the solution tank 200 is firstly pressed against the outer edge of the circular filter disc 404, then the solution tank 200 is continuously pushed downwards so that the rubber sealing ring 207 is recovered into the annular groove 2061, and therefore the outer edge between the pressing ring 206 and the bearing tray 302 is sealed, and the circular filter disc 404 is located between the pressing ring 206 and the bearing tray 302 (refer to fig. 10), and therefore subsequent suction filtration is directly performed. After the suction filtration is completed, when the filter paper needs to be replaced and crystals (namely, the refined L-5-methyltetrahydrocalcium folate) on the upper surface of the filter paper need to be recovered, the whole solution tank 200 is pushed upwards through the telescopic device 204, then the clamp ring 206 is separated from the bearing tray 302, the filter paper roll 403 extends out of the strip-shaped opening 103 under the action of the winding motor, and the circular filter disc 404 on the previous station and the next station of the filter paper roll 403 is just positioned between the clamp ring 206 and the bearing tray 302.
In order to realize the rapid recovery of the crystals on the upper surface of the filter paper, a scraping plate 407 is rotatably arranged in the winding frame 405 below the filter paper winding roller 401, the movable end of the scraping plate 407 is abutted against the filter paper winding roller 401, a torsion spring 408 is sleeved on a convex shaft at two ends of the scraping plate 407, two ends of the torsion spring 408 are respectively connected with the scraping plate 407 and the winding frame 405, and a fine material receiving groove 409 is arranged right below the scraping plate 407. The scraper plate 407 is always abutted against the filter paper take-up roll 401 by the torsion spring 408, and has a certain adjusting space. In addition, in order to prevent the filter paper from being scraped by the upper end of the strip-shaped opening 103 when the filter paper is pulled out from the strip-shaped opening 103, the height of the strip-shaped opening 103 formed on the left side surface of the case 100 is set to be greater than the height of the strip-shaped opening formed on the right side surface.
In addition, in order to keep the temperature of the mixed liquid in the solution tank 200 at a set temperature all the time during the suction filtration, in this embodiment, a heating jacket 209 is further disposed on the outer surface of the solution tank 200 located in the inner cavity of the chassis 100, heat conducting oil 210 is disposed in the heating jacket 209, a temperature sensor 211 is disposed inside the solution tank 200, the mixed liquid in the tank is heated by the heat conducting oil 210 in the heating jacket 209, and real-time feedback monitoring is performed by the temperature sensor 211.
Finally, in the present embodiment, a first liquid level sensor 212 and a second liquid level sensor 507 are respectively disposed inside the solution tank 200 and the liquid receiving tank 500. The liquid levels of the solution tank 200 and the liquid receiving tank 500 can be monitored in real time through the arrangement of the first liquid level sensor 212 and the second liquid level sensor 507, so that operators can conveniently supplement mixed liquid to the solution tank 200 in time or discharge filtered liquid in the liquid receiving tank 500.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A purification method for preparing L-5-methyl tetrahydrocalcium folate adopts a purification device for purification, and is characterized by comprising the following steps:
1) taking a proper amount of L-5-methyl tetrahydrocalcium folate crude material, putting the crude material into deionized water, heating and stirring the crude material until the crude material is uniformly mixed with the deionized water, and then carrying out ultrasonic treatment;
2) heating the mixed solution after ultrasonic treatment to reflux;
3) putting the mixed solution after heating and refluxing into a suction filtration device for suction filtration;
4) and drying the crystal after suction filtration to obtain the refined L-5-methyl tetrahydrofolic acid calcium.
2. The purification method for preparing calcium L-5-methyltetrahydrofolate according to claim 1, wherein the mass ratio of the crude calcium L-5-methyltetrahydrofolate to deionized water in step 1 is 1: 10-20.
3. The purification method for the production of calcium L-5-methyltetrahydrofolate according to claim 1, wherein the temperature of the heated and refluxed mixed solution is not lower than 50 ℃ during the suction filtration.
4. The purification device for preparing the calcium L-5-methyltetrahydrofolate according to any one of claims 1 to 3, which is a suction filtration device in step 3, and comprises a case (100), a solution tank (200), a suction filtration component (300), a filter paper switching device (400) and a liquid receiving tank (500).
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| CN202111499980.0A CN114130097A (en) | 2021-12-09 | 2021-12-09 | Purification method and device for preparing L-5-methyl tetrahydrocalcium folate |
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| CN202111499980.0A CN114130097A (en) | 2021-12-09 | 2021-12-09 | Purification method and device for preparing L-5-methyl tetrahydrocalcium folate |
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