CN114773362B - Cefoxitin sodium compound and preparation method thereof - Google Patents
Cefoxitin sodium compound and preparation method thereof Download PDFInfo
- Publication number
- CN114773362B CN114773362B CN202210672416.2A CN202210672416A CN114773362B CN 114773362 B CN114773362 B CN 114773362B CN 202210672416 A CN202210672416 A CN 202210672416A CN 114773362 B CN114773362 B CN 114773362B
- Authority
- CN
- China
- Prior art keywords
- shell
- bevel gear
- mixing
- drying
- outer side
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- GNWUOVJNSFPWDD-XMZRARIVSA-M Cefoxitin sodium Chemical compound [Na+].N([C@]1(OC)C(N2C(=C(COC(N)=O)CS[C@@H]21)C([O-])=O)=O)C(=O)CC1=CC=CS1 GNWUOVJNSFPWDD-XMZRARIVSA-M 0.000 title claims abstract description 50
- 229960003016 cefoxitin sodium Drugs 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 59
- 238000002156 mixing Methods 0.000 claims description 52
- 239000007864 aqueous solution Substances 0.000 claims description 37
- 229920006395 saturated elastomer Polymers 0.000 claims description 36
- 230000007246 mechanism Effects 0.000 claims description 35
- 238000001914 filtration Methods 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 30
- 239000003960 organic solvent Substances 0.000 claims description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- 230000005540 biological transmission Effects 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000010586 diagram Methods 0.000 claims description 6
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 4
- 229910017488 Cu K Inorganic materials 0.000 claims description 3
- 229910017541 Cu-K Inorganic materials 0.000 claims description 3
- 230000005260 alpha ray Effects 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000005057 refrigeration Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 7
- 239000003814 drug Substances 0.000 abstract description 2
- 238000003466 welding Methods 0.000 description 11
- 229960002682 cefoxitin Drugs 0.000 description 4
- 239000012043 crude product Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- HOKIDJSKDBPKTQ-GLXFQSAKSA-N cephalosporin C Chemical compound S1CC(COC(=O)C)=C(C(O)=O)N2C(=O)[C@@H](NC(=O)CCC[C@@H](N)C(O)=O)[C@@H]12 HOKIDJSKDBPKTQ-GLXFQSAKSA-N 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000588748 Klebsiella Species 0.000 description 1
- 241000219470 Mirabilis Species 0.000 description 1
- 241000588772 Morganella morganii Species 0.000 description 1
- 241000588653 Neisseria Species 0.000 description 1
- 108700020474 Penicillin-Binding Proteins Proteins 0.000 description 1
- 241000187747 Streptomyces Species 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940076266 morganella morganii Drugs 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/14—Compounds having a nitrogen atom directly attached in position 7
- C07D501/16—Compounds having a nitrogen atom directly attached in position 7 with a double bond between positions 2 and 3
- C07D501/20—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids
- C07D501/57—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids with a further substituent in position 7, e.g. cephamycines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/02—Preparation
- C07D501/12—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Cephalosporin Compounds (AREA)
Abstract
The invention belongs to the field of medicine preparation, in particular to a cefoxitin sodium compound and a preparation method thereof, and aims at the problems that the existing cefoxitin sodium compound preparation equipment is not easy and efficient, the required conditions in the preparation process are inconvenient to control and regulate, and the drying efficiency of the compound is low.
Description
Technical Field
The invention relates to the technical field of medicine preparation, in particular to a cefoxitin sodium compound and a preparation method thereof.
Background
Cefoxitin, a novel antibiotic which is prepared by semi-synthesizing the cephalosporin C produced by streptomyces in the market of cefoxitin in 1994 and developed by Merk company in the United states, is prepared by combining cefoxitin with one or more penicillin binding proteins, inhibits the biosynthesis of cell walls of cells with active bacterial division, thereby playing an antibacterial role, and the cefoxitin sodium has a stronger antibacterial role on sensitive strains of hemophilus, klebsiella, escherichia coli, morganella morganii, mirabilis, praecox and gonococcus in gram-negative bacteria, and is often not simple and efficient in preparation equipment of cefoxitin sodium compounds, inconvenient to control the preparation conditions in preparation and low in efficiency, and has a relatively low control over the drying process.
Disclosure of Invention
The invention aims to solve the defects that the preparation equipment of a cefoxitin sodium compound is not easy and efficient enough, the required conditions in the preparation process are inconvenient to control and regulate, and the drying efficiency of the compound is low in the prior art.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a cefoxitin sodium compound having a structure shown in formula i:
the X-ray powder diffraction pattern of the cefoxitin sodium compound obtained by Cu-K alpha ray measurement is shown in figure 7.
The invention also provides a preparation method of the cefoxitin sodium compound, which comprises the following steps: s1: the preparation device comprises a drying shell, a washing shell, a filtering shell, a mixing shell, a saturated aqueous solution shell and a mixed organic solvent shell, wherein the washing shell is connected with the filtering shell, the washing shell and the filtering shell are arranged at the top of the drying shell, the mixing shell is arranged at the top of the washing shell and the filtering shell, the saturated aqueous solution shell and the mixed organic solvent shell are arranged at the top of the mixing shell, a first feeding pipe is arranged at the top of the saturated aqueous solution shell, a water inlet pipe is arranged on the saturated aqueous solution shell, a heater is arranged on the outer side of the water inlet pipe, three second feeding pipes are arranged at the top of the mixed organic solvent shell, first conveying pipes are arranged at the bottoms of the saturated aqueous solution shell and the mixed organic solvent shell, the bottoms of the two first conveying pipes extend into the mixing shell, the saturated aqueous solution shell and the mixed organic solvent shell are internally provided with stirring mechanisms, one side of the mixing shell is provided with a first motor, the mixing shell is internally provided with a mixing mechanism, the first motor is matched with the stirring mechanism and the mixing mechanism, the outer side of the mixing shell is provided with refrigerating equipment, the bottom of the mixing shell is connected with a second conveying pipe, the bottom end of the second conveying pipe extends into the filtering shell, a filter screen plate is arranged in the filtering shell, the filtering shell and the washing shell are provided with the same rectangular channel pipe, the filter screen plate is connected with one end of the rectangular channel pipe, one side of the filtering shell is provided with a first discharge pipe, the washing shell is provided with a second discharge pipe, the bottom of the washing shell is connected with a third conveying pipe, the bottom end of the third conveying pipe extends into the drying shell and is rotationally connected with a throwing pipe, the drying shell is internally provided with a conveying mechanism, the top of the drying shell is provided with a vacuum pump, one side of the drying shell is provided with a transmission mechanism, the other side of the drying shell is fixedly provided with a second motor, and the second motor is matched with the transmission mechanism and the transmission mechanism;
s2: adding cefoxitin sodium into a saturated aqueous solution shell to be processed into cefoxitin sodium crude saturated aqueous solution, then respectively adding acetone, diethyl ether and acetonitrile into a mixed organic solvent shell to be processed into a mixed organic solvent, then sequentially passing through the mixed shell to be mixed and crystallized, filtering and collecting crystals through a filtering shell, washing the crystals through sewage ethanol in a washing shell, and finally drying and dehydrating the crystals in a vacuum environment through a drying shell to prepare the cefoxitin sodium compound.
Preferably, the stirring mechanism comprises a first rotating rod, and a plurality of stirring rods are arranged on the outer side of the first rotating rod.
Preferably, a transmission cavity is arranged in the mixing shell, a rotating shaft is rotatably arranged in the transmission cavity, one end of the rotating shaft extends to the outer side of the mixing shell and is welded with an output shaft of the first motor, two first bevel gears and a third bevel gear are fixedly sleeved on the outer side of the rotating shaft, a second bevel gear is fixedly connected to the bottom end of the first rotating rod, the second bevel gear is meshed with the first bevel gear, and the rotating shaft can drive the second bevel gear to rotate through the first bevel gear.
Preferably, the mixing mechanism comprises a second rotating rod rotatably arranged in the mixing shell, a plurality of mixing rods are arranged on the outer side of the second rotating rod, the top end of the second rotating rod extends into the transmission cavity and is fixedly connected with a fourth bevel gear, the fourth bevel gear is meshed with a third bevel gear, and the third bevel gear drives the fourth bevel gear to rotate.
Preferably, the conveying mechanism comprises a driving rod and a driven rod which are rotatably arranged in the drying shell, the outsides of the driving rod and the driven rod are fixedly sleeved with rotary rollers, the outsides of the two rotary rollers are sleeved with the same conveying belt, one end of the driving rod extends to the outside of the drying shell and is welded with an output shaft of the second motor, and the rotary rollers can drive the conveying belt to roll.
Preferably, the transmission mechanism comprises two fixing plates arranged on the other side of the drying shell, the two fixing plates are provided with the same third rotary rod, one end of the driving rod extends to the outer side of the drying shell and is fixedly connected with a fifth bevel gear, a sixth bevel gear is fixedly sleeved on the outer side of the third rotary rod, the sixth bevel gear is meshed with the fifth bevel gear, and the fifth bevel gear can drive the sixth bevel gear to rotate.
Preferably, the outside fixed cover of third rotary rod is equipped with two seventh bevel gears, and the opposite side of drying shell rotates and installs two fourth rotary rods, and the equal fixedly connected with eighth bevel gear of one end of two fourth rotary rods, eighth bevel gear meshes with seventh bevel gear, and seventh bevel gear can drive eighth bevel gear and rotate.
Preferably, the outer sides of the two fourth rotating rods are fixedly sleeved with half gears, the other side of the drying shell is rotatably provided with a fifth rotating rod, one end of the fifth rotating rod extends to the outer side of the drying shell and is fixedly connected with a rotating gear, the rotating gear is meshed with the half gears, and the two half gears can be alternately meshed with the rotating gears to rotate.
Preferably, the other end of the fifth rotating rod extends into the drying shell and is fixedly connected with a ninth bevel gear, a tenth bevel gear is fixedly sleeved on the outer side of the throwing pipe, the tenth bevel gear is meshed with the ninth bevel gear, and the ninth bevel gear can drive the tenth bevel gear to rotate.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the scheme, the first bevel gear is matched with the second bevel gear, the first rotating rod is matched with the stirring rod, so that the needed cefoxitin sodium crude product saturated aqueous solution and the mixed organic solvent for preparing acetone, diethyl ether and acetonitrile can be prepared quickly and effectively, and the cefoxitin sodium crude product saturated aqueous solution needs to be kept at about 70 ℃ during preparation;
2. according to the scheme, the third bevel gear is matched with the fourth bevel gear, the second rotating rod is matched with the mixing rod, so that a cefoxitin sodium crude saturated aqueous solution and a mixed organic solvent for preparing acetone, diethyl ether and acetonitrile can be effectively mixed, the temperature of the mixed solution is gradually reduced to zero ℃, and then the mixed solution is kept stand, so that the crystallization process is completed;
3. according to the scheme, the two half gears are matched with the rotary gear, and the ninth bevel gear is matched with the tenth bevel gear, so that the compound crystals can be uniformly put on a slowly rolling conveyor belt by the putting pipe, and the spread compound crystals are rapidly dried and dehydrated in a vacuum environment to finish final processing;
the invention can rapidly prepare the aqueous solution and the organic solution required by preparing the cefoxitin sodium compound, mix and crystallize the cefoxitin sodium compound under certain conditions, and then sequentially filter, wash and dry the cefoxitin sodium compound, and the efficiency of drying and dewatering is improved by spreading the cefoxitin sodium compound in a vacuum environment.
Drawings
Fig. 1 is a schematic structural diagram of a cefoxitin sodium compound and a preparation method thereof;
fig. 2 is a schematic structural diagram of a mixed shell, a saturated aqueous solution shell and a mixed organic solvent shell of the cefoxitin sodium compound and the preparation method thereof;
fig. 3 is a schematic structural diagram of a drying shell, a filtering shell and a washing shell of the cefoxitin sodium compound and the preparation method thereof;
fig. 4 is a schematic top view of a dry shell of a cefoxitin sodium compound and a preparation method thereof according to the present invention;
fig. 5 is an enlarged schematic diagram of the structure at a in fig. 4 of a cefoxitin sodium compound and a preparation method thereof;
fig. 6 is a schematic perspective view of a filter screen plate and a rectangular channel tube of a cefoxitin sodium compound and a preparation method thereof;
fig. 7 is an X-ray powder diffraction pattern of a cefoxitin sodium compound according to the present invention, as measured using Cu-ka radiation.
In the figure: a drying case, a washing case, a 3 filtration case, a 4 mixing case, a 5 saturated aqueous solution case, a 6 mixed organic solvent case, a 7 first feed pipe, an 8 water feed pipe, a 9 first feed pipe, a 10 first motor, an 11 refrigeration device, a 12 second feed pipe, a 13 filtration net plate, a 14 rectangular channel pipe, a 15 first discharge pipe, a 16 second discharge pipe, a 17 third feed pipe, a 18 second feed pipe, a 19 throw pipe, a 20 vacuum pump, a 21 second motor, a 22 first rotary rod, a 23 stirring rod, a 24 rotary shaft, a 25 first bevel gear, a 26 second bevel gear, a 27 third bevel gear, a 28 second rotary rod, a 29 mixing rod, a 30 fourth bevel gear, a 31 rotary roller, a 32 conveyor belt, a 33 third rotary rod, a 34 fifth bevel gear, a 35 sixth bevel gear, a 36 seventh bevel gear, a 37 fourth rotary rod, a 38 eighth bevel gear, a 39 half gear, a 40 fifth rotary rod, a 41 rotary gear, a 42 ninth bevel gear, and a 43 tenth bevel gear.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Example 1
Referring to fig. 1-6, a cefoxitin sodium compound has a structure shown in formula i:
an X-ray powder diffraction diagram of the cefoxitin sodium compound obtained by Cu-K alpha ray measurement is shown in figure 7.
The embodiment also provides a preparation method of the cefoxitin sodium compound, which comprises the following steps: s1: the preparation device comprises a drying shell 1, a washing shell 2, a filtering shell 3, a mixing shell 4, a saturated aqueous solution shell 5 and a mixed organic solvent shell 6, and is characterized in that the washing shell 2 and the filtering shell 3 are connected with each other, the washing shell 2 and the filtering shell 3 are arranged at the top of the drying shell 1, the mixing shell 4 is arranged at the top of the washing shell 2 and the filtering shell 3, the saturated aqueous solution shell 5 and the mixed organic solvent shell 6 are arranged at the top of the mixing shell 4, a first feeding pipe 7 is arranged at the top of the saturated aqueous solution shell 5, a water inlet pipe 8 is arranged on the saturated aqueous solution shell 5, a heater is arranged outside the water inlet pipe 8, three second feeding pipes 18 are arranged at the top of the mixed organic solvent shell 6, a first conveying pipe 9 is arranged at the bottoms of the saturated aqueous solution shell 5 and the mixed organic solvent shell 6, the bottom ends of the two first conveying pipes 9 extend into the mixing shell 4, stirring mechanisms are arranged in the saturated aqueous solution shell 5 and the mixed organic solvent shell 6, a first motor 10 is arranged on one side of the mixing shell 4, the mixing mechanism is arranged in the mixing shell 4, the first motor 10 is matched with the stirring mechanism and the mixing mechanism, a refrigerating device 11 is arranged on the outer side of the mixing shell 4, a second conveying pipe 12 is connected to the bottom of the mixing shell 4, the bottom end of the second conveying pipe 12 extends into the filtering shell 3, a filter screen 13 is arranged in the filtering shell 3, the filtering shell 3 and the washing shell 2 are provided with the same rectangular channel pipe 14, the filter screen 13 is connected with one end of the rectangular channel pipe 14, one side of the filtering shell 3 is provided with a first discharge pipe 15, the washing shell 2 is provided with a second discharge pipe 16, the bottom of the washing shell 2 is connected with a third conveying pipe 17, the bottom end of the third conveying pipe 17 extends into the drying shell 1 and is rotationally connected with a delivery pipe 19, a conveying mechanism is arranged in the drying shell 1, a vacuum pump 20 is arranged at the top of the drying shell 1, a conveying mechanism is arranged on one side of the drying shell 1, a second motor 21 is fixedly arranged on the other side of the drying shell 1, and the second motor 21 is matched with the conveying mechanism and the conveying mechanism;
s2: the cefoxitin sodium is added into a saturated aqueous solution shell 5 to be processed into a cefoxitin sodium crude saturated aqueous solution, then acetone, diethyl ether and acetonitrile are respectively added into a mixed organic solvent shell 6 to be processed into a mixed organic solvent, then the mixed organic solvent is sequentially mixed and crystallized through a mixed shell 4, the crystals are filtered and collected through a filtering shell 3, the crystals are washed through sewage ethanol in a washing shell 2, and finally the dried shell 1 is dried and dehydrated in a vacuum environment to prepare the cefoxitin sodium compound.
In this embodiment, the stirring mechanism includes a first rotating rod 22, and a plurality of stirring rods 23 are provided outside the first rotating rod 22.
In this embodiment, a transmission cavity is disposed in the hybrid housing 4, a rotation shaft 24 is rotatably mounted in the transmission cavity, one end of the rotation shaft 24 extends to the outer side of the hybrid housing 4 and is welded with an output shaft of the first motor 10, two first bevel gears 25 and a third bevel gear 27 are sleeved on the outer side of the rotation shaft 24 through welding, a second bevel gear 26 is fixedly connected to the bottom end of the first rotation rod 22 through welding, the second bevel gear 26 is meshed with the first bevel gear 25, and the rotation shaft 24 can drive the second bevel gear 26 to rotate through the first bevel gear 25.
In this embodiment, the mixing mechanism includes a second rotating rod 28 rotatably installed in the mixing housing 4, a plurality of mixing rods 29 are disposed on the outer side of the second rotating rod 28, and the top end of the second rotating rod 28 extends into the transmission cavity and is fixedly connected with a fourth bevel gear 30 through welding, the fourth bevel gear 30 is meshed with the third bevel gear 27, and the third bevel gear 27 drives the fourth bevel gear 30 to rotate.
In this embodiment, the conveying mechanism includes a driving rod and a driven rod rotatably installed in the drying shell 1, the outsides of the driving rod and the driven rod are respectively provided with a rotary roller 31 through a welded fixing sleeve, the outsides of the two rotary rollers 31 are sleeved with the same conveying belt 32, one end of the driving rod extends to the outside of the drying shell 1 and is welded with the output shaft of the second motor 21, and the rotary rollers 31 can drive the conveying belt 32 to roll.
In this embodiment, the transmission mechanism includes two fixing plates disposed on the other side of the drying shell 1, the two fixing plates are provided with the same third rotating rod 33, one end of the driving rod extends to the outer side of the drying shell 1 and is fixedly connected with a fifth bevel gear 34 through welding, a sixth bevel gear 35 is sleeved on the outer side of the third rotating rod 33 through welding, the sixth bevel gear 35 is meshed with the fifth bevel gear 34, and the fifth bevel gear 34 can drive the sixth bevel gear 35 to rotate.
In this embodiment, two seventh bevel gears 36 are sleeved on the outer side of the third rotating rod 33 through a welding fixing sleeve, two fourth rotating rods 37 are rotatably installed on the other side of the drying shell 1, one ends of the two fourth rotating rods 37 are fixedly connected with an eighth bevel gear 38 through welding, the eighth bevel gear 38 is meshed with the seventh bevel gear 36, and the seventh bevel gear 36 can drive the eighth bevel gear 38 to rotate.
In this embodiment, the outer sides of the two fourth rotating rods 37 are all provided with half gears 39 through a welding fixing sleeve, the other side of the drying shell 1 is rotatably provided with a fifth rotating rod 40, one end of the fifth rotating rod 40 extends to the outer side of the drying shell 1 and is fixedly connected with a rotating gear 41 through welding, the rotating gear 41 is meshed with the half gears 39, and the two half gears 39 can be alternately meshed with the rotating gear 41 for rotation.
In this embodiment, the other end of the fifth rotating rod 40 extends into the drying shell 1 and is fixedly connected with a ninth bevel gear 42 through welding, a tenth bevel gear 43 is sleeved on the outer side of the feeding pipe 19 through welding, the tenth bevel gear 43 is meshed with the ninth bevel gear 42, and the ninth bevel gear 42 can drive the tenth bevel gear 43 to rotate.
In the embodiment, during preparation, a certain amount of cefoxitin sodium is put into a saturated aqueous solution shell 5 through a first feed pipe 7, then water with a certain proportion is added through a water inlet pipe 8, the added water is heated through a heater to be about seventy degrees celsius, meanwhile, acetone, diethyl ether and acetonitrile are respectively added into a mixed organic solvent shell 6 through three second feed pipes 18, then a first motor 10 is started, an output shaft of the first motor 10 drives a rotating shaft 24 to rotate, the rotating shaft 24 simultaneously drives a first bevel gear 25 and a third bevel gear 27 to rotate, the first bevel gear 25 drives a second bevel gear 26 to rotate, the second bevel gear 26 drives a first rotating rod 22 to rotate, the first rotating rod 22 drives a stirring rod 23 to rotate, a saturated aqueous solution of cefoxitin sodium crude product at about seventy degrees celsius is quickly obtained in the saturated aqueous solution shell 5, a mixed solvent of acetone, diethyl ether and acetonitrile is quickly obtained in the mixed organic solvent shell 6, and the mixed solvent is five times that of the saturated aqueous solution of cefoxitin crude product; then, the mixed solvent of acetone, diethyl ether and acetonitrile is conveyed into the mixing shell 4 through the first conveying pipe 9, then, the cefoxitin sodium crude saturated aqueous solution is slowly added into the mixing shell 4 through the other first conveying pipe 9, meanwhile, the third bevel gear 27 drives the fourth bevel gear 30 to rotate, the fourth bevel gear 30 drives the second rotary rod 28 to rotate, the second rotary rod 28 drives the mixing rod 29 to rotate, the mixing rod 29 can effectively mix the materials, meanwhile, the mixing shell 4 is cooled through the refrigerating equipment 11 until the temperature of the mixed solution is reduced to zero ℃, and then, the mixed solution can be stood for crystallization; after standing crystallization is finished, the solution and the crystals are conveyed into the filter shell 3 through the second conveying pipe 12, the crystals are intercepted through the filter screen plate 13, the solution is discharged through the first discharge pipe 15, the crystals enter the washing shell 2 through the rectangular channel pipe 14, the crystals are washed through absolute ethyl alcohol in the washing shell 2, then the absolute ethyl alcohol is discharged through the second discharge pipe 16, the crystals are conveyed into the drying shell 1 through the third conveying pipe 17, a vacuum environment is formed in the drying shell 1 by the vacuum pump 20, the boiling point of water is effectively reduced, the water is easier to evaporate, the drying and the water removal of crystalline compounds are facilitated, and meanwhile, the second motor 21 is started; the output shaft of the second motor 21 drives the driving rod to rotate, the driving rod drives the conveyor belt 32 to slowly rotate through the rotating roller 31, meanwhile, the driving rod drives the fifth bevel gear 34 to rotate, the fifth bevel gear 34 drives the third rotating rod 33 to rotate through the sixth bevel gear 35, the third rotating rod 33 drives the seventh bevel gear 36 to rotate, the seventh bevel gear 36 drives the fourth rotating rod 37 to rotate through the eighth bevel gear 38, the fourth rotating rod 37 drives the half gear 39 to rotate, the two half gears 39 can alternately rotate with the rotating gear 41, the rotating gear 41 can rotate back and forth, the rotating gear 41 can drive the ninth bevel gear 42 to rotate through the fifth rotating rod 40, the ninth bevel gear 42 can drive the tenth bevel gear 43 to rotate, and the tenth bevel gear 43 can drive the throwing pipe 19 to swing back and forth, so that crystalline compounds discharged by the throwing pipe 19 can be effectively and evenly paved on the conveyor belt 32, drying and dewatering are more convenient, and collection is convenient.
Example two
The difference from the first embodiment is that: the bottom of saturated aqueous solution casing 5 and mixed organic solvent casing 6 all is provided with weight sensor for detect the ratio weight variation of solution and solvent, all be provided with temperature sensor simultaneously in saturated aqueous solution casing 5 and mixed casing 4 for detect the control to the temperature of required preparation environment, be provided with air humidity sensor in the dry casing 1, detect the humidity in the dry casing 1 constantly, thereby can obtain the dry dewatering condition of crystalline compound.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (4)
1. The preparation method of the cefoxitin sodium compound comprises the following steps:
；
wherein the X-ray powder diffraction diagram of the prepared cefoxitin sodium compound obtained by Cu-K alpha ray measurement is shown in figure 7;
the preparation method comprises the following steps:
s1: the preparation device comprises a drying shell (1), a washing shell (2), a filtering shell (3), a mixing shell (4), a saturated aqueous solution shell (5) and a mixed organic solvent shell (6), wherein the washing shell (2) and the filtering shell (3) are connected with each other, the washing shell (2) and the filtering shell (3) are arranged at the top of the drying shell (1), the mixing shell (4) is arranged at the top of the washing shell (2) and the filtering shell (3), the saturated aqueous solution shell (5) and the mixed organic solvent shell (6) are arranged at the top of the mixing shell (4), the top of the saturated aqueous solution shell (5) is provided with a first feeding pipe (7), the saturated aqueous solution shell (5) is provided with a water inlet pipe (8), the outer side of the water inlet pipe (8) is provided with a heater, the top of the mixed organic solvent shell (6) is provided with three second feeding pipes (18), the bottoms of the saturated aqueous solution shell (5) and the mixed organic solvent shell (6) are respectively provided with a first conveying pipe (9), the bottoms of the two first conveying pipes (9) are respectively extended to the top of the mixing shell (4) and the mixed organic solvent shell (6), the saturated aqueous solution (5) is respectively mixed with a first stirring mechanism (10) is arranged at one side of the mixing shell (4), the mixing mechanism is arranged in the mixing shell (4), the first motor (10) is matched with the stirring mechanism and the mixing mechanism, refrigeration equipment (11) is arranged on the outer side of the mixing shell (4), the bottom of the mixing shell (4) is connected with a second conveying pipe (12), the bottom end of the second conveying pipe (12) extends into the filtering shell (3), a filter screen plate (13) is arranged in the filtering shell (3), the filtering shell (3) and the washing shell (2) are provided with the same rectangular channel pipe (14), the filter screen plate (13) is connected with one end of the rectangular channel pipe (14), one side of the filtering shell (3) is provided with a first discharge pipe (15), the washing shell (2) is provided with a second discharge pipe (16), the bottom of the washing shell (2) is connected with a third conveying pipe (17), the bottom end of the third conveying pipe (17) extends into the drying shell (1) and is rotationally connected with a delivery pipe (19), the drying shell (1) is internally provided with a conveying mechanism, the top of the drying shell (1) is provided with a vacuum pump (20), one side of the drying shell (1) is provided with the motor, one side of the drying shell (1) is provided with the second conveying mechanism (21), and the motor is matched with the second conveying mechanism (21); the stirring mechanism comprises a first rotating rod (22), and a plurality of stirring rods (23) are arranged on the outer side of the first rotating rod (22); a transmission cavity is formed in the mixing shell (4), a rotating shaft (24) is rotatably arranged in the transmission cavity, one end of the rotating shaft (24) extends to the outer side of the mixing shell (4) and is welded with an output shaft of the first motor (10), two first bevel gears (25) and a third bevel gear (27) are fixedly sleeved on the outer side of the rotating shaft (24), a second bevel gear (26) is fixedly connected to the bottom end of the first rotating rod (22), and the second bevel gear (26) is meshed with the first bevel gear (25); the mixing mechanism comprises a second rotating rod (28) rotatably arranged in the mixing shell (4), a plurality of mixing rods (29) are arranged on the outer side of the second rotating rod (28), the top end of the second rotating rod (28) extends into the transmission cavity and is fixedly connected with a fourth bevel gear (30), and the fourth bevel gear (30) is meshed with the third bevel gear (27); the conveying mechanism comprises a driving rod and a driven rod which are rotatably arranged in the drying shell (1), the outer sides of the driving rod and the driven rod are fixedly sleeved with rotary rollers (31), the outer sides of the two rotary rollers (31) are sleeved with the same conveying belt (32), and one end of the driving rod extends to the outer side of the drying shell (1) and is welded with an output shaft of the second motor (21); the transmission mechanism comprises two fixed plates arranged on the other side of the drying shell (1), the two fixed plates are provided with the same third rotary rod (33), one end of the driving rod extends to the outer side of the drying shell (1) and is fixedly connected with a fifth bevel gear (34), a sixth bevel gear (35) is fixedly sleeved on the outer side of the third rotary rod (33), and the sixth bevel gear (35) is meshed with the fifth bevel gear (34);
s2: adding cefoxitin sodium into a saturated aqueous solution shell (5) to be processed into a cefoxitin sodium crude saturated aqueous solution, then adding acetone, diethyl ether and acetonitrile into a mixed organic solvent shell (6) to be processed into a mixed organic solvent, then sequentially mixing and crystallizing the cefoxitin sodium through a mixed shell (4), filtering and collecting crystals through a filtering shell (3), washing the crystals through absolute ethyl alcohol in a washing shell (2), and finally drying and dehydrating the crystals through a drying shell (1) in a vacuum environment to prepare the cefoxitin sodium compound.
2. The preparation method of the cefoxitin sodium compound according to claim 1, wherein two seventh bevel gears (36) are fixedly sleeved on the outer side of the third rotating rod (33), two fourth rotating rods (37) are rotatably arranged on the other side of the drying shell (1), one ends of the two fourth rotating rods (37) are fixedly connected with eighth bevel gears (38), and the eighth bevel gears (38) are meshed with the seventh bevel gears (36).
3. The preparation method of the cefoxitin sodium compound according to claim 2, wherein a half gear (39) is fixedly sleeved on the outer sides of the two fourth rotating rods (37), a fifth rotating rod (40) is rotatably arranged on the other side of the drying shell (1), one end of the fifth rotating rod (40) extends to the outer side of the drying shell (1) and is fixedly connected with a rotating gear (41), and the rotating gear (41) is meshed with the half gear (39).
4. A method for preparing a cefoxitin sodium compound according to claim 3, wherein the other end of the fifth rotating rod (40) extends into the drying shell (1) and is fixedly connected with a ninth bevel gear (42), a tenth bevel gear (43) is fixedly sleeved on the outer side of the throwing pipe (19), and the tenth bevel gear (43) is meshed with the ninth bevel gear (42).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210672416.2A CN114773362B (en) | 2022-06-15 | 2022-06-15 | Cefoxitin sodium compound and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210672416.2A CN114773362B (en) | 2022-06-15 | 2022-06-15 | Cefoxitin sodium compound and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114773362A CN114773362A (en) | 2022-07-22 |
| CN114773362B true CN114773362B (en) | 2023-12-29 |
Family
ID=82420252
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210672416.2A Active CN114773362B (en) | 2022-06-15 | 2022-06-15 | Cefoxitin sodium compound and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114773362B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304582A (en) * | 2013-06-28 | 2013-09-18 | 四川省惠达药业有限公司 | Cefoxitin sodium compound, preparation method and pharmaceutical composition thereof |
| CN103601739A (en) * | 2013-11-26 | 2014-02-26 | 悦康药业集团有限公司 | Cefoxitin sodium compound and preparation method thereof |
| CN211688287U (en) * | 2019-08-12 | 2020-10-16 | 青海启迪清源新材料有限公司 | Lithium hydroxide monohydrate crystallization separation purification device |
| CN112371069A (en) * | 2020-10-23 | 2021-02-19 | 无锡市张华医药设备有限公司 | Continuous reaction, crystallization, filtration, washing, drying system |
| CN216295255U (en) * | 2021-04-26 | 2022-04-15 | 常州市百得干燥工程有限公司 | Efficient filtering, washing and drying unit |
| CN114516659A (en) * | 2022-04-08 | 2022-05-20 | 洛阳海惠新材料股份有限公司 | Equipment and method for producing sodium pyroantimonate by pure oxygen oxidation method |
-
2022
- 2022-06-15 CN CN202210672416.2A patent/CN114773362B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304582A (en) * | 2013-06-28 | 2013-09-18 | 四川省惠达药业有限公司 | Cefoxitin sodium compound, preparation method and pharmaceutical composition thereof |
| CN103601739A (en) * | 2013-11-26 | 2014-02-26 | 悦康药业集团有限公司 | Cefoxitin sodium compound and preparation method thereof |
| CN211688287U (en) * | 2019-08-12 | 2020-10-16 | 青海启迪清源新材料有限公司 | Lithium hydroxide monohydrate crystallization separation purification device |
| CN112371069A (en) * | 2020-10-23 | 2021-02-19 | 无锡市张华医药设备有限公司 | Continuous reaction, crystallization, filtration, washing, drying system |
| CN216295255U (en) * | 2021-04-26 | 2022-04-15 | 常州市百得干燥工程有限公司 | Efficient filtering, washing and drying unit |
| CN114516659A (en) * | 2022-04-08 | 2022-05-20 | 洛阳海惠新材料股份有限公司 | Equipment and method for producing sodium pyroantimonate by pure oxygen oxidation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114773362A (en) | 2022-07-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114773362B (en) | Cefoxitin sodium compound and preparation method thereof | |
| CN107649354A (en) | A kind of agricultural sieves granulator with chemical fertilizer | |
| CN208872010U (en) | A kind of continuous roller drier | |
| CN112390243B (en) | Equipment for preparing lithium difluorophosphate | |
| CN212757304U (en) | Crystallization device for phosphate production | |
| CN103073563A (en) | Preparation method for cefotetan disodium | |
| CN207822972U (en) | Biological organic fertilizer drum granulating machine | |
| CN111829308B (en) | Dry dewatering device of fertilizer | |
| CN115253974A (en) | Dehydration kettle for piperazine compound production and working method thereof | |
| CN102746323B (en) | Crystal form of cefuroxime acid and preparation method thereof | |
| CN108101927A (en) | A kind of method for preparing rifampin crystal form II | |
| CN113042144A (en) | A grinding device for rice processing | |
| CN111729341A (en) | Freezing crystallizer mechanism | |
| CN113739534A (en) | Efficient drying device for milk powder preparation | |
| CN219934563U (en) | Raw material sterilizing and drying device with turning structure | |
| CN221172877U (en) | A filter drying device for lees is retrieved | |
| CN219120993U (en) | Drying equipment for producing medical intermediate | |
| CN111034412A (en) | Corn seed is with capsule device | |
| CN220892774U (en) | Compound fertilizer granule circulation dispersion formula drying device | |
| CN221005844U (en) | Lithium fluoride microwave drying device | |
| CN217657002U (en) | Seed coating device capable of achieving rapid drying | |
| CN220052403U (en) | Plastic granules anti-adhesion stirring bin | |
| CN219977037U (en) | Automatic feeding and discharging device of flat bed dryer | |
| CN210492438U (en) | Hot-blast wind package structure of tealeaves machinery | |
| CN219494671U (en) | Positioning and feeding mechanism of dryer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |