CN116655559A - Process and device for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor - Google Patents
Process and device for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor Download PDFInfo
- Publication number
- CN116655559A CN116655559A CN202310416872.5A CN202310416872A CN116655559A CN 116655559 A CN116655559 A CN 116655559A CN 202310416872 A CN202310416872 A CN 202310416872A CN 116655559 A CN116655559 A CN 116655559A
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- stirring
- square frame
- rotating shaft
- mercaptobenzothiazole
- columns
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- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 title claims abstract description 106
- GPRBEKHLDVQUJE-VINNURBNSA-N cefotaxime Chemical compound N([C@@H]1C(N2C(=C(COC(C)=O)CS[C@@H]21)C(O)=O)=O)C(=O)/C(=N/OC)C1=CSC(N)=N1 GPRBEKHLDVQUJE-VINNURBNSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000012452 mother liquor Substances 0.000 title claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 85
- 239000007788 liquid Substances 0.000 claims abstract description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000010413 mother solution Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 230000005540 biological transmission Effects 0.000 claims description 35
- 238000007790 scraping Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 239000003814 drug Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 239000004480 active ingredient Substances 0.000 abstract 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 238000011084 recovery Methods 0.000 description 5
- 229960000479 ceftriaxone sodium Drugs 0.000 description 4
- FDRNWTJTHBSPMW-GNXCPKRQSA-L disodium;(6r,7r)-7-[[(2e)-2-(2-amino-1,3-thiazol-4-yl)-2-methoxyiminoacetyl]amino]-3-[(2-methyl-6-oxido-5-oxo-1,2,4-triazin-3-yl)sulfanylmethyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate Chemical compound [Na+].[Na+].S([C@@H]1[C@@H](C(N1C=1C([O-])=O)=O)NC(=O)/C(=N/OC)C=2N=C(N)SC=2)CC=1CSC1=NC(=O)C([O-])=NN1C FDRNWTJTHBSPMW-GNXCPKRQSA-L 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 2
- 235000017491 Bambusa tulda Nutrition 0.000 description 2
- 241001330002 Bambuseae Species 0.000 description 2
- 229930186147 Cephalosporin Natural products 0.000 description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000011425 bamboo Substances 0.000 description 2
- 229940124587 cephalosporin Drugs 0.000 description 2
- 150000001780 cephalosporins Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- AZZMGZXNTDTSME-JUZDKLSSSA-M cefotaxime sodium Chemical compound [Na+].N([C@@H]1C(N2C(=C(COC(C)=O)CS[C@@H]21)C([O-])=O)=O)C(=O)\C(=N/OC)C1=CSC(N)=N1 AZZMGZXNTDTSME-JUZDKLSSSA-M 0.000 description 1
- 229960002727 cefotaxime sodium Drugs 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- -1 tires Substances 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
- C07D277/62—Benzothiazoles
- C07D277/68—Benzothiazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D277/70—Sulfur atoms
- C07D277/72—2-Mercaptobenzothiazole
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Accessories For Mixers (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process and a device for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor, which relate to the technical field of medicines, can obtain high-purity pharmaceutical active ingredients through a simple process, simultaneously recover high-quality MBT, can be applied to recovering MBT from cefotaxime acid mother liquor in industrial production, and reduce the content of 2-mercaptobenzothiazole in cefotaxime acid by adjusting centrifugal washing and stirring processes of cefotaxime acid. The key points of the technical scheme are as follows: the method comprises the following steps: s1, adding a sodium hydroxide solution into a cefotaxime acid mother solution in a stirring kettle, and adjusting the pH; s2, transferring the mixed solution obtained in the step S1 into a rectifying tower, heating and raising the temperature, evaporating light components from the top of the tower, and leaving the liquid in the rectifying tower; s3, transferring the residual liquid after the rectification of S2 into a crystallization tank, adding water, stirring and cooling to obtain MBT crystals; s4, performing suction filtration on the MBT crystal, and drying to obtain the MBT.
Description
Technical Field
The invention relates to the technical field of medicines, in particular to a process and a device for recovering MBT from cefotaxime acid mother liquor.
Background
2-Mercaptobenzothiazole (MBT) is an important vulcanization accelerator in the rubber industry, is widely applied to manufacturing various rubber products such as tires, rubber tapes and the like, and can be used as an electroplating additive, a brightening agent, a lubricating oil additive, a metal preservative and the like. In the production process of cephalosporin antibiotics such as ceftriaxone sodium, cefotaxime sodium and the like, a large amount of byproduct 2-mercaptobenzothiazole is generated, so that the 2-mercaptobenzothiazole exists in a large amount in cephalosporin medicine waste liquid, and how to recycle the 2-mercaptobenzothiazole and effectively avoid pollution is a research-worthy direction.
The publication No. CN109053627A discloses a comprehensive recovery method of 2-mercaptobenzothiazole, triethylamine and dichloromethane in ceftriaxone sodium dichloromethane mother liquor, which can realize comprehensive recovery of 2-mercaptobenzothiazole, triethylamine and dichloromethane, maximally recycle organic matters and reduce environmental pollution of the organic matters; the waste water generated in the recovery process is used mechanically, so that the consumption of acid and alkali in the extraction process is reduced, and the discharge of sewage is controlled, thereby having good practical prospect. Publication No. CN102351809A discloses a method for recovering 2-mercaptobenzothiazole from ceftriaxone sodium crystallization mother liquor, which comprises the following steps: (1) adjusting the pH value of the ceftriaxone sodium crystallization mother liquor to 2.0-5.0 by using sulfuric acid solution; (2) heating and distilling the mother solution obtained in the step (1), distilling the solvent, controlling the total amount of the distilled solvent to be 75-90% of the total amount of the mother solution, and reserving the distilled residual solution for later use; (3) cooling the residual solution obtained in the step (2) to 0-35 ℃, and filtering to obtain filtrate for later use; (4) adding 1-5 times of water with the volume of the filtrate obtained in the step (3) into the filtrate, stirring, and separating out solids; (5) filtering out the solid obtained in the step (4), washing with water and drying to obtain the target product 2-mercaptobenzothiazole. The method has the advantages of simple operation, high yield, low cost, little pollution and the like, and has good application prospect.
The invention provides a process and a device for recycling 2-mercaptobenzothiazole from cefotaxime acid mother liquor, which can recycle the 2-mercaptobenzothiazole with high purity through a simple process and can be applied to recycling the 2-mercaptobenzothiazole from the cefotaxime acid mother liquor in industrial production.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide a process and a device for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor, which can effectively recover high-purity 2-mercaptobenzothiazole.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a process for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor, which comprises the following steps:
s1, adding a sodium hydroxide solution into a cefotaxime acid mother solution in a stirring kettle, and adjusting the pH;
s2, transferring the mixed solution obtained in the step S1 into a rectifying tower, heating and raising the temperature, evaporating light components from the top of the tower, and leaving the liquid in the rectifying tower;
s3, transferring the residual liquid after the rectification of S2 into a crystallization tank, adding water, stirring and cooling to obtain MBT crystals;
s4, performing suction filtration on the MBT crystal, and drying to obtain the MBT.
Preferably, the concentration of the sodium hydroxide is 10%, the pH is 4-5, and the stirring temperature is 10-35 ℃;
the rectifying tower is heated to the temperature of 95 ℃ at the tower bottom and 85 ℃ at the tower top;
the drying temperature in the S4 is 40-60 ℃.
The invention further aims to provide a device applied to the process for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor, which comprises a stirring kettle in S1, wherein the stirring kettle comprises a kettle body and a feeding pipe arranged at the top end of the kettle body, a discharging pipe is arranged at the bottom end of the kettle body, a stop valve is arranged on the discharging pipe, a rotating shaft is rotatably connected to the top end of the kettle body, a stirring assembly is arranged in the kettle body, a motor for driving the rotating shaft to rotate is arranged on the kettle body, and when the rotating shaft rotates, the rotating shaft is used for driving the stirring assembly to perform multidirectional disturbance on liquid in the kettle body.
The liquid is poured into the kettle body through the feeding pipe, then the motor is turned on, the rotating shaft of the motor drives the rotating shaft to rotate, the rotating shaft drives the stirring assembly to stir the liquid in the kettle body in multiple directions, and at the moment, the stirring and mixing of the liquid can be facilitated, and the stirring kettle is simple and convenient to use.
Preferably, the stirring assembly comprises four sliding drums horizontally arranged at the top end in the kettle body, the four sliding drums are uniformly distributed along the circumference of the rotating shaft, the four sliding drums are connected with sliding columns in a sliding manner, one sides of the four sliding columns, deviating from the rotating shaft, are horizontally provided with horizontal columns with one ends extending to the outside of the sliding drums, one ends of the horizontal columns, far away from the sliding columns, are vertically and downwards provided with disturbance plates for disturbing liquid, and when the rotating shaft rotates, the bottom end of the rotating shaft drives the four sliding columns to horizontally slide in the sliding drums through transmission parts respectively.
Preferably, the driving medium includes the level setting in the oval shaped plate of pivot bottom, four the slide column is close to one side of pivot all is equipped with the fixed plate of U-shaped, and all rotates on four fixed plates to be connected with the gyro wheel with oval shaped plate lateral wall contact, four the bottom of fixed plate all is equipped with first cylinder, and all rotates on four first cylinders to be connected with the pendulum rod, four the one end that first cylinder was kept away from to the pendulum rod extends to adjacent fixed plate on all is equipped with the spout, four equal sliding connection has the second post in the spout, and four second posts fixed connection respectively on four fixed plates, and four pendulum rods form parallelogram this moment, and the spout sets up along the length direction of pendulum rod, the vertical (mixing) shaft that is equipped with in bottom of oval shaped plate, be equipped with a plurality of puddles on the (mixing) shaft, and each puddle all evenly distributes along the circumference of (mixing) shaft.
Preferably, the stirring assembly comprises a vertical column and a sleeve sleeved on the vertical column, the vertical column is vertically arranged, a supporting plate is arranged on one side of the outer wall of the sleeve, the supporting plate is fixedly connected with the inner wall of the kettle body, a plurality of disturbance sheets used for disturbing liquid are arranged on the vertical column, each disturbance sheet is located below the supporting plate and distributed along the length direction of the vertical column at intervals, a fixed column is obliquely arranged at the bottom end of the rotating shaft, a fixed cylinder is connected to the fixed column in a coaxial rotation mode, a driving column is arranged on the outer wall of the fixed cylinder, a driving cylinder is coaxially sleeved on the driving column, and the top end of the vertical column is hinged to the outer wall of the driving cylinder.
Preferably, the fixed column is kept away from the coaxial stirring post that is equipped with of one end of pivot, and is equipped with a plurality of stirring piece on the stirring post, and each stirring piece all follows the incline direction interval distribution of stirring post.
Preferably, the stirring assembly comprises a supporting shaft which is rotationally connected to the bottom end in the kettle body, a first square frame is arranged between the supporting shaft and the rotating shaft, rotating grooves are formed in the centers of two opposite sides of the first square frame, rotating columns are rotationally connected in the two rotating grooves, a second square frame is arranged between the rotating columns, the second square frame is located in the first square frame, a plurality of stirring plates are arranged between two opposite sides of the second square frame, and when the rotating shaft drives the first square frame to rotate, driving pieces for simultaneously driving the second square frame to rotate in the first square frame are arranged on the first square frame.
Preferably, the driving piece comprises a first conical gear coaxially connected to the rotating shaft in a rotating way, the top end of the first conical gear is fixedly connected with the kettle body, a first support and a second support are arranged on the outer wall of the first square frame, the first support is located at the top end of the first square frame, the second support is located at one side of the first square frame, the first support is rotationally connected with a first transmission shaft, the second support is rotationally connected with a second transmission shaft, the second transmission shaft is perpendicular to the first transmission shaft, one end of the first transmission shaft, close to the rotating shaft, is provided with a second conical gear meshed with the first conical gear, one end of the first transmission shaft, close to the second transmission shaft, is provided with a third conical gear, the top end of the second transmission shaft is provided with a fourth conical gear meshed with the third conical gear, one of the rotating posts is provided with a sixth conical gear located outside the first square frame, and the bottom end of the second transmission shaft is provided with a fifth conical gear meshed with the sixth conical gear.
Preferably, the bottom of the first square frame is vertically provided with two opposite inverted U-shaped connecting plates, the bottoms of the two connecting plates are respectively provided with a scraping plate contacted with the bottom in the kettle body, and the two connecting plates are respectively positioned at two sides of the supporting shaft.
The invention has the beneficial effects that:
the method adopts the modes of stirring, adjusting pH, heating, crystallizing and drying, and the recovery process is simple, the recovery rate of MBT can reach more than 98 percent after purification and drying for many times, the purity of MBT reaches 97.2 percent, and the method can be applied to recovering MBT from cefotaxime acid mother liquor in industrial production.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural view of the present embodiment;
FIG. 2 is a schematic diagram of the structure of the disturbance plate according to the present embodiment;
fig. 3 is a schematic structural view of an elliptical plate according to the present embodiment;
FIG. 4 is an enlarged schematic view of the portion A in FIG. 3;
fig. 5 is a schematic structural diagram of the driving post according to the present embodiment;
fig. 6 is a schematic structural view of the connecting plate according to the present embodiment.
Reference numerals illustrate:
in the figure: 1. a kettle body; 2. a feed pipe; 3. a discharge pipe; 4. a stop valve; 5. a rotating shaft; 6. a motor; 7. a slide cylinder; 8. a spool; 9. a horizontal column; 10. a disturbance plate; 12. an elliptical plate; 13. a fixing plate; 14. a roller; 15. a first column; 16. swing rod; 17. a chute; 18. a second column; 19. a stirring shaft; 20. a stirring rod; 21. a vertical column; 22. a sleeve; 23. a support plate; 24. a disturbance piece; 25. fixing the column; 26. a fixed cylinder; 27. driving the column; 28. a driving cylinder; 29. stirring the column; 30. stirring sheets; 31. a support shaft; 32. a first rectangular frame; 33. a rotary groove; 34. a rotating column; 35. a second rectangular frame; 36. a stirring plate; 37. a first bevel gear; 38. a first bracket; 39. a second bracket; 40. a first drive shaft; 41. a second drive shaft; 42. a second bevel gear; 43. a third bevel gear; 44. a fourth bevel gear; 45. a sixth bevel gear; 46. a fifth bevel gear; 47. a connecting plate; 48. a scraper.
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. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A process for recovering MBT from cefotaxime acid mother liquor, comprising the following steps:
s1, adding 10% sodium hydroxide solution into 100L cefotaxime acid mother solution in a stirring kettle, adjusting the pH to 4, and stirring for 10min at 25 ℃;
s2, transferring the mixed solution obtained in the step S1 into a rectifying tower, heating to the temperature of a tower kettle of 95 ℃, the temperature of a tower top of 85 ℃, evaporating light components from the tower top, and leaving the liquid in the rectifying tower;
s3, transferring the residual liquid after the rectification of the S2 into a crystallization tank, adding water, stirring and cooling to 20 ℃ to obtain MBT crystals;
s4, after suction filtration, the MBT crystal is transferred into a low-temperature dryer to be dried at 50 ℃ to obtain the MBT with the purity of 97.2%.
Example 2
A process for recovering MBT from cefotaxime acid mother liquor, comprising the following steps:
s1, adding 10% sodium hydroxide solution into 100L cefotaxime acid mother solution in a stirring kettle, adjusting the pH to 5, and stirring for 10min at 35 ℃;
s2, transferring the mixed solution obtained in the step S1 into a rectifying tower, heating to the temperature of a tower kettle of 95 ℃, the temperature of a tower top of 85 ℃, evaporating light components from the tower top, and leaving the liquid in the rectifying tower;
s3, transferring the residual liquid after the rectification of the S2 into a crystallization tank, adding water, stirring and cooling to 20 ℃ to obtain MBT crystals;
s4, after suction filtration, the MBT crystal is transferred into a low-temperature dryer to be dried at 60 ℃ to obtain the MBT with the purity of 96.0%.
Example 3
A process for recovering MBT from cefotaxime acid mother liquor, comprising the following steps:
s1, adding 10% sodium hydroxide solution into 100L cefotaxime acid mother solution in a stirring kettle, adjusting the pH to 5, and stirring at 10 ℃ for 10min;
s2, transferring the mixed solution obtained in the step S1 into a rectifying tower, heating to the temperature of a tower kettle of 95 ℃, the temperature of a tower top of 85 ℃, evaporating light components from the tower top, and leaving the liquid in the rectifying tower;
s3, transferring the residual liquid after the rectification of the S2 into a crystallization tank, adding water, stirring and cooling to 20 ℃ to obtain MBT crystals;
s4, after suction filtration, the MBT crystal is transferred into a low-temperature dryer to be dried at 40 ℃ to obtain the MBT with the purity of 95.5%.
Example 4
The device applied in the above embodiment 1-embodiment 4, as shown in fig. 1 and 2, comprises a stirring kettle in S1, the stirring kettle comprises a kettle body 1 and a feed pipe 2 arranged at the top end of the kettle body 1, a discharge pipe 3 is arranged at the bottom end of the kettle body 1, a stop valve 4 is arranged on the discharge pipe 3, a rotating shaft 5 is rotatably connected to the top end in the kettle body 1, a stirring assembly is arranged in the kettle body 1, a motor 6 for driving the rotating shaft 5 to rotate is arranged on the kettle body 1, and when the rotating shaft 5 rotates, the rotating shaft 5 is used for driving the stirring assembly to perform multidirectional disturbance on liquid in the kettle body 1.
As shown in fig. 1 and 2, liquid is poured into the kettle body 1 through the feed pipe 2, then the motor 6 is turned on, at this moment, the rotating shaft of the motor 6 drives the rotating shaft 5 to rotate, and the rotating shaft 5 drives the stirring assembly to perform multidirectional disturbance on the liquid in the kettle body 1, so that the stirring and mixing of the liquid can be facilitated, and the use is simple and convenient.
As fig. 2 and 3, stirring subassembly includes four slide drums 7 of level setting on the internal top of cauldron body 1, and four slide drums 7 all evenly distributed along the circumference of pivot 5, all horizontal slip is connected with slide column 8 in four slide drums 7, and four slide column 8 deviate from the horizontal post 9 outside slide drum 7 of one side equal level of pivot 5 and be equipped with one end extension, four horizontal post 9 keep away from the horizontal post 8 one end all vertically downwards be equipped with the disturbance board 10 that is used for disturbing liquid, when pivot 5 rotates, the bottom of pivot 5 drives four slide columns 8 respectively in slide drum 7 horizontal slip through the driving medium.
As shown in fig. 2 and 3, when the rotating shaft 5 rotates, the rotating shaft 5 can respectively drive the four sliding columns 8 to slide back and forth in the sliding cylinder 7 horizontally through the transmission member, at this time, the disturbance plates 10 move along with the sliding columns 8 through the horizontal columns 9, the four sliding columns 8 are opposite to each other, when the two opposite sliding columns 8 are close to each other through the transmission member, the rest two opposite sliding columns 8 are far away from each other through the transmission member, at this time, the liquid in the kettle body 1 can be disturbed in multiple directions through the four disturbance plates 10, and the use is simple and convenient.
As shown in fig. 2, fig. 3 and fig. 4, the driving medium includes oval shaped plate 12 that the level set up in pivot 5 bottom, four slide posts 8 are close to pivot 5 one side all and are equipped with U-shaped fixed plate 13, and all rotate on four fixed plates 13 and be connected with the gyro wheel 14 with oval shaped plate 12 lateral wall contact, the bottom of four fixed plates 13 all is equipped with first cylinder 15, and all rotate on four first cylinders 15 and be connected with pendulum rod 16, the one end that four pendulum rods 16 kept away from first cylinder 15 extends to adjacent fixed plate 13 on all is equipped with spout 17, all sliding connection has second post 18 in four spout 17, and four second posts 18 are fixed connection respectively on four fixed plates 13, four pendulum rods 16 form the parallelogram this moment, spout 17 sets up along the length direction of pendulum rod 16, the vertical (mixing) shaft 19 that is equipped with in bottom of oval shaped plate 12, be equipped with a plurality of puddler 20 on the (mixing) shaft 19), and each puddler 20 all evenly distributes along the circumference of puddler 19.
As shown in fig. 2, fig. 3 and fig. 4, when the rotating shaft 5 rotates, the rotating shaft 5 drives the elliptical plate 12 to rotate along the rotation axis of the rotating shaft 5, at this time, because the rollers 14 on the four fixing plates 13 are all in contact with the side walls of the elliptical plate 12, the four swinging plates are respectively connected to the first columns 15 of the four fixing plates 13 in a rotating way, the four second columns 18 are respectively connected to the four fixing plates 13 in a fixed way, and the four swinging rods 16 form a parallelogram, so when the rotating shaft 5 drives the elliptical plate 12 to rotate along the rotation axis of the rotating shaft 5, the four fixing plates 13 can be pushed by the cooperation of the elliptical plate 12, the four rollers 14, the four first columns 15, the four swinging rods 16, the four second columns 18 and the sliding grooves 17 to respectively drive the four sliding columns 8 to horizontally slide back and forth in the sliding drum 7, the four rollers 14 are always in contact with the side walls of the elliptical plate 12, and when the elliptical plate 12 rotates, the stirring shaft 19 can follow the elliptical plate 12 to rotate, and at this time, the liquid in the kettle 1 can be further stirred by the stirring rods 20 on the stirring shaft 19.
As shown in fig. 5, alternatively, the stirring assembly includes vertical post 21 and sleeve 22 of cover on vertical post 21, vertical post 21 sets up vertically, outer wall one side of sleeve 22 is equipped with backup pad 23, and backup pad 23 and the inner wall fixed connection of cauldron body 1 are equipped with a plurality of disturbance pieces 24 that are used for disturbing liquid on the vertical post 21, and each disturbance piece 24 all is located the below of backup pad 23, and along the length direction interval distribution of vertical post 21, the bottom slope of pivot 5 is equipped with fixed column 25, and coaxial rotation is connected with fixed cylinder 26 on the fixed column 25, be equipped with on the fixed cylinder 26 outer wall and drive the post 27, and coaxial cover is equipped with on the drive post 27 and drive a section of thick bamboo 28, the top of vertical post 21 is articulated with the outer wall that drives a section of thick bamboo 28.
As shown in fig. 5, when the rotating shaft 5 rotates, the rotating shaft 5 drives the fixed column 25 to rotate along the rotation axis of the rotating shaft 5, at this time, due to the inclined arrangement of the fixed column 25, the fixed column 26 is rotationally connected with the fixed column 25, the driving cylinder 28 is sleeved on the driving column 27, the vertical column 21 is hinged with the driving cylinder 28, the sleeve 22 is sleeved on the vertical column 21, and the supporting plate 23 on the sleeve 22 is fixedly connected with the inner wall of the kettle body 1, so that when the rotating shaft 5 drives the fixed column 25 to rotate along the rotation axis of the rotating shaft 5, the vertical column 21 can be pulled to vertically reciprocate through the cooperation of the fixed column 26 and the fixed column 25, the cooperation of the driving cylinder 28 and the driving column 27, and the cooperation of the sleeve 22 and the vertical column 21, and at this time, the vertical disturbance of the liquid in the kettle body 1 can be vertically disturbed by the disturbance piece 24 on the vertical column 21, and the use is simple and convenient.
As shown in fig. 5, the fixed column 25 is far away from the one end of the rotating shaft 5 and is coaxially provided with a stirring column 29, a plurality of stirring sheets 30 are arranged on the stirring column 29, and each stirring sheet 30 is distributed along the inclined direction of the stirring column 29 at intervals, the purpose of the arrangement is that when the rotating shaft 5 drives the fixed column 25 to rotate along the rotating axis of the rotating shaft 5, the stirring column 29 can rotate along the rotating axis of the rotating shaft 5 along with the fixed column 25, at the moment, liquid in the kettle body 1 can be further stirred through each stirring sheet 30 on the stirring column 29, each stirring sheet 30 on the stirring column 29 and each stirring sheet 24 on the vertical column 21 are not mutually influenced, and the use is simple and convenient.
As shown in fig. 6, alternatively, the stirring assembly comprises a supporting shaft 31 rotatably connected to the bottom end in the kettle body 1, a first square frame 32 is arranged between the supporting shaft 31 and the rotating shaft 5, rotating grooves 33 are formed in the centers of two opposite sides of the first square frame 32, rotating columns 34 are rotatably connected in the two rotating grooves 33, a second square frame 35 is arranged between the two rotating columns 34, the second square frame 35 is positioned in the first square frame 32, a plurality of stirring plates 36 are arranged between two opposite sides of the second square frame 35, and when the rotating shaft 5 drives the first square frame 32 to rotate, driving pieces for simultaneously driving the second square frame 35 to rotate in the first square frame 32 are arranged on the first square frame 32.
Referring to fig. 6, when the rotating shaft 5 rotates, the rotating shaft 5 drives the first square frame 32 to rotate along the rotation axis of the rotating shaft 5, at this time, the second square frame 35 rotates along the rotation axis of the rotating shaft 5 through the rotating groove 33 and the rotating post 34, and when the first square frame 32 and the second square frame 35 rotate along the rotation axis of the rotating shaft 5, the second square frame 35 is driven by the driving member on the first square frame 32 to rotate along the axis of the rotating post 34 through the cooperation of the rotating post 34 and the rotating groove 33 in the first square frame 32, at this time, the first square frame 32 rotates along the rotation axis of the rotating shaft 5 and simultaneously rotates along the axis of the rotating post 34, and the stirring plates 36 on the second square frame 35 can stir the liquid in the kettle body 1 in multiple directions, which is simple and convenient to use.
Referring to fig. 6, the driving member includes a first bevel gear 37 coaxially and rotatably connected to the rotating shaft 5, the top end of the first bevel gear 37 is fixedly connected to the kettle body 1, a first bracket 38 and a second bracket 39 are disposed on the outer wall of the first square frame 32, the first bracket 38 is located at the top end of the first square frame 32, the second bracket 39 is located at one side of the first square frame 32, a first transmission shaft 40 is rotatably connected to the first bracket 38, a second transmission shaft 41 is rotatably connected to the second bracket 39, the second transmission shaft 41 is perpendicular to the first transmission shaft 40, a second bevel gear 42 meshed with the first bevel gear 37 is disposed at one end of the first transmission shaft 40 close to the rotating shaft 5, a third bevel gear 43 is disposed at one end of the first transmission shaft 40 close to the second transmission shaft 41, a fourth bevel gear 44 meshed with the third bevel gear 43 is disposed at the top end of the second transmission shaft 41, a sixth bevel gear 45 located outside the first square frame 32 is disposed on one of the rotating columns 34, and a fifth bevel gear 46 meshed with the sixth bevel gear 45 is disposed at the bottom end of the second transmission shaft 41.
As shown in fig. 6, when the rotating shaft 5 rotates, the second square frame 35 rotates along the rotation axis of the rotating shaft 5 along with the first square frame 32, because the first bevel gear 37 is rotationally connected with the rotating shaft 5, and the first bevel gear 37 is fixedly connected with the kettle body 1, the first bevel gear 37 cannot rotate along with the rotating shaft 5, and at this time, because the first bracket 38 and the second bracket 39 are both disposed on the first square frame 32, when the second square frame 35 rotates along the rotation axis of the rotating shaft 5 along with the first square frame 32, the second square frame 35 rotates along the rotation axis of the rotating shaft 5, through the cooperation of the first bevel gear 37, the second bevel gear 42, the first transmission shaft 40, the third bevel gear 43, the fourth bevel gear 44, the second transmission shaft 41, the fifth bevel gear 46 and the sixth bevel gear 45, one of the rotating columns 34 can rotate in the rotating groove 33, and at this time, one of the rotating columns 34 can drive the second square frame 35 to rotate along the rotation axis of the rotating columns 34, so that the second square frame 35 rotates along with the rotation axis of the rotating shaft 5 along with the first square frame 32, and the second square frame 35 rotates along with the rotation axis of the rotating shaft 5, and the rotating columns 34 can rotate easily.
As shown in fig. 6, the bottom end of the first square frame 32 is vertically provided with two opposite inverted U-shaped connecting plates 47, the bottom ends of the two connecting plates 47 are respectively provided with a scraping plate 48 contacting with the bottom end in the kettle body 1, the two connecting plates 47 are respectively located at two sides of the supporting shaft 31, the purpose of the arrangement is that when the first square frame 32 rotates along the rotation axis of the rotation shaft 5, the two connecting plates 47 and the scraping plates 48 can rotate along with the first square frame 32, and at this time, the liquid in the kettle body 1 can be further stirred by the connecting plates 47 and the scraping plates 48 contacting with the bottom end of the kettle body 1, so that the use is simple and convenient.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (10)
1. A process for recovering 2-mercaptobenzothiazole from a mother liquor of cefotaxime acid, comprising the steps of:
s1, adding a sodium hydroxide solution into a cefotaxime acid mother solution in a stirring kettle, and adjusting the pH;
s2, transferring the mixed solution obtained in the step S1 into a rectifying tower, heating and raising the temperature, evaporating light components from the top of the tower, and leaving the liquid in the rectifying tower;
s3, transferring the residual liquid after the rectification of S2 into a crystallization tank, adding water, stirring and cooling to obtain MBT crystals;
s4, performing suction filtration on the MBT crystal, and drying to obtain the MBT.
2. The process for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to claim 1, wherein the concentration of sodium hydroxide is 10%, the pH is 4-5, and the stirring temperature is 10-35 ℃;
the rectifying tower is heated to the temperature of 95 ℃ at the tower bottom and 85 ℃ at the tower top;
the drying temperature in the S4 is 40-60 ℃.
3. The device applied to the process for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to any one of the claims 1-2 is characterized by comprising a stirring kettle in S1, wherein the stirring kettle comprises a kettle body (1) and a feeding pipe (2) arranged at the top end of the kettle body (1), a discharging pipe (3) is arranged at the bottom end of the kettle body (1), a stop valve (4) is arranged on the discharging pipe (3), a rotating shaft (5) is rotatably connected to the top end in the kettle body (1), a stirring assembly is arranged in the kettle body (1), a motor (6) for driving the rotating shaft (5) to rotate is arranged on the kettle body (1), and when the rotating shaft (5) rotates, the rotating shaft (5) is used for driving the stirring assembly to perform multidirectional disturbance on liquid in the kettle body (1).
4. A device in a process for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to claim 3, wherein the stirring assembly comprises four sliding drums (7) horizontally arranged at the inner top end of the kettle body (1), the four sliding drums (7) are uniformly distributed along the circumferential direction of the rotating shaft (5), sliding columns (8) are horizontally connected in the four sliding drums (7), one sides of the four sliding columns (8) deviating from the rotating shaft (5) are horizontally provided with horizontal columns (9) with one ends extending to the outside of the sliding drums (7), one ends of the four horizontal columns (9) far away from the sliding columns (8) are vertically and downwards provided with disturbance plates (10) for disturbing liquid, and when the rotating shaft (5) rotates, the bottom ends of the rotating shaft (5) respectively drive the four sliding columns (8) to horizontally slide in the sliding drums (7) through transmission parts.
5. The device in the process of recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to claim 4, wherein the transmission piece comprises elliptical plates (12) horizontally arranged at the bottom ends of the rotating shafts (5), four sliding columns (8) are provided with U-shaped fixed plates (13) on one sides close to the rotating shafts (5), rollers (14) in contact with the side walls of the elliptical plates (12) are rotationally connected to the four fixed plates (13), first columns (15) are respectively arranged at the bottom ends of the four fixed plates (13), swing rods (16) are respectively rotationally connected to the four first columns (15), one ends of the four swing rods (16) far away from the first columns (15) extend to the adjacent fixed plates (13) and are respectively provided with a sliding groove (17), second columns (18) are respectively and fixedly connected to the four fixed plates (13), at the moment, the four swing rods (16) form parallel sliding grooves (17) are respectively arranged along the length directions of the four first columns (15), the stirring shafts (19) are respectively provided with stirring shafts (20) and are respectively provided with stirring shafts (19) which are respectively distributed along the circumference directions of the stirring shafts (20).
6. A device in a process of recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to claim 3, wherein the stirring assembly comprises a vertical column (21) and a sleeve (22) sleeved on the vertical column (21), the vertical column (21) is vertically arranged, a supporting plate (23) is arranged on one side of the outer wall of the sleeve (22), the supporting plate (23) is fixedly connected with the inner wall of the kettle body (1), a plurality of disturbance sheets (24) for disturbing liquid are arranged on the vertical column (21), each disturbance sheet (24) is arranged below the supporting plate (23) and distributed at intervals along the length direction of the vertical column (21), a fixed column (25) is obliquely arranged at the bottom end of the rotating shaft (5), a fixed cylinder (26) is coaxially connected onto the fixed column (25), a driving column (27) is arranged on the outer wall of the fixed cylinder (26), a driving cylinder (28) is coaxially sleeved on the driving column (27), and the top end of the vertical column (21) is hinged with the outer wall of the driving cylinder (28).
7. The device in the process for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to claim 6, wherein one end of the fixed column (25) far away from the rotating shaft (5) is coaxially provided with a stirring column (29), the stirring column (29) is provided with a plurality of stirring sheets (30), and each stirring sheet (30) is distributed at intervals along the inclination direction of the stirring column (29).
8. A device in a process for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to claim 3, wherein the stirring assembly comprises a supporting shaft (31) rotatably connected to the inner bottom end of the kettle body (1), a first square frame (32) is arranged between the supporting shaft (31) and the rotating shaft (5), rotating grooves (33) are formed in the centers of two opposite sides of the first square frame (32), rotating columns (34) are rotatably connected in the two rotating grooves (33), a second square frame (35) is arranged between the two rotating columns (34), the second square frame (35) is positioned in the first square frame (32), a plurality of stirring plates (36) are arranged between the two opposite sides of the second square frame (35), and a driving piece for simultaneously driving the second square frame (35) to rotate in the first square frame (32) is arranged on the first square frame (32) when the rotating shaft (5) drives the first square frame (32) to rotate.
9. The device for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to claim 8, wherein the driving member comprises a first conical gear (37) coaxially connected to the rotating shaft (5), the top end of the first conical gear (37) is fixedly connected with the kettle body (1), a first bracket (38) and a second bracket (39) are arranged on the outer wall of the first square frame (32), the first bracket (38) is positioned at the top end of the first square frame (32), the second bracket (39) is positioned at one side of the first square frame (32), a first transmission shaft (40) is rotatably connected to the first bracket (38), a second transmission shaft (41) is rotatably connected to the second bracket (39), the second transmission shaft (41) is perpendicular to the first transmission shaft (40), one end of the first transmission shaft (40) close to the rotating shaft (5) is provided with a second conical gear (42) meshed with the first conical gear (37), the second transmission shaft (40) is positioned at one end of the second transmission shaft (40) close to the third conical gear (41), the top end (43) of the second transmission shaft (41) is meshed with the first conical gear (34), the bottom end of the second transmission shaft (41) is provided with a fifth conical gear (46) meshed with the sixth conical gear (45).
10. The device in the process for recovering 2-mercaptobenzothiazole from cefotaxime acid mother liquor according to claim 8, wherein the bottom end of the first square frame (32) is vertically provided with two opposite inverted U-shaped connecting plates (47), the bottom ends of the two connecting plates (47) are respectively provided with a scraping plate (48) contacted with the inner bottom end of the kettle body (1), and the two connecting plates (47) are respectively positioned at two sides of the supporting shaft (31).
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