The desalination and concentration system that is used for medicine intermediate
Technical field
The utility model relates to a kind ofly both can simplify original operating procedure, can obtain the product of higher degree again, reduced the desalination and concentration system that is used for medicine intermediate of the production cost of pharmaceuticals industry simultaneously, belonged to the desalination and the concentration technique field of medicine intermediate.
Background technology
Present many medicine intermediates must repeatedly be regulated PH in process of production and just can react fully and carry out, to obtain the highest yield.In the process that adds the soda acid adjusting repeatedly, a considerable amount of salt certainly will have been brought, and directly influence the quality of product quality, therefore must carry out desalination to product, just come desalination to become many medicines manufacturer to be concerned about and the focus of research as a kind of efficient easily method of row how.Along with constant development of economy, to the medicine and the proposition of heavy chemicals higher quality requirement.So the desalination to medicine intermediate seems very important more.
Carry out desalination with usual employing solvent method and ultrafiltration diafiltration and ion-exchange.The solvent method solvent in use loses bigger, and solvent recovery is difficult, and the technology operation is many, to shortcomings such as operator's occupational hazards are big; The low-molecular-weight material of ultrafiltration centering is difficult to realize filtration operation that the material less relatively for number molecular weight is difficult to realize desalination and concentration especially; Shortcomings such as there is complex operation equally in ion-exchange, and replacing resin and operating cost are higher.
Summary of the invention
Purpose of design: avoid the weak point in the background technology, design and a kind ofly both can simplify original operating procedure, can obtain the product of higher degree again, reduce the desalination and concentration system that is used for medicine intermediate of the production cost of pharmaceuticals industry simultaneously.
Design: in order to realize the foregoing invention purpose.Membrane separation technique is an emerging Development Technology, also is one of field current with the fastest developing speed.Nanofiltration (Nanofiltration) is a kind of new membrane separation process of middle and later periods eighties exploitation.The aperture of NF membrane is between counter-infiltration and ultrafiltration, and it has higher cutoff performance to the organic matter of molecular weight between 200~1000, to monovalention and micromolecular remove then relatively low.The utility model utilizes this feature just, is used for the desalination and the purification of medicine intermediate are concentrated.Because the desalination of nanofiltration constant volume is a kind of novel method for purifying and separating, do not have phase transformation in the process, need not heating, do not destroy advantages such as material molecular structure, operating pressure be relatively low, nuisanceless, effectively overcome the technical bottleneck and the environmental problem that exist in the existing technology.The application adopts the method, not only perfect film separation process, and can replace traditional desalination technology.
1, before one-level nanofiltration constant volume is handled, earlier material liquid is carried out the design of micro-filtration and ultrafiltration, this is one of technical characterictic of the present utility model.The purpose of doing like this is: remove materials such as fine suspension, colloid, prevent that effectively film from polluting, reach the effect in service life of prolongation film.
2, adopt nanofiltration constant volume technology to carry out desalination and concentrated design, this is two of a technical characterictic of the present utility model.The purpose of doing like this is: system adopts the mode of operation of nanofiltration, can carry out 2~5 times concentrating to the solution after the desalination, reaches desalination and concentrated double effects, has improved the content of active principle, produces load for subsequent treatment workshop section has reduced.
3, be provided with design through the liquid recycle device after nanofiltration, this is three of a technical characterictic of the present utility model.The purpose of doing like this is: see through the contained material of liquid if possess certain economic value, can reclaim, increase the business economic benefit.
Technical scheme: be used for the desalination of medicine intermediate and the system that concentrates, the material liquid service is connected with the water tank import, the water tank outlet is connected with the import of one-level nanofiltration membrane component with high-pressure pump by booster pump, the one-level nanofiltration membrane component is provided with concentrated solution outlet and sees through the liquid outlet, wherein seeing through the liquid outlet is connected with the water tank import by pipeline, water tank outlet passing through booster pump, high-pressure pump is connected with the import of secondary nanofiltration membrane component, concentrated solution outlet is provided with two outlets, one of them outlet is connected with the water tank import by valve and pipeline, another outlet is connected with the concentrate retracting device by valve and pipeline, the secondary nanofiltration membrane component is provided with concentrated solution outlet and the outlet of light liquid, concentrated solution outlet is provided with two outlets, and one of them outlet is connected with the concentrate retracting device by valve and pipeline, another outlet is connected with water tank by valve and pipeline, light liquid outlet is connected with light liquid retracting device by pipeline.
The utility model is compared with background technology, the one, system adopts the mode of operation of nanofiltration, can carry out 2~5 times concentrating to the solution after the desalination, the double effects that reaches desalination and concentrate, improved the content of active principle, produced load, seen through the contained material of liquid if possess certain economic value for subsequent treatment workshop section has reduced, can reclaim, increase the business economic benefit; The 2nd, do not have in the membrane separation plant running and do not add other chemical agent in phase transformation, automatic controlling level height and the process and carry out and clean production, reduced pollution to environment; Occupation area of equipment is few, flow process is simple, investment is less, operating cost is low; The 3rd, after handling by the utility model, the yield of active principle can access raising to a certain degree, sees through active ingredient in the liquid and can reach recovery more than 98%.
Description of drawings
Fig. 1 is used for the desalination of medicine intermediate and the system schematic that concentrates.
Fig. 2 is the desalination of medicine intermediate and the block flowsheet schematic diagram of method for concentration.
The specific embodiment
Embodiment 1: with reference to accompanying drawing 1.Be used for the desalination of medicine intermediate and the system that concentrates, the material liquid service is connected with water tank 1 import, water tank 1 outlet is connected with 2 imports of one-level nanofiltration membrane component with high-pressure pump 8 by booster pump 7, one-level nanofiltration membrane component 2 is provided with concentrated solution outlet and sees through the liquid outlet, wherein seeing through the liquid outlet is connected with water tank 9 imports by pipeline, water tank 9 outlets are by booster pump 10, high-pressure pump 11 is connected with 3 imports of secondary nanofiltration membrane component, concentrated solution outlet is provided with two outlets, one of them outlet is connected with water tank 1 import by valve and pipeline, another outlet is connected with concentrate retracting device 12 by valve and pipeline, secondary nanofiltration membrane component 3 is provided with concentrated solution outlet and the outlet of light liquid, concentrated solution outlet is provided with two outlets, and one of them outlet is connected with concentrate retracting device 13 by valve and pipeline, another outlet is connected with water tank 1 by valve and pipeline, light liquid outlet is connected with light liquid retracting device 14 by pipeline.Described water tank 1 outside is provided with cooling water inlet 4 and coolant outlet 5.Pipeline between described connection water tank 1 outlet and booster pump 7 imports is provided with percolate import 6.
The desalination of medicine intermediate and method for concentration: with reference to attached Fig. 1 and 2.Using nanofiltration constant volume desalting technology carries out desalination and concentrates concrete steps medicine intermediate: the medicine intermediate raw material that 1) will contain 1%~25% salt is removed macromolecular particle and organic matter and colloidal substance in the solution by micro-filtration membrane and milipore filter successively; 2) will remove material liquid behind macromolecular particle and organic matter and the colloidal substance enters water tank and is cooled to 10 ℃~25 ℃ by water quench; 3) with cooled material liquid successively by booster pump and high-pressure pump supercharging and adopt nanofiltration constant volume desalting technology to carry out the desalinization of soil by flooding or leaching of medicine intermediate and concentrate, and the speed that adds percolate in desalination processes sees through membrane flux with membrane module and equates, the control temperature is 2~45 ℃ in its process, operating pressure 2.0~3.8Mpa; 4) concentrate after the desalination directly enters subsequent processing; 5) adopt nanofiltration constant volume desalting technology to carry out in the desalinization of soil by flooding or leaching and concentration process of medicine intermediate, can carry out selectively concentrating reclaiming seeing through the material that economic worth is arranged in the liquid.The medicine intermediate raw material of described 1%~25% salt is successively by before micro-filtration and the ultrafiltration, regulates 1%~25% salt temperature and PH, the temperature of solution and PH reached enter the film system requirements.Described percolate is deionized water or other solvents.Described micro-filtration membrane module aperture is 1~5 micron, and its material is cellulose, Kynoar, polyamide or other macromolecule organic materials; Described hyperfiltration membrane assembly aperture is 0.02~0.1 micron, and material is cellulose acetate, polyether sulfone, Kynoar or other high-molecular organic materials.NF membrane used in the described NF membrane constant volume desalination operating process is 150Da through molecular cut off, film surface bear, nanofiltration membrane component can be rolling, tubular type and flat, and the NF membrane material is the macromolecule organic material of polyamide, polysulfones, polyether sulfone, polyvinyl alcohol, cellulose acetate; Described nanofiltration constant volume desalination mode of operation comprises constant volume diafiltration mode, concentrated mode, constant volume diafiltration-concentrated mode, pre-concentration-constant volume desalination-concentrated mode.The concentrate salt content is less than 0.5% after the described desalination.Described salt mainly comprises sodium chloride salt, potassium chloride salt, chlorination ammonium salt, other hydrochlorides.
Case 1: medicine intermediate Cefradine constant volume desalination and concentration method
Being 2.0% Cefradine mother liquor (TMG hydrochloride content is 6.1%, and the ammonium chloride salt content is 3.5%) with content handles through the micro-filtration of 5 microns and 1 micron, removes bulky grain suspensions such as the fragment that exists in the mother liquor, iron rust; Mother liquor is further handled under 0.15Mpa pressure through ultrafiltration again, removed materials such as fine suspension, colloid, prevent that effectively film from polluting, reach the effect in service life of prolongation film.
The native system desalination processes adopts pre-concentration-constant volume diafiltration-concentrated mode of operation, used NF membrane aperture is a nanoscale, seeing through molecular cut off is 150Da, film surface bear, has different Donan current potentials to multi-form with the ion of valence state, these properties have determined it to carry out effectively catching to Cefradine, and most TMG hydrochloride and chlorination ammonium salt then can see through film and enter light side.Enter the NF membrane piece-rate system through the pretreated liquid that sees through under the effect of booster pump and high-pressure pump, at first enter the one-level NF membrane pre-concentration stage, controlled pressure 3.5~3.8Mpa in the process after mother liquor is concentrated 37%, stops the pre-concentration operation.This moment pre-concentration concentrate Cefradine content 3.3%, TMG hydrochloride content 7.4%; See through liquid Cefradine content 0.1%, TMG hydrochloride content 2.7%.Then enter the constant volume desalination stage, the speed that control adds deionized water equates through membrane flux with the one-level NF membrane, up to when the amount that adds deionized water for stopping to add deionized water when concentrating 3.5 times of liquid measure after the pre-concentration, the discharge capacity that see through liquid this moment equates with the deionized water addition.Enter enriching stage then, after the amount that sees through liquid equals preliminary treatment, see through in the concentration process liquid measure 17% the time, stop concentration operation, close booster pump and high-pressure pump respectively.Obtain concentrate Cefradine concentration this moment is 3.8%, and the ammonium chloride salt content is 0.25%, and TMG hydrochloride content is 0.45%; See through in the liquid and contain 0.1% Cefradine.Because the Cefradine economic worth is higher, so the one-level NF membrane is reclaimed through a spot of Cefradine in the liquid, one-level film NF membrane sees through liquid and enters secondary NF membrane system, controlled pressure operating pressure 2.0~2.8MPa in the removal process, when reaching 20 times, concentration rate stops to concentrate, the concentration that reclaims Cefradine in the concentrate of back this moment is about 1.8%, reclaim the back and see through in the liquid Cefradine content less than 0.01%, concentrate is back to the import of one-level NF membrane carries out desalination and concentration again, the liquid that sees through after the recovery enters biochemistry pool and handles.
Case 2: medicine intermediate thunder rice hydride constant volume desalination and concentration method
The preliminary treatment of thunder rice hydride and operating condition are with embodiment 1.Active principle thunder rice hydride content 12% in the mother liquor, sodium chloride salt content 5%.When one-level NF membrane system brings into operation, control adds deionized water speed and equates through membrane flux with the one-level nanofiltration membrane component, controlled pressure 2.8~3.8Mpa in the process, stop to add water during 6 times of the volume that sees through liquid that after amount of water equals preliminary treatment, obtains, enter enriching stage then, stop to concentrate when liquid measure equals mother liquor amount 1/10 when seeing through, close booster pump and high-pressure pump.The concentrate thunder rice hydride content that obtain this moment is 12.8%, and sodium chloride salt content is less than 0.5%, and concentrate enters vacuum drying workshop section; See through liquid and enter the subsequent treatment stage.
What need understand is: though the foregoing description is to the utility model detailed text description of contrasting; but these text descriptions; just the simple text of the utility model mentality of designing is described; rather than to the restriction of invention mentality of designing; any combination, increase or modification that does not exceed the utility model mentality of designing all falls in the protection domain of the present utility model.