CN203545832U - Macro-porous resin organic solvent chromatographic liquid recycle system - Google Patents
Macro-porous resin organic solvent chromatographic liquid recycle system Download PDFInfo
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- CN203545832U CN203545832U CN201320735974.5U CN201320735974U CN203545832U CN 203545832 U CN203545832 U CN 203545832U CN 201320735974 U CN201320735974 U CN 201320735974U CN 203545832 U CN203545832 U CN 203545832U
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Abstract
The utility model discloses a macro-porous resin organic solvent chromatographic liquid recycle system. The system comprises a solvent-resisting ultrafiltration system, a solvent-resisting nanofiltration system, a reduced pressure distillation boiler, a solvent recycle tank and a solvent bucket; a feed port of the solvent-resisting ultrafiltration system is connected with a macro-porous resin chromatographic column, and the two ends of a discharge port of the solvent-resisting ultrafiltration system are respectively connected with the feed port of the solvent-resisting nanofiltration system and the feed port of the reduced pressure distillation boiler; the two ends of the discharge port of the solvent-resisting nanofiltration system are respectively connected with the feed port of the solvent recycle tank and the feed port of the reduced pressure distillation boiler; the discharge port of the solvent recycle tank is connected with the feed port of the solvent bucket; the discharge port of the solvent bucket is connected with the feed port of the macro-porous resin chromatographic column. The macro-porous resin organic solvent chromatographic liquid recycle system has lower energy consumption and is more environmentally-friendly than a common rectification recycle system.
Description
Technical field
The utility model belongs to bioseparation engineering field, is specifically related to a kind of macroporous resin organic solvent chromatography liquid recovery system.
Background technology
Macroporous resin chromatographic separation is important means of purification of bioseparation engineering field, and its principle is, by product and impurity, the difference of the strong and weak size of resin absorption is reached to separating effect.Separated with respect to silica gel, macroporous resin chromatographic separation has better reusability, and therefore, its use range is also more and more wider.But, in macroporous resin chromatography method, particularly adopt in nonpolar macroporous resin chromatography method, the general solvent that adopts water-soluble good organic solvent to be used as whole chromatographic system, by regulating the ratio of organic solvent and the aqueous solution, complete the process of product sorption and desorption on resin.Because macroporous resin solvent system is the aqueous solution of organic solvent, generally adopt rectifying recovery system to reclaim organic solvent layer and analyse liquid.When solubleness in the aqueous solution of product at organic solvent is lower, the volume of the aqueous solutions of organic solvent that whole chromatography process is used can be quite large; Especially larger to those separating difficulties product, in order to reach separating effect, must adopt a large amount of relatively low aqueous solution of organic solvent content to carry out gradient elution to product, and whole chromatography process gradient kind is many, and the amount of the organic solvent of use is larger.Adopt general rectifying recovery system to reclaim chromatography organic solvent, its process length consuming time, energy consumption is high.
At present; along with country's improving constantly environmental protection requirement; the use cost that rectifying recovery system reclaims chromatographic solution is also more and more higher; thereby macroporous resin chromatography method is also subject to many limitations in actual production use procedure; therefore, the system of the Discarded organic solvent aqueous solution of the recycling macroporous resin chromatography of a kind of more high efficiency, low cost of needs.
Utility model content
In order to address the above problem, the utility model provides a kind of macroporous resin organic solvent chromatography liquid recovery system, and this system is lower than common rectifying recovery system energy consumption, and more environmental protection.
The technical scheme that the utility model provides is macroporous resin organic solvent chromatography liquid recovery system, comprises the ultrafiltration system of resistance to solvent, resistance to solvent nanofiltration system, underpressure distillation pot, solvent recovery tank and solvent storage bucket, wherein:
The opening for feed of the described ultrafiltration system of resistance to solvent is connected with the discharge port of macroporous resin chromatography column, be used for receiving macroporous resin organic solvent chromatography liquid, the two ends of the discharge port of the ultrafiltration system of resistance to solvent are connected with the opening for feed of described resistance to solvent nanofiltration system and the opening for feed of described underpressure distillation pot respectively;
The two ends of described resistance to solvent nanofiltration system discharge port are connected with the opening for feed of described solvent recovery tank and the opening for feed of underpressure distillation pot respectively;
The discharge port of described solvent recovery tank is connected with the opening for feed of solvent storage bucket;
The discharge port of described solvent storage bucket is connected with the opening for feed of macroporous resin chromatography column.
Further, in above-mentioned macroporous resin organic solvent chromatography liquid recovery system:
The ultra-filtration membrane of the described ultrafiltration system of resistance to solvent is preferably polyethersulfone composite membrane;
The film pattern of the ultra-filtration membrane of the described ultrafiltration system of resistance to solvent is preferably board-like film or tubular membrane;
The nanofiltration membrane of described resistance to solvent nanofiltration system is preferably polyamide composite film;
The film pattern of the nanofiltration membrane of described resistance to solvent nanofiltration system is preferably rolled film;
Described solvent storage bucket can have a plurality of.
Above-mentioned macroporous resin organic solvent chromatography liquid recovery system is preferred, between the described ultrafiltration system of resistance to solvent and macroporous resin chromatography column, between the ultrafiltration system of resistance to solvent and resistance to solvent nanofiltration system, between the ultrafiltration system of resistance to solvent and underpressure distillation pot, between resistance to solvent nanofiltration system and solvent recovery tank, between resistance to solvent nanofiltration system and underpressure distillation pot, between solvent recovery tank and solvent storage bucket, between solvent storage bucket and macroporous resin chromatography column, all by pipeline, be connected, one or more by-pass valve controls are all installed on described pipeline.
The macroporous resin organic solvent chromatography liquid recovery system that the utility model provides is when work, and macroporous resin chromatography organic solvent is any mixing solutions of methyl alcohol, ethanol or these two kinds of solvents; The molecular weight of the polyethersulfone complexes membrane that the ultrafiltration system of resistance to solvent is used is 1500-2500, can tolerate 0-99.9(V/V) methyl alcohol or the aqueous ethanolic solution of concentration; The film pattern that the ultrafiltration system of resistance to solvent adopts is board-like film or tubular membrane, and operating pressure is 0.5-0.8MPa.The ultrafiltration system of resistance to solvent filters the macroporous resin chromatographic solution waste liquid of collecting for the first time, remove the macromolecule material in chromatography waste liquid, finally, the concentrated solution that contains the macromolecular substance such as a large amount of pigments, albumen enters underpressure distillation pot to reclaim solvent by concentrated solution recovery channel, and filter membrane filtrate enters by filter membrane filtrate recovery channel the resistance to solvent nanofiltration system being connected with the ultrafiltration system of resistance to solvent.The molecular weight of the polyamide compound film that resistance to solvent nanofiltration system is used is 200-300, can tolerate 0-99.9(V/V) methyl alcohol or the aqueous ethanolic solution of concentration; Its film pattern is rolled film, and operating pressure is 0.8-1MPa; Small-molecule substance in the solvent that the further enrichment of the resistance to solvent nanofiltration system ultrafiltration system of resistance to solvent leaches, be enriched to after finite concentration, concentrated solution enters underpressure distillation pot to reclaim solvent by concentrated solution recovery channel, and filter membrane filtrate enters the solvent recovery tank being connected with resistance to solvent nanofiltration system by filter membrane filtrate recovery channel.Solvent recovery tank is collected the solvent leaching in resistance to solvent nanofiltration system, and in the aqueous solutions of organic solvent that nanofiltration is reclaimed, the meeting of the content (V/V) of organic solvent is than the low 2-3%(V/V of the organic solvent content in aqueous solutions of organic solvent before ultrafiltration (V/V)); Solvent recovery tank is collected after certain volume, and the aqueous solutions of organic solvent of recovery is adjusted the concentration of organic solvent in filtrate by adding a small amount of organic solvent, according to the concentration of organic solvent, organic solvent is imported to corresponding solvent storage bucket.Solvent storage bucket is connected with the inlet part of macroporous resin column chromatography system, and the organic solvent in solvent storage bucket can directly be used in macroporous resin column chromatography system.
At the ultrafiltration system of resistance to solvent and resistance to solvent nanofiltration system, reclaim in the process of organic solvent, the clarity of the reflux solvent in the ultrafiltration system of resistance to solvent surpasses after No. 3, and all aqueous solutions of organic solvent in the current ultrafiltration system of resistance to solvent need to all be poured underpressure distillation pot into and reclaim remaining organic solvent.The ultrafiltration system of resistance to solvent again imports the feed liquid of new need recovery and carries out ultrafiltration.The clarity of the concentrated feed liquid that described resistance to solvent nanofiltration system is moved in system arrives after No. 2, need to need to all pour all aqueous solutions of organic solvent in current resistance to solvent nanofiltration system into underpressure distillation pot and reclaim remaining organic solvent.Resistance to solvent nanofiltration system again imports new ultrafiltration filtrate and carries out nanofiltration.
Wherein, the judgement of described clarity of solution is carried out according to the regulation in Chinese Pharmacopoeia appendix IX B, and clarity of solution inspection method is specific as follows:
At ambient temperature, by being diluted with water to the turbidity standard of certain density need testing solution with equivalent, be placed in respectively the turbid Glass tubing of using of ratio of pairing, than turbid, with Glass tubing, with colourless, transparent, neutral hard glass, make, internal diameter is 15～16mm, flat, tool plug; At turbidity standard, prepare after 5 minutes, vertical in darkroom with being placed under umbrella canopy lamp, illumination is 1000lx, from horizontal direction, observes, compares, in order to check clarity or its muddy degree of solution.Unless otherwise specified, trial-product should be inspected after dissolving immediately.
Wherein, turbidity standard need be got turbidity standard stoste and water configures in proportion and obtains; The preparation of turbidity standard stoste need be prepared turbidity standard stock solution.
The preparation method of turbidity standard stock solution: take the hydrazonium sulfate 1.00g that is dried to constant weight in 105 ℃, be placed in 100ml measuring bottle, add water and make it in right amount to dissolve, if desired can warm dissolving in the water-bath of 40 ℃, and be diluted with water to scale, and shake up, place 4～6 hours; Get this solution and mix with waiting 10% urotropine solution of capacity, shake up, in standing 24 hours of 25 ℃ of lucifuges, obtain.This liquid is put cold place and is kept in Dark Place, and can in two months, use, with front shaking up.
The preparation method of turbidity standard stoste: get turbidity standard stock solution 15.0ml, be placed in 1000ml measuring bottle, be diluted with water to scale, shake up, get in right amount, be placed in 1cm cuvette, according to the spectrophotometry in Chinese Pharmacopoeia appendix IX A, irradiate ultraviolet-visible ray, at the wavelength place of 550nm, measure, its absorbancy should be in 0.12～0.15 scope.This liquid should be used in 48 hours, with front shaking up.
The preparation method of turbidity standard: get turbidity standard stoste and water, the ratio preparation in table 1, obtains.This liquid should face used time preparation, before use, fully shakes up.
The preparation of table 1 turbidity standard
The beneficial effects of the utility model are: in organic solvent same treatment amount situation, the macroporous resin organic solvent chromatography liquid recovery system that the utility model provides is compared rectifying recovery system, its power consumption is lower, more obvious to its effect of the organic solvent of lower concentration; The main energy sources that the macroporous resin organic solvent chromatography liquid recovery system that the utility model provides is used is electric energy, need to produce the more environmental protection of steam rectifying recovery system of a large amount of combustion exhaust with respect to whole process.The macroporous resin organic solvent chromatography liquid recovery system that provides by the utility model reclaims the aqueous solutions of organic solvent that obtains through adjustment slightly, can directly use in macroporous resin column chromatography system corresponding step, simplify waste liquid and recycled the process reconfiguring, saved the time.
The utility model effect in actual experiment is remarkable, when the organic solvent-resistant ultra-filtration membrane that uses 1500-2500 molecular weight is as first filtration, the molecular configuration that this film is even 400-500 for molecular weight is that the material of macrocyclic ester material, ring texture or direct-connected shape structure also has good rejection, according to the difference of material, in recovery organic solvent waste liquid, except organic solvent, water, small molecules inorganic salt, the 80%-90% of solid substance total content is trapped.
After using the resistance to solvent nanofiltration membrane that molecular weight is 200-300, remove organic solvent, water and monovalent salt, filtrate concentrated dry after solid substance containing quantity not sufficient 4 ‰, this has met goes up the requirement of column chromatography to organic solvent again.Reuse like this efficiency that has improved solvent turnover, reduced the demand of on-the-spot solvent, further reached the effect reducing costs.
On the other hand, although being concentrated to recovery liquid after finite concentration in ultrafiltration system and nanofiltration system must import rectifying tower and reclaim solvent, but according to the difference of material properties, its volume is generally 1/10～1/40 of the front liquor capacity of whole ultrafiltration/nanofiltration, can make rectifying tower power consumption greatly reduce.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the utility model macroporous resin organic solvent chromatography liquid recovery system, wherein, and 1-macroporous resin chromatography column; 2-the ultrafiltration system of resistance to solvent; 3-resistance to solvent nanofiltration system; 4-solvent recovery tank; 5-underpressure distillation pot; 6-solvent storage bucket.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, further describe the utility model, but limit never in any form scope of the present utility model.
Embodiment mono-, two and three all recycles and adopts the various organic solvent waste water that need recovery that produce in Amberlyst process production high purity nimoctin product process by macroporous resin organic solvent chromatography liquid recovery system as shown in Figure 1.This macroporous resin organic solvent chromatography liquid recovery system comprises the ultrafiltration system of resistance to solvent 2, resistance to solvent nanofiltration system 3, underpressure distillation pot 5, solvent recovery tank 4 and solvent storage bucket 6, wherein: the ultrafiltration system of resistance to solvent 2 and resistance to solvent nanofiltration system 3 all adopt the product that is reached production by producer Xiamen three, be respectively the resistance to solvent nanofiltration equipment that the ultrafiltration apparatus of resistance to solvent that specification is SPPM-C-05 and specification are SPPM-25S-1; The ultra-filtration membrane of the ultrafiltration system of resistance to solvent 2 is that specifications and models are 7/6, area is 0.4m
2flat sheet membrane, the nanofiltration membrane of resistance to solvent nanofiltration system 3 is that specifications and models are 1812, area is 0.24m
2rolled film.The opening for feed of the ultrafiltration system of resistance to solvent 2 is connected with the discharge port of macroporous resin chromatography column 1, the ethanol organic solvent waste water reclaiming for receiving need that Amberlyst process production high purity nimoctin product process produces, its discharge port interconnects with the opening for feed of resistance to solvent nanofiltration system 3 and the opening for feed of underpressure distillation pot 5 respectively; The two ends of resistance to solvent nanofiltration system 3 discharge ports are connected with the opening for feed of solvent recovery tank 4 and the opening for feed of underpressure distillation pot 5 respectively; The discharge port of solvent recovery tank 4 is connected with the opening for feed of solvent storage bucket 6; The discharge port of solvent storage bucket 6 is connected to the opening for feed of macroporous resin chromatography column 1.Solvent storage bucket 6 has a plurality of.Between the ultrafiltration system of resistance to solvent 2 and macroporous resin chromatography column 1, between the ultrafiltration system of resistance to solvent 2 and resistance to solvent nanofiltration system 3, between the ultrafiltration system of resistance to solvent 2 and underpressure distillation pot 5, between resistance to solvent nanofiltration system 3 and solvent recovery tank 4, between resistance to solvent nanofiltration system 3 and underpressure distillation pot 5, between solvent recovery tank 4 and solvent storage bucket 6, between solvent storage bucket 6 and macroporous resin chromatography column 1, all by pipeline, be connected, one or more by-pass valve controls are all installed on described pipeline, for each, interconnect the switching between equipment.
In Amberlyst process production high purity nimoctin product process, produce the various organic solvent waste water need reclaiming, the organic solvent waste water of different concns and alcohol concn wherein respectively: upper prop waste water is 51% containing alcohol concn; Prewashing waste water is 60% containing alcohol concn; Regenerative wastewater is 95% containing alcohol concn.
Embodiment mono-: the chromatography column upper prop waste water 200L that reclaims 51% alcohol concn.In removal process, the present embodiment is used the chromatography of macroporous resin organic solvent shown in above-mentioned Fig. 1 liquid recovery system, specific as follows:
A1. the ethanol upper prop waste water of 51% concentration is imported to the ultrafiltration system of resistance to solvent 2 from macroporous resin chromatography column 1, the ultrafiltration system of resistance to solvent 2 operating pressure are 0.5MPa, and ultra-filtration membrane filtrate imports resistance to solvent nanofiltration system 3, and flow is 45ml/min; After ultrafiltration 106L, operating pressure is raised to 0.8Mpa; Ultra-filtration membrane filtrate imports resistance to solvent nanofiltration system 3, and flow is 39ml/min; Detect clarity of solution between No. 3-4 time, stop ultrafiltration, the about 5.2L of all concentrated solutions in the ultrafiltration system of resistance to solvent 2 is produced to underpressure distillation pot 5, the upper prop waste water more renewing carries out ultrafiltration, and the concentrated solution producing reclaims remaining ethanol with underpressure distillation pot 5.Residue fresh material is concentrated to after the minimum volume that ultra-filtration membrane need to move, and concentrated solution produces underpressure distillation pot 5 and reclaims remaining ethanol.
A2. ultrafiltration filtrate is imported to resistance to solvent nanofiltration system 3 from the ultrafiltration system of resistance to solvent 2, resistance to solvent nanofiltration system 3 operating pressure are 0.8MPa, and nanofiltration membrane filtrate imports solvent recovery tank 4 from resistance to solvent nanofiltration system 3, and flow is 60ml/min; Nanofiltration is concentrated to behind surplus 5L left and right, and operating pressure is 0.9MPa, and the clarity of concentrated solution is between No. 1-2 time, stops nanofiltration, concentrated solution is produced to underpressure distillation pot 5 from resistance to solvent nanofiltration system 3 and reclaim remaining ethanol.
The alcohol concn of the aqueous ethanolic solution that A3. nanofiltration goes out is 49%, and concentrated dry rear solid content is 0.29%.
Embodiment bis-: reclaim 60% alcohol concn column chromatography post prewashing waste water 200L.In removal process, the present embodiment is used the chromatography of macroporous resin organic solvent shown in above-mentioned Fig. 1 liquid recovery system, specific as follows:
B1. the ethanol prewashing waste water of 60% concentration is imported to the ultrafiltration system of resistance to solvent 2 from macroporous resin chromatography column 1, operating pressure is 0.5MPa, and ultra-filtration membrane filtrate imports resistance to solvent nanofiltration system 3, and flow is 46ml/min; Ultrafiltration 173L, operating pressure is raised to 0.8MPa, and ultra-filtration membrane filtrate flow is 35ml/min; Between No. 3-4, detection clarity of solution, stop ultrafiltration, the about 5.5L of all concentrated solutions in the ultrafiltration system of resistance to solvent 2 is produced to underpressure distillation pot 5, the upper prop waste water more renewing carries out ultrafiltration, and the concentrated solution producing reclaims remaining ethanol with underpressure distillation pot 5.Residue fresh material is concentrated to after the minimum volume that ultra-filtration membrane need to move, and concentrated solution produces underpressure distillation pot 5 and reclaims remaining ethanol.
B2. ultrafiltration filtrate is imported to resistance to solvent nanofiltration system 3 from the ultrafiltration system of resistance to solvent 2, operating pressure is 0.8MPa, and nanofiltration membrane filtrate imports solvent recovery tank 4 from resistance to solvent nanofiltration system 3, and flow is 60ml/min; Nanofiltration is concentrated to behind surplus 5L left and right, and operating pressure is 0.9MPa, and the clarity of concentrated solution is between No. 1-2 time, stops nanofiltration, concentrated solution is produced to underpressure distillation pot 5 from resistance to solvent nanofiltration system 3 and reclaim remaining ethanol.
The alcohol concn of the aqueous ethanolic solution that B3. nanofiltration goes out is 58.6%, and concentrated dry rear solid content is 0.13%.
Embodiment tri-: the column chromatography regenerative wastewater 200L that reclaims 95% alcohol concn.In removal process, the present embodiment is used the chromatography of macroporous resin organic solvent shown in above-mentioned Fig. 1 liquid recovery system, specific as follows:
C1. the ethanol regenerative wastewater of 95% concentration is imported to the ultrafiltration system of resistance to solvent 2 from macroporous resin chromatography column 1, operating pressure is 0.5MPa, and ultra-filtration membrane filtrate imports resistance to solvent nanofiltration system 3, and flow is 40ml/min; Ultrafiltration 148L, operating pressure is raised to 0.8MPa, and ultra-filtration membrane filtrate flow is 31ml/min; Between No. 3-4, detection clarity of solution, stop ultrafiltration, the about 5.4L of all concentrated solutions in the ultrafiltration system of resistance to solvent 2 is produced to underpressure distillation pot 5, the upper prop waste water more renewing carries out ultrafiltration, and the concentrated solution producing reclaims remaining ethanol with underpressure distillation pot 5.Residue fresh material is concentrated to after the minimum volume that ultra-filtration membrane need to move, and concentrated solution produces underpressure distillation pot 5 and reclaims remaining ethanol.
C2. ultrafiltration filtrate is imported to resistance to solvent nanofiltration system 3 from the ultrafiltration system of resistance to solvent 2, operating pressure is 0.8MPa, and nanofiltration membrane filtrate imports solvent recovery tank 4 from resistance to solvent nanofiltration system 3, and flow is 56ml/min; Nanofiltration is concentrated to behind surplus 5L left and right, and operating pressure is 0.9MPa, and the clarity of concentrated solution is between No. 1-2 time, stops nanofiltration, concentrated solution is produced to underpressure distillation pot 5 from resistance to solvent nanofiltration system 3 and reclaim remaining ethanol.
The alcohol concn of the aqueous ethanolic solution that C3. nanofiltration goes out is 94.5%, and the content of concentrated dry rear solid substance is 0.32%.
Embodiment tetra-, five and six all recycles and adopts the various organic solvent waste water that need recovery that produce in Amberlyst process production high purity lovastatin product process by macroporous resin organic solvent chromatography liquid recovery system as shown in Figure 1.This macroporous resin organic solvent chromatography liquid recovery system comprises the ultrafiltration system of resistance to solvent 2, resistance to solvent nanofiltration system 3, underpressure distillation pot 5, solvent recovery tank 4 and solvent storage bucket 6, wherein: the ultrafiltration system of resistance to solvent 2 and resistance to solvent nanofiltration system 3 all adopt the product that is reached production by producer Xiamen three, be respectively the resistance to solvent nanofiltration equipment that the ultrafiltration apparatus of resistance to solvent that specification is SPPM-C-05 and specification are SPPM-25S-1; The ultra-filtration membrane of the ultrafiltration system of resistance to solvent 2 is that specification is that the long 3m of single internal diameter 5mm, area are 0.8m
2ultrafiltration tubular membrane component, the nanofiltration membrane of resistance to solvent nanofiltration system 3 is that specifications and models are 1812, area is 0.24m
2rolled film.The opening for feed of the ultrafiltration system of resistance to solvent 2 is connected with the discharge port of macroporous resin chromatography column 1, the methyl alcohol organic solvent waste water reclaiming for receiving need that Amberlyst process production high purity lovastatin product process produces, its discharge port interconnects with the opening for feed of resistance to solvent nanofiltration system 3 and the opening for feed of underpressure distillation pot 5 respectively; The two ends of resistance to solvent nanofiltration system 3 discharge ports are connected with the opening for feed of solvent recovery tank 4 and the opening for feed of underpressure distillation pot 5 respectively; The discharge port of solvent recovery tank 4 is connected with the opening for feed of solvent storage bucket 6; The discharge port of solvent storage bucket 6 is connected to the opening for feed of macroporous resin chromatography column 1.Solvent storage bucket 6 has a plurality of.Between the ultrafiltration system of resistance to solvent 2 and macroporous resin chromatography column 1, between the ultrafiltration system of resistance to solvent 2 and resistance to solvent nanofiltration system 3, between the ultrafiltration system of resistance to solvent 2 and underpressure distillation pot 5, between resistance to solvent nanofiltration system 3 and solvent recovery tank 4, between resistance to solvent nanofiltration system 3 and underpressure distillation pot 5, between solvent recovery tank 4 and solvent storage bucket 6, between solvent storage bucket 6 and macroporous resin chromatography column 1, all by pipeline, be connected, one or more by-pass valve controls are all installed on described pipeline, for each, interconnect the switching between equipment.
In Amberlyst process production high purity lovastatin product process, produce the various organic solvent waste water need reclaiming, the organic solvent waste water of different concns and methanol concentration wherein respectively: upper prop waste water is containing methanol concentration 60%; Prewashing waste water is containing methanol concentration 70%; Regenerative wastewater is containing methanol concentration 95%.
Embodiment tetra-: reclaim 60% methanol concentration column chromatography upper prop waste water 400L.In removal process, the present embodiment is used the chromatography of macroporous resin organic solvent shown in above-mentioned Fig. 1 liquid recovery system, specific as follows:
D1. the methyl alcohol upper prop waste water of 60% concentration is imported to the ultrafiltration system of resistance to solvent 2 from macroporous resin chromatography column 1, operating pressure is 0.5MPa, and ultra-filtration membrane filtrate imports resistance to solvent nanofiltration system 3, and flow is 58ml/min; Ultrafiltration 181L, operating pressure is raised to 0.8MPa, and ultra-filtration membrane filtrate flow is 51ml/min; Between No. 3-4, detection clarity of solution, stop ultrafiltration, the about 5.2L of all concentrated solutions in the ultrafiltration system of resistance to solvent 2 is produced to underpressure distillation pot 5, the upper prop waste water more renewing carries out ultrafiltration, and the concentrated solution producing reclaims remaining methyl alcohol to underpressure distillation pot 5.Residue fresh material is concentrated to after the minimum volume that ultra-filtration membrane need to move, and concentrated solution produces underpressure distillation pot 5 and reclaims remaining methyl alcohol.
D2. ultrafiltration filtrate is imported to resistance to solvent nanofiltration system 3 from the ultrafiltration system of resistance to solvent 2, operating pressure is 0.8MPa, and nanofiltration membrane filtrate imports solvent recovery tank 4 from resistance to solvent nanofiltration system 3, and flow is 67ml/min; Nanofiltration is concentrated to behind surplus 13L left and right, and operating pressure is 0.9MPa, and the clarity of concentrated solution is between No. 3-4.Concentrated solution produces underpressure distillation pot 5 from resistance to solvent nanofiltration system 3 and reclaims remaining methyl alcohol, again imports fresh ultra filtration filtrate and again carries out nanofiltration.Nanofiltration is concentrated to behind surplus 5L left and right, and operating pressure is 0.9MPa, and the clarity of concentrated solution is between No. 1-2 time, stops nanofiltration, concentrated solution is produced to underpressure distillation pot 5 from resistance to solvent nanofiltration system 3 and reclaim remaining methyl alcohol.
The methanol concentration of the methanol aqueous solution that D3. nanofiltration goes out is 59.2%, and the content of concentrated dry rear solid substance is 0.21%.
Embodiment five: reclaim 70% methanol concentration column chromatography prewashing waste water 200L.In removal process, the present embodiment is used the chromatography of macroporous resin organic solvent shown in above-mentioned Fig. 1 liquid recovery system, specific as follows:
E1. the methyl alcohol prewashing waste water of 70% concentration is imported to the ultrafiltration system of resistance to solvent 2 from macroporous resin chromatography column 1, operating pressure is 0.5MPa, and ultra-filtration membrane filtrate imports resistance to solvent nanofiltration system 3, and flow is 56ml/min; The complete 200L of ultrafiltration, operating pressure is raised to 0.8MPa, and it is 51ml/min that membrane filtration goes out flow quantity; While detecting between No. 3-4, clarity of solution, stop ultrafiltration, the about 5.1L of all concentrated solutions in the ultrafiltration system of resistance to solvent 2 is produced to underpressure distillation pot 5, the concentrated solution producing reclaims remaining methyl alcohol with underpressure distillation pot 5.
E2. ultrafiltration filtrate is imported to resistance to solvent nanofiltration system 3 from the ultrafiltration system of resistance to solvent 2, operating pressure is 0.8MPa, and nanofiltration membrane filtrate imports solvent recovery tank 4 from resistance to solvent nanofiltration system 3, and flow is 66ml/min; Nanofiltration is concentrated to behind surplus 5L left and right, and operating pressure is 0.9MPa, and the clarity of concentrated solution is between No. 1-2 time, stops nanofiltration, concentrated solution is produced to underpressure distillation pot 5 from resistance to solvent nanofiltration system 3 and reclaim remaining methyl alcohol.
The methanol concentration of the methanol aqueous solution that E3. nanofiltration goes out is 69.5%, and the content of concentrated dry rear solid substance is 0.11%.
Embodiment six: reclaim 95% methanol concentration column chromatography regenerative wastewater 300L.In removal process, the present embodiment is used the chromatography of macroporous resin organic solvent shown in above-mentioned Fig. 1 liquid recovery system, specific as follows:
F1. the Mathanol regenerating waste water of 95% concentration is imported to the ultrafiltration system of resistance to solvent 2 from macroporous resin chromatography column 1, operating pressure is 0.5MPa, and ultra-filtration membrane filtrate imports resistance to solvent nanofiltration system 3, and flow is 54ml/min; The complete 186L of ultrafiltration, operating pressure is raised to 0.8MPa, and it is 50ml/min that membrane filtration goes out flow quantity; Between No. 3-4, detection clarity of solution, stop ultrafiltration, the about 5.3L of all concentrated solutions in the ultrafiltration system of resistance to solvent 2 is produced to underpressure distillation pot 5, the upper prop waste water more renewing carries out ultrafiltration, and the concentrated solution producing reclaims remaining methyl alcohol with underpressure distillation pot 5.Residue fresh material is concentrated to after the minimum volume that ultra-filtration membrane need to move, and concentrated solution produces underpressure distillation pot 5 and reclaims remaining methyl alcohol.
F2. ultrafiltration filtrate is imported to resistance to solvent nanofiltration system 3 from the ultrafiltration system of resistance to solvent 2, operating pressure is 0.8MPa, and nanofiltration membrane filtrate imports solvent recovery tank 4 from resistance to solvent nanofiltration system 3, and flow is 63ml/min; Nanofiltration is concentrated to behind surplus 8.5L left and right, and operating pressure is 0.9MPa, and the clarity of concentrated solution is between No. 3-4.Concentrated solution produces with underpressure distillation pot 5 and reclaims remaining methyl alcohol from resistance to solvent nanofiltration system 3, again imports fresh ultra filtration filtrate and again carries out nanofiltration.Nanofiltration is concentrated to behind surplus 5L left and right, and operating pressure is 0.9MPa, and the clarity of concentrated solution is between No. 1-2 time, stops nanofiltration, concentrated solution is produced to underpressure distillation pot 5 from resistance to solvent nanofiltration system 3 and reclaim remaining methyl alcohol.
The methanol concentration of the methanol aqueous solution that F3. nanofiltration goes out is 93.8%, and the content of concentrated dry rear solid substance is 0.4%.
Claims (7)
1. a macroporous resin organic solvent chromatography liquid recovery system, it is characterized in that: comprise the ultrafiltration system of resistance to solvent (2), resistance to solvent nanofiltration system (3), underpressure distillation pot (5), solvent recovery tank (4) and solvent storage bucket (6), the opening for feed of the described ultrafiltration system of resistance to solvent (2) is connected with the discharge port of macroporous resin chromatography column (1), be used for receiving macroporous resin organic solvent chromatography liquid, the two ends of the ultrafiltration system of resistance to solvent (2) discharge port are connected with the opening for feed of described resistance to solvent nanofiltration system (3) and the opening for feed of described underpressure distillation pot (5) respectively; The two ends of described resistance to solvent nanofiltration system (3) discharge port are connected with the opening for feed of described solvent recovery tank (4) and the opening for feed of underpressure distillation pot (5) respectively; The discharge port of described solvent recovery tank (4) is connected with the opening for feed of solvent storage bucket (6); The discharge port of described solvent storage bucket (6) is connected with the opening for feed of macroporous resin chromatography column (1).
2. macroporous resin organic solvent chromatography liquid recovery system as claimed in claim 1, is characterized in that: the ultra-filtration membrane of the described ultrafiltration system of resistance to solvent (2) is polyethersulfone composite membrane.
3. macroporous resin organic solvent chromatography liquid recovery system as claimed in claim 1, is characterized in that: the nanofiltration membrane of described resistance to solvent nanofiltration system (3) is polyamide composite film.
4. macroporous resin organic solvent chromatography liquid recovery system as claimed in claim 1, is characterized in that: the ultra-filtration membrane of the described ultrafiltration system of resistance to solvent (2) is board-like film or tubular membrane.
5. macroporous resin organic solvent chromatography liquid recovery system as claimed in claim 1, is characterized in that: the nanofiltration membrane of described resistance to solvent nanofiltration system (3) is rolled film.
6. macroporous resin organic solvent chromatography liquid recovery system as claimed in claim 1, is characterized in that: described solvent storage bucket (6) has a plurality of.
7. macroporous resin organic solvent chromatography liquid recovery system as claimed in claim 1, it is characterized in that: between the described ultrafiltration system of resistance to solvent (2) and macroporous resin chromatography column (1), between the ultrafiltration system of resistance to solvent (2) and resistance to solvent nanofiltration system (3), between the ultrafiltration system of resistance to solvent (2) and underpressure distillation pot (5), between resistance to solvent nanofiltration system (3) and solvent recovery tank (4), between resistance to solvent nanofiltration system (3) and underpressure distillation pot (5), between solvent recovery tank (4) and solvent storage bucket (6), between solvent storage bucket (6) and macroporous resin chromatography column (1), all by pipeline, be connected, one or more by-pass valve controls are all installed on described pipeline.
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| CN201320735974.5U CN203545832U (en) | 2013-11-20 | 2013-11-20 | Macro-porous resin organic solvent chromatographic liquid recycle system |
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| CN201320735974.5U CN203545832U (en) | 2013-11-20 | 2013-11-20 | Macro-porous resin organic solvent chromatographic liquid recycle system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356140A (en) * | 2014-09-30 | 2015-02-18 | 大连九信生物化工科技有限公司 | Method for separating and preparing high-purity Moxidectin membrane |
| CN111573950A (en) * | 2020-05-29 | 2020-08-25 | 盛隆资源再生（无锡）有限公司 | Method for recycling and treating wastewater containing organic solvent |
-
2013
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356140A (en) * | 2014-09-30 | 2015-02-18 | 大连九信生物化工科技有限公司 | Method for separating and preparing high-purity Moxidectin membrane |
| CN104356140B (en) * | 2014-09-30 | 2016-06-08 | 大连九信生物化工科技有限公司 | A kind of membrance separation preparation method of high-purity moxidectin |
| CN111573950A (en) * | 2020-05-29 | 2020-08-25 | 盛隆资源再生（无锡）有限公司 | Method for recycling and treating wastewater containing organic solvent |
| CN111573950B (en) * | 2020-05-29 | 2022-07-26 | 盛隆资源再生（无锡）有限公司 | Recovery treatment method of organic solvent-containing wastewater |
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Address after: 100871 Beijing, Haidian District, into the mansion building, No. 298 Patentee after: Peking Founder Group Co., Ltd. Patentee after: CHONGQING DAXIN PHARMACEUTICAL CO., LTD. Patentee after: PKU HEALTHCARE INDUSTRY GROUP Address before: 100871 Beijing, Haidian District, into the mansion building, No. 298 Patentee before: Peking Founder Group Co., Ltd. Patentee before: Chongqing Daxin Pharmaceuticals Co., Ltd. of PKU International HealthCare Group Patentee before: PKU HEALTHCARE INDUSTRY GROUP |
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