CN209645878U - Aqueous organic liquid waste and organic solvent separation and recovery system - Google Patents
Aqueous organic liquid waste and organic solvent separation and recovery system Download PDFInfo
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- CN209645878U CN209645878U CN201920174327.9U CN201920174327U CN209645878U CN 209645878 U CN209645878 U CN 209645878U CN 201920174327 U CN201920174327 U CN 201920174327U CN 209645878 U CN209645878 U CN 209645878U
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Abstract
The utility model provides aqueous organic liquid waste and organic solvent separation and recovery system, the separation and recovery system are connected by process pipelines with infiltration evaporation film separation system by distillation system and formed.Wherein, rectifying column uses packed tower, and the feed inlet of packed tower is arranged at Liquid Distribution in Packed Columns center.Damping structure is provided in the infiltration evaporation film unit of the infiltration evaporation film separation system.Separation and recovery system described in the utility model is suitable for a variety of aqueous and two kinds with the above azeotropic or azeotropic organic solvent is not dehydrated recycling online and organic solvent is separated, applied.
Description
Technical field
The utility model belongs to organic liquid waste recycling field, and in particular to a kind of miniaturization solvent recovery unit and method.
Background technique
Currently, with the continuous improvement of global economy fast development and integrated degree, the scientific research of each scientific domain of China
Activity also enters the fast traffic lane of high speed development, and the Board Lot for being engaged in scientific research is also doubled and redoubled, especially chemistry and life
Scientific domain development is very fast, and more stringent requirements are proposed for and environment-protecting industrial industrial to basic material, makes in research process
Solvent quality requirement is higher and higher, and dosage is also increasing, and solvent type is more, and constituent parts demand is again more scattered, receives
Collection processing intricate operation.
In pharmaceutical industry, it is high with extensive universality, ease-to-operate and separation for preparative liquid chromatography system addresses
The outstanding advantages such as effect property have become the mainstream technology for isolating and purifying drug, however the things of many company's headaches is allowed to be exactly to prepare
The solvent slop generated in journey not only causes environmental pollution also and will cause production cost high if directly discharged；Separately
Outside since preparing chromatography system is to the high request of solvent quality, so that solvent slop can not be real by simple recovery processing energy
Existing reuse is applied.
Existing solvent recovering system is mostly the biggish industrialized unit for the treatment of capacity, which has policy threshold height,
Construction period is long, and cost of investment is high, takes up a large area, the more demanding feature of security of system, operability, and at present molten
Agent recyclable device mostly by simply evaporating, distillation technique forms, only will organic solvent carry out simply be concentrated after weight
Multiple to use, it is only minimizing actually for solvent recovery that there is still a need for discharges after impurities accumulation is to a certain concentration
Effect.Therefore, most of device can only can be regarded as organic solvent thickener, and recycling obtained organic solvent can not directly make
With.Higher to the purity requirement of organic solvent especially for the enterprise for using preparation chromatography, existing equipment recycles organic molten
Agent cannot be used directly for preparation chromatography.There is presently no can make the equipment of recovered solvent repurity to reuse standard
Medicine enterprise and large and medium-sized drug research mechanism substantial amounts with preparation chromatography, if can develop a kind of for laboratory, research and development
Mechanism and the miniaturization device for meeting GMP solvent reclaiming requirement, and installation area is small, easy to operate, for enterprise head
Phase existence reduces influence to environment, reduces production cost and be of great significance.
Summary of the invention
The utility model aim is to provide water-containing organic solvent purifying and organic solvent separation and recovery system, be suitable for more
Kind is aqueous and two kinds with the above azeotropic or azeotropic organic solvent is not dehydrated recycling online and organic solvent is separated, applied.
Separation and recovery system provided by the utility model passes through process duct by distillation system and infiltration evaporation film separation system
Line connection composition；
The distillation system includes quenched kettle, rectifying column, segregator, complete condenser and product receiving slit one, the quenched kettle
Discharge port be connected to the feed inlet of rectifying column, segregator setting is at the top of the rectifying column in tower body, the complete condenser setting
In rectifying tower top, the low boiling component for that will not condensed by segregator is condensed, and bypass line is arranged in complete condenser discharge port, is used
A part of condensable product enters product receiving slit one, and a part flows back into rectifying column；
The infiltration evaporation film separation system includes vaporizer, vapour liquid separator, reheater, infiltration vaporization membrane module, infiltration
Transparent liquid condenser, product condenser, product receiving slit two form；The feed inlet and product receiving slit two of the vaporizer with production
Product receiving slit one is connected to, and the discharge port of vaporizer be connected to the feed inlet of vapour liquid separator, the discharge port of vapour liquid separator and again
The feed inlet of hot device is connected to, and the discharge port of reheater connects membrane module, and the infiltrating and vaporizing membrane group is by 1~6 grade of (infiltrating and vaporizing membrane
Series and every level-one setting infiltrating and vaporizing membrane quantity, be to be determined according to by separation system) infiltration evaporation film unit
In series, every unit is made of in parallel or series 2-6 infiltration vaporization membrane module, and infiltration is respectively configured in every grade of infiltrating and vaporizing membrane
Liquid cooling condenser and infiltration liquid bath, the infiltration liquid bath is connected to distillation system rectifying column feed inlet or direct waste discharge, membrane module
Discharge port connects product condenser and product receiving slit.
Further, the rectifying column is efficient, multi-functional packed tower, which is respectively arranged at the top of tower body and middle part
The operation of the special extract rectifications such as extracting rectifying or azeotropic distillation may be implemented in one feed inlet.Rectifying column uses side entry feed, in tower body
Top and middle part one feed inlet is respectively set, feed inlet is located at the overcentre of Liquid Distribution in Packed Columns, the liquid point
Cloth device is made of disk and several tap holes being uniformly arranged on disk, and disc surfaces are provided in connection tap hole and disk
The groove of heart point, the path of groove meet each tap hole being equidistant to disc centre point.
Preferably, the tap hole is cylindrical hole, and crown cap is arranged in the top of each tap hole, and the top cap is by setting
It sets and is fixed in the support column support for shunting aperture, realize and keep gap to pass through for the vapour phase of rising between shunting aperture.Rectifying
Built-in segregator is arranged for top of tower, it can be achieved that the gas phase of rectifying column discharges, and condensation uses 0~12 DEG C of water at low temperature, and water at low temperature is by cold
Water dispenser provides；Tower body is using 304 stainless steel materials, it can be achieved that pressurization, normal pressure and the decompression operation of rectifying column；Tower bottom of rectifying tower holds
Product is 0.5~50L (being set according to treating capacity).Feed inlet is set simultaneously, the third substance can be added into tower reactor, realizes reaction
Rectifying function.To sum up, the rectifying column has multi-functional characteristic, and distillation process can realize pressurization, normal pressure, decompression essence respectively
It evaporates, extracting rectifying and azeotropic distillation, the different function such as reactive distillation.
Preferably, the filler of the rectifying column is efficient dumped packing, can be but be not limited only to stainless steel wire net forming
θ type or triangle spring filler, glass ceramics and plastic material etc..
Further, the tower bottom of rectifying tower is using electricity, steam or heat-conducting oil heating mode.
Further, the preheater of preheating material is provided on the rectifying column feeding line.
Further, distillation system further includes the extraction/entrainer storage tank for storing extractant or entrainer, and is used for essence
Evaporate the feed pump in tower tower into extractant or entrainer.By adding third party's solvent (extractant/entrainer), to change, mention
Height is by the relative volatility of separation solvent, to achieve the purpose that separation by rectifying.
Further, extraction/azeotropic is provided on the pipeline of the extraction/between entrainer storage tank and rectifying column feed inlet
Agent cooler.
Further, the quenched kettle is the reaction kettle with stirring structure, for aqueous organic liquid waste to be passed through addition chela
Mixture carries out just separation, so that impurity therein and heavy constituent form chelate, separates and is easier in rectifying.
Further, each membrane module of the infiltration evaporation film unit is by several infiltration evaporation membrane tube (such as molecular sieves
Ceramic-film tube), cylindrical putamina and film partition constitute, the membrane tube is uniformly fixed on the fixed disk for being provided with multiple fixation holes
On, the fixed disk is located at the top of putamina, and film partition one end is fixed in fixed disk, and the other end stretches to putamina bottom, will
Space uniform is divided into the two parts communicated in putamina.
Further, it is increase membrane tube permeation flux, can choose using one of following two setting:
(1) in the infiltration evaporation film separation system, corrosion-resistant material (such as tetrafluoro is cased with outside every infiltration evaporation membrane tube
Material etc.) internal diameter of production is the damping spring of φ 13, the effect of the spring is embodied in following two points, and one side spring increases
The turbulance for having added medium in infiltration evaporation putamina, makes to expect more uniform in the distribution of putamina radial direction, is avoided as much as back-mixing；
On the other hand, because of the perturbation action of spring, keep the concentration polarization layer of infiltration evaporation film surface significantly thinning, substantially increase object
The mass transfer rate of material.Therefore, the flux and separative efficiency of infiltrating and vaporizing membrane are substantially increased by damping setting.
(2) the putamina inner wall and film baffle surface are provided with multiple amortisseur bars, and the amortisseur bar is by mounting bar and interval
Certain distance is uniformly arranged on the composition of the damping block on mounting bar, and putamina inner wall is provided with and the matched installation of mounting bar size
Slot, the mounting bar are embedded in the fixation that damping block is realized in mounting groove.Preferably, resistant block is similar to contract type, and damping block is to putamina
Interior space downstream direction protrusion.The effect of resistant block is the resistance on raising steam flow direction, increases steam flow in putamina
Turbulent extent can also effectively reduce the influence of concentration polarization, also residence time of the raising steam in putamina, to effectively improve
The flux of infiltration vaporization membrane module, the quantity for reducing membrane module also just reduce the cost of investment of membrane module.
Further, the rectifying column, vaporizer are provided with feed pump, and the tower bottom of rectifying tower discharge port is provided with out
Material pump.
Further, in the infiltration evaporation film separation system, infiltrating and vaporizing membrane group afterbody infiltration evaporation film unit
(material steam outlet) is provided with counterbalance valve between product condenser.
The chief motivation of infiltration evaporation UF membrane is the pressure difference inside and outside film, and the effect that counterbalance valve is arranged is increased outside membrane tube
The pressure of material steam to be separated improves the pressure difference of outside material in infiltrating and vaporizing membrane, improves moisture etc. and penetrates infiltrating and vaporizing membrane
The flux of component is fast and efficiently separated with realizing.It is operated in the molecular sieve membrane tube of infiltrating and vaporizing membrane for vacuum state, it is practical
Film device is to realize the vacuumizing in membrane tube equipped with vacuum pump in use process, by vacuum pump frequency conversion and vacuum pump into
Regulating valve is arranged to realize the regulation and control of vacuum degree in port.
Further, afterburner is provided between infiltration vaporization membrane module upper level and next stage seperation film.
Further, in the infiltration evaporation film separation system, infiltration liquid bath connects vacuum pump simultaneously, keeps infiltration liquid cooling
There is larger and stable vacuum degree on the inside of condenser and membrane tube, to ensure to keep biggish pressure difference inside and outside infiltrating and vaporizing membrane,
The motive force for further increasing infiltration evaporation membrane separating process makes infiltrating and vaporizing membrane flux with higher and separative efficiency.
Further, the vaporizer, reheater are heating equipment, allow the liquid to be vaporized into steam, are seeped with entering
Saturating vaporization membrane module carries out lock out operation.
Preferably, recycling separation system described in the utility model is made of corrosion resistant 304 material or 316L material.
The utility model provide based on above-mentioned separation and recovery system be applicable to a variety of aqueous and two kinds and the above azeotropic or
Azeotropic organic solvent is not dehydrated recycling online and separates with solvent, applies that (organic solvent of recycling returns to life as novel solvent
Produce and used in workshop section), especially there is preferable separating effect to the system of azeotrope with water.The system dimension is small, and length is 1~5
Rice, width are 1~3 meter, are highly 1.5~4 meters, save space, the totally-enclosed operation of equipment.Total system is closed in cabinet,
And the minimal amount of organic solvent extraction that will likely be escaped in time by the way that extractor fan is arranged, it avoids organic solvent from gathering, improves
The safety of device.Device integrally uses stainless steel material, using the company of flange or fast disassembly type clip between equipment and pipeline
It connects, it is ensured that the sealing performance of device.The system operation controls related input and output material valve, feed pump, vacuum pump by PLC and moves
Make, adjustment parameter such as temperature, pressure, flow etc..If PLC controller sends control signals to inlet control valve, control valve is made
There can be different apertures according to the variation of controller signals for actuator, flowmeter real-time measurement flow is set after control valve, and
Flow signal is sent to controller, the flow signal that controller is returned according to flowmeter, by after operation control signal weight
It newly is sent to regulating valve, until flowmeter measuring flow reaches preset flow.Whole system is all automatic by PLC programming Control
Change, without human intervention.
Separation and recovery system described in the utility model can be widely used for but be not limited to polypeptide industry (acetonitrile, tetrahydrofuran, second
Alcohol, methyl tertiary butyl ether(MTBE) dehydration, methylene chloride, Methanol Recovery etc.), electronics industry (isopropanol, butanone dehydration, acetone recycling etc.)
And it the online recycling of laboratory spent organic solvent and applies.It is the acetonitrile that is related in the above industry, tetrahydrofuran, ethyl alcohol, different
Propyl alcohol, butanone, methanol, methylene chloride, methyl tertbutyl water content be applicable in the device and two or more from 0~99%
The separation of mixed solvent.After the device in waste water the content of organic solvent less than 0.1%.
The device can be widely used for but be not limited only to polypeptide industry (acetonitrile, methanol, DMF, tetrahydrofuran, ethanol dehydration
Deng), the online recycling of electronics industry (isopropanol dehydration etc.) and laboratory spent organic solvent and apply, it is molten to substantially reduce enterprise
Agent outsourcing amount and dangerous waste yield greatly reduce the production cost and environmental protection cost of enterprise.
Separation and recovery method provided by the utility model based on above-mentioned separation and recovery system, includes the following steps, will contain
Aqueous organic solvent or two kinds of azeotropic or non-vapor of mixture solvent continuously enter rectifying column, control essence by pump after quenched
Evaporating tower inlet amount is 10~300L/h, and bottom temperature is 60~300 DEG C, and tower top temperature is 40~200 DEG C, and the operating pressure of tower is
10~300kPa, reflux ratio are 0.5~5, and by rectifying, solvent is purified to 80wt% or more, into infiltration vaporization membrane module
Depth separation is carried out, infiltration vaporization membrane module feeding temperature is 80~150 DEG C, and inlet amount is 0.5~50L/h, and operating pressure is
100~600kPa purifies to organic solvent purity >=99.9% (wt).
Separation and recovery system described in the utility model, can according to by the component of separation waste liquid and to the needs of separation purity,
Selection use is carried out to the separation and recovery system.
1. water-containing organic solvent is purified to 80% (wt) or more, deep dehydration, warp are carried out into infiltration vaporization membrane module
Cross organic solvent purity >=99.9% (wt) of dehydration, waste discharge organic solvent content≤0.1% after the device.
2. not two kinds of solvents of azeotropic, highly efficient distilling column overhead obtains a kind of lower organic solvent content >=99% of boiling point
(wt), tower bottom obtains higher organic solvent content >=99% of second of boiling point (wt).
3. two kinds of organic solvents of azeotropic are by being added extractant, highly efficient distilling column overhead obtains water content to be had less than 20%
Solvent, tower bottom obtain second of organic solvent content >=99% (wt).
For the small-sized solvent recovery unit according to the difference for the treatment of capacity, rectifier unit inlet amount is 10~300L/h, infiltration
Vaporization membrane module inlet amount is 0.5~50L/h.The utility model recycles separation system, and the exhaust gas generated in removal process passes through
Pipeline drains into processing system through negative-pressure air fan, by deep condensation, spray-absorption and activated carbon adsorption qualified discharge.
Compared with prior art, the utility model has following beneficial effect:
1. the utility model recycles separation system, entire removal process is controlled using PLC, and recyclable device is placed in cabinet,
Cabinet is equipped with extractor fan, and the minimal amount of organic solvent extraction that will likely be escaped in time avoids organic solvent from gathering, improves dress
The safety set.
2. the utility model recycles separation system, device realizes closure operation, and device integrally uses stainless steel material, if
The standby connection that flange or fast disassembly type clip are used between pipeline, it is ensured that the sealing performance of device, rectifying column is using advanced
High standard filler has the characteristics that the number of plates is high, load is big, plate efficiency is high, shortens the operating time, reduces solvent and wave
Hair, the possibility exposed.
3. the utility model recycles separation system, the condenser of rectifying tower top uses negative pressure cryogenic operations, it is ensured that maximum limit
Degree recycling organic solvent, can reduce the outlet temperature of product in distillation process.
4. separation and recovery system described in the utility model due in stuffing rectification column liquid distribution trough solve side-fed
Bring liquid stream is unevenly distributed problem, and vapour, gas-liquid two-phase liquid are evenly distributed, contact abundant, mass transfer on packed tower horizontal cross-section
Heat transfer efficiency is high, pressure drop is small, do not block, does not easily cause liquid foam entrainment and foaming, and rectification efficiency is high.
5. separation and recovery system described in the utility model, damping spring is devised in membrane module, is improved on steam flow direction
Resistance increases turbulent extent of the steam flow in putamina, can also effectively reduce the influence of concentration polarization, and also extension steam is in putamina
Residence time, to effectively improve the flux of infiltration vaporization membrane module, the quantity for reducing membrane module also just reduces membrane module
Cost of investment.Meanwhile structure is simple, production easy to process, processing cost is low.
6. separation and recovery system described in the utility model, organic liquid waste first pass through rectifying, using infiltrating and vaporizing membrane, pass through
Rectifying removes most water, further separates by infiltrating and vaporizing membrane, is conducive to protect infiltrating and vaporizing membrane, extends and use the longevity
Life.
7. system described in the utility model realize aqueous, azeotropic or not the separation of organic mixed solvent waste liquid of azeotropic mention
Pure, organic solvent purity >=99.9% (wt) after purification, obtained organic solvent can be used directly.It especially meets using system
The enterprise of standby chromatography is to the higher requirement of the purity of organic solvent, and the system bulk is small, saves space, is to be suitble to experiment
Room, research and development institution and the miniaturization device for meeting GMP solvent reclaiming requirement, occupied area is small, easy to operate, saves a large amount of
Solvent outsourcing cost, influence, reduction production cost for enterprise's long term survival, reduction to environment are of great significance.
Detailed description of the invention
Fig. 1 is the overall structure diagram of separation and recovery system described in the utility model；
Fig. 2 is the sectional view of rectifying column described in the utility model；
Fig. 3 is the top view of the liquid distribution trough of rectifying column described in the utility model.
Fig. 4 is the bottom view of the liquid distribution trough of rectifying column described in the utility model.
Fig. 5 is that tap hole and the schematic diagram of top cap (are only shown in figure on liquid distributor for rectifying tower described in the utility model
One tap hole).
Fig. 6 is the top view of membrane module described in the utility model；
Fig. 7 is membrane module front view described in the utility model；
Fig. 8 is the film schematic diagram of set loading damp spring described in the utility model.
In figure, the quenched kettle of 1-, 2- rectifying column, 3- segregator, 4- complete condenser, 5- product receiving slit one, 6- vapour liquid separator,
7- vaporizer, 8- reheater, 9- infiltrating and vaporizing membrane group, 10- counterbalance valve, 11- product condenser, 12- product receiving slit two, 13-
Permeate condenser, 14- permeate liquid bath, 15- extraction/entrainer slot, 16- extraction/entrainer condenser, 17- preheater, 18-
Feed pump, 19- tower body, 20- tower reactor, 21- segregator, 22- liquid distribution trough, 22-1 disk, 22-2 tap hole, 22-3 groove,
22-4 top cap, 23- feed pipe, 24- infiltration evaporation membrane tube, 25- cylinder putamina, 26- fixed disk, 27- partition, 28- damp bullet
Spring.
Specific embodiment
The utility model is described in further detail below by specific embodiment.But those skilled in the art will
Understand, the following example is merely to illustrate the utility model, and should not be regarded as limiting the scope of the utility model.According to this field
Technology or conditions described in interior document are carried out according to product description.Production firm is not specified in agents useful for same or instrument
Person, being can be with conventional products that are commercially available.
Succinct in order to describe, term " rectifying column " is practical new at this in the case where no specified otherwise in the utility model
In improvement structure basis described in type, it can respectively refer to for common rectifying tower tower containing compression rectification, atmospheric distillation tower, rectification under vacuum
Tower, extractive distillation column and azeotropy rectification column, reactive distillation column.
In implementing below, in addition to the present invention is particularly described, commercial equipment is can be used in conventional equipment.
Embodiment 1
Separation and recovery system is connected by process pipelines with infiltration evaporation film separation system by distillation system and is formed；
The distillation system includes quenched kettle 1, rectifying column 2, segregator 3, complete condenser 4 and product receiving slit 1, the tune
The discharge port of matter kettle is connected to the feed inlet of rectifying column, and segregator setting is at the top of the rectifying column in tower body, the complete condenser
Setting is in rectifying tower top, and the low boiling component for that will not condensed by segregator condenses, and bypass line is arranged in complete condenser discharge port,
A part of condensable product is set to enter product receiving slit one, a part flows back into rectifying column；
The infiltration evaporation film separation system include vaporizer 7, vapour liquid separator 6, reheater 8, infiltrating and vaporizing membrane group 9,
Permeate condenser 13, product condenser 11, product receiving slit 2 12 form；The feed inlet and product receiving slit of the vaporizer
Two are connected to product receiving slit one, and the discharge port of vaporizer is connected to the feed inlet of vapour liquid separator, and vapour liquid separator goes out
Material mouth is connected to the feed inlet of reheater, and the discharge port of reheater connects membrane module, and the infiltrating and vaporizing membrane group is seeped by 1~6 grade
Vaporization film unit is in series thoroughly, and every unit is made of 2-6 infiltration vaporization membrane module parallel connection, and every grade of infiltrating and vaporizing membrane is matched respectively
Permeate condenser and infiltration liquid bath 14 are set, the infiltration liquid bath is connected to distillation system rectifying column feed inlet or direct waste discharge,
The discharge port connection product condenser and product receiving slit of membrane module.
The rectifying column be packed tower, rectifying column use side entry feed, the top of tower body and middle part be respectively arranged one into
Material mouth, feed inlet are located at the overcentre of Liquid Distribution in Packed Columns, and the liquid distribution trough is by disk and is uniformly arranged on circle
Several tap holes on disk are constituted, and disc surfaces are provided with the groove of connection tap hole and disc centre point, and the path of groove is full
Each tap hole being equidistant to disc centre point of foot.The tap hole is cylindrical hole, and the top of each tap hole is arranged
Crown cap, the top cap shunt the support column support fixation in aperture by being arranged in, realize and keep gap between shunting aperture
Pass through for the vapour phase of rising.The filler of the rectifying column is the molding θ type filler of stainless steel cloth, triangle spring filler, glass
Ceramics or plastics material filler.The preheater of preheating material is provided on the rectifying column feeding line；The quenched kettle is band
The reaction kettle of stirring structure.Distillation system further includes the extraction/entrainer storage tank 15 for storing extractant or entrainer, and for
Into extractant or the feed pump 18 of entrainer in rectifying tower.The extraction/between entrainer storage tank and rectifying column feed inlet
Extraction/entrainer cooler 16 is provided on pipeline.The tower bottom of rectifying tower is using electricity, steam or heat-conducting oil heating mode.Institute
State the preheater 17 that preheating material is provided on rectifying column feeding line.
In the infiltration evaporation film separation system, the infiltration vaporization membrane module is by several infiltration evaporation membrane tubes, cylinders
Shape putamina and film partition are constituted, and the membrane tube is uniformly fixed in the fixed disk for being provided with multiple fixation holes, the fixed disk position
At the top of putamina, film partition one end is fixed in fixed disk, and the other end stretches to putamina bottom, by space in putamina and membrane tube
It is uniformly divided into the two parts communicated, in the infiltration evaporation film separation system, is cased with outside every infiltration evaporation membrane tube corrosion-resistant
The damping spring that the internal diameter of material (such as tetrafluoro material) production is φ 13, the effect of the spring are embodied in following two points,
One side spring increases the turbulance of medium in infiltration evaporation putamina, makes to expect more uniform in the distribution of putamina radial direction, to the greatest extent may be used
Avoid back-mixing to energy；On the other hand, because of the perturbation action of spring, keep the concentration polarization layer of infiltration evaporation film surface significantly thinning,
Substantially increase the mass transfer rate of material.Therefore, the flux of infiltrating and vaporizing membrane is substantially increased by damping setting and divided
From efficiency.
In the infiltration evaporation film separation system, last group of infiltration evaporation film unit of infiltration vaporization membrane module and product are cold
Counterbalance valve 10 is provided between condenser.Afterburner is provided between infiltration vaporization membrane module upper level and next stage seperation film.
Embodiment 2
Separation and recovery system described in the present embodiment, difference from example 1 is that:
(1) the putamina inner wall and film baffle surface are provided with multiple amortisseur bars, and the amortisseur bar is by mounting bar and interval
Certain distance is uniformly arranged on the composition of the damping block on mounting bar, and putamina inner wall is provided with and the matched installation of mounting bar size
Slot, the mounting bar are embedded in the fixation that damping block is realized in mounting groove.Preferably, resistant block is similar to contract type, and damping block is to putamina
Interior space downstream direction protrusion.The effect of resistant block is the resistance on raising steam flow direction, increases steam flow in putamina
Turbulent extent can also effectively reduce the influence of concentration polarization, also residence time of the raising steam in putamina, to effectively improve
The flux of infiltration vaporization membrane module, the quantity for reducing membrane module also just reduce the cost of investment of membrane module.
The separation of 3 acetonitrile-water of embodiment
Illustrate the operating method of small-sized solvent recovery unit by taking the acetonitrile waste liquid of polypeptide industry as an example.Polypeptide industry acetonitrile is useless
Liquid (mixed solvent) include about 10~15%wt. acetonitrile and 85~90%wt. water (this example with 15%wt. acetonitrile, 85%wt.'s
Water illustrates as example), additionally contain a small amount of high boiling substance.Mixed solvent is pumped, and with 100L/h, (mass flow is
Flow 90.73kg/h) continuously enters in rectifying column, and built-in condenser is used at the top of rectifying column, is followed according to tower top temperature control
The inlet amount of ring water, tower top temperature control are 88.4 DEG C, and pressure control is 0.15MPa, and overhead extraction gas phase mass flow is
17kg/h, acetonitrile quality group become 80.1%wt., and water quality group becomes 19.9%wt.；Tower reactor is controlled at 111.4 DEG C, even
Continuous extracted waste water, flow 73.73kg/h, the content of acetonitrile is not higher than 500ppm in waste water, furthermore some high boiling impurity
Liquid gives off this device with waste water, carries out subsequent processing.
The acetonitrile-water gas phase mixture of overhead extraction, into first order infiltrating and vaporizing membrane (area about 1.5m2), the first order
Vaporization film permeate side controls vacuum degree 10kPa thoroughly, and penetrating fluid is cold by the two-stage of water at low temperature (7 DEG C) and chilled water (- 20 DEG C)
Solidifying cooling is discharged into level-one penetrating fluid storage tank.Controlled at 88.4 DEG C, feed pressure is for the charging of infiltrating and vaporizing membrane
0.15MPa, after the centrifugation of level-one infiltrating and vaporizing membrane, the flow of permeate is 3.09kg/h, and wherein the content of acetonitrile is small
In 500ppm, the device is discharged as waste water in this permeate；By the quality group of acetonitrile in the material of first order infiltrating and vaporizing membrane
As 98.7%, flow 13.91kg/h.Acetonitrile-water mixed solvent seeps after afterburner is preheated to 100 DEG C into the second level
Vaporization film (area about 2.5m thoroughly2), second level infiltrating and vaporizing membrane permeate side controls vacuum degree 10kPa, and penetrating fluid passes through low temperature
The cooling of the condensed in two stages of water (7 DEG C) and chilled water (- 20 DEG C) is discharged into second level penetrating fluid storage tank, point through second level infiltrating and vaporizing membrane
After effect, the flow of permeate is 0.3kg/h, wherein the quality composition about 1% of acetonitrile, this permeate accumulation a period of time
Heel row enters penetrating fluid slot and further recycles acetonitrile；Quality group by acetonitrile in the material of second level infiltrating and vaporizing membrane becomes
99.99%, flow 13.61kg/h.The acetonitrile of high purity steam of acquisition enters acetonitrile product slot, acetonitrile after being condensed, being cooled down
Recycled in its entirety rate >=98%, acetonitrile after the recovery fully achieves reuse requirement.Ethane nitrile content≤0.1% in waste water, it is maximum
Degree reduces enterprise's dangerous waste yield, 10 tons -900 tons of annual recycling design amount.
The separation of embodiment 4THF- water
Illustrate the operating method of small-sized solvent recovery unit, THF by taking tetrahydrofuran (THF) waste liquid of certain pharmacy corporation as an example
Waste liquid includes that (for this example with 20%wt.THF, the water of 80%wt. is as example for about 20~25%wt.THF and 75~80%wt. water
Illustrate), additionally contain a small amount of high boiling substance and a small amount of insoluble impurities.THF waste liquid is wherein insoluble through filtering removal
It after impurity, is continuously entered in rectifying column through pumping with the flow of 100L/h (mass flow 98.78kg/h), is used at the top of rectifying column
Built-in condenser, according to the inlet amount of tower top temperature control loop water, tower top temperature control is 97.8 DEG C, and pressure control is
0.3MPa, overhead extraction gas phase mass flow are 22kg/h, and THF quality group becomes 89.81%wt., and water quality group becomes
10.19%wt.；Tower reactor is controlled at 133.6 DEG C, continuous extracted waste water, flow 76.79kg/h, the content of THF in waste water
Not higher than 500ppm, in addition, some high boiling impurity also give off this device with waste water, subsequent processing is carried out.Tower top
The THF- aqueous vapor phase mixture of extraction, into first order infiltrating and vaporizing membrane (area about 1.0m2), the first order vaporizes film permeate thoroughly
Side controls vacuum degree 10kPa, and penetrating fluid is discharged into level-one by the cooling of the condensed in two stages of water at low temperature (7 DEG C) and chilled water (- 20 DEG C)
In penetrating fluid storage tank, the charging of infiltrating and vaporizing membrane is controlled at 97.8 DEG C, feed pressure 0.3MPa, through level-one infiltration evaporation
After the centrifugation of film, the flow of permeate is 1.79kg/h, and wherein the content of THF is less than 500ppm, this permeate is as useless
The device is discharged in water；Become 97.78% by the quality group of THF in the material of first order infiltrating and vaporizing membrane, flow is
20.21kg/h.THF- water mixed solvent is after afterburner is preheated to 100 DEG C, and into second level infiltrating and vaporizing membrane, (area is about
2.0m2), second level infiltrating and vaporizing membrane permeate side controls vacuum degree 10kPa, and penetrating fluid passes through water at low temperature (7 DEG C) and chilled water
The condensed in two stages cooling of (- 20 DEG C) is discharged into second level penetrating fluid storage tank, after the centrifugation of second level infiltrating and vaporizing membrane, permeate
Flow be 0.45kg/h, wherein THF quality composition about 1%, this permeate accumulation a period of time heel row enter penetrating fluid slot
Further recycle THF；Become 99.99% by the quality group of THF in the material of second level infiltrating and vaporizing membrane, flow is
19.75kg/h.The high-purity THF steam of acquisition enters product slot after being condensed, being cooled down, recycled in its entirety rate >=98% of THF returns
THF after receipts fully achieves reuse requirement.
The separation of 5 acetone-methanol of embodiment
Illustrate the operating method of small-sized solvent recovery unit by taking the acetone-methanol waste liquid of certain pharmacy corporation as an example, the waste liquid
Comprising about 25~30%wt. acetone and 70~75%wt. water, (for this example with 25%wt. acetone, the methanol of 75%wt. is as example
Illustrate), additionally contain a small amount of insoluble impurities.Acetone-methanol waste liquid first passes around elimination except after wherein insoluble impurities, warp
Pump is continuously entered in rectifying column with the flow of 100L/h (mass flow 79.4kg/h), and built-in condensation is used at the top of rectifying column
Device, according to the inlet amount of tower top temperature control loop water, since the boiling point of methanol and acetone is closer to, so distillation process need to add
Enter water as extractant, carries out extracting rectifying, the inlet amount control of extractant water is 60L/h, from the upper feed inlet of rectifying column
Charging.The control of rectifying tower top temperature is 89.3 DEG C, and pressure control is 0.3MPa, and overhead extraction gas phase mass flow is 20kg/h,
Acetone quality group becomes 94.2%wt., and water quality group becomes 5.8%wt., and the content of methanol is not more than 500ppm；Tower reactor control
Temperature is 105.8 DEG C, continuous recovered water, methanol and acetone, flow 109.13kg/h, water-methanol-acetone in tower reactor discharging
Quality group is at respectively 44.48%-54.54%-0.93%, and furthermore some high boiling impurity also give off this with waste water
Device carries out subsequent processing.The acetone-water gas phase mixture of overhead extraction, into first order infiltrating and vaporizing membrane, (area is about
1.0m2), the first order vaporizes film permeate side control vacuum degree 10kPa thoroughly, penetrating fluid by water at low temperature (7 DEG C) and chilled water (-
20 DEG C) condensed in two stages cooling be discharged into level-one penetrating fluid storage tank, the charging of infiltrating and vaporizing membrane controlled at 89.3 DEG C, charging
Pressure is 0.3MPa, after the centrifugation of level-one infiltrating and vaporizing membrane, the flow of permeate is 0.93kg/h, and wherein acetone contains
Amount is less than 500ppm, and the device is discharged as waste water in this permeate；By the quality of THF in the material of first order infiltrating and vaporizing membrane
Group becomes 98.78%, flow 19.07kg/h.Acetone-water mixed solvent is after afterburner is preheated to 100 DEG C, into the second level
Infiltrating and vaporizing membrane (area about 2.0m2), second level infiltrating and vaporizing membrane permeate side controls vacuum degree 10kPa, and penetrating fluid is through too low
The cooling of the condensed in two stages of warm water (7 DEG C) and chilled water (- 20 DEG C) is discharged into second level penetrating fluid storage tank, through second level infiltrating and vaporizing membrane
After centrifugation, the flow of permeate is 0.23kg/h, wherein the quality composition about 1% of acetone, this permeate accumulates one section
Time heel row enters penetrating fluid slot and further recycles acetone；Quality group by acetone in the material of second level infiltrating and vaporizing membrane becomes
99.99%, flow 18.84kg/h.The high-purity acetone steam of acquisition condensed, cooled down after enter product slot, acetone it is whole
The body rate of recovery is about 95%, and acetone after the recovery fully achieves reuse requirement.
Claims (10)
1. aqueous organic liquid waste and organic solvent separation and recovery system, which is characterized in that by distillation system and infiltrating and vaporizing membrane point
It is connected and is formed by process pipelines from system；
The distillation system includes quenched kettle, rectifying column, segregator, complete condenser and product receiving slit one, and the quenched kettle goes out
Material mouth is connected to the feed inlet of rectifying column, and at the top of the rectifying column in tower body, the complete condenser is arranged in essence for segregator setting
Tower top is evaporated, the low boiling component for that will not condensed by segregator condenses, and bypass line is arranged in complete condenser discharge port, makes a part
Condensable product enters product receiving slit one, and a part flows back into rectifying column；
The infiltration evaporation film separation system includes vaporizer, vapour liquid separator, reheater, infiltrating and vaporizing membrane group, infiltration liquid cooling
Condenser, product condenser, product receiving slit two form；The feed inlet and product receiving slit two of the vaporizer are received with product
Slot one is connected to, and the discharge port of vaporizer is connected to the feed inlet of vapour liquid separator, the discharge port of vapour liquid separator and reheater
The discharge port of feed inlet connection, reheater connects membrane module, and the infiltrating and vaporizing membrane group is by 1~6 grade of infiltration evaporation film unit
In series, every unit is in series or in parallel to form by 2-6 infiltration vaporization membrane module, and infiltration is respectively configured in every grade of infiltrating and vaporizing membrane
Transparent liquid condenser and infiltration liquid bath, the infiltration liquid bath is connected to distillation system rectifying column feed inlet or direct waste discharge, membrane module
Discharge port connection product condenser and product receiving slit.
2. the separation and recovery system according to claim 1, which is characterized in that the rectifying column is packed tower, essence
Tower is evaporated using side entry feed, one feed inlet is respectively set at the top of tower body and middle part, feed inlet is located at packed tower liquid
The overcentre of distributor, the liquid distribution trough are made of disk and several tap holes being uniformly arranged on disk, disk
Surface is provided with the groove of connection tap hole and disc centre point, and the path of groove meets each tap hole to disc centre point
It is equidistant.
3. the separation and recovery system according to claim 2, which is characterized in that the tap hole is cylindrical hole,
Crown cap is arranged in the top of each tap hole, and the top cap, which passes through, is arranged in the support column support fixation for shunting aperture,
Realizing and shunt between aperture keeps gap to pass through for the vapour phase of rising.
4. any one of -3 separation and recovery system according to claim 1, which is characterized in that the infiltration evaporation film separation system
In, the infiltration vaporization membrane module is made of several infiltration evaporation membrane tubes, cylindrical putamina and film partition, and the membrane tube is uniform
It is fixed in the fixed disk for being provided with multiple fixation holes, the fixed disk is located at the top of putamina, and film partition one end is fixed on
In fixed disk, the other end stretches to putamina bottom, and space in putamina and membrane tube be uniformly divided into the two parts communicated, outside the membrane tube
It is cased with the damping spring of corrosion-resistant material production.
5. the separation and recovery system according to claim 3, which is characterized in that in the infiltration evaporation film separation system, seep
Counterbalance valve is provided between saturating last group of infiltration evaporation film unit of vaporization membrane module and product condenser.
6. the separation and recovery system according to claim 3, which is characterized in that infiltration vaporization membrane module upper level and next stage
Afterburner is provided between seperation film.
7. the separation and recovery system according to claim 2, which is characterized in that the filler of the rectifying column is stainless steel cloth
Molding θ type filler, triangle spring filler, glass ceramics or plastic material filler.
8. the separation and recovery system according to claim 2, which is characterized in that be provided on the rectifying column feeding line pre-
The preheater of thermal material；The quenched kettle is the reaction kettle with stirring structure.
9. the separation and recovery system according to claim 2, which is characterized in that distillation system further includes storing extractant or total
Boil agent extraction/entrainer storage tank, and for into rectifying tower into extractant or the feed pump of entrainer.
10. the separation and recovery system according to claim 2, which is characterized in that the vaporizer, reheater are that heating is set
It is standby, it allows the liquid to be vaporized into steam, carries out lock out operation to enter infiltration vaporization membrane module.
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