EP0968036A1 - Dispositif pour la separation de substances par adsorption au moyen de membranes adsorbantes - Google Patents

Dispositif pour la separation de substances par adsorption au moyen de membranes adsorbantes

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Publication number
EP0968036A1
EP0968036A1 EP98914881A EP98914881A EP0968036A1 EP 0968036 A1 EP0968036 A1 EP 0968036A1 EP 98914881 A EP98914881 A EP 98914881A EP 98914881 A EP98914881 A EP 98914881A EP 0968036 A1 EP0968036 A1 EP 0968036A1
Authority
EP
European Patent Office
Prior art keywords
adsorber
filter stage
adsorption
adsorber module
core
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP98914881A
Other languages
German (de)
English (en)
Inventor
Dietmar Nussbaumer
Khuong To Vinh
Abdul Weiss
Wolfgang Demmer
Hans-Heinrich Hoerl
Andreas Graus
Günter Pradel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sartorius AG
Original Assignee
Sartorius AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sartorius AG filed Critical Sartorius AG
Publication of EP0968036A1 publication Critical patent/EP0968036A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07K—PEPTIDES
    • C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
    • C07K14/795—Porphyrin- or corrin-ring-containing peptides
    • C07K14/805—Haemoglobins; Myoglobins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/60—Construction of the column

Definitions

  • the invention relates to devices for adsorptive separations by means of permeation of liquids through porous adsorption membranes and uses of the devices for carrying out adsorptive separations
  • the device can be used for the selective separation and purification of substances, such as, for example, bio-specific molecules, proteins, enzymes, ionogenic substances, metal ions, in particular heavy metal ions from different media.
  • substances such as, for example, bio-specific molecules, proteins, enzymes, ionogenic substances, metal ions, in particular heavy metal ions from different media.
  • the invention allows the device to be used for work in the laboratory, in the technical center and in the Production. Due to their structure, work for scale adjustment is possible both in scale-up and in scale-down.
  • Devices according to the invention can be used in the fields of biotechnology, genetic engineering, pharmacy, chemistry, the beverage and food industry and environmental protection
  • Adsorptive material separation is understood to mean a specific separation or purification of substances (components) from a liquid phase (medium) which are specifically adsorbed by a solid adsorbent.
  • a medium to be filtered which contains the substances to be separated or cleaned, is placed on the adsorbent or pressed through it and separated by means of one or more elution liquids (eluents) which are pressed through the adsorbent under pressure, depending on the extent of the interaction of the components of the medium with the adsorbent and the elution liquids, the individual components of the adsorbent are held to different extents and come out fractionally from the adsorbent.
  • elution liquids eluents
  • the substances to be separated contained in the medium can be adsorbed on the adsorbent either alone or together.
  • the medium with the mixture of substances to be separated is filtered, for example, through the adsorber module until the Desired substance appears at the outlet of the module
  • suitable elution liquids which are filtered through the module, for example, it can be eluted separately from other substances held on the adsorbent (step elution).
  • an undesired substance can also be separated from the medium
  • chromatography in which only a part of the adsorption capacity of the adsorber is used for adsorption and the separation of the adsorbed components is based on the fact that different volumes of the eluent are required for the elution, although not expressly related to the chromatography below is used as an application in the scope of the invention
  • Non-particulate matrices with continuous pore structures such as porous membranes, offer the possibility of predominantly convective mass transfer under the influence of a pressure difference and thus to one effective elimination of the undesired diffusion limitation.
  • Adsorption membranes are to be understood as meaning membranes which, on their inner and outer surfaces, carry functional groups ligands or reactants which are capable of interacting with at least one substance in a liquid phase in contact with it
  • adsorption membrane is to be understood as a generic term for different types of adsorption membranes, such as cation, anion, ligand, affinity or activated membranes, which in turn are divided into different adsorption membrane types depending on the functional groups, ligands or reactants
  • Adsorption membranes are membranes whose average pore diameter is in the microfiltration range and is between approximately 0.1 ⁇ m to approximately 15 ⁇ m. The thickness of the porous adsorption membranes used is between approximately 100 ⁇ m and approximately 500 ⁇ m
  • DE-OS 44 32 628 and US Pat. Nos. 5,575,910 and 4,895,806 disclose devices and methods for carrying out adsorptive substance separations by means of permeation of liquids through porous adsorption membranes, in which the adsorption membranes are subjected to axial or radial flow in pressure filtration devices to increase the adsorption capacity
  • Adsorption modules from a large number of flat blanks of porous adsorption membranes used in stack form The proposed solutions have the disadvantage that a relatively high waste of valuable adsorption membranes occurs in the production of the flat blanks, which are known to be highly refined and cost-intensive products.
  • the number of blanks is increased porous adsorption membranes through which the medium to be filtered flows as a stack, with a reduction in the flow rate and a relatively rapid blocking of the upper layers of the blanks of the A adsorption membranes connected
  • the solution further has the disadvantage that the flow rate decreases rapidly and the service life is relatively short due to membrane fouling and membrane defects
  • the wrap used according to US Pat. No. 4,986,909 is also flowed through from the outside in.
  • its web material does not consist of adsorption membranes, but of a flat structure made of fibers.
  • the known devices which use a roll consisting of a web material for adsorptive material separation, also have the disadvantage that they have a rigid configuration which does not allow flexible adaptation to the separation tasks to be performed
  • the invention is therefore based on the object of providing an apparatus equipped with an adsorber module for carrying out adsorptive material separations by means of permeation of liquids through porous adsorption membranes, which is constructed in such a way that it is characterized by a small dead volume, an optimal apparatus volume with the largest possible binding capacity, a good flow rate and long service life as well as a high flexibility to adapt to the separation tasks to be solved and to propose uses of the devices for carrying out adsorptive material separations
  • a device made of a jacket tube, which is connected to a base and a cover element to form a cylindrical housing with liquid inlets and outlets, which has at least one hollow cylindrical adsorber module with at least one winding made of at least one turn of an adsorption membrane and accommodates with a cylindrical core arranged concentrically therein.
  • the at least one adsorber module is enclosed between the base and the cover element to form at least one liquid inlet and at least one liquid outlet space in such a way that the liquids permeate from the liquid inlet to the liquid outlet As intended, pass through the porous adsorption membranes of the adsorber module.
  • the hollow cylindrical adsorber module is dimensioned so that an inner and an outer annular gap is formed between its inner surface and the cylindrical core and between its outer surface and the jacket tube.
  • the connection for the liquid supply through radial bores in the Core connected to the inner annular gap and the connection for the liquid discharge through radial channels in the base element with the outer annular gap
  • the adsorption membranes suffer due to their high pore volume Compression is a reduction in its thickness, which is accompanied by a reduction in its flow rate.
  • the reduction in thickness has another, much more serious consequence than the reduction in flow.
  • the first perfused layers of the adsorption membranes are particularly exposed to the blockage by 'particulate contaminants of the medium to be filtered as well as by fouling effects.
  • the total working pressure is not only for compressing the innermost, practically all turns are effective.
  • the flow from the inside to the outside avoids the disadvantageous compression effects described. If, in extreme cases, the innermost turn is blocked, it is subjected to tensile stress, with the result that the web material is stretched and not compressed, which prevents wrinkling.
  • an adsorption membrane coil when subjected to pressure from the outside or from the inside is comparable to that of a hose, which collapses in the former case, while in the other case it does not undergo any significant dimensional changes.
  • the use of an annular gap instead of a porous tube on the inside of the hollow cylindrical adsorber module and an annular gap on the outside means that the dead volume can be kept small.
  • the annular gaps are kept open continuously by spacers, which at the same time have support functions for the adsorber module. All materials customary for the person skilled in the art for the construction of permeation modules can be used as spacers.
  • the spacers are formed by grooves which are located on the surface of the cylindrical core and on the inner peripheral surface of the casing tube.
  • the grooves can have a different shape and a different course. For example, they can have a helical design.
  • the optimal annular gap is dimensioned in such a way that the disadvantageous phenomena caused by undersizing and oversizing are avoided.
  • the optimal gap width depends on the specific flow rate of the adsorption membrane, the thickness of the adsorption membrane, the ratio of the inner to the outer diameter of the adsorber membrane formed hollow cylinder and the length of the adsorber module
  • dimensionless resistance parameter A which enables mathematical relationships between the geometic and hydraulic conditions of the device according to the invention with their quality-determining properties to be established and which is defined as follows in the case of a radially flowed through membrane winding:
  • R 2 outer radius of the adsorber hollow cylinder [cm]
  • k width of the outer annular gap [cm]
  • A is derived from the flow conditions in a device according to the invention under simplifying assumptions (validity of Hagen-Poiseuille's law in the annular gap, linear relationship between pressure difference and flow through the membranes, neglecting the dynamic pressure). Neglecting the different flow resistances in the inner and outer annular gap, the local static pressure in the annular gaps and the local static pressure difference can be determined. The following are important for the operation of an adsorber: the mean pressure difference ⁇ P m , which determines the achievable filtration capacity the maximum pressure difference that determines the beginning of the breakthrough of the target substance and thus the loss-free capacity utilization K n of the adsorber
  • ⁇ P P ⁇ A) m ° A (cosh (A) + A s ⁇ n (A))
  • the gap widths of the annular gaps are chosen so that the outer and the inner annular gap have the same volume. Therefore, the outer has a smaller gap width and thus a higher flow resistance than the inner one and is used for the assessment of the pressure drop
  • devices according to the invention can also be produced in which the adsorption membrane is firmly connected to the housing (disposables), the focus is in the field of technical units for the process scale.
  • the re-equipment of a device or of systems with such devices is also included
  • Adsorption membranes with the least possible Combined use of materials According to the invention, this is achieved in that the device is made up of only the five basic components casing tube, base element, cover element, adsorber module and core.
  • auxiliary components which are described in detail below.
  • An essential aspect of the invention is therefore that for different adsorber modules, i.e.
  • adsorber modules with different numbers of turns have different core diameters, but they can be used in the same housings the dimensions of the connecting piece between the cover element and the core are the same for all modules regardless of the number of turns
  • a preferred embodiment of the present invention offers the possibility of complete scale-up and scale-down via one It is essential that the test results obtained with small units can be directly transferred to scale-up.
  • This is based on a so-called unit module, the length of which suitably corresponds to the manufacturing range of the adsorption membrane.
  • the scale-up principle is the parallel connection of unit modules, namely both within a common housing as well as in several housings, the scale-down principle is the shortening of unit modules
  • a further advantage of embodiment I is that the housing according to this construction can be produced equally easily from metallic materials and from machinable plastics and, moreover, the components made from different materials can be freely combined with one another. down to use the same material as for scale-up.
  • a robust construction material such as For example, if stainless steel is to be preferred, it is advantageous for preliminary tests on a laboratory scale to be able to use inexpensive, lightweight plastic units.
  • transparent materials such as glass or plexiglass in test devices, even if neither the target substance nor contaminants to be bound have their own color , the visual assessment of the chromatographic process can provide decisive conclusions.
  • Embodiment II takes account of these aspects.
  • Embodiments I and II differ primarily in that in embodiment I the mechanical connection between the base and the cover element and the absorption of the axial sealing forces by the jacket tube takes place, while in embodiment II the mechanical tasks are taken over by the core and the task of the jacket tube is reduced to collecting the permeate.
  • the aforementioned transparent materials which are available in suitable tubes, can also be used for the jacket tube.
  • the adsorber module is identical for both embodiments
  • Embodiments I and II correspond in terms of flow control to what the term “dead end filtration” has become common for filtration, ie the entire medium to be treated flows through the adsorbent and is removed as permeate from the device.
  • it is also possible to implement the so-called "cross flow” operation i.e. only a part of the medium supplied flows through the adsorbent and accumulates as permeate, while another is discharged again at the end of the inner ring channel as a so-called retentate.
  • This procedure is advantageous according to the invention if that Medium contains particular contaminants, Permeate and retentate can either be removed separately from the device or back-mixed before removal. In the latter case, there is the additional advantage that the high particle concentration, which in extreme cases leads to a pasty consistency and the associated difficulties, no longer than is absolutely necessary to be maintained
  • a device of the latter type is represented by embodiment III, in which the permeate is mixed back with the particle concentrate within the device, the quantity ratio of the amount of liquid to be permeated to be overflowing being regulated by means of a needle valve-like construction.
  • a particle suspension containing the target substance is thus supplied and applied Particle suspension depleted of target substance removed
  • the focus is on removing a target substance from a medium and obtaining it in the form of a highly concentrated eluate, for which minimizing the dead volume is an important prerequisite .
  • the concentration of the eluate is of little or no importance, for example in the removal of contaminants such as pyrogens, DNA fragments or disruptive enzymes (e.g. proteases)
  • the medium is supplied from below through the hollow core.
  • the flow in the annular gaps is similar to that of the other preferred embodiments.
  • the permeate is discharged via a separate connecting piece in the base plate.
  • the sealing points are dimensioned so that the same modules as for the other embodiments can be used
  • a special flow design is provided when the medium is deflected from the hollow core into the inner ring channel, abrupt changes in direction are avoided and the entry into the ring channel is as flat as possible Angle
  • a lower limit of the number of turns of 5 is preferred, an upper limit of 150.
  • the upper limit of the outer cylinder diameter is preferably 200 mm, the lower limit, for example in laboratory units, 5 mm.
  • the preferred ratio of inner to outer cylinder diameter can also be fluctuate within wide limits, namely between 0.25 and 0.95 If extreme dimensions can also prove to be expedient in individual cases, it is possible within the scope of the invention to cover a broad spectrum of applications for the process area with a minimum of technical outlay is achieved by a modular system, in which the individual components are largely interchangeable, and a series of adsorber modules, the number of turns of which are graded approximately in a ratio of 1 2
  • adsorber modules with 8, 15, 30 and 60 turns can be used in uniform Housings of 10 0 mm inner diameter of the jacket tube can be created
  • the exemplary addition does not represent a limitation of the invention
  • the hollow cylindrical adsorber module consists of a
  • end caps made of plastic are attached to the open ends of the hollow cylindrical adsorber module and extend transversely thereto.They embed the end faces of the adsorber module in a fluid-tight manner in a casting compound made of plastic, at least one of the end caps being annular, preferably both end caps being annular
  • the support elements located on the outer surfaces are permeable to fluids.They not only have the task of protecting the membrane against hydraulic pressure differences, but also give the adsorber module the rigidity required for handling, e.g. when inserting it into the housing Cylinder fabrication is also used.
  • the outer support element which supports the membrane against the internal pressure under operating conditions, does not need to be designed for the full hydraulic pressure difference occurring, because this is largely absorbed by the individual turns of the membrane Support element has no pressure stress at all under operating conditions and could therefore be omitted in principle. In practical operation, however, it proves to be expedient to start a rewinding step at low pressure when the inner winding begins to become blocked In this case, the inner support element prevents the membrane roll from collapsing.
  • the support elements are preferably at both ends somewhat longer than the width of the adsorption membrane web from which the roll is made (preferably about 2 to 10 mm), so that they are in the sealing compound
  • the materials used for the support elements are both plastics (e.g. polypropylene, polyester, polyamides, polyurethanes) and metals (e.g. corrosion-resistant stainless steel, especially those with high chloride resistance)
  • a non-metallic spacer element is preferably additionally used between the adsorption membrane and the support element, for example a plastic fabric, in order to ensure direct contact to avoid between membrane and metal
  • This spacer element can also be used in several layers in order to increase the wall thickness of the resulting hollow cylinder, which is desirable particularly in the case of small numbers of turns in the interest of better manageability to be able to use the same end caps as for 15 windings.
  • Semi-finished products fabric, fleeces, perforated plates, perforated foils
  • wire sizes between 0 , 2 and 0.5 mm preferred for mesh sizes between 0.3 and 1 mm
  • wire thicknesses between 0.5 and 1 mm for mesh sizes between 1 and 2 mm are preferred.
  • the preferred thickness range is between 0. 2 and 1 mm
  • the potting compound has the opening gabe to seal the ends of the adsorption membrane wrap and connect support elements, adsorption membranes and end caps to each other For reliable sealing, it is necessary that the potting compound in liquid form under pressure comes into contact with the end faces of the adsorption membrane wrap.
  • the manufacture and casting of the wrap is carried out using a Winding device and a pouring device
  • the winding device consists of the winding core and two side cheeks A and B.
  • the outer diameter of side cheek A corresponds to the inner diameter of the outer support element, while side cheek B is only turned to the length of the protruding part of the outer support element, so that there is still one
  • the inner support element is attached to the winding core, then the side cheeks. These are turned out inside to accommodate the protruding part of the support element.
  • the outer part of the side cheeks limits d The position that the edges of the adsorption membrane wrap should take. After tightly winding the adsorption membrane, the end of the web is usually glued to the wrap, for example by dot or line application of the liquid casting compound. Now the outer support element is opened over side wall A until it stops Side panel B pushed on
  • the winding can be poured in either in one operation with the application of the end caps or with the aid of a removable mold, the end caps to be attached later
  • the first way is preferred, but it requires a more complex construction of the winding and pouring device.
  • both hard casting resins such as polyurethane resins, epoxy resins and, particularly preferably, silicone rubber, and thermoplastics such as polypropylene are essential for the casting process is that the liquid casting compound is brought up from below to the vertical winding and, as soon as it comes into contact with the edge of the winding, recognizable by the emergence over the edge, the lifting is interrupted or continued so slowly that there is no significant leakage of casting compound This ensures that the potting compound not only fills the space up to the adsorption membrane wrap without bubbles, but also occurs between the membrane edges and into the membrane pores.
  • the end caps create the sealing connection between the adsorption membrane winding and the core.
  • the sealing of the inner ring channel is explained in more detail in connection with the construction of the core.
  • the upper end cap preferably has a web on its inside which fits into a corresponding recess in the core. This web serves on the one hand the exact positioning of the module on the stop, it also transfers the weight of the module to the core.This is particularly important if, as is possible with embodiment I of the invention, several adsorber modules are arranged one above the other in a housing. In this case, otherwise The weight of all adsorber modules act on the lowest, which entails the risk of compression of the inner and outer support elements.
  • the upper end cap also has a groove on the outside for receiving a sealing element (e.g.
  • the purpose of this seal is not to separate the medium and permeate, because di ese occurs between the inner surfaces of the end caps and the core.
  • the seal at this point rather prevents permeate, eluate or cleaning agent from penetrating into the gap between the end cap and cover element (or between two end caps in the case of several modules) and can lead to contamination
  • the end caps can also be molded in one step by pouring the membrane from the potting compound. If an elastic, self-sealing material such as silicone rubber is used, the sealing elements between the module and the core can be omitted, as can be seen by the person skilled in the art If separate components are attached, they expediently have undercuts which serve for the additional mechanical anchoring of the casting compound in the end cap. This is particularly the case with casting compounds which, like the silicone resins preferred for pharmaceutical applications, have no liability with the cap material
  • adsorption membranes with different adsorption properties are accommodated in the same adsorber module.This is expedient for applications when, for example, several target substances or contaminants are to be bound at the same time.
  • adsorption membranes with the same adsorption properties but different porosities are combined in one adsorber module.A reason for this is that the more favorable breakthrough characteristics of fine-pored adsorption membranes are used and the disadvantage of their lower flow rate should be minimized In this case a A coarse-pored adsorption membrane is arranged on the upstream side and a fine-pored adsorption membrane on the downstream side
  • Another reason for using different membrane porosities may be that the flow rate of the adsorber modules should be standardized.
  • the uniformity of the flow rate is of particular importance, especially when several adsorption modules are connected in parallel. This aspect distinguishes the requirements for adsorption modules from those for conventional filtration modules. For example, when connecting sterile filtration units in parallel, a particularly high flow rate of a single unit can only have a positive effect on the performance of the overall system.
  • a safety filter is arranged on the inside of the hollow cylinder of the adsorber module.
  • the safety filter is preferably designed as an exchangeable, cylindrically shaped safety filter.
  • the material used is a fine-pored microfiltration membrane, but preferably the adsorption membrane from which the adsorber module is also built under operating conditions , under which an irreversible blocking of the adsorption membrane can occur, is generally practically only the membrane system through which the flow first flows. For this reason, it is generally preferred to place a single layer of the adsorption membrane in front of the device according to the invention, which is easy to replace.
  • an adsorber module is rendered unusable by irreversible blocking of the inner turn.
  • This can also be done by the fact that the aforementioned prefiltration takes place, but contaminants arise behind the prefilter in the pipe system, for example by coagulation or corrosion processes.
  • the use of the aforementioned safety filter in the adsorber module itself is preferred according to the invention.
  • the same adsorption properties as that should preferably be used have used adsorber material because the coagulation or corrosion products mentioned can be of a type that they cannot be retained by inert filter material.
  • the safety filter consisting of the adsorptive filter material is preferably designed as a membrane tube, which is produced by welding or gluing the adsorption membrane. Its diameter is adapted to the inner diameter of the inner support element and is loosely inserted into the hollow cylinder, so that it is pressed against it by the operating pressure. A special seal at the ends is not absolutely necessary.
  • the advantage of the safety filter is that the amount of work associated with its replacement is so low that it bears no relation to the damage that an adsorber module that has become unusable would represent
  • the outer diameter of the core together with the inner diameter of the adsorber module determines the height of the inner annular gap. It generally fulfills the tasks of positioning the adsorber module (s) in the housing, displacing the volume to reduce the dead volume and distributing the supplied medium in the annular gap. In the embodiment II there is the additional task of mechanically connecting the base and cover elements and absorbing the axial sealing forces. In embodiment I, as long as there are further parallel adsorber modules behind it, the medium is added to the adsorber modules located behind it conduct.
  • two different designs of the core can thus be distinguished, depending on whether there are further adsorber modules behind them or not.
  • it has channels as an extension core at both ends, for example in the form of bores, for passage of the medium , in the latter case only at the top
  • the core can be made both from solid material and also for Fluid-impermeable hollow bodies are made.
  • the materials from which the end caps can also be made are suitable, namely, for example, polyacetals, polypropylene and polyamides. Polyacetals are preferred
  • the general task of the jacket tube is to collect the permeate in the Embodiment I add the mechanical connection of the base and cover element and the absorption of the axial sealing forces
  • casing pipes with clamp connections (clamp connections) and O-ring seals or flange connections with the base and cover element are preferably used.
  • the connection is mechanical contact between the casing tube and the base or cover element to geometrically defined conditions to ensure clamp connections with flat seals, in which an uneven compression of the seal can occur, are not suitable.
  • the modular system of embodiment I makes it possible in a simple manner to upgrade existing casing pipes by using extension pieces for a larger number of modules
  • a largely rotationally symmetrical discharge of the liquid to the axially arranged line connection is effected through the base element via approximately 3 to 8 bores
  • the cover element also preferably has an axial clamping connection and, in the preferred embodiments, a ventilation opening for the outer annular gap
  • any suitable fitting e.g. a simple vent screw
  • the use of a screw-in non-return valve with or without spring loading is preferred, with the sealing element being arranged directly in a corresponding hole in the cover element Locking device attached When this is opened, the outer annular gap is vented by the overpressure prevailing in the device.
  • the advantage of the check valve is on the one hand that the seal is made directly in the cover element and a dead space that can lead to contamination is avoided. On the other hand, it is this also makes it possible to vent several modules connected in parallel, in which the discharge valves of the non-return valves are connected to one another, via a common valve.
  • the object of the invention is achieved by using the devices according to the invention, in which the winding-shaped adsorber module of the device according to the invention is flowed through radially from the inside outwards with the medium under the action of a pressure difference.
  • the device is preferably operated with a vertical cylinder axis
  • the eluate which has a high density due to a high concentration of desorbed target substance and a high content of the eluent in electrolytes, can flow more easily downwards of the medium to be filtered and the permeate removed preferably at opposite ends of the device.
  • a venting device located in the cover unit, for example in the form of a venting screw but also possible to design the device so that the supply of the medium in the inner ring channel
  • the ventilation opening in the cover unit is connected to the inner ring channel
  • the invention also makes it possible to use the adsorber modules and devices according to the invention for the construction of plants for adsorptive material separations which are distinguished by a high degree of flexibility.
  • possibilities for parallel connection of the inventive adsorber modules or devices are created in two ways, namely by connecting several individual modules in parallel in a jacket tube or by connecting several jacket tubes equipped in the same way
  • n adsorber modules with 60 turns on adsorption membranes are connected in parallel in the first stage, in the second Stage n / 2 modules with 30 turns and in a third stage n / 4 modules with 15 turns, the pressure drop is approximately the same in all three stages and the binding capacity of the following stages is a quarter of the previous one in that the result is a gradual breakthrough of the mentioned irregularities that have penetrated through the following stage, the dynamic capacity (that is, the binding capacity that can be used up to a certain concentration of target substance in the permeate) can be significantly increased.
  • the particular advantage of the mentioned gradation is that the pressure drop is evenly distributed over the individual stages and therefore all stages can be loaded up to the maximum permissible pressure drop In the gradation of the individual components described, the last stage contributes only a relatively small proportion to the overall capacity of the system, which is advantageous for the overall usable proportion of the total capacity.
  • the unusable capacity is 20% of the installed capacity
  • the second stage has 20% of the total capacity
  • the first stage is 100%
  • the second stage 80% usable so that of the total installed Only 4% of the capacity is unusable
  • the unusable portion is reduced to 1% (77.1% of the total capacity in the first, 19.1% in the second and 4.8% in the last stage) the 20% cannot be used
  • a particularly preferred form of the series connection is referred to here as a tandem system.
  • the principle is based on the fact that the breakthrough of the target substance in an adsorber only occurs in the last phase of the loading and the series connection therefore only brings advantages.
  • two identical stages A and B used, cyclically either one being loaded and the other being eluted or regenerated, or both being operated in series. The sequence is as follows. Stage A is loaded with the medium.
  • stage A Before the target substance breaks through in the permeate, it is freshly cleaned Regenerated stage B switched As soon as stage A is fully loaded, the remaining medium is rinsed with buffer from stage A at stage B and then the pre-loaded stage B is directly loaded with medium, while stage A is eluted, which means that the initial state is reached again with exchanged stages
  • Stage A When controlled by a process computer Very short cycle times and thus very high plant productivity can be achieved in this way, in particular using the device according to the invention with adsorption membranes.Short cycle times are understood here to be 15 minutes and less, whereas conventional chromatography columns are usually used for several hours Such a system uses a variety of shut-off and
  • Liquid contaminated by the previous MarcValve Corporation (Tewksbury, Massachusetts) has launched a system of diaphragm valves that combine a variety of functions in a single assembly (up to 6 ports with one outlet, by pass valves and valves for Flow reversal) and which have a negligible dead volume
  • This or equivalent Liquid contaminated by the previous MarcValve Corporation (Tewksbury, Massachusetts) has launched a system of diaphragm valves that combine a variety of functions in a single assembly (up to 6 ports with one outlet, by pass valves and valves for Flow reversal) and which have a negligible dead volume
  • Fittings are particularly preferably used according to the invention.
  • FIG. 1 schematically shows a vertical section through a device according to the invention in embodiment I
  • Fig. 2 schematically shows a vertical section through a connector for the
  • FIG. 3 schematically shows a vertical section through a device according to the invention in embodiment I with two in one
  • Fig. 6 schematically shows a vertical section through an inventive
  • ig 8 schematically shows the external structure in the three-stage Se ⁇ enscnies of devices according to the embodiment II, ig 9a to b to scale a vertical section and a floor plan of a
  • Adsorber stage consisting of four devices according to embodiment I (dimensions in mm), ig 10a to b, connected in parallel in four individual tubes, ig 10a to b a vertical section and plan view of a three-stage
  • Adsorber system consisting of 12 modules in four individual tubes in the first stage, 6 modules in 2 individual tubes in the second stage and 3 modules in a single tube in the third stage according to embodiment I (dimensions in mm), ig 1 1 schematically a vertical section through one according to the invention
  • ig 12 schematically shows a vertical section through an inventive
  • ig 13a to c the schematic representations of a flow diagram of a tandem system according to the invention and ig 14a to c graphically the relationships between the dimensionless
  • a base element 7 is screwed onto a mounting thread 24 with a
  • Adsorber module 45 is plugged onto core 15 from above in such a way that a web 27 of an upper end cap 5 comes into abutment against core 15.
  • the elements designated by reference numerals 28-31 represent connecting flanges. Their construction is not shown in detail in FIG executed Preferably, these are connections which are known under the name "Aseptic connections” and which have a minimum non-flowed gap due to a specially shaped O-ring groove. They can be designed as real flanges, but are preferably " Aseptic clamp connections "provided. Such connections allow a geometrically particularly precise connection of the components by means of metallic contact, which is necessary in particular for the perfect effectiveness of diff
  • a casing tube 9 is connected via the connecting flange 29 to the connecting flange 28 of the
  • Compensating elements 17 tightened
  • the compensating element 17 is used for the
  • compressed air can also be used to apply the axial sealing force, the compensating element 17 being designed in principle as a pneumatic cylinder.
  • This variant is particularly preferred for larger systems in which one A large number of individual tubes can be operated, which can then be pressurized with compressed air at the same time.
  • Another advantage is obtained when different temperatures occur during operation of the device, for example when using hotter temperatures Cleaning media
  • the pneumatic application of the axial sealing force then causes the different expansion coefficients of the casing tube and the core to be compensated for.
  • Another way of achieving this is to provide a resilient element between the pressure screw 18 and the compensating element 17
  • connection 12 After construction of the device, 13 pipe connections and fittings are connected to an axial connection 12 for the supply of the medium and an axial connection for the removal of permeate.
  • the connections 12 and 13 are preferably prepared for a useful type of pipe connection, for example a clamp connection Venting of the device is first fed through the connection 13, a rinsing medium, for example a buffer, and the venting device 16 is opened as long as air comes in. Then it is closed and the supply of the rinsing medium is continued until the connection 12 is also filled with liquid the adsorber is loaded with medium from the connection 12, the entry of air being avoided.
  • an air separation in the pipe system is expediently provided
  • a back pressure valve attached after the connection 13 pays.
  • the medium flows from the connection 12 through distribution channels 14 via e Distribution slope 32 in the inner annular gap 10
  • the distribution slope causes the largely rotationally symmetrical flow distribution of the medium and thus a uniform pressure distribution
  • the permeate flows through the outer ring gap 11 via distribution channels 34, likewise provided with a distribution slope, to the connection 13
  • a distribution channel 33 has the task of distributing the liquid flow from the outer annular gap 11 when the venting device 16 is used to wind the upper region of the outer annular gap 11.
  • An O-ring groove 35 is normally of no importance. However, it enables instead of the core 15 also to use an extension core 36 (FIG. 3)
  • the hollow cylindrical adsorber modules 45 according to the invention consist of coils with a different number of turns of the adsorption membrane 1, of the lower 6 and the upper end cap 5, the sealing compound 4 for embedding the adsorption membrane in the end caps and in a preferred one Embodiment of an inner 3 and an outer support element 2, which are permeable to liquids
  • the end caps 5 and 6 made of plastic are fastened to the open ends of the hollow cylindrical adsorber module and extend transversely thereto. They embed the end faces of the adsorber module in a fluid-tight manner into the sealing compound 4 made of plastic.
  • Fig. 3 the device according to embodiment I is shown, in which two individual adsorber modules are connected in terms of flow in parallel in a common jacket tube 9 (in this illustration, the cover element 8 is shown without the compensation unit for simplification).
  • the jacket tube 9 shown here it is also possible to assemble the jacket tube from several parts, which is a simplified handling, in particular if there are more than two adsorber modules in one tube.
  • the two adsorber modules are identical to the adsorber modules shown in FIG. 1.
  • the only different component is the extension core 36, which extends from the core 15 differs as a base core only in the lower part, namely by the presence of feed-through channels 38.
  • the outer ring channel 11 is present for both modules together. Also shown are spacer webs 39, which are useful when using several modules in a tube. They can be molded onto the upper end cap 5 or onto a casting compound 4, which is let it be accomplished by a suitable casting mold. Your task is the lateral support of the adsorber modules on the jacket pipe in order to avoid tilting
  • the entire system of embodiment I consists, for example, of five lengths (3.1, 6 25, 12.5, 25 and 50 cm) and 4 steps of the number of turns (8, 15, 30 and 60) of the adsorption membranes 1 of the wrap-like adsorber modules 45, as shown by way of example in FIGS. 4a-c.
  • the different wall thicknesses of the module hollow cylinders at 15 and 8 turns are compensated in the latter case by additional layers of the spacer element (not shown).
  • the base element 7, the cover element 8 and the casing tubes 9 are for the three winding numbers shown are the same. Overall, it is a modular system that in this case allows the combination of 20 different configurations with a minimum of different components.
  • the modules in the device according to embodiment I as well as according to embodiments II, III and IV can be used because the ring gaps are designed with this in mind was that they allow the use of about 3 unit modules of 50 cm without an inadmissible pressure drop (if the adsorber modules with 60 turns are used, 5 modules can in principle also be used in a single tube, with 8 turns, however, certain losses can already be expected with 3 modules) , there is a wide range of devices that are identical in terms of flow technology, which enable reliable preliminary studies for the scale-up of technical processes.
  • Table 1 The conditions for the combination mentioned by way of example are shown in Table 1 below
  • the structure of adsorber module 45 is identical to that of embodiment I.
  • the core 15 is connected to an external thread 46 of the base element 7 by an internal thread 47 at the bottom via a core extension 48.
  • the core extension 48 can have different lengths, So that modules of different lengths can be used.
  • the jacket tube 9 has different lengths. The dimensions of the core extensions 48, the base element 7, the core 15 and the jacket tubes 9 are selected so that adsorber modules in the length increments of, for example, 50, 25, 12 5 and 6.25 cm can be used, the core extension 48 being omitted for the shortest unit and the core 15 being screwed directly to the base element 7.
  • the core 15 has an external thread 43 on top, onto which a connector 44 is screwed, which fixes the cover element 8 between Floor element 7 and Deckelelem ent 8 the jacket pipe 9 is clamped thereby, whereby the outer annular gap is sealed to the outside with the help of jacket pipe seals 49 and 50.
  • a pin 52 which engages in the groove 53 in the cover element 8, prevents twisting when the connector 44 is screwed onto the thread 43
  • the web 27 of the upper end cap 5 is clamped between the cover element 8 and the core 15, as a result of which the contact pressure for the diffusion-resistant seal 21 is applied
  • the permeate flows around the lower end cap 6 and is discharged via the distribution bores 34.
  • the groove of the lower casing tube seal 50 has openings 51 on the inside in order to avoid the accumulation of specifically heavy liquids in the seal groove.
  • the diffusion inhibition seals 52 prevent liquid from penetrating into the threads 46 and 47, avoiding contamination.
  • the body 40 is designed in its upper part as a bottom element, in the lower part as a cover element and is connected via the connecting flange 28 to the upper and the connecting flange 31 to the lower casing tube through the distribution channels 34, which are in the form of bores can, the permeate of the preceding (upper) stage is fed from the outer annular gap to the inner annular gap of the following (lower) stage.
  • a venting opening of the venting unit 16 is arranged laterally here.
  • the contact pressure for the compensating unit 17 is applied pneumatically via the compressed air connection 42, with compressed air area between the body 40 and the compensation unit 17 is sealed by the sealing elements 23 and 41
  • FIG. 6 shows the installation situation of this connecting piece in a two-stage system according to embodiment I, the first stage consisting of two identical adsorber modules and the second stage consisting of an adsorber module with half the number of turns.
  • 9a is a scale representation of a vertical section through a single stage, consisting of 4 devices according to embodiment I, of which the casing tubes 9, the base elements 7 and the cover elements 8 of the two devices at the rear are visible and which are mounted together on a support frame 54, the single device are connected in parallel via the pipe distributor 126 and downstream and via the pipe distributor 127 and can thus be used as a single stage of a tandem system or a multi-stage system.
  • this arrangement which is the basic unit of the scale-up system according to the invention, can of course also be used as an independent unit
  • the valves 55, 56, 57 and 58 are pneumatically operated diaphragm valves and are used to control filling and venting.
  • the inflow pipe 133 and the venting and spooling line 129 are on the support frame 54 through the pipe leadthrough ungen 59 fixed
  • the cover elements 8 correspond to the design Pneumatic pressure of the compensation unit, as shown in detail in Fig. 6
  • the pipe distributor 126, the compressed air supply 134 and the ventilation lines 130 are combined to form a supply part 131, from which the ventilation and coil connection 132 leads to the valve 56.
  • the supply part 131 is on the Center column 128 fixed in such a way that it can be fixed under assembly conditions (for example when changing modules) in a position rotated to the axis of the center column. The same applies to the downstream pipe distributions 127.
  • the valve 58 serves to empty the step when decommissioned
  • Fig. 10 shows an example of how simple and clear, starting from the arrangement according to Fig. 9, the further scale-up according to the invention is shown.
  • a three-stage system with 12 modules in the first stage, six in the second and three in the is shown to scale third stage, which corresponds to 96, 24 and 6 m 2 , i.e. a total of 126 m 2 membrane area, if the module is equipped accordingly.
  • the claimed base area is less than 1 m 2 with an acceptable overall height of just under 2.30 m
  • Parallel connection is not limited to four individual pipes and in large systems, several groups of four can also be connected in parallel within the stages, provided that the required symmetry in the line routing is maintained.This symmetry and the resulting symmetrical pressure distribution is, however, a prerequisite for optimal results.An aspect of the preferred modular system i It also means that the operator can design industrial systems based on existing basic examinations or, if requirements increase, independently upgrade them with components that are available as standard
  • FIG. 8 shows a test setup with three series-connected devices according to embodiment II in a suitable holding frame with interposed pressure gauges.
  • this arrangement also allows the operations in multi-stage operation to be observed visually
  • FIG. 12 shows a variant of embodiment III for crossflow operation, in which only the base element 7 is changed compared to embodiment II.
  • the modified base element 7 there are radial connecting channels 60 from inner annular gap 10 to an axial bore 61 which can be closed or partially opened by a sealing cone 62.
  • the sealing cone 62 is located on a closing element 63, which is arranged with a thread 64 in the bottom element 7.
  • the closing element 63 has a recess 65, which leaves a space between the closing element 63 and the bottom element 7, in the distribution bores 34 from the outer annular gap 11 mouths In the area of the recess 65, the closing element 63 also has bores 66 through which the liquid enters the interior of the closing element 63 and can flow out via the axial drain connection 13 designed as a hose nozzle.
  • the area of the recess 65 is opened to the outside by a sealing element 67 sealed By more or less unscrewing the closing element 63, the sealing cone 62 is opened more or less so that the quantitative ratio of the liquid flowing out of the inner annular gap 10 and the outer annular gap 11 can be changed.
  • overflowing medium and permeate are not separated separately Leads, but mixes back within the device, so that it only requires a single outflow.
  • a particle suspension containing target substance is thus fed in and a particle suspension depleted in target substance is removed.
  • To completely adsorb the target substance it can be operated in a circuit
  • Fig. 11 shows a device according to the invention according to embodiment IV in a stainless steel version.
  • the structure is based on housings such as are used for operating conventional pleated filter cartridges, with the exception that the direction of flow is from the inside out and therefore has two venting devices 16.
  • the core formed by tube 121 and end part 124, is welded to the base plate and contains the riser tube 122 inside.
  • Base plate 7, tube 121, riser tube 122 and end part 124 delimit a tightly welded cavity 123.
  • the end part 124 and the compensation unit 17 are shaped in such a way that that they form an arc, which causes a gentle deflection of the liquid flow.
  • the end part 124 contains the distribution channels 14, which flow into the inner annular gap 10 at a steep angle.This minimizes the negative effects that a dynamic pressure directed in the direction of the adsorption membrane 1 could have lubricated
  • the flow diagram of a tandem system is shown in Fig. 13 ac. It is an embodiment for the two-stage elution in which, after loading, a bound contaminant is eluted first with eluent 1 and then with eluent 2 the product, or vice versa.
  • Stages A and B are identical adsorber units, which either consist of a single module or of individual modules connected in parallel and / or in series, pAl, pA2, pBl, pB2, pM, pR are pressure measuring devices, UNA, UVB are monitors for determining the UN Extinction, LA, LB conductivity monitors, LDM and LDE air detectors (dry running protection for the pumps), PM, PE pumps, FA, FB and FR norfilter units, the numbers 68 to 109 designate the individual open-close functions of the valves, whereby valve functions have identical tasks have the same numbers in the two stages and are distinguished by the additional letters A and B
  • the valves with the valve functions 96 to 98 and 100 to 102 are by pass valves, the valve functions 4A and 4B serve as backflow valves, the valve functions 5A , 5B, 89 and 99 are used for draining the pipes, the valve functions 1A, 1B, 3A and 3B for bleeding, 6A and 6B for opening
  • FIG. 13 a shows the operating state of the system in which stage A is acted upon with medium, while the product is eluted from stage B.
  • FIG. 13 b represents the application of stages A and B with medium in series connection
  • FIG. 13 c shows one of the options that result from the special valve configuration of the embodiment. While stage A is supplied with medium, regeneration takes place in stage B in a closed circuit and with backwashing. Here is the regenerant filter, whose by pass with all others Liquids are closed, switched into the circuit so that particulate contaminants, which can become detached from the adsorber, do not deposit again.
  • the circuit can also be used with the other liquids required by the pump PE, and in both directions. the eluent 2, which causes the product to elute in the assumed application, is possible in the circuit Pipe system of the circuit located product with buffer over the product discharge 69 from the system
  • valve functions 101 to 107 For simpler applications, for example, backwashing can be dispensed with, which makes the direction reversing valve (valve functions 101 to 107) unnecessary.
  • the permeate is to be regarded as a product, namely when contaminants are to be removed from the medium, the with The lines designated for product discharge and the corresponding fittings are dispensed with.
  • Those valve functions e.g. 14 A, B and 15 A, B) in which there is always the same liquid on both sides (product or permeate) serve primarily for effective flushing because they enable the separate winding of the stages without contamination of the lines through which the lines are not flushed is possible
  • 14 a shows the local static pressure 118 in the inflow ring gap, the local static pressure 119 in the outflow ring gap (with free outflow) and the local pressure difference 120 in the dimensionless resistance parameter A 1, where s symbolizes the length of the distance from the entry into the ring pact
  • FIG. 14 b shows the mean pressure difference as a function of A and in FIG. 14 c the loss-free capacity utilization as a function of A.
  • devices are preferred whose annular gap dimensions result in values of less than 0.2, preferably less than 0.1, according to the above calculation.
  • a value of 0.02 is preferred as the lower limit for A.
  • a device according to embodiment II according to the invention equipped with a strongly basic adsorption membrane (EP 0 538 315 B1, US Pat. No. 5,547,575), was used.
  • the number of turns of the adsorption membrane in the winding-shaped adsorber module was 30 and the membrane area was 1 m 2
  • the device was charged with 2 liters of 1 M sodium hydroxide for depyrogemesis and after 60 min with 5 1 buffer was rinsed.
  • the pyrogen test revealed the absence of pyrogens 20 1 of a solution of 0.5 g / 1 ⁇ -globulin fraction from bovine (Sigma Deisenhofen Best No. G 7516, Lot No.
  • the starting solution was the process stream of a multi-stage processing of monoclonal antibodies from a cell culture of mammalian cells, which had been pre-cleaned via a Protein A column from Pharmacia.
  • the process stream of 550 to 650 liters leaving this column contained between 640 and 766 g of antibodies and between 67 and 370 picograms of DNA per mg of antibody
  • the process stream was conducted via a unit according to embodiment I according to the invention with 15 layers (2 m 2 ) of a strongly basic membrane ion exchanger at a flow rate of around 5 l / min After leaving the unit, the DNA content was below 5 picograms per mg of antibody
  • the hemoglobin (Hb) concentration was determined by recording the UV absorption at 280 nm using a model 662 flow photometer with sensor AF44, both products from Wedgewood Technology, Ine San Carlos CA, US. The measurement signal obtained was displayed on a commercially available flatbed recorder The Hb concentration was determined using calibration standards
  • the Hb solution was conducted at a flow rate of around 2 l / min by means of a positive-displacement pump over two units according to the invention according to embodiment I connected in parallel according to FIG. 3 and having 60 layers, corresponding to 16 m 2 , of a strongly acidic membrane ion exchanger.
  • the UV absorption of the escaping stream was continuously recorded and recorded
  • the Hb solution was at a flow rate of around 2 l / min by means of a positive displacement pump via a two-stage unit according to FIG. 6 of embodiment I, the first stage as in experiment B with 16 m 2 and the second stage as in experiment A. was equipped with 4 m 2 of a strongly acidic membrane ion exchanger. The UV absorption of the emerging current was continuously recorded and recorded. The dynamic binding capacity at 50% breakthrough was determined to be 0.64 mg Hb per cm 2 membrane area.
  • the 3 experiments A, B, C are shown in FIG. 5.
  • test C leads to a drastic increase in the binding capacity, that is to say up to 10% breakthrough of the Hb solution and an improved course of the breakthrough curve.
  • Body of the connector in the upper part as a bottom and in the lower
  • Sealing element, -109 open-close functions of the valves, 69 product removal,
  • UVA, UVB monitors for determining UV extinction

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Abstract

L'invention concerne des dispositifs pour des séparations de substances par adsorption, par perméation de liquides au moyen de membranes adsorbantes poreuses, ainsi que les utilisations de ces dispositifs. Les dispositifs selon l'invention comportent un boîtier cylindrique constitué d'une gaine tubulaire, d'un fond et d'un couvercle et qui entoure au moins un module adsorbant fait de membranes adsorbantes, réalisé comme une bobine sous forme de cylindre creux, dans lequel un noyau cylindrique est disposé concentriquement. Une fente annulaire intérieure et une fente annulaire extérieure sont formées entre la surface intérieure du cylindre creux et le noyau cylindrique et entre la surface extérieure du cylindre creux et la gaine tubulaire. De préférence, des canaux radiaux reliés à la fente annulaire intérieure se trouvent dans le noyau pour l'alimentation en liquides et des canaux radiaux reliés à la fente annulaire extérieure se trouvent dans le fond pour assurer l'évacuation du perméat. Des couplages en parallèle et en série permettent d'utiliser le dispositif pour des travaux de type scale-up et scale-down en laboratoire, dans les écoles techniques et dans la production.
EP98914881A 1997-03-18 1998-03-12 Dispositif pour la separation de substances par adsorption au moyen de membranes adsorbantes Withdrawn EP0968036A1 (fr)

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DE19711083A DE19711083C2 (de) 1997-03-18 1997-03-18 Vorrichtung und Verfahren für die adsorptive Stofftrennung mit Adsorptionsmembranen
DE19711083 1997-03-18
PCT/EP1998/001424 WO1998041300A1 (fr) 1997-03-18 1998-03-12 Dispositif pour la separation de substances par adsorption au moyen de membranes adsorbantes

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WO1998041300A1 (fr) 1998-09-24
DE19711083A1 (de) 1998-09-24
JP4198760B2 (ja) 2008-12-17
AU6921198A (en) 1998-10-12
JP2001515403A (ja) 2001-09-18
US6294090B1 (en) 2001-09-25
DE19711083C2 (de) 1999-04-29

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