• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a sack-like filter element (20) and a device containing this filter element (20) for adsorption filtration of liquids, for precoat filtration or for adsorption chromatography, as well as the use of the device for separating mixtures of substances, in particular for purifying reaction products.
    公开号:CH712421B1
    申请号:CH00541/17
    申请日:2017-04-24
    公开日:2021-02-26
    发明作者:Haumann Jens；Grein Raimund
    申请人:Merck Patent Gmbh；
    IPC主号:
    专利说明:

    The present invention relates to a bag-like filter element and a device containing this filter element for adsorption filtration of liquids, for precoat filtration or for adsorption chromatography, and the use of the device for separating mixtures of substances, in particular for purifying reaction products.
    The purification of reaction products by adsorption filtration, adsorption filtering, precoat filtration or adsorption chromatography is known.
    According to A. Wüst, Römpp online, Georg Thieme Verlag KG, Stuttgart, 2016, filtering adsorption is a process in which two chemically different substances are separated from one another due to their different adsorption capacity when the mixture to be separated is in a suitable one Solvent dissolves and the solution is filtered through an adsorbent that only retains one component. Filtering adsorption differs from normal adsorption in its selectivity, which is achieved through the selection of a selective solvent and an appropriate adsorbent. This method is thus characterized in that an adsorbent is placed in a filter housing. Closely related to this technique is the so-called precoat filtration, in which a filter aid, e.g. kieselguhr, is added to the unfiltrate stream to be filtered. The structure of the actual filter layer on the surface of the filter elements then takes place through the deliberate retention of the filter aid on the surface of the filter elements that is only permeable to the liquid. During the filtration, a loose filter cake of filter aid is formed which retains the impurities to be separated so that the liquid dispersing medium can run off as a clear filtrate. The only difference between chromatography and adsorption filtration is the higher separation efficiency of the stationary phase used (adsorbent) and the collection of product fractions if, for example, several products are to be eluted from the adsorbent one after the other.
    Frequently used filter devices consist of a container, which in its interior made of permeable material, contains horizontally arranged plates as the actual filter, to which the adsorbent or filter aid is applied.
    All these methods bring the problem in the pilot plant or production scale with it that the adsorbent or the filter aid must be removed manually from the filter housing at the end of the process, which exposes the staff especially when using organic, volatile solvents and also represents an ergonomically unfavorable activity, which represents a great burden for the staff and can lead to health impairments in the long term.
    The object of the present invention is to provide a device for adsorption filtration of liquids, for precoat filtration or for adsorption chromatography on a pilot plant or production scale, which does not have the above-mentioned disadvantages of the devices known from the prior art, or to a much lesser extent.
    According to the invention, this object is achieved by the subject matter defined in the independent claims. Preferred embodiments are specified in the dependent claims and explained in more detail below. The main advantages of the invention over the prior art are to be seen in the fact that in the device according to the invention there is an adsorbent or filter aid in a sack-like filter element, which is fixed in a filter housing by a clamping ring and after the filtration has ended, the sack-like filter element together with the The adsorbent contained therein is removed from the filter housing by means of a lifting device and disposed of.
    A liquid for the purposes of the present invention is a solution of a substance or a mixture of substances in a solvent that can be filtered under normal pressure or under increased pressure, which may additionally contain solid or liquid components or impurities which are not soluble in the solvent or miscible with the solvent .
    The bag-like filter element (20) according to the invention consists of a side wall (2) and a bottom part (1), the shape and size of which correspond essentially to the shape and size of the interior of the filter housing used. It is preferred that the side wall (2) is made from an essentially rectangular piece of fabric which is sewn together on two opposite edges by at least one row of seams, preferably by two or three rows of seams, to form a tube, preferably by a felled seam, with a corresponding Way, a preferably substantially circular bottom part is sewn into the tube.
    In an alternative embodiment, the side wall (2) can also be made from a single piece of tubular fabric into which a bottom part (1) is sewn.
    The bag-like filter element can be made of all common and known materials that are used for the production of filter fabrics, in particular plastics such as polyester, polyamides, polyethylene, polypropylene or polyacrylonitrile.
    Practically all conventional filament-forming polyesters such as polyethylene terephthalate (PET), polybutylene terephthalate (PBT), poly (cyclohexane-1,4-dimethanol terephthalate), etc., and copolyesters are suitable as polyester; however, polyethylene terephthalate is preferred. Practically all conventional filament-forming polyamides such as nylon-6, nylon-66, poly-m-phenylene isophthalamide, etc., and copolyamide can be used as the polyamide in a similar manner.
    Within these material classes, high-strength materials are preferred.
    In the present application, “high strength” means a strength of the filament yarns used of at least about 40-60 cN / tex or more.
    The filter material particularly preferably consists of high-strength polyester fabric with a weight per unit area between 100 g / m 2 and 300 g / m 2, preferably between 150 g / m 2 and 250 g / m 2, entirely particularly preferably between 180 g / m 2 and 220 g / m 2 and a tensile strength of the chain of 2000 N / 5 cm to 3000 N / 5 cm (chain), preferably from 2200 N / 5 cm to 2800 N / 5 cm, particularly preferably from 2400 N / 5 cm to 2600 N / 5 cm, and a tear strength of the weft of 1700 N / 5 cm to 2700 N / 5 cm, preferably from 1900 N / 5 cm to 2500 N / 5 cm, particularly preferred from 2100 N / 5cm to 2300 N / 5cm.
    The filter material very particularly preferably consists of polyethylene terephthalate.
    The term “consist of” in the context of the present application means that a material contains 90% or more, preferably 95% or more, particularly preferably 99% or more, of a substance or class of compounds specified as a manufacturing material.
    To remove the sack-like filter element (20) from the filter housing (11), transport belts (3) are attached to the outer surface of the side wall and are equipped with transport loops (4) at their ends for attachment to a hoist. The transport loops (4) are formed, for example, in that the transport belt (3) is folded over outwards or inwards above the upper edge of the filter element and then the two legs of the transport loop formed in this way are fastened in contact with one another, preferably by a seam.
    The removal of the filter element (20) according to the invention by means of a hoist is carried out either by direct attachment to the hoist, preferably on a hook, or with the help of another load-bearing means, such as a cross-beam, in particular a cross-beam. Such trusses are known to the person skilled in the art and are commercially available.
    The conveyor belts (3) are made of tear-resistant material, which is basically selected from the materials described above for the filter fabric, but preferably from a polyester.
    For the transport belts, it is preferred to use flat material, such as in particular a belt made of a woven material such as woven polyester or nylon, preferably polyester. For a given circumference of the bag-like filter element, the width of the belt is from about 150 cm to 250 cm in a range from 2 cm to 10 cm, preferably 2.5 cm to 8 cm, particularly preferably 3 cm to 4 cm. The breaking strength of the conveyor belts is 7000 N or more, preferably 8000 N or more, particularly preferably 9500 N or more, and the weight per unit area is 500 g / m 2 to 1800 g / m 2, preferably 750 to 1500 g / m 2 2> and particularly preferably 1000 to 1200 g / m 2.
    In a preferred embodiment, the conveyor belts (3) are equipped with electrically conductive fibers in order to avoid electrostatic charging, as described, for example, in DE 3938414 A1.
    To attach the sack-like filter element (20) inside the filter housing (11) is a detachably attached inside and on the upper edge of the sack-like filter element clamping ring (19), the circumference of which can be expanded by means of, for example, a clamping screw (32) and so that The filter element is both fixed and prevents the unfiltrate from crossing the edge of the filter element. The clamping ring (19) can have a circular or cylindrical outer circumference, preferably a cylindrical one.
    It is preferred that the bag-like filter element (20) at the upper edge on its outside or inside, preferably on its outside, is equipped with a sealing tape (5) which serves to reinforce the filter element (20) and at the same time Sealing improved by the clamping ring (19).
    For the sealing tape (5), it is preferred to use flat material that is in contact while the method according to the invention is being carried out essentially over the entire width of a clamping ring used for fastening the filter element (20) within the filter housing (11) . The sealing tape (5) is preferably made of rubber, silicone or a woven material made of polyester or nylon. The sealing tape (5) is preferably made of a woven material.
    Particularly preferably, the sealing tape (5) consists essentially, very particularly preferably completely, of the same material from which the conveyor belts (3) are made. Surprisingly, filter elements can be produced in a simplified manner which combine sufficient mechanical strength, very good handling when the filter element (20) is attached in the filter housing by means of a clamping ring (19) and high tightness.
    The filter housing (11) used is known per se and is commercially available. It consists of an upright, cylindrical container with a lid that holds one or more filter elements and in which, in the lower part, a liquid-permeable intermediate plate (12) designed as a spoke wheel, grate, sieve bottom or the like separates an unfiltrate space (14) from a filtrate space (13) . The intermediate plate (12) ensures that the filter element (20) maintains a certain distance from the base plate (14) so that the passage of the liquid is guaranteed at all. The filtrate space is closed at the bottom by a bowl-shaped base plate (14) with an integrated outlet nozzle (15). An inlet port (16) preferably leads centrally through the housing cover (17). Between the cylindrical upper housing part and the cover, as well as between the upper housing part and the intermediate base and between the latter and the base plate, axially acting ring seals are arranged in the edge area, so that all four housing parts are sealed against each other and can be braced against one another by clamping bolts arranged on the circumference, so that the Housing is fluid-tight even under pressure.
    In a preferred embodiment, a further filter element (40) is attached to improve the filter performance between the bag-like filter element (20) and the intermediate plate (12), for example a commercially available filter plate or depth filter layer, which is preferably made of cellulose coated with kieselguhr or perlite is, or a circular piece of fabric made of filter fabric, which is preferably made of the same material as the bag-like filter element (20) according to the invention.
    As an adsorbent or filter aid, all common adsorbents, filter aids and chromatography materials known as such are suitable, such as silica gel, kieselguhr, aluminum oxide, Florisil®, microcrystalline cellulose, activated carbon or coke, carbon black and synthetic porous adsorber resins (e.g. Amberlite® XAD) or carrier materials suitable for reverse phase chromatography (so-called "RP Gel").
    The adsorbent used is preferably silica gel or aluminum oxide, particularly preferably silica gel. Perlite, charcoal and wood flour are also suitable as filter aids.
    The adsorbent or the filter aid are in powder form. The grain size and the grain size distribution are selected so that on the one hand there is a surface that is large enough for the rapid contact between the unfiltrate and the adsorbent or the filter aid, but on the other hand that it is easy to filter, i.e. that there is no too high pressure builds up. The person skilled in the art can therefore determine the suitable grain sizes and grain size distributions in a simple manner on the basis of his general specialist knowledge, if necessary with the aid of a few preliminary experiments.
    The adsorbents preferably have an average particle size determined by sieve analysis of 50 to 200 μm, more preferably 50 to 150 μm and in particular about 80 to 120 μm. Preferably the maximumGrain size <500 µm. The adsorbents preferably contain no or only a small fine fraction with grain sizes <5 μm.
    In the method according to the invention, the adsorbent or the filter aid is preferably present within the bag-like filter element (20) in the form of a bulk bed (18) through which the unfiltrate flows.
    The process according to the invention is preferably carried out at temperatures between -10 and 60.degree. C., preferably at 0 to 40.degree. C. and in particular at 15 to 35.degree. It can take place under normal pressure or increased pressure, preferably under a pressure of 1 to 20 bar, particularly preferably from 2 to 15 bar, very particularly preferably from 4 to 8 bar.
    Embodiments of the invention are explained in more detail below with reference to the drawings. In the drawings: FIG. 1 shows the sack-like filter element in a perspective view; 2 shows a vertical section through the most important components of the device according to the invention; 3 shows a plan view of a preferred embodiment of a clamping ring; 4 shows an inside view of a preferred embodiment of a clamping ring; 5 shows the double spindle used to open and close the clamping ring.
    In detail, Fig. 1 shows a sack-like filter element with a tubular, from a circular bottom part (1) in a constant radius upwardly extending side wall (2), characterized by two from each side of the side wall (2) over the bottom part (1) Conveyor belts (3) which run to the opposite side of the outer wall of the bag and cross one another in the middle of the bottom part, the ends of which are designed as conveyor loops (4) and which are additionally connected to one on the upper edge of the filter element by one over the entire edge on the outer surface of the side part extending sealing tape (5) are connected. The transport loops (4) are designed in that the transport belt (3) is folded over outwards above the edge of the filter element and the two legs of the transport loop formed in this way are fastened in contact with one another.
    The device shown in Fig. 2 consists of a filter housing (11) with housing cover (17), a bowl-shaped base plate (14) and a liquid-permeable intermediate plate (12), which the filter housing into an unfiltered fluid space (14) and a filtrate space ( 13) shares. The sack-like filter element (20) is secured in a detachable sealing manner by means of a clamping ring (19) in the interior of the filter housing at the level of the sealing tape (5) and is mounted with its underside on the intermediate plate (12). The adsorbent or filter aid is located in the interior of the bag-like filter element in the form of a bed (18). The unfiltrate is fed to the filter element through the unfiltrate inlet (16) in the housing cover (17) and the filtrate is drawn off through the filtrate outlet (15) in the base plate (14).
    In a preferred embodiment, there is an additional disk-shaped filter plate, preferably a depth filter layer (40), between the sack-like filter element (20) and the intermediate plate (12).
    The clamping ring shown in Fig. 3 consists of two half-rings (30, 30 ') which are detachably screwed together at their ends, each with a clamping screw (32, 32'), which at their ends for receiving the clamping screws (32, 32 ') ) each open into a reinforcement (31, 31 ') provided with a bore running in the circumferential direction. The holes are each equipped with an internal thread that runs in the same direction in each half-ring and in opposite directions to the internal threads in the other half-ring. The clamping screws (32, 32 ') located therein are designed as double spindles, the ends of which are equipped with threads running in opposite directions and which are provided with multiple edges, preferably hexagons, and can thus be adjusted by means of a wrench.
    4 shows a detailed inside view of a preferred clamping ring, namely the reinforcements (31, 31 ') of two half-rings which receive a clamping screw (32) and are each provided with a bore running in the circumferential direction.
    Fig. 5 shows a preferred embodiment of the double spindle clamping screws (32), the ends of which are equipped with opposing threads (33, 34) and which are provided with a hexagon (35) and are thus adjustable by means of a wrench.
    Another object of the invention is the use of the device according to the invention for filtering adsorption, for adsorption filtration of liquids, for precoat filtration or for chromatographic separation of mixtures of substances by adsorption chromatography and a method for adsorption filtration of liquids.
    Another object of the invention is the use of the device according to the invention for the chromatographic separation of mixtures of substances by adsorption chromatography, in particular for the purification of reaction products, preferably on a pilot plant or production scale.
    The invention further relates to a method for adsorption filtration of liquids, characterized in that an adsorbent, preferably silica gel, suspended in a solvent with a solvent, is subsequently placed in the filter element (20) in the form of a bed (18) in a device according to the invention a solution of a mixture of substances in a solvent is supplied and then an eluent is supplied under a pressure in the range from 1 to 20 bar, one or more fractions of the eluate being removed from the filtrate space (13). In an alternative embodiment, the adsorbent is presented dry in the form of a bed (18) and slurried or moistened with a solvent in the device, preferably with the unfiltrate itself.
    The process according to the invention is preferably used to purify synthesis products, the raw products dissolved in a solvent or products pre-cleaned in another process in the device according to the invention by filtering adsorption, adsorption filtration, precoat filtration or adsorption chromatography, preferably by filtering adsorption or adsorption filtration of unwanted impurities or by-products are exempted.
    Usage example
    The use of the device according to the invention in accordance with a method according to the invention is explained in greater detail below by way of example without limiting the invention.
    According to the method disclosed in DE 10151300 A1, 3,4,5-trifluorophenol with 2- (4-bromo-2,6-difluorophenyl) -5,6-dihydro-4H-1,3-dithiin-1- iumtrifluoromethansulfonat converted to 5-bromo-2- [difluoro- (3,4,5-trifluorophenoxy) methyl] -1,3-difluorobenzene and the crude product obtained after aqueous work-up (70 kg) was taken up in 180 kg of n-heptane.
    The device according to the invention shown in FIG. 2, containing a filter element (20) with a diameter of 58.5 cm and a height of 52.5 cm, which is mounted on a depth filter layer (BECO® KD3) (40), is equipped with a bulk bed (18) filled from 125 kg of silica gel (grain size 0.063 mm - 0.2 mm, Merck KGaA, Darmstadt). With the housing cover (17) closed, 230 kg of n-heptane is first pumped through the unfiltrate inlet (16) and at the same time withdrawn at the filtrate outlet (15) so that the bulk bed (18) is covered by solvent during the entire process. The solution of the crude product is then pumped through the apparatus in a corresponding manner and 200 kg of filtrate is collected at the filtrate outlet (15). The bulk bed is washed with 300 kg of n-heptane and the combined filtrates (500 kg) i. Vac. concentrated and the product recrystallized once for final purification.
    To empty the device according to the invention, 80 kg of isopropanol are pumped over the silica gel in the manner described above and fed to the disposal to remove impurities. The silica gel is then blown dry in a stream of nitrogen, the nitrogen being fed under pressure to the device through the unfiltrate inlet (16) and discharged through the filtrate outlet (15). After drying is complete, the housing cover (17) is opened, the clamping ring (19) is removed, the filter element (20) with the silica gel contained in it is attached to a cross-beam using the transport loops (4) and removed from the filter housing (11) with a hoist. taken.
    权利要求:
    Claims (14)
    [1]
    1. Sack-like filter element (20) made of high-strength filter fabric, which has a tenacity of more than 40 cN / tex, with a tubular side wall (2) extending upwards from a circular base part (1) in a constant radius, characterized by two to four Conveyor belts (3) made of high-strength fabric, which have a tensile strength of more than 40, run from one outer surface of the side wall (2) over the bottom part (1) to the opposite outer surface of the side wall (2) and cross each other in the middle of the bottom part (1) cN / tex, the ends of which are formed into transport loops (4) and which are additionally connected to a sealing tape (5) running over the entire edge of the outer surface of the side wall (2) on the upper edge of the filter element (20).
    [2]
    2. Filter element (20) according to claim 1, characterized in that the transport loops (4) are formed in that the transport belt (3) is folded outwards or inwards above the upper edge of the filter element (20) and the two legs thus formed the transport loop (4) are attached in contact with each other.
    [3]
    3. Filter element (20) according to claim 1, characterized in that the conveyor belts (3) are made of polyester.
    [4]
    4. Filter element (20) according to one of claims 1 to 3, characterized in that the sealing tape (5) is made of the same material as the conveyor belts (3).
    [5]
    5. Filter element (20) according to one of claims 1 to 4, characterized in that the material of the filter fabric made of polyester with a tensile strength of the warp of 2000 N / 5 cm to 3000 N / 5 cm and a tensile strength of the weft of 1700 N / 5 cm to 2700 N / 5 cm.
    [6]
    6. Filter element (20) according to claim 5, characterized in that the material of the filter fabric is selected from polyethylene terephthalate, polybutylene terephthalate and polynaphthyl terephthalate.
    [7]
    7. Filter element (20) according to claim 6, characterized in that the material of the filter fabric consists of polyethylene terephthalate.
    [8]
    8. Device for precoat filtration, adsorption filtration or adsorption chromatography of liquids with an adsorbent or filter aid located in a filter housing (11), which divides by means of a liquid-permeable intermediate plate (12) into a filtrate space (13) and one or more filter elements receiving unfiltrate space (14) The filtrate space (13) is formed by a bowl-shaped base plate (14) arranged parallel to the intermediate plate (12) and has a filtrate outlet (15), while an unfiltrate inlet (16) for the medium to be filtered through a housing cover (17) in the upper part of the housing is passed through, characterized in that the adsorbent or filter aid in the form of a bed (18) in a sack-like filter element which is detachably fastened inside the filter housing (11) with a clamping ring (19) and which is mounted with its underside on the intermediate plate (12) (20) according to one of claims 1 to 7 g is filled, and to which the liquid to be filtered in the unfiltrate space (14) can be fed and from which the liquid filtrate in the filtrate space (13) can be withdrawn.
    [9]
    9. The device according to claim 8, characterized in that the clamping ring (19) consists of two half-rings (30, 30 ') which are detachably screwed to one another at their ends with a respective clamping screw (32, 32') and which at their ends for receiving the Tensioning screws (32, 32 ') each open into a reinforcement (31, 31') provided with a bore running in the circumferential direction, the bores each being equipped with an internal thread which runs in the same direction in each half-ring and in opposite directions to the internal thread in the other half-ring , and wherein the tensioning screws (32, 32 ') are designed as double spindles, the ends of which are provided with opposing threads (33, 34) and a polygon (35) and are adjustable by means of a wrench.
    [10]
    10. The device according to claim 8 or 9, characterized in that one or more disc-shaped filter elements (40) are attached between the bag-like filter element (20) and the intermediate plate (12).
    [11]
    11. Use of the device according to one of claims 8 to 10 for the filtering adsorption of liquids, for precoat filtration or for the chromatographic separation of mixtures of substances by adsorption chromatography.
    [12]
    12. Use according to claim 11 for the purification of reaction products.
    [13]
    13. A method for adsorption filtration of liquids, characterized in that in a device according to any one of claims 8 to 10, an adsorbent is attached to a solvent in the filter element (20) in the form of a bed (18), then a solution of a mixture of substances in fed to a solvent and then an eluent is fed under a pressure in the range from 1 to 20 bar, one or more fractions of the eluate being removed from the filtrate space (13).
    [14]
    14. The method according to claim 13, characterized in that silica gel is used as the adsorbent.
    类似技术:
    公开号 | 公开日 | 专利标题
    DE2118777C3|1981-04-30|Filters for cleaning contaminated fluids
    DE1761716C3|1976-01-02|Process for reducing the liquid content of a moist, finely divided solid and device for carrying out the process
    DE2455853C2|1983-08-18|Device for separating blood into a light and a heavy phase
    DE10327988A1|2004-07-15|Filter module, for treatment of drinking water, has wood filter membranes and parallel filament filters modified by selective sorbents
    CH712421B1|2021-02-26|Filter element.
    DE1008712B|1957-05-23|Filter wire system for filtering liquids
    EP2514498A1|2012-10-24|Filter cloth
    CH688988A5|1998-07-15|Filter centrifuge.
    DE2627283B2|1980-02-07|Filter element with frame and filter bag
    DE2854830A1|1979-06-21|PIPE PRESSURE FILTER
    CH653978A5|1986-01-31|SYSTEM FOR THE BIOLOGICAL PURIFICATION OF WATER OR WASTEWATER.
    EP1468743A1|2004-10-20|Pusher centrifuge
    DE2846302C2|1984-07-19|Blood transfusion filters
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    DE4205550C2|1997-01-30|Process and filter system for filtering industrial and process water and for dewatering sludge
    DE2134908A1|1972-01-20|Separation process for solid particles of different shapes
    DE1063121B|1959-08-13|Continuous process for the regeneration of used filter aids
    DE19714959A1|1998-10-15|Filter assembly for fine, slimy compressible particles
    DE102012104759B4|2022-01-05|Device for the separation of blood cells and blood plasma
    EP0638347B1|1997-05-28|Filter element
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    DE102009018934B4|2013-01-03|Pressure filter device and method for filtration
    EP2949390B1|2018-08-15|Adsorption plant
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    同族专利:
    公开号 | 公开日
    FR3050653A1|2017-11-03|
    DE102017003350A1|2017-11-02|
    CN107335260A|2017-11-10|
    CH712421A2|2017-10-31|
    CN107335260B|2021-07-09|
    引用文献:
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    CN102961912B|2012-11-20|2015-08-19|黎泊汐|A kind of oil filter|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE102016005295|2016-04-29|
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