WO1996035497A1 - Filtration adjuvants, filtration supports, filtration process using them and process for regenerating said adjuvants - Google Patents

Filtration adjuvants, filtration supports, filtration process using them and process for regenerating said adjuvants Download PDF

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Publication number
WO1996035497A1
WO1996035497A1 PCT/IB1996/000440 IB9600440W WO9635497A1 WO 1996035497 A1 WO1996035497 A1 WO 1996035497A1 IB 9600440 W IB9600440 W IB 9600440W WO 9635497 A1 WO9635497 A1 WO 9635497A1
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WO
WIPO (PCT)
Prior art keywords
approximately
filtration
varying
grains
filter
Prior art date
Application number
PCT/IB1996/000440
Other languages
French (fr)
Inventor
Erik Van Den Eynde
Jacques Hermia
Georges Rahier
Original Assignee
Interbrew
Krontec S.A.
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
Priority claimed from FR9505636A external-priority patent/FR2733922B1/en
Priority to AT96911085T priority Critical patent/ATE204197T1/en
Priority to DK96911085T priority patent/DK0831960T3/en
Priority to US08/952,142 priority patent/US6117459A/en
Priority to AU54075/96A priority patent/AU709244C/en
Priority to JP53392096A priority patent/JP3667342B2/en
Application filed by Interbrew, Krontec S.A. filed Critical Interbrew
Priority to KR1019970708059A priority patent/KR100356575B1/en
Priority to EP96911085A priority patent/EP0831960B1/en
Priority to CA2220445A priority patent/CA2220445C/en
Priority to HU9802386A priority patent/HU228585B1/en
Priority to BR9608304A priority patent/BR9608304A/en
Priority to DE69614534T priority patent/DE69614534T2/en
Publication of WO1996035497A1 publication Critical patent/WO1996035497A1/en

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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/02—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
    • C12H1/06—Precipitation by physical means, e.g. by irradiation, vibrations
    • C12H1/063—Separation by filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D37/00—Processes of filtration
    • B01D37/02—Precoating the filter medium; Addition of filter aids to the liquid being filtered
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/02—Loose filtering material, e.g. loose fibres
    • B01D39/04—Organic material, e.g. cellulose, cotton
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/02—Loose filtering material, e.g. loose fibres
    • B01D39/06—Inorganic material, e.g. asbestos fibres, glass beads or fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D41/00—Regeneration of the filtering material or filter elements outside the filter for liquid or gaseous fluids
    • B01D41/02—Regeneration of the filtering material or filter elements outside the filter for liquid or gaseous fluids of loose filtering material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28011—Other properties, e.g. density, crush strength
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B01J20/28019—Spherical, ellipsoidal or cylindrical
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3425—Regenerating or reactivating of sorbents or filter aids comprising organic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
    • B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/02—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
    • C12H1/04—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2201/00—Details relating to filtering apparatus
    • B01D2201/08—Regeneration of the filter
    • B01D2201/085—Regeneration of the filter using another chemical than the liquid to be filtered

Definitions

  • Filtration aids filtration media, a filtration process using them and a 'reigning ' method of said adjuvants.
  • the present invention relates to new filter aids, which can be used in the filtration of liquids, especially fine beer. It also relates to a new filtration process using said new filtration aids. Finally, it relates to a new process for the in situ regeneration of said filtration aids as well as to new filtration media.
  • Filter aids are substances used in solid-liquid separations with the formation of a deposit on a sieve or a support, either alone or in admixture with the substances to be retained and ensure by a mainly mechanical action, the efficiency of the separation. 5
  • filter aids can be differentiated according to their main constituents.
  • additives include perlites from volcanic rock, starch, cellulose and fibrous polymeric synthetics.
  • the adjuvants described in the foregoing can be used either 0 in the technique known as pre-coating, or in the technique known as alluviation.
  • One industrial sector in which filter aids are used is the brewery industry.
  • beer after maturing in storage tanks, must be clarified and filtered prior to packaging to remove a certain number of impurities, in particular colloidal cloudiness as well as yeasts. After filtration, the beer then has a brilliant color and sufficient stability for its conservation.
  • Beer adjuvant filtration is generally carried out using one of the following two techniques, namely mass filtration or alluvial filtration, the latter requiring the formation of a prelayer.
  • Alluvial filtration by far the most commonly used, consists of depositing on the filtering medium and prior to the filtration proper, a first coarse size of the filter aid to protect the filtration medium (for example Hugies filters or flat filters) on the one hand and facilitate the cleaning of the filter after filtration and the cleaning of the filtration support on the other hand.
  • a second precoat of the adjuvant of a size similar to that used for alluviation is deposited to help obtain a clear filtrate from the start of the filtration cycle.
  • the adjuvant is mixed with the beer before filtration to form a suspension.
  • This suspension forms during filtration a mixed cake containing both impurities and the adjuvant.
  • the adjuvant cake containing the retained impurities, in particular the yeasts is removed by degreasing in the form of a thick suspension, commonly called slurry.
  • the defatting is generally carried out by sending counter-direction in the filtering medium a pressurized gas-water emulsion which takes off the cake from said filtering medium and causes it to fall into the bottom of the filtration tank where it is collected.
  • the adjuvant is deposited directly on the filter medium before the beer is filtered.
  • filter aids in particular kieselguhr, however has a number of drawbacks.
  • One of the main drawbacks is that the adjuvant can only be used for one filtration cycle.
  • the brewer is then obliged to reject the adjuvant, in particular the kieselguhr, and to use a new quantity of fresh adjuvant.
  • the almost spherical shape of the adjuvant particles requires the use of particles of a relatively large size, in particular greater than 100 ⁇ m, in order to obtain an acceptable permeability of the cake and leads to a filter medium of considerable thickness.
  • the filtration efficiency is generally insufficient.
  • the main object of the invention is to remedy these drawbacks in large part, by proposing new additives which can be regenerated to a satisfactory level without using special installations.
  • the object of the invention is also to propose a new filtration process using the new adjuvants of the invention, which makes it possible to obtain a liquid which meets current quality requirements.
  • Another object of the invention is to propose a new process for regenerating filter aids.
  • the invention finally aims to propose new filtration media which can be used in particular with the adjuvants of the invention.
  • the new regenerable filter aids according to the invention which can be used for the filtration of liquids, especially fine beer, are characterized in that they include synthetic or natural polymeric incompressible grains or natural incompressible grains having a sphericity coefficient varying between approximately 0.6 and approximately 0.9.
  • the sphericity coefficient is defined according to the method described in the publication "Particle size measurement", T. Allen, p. 76-77, Chapman and Hall Ed., London 1974.
  • the new adjuvants according to the invention comprise grains of an average size varying between approximately 20 ⁇ m and approximately 70 ⁇ m, forming a filtration cake with a porosity of between approximately 0.4 and approximately 0.8 and d '' a specific mass varying between approximately 1000 and approximately 1500 kg / m 3 .
  • the porosity of the filter cake is determined by the method described by R. Leenaerts in: La Filtration Industrielle des Liquides, Tome 1, Chapitre 2, governing Belge de Filtration Ed., 1974.
  • the new adjuvants according to the invention comprise grains of an average size varying between approximately 20 ⁇ m with a standard deviation of approximately 10 ⁇ m and approximately 70 ⁇ m with a standard deviation of approximately 25 ⁇ m.
  • the adjuvants of the invention have an average grain size of approximately 35 ⁇ m with a standard deviation of approximately 15 ⁇ m and a specific mass of approximately 1200 kg / m.
  • the additives according to the invention form the framework of a porous medium which traps the impurities when they are deposited on its surface without immediately clogging up. To do this, there must be bridging between the particles adjuvant so that the impurities are lodged in the crevices located between the adjuvant particles without undergoing deformation or participating in the structure of the granular medium.
  • Obtaining an adequate porosity of the porous medium is based on the use of an adjuvant whose shape promotes the formation of contact surface between the particles and whose particle size distribution is sufficiently tight to not give rise to a distribution of the pore size too large.
  • the adjuvants have a grain form, intermediate between the fibrous and compressible form of the kieselguhr type adjuvants and the practically spherical shape of the synthetic ball-type adjuvants of the prior art which generate cakes of low porosity.
  • the adjuvants of the invention comprise synthetic or natural polymeric incompressible grains or natural incompressible grains obtained in particular from polyamide, polyvinyl chloride, fluorinated products such as TEFLON, polypropylene, polystyrene, polyethylene, certain silica derivatives, for example ryolites or glass, as well as their mixtures.
  • polyamides belong to the family of products sold under the brand NYLON.
  • the polyamide constituting the main constituent of the adjuvants of the present invention is polyundecanolactam.
  • the adjuvants of the present invention are food grade and resistant to dilute acid and alkaline solutions. They also have sufficient resistance to abrasion and to regenerating agents, as well as to temperatures of the order of 100 ° C. They are moreover non-deformable under the effect of the filtration pressure.
  • the invention also relates to a new method for filtering liquids.
  • the process for filtering a liquid, especially fine beer, comprising deaeration steps, depositing a pre-layer on a filtration support, and recirculating, is characterized in that the filtration step is carried out with a filter aid according to the present invention.
  • the proportions between the adjuvant and the liquid to be filtered vary between about 25 g of adjuvant / hl of liquid and about 250 g of adjuvant / hl of liquid.
  • the filtration process follows the same stages as a filtration with kieselguhr until the end of the stage of the nachlaufs.
  • the term “nachlauf” generally designates the step consisting, after the filtration cycle, of evacuating the beer from the filter medium by washing with water.
  • steps consist in particular of degassing or deaeration of the filter comprising the filtering medium and the filtration apparatus.
  • a pre-coat is deposited on the filtering support according to the conventional technique, namely at a flow rate close to 25 hl / hm 2 .
  • the water filling the filter is then evacuated by passing the beer with adjuvant in the step called vorlauf.
  • the filtration step begins and the filtrate obtained is then sent to the bottling unit.
  • the method further comprises a stabilization step.
  • This step can be carried out during or after the filtration step proper, using conventionally used additives, such as in particular silica gels, gallic tannins, etc.
  • conventionally used additives such as in particular silica gels, gallic tannins, etc.
  • PVPP polyvinylpyrrolidone
  • stabilization is carried out concomitantly with filtration.
  • the filtration method further comprises a step of in situ regeneration of the filtration aid.
  • this step of in situ regeneration of the filter aid comprises the steps consisting in: - washing the filter medium with a solut : of soda, at a concentration varying between approximately 2% and approximately 5%. a temperature of at least approximately 80 ° C., for a period varying between ⁇ . ⁇ ⁇ : on 60 minutes and approximately 120 minutes, and
  • the enzymatic composition comprises proteases as well as agents capable of lysing the yeasts.
  • Enzyme catalysis agents can optionally be added to the enzyme composition in order to further improve its effectiveness.
  • the enzymatic treatment is carried out when the pressure build-up per hour becomes too great and significantly higher than with an unclogged filter aid.
  • unclean adjuvant is meant a fresh or fully regenerated adjuvant.
  • the enzymatic treatment is carried out when the pressure rise in the filtration tank reaches approximately 80% of the maximum pressure authorized by the mechanical structure of the filter, that is to say in a significantly shorter period of time than with an unclogged adjuvant. , either with a significantly lower volume of filtered beer than with an unclogged adjuvant.
  • the regeneration of the filtration aid also causes the regeneration of the stabilizing agent, for example PVPP.
  • the filtration process according to the present invention therefore makes it possible to obtain a beer meeting the requirements in terms of clarity and stability and also makes it possible to regenerate the filter aid directly in the filtration tank without having to transport it and without having to modify existing installations.
  • the filtration method according to the invention can be implemented with different filtration media.
  • the filtration is carried out on candle filters, already widely used in breweries.
  • the candle filters usable in the context of the implementation of the method according to the invention comprise a wire wound in turns around a vertical support, the distance between two turns varying between approximately 20 ⁇ m and approximately 70 ⁇ m, preferably between approximately 20 ⁇ m and approximately 45 ⁇ m.
  • the wire is made from food grade material, resistant to the reagents used in the filtration process.
  • the wire wound in turns has a trapezoidal shape, the long side of the trapezium being directed towards the outside of the candle filter, on the side of the material to be filtered. In this way, the particles contained in the beer and of size smaller than the distance between the turns, pass through the filter, without the risk of clogging in the thickness of the wire and thus obstructing the 35497
  • the dimensions of the passage in the thickness of the wire being greater than the distance of passage between two turns.
  • the filtration support comprises sieves, preferably horizontal, also called plane filters, with a mesh size varying between approximately 10 ⁇ m and approximately 70 ⁇ m, preferably between approximately 10 ⁇ m and approximately 20 ⁇ m.
  • the flat filters are made of a food-grade material, resistant to the solvents and reagents used in filtration.
  • Ml 5 type sieve sold by the company South West Screen, Belgium.
  • the invention also relates to a new process for the in situ regeneration of filter aids, new in itself and which can be used in particular for the regeneration of the aids of the invention.
  • washing the filter medium with a sodium hydroxide solution at a concentration varying between approximately 2% and approximately 5%, at a temperature of at least approximately 80 ° C., for a period varying between approximately 60 minutes and approximately 120 minutes, and carrying out an enzymatic treatment of the filtering medium with an enzymatic composition, at a temperature varying between approximately 40 ° C. and approximately 60 ° C., for a duration varying between approximately 100 minutes and approximately 200 minutes, said enzymatic treatment being carried out after several cycles of filtration.
  • the enzymatic composition comprises proteases, agents capable of lysing yeasts, possibly agents of enzymatic catalysis, as defined in the above.
  • the in situ regeneration process according to the invention is particularly well suited to the regeneration of the new adjuvants of the invention, but cannot be limited to these particular adjuvants, nor to the filtration process according to the invention described above.
  • the invention relates to new filtration media.
  • the filtration supports according to the invention are characterized in that they consist of candles comprising a wire made from food-grade material resistant to the reagents used in the filtration process, wound in turns around a vertical support, the distance between two turns varying between approximately 20 ⁇ m and approximately 70 ⁇ m, preferably between approximately 20 ⁇ m and approximately 45 ⁇ m and have the trapezoidal shape as defined in the above.
  • the filtration supports according to the invention are characterized in that they consist of sieves, preferably horizontal, made from food-grade material resistant to the reagents used in the filtration process, d '' a mesh size varying between approximately 10 ⁇ m and approximately 70 ⁇ m, preferably between approximately 10 ⁇ m and approximately 20 ⁇ m.
  • the new filtration media according to the invention are particularly well suited for implementing the filtration process of the invention, but their use cannot be limited to this particular process.
  • the adjuvant used is Nylon 11, commercially available under the name RILSAN from the company Atochem, France.
  • the candle filter used consists of a conical feeding zone, a cylindrical shell with a diameter of 215 mm and a height of 2.05 m.
  • Three 32 mm diameter candles, the interior of which communicates with the filtrate collection area, are suspended in the shell.
  • the height of the candles is 1.5 m and the distance between their axes is 86 mm, to deposit a cake with a thickness of 25 mm maximum while preserving a distance of 15 mm between the surface of the cake and the wall of the shell.
  • the total volume of the filter is 78 1 and the filtration area 0.45 m 2 .
  • the spark plug cut-off threshold is 30 ⁇ m and the profile of the trapezoidal wire.
  • the installation is first of all sterilized and deaerated before depositing the precoat which is carried out at a flow rate of 20 to 30 hl / hm 2 , and in the same manner as on an industrial filter.
  • the injection of the must suspension containing RILSAN is carried out for an average of 7 minutes and a recirculation of 15 minutes allows the entire adjuvant to be deposited.
  • the precoat comprises a mixture of PVPP and RILSAN ® commercially available from GAF, USA
  • the proportions between these two constituents are the same as for alluvialization, namely 2/1 to 1/4 by weight, so that, after decompression, the composition of the regenerated filter mass is not changed.
  • the pre-layer concentration reaches 1.5 to 2 kg m, a value greater than the levels recommended conventionally, but which represents a thickness of cake substantially close to that obtained for traditional adjuvants.
  • the choice of filtration rate is conditioned by the pressure build-up as well as by the contact time necessary to obtain a sufficient stabilizing effect. To do this, the PVPP stabilization installations operate at a flow rate close to 10 hl hm 2 .
  • a second test is carried out with a Pils type beer obtained by Schwarzing and whose load after centrifugation reaches 300,000 yeasts / ml. It leads, for a total concentration in alluviation of 150 g / hl (100 g hl of adjuvant and 50 g / hl of PVPP) to a pressure difference between the inlet and the outlet of the filter of 50,000 Nm "2 after 20 hours of filtration and this for a flow of
  • the clarity of the beer after filtration meets the relevant standards. It is considerably lower than 0.7 ° EBC, recommended value and is, during tests carried out at low temperature, lower than 0.5 ° EBC. Values of 0.3 ° EBC were regularly measured.
  • the sterility of the filtration is checked by taking samples of 0.5 1 which are filtered on a cellulose nitrate membrane with a cut-off threshold of 0.45 ⁇ m.
  • the membrane is seeded using a medium of culture of malt extract agar type and incubated at 30 ° C. for 5 days.
  • Two reference beers one being filtered with the process according to the invention, the other with a conventional process, were subjected to tasting by a group of eight experts. No significant difference in taste was detected.
  • a washing of the filtering mass carried out in the filtration tool and without defatting with a 2% sodium hydroxide solution at a temperature of 80 ° C. resulted in a reduction in the size of the yeasts by 40% after two hours of treatment.
  • An enzymatic treatment makes it possible to remedy this situation, by reducing the size of the yeasts from 25% to 35% after treatment for two to three hours.
  • the enzymatic treatment is carried out by washing the filtering mass with an enzyme solution commercially available under the name YLE from the company Amano.
  • the enzymatic treatment is carried out at a pH of 5-6 and at a temperature of 50 ° C. after the attack with sodium hydroxide, which implies bringing the pH and temperature to the above values.
  • the waste from this lysis is then removed by a second washing with soda.
  • the frequency of the enzyme treatment depends on the initial charge of the beer before filtration, the type of filter used and the desired cycle length.
  • the volumes of beer filtered by the process of the invention and by a conventional filtration process were compared by extrapolation, on a filtration unit consisting of a single candle filter.
  • the filtration surface is 80 m 2 and makes it possible to deposit a cake with a volume of 3 m with a distance between the cakes deposited on the candles of 5 mm at the end of filtration.
  • the beer load before filtration is assumed to be one million yeasts / ml and the filtration rate is 10 hl / hm.
  • the volume filtered per cycle is calculated so that the volume left free for the sludge is completely filled at the end of the cycle and that the final pressure difference does not exceed 400,000 Nm ' , a value allowing a significant back pressure.
  • Vf is c aallccuulléé àà pcuprttiirr dduu vvoolluummee lliibbrree ppoouurr llee ggââtteeaauu (3 m) and the adjuvant concentration of the precoat (a p ) according to the reaction: 3 steps - 80 a ?
  • the final pressure is then calculated according to the operating law relating to a cylindrical filtration carried out at constant flow rate, as described by J. Hermia et al., In Filtration and Separation, 1994, 31, 721-725.
  • Z p denotes the weight of additive per square meter of surface
  • a denotes the weight of adjuvant per hl of beer
  • p GS denotes the specific apparent mass of the cake
  • ⁇ P denotes the pressure drop of the cake
  • t the filtration time and Vf the filtered volume.
  • the new method according to the invention makes it possible to filter generally larger volumes of beer than conventional methods.

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Abstract

The invention relates to new regeneratable filtration adjuvants which are usable for the filtration of liquids, particularly beer at the end of the secondary fermentation storage, characterized in that they comprise synthetic or natural incompressible polymer grains or natural incompressible grains having a sphericity coefficient varying between 0.6 and 0.9 approximately.

Description

Adjuvants de fi ltration, supports de fi ltration, procédé de fi ltration les ut1 U sant et procède' de régéne'ratl on desdits adjuvants.Filtration aids, filtration media, a filtration process using them and a 'reigning ' method of said adjuvants.
La présente invention se rapporte à de nouveaux adjuvants de 5 filtration, utilisables dans la filtration de liquides, notamment de bière fin de garde. Elle se rapporte également à un nouveau procédé de filtration utilisant lesdits nouveaux adjuvants de filtration. Elle concerne enfin un nouveau procédé de régénération in situ desdits adjuvants de filtration ainsi que de nouveaux supports de filtration. 0The present invention relates to new filter aids, which can be used in the filtration of liquids, especially fine beer. It also relates to a new filtration process using said new filtration aids. Finally, it relates to a new process for the in situ regeneration of said filtration aids as well as to new filtration media. 0
Les adjuvants de filtration constituent des substances utilisées dans les séparations solide - liquide avec formation d'un dépôt sur un tamis ou un support, soit seules, soit en mélange avec les substances à retenir et assurent par une action principalement mécanique, l'efficacité de la séparation. 5Filter aids are substances used in solid-liquid separations with the formation of a deposit on a sieve or a support, either alone or in admixture with the substances to be retained and ensure by a mainly mechanical action, the efficiency of the separation. 5
Plusieurs types d'adjuvants de filtration peuvent être différenciés selon leurs constituants principaux.Several types of filter aids can be differentiated according to their main constituents.
Le type d'adjuvant le plus fréquemment utilisé en brasserie est le kieselguhr, composé principalement de diatomées calcinées. 0The most frequently used type of adjuvant in a brewery is kieselguhr, mainly composed of calcined diatoms. 0
D'autres types d'adjuvants comprennent notamment les perlites issues de roche volcanique, l'amidon, la cellulose ainsi que les matières synthétiques polymériques fibreuses.Other types of additives include perlites from volcanic rock, starch, cellulose and fibrous polymeric synthetics.
5 Ces différents adjuvants forment, pendant la filtration, un milieu poreux captant les impuretés à éliminer et facilitent l'écoulement de la phase liquide.These various adjuvants form, during filtration, a porous medium which captures the impurities to be removed and facilitates the flow of the liquid phase.
Les adjuvants décrits dans ce qui précède peuvent être utilisés soit 0 dans la technique dite en précouche, soit dans la technique dite d'alluvionnage. Un secteur industriel dans lequel les adjuvants de filtration sont utilisés est le domaine de la brasserie.The adjuvants described in the foregoing can be used either 0 in the technique known as pre-coating, or in the technique known as alluviation. One industrial sector in which filter aids are used is the brewery industry.
En effet, la grande majorité des bières mises sur le marché doivent présenter une couleur brillante et être exemptes de micro-organismes. Pour le brasseur, ces exigences sont généralement respectées lorsque la bière possède une valeur de clarté E.B.C. (European Brewing Convention) inférieure à 0,5° EBC et une teneur en micro-organismes inférieure à 5 levures par litre.Indeed, the vast majority of beers on the market must have a bright color and be free from microorganisms. For the brewer, these requirements are generally met when the beer has an E.B.C. (European Brewing Convention) below 0.5 ° EBC and a microorganism content below 5 yeasts per liter.
Les valeurs de clarté E.B.C. et leur appréciation sont définies dans la publication : Analytica-E.B.C, 4ème Ed., 1987, Revue de la Brasserie et des Boissons Ed., Zurich.E.B.C. clarity values and their appreciation are defined in the publication: Analytica-E.B.C, 4th Ed., 1987, Revue de la Brasserie et des Boissons Ed., Zurich.
Jusqu'à présent, le procédé le plus économique et le plus efficace pour atteindre ces valeurs consiste à utiliser un adjuvant de filtration dans le processus de fabrication de la bière.So far, the most economical and efficient process for achieving these values has been to use a filter aid in the beer making process.
En effet, la bière, après sa maturation dans des réservoirs de garde, doit être clarifiée et filtrée préalablement à son conditionnement pour éliminer un certain nombre d'impuretés, en particulier un trouble colloïdal ainsi que des levures. Après filtration, la bière présente alors une couleur brillante et une stabilité suffisante pour sa conservation.Indeed, beer, after maturing in storage tanks, must be clarified and filtered prior to packaging to remove a certain number of impurities, in particular colloidal cloudiness as well as yeasts. After filtration, the beer then has a brilliant color and sufficient stability for its conservation.
La filtration avec adjuvant de la bière est généralement réalisée en utilisant l'une des deux techniques suivantes, à savoir la filtration sur masse ou la filtration en alluvionnage, cette dernière nécessitant la formation d'une précouche préalable. La filtration en alluvionnage, de loin la plus couramment utilisée, consiste à déposer sur le milieu filtrant et préalablement à la filtration proprement dite, une première précouche de l'adjuvant de filtration d'une taille grossière pour protéger le support de filtration (par exemple des filtres à Hugies ou des filtres- plans) d'une part et faciliter le débâtissage du filtre après filtration et le nettoyage du support de filtration d'autre part. Fréquemment, une seconde précouche de l'adjuvant d'une taille similaire à celle utilisée pour l'alluvionnage est déposée pour aider à l'obtention d'un filtrat clair dès le début du cycle de filtration.Beer adjuvant filtration is generally carried out using one of the following two techniques, namely mass filtration or alluvial filtration, the latter requiring the formation of a prelayer. Alluvial filtration, by far the most commonly used, consists of depositing on the filtering medium and prior to the filtration proper, a first coarse size of the filter aid to protect the filtration medium (for example Hugies filters or flat filters) on the one hand and facilitate the cleaning of the filter after filtration and the cleaning of the filtration support on the other hand. Frequently, a second precoat of the adjuvant of a size similar to that used for alluviation is deposited to help obtain a clear filtrate from the start of the filtration cycle.
En alluvionnage, l'adjuvant est mélangé à la bière avant la filtration pour former une suspension. Cette suspension forme lors de la filtration un gâteau mixte contenant à la fois des impuretés et l'adjuvant.In alluviation, the adjuvant is mixed with the beer before filtration to form a suspension. This suspension forms during filtration a mixed cake containing both impurities and the adjuvant.
Lorsque le cycle de filtration est terminé, le gâteau d'adjuvant renfermant les impuretés retenues, notamment les levures, est éliminé par débâtissage sous la forme d'une suspension épaisse, communément appelée bourbe.When the filtration cycle is finished, the adjuvant cake containing the retained impurities, in particular the yeasts, is removed by degreasing in the form of a thick suspension, commonly called slurry.
Dans le cas où la filtration est réalisée en utilisant des filtres à bougies, le débâtissage est généralement réalisé en envoyant à contre-sens dans le milieu filtrant une émulsion gaz-eau sous pression qui décolle le gâteau dudit milieu filtrant et le fait tomber dans le fond de la cuve de filtration où il est recueilli.In the case where the filtration is carried out using candle filters, the defatting is generally carried out by sending counter-direction in the filtering medium a pressurized gas-water emulsion which takes off the cake from said filtering medium and causes it to fall into the bottom of the filtration tank where it is collected.
Dans le cas où la filtration est réalisée en utilisant des filtres à plateaux horizontaux, le gâteau est éliminé par la force centrifuge créée par la rotation des éléments filtrants.In the case where the filtration is carried out using filters with horizontal plates, the cake is eliminated by the centrifugal force created by the rotation of the filter elements.
Dans la filtration sur masse, l'adjuvant est déposé directement sur le support filtrant avant la filtration de la bière. L'utilisation d'adjuvants de filtration, en particulier de kieselguhr, présente cependant un certain nombre d'inconvénients.In mass filtration, the adjuvant is deposited directly on the filter medium before the beer is filtered. The use of filter aids, in particular kieselguhr, however has a number of drawbacks.
L'un des principaux inconvénients réside dans le fait que l'adjuvant ne peut être utilisé que pour un seul cycle de filtration.One of the main drawbacks is that the adjuvant can only be used for one filtration cycle.
Le brasseur est alors obligé de rejetter l'adjuvant, notamment le kieselguhr, et d'utiliser une nouvelle quantité d'adjuvant frais. On conçoit alors les problèmes que pose ce rejet pour l'environnement, en plus du coût supplémentaire du produit final lié à un approvisionnement régulier en adjuvant.The brewer is then obliged to reject the adjuvant, in particular the kieselguhr, and to use a new quantity of fresh adjuvant. We then understand the problems posed by this release to the environment, in addition to the additional cost of the final product linked to a regular supply of adjuvant.
Des techniques de régénération de l'adjuvant, en particulier du kieselguhr, ont donc été envisagées, sans répondre cependant totalement aux besoins des industriels.Techniques for regenerating the adjuvant, in particular kieselguhr, have therefore been considered, without however fully meeting the needs of manufacturers.
En effet, les techniques actuelles de régénération des adjuvants, en particulier du kieselguhr, ne permettent d'obtenir qu'une régénération partielle de l'adjuvant. Le brasseur est ainsi obligé d'ajouter, à chaque nouveau cycle de filtration, une certaine quantité d'adjuvant frais pour compenser la baisse d'efficacité de la filtration due notamment à l'accroissement de la quantité d'impuretés présentes, voire de rejetter, après plusieurs cycles de filtration, l'adjuvant régénéré partiellement, avec les problèmes déjà évoqués ci-dessus.Indeed, current techniques for regenerating adjuvants, in particular kieselguhr, only allow partial regeneration of the adjuvant. The brewer is thus obliged to add, to each new filtration cycle, a certain amount of fresh adjuvant to compensate for the drop in filtration efficiency due in particular to the increase in the amount of impurities present, or even to reject , after several filtration cycles, the adjuvant partially regenerated, with the problems already mentioned above.
En outre, ces procédés nécessitent l'utilisation d'installations particulières et distinctes de celles des installations de filtration. Elles entraînent de ce fait des frais importants en investissement et en fonctionnement, notamment de frais de transport de l'adjuvant vers le site de régénération.In addition, these methods require the use of special installations which are distinct from those of filtration installations. They therefore entail significant investment and operating costs, in particular transport costs for the additive to the regeneration site.
Des recherches ont alors été menées pour développer un adjuvant régénérable permettant de résoudre les problèmes décrits dans ce qui précède. Un adjuvant de filtration de ce type a notamment été proposé, consistant en des billes sphériques de matériau synthétique, pouvant être régénéré dans les installations de filtration existantes. Cet adjuvant ne permet toutefois de résoudre qu'en partie les inconvénients évoqués ci-dessus.Research was then carried out to develop a regenerable adjuvant making it possible to solve the problems described in the foregoing. A filter aid of this type has in particular been proposed, consisting of spherical balls of synthetic material, which can be regenerated in existing filtration installations. However, this adjuvant only partially resolves the drawbacks mentioned above.
En effet, la forme quasiment sphérique des particules d'adjuvant nécessite l'utilisation de particules d'une taille relativement importante, notamment supérieure à 100 μm, pour obtenir une perméabilité acceptable du gâteau et conduit à un milieu filtrant d'une épaisseur importante. De plus l'efficacité de la filtration est généralement insuffisante.Indeed, the almost spherical shape of the adjuvant particles requires the use of particles of a relatively large size, in particular greater than 100 μm, in order to obtain an acceptable permeability of the cake and leads to a filter medium of considerable thickness. In addition, the filtration efficiency is generally insufficient.
En outre, le degré de régénération obtenu par les techniques conventionnelles s'avère encore insatisfaisant.In addition, the degree of regeneration obtained by conventional techniques is still unsatisfactory.
L'invention a pour principal but de remédier en grande partie à ces inconvénients, en proposant de nouveaux adjuvants régénérables à un niveau satisfaisant sans utiliser d'installations spéciales.The main object of the invention is to remedy these drawbacks in large part, by proposing new additives which can be regenerated to a satisfactory level without using special installations.
L'invention a également pour but de proposer un nouveau procédé de filtration utilisant les nouveaux adjuvants de l'invention, qui permette d'obtenir un liquide répondant aux exigences actuelles de qualité.The object of the invention is also to propose a new filtration process using the new adjuvants of the invention, which makes it possible to obtain a liquid which meets current quality requirements.
L'invention a également pour but de proposer un nouveau procédé de régénération des adjuvants de filtration.Another object of the invention is to propose a new process for regenerating filter aids.
L'invention a enfin pour but de proposer de nouveaux supports de filtration utilisables notamment avec les adjuvants de l'invention.The invention finally aims to propose new filtration media which can be used in particular with the adjuvants of the invention.
Les nouveaux adjuvants de filtration régénérables selon l'invention, utilisables pour la filtration de liquides, notamment de bière fin de garde, se caractérisent en ce qu'ils comprennent des grains incompressibles polymériques synthétiques ou naturels ou des grains incompressibles naturels possédant un coefficient de sphéricité variant entre environ 0,6 et environ 0,9.The new regenerable filter aids according to the invention, which can be used for the filtration of liquids, especially fine beer, are characterized in that they include synthetic or natural polymeric incompressible grains or natural incompressible grains having a sphericity coefficient varying between approximately 0.6 and approximately 0.9.
Dans le cadre de la présente invention, le coefficient de sphéricité est défini selon la méthode décrite dans la publication "Particle size measurement", T. Allen, p. 76-77, Chapman and Hall Ed., London 1974.In the context of the present invention, the sphericity coefficient is defined according to the method described in the publication "Particle size measurement", T. Allen, p. 76-77, Chapman and Hall Ed., London 1974.
De préférence, les nouveaux adjuvants selon l'invention comprennent des grains d'une taille moyenne variant entre environ 20 μm et environ 70 μm, formant un gâteau de filtration d'une porosité comprise entre environ 0,4 et environ 0,8 et d'une masse spécifique variant entre environ 1000 et environ 1500 kg/m3.Preferably, the new adjuvants according to the invention comprise grains of an average size varying between approximately 20 μm and approximately 70 μm, forming a filtration cake with a porosity of between approximately 0.4 and approximately 0.8 and d '' a specific mass varying between approximately 1000 and approximately 1500 kg / m 3 .
Dans le cadre de la présente invention, la porosité du gâteau de filtration est déterminée par la méthode décrite par R. Leenaerts dans : La Filtration Industrielle des Liquides, Tome 1, Chapitre 2, Société Belge de Filtration Ed., 1974.In the context of the present invention, the porosity of the filter cake is determined by the method described by R. Leenaerts in: La Filtration Industrielle des Liquides, Tome 1, Chapitre 2, Société Belge de Filtration Ed., 1974.
De préférence, les nouveaux adjuvants selon l'invention comprennent des grains d'une taille moyenne variant entre environ 20 μm avec un écart-type d'environ 10 μm et environ 70 μm avec un écart-type d'environ 25 μm.Preferably, the new adjuvants according to the invention comprise grains of an average size varying between approximately 20 μm with a standard deviation of approximately 10 μm and approximately 70 μm with a standard deviation of approximately 25 μm.
De préférence, les adjuvants de l'invention possèdent une taille moyenne de grains d'environ 35 μm avec un écart-type d'environ 15 μm et une masse spécifique d'environ 1200 kg / m .Preferably, the adjuvants of the invention have an average grain size of approximately 35 μm with a standard deviation of approximately 15 μm and a specific mass of approximately 1200 kg / m.
Les adjuvants selon l'invention forment l'ossature d'un milieu poreux qui piège les impuretés lorsqu'elles se déposent à sa surface sans pour autant se colmater instantanément. Pour ce faire, il doit y avoir pontage entre les particules d'adjuvant afin que les impuretés se logent dans les anfractuosités situées entre les particules d'adjuvant sans subir de déformation ni participer à la structure du milieu granulaire.The additives according to the invention form the framework of a porous medium which traps the impurities when they are deposited on its surface without immediately clogging up. To do this, there must be bridging between the particles adjuvant so that the impurities are lodged in the crevices located between the adjuvant particles without undergoing deformation or participating in the structure of the granular medium.
L'obtention d'une porosité adéquate du milieu poreux repose sur l'emploi d'un adjuvant dont la forme favorise la formation de surface de contact entre les particules et dont la distribution granulométrique est suffisamment serrée pour ne pas donner lieu à une distribution de la taille des pores trop importante.Obtaining an adequate porosity of the porous medium is based on the use of an adjuvant whose shape promotes the formation of contact surface between the particles and whose particle size distribution is sufficiently tight to not give rise to a distribution of the pore size too large.
Selon l'invention, les adjuvants possèdent une forme de grains, intermédiaire entre la forme fibreuse et compressible des adjuvants de type kieselguhr et la forme pratiquement sphérique des adjuvants synthétiques en billes de l'art antérieur qui engendrent des gâteaux de faible porosité.According to the invention, the adjuvants have a grain form, intermediate between the fibrous and compressible form of the kieselguhr type adjuvants and the practically spherical shape of the synthetic ball-type adjuvants of the prior art which generate cakes of low porosity.
Selon une forme de réalisation préférée de l'invention, les adjuvants de l'invention comprennent des grains incompressibles polymériques synthétiques ou naturels ou des grains incompressibles naturels obtenus notamment à partir de polyamide, de polychlorure de vinyle, de produits fluorés tels que le TEFLON , de polypropylène, de polystyrène, de polyéthylène, de certains dérivés de silice, par exemple de ryolites ou de verre, ainsi que leurs mélanges.According to a preferred embodiment of the invention, the adjuvants of the invention comprise synthetic or natural polymeric incompressible grains or natural incompressible grains obtained in particular from polyamide, polyvinyl chloride, fluorinated products such as TEFLON, polypropylene, polystyrene, polyethylene, certain silica derivatives, for example ryolites or glass, as well as their mixtures.
A titre illustratif et non limitatif de polyamides utilisables dans le cadre de la présente invention, on citera notamment le polycaprolactame, l'adipamide de poly(hexaméthylène), le nonanediamide de poly(hexaméthylène), le sébacamide de poly(hexaméthylène), le dodécanodiamide de poly(hexaméthylène), le polyundécanolactame, le polylauryllactame et/ou leurs mélanges.By way of nonlimiting illustration of polyamides which can be used in the context of the present invention, mention will be made in particular of polycaprolactam, poly (hexamethylene) adipamide, poly (hexamethylene) nonanediamide, poly (hexamethylene) sebacamide, dodecanodiamide poly (hexamethylene), polyundecanolactam, polylauryllactam and / or mixtures thereof.
Les polyamides ci-dessus appartiennent à la famille des produits commercialisés sous la marque NYLON . Selon une forme particulièrement préférée de l'invention, le polyamide constituant le constituant principal des adjuvants de la présente invention est le polyundécanolactame.The above polyamides belong to the family of products sold under the brand NYLON. According to a particularly preferred form of the invention, the polyamide constituting the main constituent of the adjuvants of the present invention is polyundecanolactam.
De préférence, les adjuvants de la présente invention sont de qualité alimentaire et résistent aux solutions acides et alcalines diluées. Ils présentent de plus une résistance suffisante à l'abrasion et aux agents de régénération, ainsi qu'à des températures de l'ordre de 100°C. Ils sont de plus indéformables sous l'effet de la pression de filtration.Preferably, the adjuvants of the present invention are food grade and resistant to dilute acid and alkaline solutions. They also have sufficient resistance to abrasion and to regenerating agents, as well as to temperatures of the order of 100 ° C. They are moreover non-deformable under the effect of the filtration pressure.
L'invention a également pour objet un nouveau procédé de filtration de liquides.The invention also relates to a new method for filtering liquids.
Le procédé de filtration d'un liquide, notamment de bière fin de garde comprenant des étapes de désaération, de dépôt d'une précouche sur un support de filtration, de recirculation, se caractérise en ce que l'étape de filtration est réalisée avec un adjuvant de filtration selon la présente invention.The process for filtering a liquid, especially fine beer, comprising deaeration steps, depositing a pre-layer on a filtration support, and recirculating, is characterized in that the filtration step is carried out with a filter aid according to the present invention.
De préférence, les proportions entre l'adjuvant et le liquide à filtrer varient entre environ 25 g d'adjuvant / hl de liquide et environ 250 g d'adjuvant / hl de liquide.Preferably, the proportions between the adjuvant and the liquid to be filtered vary between about 25 g of adjuvant / hl of liquid and about 250 g of adjuvant / hl of liquid.
Selon l'invention, le procédé de filtration suit les mêmes étapes qu'une filtration avec kieselguhr jusqu'à la fin de l'étape des nachlaufs. On désigne généralement par nachlauf l'étape consistant, après le cycle de filtration, à évacuer la bière hors du milieu filtrant en effectuant un lavage à l'eau.According to the invention, the filtration process follows the same stages as a filtration with kieselguhr until the end of the stage of the nachlaufs. The term “nachlauf” generally designates the step consisting, after the filtration cycle, of evacuating the beer from the filter medium by washing with water.
Ces étapes consistent notamment en un dégazage ou une désaération du filtre comprenant le milieu filtrant et l'appareillage de filtration. Une précouche est déposée sur le support filtrant selon la technique conventionnelle, à savoir à un débit proche de 25 hl / hm2.These steps consist in particular of degassing or deaeration of the filter comprising the filtering medium and the filtration apparatus. A pre-coat is deposited on the filtering support according to the conventional technique, namely at a flow rate close to 25 hl / hm 2 .
L'eau remplissant le filtre est ensuite évacuée en effectuant un passage de la bière additionnée d'adjuvant dans l'étape appelée vorlauf. Lorsque la composition du mélange eau-bière est satisfaisante, l'étape de filtration débute et le filtrat obtenu est ensuite envoyé vers l'unité d'embouteillage.The water filling the filter is then evacuated by passing the beer with adjuvant in the step called vorlauf. When the composition of the water-beer mixture is satisfactory, the filtration step begins and the filtrate obtained is then sent to the bottling unit.
Selon une forme de réalisation préférée de l'invention, le procédé comporte de plus une étape de stabilisation. Cette étape peut être effectuée pendant ou après l'étape de filtration proprement dite, en utilisant des additifs conventionnellement employés, tels que notamment les gels de silice, les tanins galliques, etc. Généralement, lorsque la stabilisation est effectuée après la filtration, des enzymes protéolytiques et du polyvinylpyrrolidone (PVPP), de préférence régénérables, sont utilisés.According to a preferred embodiment of the invention, the method further comprises a stabilization step. This step can be carried out during or after the filtration step proper, using conventionally used additives, such as in particular silica gels, gallic tannins, etc. Generally, when stabilization is carried out after filtration, proteolytic enzymes and polyvinylpyrrolidone (PVPP), preferably regenerable, are used.
Avantageusement, la stabilisation est effectuée de façon concomittante à la filtration.Advantageously, stabilization is carried out concomitantly with filtration.
Selon une forme de réalisation préférée de la présente invention, le procédé de filtration comporte de plus une étape de régénération in situ de l'adjuvant de filtration.According to a preferred embodiment of the present invention, the filtration method further comprises a step of in situ regeneration of the filtration aid.
Selon l'invention, cette étape de régénération in situ de l'adjuvant de filtration, comprend les étapes consistant à : - laver le milieu filtrant avec une solut:
Figure imgf000011_0001
de soude, à une concentration variant entre environ 2 % et environ 5 %. -ine température d'au moins environ 80°C, pendant une durée variant entre ι.\ \ :on 60 minutes et environ 120 minutes, etAccording to the invention, this step of in situ regeneration of the filter aid, comprises the steps consisting in: - washing the filter medium with a solut :
Figure imgf000011_0001
of soda, at a concentration varying between approximately 2% and approximately 5%. a temperature of at least approximately 80 ° C., for a period varying between ι. \ \: on 60 minutes and approximately 120 minutes, and
- effectuer un traitement enzymatique du i.-v _ filtrant avec une composition enzymatique, à une température variant entre environ 40°C et environ 60°C, pendant une durée variant entre environ 100 minutes et environ 200 minutes, ledit traitement enzymatique étant réalisé après plusieurs cycles de filtration.- perform an enzymatic treatment of the filtering i.v. with an enzymatic composition, at a temperature varying between approximately 40 ° C. and approximately 60 ° C, for a period varying between approximately 100 minutes and approximately 200 minutes, said enzymatic treatment being carried out after several filtration cycles.
Avantageusement, la composition enzymatique comprend des protéases ainsi que des agents capables de lyser les levures.Advantageously, the enzymatic composition comprises proteases as well as agents capable of lysing the yeasts.
On citera à titre non limitatif de compositions enzymatiques utilisables dans le cadre de la présente invention, le produit disponible commercialement sous la dénomination SP299 auprès de la société Novo, Danemark et le produit YLE disponible commercialement auprès de la société Amano, Japon.Mention will be made, without limitation, of enzymatic compositions which can be used in the context of the present invention, the product commercially available under the name SP299 from the company Novo, Denmark and the product YLE commercially available from the company Amano, Japan.
Des agents de catalyse enzymatique peuvent éventuellement être ajoutés à la composition enzymatique dans le but d'améliorer encore son efficacité.Enzyme catalysis agents can optionally be added to the enzyme composition in order to further improve its effectiveness.
On remarquera au sujet du traitement enzymatique de l'adjuvant que ce traitement n'est pas effectué nécessairement à la fin de chaque cycle de filtration, mais seulement lorsque la montée en pression dans le filtre durant le cycle de filtration devient trop importante.It will be noted with regard to the enzymatic treatment of the adjuvant that this treatment is not necessarily carried out at the end of each filtration cycle, but only when the pressure rise in the filter during the filtration cycle becomes too great.
De préférence, le traitement enzymatique est réalisé lorsque la montée en pression par heure devient trop importante et significativement plus élevée qu'avec un adjuvant de filtration non encrassé. On entend par adjuvant non encrassé un adjuvant frais ou totalement régénéré.Preferably, the enzymatic treatment is carried out when the pressure build-up per hour becomes too great and significantly higher than with an unclogged filter aid. By unclean adjuvant is meant a fresh or fully regenerated adjuvant.
Par exemple, le traitement enzymatique est réalisé lorsque la montée en pression dans la cuve de filtration atteint environ 80 % de la pression maximale autorisée par la structure mécanique du filtre, soit dans une période de temps significativement plus courte qu'avec un adjuvant non encrassé, soit avec un volume de bière filtrée significativement plus réduit qu'avec un adjuvant non encrassé.For example, the enzymatic treatment is carried out when the pressure rise in the filtration tank reaches approximately 80% of the maximum pressure authorized by the mechanical structure of the filter, that is to say in a significantly shorter period of time than with an unclogged adjuvant. , either with a significantly lower volume of filtered beer than with an unclogged adjuvant.
Lorsque le procédé de filtration selon l'invention comprend une étape de stabilisation, la régénération de l'adjuvant de filtration provoque également la régénération de l'agent stabilisant, par exemple du PVPP.When the filtration method according to the invention comprises a stabilization step, the regeneration of the filtration aid also causes the regeneration of the stabilizing agent, for example PVPP.
Le procédé de filtration selon la présente invention permet donc d'obtenir une bière répondant aux exigences en termes de clarté et de stabilité et permet également de régénérer l'adjuvant de filtration directement dans la cuve de filtration sans avoir à le transporter et sans avoir à modifier les installations existantes.The filtration process according to the present invention therefore makes it possible to obtain a beer meeting the requirements in terms of clarity and stability and also makes it possible to regenerate the filter aid directly in the filtration tank without having to transport it and without having to modify existing installations.
Le procédé de filtration selon l'invention peut être mis en oeuvre avec différents supports de filtration.The filtration method according to the invention can be implemented with different filtration media.
Selon une première forme de réalisation, la filtration est réalisée sur des filtres à bougies, déjà largement utilisés en brasserie. Les filtres à bougies utilisables dans le cadre de la mise en oeuvre du procédé selon l'invention comprennent un fil enroulé en spires autour d'un support vertical, la distance entre deux spires variant entre environ 20 μm et environ 70 μm, de préférence entre environ 20 μm et environ 45 μm.According to a first embodiment, the filtration is carried out on candle filters, already widely used in breweries. The candle filters usable in the context of the implementation of the method according to the invention comprise a wire wound in turns around a vertical support, the distance between two turns varying between approximately 20 μm and approximately 70 μm, preferably between approximately 20 μm and approximately 45 μm.
Avantageusement, le fil est réalisé à partir de matière de qualité alimentaire, résistante aux réactifs utilisés dans le procédé de filtration. Selon une forme particulièrement avantageuse, le fil enroulé en spires a une forme trapézoïdale, le grand côté du trapèze étant dirigé vers l'extérieur du filtre à bougies, du côté de la matière à filtrer. De cette façon, les particules contenues dans la bière et de taille inférieure à la distance entre les spires, passent au travers du filtre, sans risquer de se colmater dans l'épaisseur du fil et d'obstruer ainsi le 35497Advantageously, the wire is made from food grade material, resistant to the reagents used in the filtration process. According to a particularly advantageous form, the wire wound in turns has a trapezoidal shape, the long side of the trapezium being directed towards the outside of the candle filter, on the side of the material to be filtered. In this way, the particles contained in the beer and of size smaller than the distance between the turns, pass through the filter, without the risk of clogging in the thickness of the wire and thus obstructing the 35497
filtre, les dimensions du passage dans l'épaisseur du fil étant plus grandes que la distance de passage entre deux spires.filter, the dimensions of the passage in the thickness of the wire being greater than the distance of passage between two turns.
A titre d'exemples non limitatifs de filtres à bougies utilisables, on citera les produits de type "Trislot", commercialisés par la société Bekaert, Belgique.By way of nonlimiting examples of usable candle filters, mention will be made of products of the "Trislot" type, sold by the company Bekaert, Belgium.
Selon une autre forme de réalisation de la présente invention, le support de filtration comprend des tamis, de préférence horizontaux, encore appelés filtres-plans, d'une grandeur de maille variant entre environ 10 μm et environ 70 μm, de préférence entre environ 10 μm et environ 20 μm.According to another embodiment of the present invention, the filtration support comprises sieves, preferably horizontal, also called plane filters, with a mesh size varying between approximately 10 μm and approximately 70 μm, preferably between approximately 10 μm and approximately 20 μm.
De la même façon que précédemment, les filtres-plans sont réalisés en un matériau de qualité alimentaire, résistent aux solvants et réactifs utilisés dans la filtration.In the same way as above, the flat filters are made of a food-grade material, resistant to the solvents and reagents used in filtration.
A titre d'exemple non limitatif de tamis utilisable, on citera le tamis de type Ml 5 commercialisé par la société South West Screen, Belgique.By way of nonlimiting example of a sieve that can be used, mention may be made of the Ml 5 type sieve sold by the company South West Screen, Belgium.
L'invention se rapporte également à un nouveau procédé de régénération in situ d'adjuvants de filtration, nouveau en lui-même et pouvant être utilisé notamment pour la régénération des adjuvants de l'invention.The invention also relates to a new process for the in situ regeneration of filter aids, new in itself and which can be used in particular for the regeneration of the aids of the invention.
Le procédé de régénération selon l'invention se caractérise en ce qu'il comprend les étapes consistant à :The regeneration process according to the invention is characterized in that it comprises the steps consisting in:
- laver le milieu filtrant avec une solution de soude, à une concentration variant entre environ 2 % et environ 5 %, à une température d'au moins environ 80°C, pendant une durée variant entre environ 60 minutes et environ 120 minutes, et - effectuer un traitement enzymatique du milieu filtrant avec une composition enzymatique, à une température variant entre environ 40°C et environ 60°C, pendant une durée variant entre environ 100 minutes et environ 200 minutes, ledit traitement enzymatique étant réalisé après plusieurs cycles de filtration.washing the filter medium with a sodium hydroxide solution, at a concentration varying between approximately 2% and approximately 5%, at a temperature of at least approximately 80 ° C., for a period varying between approximately 60 minutes and approximately 120 minutes, and carrying out an enzymatic treatment of the filtering medium with an enzymatic composition, at a temperature varying between approximately 40 ° C. and approximately 60 ° C., for a duration varying between approximately 100 minutes and approximately 200 minutes, said enzymatic treatment being carried out after several cycles of filtration.
Selon l'invention, la composition enzymatique comprend des protéases, des agents capables de lyser les levures, éventuellement des agents de catalyse enzymatique, tels que définis dans ce qui précède.According to the invention, the enzymatic composition comprises proteases, agents capable of lysing yeasts, possibly agents of enzymatic catalysis, as defined in the above.
Le procédé de régénération in situ selon l'invention est particulièrement bien adapté à la régénération des nouveaux adjuvants de l'invention, mais ne saurait être limité à ces adjuvants particuliers, ni au procédé de filtration selon l'invention décrit plus haut.The in situ regeneration process according to the invention is particularly well suited to the regeneration of the new adjuvants of the invention, but cannot be limited to these particular adjuvants, nor to the filtration process according to the invention described above.
L'invention concerne enfin de nouveaux supports de filtration.Finally, the invention relates to new filtration media.
Selon une première forme de réalisation, les supports de filtration selon l'invention se caractérisent en ce qu'ils consistent en des bougies comprenant un fil réalisé à partir de matière de qualité alimentaire résistante aux réactifs utilisés dans le procédé de filtration, enroulé en spires autour d'un support vertical, la distance entre deux spires variant entre environ 20 μm et environ 70 μm, de préférence entre environ 20 μm et environ 45 μm et possèdent la forme trapézoïdale telle que définie dans ce qui précède.According to a first embodiment, the filtration supports according to the invention are characterized in that they consist of candles comprising a wire made from food-grade material resistant to the reagents used in the filtration process, wound in turns around a vertical support, the distance between two turns varying between approximately 20 μm and approximately 70 μm, preferably between approximately 20 μm and approximately 45 μm and have the trapezoidal shape as defined in the above.
Selon une autre forme de réalisation, les supports de filtration selon l'invention se caractérisent en ce qu'ils consistent en des tamis, de préférence horizontaux, réalisés à partir de matière de qualité alimentaire résistante aux réactifs utilisés dans le procédé de filtration, d'une grandeur de maille variant entre environ 10 μm et environ 70 μm, de préférence entre environ 10 μm et environ 20 μm.According to another embodiment, the filtration supports according to the invention are characterized in that they consist of sieves, preferably horizontal, made from food-grade material resistant to the reagents used in the filtration process, d '' a mesh size varying between approximately 10 μm and approximately 70 μm, preferably between approximately 10 μm and approximately 20 μm.
Les nouveaux supports de filtration selon l'invention sont particulièrement bien adaptés pour la mise en oeuvre du procédé de filtration de l'invention mais leur utilisation en saurait être limitée à ce procédé particulier.The new filtration media according to the invention are particularly well suited for implementing the filtration process of the invention, but their use cannot be limited to this particular process.
Des avantages et caractéristiques supplémentaires de l'invention apparaîtront encore à la lumière de la description plus détaillée qui suit de formes de réalisation de l'invention, données à titre purement illustratif et non limitatif.Additional advantages and characteristics of the invention will become apparent in the light of the more detailed description which follows of embodiments of the invention, given purely by way of non-limiting illustration.
Exemple.Example.
1) Installation.1) Installation.
L'adjuvant utilisé est du Nylon 11, disponible commercialement sous la dénomination RILSAN auprès de la société Atochem, France.The adjuvant used is Nylon 11, commercially available under the name RILSAN from the company Atochem, France.
Le filtre à bougies utilisé est constitué d'une zone d'alimentation conique, d'une virole cylindrique d'un diamètre de 215 mm et d'une hauteur de 2,05 m. Trois bougies de 32 mm de diamètre dont l'intérieur communique avec la zone de récolte du filtrat sont suspendues dans la virole. La hauteur des bougies est de 1 ,5 m et la distance entre leurs axes est de 86 mm, pour déposer un gâteau d'une épaisseur de 25 mm au maximum tout en préservant une distance de 15 mm entre la surface du gâteau et la paroi de la virole. Le volume total du filtre est de 78 1 et la surface de filtration de 0,45 m2. Le seuil de coupure des bougies est de 30 μm et le profil du fil trapézoïdal.The candle filter used consists of a conical feeding zone, a cylindrical shell with a diameter of 215 mm and a height of 2.05 m. Three 32 mm diameter candles, the interior of which communicates with the filtrate collection area, are suspended in the shell. The height of the candles is 1.5 m and the distance between their axes is 86 mm, to deposit a cake with a thickness of 25 mm maximum while preserving a distance of 15 mm between the surface of the cake and the wall of the shell. The total volume of the filter is 78 1 and the filtration area 0.45 m 2 . The spark plug cut-off threshold is 30 μm and the profile of the trapezoidal wire.
2) Filtration, 2.1) Dépôt de la précouche.2) Filtration, 2.1) Deposit of the precoat.
L'installation est en premier lieu stérilisée et désaérée avant le dépôt de la précouche qui est mené à un débit de 20 à 30 hl/hm2, et de la même manière que sur un filtre industriel. L'injection de la suspension de moût contenant le RILSAN est réalisée pendant 7 minutes en moyenne et une recirculation de 15 minutes permet de déposer la totalité de l'adjuvant. Si la stabilisation de la bière est effectuée en même temps que la filtration, la précouche est constituée d'un mélange de RILSAN® et de PVPP disponible commercialement auprès de la société Gaf, U.S.A.The installation is first of all sterilized and deaerated before depositing the precoat which is carried out at a flow rate of 20 to 30 hl / hm 2 , and in the same manner as on an industrial filter. The injection of the must suspension containing RILSAN is carried out for an average of 7 minutes and a recirculation of 15 minutes allows the entire adjuvant to be deposited. If the stabilization of the beer is effected simultaneously with the filtration, the precoat comprises a mixture of PVPP and RILSAN ® commercially available from GAF, USA
Dans ce cas, les proportions entre ces deux constituants (PVPP / RILSAN ) sont les mêmes que pour l'alluvionnage, à savoir 2/1 à 1/4 en poids, pour qu'après débâtissage, la composition de la masse filtrante régénérée ne soit pas modifiée. Indépendamment de l'addition de PVPP, la concentration en précouche atteint de 1 ,5 à 2 kg m , valeur supérieure aux teneurs recommandées conventionnellement, mais qui représente une épaisseur de gâteau sensiblement voisine de celle obtenue pour des adjuvants traditionnels.In this case, the proportions between these two constituents (PVPP / RILSAN) are the same as for alluvialization, namely 2/1 to 1/4 by weight, so that, after decompression, the composition of the regenerated filter mass is not changed. Regardless of the addition of PVPP, the pre-layer concentration reaches 1.5 to 2 kg m, a value greater than the levels recommended conventionally, but which represents a thickness of cake substantially close to that obtained for traditional adjuvants.
2.2) Filtration.2.2) Filtration.
Le choix du débit de filtration est conditionné par la montée en pression ainsi que par le temps de contact nécessaire pour obtenir un effet stabilisant suffisant. Pour ce faire, les installations de stabilisation au PVPP fonctionnent à un débit voisin de 10 hl hm2.The choice of filtration rate is conditioned by the pressure build-up as well as by the contact time necessary to obtain a sufficient stabilizing effect. To do this, the PVPP stabilization installations operate at a flow rate close to 10 hl hm 2 .
Un premier essai réalisé sur un filtre-plan, avec une bière de type Pils contenant un million de levures / ml additionnée d'un mélange de 25 à 200 g / hl de RILSAN® et de 50 g / hl de PVPP a donné lieu à une montée en pression variant entre 15000 et 30000 N.m'2 / heure selon la composition du mélange, le PVPP représentant entre 20 % et 67 % en poids de l'alluvionnage total. Pour des teneurs identiques en kieselguhr, une montée en pression supérieure à 80000 N.m" A first test carried out on a flat filter, with a Pils type beer containing a million yeasts / ml added with a mixture of 25 to 200 g / hl of RILSAN ® and 50 g / hl of PVPP gave rise to a pressure rise varying between 15,000 and 30,000 Nm '2 / hour depending on the composition of the mixture, the PVPP representing between 20% and 67% by weight of the total alluviation. For identical kieselguhr contents, a pressure rise greater than 80,000 Nm "
22
/ heure est constatée dans le mêmes conditions./ hour is noted under the same conditions.
Un deuxième essai est réalisé avec une bière de type Pils obtenue par darauflassen et dont la charge après centrifugation atteint 300 000 levures / ml. Elle conduit, pour une concentration totale en alluvionnage de 150 g/hl (100 g hl d'adjuvant et 50 g/hl de PVPP) à une différence de pression entre l'entrée et la sortie du filtre de 50000 N.m"2 après 20 heures de filtration et ce pour un débit deA second test is carried out with a Pils type beer obtained by darauflassen and whose load after centrifugation reaches 300,000 yeasts / ml. It leads, for a total concentration in alluviation of 150 g / hl (100 g hl of adjuvant and 50 g / hl of PVPP) to a pressure difference between the inlet and the outlet of the filter of 50,000 Nm "2 after 20 hours of filtration and this for a flow of
10 hl /hm2 10 hl / hm 2
11
Toujours à 10 hl m et pour la même teneur en alluvionnage, une bière dont la charge est de 5 millions de levures par ml conduit à une montée en pression de 35000 N.m"2 / heure.Still at 10 hl m and for the same alluvial content, a beer whose charge is 5 million yeasts per ml leads to a pressure increase of 35000 Nm "2 / hour.
2.3) Qualité de la bière.2.3) Quality of the beer.
La clarté de la bière après filtration répond aux normes en la matière. Elle est largement inférieure à 0,7° EBC, valeur recommandée et est, lors d'essais menés à basse température, inférieure à 0,5° EBC. Des valeurs de 0,3° EBC ont été régulièrement mesurées.The clarity of the beer after filtration meets the relevant standards. It is considerably lower than 0.7 ° EBC, recommended value and is, during tests carried out at low temperature, lower than 0.5 ° EBC. Values of 0.3 ° EBC were regularly measured.
" La stérilité de la filtration est vérifiée par prélèvement d'échantillons de 0,5 1 qui sont filtrés sur une membrane en nitrate de cellulose de 0,45 μm de seuil de coupure. La membrane est ensemencée à l'aide d'un milieu de culture de type malt extract agar et incubée à 30°C pendant 5 jours. Un seuil de 0 levure / 0,5 " The sterility of the filtration is checked by taking samples of 0.5 1 which are filtered on a cellulose nitrate membrane with a cut-off threshold of 0.45 μm. The membrane is seeded using a medium of culture of malt extract agar type and incubated at 30 ° C. for 5 days. A threshold of 0 yeast / 0.5
1 est atteint à la fin du vorlauf.1 is reached at the end of the vorlauf.
En comparant les caractéristiques de la bière avant et après filtration et indépendamment de la concentration en adjuvant, aucun phénomène d'adsorption par l'adjuvant de filtration selon l'invention n'est détectable, en particulier en ce qui concerne la couleur et la teneur en isohumulones. De plus, l'ajout de 50 g / hl de PVPP à l'alluvionnage conduit à une réduction de 50 % en concentration des polyphénols totaux même en présence de levures.By comparing the characteristics of the beer before and after filtration and independently of the concentration of adjuvant, no adsorption phenomenon by the filter aid according to the invention is not detectable, in particular as regards the color and the content of isohumulones. In addition, the addition of 50 g / hl of PVPP to alluviation leads to a reduction of 50% in the concentration of total polyphenols even in the presence of yeasts.
Deux bières de référence, l'une étant filtrée avec le procédé selon l'invention, l'autre avec un procédé conventionnel ont été soumises à une dégustation par un groupe de huit experts. Aucune différence significative de goût n'a été détectée.Two reference beers, one being filtered with the process according to the invention, the other with a conventional process, were subjected to tasting by a group of eight experts. No significant difference in taste was detected.
Les résultats obtenus sont résumés dans le tableau I figurant en annexe de la présente demande de brevet.The results obtained are summarized in Table I appearing in the appendix to this patent application.
2.4) Régénération,2.4) Regeneration,
Un lavage de la masse filtrante réalisé dans l'outil de filtration et sans débâtissage avec une solution de soude à 2 % à une température de 80°C a entraîné une réduction de la taille des levures de 40 % après deux heures de traitement.A washing of the filtering mass carried out in the filtration tool and without defatting with a 2% sodium hydroxide solution at a temperature of 80 ° C. resulted in a reduction in the size of the yeasts by 40% after two hours of treatment.
Ces déchets demeurent trop gros pour pouvoir être éliminés du gâteau par simple lavage et provoquent en s'accumulant un accroissement de la montée en pression durant la filtration. Ainsi, pour une bière, contenant initialement un million de levures / ml, filtrée à un débit de 10 hl / hm en présence de 50 g / hl de RILSAN® et de 50 g / hl de PVPP, la montée en pression varie d'un facteur trois après cinq cycles.This waste remains too large to be able to be removed from the cake by simple washing and cause, by accumulating, an increase in pressure build-up during filtration. Thus for one beer, initially containing one million yeasts / ml, filtered at a flowrate of 10 hl / hm in the presence of 50 g / hl of RILSAN ® and 50 g / hl of PVPP, the pressure rise varied from a factor of three after five cycles.
Un traitement enzymatique permet de remédier à cette situation, en réduisant la taille des levures de 25 % à 35 % après traitement pendant deux à trois heures. Le traitement enzymatique est réalisé en lavant la masse filtrante par une solution d'enzymes disponible commercialement sous la dénomination YLE auprès de la société Amano. Le traitement enzymatique est effectué à un pH de 5- 6 et à une température de 50°C après l'attaque à la soude, ce qui implique de ramener pH et température aux valeurs ci-dessus.An enzymatic treatment makes it possible to remedy this situation, by reducing the size of the yeasts from 25% to 35% after treatment for two to three hours. The enzymatic treatment is carried out by washing the filtering mass with an enzyme solution commercially available under the name YLE from the company Amano. The enzymatic treatment is carried out at a pH of 5-6 and at a temperature of 50 ° C. after the attack with sodium hydroxide, which implies bringing the pH and temperature to the above values.
Les déchets de cette lyse sont ensuite éliminés par un second lavage à la soude. La périodicité du traitement enzymatique dépend de la charge initiale de la bière avant filtration, du type de filtre utilisé et de la longueur de cycle souhaitée.The waste from this lysis is then removed by a second washing with soda. The frequency of the enzyme treatment depends on the initial charge of the beer before filtration, the type of filter used and the desired cycle length.
Exemple comparatif.Comparative example.
Les volumes de bière filtrée par le procédé de l'invention et par un procédé de filtration conventionnel ont été comparés par extrapolation, sur une unité de filtration constituée d'un filtre unique à bougies. Dans cet essai comparatif, la surface de filtration est de 80 m2 et permet de déposer un gâteau d'un volume de 3 m avec une distance entre les gâteaux déposés sur les bougies de 5 mm en fin de filtration.The volumes of beer filtered by the process of the invention and by a conventional filtration process were compared by extrapolation, on a filtration unit consisting of a single candle filter. In this comparative test, the filtration surface is 80 m 2 and makes it possible to deposit a cake with a volume of 3 m with a distance between the cakes deposited on the candles of 5 mm at the end of filtration.
La charge de la bière avant filtration est supposée être de un million de levures / ml et le débit de filtration est de 10 hl / hm . Le volume filtré par cycle est calculé de façon à ce que le volume laissé libre pour les bourbes soit totalement rempli en fin de cycle et que la différence de pression finale ne dépasse pas 400000 N.m' , valeur permettant une contre-pression importante.The beer load before filtration is assumed to be one million yeasts / ml and the filtration rate is 10 hl / hm. The volume filtered per cycle is calculated so that the volume left free for the sludge is completely filled at the end of the cycle and that the final pressure difference does not exceed 400,000 Nm ' , a value allowing a significant back pressure.
Pour une teneur en alluvionnage (a) donnée, le volume filtré par cycleFor a given alluvial content (a), the volume filtered by cycle
(Vf) est c aallccuulléé àà ppaarrttiirr dduu vvoolluummee lliibbrree ppoouurr llee ggââtteeaauu (3 m ) et de la concentration en adjuvant de la précouche (ap) selon la réaction : 3 pas - 80 a? (Vf) is c aallccuulléé àà ppaarrttiirr dduu vvoolluummee lliibbrree ppoouurr llee ggââtteeaauu (3 m) and the adjuvant concentration of the precoat (a p ) according to the reaction: 3 steps - 80 a ?
Vf =Vf =
dans laquelle pGS représente la masse spécifique apparente du gâteau.in which p GS represents the apparent specific mass of the cake.
La pression finale est alors calculée selon la loi de fonctionnement relative à une filtration cylindrique menée à débit constant, telle décrite par J. Hermia et al., dans Filtration and Séparation, 1994, 31, 721-725.The final pressure is then calculated according to the operating law relating to a cylindrical filtration carried out at constant flow rate, as described by J. Hermia et al., In Filtration and Separation, 1994, 31, 721-725.
Les résultats sont illustrés dans le tableau II figurant en annexe de la présente demande de brevet.The results are illustrated in Table II appearing in the appendix to this patent application.
Dans le tableau II, Zp désigne le poids d'adjuvant par mètre carré de surface; a désigne le poids d'adjuvant par hl de bière; pGS désigne la masse apparente spécifique du gâteau; Δ P désigne la perte de charge du gâteau; t le temps de filtration et Vf le volume filtré.In Table II, Z p denotes the weight of additive per square meter of surface; a denotes the weight of adjuvant per hl of beer; p GS denotes the specific apparent mass of the cake; Δ P denotes the pressure drop of the cake; t the filtration time and Vf the filtered volume.
Outre l'avantage de pouvoir régénérer in situ la masse filtrante, le nouveau procédé selon l'invention permet de filtrer des volumes généralement plus importants de bière que les procédés conventionnels.In addition to the advantage of being able to regenerate the filter mass in situ, the new method according to the invention makes it possible to filter generally larger volumes of beer than conventional methods.
Il va de soi que l'invention ne se limite nullement aux formes de réalisation qui viennent d'être décrites dans ce qui précède et qui sont données à titre purement illustratif et non limitatif, mais en embrasse au contraire toutes les variantes.It goes without saying that the invention is in no way limited to the embodiments which have just been described in the foregoing and which are given purely by way of illustration and not limitation, but on the contrary embraces all variants thereof.
Ainsi, bien que l'invention ait été décrite dans ce qui précède plus particulièrement en utilisant la technique de filtration en alluvionnage, les nouveaux adjuvants et supports de l'invention et les procédés de filtration et de régénération de l'invention peuvent être utilisés avec la même efficacité dans la technique de filtration en précouche. L'homme du métier aura toute possibilité d'apporter des modifications à la présente invention, relevant de la simple mise au point de l'invention, sans pour autant sortir du cadre de ses éléments caractéristiques, tel que défini dans les revendications qui suivent. Thus, although the invention has been described in the foregoing more particularly using the alluvial filtration technique, the new adjuvants and supports of the invention and the filtration and regeneration methods of the invention can be used with the same efficiency in the pre-layer filtration technique. A person skilled in the art will have every possibility of making modifications to the present invention, pertaining to the simple development of the invention, without going beyond the scope of its characteristic elements, as defined in the claims which follow.
AnnexeAnnex
Tableau I.Table I.
Caractéristiques de la bière filtrée.Characteristics of filtered beer.
Essai avec RILSAN*" seul Essai avec mélange RILSAN*1 / PVPPTest with RILSAN * "only Test with mixture RILSAN * 1 / PVPP
Bière non filtrée Bière filtrée Bière non filtrée Bière filtréeUnfiltered beer Filtered beer Unfiltered beer Filtered beer
Couleur (EBC) 6,2 6,1 5,4 5,0Color (EBC) 6.2 6.1 5.4 5.0
Isohumulones 23,1 22,8 23,3 22,9 (EBU)Isohumulones 23.1 22.8 23.3 22.9 (EBU)
Polyphénols 196 184 200 90 (mg / 1)Polyphenols 196 184 200 90 (mg / 1)
Tableaij H,Tableaij H,
Volumes filtrés selon le tvpe d'alluvionnage.Volumes filtered according to the alluvial tvpe.
Figure imgf000023_0001
Figure imgf000023_0001

Claims

Revendications. Claims.
1. Adjuvants de filtration régénérables, utilisables pour la filtration de liquide, notamment de bière fin de garde, caractérisés en ce qu'ils comprennent des grains polymériques incompressibles synthétiques ou naturels ou des grains incompressibles naturels possédant un coefficient de sphéricité variant entre environ 0,6 et environ 0,9.1. Regenerable filter aids, usable for the filtration of liquid, in particular fine beer, characterized in that they comprise synthetic or natural incompressible polymer grains or natural incompressible grains having a sphericity coefficient varying between approximately 0, 6 and about 0.9.
2. Adjuvants de filtration selon la revendication 1, caractérisés en ce qu'ils comprennent des grains d'une taille moyenne variant entre environ 20 μm et environ 70 μm, formant un gâteau de filtration d'une porosité comprise entre environ 0,4 et environ 0,8 et d'une masse spécifique variant entre environ2. Filtration aids according to claim 1, characterized in that they comprise grains of an average size varying between approximately 20 μm and approximately 70 μm, forming a filtration cake with a porosity of between approximately 0.4 and about 0.8 and a specific mass varying between about
1000 et environ 1500 kg/m3.1000 and around 1500 kg / m 3 .
3. Adjuvants de filtration selon la revendication 2, caractérisés en ce qu'ils comprennent des grains d'une taille moyenne variant entre environ 20 μm avec un écart-type d'environ 10 μm et environ 70 μm avec un écart-type d'environ 25 μm.3. Filtration aids according to claim 2, characterized in that they comprise grains of an average size varying between approximately 20 μm with a standard deviation of approximately 10 μm and approximately 70 μm with a standard deviation of about 25 μm.
4. Adjuvants de filtration selon l'une quelconque des revendications 1 à 3, caractérisés en ce qu'ils comprennent des grains d'une taille moyenne d'environ 35 μm avec un écart-type d'environ 15 μm et d'une masse spécifique d'environ 1200 kg/m3.4. Filtration aids according to any one of claims 1 to 3, characterized in that they include grains with an average size of approximately 35 μm with a standard deviation of approximately 15 μm and with a mass specific around 1200 kg / m 3 .
5. Adjuvants de filtration selon l'une quelconque des revendications 1 à 4, caractérisés en ce que les grains polymériques synthétiques ou naturels ou les grains incompressibles naturels sont des grains obtenus notamment à partir de polyamide, de polychlorure de vinyle, de produits fluorés, de polypropylène, de polystyrène, de polyéthylène, de certains dérivés de silice, par exemple de ryolites, de verre, ainsi que leurs mélanges.5. Filtration aids according to any one of claims 1 to 4, characterized in that the synthetic or natural polymer grains or the natural incompressible grains are grains obtained in particular from polyamide, polyvinyl chloride, fluorinated products, polypropylene, polystyrene, polyethylene, certain silica derivatives, for example ryolites, glass, as well as their mixtures.
6. Adjuvants de filtration selon l'une quelconque des revendications 1 à 5, caractérisés en ce que les grains de polyamide consistent de préférence en des grains de polycaprolactame, d'adipamide de poly(hexaméthylène), de nonanediamide de poly(hexaméthylène), de sébacamide de poly(hexaméthylène), de dodécanodiamide de poly(hexaméthylène), de polyundécanolactame, de polylauryllactame et/ou leurs mélanges.6. Filtration aids according to any one of claims 1 to 5, characterized in that the polyamide grains preferably consist of grains of polycaprolactam, of adipamide of poly (hexamethylene), of nonanediamide of poly (hexamethylene), poly (hexamethylene) sebacamide, poly (hexamethylene) dodecanodiamide, polyundecanolactam, polylauryllactam and / or mixtures thereof.
7. Adjuvants de filtration selon l'une quelconque des revendications 1 à 6, caractérisé en ce que les grains consistent en des grains de polyundécanolactame.7. filter aids according to any one of claims 1 to 6, characterized in that the grains consist of polyundecanolactam grains.
8. Procédé de filtration d'un liquide, notamment de bière fin de garde comprenant des étapes de désaération, de dépôt d'une précouche sur un support de filtration, de recirculation, caractérisé en ce que l'étape de filtration est réalisée avec un adjuvant de filtration selon l'une quelconque des revendications 1 à 7.8. A method of filtering a liquid, especially fine beer, comprising deaeration steps, depositing a precoat on a filtration support, recirculating, characterized in that the filtration step is carried out with a filter aid according to any one of claims 1 to 7.
9. Procédé de filtration selon la revendication 8, caractérisé en ce que la proportion entre l'adjuvant de filtration et le liquide à filtrer varie entre environ 25 g d'adjuvant / hl de liquide et environ 250 g d'adjuvant / hl de liquide.9. A filtration method according to claim 8, characterized in that the proportion between the filter aid and the liquid to be filtered varies between approximately 25 g of aid / hl of liquid and approximately 250 g of aid / hl of liquid .
10. Procédé de filtration selon la revendication 8 ou 9, caractérisé en ce qu'il comprend de plus une étape de stabilisation.10. A filtration method according to claim 8 or 9, characterized in that it further comprises a stabilization step.
11. Procédé de filtration selon la revendication 10, caractérisé en ce que l'étape de stabilisation est réalisée de façon concomittante avec l'étape de filtration. P 549711. The filtration method according to claim 10, characterized in that the stabilization step is carried out concomitantly with the filtration step. P 5497
12. Procédé de filtration selon la revendication 10 ou 11, caractérisé en que l'étape de stabilisation comprend l'utilisation d'un agent de stabilisation, par exemple du PVPP.12. The filtration method according to claim 10 or 11, characterized in that the stabilization step comprises the use of a stabilizing agent, for example PVPP.
13. Procédé de filtration selon l'une quelconque des revendications 8 à 12, caractérisé en ce qu'il comprend de plus, après l'étape de filtration de la bière, une étape de régénération in situ de l'adjuvant de filtration, comprenant les étapes consistant à : - laver le milieu filtrant avec une solution de soude, à une concentration variant entre environ 2 % et environ 5 %, à une température d'au moins environ 80°C, pendant une durée variant entre environ 60 rninutes et environ 120 minutes, et13. A filtration method according to any one of claims 8 to 12, characterized in that it further comprises, after the beer filtration step, a step of in situ regeneration of the filtration aid, comprising the steps consisting in: washing the filtering medium with a sodium hydroxide solution, at a concentration varying between approximately 2% and approximately 5%, at a temperature of at least approximately 80 ° C., for a period varying between approximately 60 minutes and about 120 minutes, and
- effectuer un traitement enzymatique du milieu filtrant avec une composition enzymatique, à une température variant entre environ 40°C et environ 60°C, pendant une durée variant entre environ 100 minutes et environ 200 minutes, ledit traitement enzymatique étant réalisé après plusieurs cycles de filtration.carrying out an enzymatic treatment of the filtering medium with an enzymatic composition, at a temperature varying between approximately 40 ° C. and approximately 60 ° C., for a duration varying between approximately 100 minutes and approximately 200 minutes, said enzymatic treatment being carried out after several cycles of filtration.
14. Procédé de filtration selon la revendication 13, caractérisé en ce que la composition enzymatique comprend des protéases, des agents capables de lyser les levures, éventuellement des agents de catalyse enzymatique.14. The filtration method according to claim 13, characterized in that the enzymatic composition comprises proteases, agents capable of lysing yeasts, optionally agents of enzymatic catalysis.
15. Procédé de filtration selon la revendication 13 ou 14, caractérisé en ce que le traitement enzymatique est réalisé lorsque la montée en pression par heure devient trop importante et significativement plus élevée qu'avec un adjuvant de filtration non encrassé.15. Filtration method according to claim 13 or 14, characterized in that the enzymatic treatment is carried out when the pressure increase per hour becomes too great and significantly higher than with an unclogged filter aid.
16. Procédé de filtration selon la revendication 15, caractérisé en ce que le traitement enzymatique est réalisé quand la montée en pression dans la cuve de filtration atteint environ 80 % de la pression maximale autorisée par la construction mécanique du filtre.16. A filtration method according to claim 15, characterized in that the enzymatic treatment is carried out when the pressure rise in the filtration tank reaches approximately 80% of the maximum pressure authorized by the mechanical construction of the filter.
17. Procédé de filtration selon l'une quelconque des revendications 8 à 16, caractérisé en ce que le support de filtration comprend des bougies comprenant un fil enroulé en spires autour d'un support vertical, la distance entre deux spires variant entre environ 20 μm et environ 70 μm, de préférence entre environ 20 μm et environ 45 μm.17. A filtration method according to any one of claims 8 to 16, characterized in that the filtration support comprises candles comprising a wire wound in turns around a vertical support, the distance between two turns varying between approximately 20 μm and approximately 70 μm, preferably between approximately 20 μm and approximately 45 μm.
18. Procédé de filtration selon la revendication 17, caractérisé en ce que le fil enroulé en spires a une forme trapézoïdale, le grand côté du trapèze étant dirigé vers l'extérieur du filtre à bougies, du côté de la matière à filtrer.18. The filtration method according to claim 17, characterized in that the wire wound in turns has a trapezoidal shape, the long side of the trapezium being directed towards the outside of the candle filter, on the side of the material to be filtered.
19. Procédé de filtration selon l'une quelconque des revendications 8 à 16, caractérisé en ce que le support de filtration comprend des tamis, de préférence horizontaux, d'une grandeur de maille variant entre environ 10 μm et environ 70 μm, de préférence entre environ 10 μm et environ 20 μm.19. A filtration method according to any one of claims 8 to 16, characterized in that the filtration medium comprises sieves, preferably horizontal, with a mesh size varying between approximately 10 μm and approximately 70 μm, preferably between approximately 10 μm and approximately 20 μm.
20. Procédé de filtration selon selon l'une quelconque des revendications 17 à 19, caractérisé en ce que les fils ou les tamis sont réalisés à partir de matière de qualité alimentaire résistante aux réactifs utilisés dans le procédé de filtration.20. A filtration method according to any one of claims 17 to 19, characterized in that the son or the sieves are made from food-grade material resistant to the reagents used in the filtration process.
21. Procédé de régénération in situ d'un adjuvant de filtration caractérisé en ce qu'il comprend les étapes consistant à :21. A method of in situ regeneration of a filter aid, characterized in that it comprises the steps consisting in:
- laver le milieu filtrant avec une solution de soude, à une concentration variant entre environ 2 % et environ 5 %, à une température d'au moins environ 80°C, pendant une durée variant entre environ 60 minutes et environ 120 minutes, et - effectuer un traitement enzymatique du milieu filtrant avec une composition enzymatique, à une température variant entre environ 40°C et environ 60°C, pendant une durée variant entre environ 100 minutes et environ 200 minutes, ledit traitement enzymatique étant réalisé après plusieurs cycles de filtration.washing the filter medium with a sodium hydroxide solution, at a concentration varying between approximately 2% and approximately 5%, at a temperature of at least approximately 80 ° C., for a period varying between approximately 60 minutes and approximately 120 minutes, and carrying out an enzymatic treatment of the filtering medium with an enzymatic composition, at a temperature varying between approximately 40 ° C. and approximately 60 ° C., for a duration varying between approximately 100 minutes and approximately 200 minutes, said enzymatic treatment being carried out after several cycles of filtration.
22. Procédé de régénération selon la revendication 21, caractérisé en ce que la composition enzymatique comprend des protéases, des agents capables de lyser les levures, éventuellement des agents de catalyse enzymatique.22. A regeneration method according to claim 21, characterized in that the enzymatic composition comprises proteases, agents capable of lysing yeasts, optionally agents of enzymatic catalysis.
23. Procédé de régénération selon la revendication 21 ou 22, caractérisé en ce que le traitement enzymatique est réalisé quand la montée en pression par heure devient trop importante et significativement plus élevée qu'avec un adjuvant de filtration non encrassé.23. Regeneration method according to claim 21 or 22, characterized in that the enzymatic treatment is carried out when the pressure build-up per hour becomes too great and significantly higher than with an unclogged filter aid.
24. Procédé de régénération selon la revendication 23, caractérisé en ce que le traitement enzymatique est réalisé quand la montée en pression dans la cuve de filtration atteint environ 80 % de la pression maximale autorisée par la construction mécanique du filtre.24. A regeneration method according to claim 23, characterized in that the enzymatic treatment is carried out when the pressure increase in the filtration tank reaches approximately 80% of the maximum pressure authorized by the mechanical construction of the filter.
25. Procédé de régénération selon l'une quelconque des revendications 21 à 24, caractérisé en ce que l'adjuvant consiste en un adjuvant selon l'une quelconque des revendications 1 à 7.25. Regeneration method according to any one of claims 21 to 24, characterized in that the adjuvant consists of an adjuvant according to any one of claims 1 to 7.
26. Support de filtration, caractérisé en ce qu'il comprend des bougies comprenant un fil réalisé à partir de matière de qualité alimentaire résistante aux réactifs utilisés dans le procédé de filtration, enroulé en spires autour d'un support vertical, la distance entre deux spires variant entre environ 20 μm et environ 70 μm, de préférence entre environ 20 μm et environ 45 μm. 26. Filtration support, characterized in that it includes candles comprising a wire made from food-grade material resistant to the reagents used in the filtration process, wound in turns around a vertical support, the distance between two turns varying between approximately 20 μm and approximately 70 μm, preferably between approximately 20 μm and approximately 45 μm.
27. Support de filtration selon la revendication 26, caractérisé en ce que le fil enroulé en spires a une forme trapézoïdale, le grand côté du trapèze étant dirigé vers l'extérieur du filtre à bougies, du côté de la matière à filtrer.27. Filtration support according to claim 26, characterized in that the wire wound in turns has a trapezoidal shape, the long side of the trapezium being directed towards the outside of the candle filter, on the side of the material to be filtered.
28. Support de filtration, caractérisé en ce qu'il comprend des tamis, de préférence horizontaux, réalisés à partir de matière de qualité alimentaire résistante aux réactifs utilisés dans le procédé de filtration, d'une grandeur de maille variant entre environ 10 μm et environ 70 μm, de préférence entre environ 10 μm et environ 20 μm. 28. Filtration support, characterized in that it comprises sieves, preferably horizontal, made from food-grade material resistant to the reagents used in the filtration process, with a mesh size varying between approximately 10 μm and approximately 70 μm, preferably between approximately 10 μm and approximately 20 μm.
PCT/IB1996/000440 1995-05-12 1996-05-10 Filtration adjuvants, filtration supports, filtration process using them and process for regenerating said adjuvants WO1996035497A1 (en)

Priority Applications (11)

Application Number Priority Date Filing Date Title
DE69614534T DE69614534T2 (en) 1995-05-12 1996-05-10 METHOD FOR REGENERATING FILTER TOOLS AND FILTRATION METHOD USING THE SAME
DK96911085T DK0831960T3 (en) 1995-05-12 1996-05-10 Process for regenerating filter adjuvants and method utilizing such a method for regeneration
US08/952,142 US6117459A (en) 1995-05-12 1996-05-10 Filtration adjuvants, filtration supports, filtration process using them and process for regenerating said adjuvants
AU54075/96A AU709244C (en) 1995-05-12 1996-05-10 Filtration adjuvants, filtration supports, filtration process using them and process for regenerating said adjuvants
JP53392096A JP3667342B2 (en) 1995-05-12 1996-05-10 Filtration aid, filtration method using the same, and regeneration method of the filtration aid
AT96911085T ATE204197T1 (en) 1995-05-12 1996-05-10 METHOD FOR REGENERATING FILTER AID AND FILTRATION METHOD USING THE SAME
KR1019970708059A KR100356575B1 (en) 1995-05-12 1996-05-10 Filtration aid, filtration support, filtration method using these, and regeneration method of filtration aid
EP96911085A EP0831960B1 (en) 1995-05-12 1996-05-10 Process for regenerating filtration adjuvants and filtration process using such a regeneration process
CA2220445A CA2220445C (en) 1995-05-12 1996-05-10 Filtration adjuvants, filtration supports, filtration process using them and process for regenerating said adjuvants
HU9802386A HU228585B1 (en) 1995-05-12 1996-05-10 Filtration adjuvants, filtration supperts, filtration process using them and process for regenerating said adjuvants
BR9608304A BR9608304A (en) 1995-05-12 1996-05-10 Filtration aids filtration media filtration process that uses them and regeneration process for those aids

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR95/05636 1995-05-12
FR9505636A FR2733922B1 (en) 1995-05-12 1995-05-12 NOVEL FILTRATION ADJUVANTS, NOVEL FILTRATION MEDIA, FILTRATION METHOD USING THE SAME AND REGENERATION METHOD OF THE SAME
FR9513731A FR2733920B1 (en) 1995-05-12 1995-11-20 METHOD FOR REGENERATING FILTRATION ADJUVANTS

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AU2001295620B2 (en) * 2000-10-16 2005-11-10 Basf Aktiengesellschaft Use of polymers as filtering aids and/or stabilizers
WO2002032544A1 (en) * 2000-10-16 2002-04-25 Basf Aktiengesellschaft Use of polymers as filtering aids and/or stabilizers
US6733680B2 (en) 2000-12-27 2004-05-11 Basf Aktiengesellschaft Use of particulate polymers as filter aids for aqueous liquids
US6736981B2 (en) 2001-02-21 2004-05-18 Basf Aktiengesellschaft Particulate polymers as filter aids
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WO2003084639A2 (en) * 2002-04-05 2003-10-16 Basf Aktiengesellschaft Use of polymers comprising thermoplastic polymers as filtration aids and/or stabilising agent
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WO2005113738A1 (en) * 2004-05-18 2005-12-01 Inbev S.A. Method of preparing a liquid, containing proteins for subsequent separation, by using one or more protein-complexing agents
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WO2008037777A1 (en) * 2006-09-29 2008-04-03 Basf Se Method for regenerating an auxiliary filtering agent
US7993533B2 (en) 2006-09-29 2011-08-09 Basf Se Method for regenerating an auxiliary filtering agent
US8394279B2 (en) 2007-03-15 2013-03-12 Basf Se Method for regenerating a filter aid
WO2020188222A1 (en) * 2019-03-20 2020-09-24 Arkema France Filtration adjuvant
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