Classifications

• • 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
  • 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
  • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
  • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
  • B01J20/14—Diatomaceous earth
• • 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
  • B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
• • 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

Definitions

• the present invention relates to a method for regenerating spent diatomaceous earth, used as a filtration aid, as well as to an installation for regenerating spent diatomaceous earth.
• the diatomaceous earth also known as kieselguhr, is a variety of powdery silica formed from microscopic shells of very small animals, fossil diatomaceous earths, known as diatoms.
• the shells that form the kieselguhr have very varied shapes (circular, elliptical, rectangular, lozenge), since there are 5000 different species of diatoms. With a chalky appearance and a whitish color, the diatomaceous earth has a low density. Very porous, it is capable of absorbing large quantities of liquid. It is widely used in industry as an absorbent, catalyst support, abrasive, filler, but especially as a filtration aid.
• beer In the brewing industry, beer must most often be obtained in the form of a limpid and clear product, of appearance acceptable to the consumer. It is therefore necessary to eliminate the colloids and yeasts which are responsible for the cloudiness of beer, by a filtration stage at the end of fermentation.
• this filtration is carried out in closed enclosures comprising filtering interfaces (filtration media), the diatomaceous earth being used as a filtration aid. Its role is to increase the total filtration area. It also allows, by its porosity of the order of a micrometer, to use filtration grids less tight meshes (typically, the mesh size is around 70 ⁇ m ⁇ 30 ⁇ m) which results in less pressure drop.
• filtering interfaces filtration media
• the diatomaceous earth being used as a filtration aid. Its role is to increase the total filtration area. It also allows, by its porosity of the order of a micrometer, to use filtration grids less tight meshes (typically, the mesh size is around 70 ⁇ m ⁇ 30 ⁇ m) which results in less pressure drop.
• the diatomaceous earth retains colloids, yeasts and other waste, mainly of an organic nature. It becomes more and more loaded with organic residues, which leads to a pressure drop and therefore requires an increase in the pressure at the inlet of the filter. It then becomes necessary to remove the exhausted diatomaceous earth from the filtration media, either to replace it with virgin diatomaceous earth, or to regenerate it for reuse.
• the aim of the present invention is therefore to design a process for the regeneration of a depleted diatomaceous earth which better meets the needs of the practice than the previously known processes, in particular in that the process according to the invention: is more economical than the processes of the prior art, - does not imply a longer immobilization of the filter than in previously existing processes,
• the subject of the invention is a method of regenerating spent diatomaceous earth, said diatomaceous earth being used as a filtration aid and being retained in the enclosure of a filter, said method comprising a step of introducing of an alkaline solution inside the filter enclosure, with contacting said solution with the diatomaceous earth to be regenerated, characterized in that said process is followed by a recovery step, at outside the filter enclosure, diatomaceous earth regenerated for reuse, during a subsequent filtration of beer, as a filter aid, said regenerated diatomaceous earth being introduced into the enclosure of the filter as a mixture with the beer to be filtered.
• the regeneration described above is carried out by elimination of organic waste accumulated in the diatomaceous earth during filtration.
• the organic waste accumulated in the diatomaceous earth during filtration are, for example, proteins, yeasts, tannins, polyphenols and various colloids present in beer following its fermentation.
• the recovery, outside of the filter enclosure, regenerated diatomaceous earth includes a step of opening the filter enclosure.
• Any filter whose enclosure is capable of chemically withstanding contact with an alkaline solution can be used to carry out the method according to the present invention. Mention may be made, by way of nonlimiting examples, of metal filters with candles or trays.
• said filter is a candle filter.
• the process for regenerating the spent diatomaceous earth comprises the following steps:
• step (a) Rinsing the filter with water at the temperature indicated in step (a) makes it possible in particular to remove part of the organic matter accumulated in the diatomaceous earth and to make the latter less compact, therefore more permeable.
• step (c) it makes it possible to eliminate the alkaline solution introduced. in the filter enclosure during step (b) and the silicates formed by the attack in an alkaline medium of the silica constituting the diatomaceous earth.
• Step (d) of rinsing the filter with an acid solution makes it possible on the one hand to neutralize the diatomaceous earth in the enclosure of the filter by reacting with the residual alkaline solution, and on the other hand hydrolyze the polysaccha ⁇ des which would possibly still be present in the diatomaceous earth.
• said acid solution is carbonated deaerated water.
• the term "deaerated” means water which does not contain dissolved oxygen in gaseous form. Such water can be obtained for example by passing carbon dioxide against the flow of water. Typically, this operation is carried out in a deaeration column. It makes it possible to obtain water in which the gaseous dioxygen has been eliminated and which contains dissolved carbon dioxide, called carbonated deaerated water.
• the method according to the present invention comprises, between steps (b) and (c), a step (e) of recirculation, in a closed circuit, of a volume of alkaline solution equal to the internal volume of the filter minus the volume occupied by the diatomaceous earth.
• said method comprises, between steps (e) and (c), a step (f) of introducing into the filter a new volume of alkaline solution equal to the internal volume of the filter minus the volume occupied by the earth diatom.
• new volume of alkaline solution is meant a volume of "virgin” alkaline solution, which has not been subjected to recirculation in a closed circuit as described above.
• Said alkaline solution is for example introduced at a temperature of 35 to 95 ° C, preferably about 75 ° C. Such a temperature makes it possible to favor the hydrolysis reactions of proteins and to make more effective the degradation of the organic matters present within the diatomaceous earth. In addition, it can possibly ensure, in a single step, the regeneration of the diatomaceous earth and its sterilization.
• Said alkaline solution is for example a sodium hydroxide solution of 0.1 to 15%, preferably about 1% (V / V).
• the method as described above effectively makes it possible, by treatment m if you of the spent diatomaceous earth, to regenerate the latter at a lower cost and without immobilizing the filter longer than in the methods previously known (masked time).
• the method according to the present invention makes it possible to ensure, in a single step, the regeneration of the diatomaceous earth and the sterilization of the filter.
• the costs associated with transporting the depleted diatomaceous earth or the ancillary facilities required to process it are avoided.
• Such a process also makes it possible to avoid the rejection of the soil of diatomaceous earth exhausted in a purification station or in a calcination installation and proves to be less polluting for the environment.
• the efficiency of the process according to the invention also makes it possible to reuse the regenerated diatomaceous earth at least once as a filtration aid, in a new filtration cycle, the regenerated diatomaceous earth being introduced into the filter enclosure as a mixture with the beer to be filtered.
• the present invention therefore also relates to a beer filtration process using a diatomaceous earth as a filter aid, characterized in that it comprises the following stages:
• the subject of the present invention is a device for filtering beer comprising an enclosure in which are arranged means capable of retaining diatomaceous earth used as filter aid and filtration residues, means of supply in the enclosure of an alkaline solution for reacting with said filtration residues and means for discharging said alkaline solution charged with at least a portion of said filtration residues, characterized in that said device also comprises means for introduction of a mixture of mussusoires / beer to be filtered, said diatomaceous earth being a diatomaceous earth regenerated by the process described above.
• said means capable of retaining diatomaceous earth used as filter aid and filtration residues consist of a candle filter.
• the latter further comprises means for circulating in a closed circuit the alkaline solution through said enclosure.
• the invention also comprises other arrangements which will emerge from the description which follows, which refers to examples of implementation of the present invention, as well as to the appended drawing, which represents an installation. according to the present invention.
• Figure 1 is a schematic view of a beer filtration installation according to one invention.
• FIG. 1 we can see an installation according to the present invention of beer filtration comprising regeneration means m if you filter aids, especially diatomaceous earth.
• the installation comprises a filter 1, for example a filter with trays or, advantageously, a candle filter having for example a volume of 4 m and a filtering surface of 80 m 2 (388 , allowing to filter from 5.5.10 ⁇ 3 to 11.10 ⁇ 3 m / s of beer for a maximum pressure difference of 5.10 5 Pa.
• An inlet 3 of the filter 1 is connected by a valve 5 to a pipe 7 for supplying the beer to be filtered equipped with a device 9 for distributing diatomaceous earth, thus a mixture of diatomaceous earth / beer to be filtered introduced into inlet 3 of filter 1.
• the maximum quantity of diatomaceous earth injected is 320 kg.
• An outlet 11 of the filter 1 is connected by a valve 13 and a pipe 15 to an inlet 17 of a buffer tank 19, making it possible to avoid pressure surges.
• a valve 21 mounted at an outlet 23 of the tank 19 makes it possible either to send the filtered beer, by a valve 22, to a tank (not shown in FIG.
• the installation according to the present invention furthermore comprises means for regenerating spent diatomaceous earth, that is to say too loaded with filtration residues and consequently inducing excessive pressure drops.
• the preferred embodiment example of installations illustrated in FIG. 1 comprises a tank 25 of carbonated deaerated water connected by a valve 2 ⁇ to the outlet 11 of the filter 1 and by a valve 26 to the inlet 3 of the filter 1, a tank 29 of alkaline reagent, preferably sodium hydroxide, fed by a valve 31 at the inlet 3 of the filter 1, a tank 33 for recovering alkaline reagent connected by a valve 35 to the inlet 3 of the filter 1 and by a valve 37 ⁇ the 11 filter output 1 and a tank 39 for hot water connected by a valve 41 to the inlet 3 of the filter 1.
• a line 43 and valve 45 allow the discharge of the content filter 1 to the sewer, to a storage bath, or to a treatment plant.
• a pipe 47 and a valve 49 allow the evacuation of the contents of the filter, for example regenerating filtration aid, in a preparation tank 55, as will be described in more detail below.
• the installation may also include hot water or desaeree water recovery tanks (not shown) allowing the circulation in a closed circuit of these fluids through the filter 1.
• the installation also includes equipment not shown such as heating means, thermal insulation means, pumping means for ensuring the circulation of the desired fluids and remote control means from a control room of the valve brewery 5, 13, 21, 22, 24, 26, 27, 31, 35, 37, 41, 45, 49, pumping means and heating means to ensure the desired circulation of the various fluids at temperatures of instructions.
• the device further comprises safety means or a programmable automaton for controlling the installation preventing an accidental command to open a valve causing undesired circulation of fluid.
• the valves a programmable automaton
• valves 41 and 45 are open, the other valves being closed.
• valve 31 and / or the valve 35 as well as the valve 45 are open, the other valves being closed.
• valves 31 and / or 35 and the valve 37 are open, the other valves being closed.
• the valve 27 When introducing the deaerated water, via the outlet 11 of the filter 1, the valve 27 is open and the mixture of deaerated water (or other fluid present at this time in the filter 1) / regenerated diatomaceous earth is recovered via the pipe 47 and the valve 49.
• the carbonated deaerated water coming from the tank 25 fills the internal volume of the filter 1 at the end of the regeneration process so as to avoid the presence of the molecules of 0 2 in the filter enclosure during the next filtration cycle, which could compromise the quality of the beer.
• Land recovered diatomaceous earth is stored in the container
• the beer is pushed from the filter by cold deaerated water (approximately 4 ° C., for example). She will then be guided to a PVPP treatment station
• the filter which still contains the diatomaceous earth used, is rinsed with hot water (step 1)
• (a)) between 35 and 95 ° C, preferably about 75 ° C.
• the flow rate for sending hot water is approximately 17.10 " m / s and the volume of water used is 12 m.
• An alkaline solution is then introduced into the filter enclosure (step (b)).
• it is a sodium hydroxide solution of 0.1 to 15% (V / V), preferably about 1%, but it can be any other alkaline solution, for example a solution of potassium hydroxide or also alkaline commercial solutions based on soda, such as the solutions PE 1700 or PE 1900 marketed by HENKEL, GALOR 8/74 or GALOR C7 marketed by CFPI.
• the temperature of the alkaline solution is between 35 and 95 ° C, preferably about 75 ° C.
• the flow rate can be regulated to 22.10 " m / s, for example.
• the introduction of the sodium hydroxide solution ends if (for example and without limitation) the volume introduced is greater than 15 m, or if the brightness of the solution measured at the filter outlet is less than 0.06 ebc (European Brewery Convention units).
• a step of recirculating the soda on the filter (step (e)) can then be implemented, by example for 30 minutes, the recirculation flow can be regulated at around 22.10 m / s.
• a predetermined threshold advantageously between 0.04 and 0.1 ebc, for example 0 , 06 ebc, at the end of 30 minutes. Otherwise, the recirculation step ends.
• the sodium hydroxide solution used for recirculation can be recovered for later use during step (b) of another regeneration cycle.
• a small volume ( ⁇ 4 m 3 ) of fresh sodium hydroxide is introduced into the filter in order to optimize the efficiency of the regeneration (step (f)).
• the filter is rinsed with hot water (step 1)
• the water volume is for example 8 m with a sending flow of 24.10 m / s.
• the final rinsing with deaerated water saturated with carbon dioxide ends if the two following cumulative conditions are met: the volume of water sent to the filter is greater than or equal to a given volume (8 m for example) and the pH of the solution at the filter outlet is less than 6.
• the regeneration of the diatomaceous earth is then complete.
• the latter is recovered by sending deaerated water upside down on the filter (unclogging the candles) for about 90 seconds for example.
• the regenerated diatomaceous earth is characterized by a rate of organic matter less than or equal to 5% by weight. It can be reused as a filtration aid, after cleaning the filter plugs in the same way as a conventional settling.
• the regenerated diatomaceous earth is then, for example, reintroduced into the diatomaceous earth distribution device 9, via the pipes 47 and 57 and the valve 49, another valve, not shown in FIG. 1 , being provided on line 57.
• the rate of recovery of the diatomaceous earth being around 75% by weight relative to the diatomaceous earth used, it is preferable to reconcentrate it by adding a small amount of diatomaceous earth new.
• the regenerated diatomaceous earth is recovered in the preparation tank 55, which is for example of a volume of 4 m 3 , via the pipes 47 and 51 and the valve 49, another valve , not shown in Figure 1 being provided on the line 51; new diatomaceous earth is added to the regenerated diatomaceous earth in the tank 55, in order to reconcentrate the regenerated diatomaceous earth; the mixture of regenerated diatomaceous earth / new diatomaceous earth is then introduced into the device 9 for distributing diatomaceous earth via the line 53.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Analytical Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Life Sciences & Earth Sciences (AREA)
• Health & Medical Sciences (AREA)
• Engineering & Computer Science (AREA)
• Bioinformatics & Cheminformatics (AREA)
• Wood Science & Technology (AREA)
• Biochemistry (AREA)
• Toxicology (AREA)
• General Engineering & Computer Science (AREA)
• General Health & Medical Sciences (AREA)
• Genetics & Genomics (AREA)
• Food Science & Technology (AREA)
• Zoology (AREA)
• Geochemistry & Mineralogy (AREA)
• Inorganic Chemistry (AREA)
• Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
• Solid-Sorbent Or Filter-Aiding Compositions (AREA)
• Physical Water Treatments (AREA)

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• 1998
  • 1998-06-16 FR FR9807552A patent/FR2779665B1/fr not_active Expired - Fee Related
• 1999
  • 1999-06-15 AU AU41492/99A patent/AU755787B2/en not_active Ceased
  • 1999-06-15 CA CA002302812A patent/CA2302812A1/fr not_active Abandoned
  • 1999-06-15 WO PCT/FR1999/001413 patent/WO1999065603A1/fr not_active Application Discontinuation
  • 1999-06-15 EP EP99925084A patent/EP1009525A1/de not_active Withdrawn
• 2000
  • 2000-02-09 ZA ZA200000598A patent/ZA200000598B/xx unknown

Non-Patent Citations (1)

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