Classifications

• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
  • C12G1/00—Preparation of wine or sparkling wine
  • C12G1/06—Preparation of sparkling wine; Impregnation of wine with carbon dioxide
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/30—Active carbon
  • C01B32/354—After-treatment
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/30—Active carbon
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/30—Active carbon
  • C01B32/312—Preparation
• • 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
  • C12H1/0408—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 with the aid of inorganic added material
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/60—Particles characterised by their size
  • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/60—Particles characterised by their size
  • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
• • C—CHEMISTRY; METALLURGY
  • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
  • C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
  • C12G2200/00—Special features
  • C12G2200/21—Wine additives, e.g. flavouring or colouring agents

Definitions

• the present invention relates to a sparkling wine and its production process, sparkling white wine packaged in a bottle.
• Special wines include sparkling wines, coming from grapes, musts or wines treated according to the techniques accepted by the OIV, characterized, at uncorking, by the production of a more or less persistent foam resulting from a release. of carbon dioxide of exclusively endogenous origin.
• the overpressure of this gas in the bottle is at least equal to 3.5 bars at 20 ° C. However, for cylinders with a capacity of less than 0.25 1, the minimum overpressure is reduced to 3 bars at 20 ° C.
• the wine is said:
• Sparkling wines are also defined and regulated by regulation EC 478/2008 which describes eight main categories of sparkling wines.
• Sparkling wines are, for example, obtained according to the traditional method, commonly called the Champagne method which can be summed up in a few stages including the fermentation of the must and then the still wine is bottled with a liqueur de tirage and sourdoughs in order to 'carry out a second fermentation. After a minimum of fifteen months of aging, the bottles are stirred (riddling) then de-gorged (disgorging) and before final corking (cork), the shipping liquor is added.
• This sparkling wine exists either in white or in rosé.
• the quantitative characteristics of these colors are not referenced in any code or technical charter.
• CAO oenological activated carbon
• the activated carbon added if necessary to the must having absorbed the chemical compo- nents having a negative influence at the sanitary or sensory level, is evacuated with the deposits of the must from the tank after various operations such as racking.
• the wine collected from the vat no longer contains oenological activated carbon.
• the object of the present invention is to develop a sparkling, opacified, stable white wine and means for obtaining in particular such a wine.
• the invention relates to an effervescent white wine packaged in a bottle, characterized in that it contains a dose of activated carbon which does not alter the organoleptic properties of the wine, the opacifier dose consisting of a suspension in a liquid food, of enological activated charcoal, finely divided, having a particle size less than or equal to 5 ⁇ m.
• the finely divided oenological carbon has a particle size of less than 3 ⁇ m for 90% of the oenological activated carbon particles.
• the particle size of the oenological activated carbon according to the invention is a particle size measured, for example, by the laser particle size method. This process consists in determining the mean diameter by volume Dv of oenological activated carbon particles. This measurement is the average diameter of a sphere enveloping a grain of oenological activated carbon in its finely divided state.
• the food liquid is distilled water or wine.
• the concentration of finely divided oenological activated charcoal in the dose is between 5 and 50 mg.
• the subject of the invention is also a process for producing an opacified effervescent white wine.
• This process is characterized by the addition of a dose of opacifier, before the final stoppering step, which consists of a suspension of finely divided oenological activated carbon in a food liquid, the concentrate resulting from the sonication is filtered. filtration with a 5 ⁇ m filter.
• the process for making an effervescent white wine consists in adding, at the time of drawing, a dose of opacifier which consists of a suspension of enological activated carbon finely divided in a liquid food. filters the concentrate resulting from sonication to filtration with a 5 ⁇ m filter.
• the subject of the invention is also a suspension of finely divided oenological activated carbon in a food liquid, the concentrate resulting from the sonication is filtered through filtration with a 5 ⁇ m filter.
• the subject of the invention is also a dosage suspension of an effervescent white wine with activated charcoal consisting of using a suspension of 20 g / l of finely divided oenological activated charcoal.
• a process for preparing oenological activated carbon according to the invention consists of:
• This process also consists of:
• the process for making an effervescent white wine is characterized in that at the first so-called alcoholic fermentation, a dose of between 0.01 - 1 g / L of finely divided oenological activated carbon is added (S ' 2), having a particle size less than or equal to 5 ⁇ m.
• the process for making a sparkling white wine is characterized in that at the clarification stage a dose of between 0.01 - 1 g / L of finely divided enological activated carbon (S'2) is added , having a particle size less than or equal to 5 ⁇ m.
• the method of elaboration according to the traditional method of effervescent white wine 1, opacified, presented in the bottle consists in carrying out a first fermentation of the must Al, then the drawing of still wine A2 in the bottle with the addition of a tirage liqueur and A21 yeasts as well as glue or stirring aid.
• Bottled wine ages for at least fifteen months. At the end of this aging period, the deposits accumulated in the neck of the bottle following the riddling step are removed during the A4 disgorging. Before final corking (cork), the A51 shipping (or dosing) liquor is added before marketing.
• a dose of opacifier A52 is added which does not alter the organoleptic properties of the wine. Then the bottle is corked.
• Figure 2 shows the diagram of an example of a process for the preparation of an oenological activated carbon and of a process 2 for the preparation of the dosage liquid to opacify an effervescent white wine.
• Process 2 begins with a step of preparing a master suspension E1 of oenological activated carbon Eli in food liquid E 12 such as distilled water or better still wine.
• Eli oenological activated carbon is of plant origin in the form of powder of fine particles of size between 1 and 100 ⁇ m.
• This oenological active charcoal meets the requirements of the international oenological CODEX (INS 153 OENO7 / 2007; OIV-OEN 604/218).
• This SI oenological activated carbon suspension thus prepared will undergo several treatments to obtain a finely divided oenological activated carbon suspension forming the dosage liquor as fine as possible having filtered the concentrate resulting from the sonication to filtration with a filter. at 5 ⁇ m.
• the SI stock suspension is prepared with a concentration in the range of 1 to 100 g / L.
• the mother suspension SI is then first homogenized E2 by mechanical stirring, for example.
• the homogenized stock suspension S2 is sonicated with ultrasound for three hours E3 to obtain a suspension based on defragmented CAO S3. All the liquid is collected which will be subjected to successive E4 centrifugation steps.
• a first E41 centrifugation step carried out at a rotational speed of the order of 1200 RCF for a period of around 30 minutes, the supernatant S41 is collected, that is to say a suspension volume. in the upper part of the pot used for centrifugation.
• This supernatant is subjected to S41 a new E42 centrifugation step to collect a new supernatant S42.
• centrifugation steps E4 reduce the volume of liquid, several series of centrifugation are carried out in parallel to obtain, at the end, by addition, a final supernatant volume S4.
• the filtered supernatant is then reduced by E5 evaporation with a reduction rate giving between 1 and 2% of S5 concentrate.
• the centrifugation steps are carried out for a duration of the order of 30-180 minutes at speeds of the order of 500-2200 RCF.
• the supernatants are checked by measurements of the optical density OD at 620nm.
• the concentrate S5 is sonicated with ultrasound for three hours E6 to finally obtain a defragmented concentrate S6.
• the final concentrate S7 resulting from this step E7 is filtered with a filter retaining particles of size greater than 5 microns.
• the finely divided oenological activated carbon thus obtained was analyzed by laser granulometry. It showed that the mean diameter by volume Dv of the finely divided oenological activated carbon particles was less than 3 microns for 90% of the particles.
• the volume-mean diameter is, by definition, the diameter of the envelope sphere or sphere circumscribed by a grain of activated carbon analyzed. Tests have shown that the finely divided oenological activated carbon according to the invention remains in suspension in a particularly stable manner in the wine.
• the concentrate S7 thus collected is added to E8 with an additional food liquid to obtain the dosage suspension S8 (dosage liquor).
• This S8 dosage suspension is added A5 to the bottled and disgorged white wine, before final corking, in parallel or with the dosage / expedition liqueur.
• the concentration of oenological activated charcoal in one dose is between 5 and 50 mg.
• the concentration of the dosage liquor is advantageously between 0.01 and 10 g / L of finely divided oenological charcoal.
• Figure 3 shows the diagram of a variant of the process for the preparation of an oenological activated carbon and of a process for the preparation of the dosage liquid to opacify an effervescent white wine.
• Process 3 begins with a step of preparing a stock suspension E’1 of oenological activated carbon E’11 in food liquid E’12 such as distilled water or better still wine.
• E'11 oenological activated carbon is of plant origin in the form of powder of fine particles between 1 and 100 ⁇ m in size.
• This oenological activated carbon meets the requirements of the international oenological CODEX (INS 153 OENO7 / 2007; OIV-OEN 604/218).
• This S’1 oenological activated carbon suspension thus prepared will undergo several treatments to obtain a finely divided oenological activated carbon suspension forming the dosage liquor as fine as possible.
• the S’1 stock suspension is prepared with a concentration in the range of 50 to 1000 g / L.
• the mother suspension S’1 is then finely ground or micronized E’2 using a horizontal microbead mill, for example a Netzsch Labstar mill, using metal or metal oxide microbeads with a diameter between 100 - 1000 ⁇ m.
• the filling rate of the crusher is between 10 - 90% of its capacity and the rotational speed is between 1000 - 5000 rpm.
• the grinding time is between 1 - 24 hours to reach a final carbon content in the mother suspension of between 1 - 20% by mass concentration.
• the micronized mother suspension is diluted E’3 in food liquid E’13 such as deionized water.
• micronized and diluted parent suspension S'3 is disaggregated by ultrasonic homogenization for a period of between 1 to 15 min E'4 to obtain a suspension based on defragmented enological activated carbon S'4.
• the concentrate obtained S'6 is again disaggregated by a first ultrasonic homogenization step for a period of between 1 - 15 min E'7 then the resulting S'7 is again subjected to another step of sonication in baths at ultrasound for a period of between 1 - 3 h E'8.
• the time of the ultrasonic homogenization step is quite short given the energy supplied by the probe, in order to avoid any caramelization of the liquor.
• the concentrate obtained S’8 is finally filtered through 5 ⁇ m E’9 filters retaining particles larger than 5 ⁇ m in order to obtain a filtered concentrate S’9 with particles smaller than 5 ⁇ m.
• the filtered concentrate is subjected to E'10 centrifugation to collect a final S'10 supernatant.
• the centrifugation step is carried out at a speed of between 2000 - 4000 rpm for a period of around 30 - 180 minutes.
• the supernatant S'10 which is a volume of suspension in the upper part of the tube used for centrifugation, is collected. In the end, the opacification liquor is obtained.
• the analysis of the size distribution of the thus finely divided activated carbon was carried out by laser granulometry. It shows that the mean diameter by volume Dv of the finely divided oenological activated carbon particles was less than 0.33 microns for 50% of the particles (The mean diameter by volume is, by definition, the diameter of an enveloped sphere or sphere limited to a grain of activated carbon analyzed). Tests have shown that the finely divided oenological activated carbon according to the invention remains in suspension in a particularly stable manner in the wine.
• This dosing S'10 opacification liqueur is added A5 to the bottled and disgorged white wine, before final corking, in parallel or with the dosing / shipping liquor.
• the final charcoal concentration is between 1 and 50 mg in a 750 mL bottle.
• the concentration of the dosage liquor is advantageously between 0.01 and 50 g / L of finely divided oenological charcoal.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Engineering & Computer Science (AREA)
• General Engineering & Computer Science (AREA)
• Zoology (AREA)
• Biochemistry (AREA)
• Bioinformatics & Cheminformatics (AREA)
• Health & Medical Sciences (AREA)
• General Health & Medical Sciences (AREA)
• Genetics & Genomics (AREA)
• Life Sciences & Earth Sciences (AREA)
• Wood Science & Technology (AREA)
• Food Science & Technology (AREA)
• Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
• Alcoholic Beverages (AREA)
• Carbon And Carbon Compounds (AREA)
• Food Preservation Except Freezing, Refrigeration, And Drying (AREA)

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• 2020
  • 2020-06-30 FR FR2006897A patent/FR3111885A3/fr not_active Ceased
• 2021
  • 2021-06-24 FR FR2106766A patent/FR3111884B1/fr active Active
  • 2021-06-29 US US18/003,537 patent/US12624321B2/en active Active
  • 2021-06-29 EP EP21745372.9A patent/EP4172302A1/de active Pending
  • 2021-06-29 AU AU2021298915A patent/AU2021298915A1/en active Pending
  • 2021-06-29 EP EP23189313.2A patent/EP4257665A3/de active Pending
  • 2021-06-29 WO PCT/FR2021/051196 patent/WO2022003292A1/fr not_active Ceased
• 2022
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  • 2022-12-28 CL CL2022003794A patent/CL2022003794A1/es unknown

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