EP4698621A1 - Agents de clarification - Google Patents

Agents de clarification

Info

Publication number
EP4698621A1
EP4698621A1 EP24726448.4A EP24726448A EP4698621A1 EP 4698621 A1 EP4698621 A1 EP 4698621A1 EP 24726448 A EP24726448 A EP 24726448A EP 4698621 A1 EP4698621 A1 EP 4698621A1
Authority
EP
European Patent Office
Prior art keywords
wort
silica particles
porous silica
porous
particles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP24726448.4A
Other languages
German (de)
English (en)
Inventor
Simon STEBBING
Miguel MONSANTO
Philippe CARIO
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pq LLC
Original Assignee
Pq LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Pq LLC filed Critical Pq LLC
Publication of EP4698621A1 publication Critical patent/EP4698621A1/fr
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
    • C12C7/00—Preparation of wort
    • C12C7/24—Clarifying beerwort between hop boiling and cooling
    • 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

Definitions

  • the present invention relates to use of porous silica particles in treating a wort, a method of treating a wort, and to a method of preparing liquid beverages.
  • beverages obtainable from a wort are clarified after fermentation in the cold block by treatment with a colloidal stabilizer agent. These agents are then removed from the end product by filtration.
  • a colloidal stabilizer agent Various clarifying agents have been employed in the art for such post-production clarification and for instance it is known to use silica hydrogels for this purpose.
  • beer producers are also known to add finings agents to the wort prior to fermentation. These agents have the effect of coagulating coarse particles and / or removing at least some haze from the wort.
  • the invention proposes the novel use of particular porous silica particles for treating a wort, with surprisingly advantageous benefits.
  • it has been found to be possible to reduce the haze and, in certain embodiments, also the protein content of a wort using porous silica gel particles or porous precipitated silica particles as described herein.
  • the use of these silicas has been found to offer distinct advantages over prior art processes such as those described above, e.g. compared to the use of silica sols.
  • the use of the silica particles described herein has been found to provide a significant reduction in the haze of the wort at comparatively low loadings (see examples).
  • some embodiments of the present invention have also been found to reduce the amount of sensitive proteins present.
  • sensitive proteins it is meant the fraction of proteins which are tannic acid precipitable.
  • the amount of sensitive proteins is therefore determined by measurement of the haze formed (EBC units) after the addition of a specific amount of tannic acid as described in the method section below.
  • EBC units haze formed
  • the reduction in sensitive protein may allow the brewery to reduce or avoid the need for stabilising the beer after fermentation. This is particularly advantageous for smaller breweries that do not have a possibility to stabilize and filter in the cold block or breweries that want to avoid process bottlenecks at a late stage of the process which can reduce throughput of the final product.
  • Wort treated with silica particles according to the present invention have shown the potential to spend less time in the whirlpool stage of the process while producing a more compact trub leading to yield improvements. Moreover, it has unexpectedly been observed that using the method according to the present invention results in an improvement in the subsequent filtration of the fermented beer obtained from the treated wort.
  • Using the porous silica particles within a brewing process as described herein has for instance been shown to result in less charge going to the filter, and therefore less pressure build up on filter over longer filtration runs. For example, as described below, it was found to be possible to filter about two times the beer volume in the same run compared to beer fermented from a wort that had not been treated with porous silica particles of the invention.
  • the use of the silica particles described herein has been found to provide high levels of haze reduction, and in some embodiments, high levels of sensitive protein removal, even when used at a low dosage, whilst also delivering practical benefits in terms of processability.
  • the use of the silica particles described herein can therefore improve the overall efficiency of a brewing process.
  • the methods described can provide reduced waste compared to traditional brewing methods involving clarification after fermentation.
  • the silica particles used can be separated with the spent grains of the wort and used in animal feed or sent to methanisation (biogas) plants.
  • methanisation biogas
  • porous silica gel particles or porous precipitated silica particles in treating a wort, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml/g or more.
  • the porous silica particles refers to the porous silica gel particles and porous precipitated silica particles mentioned.
  • wort is well known in the art and is intended to be given its conventional meaning.
  • the term for instance includes the liquid extracted from grains obtained during the mashing step of a brewing process.
  • wort obtained from the brewing of beers such as lager, pilsner, Dortmund and Kunststoff beers as well as top fermented beverages such as ale, porter and stout.
  • the wort typically contains proteins in addition to the sugars, e.g. maltose, that will (in the case of fermented products) be fermented by yeast to produce a fermented beverage.
  • the wort may for example be a full malt brew, or may be a partial malt brew with adjuncts, e.g. 60% malt with 40% adjuncts.
  • Reference to the “water content” of the particles refers to the water content of the particles before being added to the wort in the process. The water content may be calculated by the method for “Determining water content” described below in the general methods section.
  • the method has advantageously been shown to result in large reductions in the levels of haze and in some embodiments also protein. This reduction may avoid the need for further processing after fermentation and can improve efficiencies in the whirlpool and filtration stages of the brewing process, leading to a more optimised brewing process.
  • a method for treating a wort comprising contacting the wort with porous silica gel particles or porous precipitated silica particles, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml/g or more.
  • the porous silica particles refers to the porous silica gel particles and porous precipitated silica particles mentioned.
  • a method of preparing a beverage comprising: treating grains to produce a wort; contacting the wort with porous silica gel particles or porous precipitated silica particles; and using the resulting wort to produce the beverage; wherein the porous silica particles have water content of 30% by weight or less and a pore volume of 0.4 ml/g or more.
  • the porous silica particles refers to the porous silica gel particles and porous precipitated silica particles mentioned.
  • treating a wort according to the present uses and methods has the effect of reducing the haze of the wort (according to the haze value determined by the methods described herein) and may in embodiments also reduce protein levels in the wort, particularly levels of sensitive proteins (as also described further herein).
  • treating a wort may be use in, or a method of, reducing the haze of the wort and, optionally, reducing the protein content of the wort.
  • porous silica gel particles or porous precipitated silica particles in reducing the haze of a wort (and optionally also the protein content of the wort), wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml/g or more.
  • the porous silica particles refers to the porous silica gel particles and porous precipitated silica particles mentioned.
  • Also provided is a method for reducing the haze of a wort (and optionally also the protein content of the wort) comprising contacting the wort with porous silica gel particles or porous precipitated silica particles, wherein the porous silica particles have a water content of 30% by weight or less and a pore volume of 0.4 ml/g or more.
  • the porous silica particles refers to the porous silica gel particles and porous precipitated silica particles mentioned.
  • a method of preparing a beverage comprising: treating grains to produce a wort; contacting the wort with porous silica gel particles or porous precipitated silica particles to reduce the haze of the wort (and optionally also reduce the protein content of the wort); and using the resulting wort to produce the beverage; wherein the porous silica particles have water content of 30% by weight or less and a pore volume of 0.4 ml/g or more.
  • the porous silica particles refers to the porous silica gel particles and porous precipitated silica particles mentioned.
  • the porous silica particles may have a pore volume of 0.6 ml/g or more, such as 0.75 ml/g or more, or 0.8 ml/g or more.
  • the porous silica particles may have a pore volume of 2 ml/g or less.
  • the porous silica particles i.e. the porous silica gel particles and porous precipitated silica particles
  • the porous silica particles may have a pore volume of 1.2 ml/g or more.
  • the porous silica particles may have a pore volume of from 1.2 ml/g to 2 ml/g.
  • the porous silica particles may have a pore volume of from 1.2 ml/g to 1.8 ml/g.
  • the porous silica particles may have a pore volume of from 1.2 ml/g to 1.3 ml/g, for example, a pore volume of about 1.28 ml/g.
  • the porous silica particles may have a pore volume of 1.5 ml/g or more, for example, the porous silica particles may have a pore volume of from 1.5 ml/g to 2ml/g.
  • the porous silica particles may advantageously have a pore volume of from 1.5 ml/g to 1.8ml/g.
  • the porous silica particles may have a pore volume of 1.6 ml/g or more.
  • the porous silica particles may have a pore volume of from 1.6 ml/g to 1.8 ml/g, for example about 1.7 ml/g.
  • the porous silica particles may have a pore volume of 1.75 ml/g or more, such as 1.8 ml/g or more. In other embodiments, the porous silica particles have a pore volume of 1.75ml/g or less, such as 1.6 ml/g or less, such as 1.5 ml/g or less. Optionally, the bottom end of these ranges may be a pore volume of 1.0 ml/g.
  • the porous silica particles may have a water content of 20% by weight or less.
  • the porous silica particles may have a water content of 15% by weight or less, such as 10% by weight or less.
  • the porous silica particles may have a water content of 7.5% by weight or less.
  • the porous silica particles may have a water content of 5% by weight or less.
  • the porous silica particles may have a water content of from 1 % to 10% by weight.
  • the porous silica particles may have a water content of from 2% to 6% by weight.
  • the porous silica particles may have a water content of from 2% to 4% by weight.
  • silica particles with a water content below 30% provides greater clarification compared to the same dosage of silica particles having a higher water content.
  • silica particles with a low water content has also been found to provide improvements in the overall processing efficiency and ease of handling.
  • porous silica gel particles or porous precipitated silica particles having water content of 30% by weight or less and a pore volume of 0.4 ml/g or more.
  • Both porous silica gel particles and porous precipitated silica particles may be present, or solely porous silica gel particles, or solely porous precipitated silica particles.
  • the porous silica particles may thus be porous silica gel particles.
  • the porous silica particles may be porous silica xerogel particles.
  • the porous silica particles may be porous precipitated silica particles. Both types of particles have been shown to be particularly effective at reducing haze of a wort, as evidenced by the examples below.
  • the porous silica particles may have a surface area of 800 m 2 /g or less, such as 700 m 2 /g or less, or 600 m 2 /g or less.
  • the porous silica particles may have a surface area of 500 m 2 /g or less, for example, 450 m 2 /g or less.
  • the porous silica particles may have a surface area of 200 m 2 /g or more. Accordingly, the porous silica particles may have a surface area of from 200 m 2 /g to 800 m 2 /g.
  • the porous silica particles Preferably have a surface area of from 200 m 2 /g to 500 m 2 /g.
  • the porous silica particles may be used in an amount of 1 g to 50 g per 100 litres of wort, such as 5 g to 20 g, or 10 g to 30 g per 100 litres of wort.
  • the porous silica particles may be used in an amount of no more than 25 g per 100 litres of wort, e.g. at around 20 g per 100 litres of wort.
  • the silica particles described herein have been found to provide a significant reduction in the haze of the wort even at comparatively low loadings, leading to excellent efficiency (see table 4 in examples below).
  • the porous silica particles may be used in an amount of no more than 20 g per 100 litres of wort.
  • the porous silica particles may be used in an amount of no more than 15 g per 100 litres of wort, no more than 10 g per 100 litres of wort or no more than 8 g per 100 litres of wort.
  • the porous silica particles may be used in an amount of 1 g to 15 g per 100 litres of wort, such as 1 g to 10 g, or 1 g to 8 g, or 1 g to 5 g per 100 litres of wort.
  • the porous silica particles may have a weight median particle diameter (D50) of 1 pm or more.
  • the porous silica particles may have a weight median particle diameter (D50) of 2.5 pm or more.
  • the porous silica particles may have a weight median particle diameter (D50) of 5 pm or more, such as 7.5 pm or more, or 10 pm or more.
  • using particle sizes on the micron scale allows for the silica particles to more easily settle out of solution and therefore be removed from the wort after treatment. This represents an improvement over colloidal silicas.
  • the porous silica particles may have a weight median particle diameter (D50) of 200 pm or less.
  • the porous silica particles may have a weight median particle diameter (D50) of 150 pm or less, 100 pm or less, 80 pm or less, or 50 pm or less.
  • the porous silica particles have a weight median particle diameter (D50) of 30 pm or less.
  • the porous silica particles have a weight median particle diameter (D50) of 20 pm or less, such as 15 pm or less. Accordingly, the porous silica particles may have a weight median particle diameter (D50) of from 1 pm to 200 pm.
  • the porous silica particles have a weight median particle diameter (D50) of from 2.5 pm to 80 pm.
  • the porous silica particles have a pore volume of 1.0 ml/g to 1.2 ml/g, a water content of from 2 to 6%, and a weight median particle diameter (D50) of 2.5 pm to 50 pm.
  • the porous silica particles of this preferred embodiment may be precipitated silica particles.
  • the porous silica particles have a pore volume of 1.6 ml/g to 1.8 ml/g, a water content of from 2 to 4%, and a weight median particle diameter (D50) of 5 pm to 50 pm.
  • the porous silica particles of this preferred embodiment may be porous silica gel particles, e.g. silica xerogel particles.
  • the wort may be treated at any suitable point in a beverage preparation process. It will be appreciated that the method is not particularly limited by the location of the wort. For example, contacting the porous silica particles with the wort may occur within a mash tun, a lautertun, a press filter, a wort kettle, a whirlpool/decanter or a fermenter, or between any two of the above. It also may occur in a different location.
  • the uses and methods described herein may further comprise allowing the silica particles to settle out of the wort and separating the wort from the silica particles. This allows the silica particles and any adsorbed compounds to be easily removed from the wort.
  • Methods according to the third aspect or its embodiments may further comprise separating the silica particles from the wort prior to using the resulting wort to produce the beverage. Separating the particles at this stage may improve the downstream processing, for example the pressure on the filter elements.
  • Figure 2 is a graph showing protein reduction in wort samples after lab scale treatment with low water content silica gels of differing pore volumes.
  • the effect of the porous silica clarifying agents of the invention on reducing sensitive protein was tested.
  • the amount of sensitive proteins as referenced herein refers to the fraction of proteins which are tannic acid precipitable. More information can be found in K. A. Leiper et al, Optimising Beer Stabilisation by the Selective Removal of Tannoids and Sensitive Proteins”, Journal of the Institute of Brewing, 111(2), 118-127, 2005.
  • Sensitive protein was determined using the method described in European Brewery Convention (EBC) Analytica, Section 9.40, Sensitive proteins in beer by nephelometry, suverlag Hans Carl, Nurenberg, Germany, 1998. The method was modified by taking the measurements after 30 minutes. In brief, after the haze measurement protocol (described above) was conducted, the haze values were re-measured and 0.1 g/l aqueous tannic acid solution was added to both the wort sample treated with silica particles and to the corresponding reference sample. The amount of precipitated “sensitive proteins” was then measured as an increase in the haze of the wort at defined time (30 minutes) after addition of the tannic acid.
  • EBC European Brewery Convention

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Food Science & Technology (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne l'utilisation de particules de gel de silice poreuses ou de particules de silice précipitée poreuse pour le traitement d'un moût, les particules de silice poreuses présentant une teneur en eau inférieure ou égale à 30 % en poids et un volume de pores supérieur ou égal à 0,4 ml/g. L'invention concerne également des procédés de traitement d'un moût et des procédés de préparation d'une boisson.
EP24726448.4A 2023-04-21 2024-04-19 Agents de clarification Pending EP4698621A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GBGB2305914.0A GB202305914D0 (en) 2023-04-21 2023-04-21 Clarifying agents
PCT/US2024/025422 WO2024220813A1 (fr) 2023-04-21 2024-04-19 Agents de clarification

Publications (1)

Publication Number Publication Date
EP4698621A1 true EP4698621A1 (fr) 2026-02-25

Family

ID=86605503

Family Applications (1)

Application Number Title Priority Date Filing Date
EP24726448.4A Pending EP4698621A1 (fr) 2023-04-21 2024-04-19 Agents de clarification

Country Status (6)

Country Link
EP (1) EP4698621A1 (fr)
CN (1) CN121666444A (fr)
AR (1) AR132483A1 (fr)
GB (1) GB202305914D0 (fr)
MX (1) MX2025012528A (fr)
WO (1) WO2024220813A1 (fr)

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1279250A (en) * 1968-10-28 1972-06-28 Unilever Ltd Improvements in or relating to a method for the reduction of haze in beer
PH18548A (en) 1982-09-08 1985-08-09 Unilever Nv Calcined silicas and their use in beer clarification
US4636394A (en) 1984-04-16 1987-01-13 J. E. Siebel Sons' Company, Inc. Method and compositions for chillproofing beverages
GB8431290D0 (en) * 1984-12-12 1985-01-23 Whitbread & Co Plc Coagulable material removal from extracts of malted barley
GB8707526D0 (en) 1987-03-30 1987-05-07 Unilever Plc Amorphous silicas
GB2280908B (en) 1993-08-11 1997-05-28 Laporte B S D Limited Clarification of a beverage brew
AU690657B2 (en) 1994-05-18 1998-04-30 Mizusawa Industrial Chemicals, Ltd. Stabilizing agent for beer
JP3316325B2 (ja) 1994-12-20 2002-08-19 富士シリシア化学株式会社 ビール安定化処理用シリカゲル及びその製造方法並びにビールの安定化処理方法
US6045852A (en) 1997-12-16 2000-04-04 Charvid Limited Liability Co. Composition for clarifying beverage solutions used to prepare fermented beverages
US6555151B2 (en) 2001-01-12 2003-04-29 Pq Corporation Process for making and using a low beverage soluble iron content adsorbent and composition made thereby
SI1807500T1 (sl) 2004-09-20 2014-09-30 Carlton And United Beverages Limited Postopki in sestavki za bistrenje napitkov
WO2008017393A1 (fr) * 2006-08-07 2008-02-14 Grace Gmbh & Co. Kg Auxiliaire de clarification de la bière à base de xérogel de silice à haute filtrabilité

Also Published As

Publication number Publication date
GB202305914D0 (en) 2023-06-07
WO2024220813A1 (fr) 2024-10-24
MX2025012528A (es) 2026-02-03
AR132483A1 (es) 2025-07-02
CN121666444A (zh) 2026-03-13

Similar Documents

Publication Publication Date Title
EP0235352A2 (fr) Gel de silice hydraté pour la stabilisation de la bière
CA2653809C (fr) Procede de production d'une boisson brillante fermentee a la levure
EP2041256A2 (fr) Procede de brassage ameliore
US20250145918A1 (en) Foam Stability
US5194279A (en) Glucoamylase removal using nitrogen-functionalized amorphous precipitated silica
CN1965072B (zh) 制备含蛋白质的液体以及随后用一种或多种蛋白质络合剂将其分离的方法
CA2653810C (fr) Procede de production d'un extrait de maische et dispositif pour la mise en oeuvre de ce procede
HK1222671A1 (zh) 基於高过滤率硅干凝胶的啤酒澄清助剂
JP7049821B2 (ja) ビール様発酵麦芽飲料の製造方法及びビール様発酵麦芽飲料の泡持ち向上方法
CN110831679A (zh) 生产物理稳定的高比重啤酒的系统和方法
Poreda et al. Effects of Wort Clarifying by using Carrageenan on Diatomaceous Earth Dosage for Beer Filtration.
Delvaux et al. Characterisation of the colloidal haze in commercial and pilot scale Belgian white beers
EP4698621A1 (fr) Agents de clarification
US8563056B2 (en) Continuous method for the production of a yeast fermented beverage
JPH0659202B2 (ja) ビ−ルの処理方法
WO1991019780A1 (fr) Elimination de proteine au moyen de dioxyde de silicium precipite
EP0188882A1 (fr) Extraction de matière coagulable d'extraits orge-malte
RU2330879C2 (ru) Применение коллоидного, анионного кремниевого золя в качестве осветлителя
JP7461806B2 (ja) ビールテイスト飲料の製造方法
Munroe Aging and finishing
Razan et al. The efficiency of using new brands silica gel for colloidal stabilization of beer
Taylor Aging, Dilution, and Filtration
GB2280908A (en) Process for clarifying a beverage brew
Gadon A novel beer fining agent extracted from hops
JPH09173045A (ja) ビール用清澄剤およびビールの清澄化方法

Legal Events

Date Code Title Description
STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: UNKNOWN

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE INTERNATIONAL PUBLICATION HAS BEEN MADE

PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE

17P Request for examination filed

Effective date: 20251010

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC ME MK MT NL NO PL PT RO RS SE SI SK SM TR