EP2217691B1 - Acid cleaning method in the brewing industry - Google Patents
Acid cleaning method in the brewing industry Download PDFInfo
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- EP2217691B1 EP2217691B1 EP08855377.1A EP08855377A EP2217691B1 EP 2217691 B1 EP2217691 B1 EP 2217691B1 EP 08855377 A EP08855377 A EP 08855377A EP 2217691 B1 EP2217691 B1 EP 2217691B1
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- EP
- European Patent Office
- Prior art keywords
- sulphonic acid
- formulation
- installation
- beer
- cleaning
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
- B08B9/027—Cleaning the internal surfaces; Removal of blockages
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/0804—Cleaning containers having tubular shape, e.g. casks, barrels, drums
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/143—Sulfonic acid esters
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/34—Organic compounds containing sulfur
- C11D3/3409—Alkyl -, alkenyl -, cycloalkyl - or terpene sulfates or sulfonates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/34—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/20—Industrial or commercial equipment, e.g. reactors, tubes or engines
Definitions
- the present invention relates to an acid cleaning process in the brewing industry, and in particular to an improved acid cleaning process of the various materials used in the manufacture of beer and other related fermented beverages.
- the beer is packaged in barrels or in bottles or even cans.
- bitter or yeast ring, in English
- fermentor bottoms and on its walls form "beer stones” ("beerstones” in English), which consist mainly of calcium oxalate and various organic materials.
- the fermenter is therefore commonly soiled by two distinct types of soiling: organic soils (mainly bitter crown) and inorganic soils (mainly "beer stones").
- a crucial aspect in the preparation of beer, or other related fermented beverages is to dispose of drums, containers, fermenters, pipes and other devices for the transport or residence of the liquids used in the preparation of the beer and other beverages.
- fermented which are absolutely clean and in particular free from any trace of organic and inorganic soils. Indeed, such fouling could cause the presence and growth of bacteria or any other elements harmful to the prepared products, or even make them unfit for consumption.
- the barrels are cleaned hot (typically about 80 ° C) with phosphoric acid, the sulfuric acid being too corrosive at this temperature, as indicated above.
- a first object of the present invention is to provide a method of cleaning facilities used in the manufacture and storage of beer simpler and faster than those currently used.
- Another object of the present invention is to provide a simple and effective method for both efficient cleaning of "beer stones” and bitter crowns.
- Yet another object is to provide a method of cleaning the facilities used in the preparation and storage of beer and other related fermented beverages, by means of a unique formulation allowing the elimination of all types of soiling, including "beer stones” and bitter crowns.
- alkanesulfonic acid formulation allows both the removal of the bitter crown (commonly eliminated by phosphoric acid) and the elimination of beer '(usually removed by the action of sulfuric acid).
- an alkanesulfonic acid-based formulation avoids the use of several cleaning formulations, such as a phosphoric acid formulation and a sulfuric acid based formulation.
- the use of an alkanesulfonic acid-based formulation may also make it possible to avoid several successive washing operations and also several intermediate rinses.
- the benefits are therefore mainly a saving of time, costs, productivity, energy, as well as a decrease in the number of cleaning chemicals present at the manufacturing site.
- the phosphoric acid usually used is released in the form of phosphates, which can harm the environment, and increasingly stringent environmental standards aim to outlaw phosphate releases.
- the method of the invention makes it possible on the one hand to reduce the number of cleaning steps, and on the other hand to reduce the number of acid formulations used, from two (phosphoric acid and sulfuric acid) to a single formulation cleaning of dirt.
- the formulation used in the process of the invention being less corrosive than sulfuric acid, it can be used for cleaning hot drums.
- the process of the present invention relates to the cleaning of facilities used for the preparation and storage of beer and other related fermented beverages.
- “Installation” means the various elements commonly used in breweries, including vats, barrels, fermenters, pipelines, valves, bottles, cans, and others, that is, all the elements likely to enter in contact with beer and other liquids or solids necessary for its manufacture.
- the materials of the various components of the installation are generally selected from stainless steel, aluminum, copper, brass, steel coated or not, for example by an epoxy resin, plastic, in particular polypropylene, polyethylene, poly (vinyl chloride), glass, and others.
- the materials used for the brewery installations are chosen from stainless steel 304L or 316L, aluminum, and steel coated with epoxy resin.
- the process of the invention applies to all or only one or more parts of the beer manufacturing facility or other related fermented beverages.
- installation refers to the entire installation or one or more parts of the installation.
- the method according to the invention comprises a possible first prewash stage, intended to mechanically remove the largest part of the impurities.
- the prewash is carried out by circulation of water, alone or in combination with “shots” of an alkaline solution, preferably diluted, for example an aqueous solution of potassium hydroxide or sodium hydroxide.
- shots of an alkaline solution, preferably diluted, for example an aqueous solution of potassium hydroxide or sodium hydroxide.
- shots sending in the part of the installation to clean with an alkaline solution, usually weakly concentrated, that we let act for a short time. In short time, it is understood a period ranging from a few seconds to several minutes or even hours.
- the washing of the installation is carried out by circulation of a formulation comprising at least one alkanesulfonic acid.
- alkanesulphonic acid is understood to mean alkanesulphonic acids comprising a saturated hydrocarbon chain, linear or branched, containing from 1 to 4 carbon atoms.
- Alkanesulfonic acids used in the process of the present invention are particularly selected from methanesulfonic acid, ethanesulfonic acid, n-propanesulfonic acid, iso propanesulfonic acid, n-butanesulfonic acid, iso acid -butanesulfonique, the sec-butanesulfonic acid, tert -butanesulfonique acid, and mixtures of two or more of them in any proportion.
- the alkanesulfonic acid used in the process of the present invention is methanesulfonic acid or ethanesulfonic acid, most preferably the acid used is methanesulfonic acid.
- the cleaning formulation comprising at least one alkanesulfonic acid used in the process of the invention comprises one or more linear or branched chain alkanesulfonic acids comprising from 1 to 4 carbon atoms, and preferably comprises at least one carbon atom.
- the formulation comprises from 0.1% to 100% by weight of alkanesulfonic acid, more generally from 0.5% to 90% by weight, in particular from 0.5% to 20% by weight of acid. alkanesulfonic acid, and more particularly from 0.5% to 5% by weight.
- the formulation is generally an aqueous formulation that can be prepared as a concentrated mixture that is diluted by the end user.
- the formulation may also be a ready-to-use formulation, i.e., which does not need to be diluted. It is possible, for example, to use methanesulphonic acid in solution at 70% by weight in water and marketed by the Arkema under the name Scaleva TM , ready for use or diluted with water in the proportions indicated above.
- the cleaning formulation may optionally comprise one or more additives, solvents, biocides and other rheological or textural agents chosen from solvents and co-solvents, organic or inorganic acids (for example sulfuric, phosphoric or nitric acids). sulfamic, citric), thickening agents, surfactants, foaming agents, anti-foaming agents, and others known to those skilled in the art.
- alkanesulfonic acids as just described are effective in cleaning the soils present or formed in facilities used in the preparation of beer and other related fermented beverages.
- alkanesulfonic acids thus makes it possible to eliminate organic and inorganic soils, such as carbohydrates, fats, proteins, inorganic minerals such as calcium carbonate, calcium phosphate, and other types of scale comprising oxalates and sulphates. hydroxides and / or sulfides, whether or not combined with various organic materials and / or metals, metalloids, alkalis or alkaline earths, and other residues encountered in the preparation of beer or other related fermented beverages.
- Alkanesulfonic acids are particularly effective in removing "beer stone” and "bitter crown” residues as previously indicated.
- the washing (or cleaning) of all or part of the installation is carried out by circulating an effective amount of a formulation comprising at least one alkanesulfonic acid, as just described.
- effective amount is meant an amount for the removal of all soils, which, if not properly removed, could promote the development of bacteria.
- the process of the invention makes it possible to eliminate all types of soiling, and consequently the bacteria that could adversely affect the manufacture, the preservation, the flavor, the texture, and the non-toxicity for humans. , beer or other related fermented drink prepared in the facility and stored in drums, bottles, cans and others.
- This quantity can vary in large proportions, depending on the volume of the installation to be cleaned, the nature and amount of dirt that it is desired to eliminate, the temperature and pressure of the formulation used, and others.
- an effective amount of the acidic cleaning formulation is circulated in the plant, this circulation being established for a time sufficient to allow complete removal of soil.
- the amount of formulation and the duration of circulation will be established to allow a total elimination of soiling, while observing both a minimal amount of formulation (mainly for economic and environmental reasons) and a shortest possible circulation time (also mainly for economic reasons).
- the acid cleaning with the formulation comprising at least one alkanesulfonic acid as indicated above can be carried out at all temperatures, generally between 0 ° C and 100 ° C, more generally between 5 ° C and 40 ° C, typically between 5 ° C and 20 ° C in the fermenter or guard reactor and between 60 ° C and 80 ° C in the packaging containers (drums, bottles or cans) of the beer or other related fermented beverage.
- the installation is advantageously rinsed by circulation of a rinsing solution, for example with water, in a manner known to the man of the job.
- a rinsing solution for example with water
- the washing of a facility useful for the preparation of beer or other related fermented drinks is carried out in a single step of acid washing, unlike the techniques known today.
- This single stage of acid washing eliminates in particular "Beer stones” and bitter crowns formed during the manufacture of said beer and other related fermented beverages.
- the present invention relates to the use of a formulation comprising at least one alkanesulfonic acid, in particular at least methanesulphonic acid, for the removal of organic and inorganic soils, such as carbohydrates, fats , proteins, inorganic minerals such as calcium carbonate, calcium phosphate, and other types of scale comprising oxalates, sulphates, hydroxides and / or sulphides, whether or not combined with various organic materials and / or metals, metalloids, alkalis or alkaline earths earthy, and other residues encountered in the preparation of beer or other related fermented beverage.
- organic and inorganic soils such as carbohydrates, fats , proteins, inorganic minerals such as calcium carbonate, calcium phosphate, and other types of scale comprising oxalates, sulphates, hydroxides and / or sulphides, whether or not combined with various organic materials and / or metals, metalloids, alkalis or alkaline earths earthy, and other residues encountered
- the invention relates to the use of a formulation comprising at least one alkanesulfonic acid, in particular at least methanesulfonic acid, for the removal of "beer stones” and bitter crowns formed during the development and / or preservation of beer.
- other related fermented beverages means any type of beverage such as for example wine, cider, whiskey, sake, and more generally any type of alcoholic beverages whose production process uses yeasts or any other aerobic fermentation capable of releasing carbon dioxide.
- Example 1 Cleaning of dirt obtained from an industrial must
- the brewer's yeast Saccharomyces cerevisae
- the brewer's yeast is then introduced respecting the necessary amount of live yeast (50 mL of liquid yeast for 15 liters of must) in order to be placed in industrial conditions.
- the fermentation takes place at room temperature (between 15 and 25 ° C) for a period of 6 days. At the end of this time, the tank is drained.
- a crown of bitter is observed at the liquid / air interface in the top of the cylindro-conical tank.
- a prewashing step is carried out by circulation of 3 times 5 seconds of an alkaline solution containing 1.5% of sodium hydroxide (pause time between circulations: 5 minutes).
- the cleaning of the soil is carried out via the circulation of a cleaning formulation under stable and controlled hydrodynamic conditions, via a fixed spraying ball (Brand Stre, type M1-1 DN8) located on the part high of the tank. More particularly, the flow rate is 1400 L / min and the spraying pressure is 0.2 bar relative (1.2 bar absolute), the solution being maintained at ambient temperature (between 15 ° C and 25 ° C). ) until total disappearance of the stains. Every 5 minutes, the circulation is interrupted to check the disappearance of the eye in the tank. The cleaning is estimated visually and the time required to obtain a visibly clean tank is thus established.
- a fixed spraying ball Brand
- test is replicated at least 6-fold (2 fermentations in 3 distinct fermentation sequences).
- Table 1 shows the durations, expressed in additional or less time (minutes), necessary for the total visual removal of soiling, compared with a cleaning carried out with reference formulation A (1.15% by mass of acid). phosphoric). ⁇ b> ⁇ u> - Table 1 - ⁇ / u> ⁇ /b> Formulation of cleaning Time greater or less in minutes than the reference 1.5% volume of formulation reference A 0 1.5% formulation volume 1 30 1% formulation volume 2 -10
- the acid formulation 2 according to the invention allows a time saving of 40 minutes compared to another acid formulation (formic acid) and even 10 minutes compared to the reference formulation (phosphoric acid).
- the reconstituted must is a must obtained by dilution of a commercially available kit for the manufacture of beer (reference "Brewferm” type of beer: white beer, wheat basis).
- the must is reconstituted according to the manufacturer's instructions: dilution of must concentrate (1 L) in 14 L of cold water and addition of 750 g of sugar.
- the lyophilized yeast sachet included in the kit is added to the reconstituted must just before fermentation.
- Table 2 shows the durations expressed in additional or less time (minutes) necessary for the removal of soil, compared to the reference formulation (1.15% by mass of phosphoric acid). ).
- Table 2 ⁇ / b> - ⁇ / u> Formulation of cleaning Time greater or less in minutes than the reference 1.5% volume of formulation reference A 0 1.5% formulation volume 1 + 15 1% formulation volume 2 -10
- This solid residue is dried for 24 hours at 40 ° C and weighed.
- Table 3 below shows the average percentage of "beer stones" dissolved in two samples according to each cleaning formulation used:
- methanesulfonic acid formulation has an effectiveness in terms of bitter corona removal similar to a phosphoric acid formulation, and an efficiency similar to that of sulfuric acid, in terms of elimination of beer stones.
- the method of the invention eliminates the two acid cleaning steps (phosphoric and sulfuric) recommended so far, with a single acid cleaning formulation comprising at least one alkanesulfonic acid effective for the elimination at a time "beer stones" and bitter crown.
- Calcium oxalate (6 g) is placed in 100 g of a solution of methanesulphonic acid (4 g / l and 12 g / l) on the one hand and in 100 g of a phosphoric acid solution (4 g / L and 12 g / L) secondly, for 24 hours at 70 ° C.
- the solution is then filtered and the filtrate is analyzed for ICP spectrometry assay of the calcium ions present in the solution.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Detergent Compositions (AREA)
- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Cleaning In General (AREA)
- Devices For Dispensing Beverages (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
La présente invention concerne un procédé de nettoyage acide dans l'industrie brassicole, et en particulier un procédé amélioré de nettoyage acide des divers matériels utilisés pour la fabrication de la bière et autres boissons fermentées apparentées.The present invention relates to an acid cleaning process in the brewing industry, and in particular to an improved acid cleaning process of the various materials used in the manufacture of beer and other related fermented beverages.
Il convient de rappeler tout d'abord le procédé de fabrication de la bière, qui se déroule le plus souvent en quatre étapes successives :
- 1. le brassage : cette étape consiste à mélanger les céréales (orge, malt (orge germée), blé, riz) avec de l'eau chaude (avec des paliers de température de 40°C à 100°C) et des aromates tels que le houblon et éventuellement des épices diverses et variées. Cette étape permet d'extraire des céréales les sucres et protéines pour former ce qu'on appelle le moût ;
- 2. la filtration : le moût ainsi obtenu est filtré pour donner d'un côté le moût dit clarifié et refroidi et de l'autre les résidus solides insolubles de céréales appelés drêche ;
- 3. la fermentation : le moût clarifié, après refroidissement est introduit dans le fermenteur (généralement un réacteur cylindro-conique) appelé FVT. La levure est ajoutée et l'ensemble macère durant trois à sept jours à une température de 6 à 10°C. Cette étape transforme le glucose et les sucres en dioxyde de carbone et éthanol.
- 4. la garde : à la fin de la fermentation, le mélange subit un choc froid à 3°C pour faire coaguler les levures et les protéines. Cette étape a lieu soit dans le fermenteur soit dans une autre cuve. La bière obtenue est mise à maturation dans le réacteur de garde puis clarifiée.
- 1. brewing : this stage consists in mixing the cereals (barley, malt (germinated barley), wheat, rice) with hot water (with temperature levels from 40 ° C to 100 ° C) and aromatics such as as hops and possibly various and varied spices. This stage makes it possible to extract cereals sugars and proteins to form what is called must;
- 2. filtration : the must thus obtained is filtered to give on one side the so-called clarified and cooled must and on the other the insoluble solid residues of cereals called distillers;
- 3. fermentation : the clarified must, after cooling is introduced into the fermenter (usually a cylindro-conical reactor) called FVT. The yeast is added and the whole macerates for three to seven days at a temperature of 6 to 10 ° C. This step converts glucose and sugars into carbon dioxide and ethanol.
- 4. the guard : at the end of the fermentation, the mixture is shocked cold at 3 ° C to coagulate the yeasts and proteins. This step takes place either in the fermenter or in another tank. The resulting beer is matured in the guard reactor and clarified.
À l'issue de ces quatre étapes de préparation, la bière est conditionnée dans des fûts ou dans des bouteilles, voire des canettes.At the end of these four preparation stages, the beer is packaged in barrels or in bottles or even cans.
Lors de l'étape de fermentation (étape 3), on observe souvent la formation d'une couronne d'amer (ou couronne de levure, « yeast ring » en langue anglaise) à l'interface phase gaz/phase liquide. L'amer est constitué principalement d'insolubles organiques : résidu de levure, paroi cellulaire, sucres insolubles.During the fermentation stage (step 3), the formation of a crown of bitter (or yeast ring, in English) is often observed. at the gas phase / liquid phase interface. Bitter is mainly composed of organic insolubles: yeast residue, cell wall, insoluble sugars.
En outre, en fond de fermenteur et sur ses parois se forment des « pierres de bière » (« beerstones » en langue anglaise), qui sont majoritairement constituées d'oxalate de calcium et de diverses matières organiques.In addition, fermentor bottoms and on its walls form "beer stones" ("beerstones" in English), which consist mainly of calcium oxalate and various organic materials.
Le fermenteur est par conséquent couramment souillé par deux types de salissures bien distinctes : des salissures organiques (majoritairement couronne d'amer) et des salissures inorganiques (principalement les « pierres de bière »).The fermenter is therefore commonly soiled by two distinct types of soiling: organic soils (mainly bitter crown) and inorganic soils (mainly "beer stones").
Or, un aspect primordial lors de la préparation de la bière, ou d'autres boissons fermentées apparentées, est de disposer de fûts, récipients, fermenteurs, canalisations et autres dispositifs de transport ou séjour des liquides utilisés dans la préparation desdites bière et autres boissons fermentées, qui soient absolument propres et en particulier exempt de toute trace de salissures organiques et inorganiques. En effet, de telles salissures pourraient engendrer la présence et la croissance de bactéries ou de tout autres éléments nuisibles aux produits préparés, voire les rendre impropres à la consommation.However, a crucial aspect in the preparation of beer, or other related fermented beverages, is to dispose of drums, containers, fermenters, pipes and other devices for the transport or residence of the liquids used in the preparation of the beer and other beverages. fermented, which are absolutely clean and in particular free from any trace of organic and inorganic soils. Indeed, such fouling could cause the presence and growth of bacteria or any other elements harmful to the prepared products, or even make them unfit for consumption.
Afin d'éviter les souillures organiques et inorganiques, chaque réacteur subit un lavage, soit en milieu basique soit en milieu acide selon l'étape concernée de la préparation de la bière. Le lavage des différents éléments de l'installation servant à la préparation de la bière est habituellement effectué selon les étapes suivantes :
- A) réacteur de brassage : lavage basique à l'hydroxyde de sodium ;
- B) cuve de fermentation contenant salissures organiques et inorganiques : lavage mixte en 3 étapes :
- 1. Pré nettoyage dit lavage « one way » (élimination directe à la station) à l'eau claire (élimination de 10 % des salissures), ou en présence de soude diluée (élimination de 80-90 % des salissures) sous forme de « shot » rapide, qui permet une meilleure élimination des salissures. L'hydroxyde de sodium ne peut cependant pas être utilisé en grande quantité car la cuve de fermentation contient du dioxyde de carbone susceptible de réagir avec l'hydroxyde de sodium qui pourrait entraîner l'implosion de la cuve par dépression ;
- 2. Nettoyage à l'aide d'acide phosphorique (généralement à 1,5% volumique d'une solution à 56% poids d'acide phosphorique) ; et
- 3. Désinfection à l'aide d'un mélange d'acide sulfurique à faible teneur et d'un biocide.
À l'heure actuelle, les étapes 2 et 3 de lavage sont réalisées de manière successive à l'aide de deux acides différents, chacun étant efficace pour l'élimination d'un type de salissure :- l'acide phosphorique est utilisé pour nettoyer la couronne d'amer :
- l'acide sulfurique est utilisé pour nettoyer les pierres de bière, l'acide phosphorique étant inefficace vis-à-vis de ce type de salissure (oxalate de calcium). L'utilisation de l'acide sulfurique n'est toutefois pas sans inconvénient en raison de son pouvoir corrosif. Cet effet de corrosion peut toutefois être atténué en travaillant à basse température.
- C) garde : celle-ci comporte généralement moins de salissures que le fermenteur et en particulier peu ou pas de couronne d'amer ; on réalise par conséquent le plus souvent un simple nettoyage à l'eau suivi d'un nettoyage avec le mélange acide sulfurique + biocide indiqué ci-dessus.
- A) brewing reactor: basic washing with sodium hydroxide;
- B) fermentation tank containing organic and inorganic soils: mixed wash in 3 steps:
- 1. Pre-cleaning called "one-way" washing with clean water (removal of 10% of the soil), or in the presence of dilute soda (removal of 80-90% of the soil) in the form of Fast "shot", which allows a better elimination of soiling. Sodium hydroxide, however, can not be used in large quantities because the fermentation tank contains carbon dioxide that may react with sodium hydroxide which could cause the vessel to collapse by depression;
- 2. Cleaning with phosphoric acid (generally 1.5% by volume of a 56% by weight solution of phosphoric acid); and
- 3. Disinfection with a mixture of low sulfuric acid and a biocide.
At present, the washing steps 2 and 3 are carried out successively with the aid of two different acids, each being effective for the removal of a type of soiling:- phosphoric acid is used to clean the bitter crown:
- sulfuric acid is used to clean beer stones, since phosphoric acid is ineffective against this kind of soiling (calcium oxalate). The use of sulfuric acid is however not without inconvenience because of its corrosive power. This corrosion effect can however be mitigated by working at low temperatures.
- C) guard: this generally has less soil than the fermentor and in particular little or no bitter crown; therefore, most often a simple cleaning with water followed by cleaning with sulfuric acid + biocide mixture indicated above.
Par ailleurs, les fûts sont nettoyés à chaud (typiquement environ 80°C) au moyen d'acide phosphorique, l'acide sulfurique étant trop corrosif à cette température, comme indiqué supra. Moreover, the barrels are cleaned hot (typically about 80 ° C) with phosphoric acid, the sulfuric acid being too corrosive at this temperature, as indicated above.
Il doit en outre être compris qu'entre chaque étape de nettoyage, un rinçage à l'eau claire est effectué. Le document
Ainsi, un premier objectif de la présente invention consiste à proposer un procédé de nettoyage des installations utilisées dans la fabrication et le stockage de la bière plus simple et plus rapide que ceux utilisés actuellement.Thus, a first object of the present invention is to provide a method of cleaning facilities used in the manufacture and storage of beer simpler and faster than those currently used.
Un autre objectif de la présente invention est de proposer un procédé simple et efficace permettant à la fois un nettoyage efficace de « pierres de bière » et des couronnes d'amer.Another object of the present invention is to provide a simple and effective method for both efficient cleaning of "beer stones" and bitter crowns.
Un autre objectif encore est de proposer un procédé de nettoyage des installations utilisées lors de la préparation et du stockage de la bière et autres boissons fermentées apparentées, au moyen d'une formulation unique permettant l'élimination de tous les types de salissures, notamment les « pierres de bière » et les couronnes d'amer.Yet another object is to provide a method of cleaning the facilities used in the preparation and storage of beer and other related fermented beverages, by means of a unique formulation allowing the elimination of all types of soiling, including "beer stones" and bitter crowns.
D'autres avantages encore apparaîtront au cours de la description de la présente invention qui suit.Still other advantages will become apparent from the description of the present invention which follows.
Les documents
Il a maintenant été découvert de manière tout à fait surprenante qu'il est possible d'effectuer un nettoyage complet et efficace des installations utilisées pour la fabrication de la bière en utilisant une formulation à base d'acide alcanesulfonique.It has now been discovered quite surprisingly that it is possible to perform a complete and efficient cleaning of the facilities used for the manufacture of beer using an alkanesulfonic acid-based formulation.
En effet, il a pu être mis en évidence qu'une formulation à base d'acide alcanesulfonique permet à la fois l'élimination de la couronne d'amer (couramment éliminée par l'acide phosphorique) et l'élimination des « pierres de bière » (habituellement éliminées par action d'acide sulfurique).Indeed, it has been demonstrated that an alkanesulfonic acid formulation allows both the removal of the bitter crown (commonly eliminated by phosphoric acid) and the elimination of beer '(usually removed by the action of sulfuric acid).
Ainsi, l'utilisation d'une formulation à base d'acide alcanesulfonique permet d'éviter l'utilisation de plusieurs formulations nettoyantes, telles qu'une formulation à base d'acide phosphorique et une formulation à base d'acide sulfurique. L'utilisation d'une formulation à base d'acide alcanesulfonique peut également permettre d'éviter plusieurs opérations de lavages successives et également plusieurs rinçages intermédiaires.Thus, the use of an alkanesulfonic acid-based formulation avoids the use of several cleaning formulations, such as a phosphoric acid formulation and a sulfuric acid based formulation. The use of an alkanesulfonic acid-based formulation may also make it possible to avoid several successive washing operations and also several intermediate rinses.
Les avantages sont donc principalement un gain de temps, de coûts, de productivité, d'énergie, ainsi qu'une diminution du nombre de produits chimiques de nettoyage présents sur le site de fabrication.The benefits are therefore mainly a saving of time, costs, productivity, energy, as well as a decrease in the number of cleaning chemicals present at the manufacturing site.
Par ailleurs, l'acide phosphorique habituellement utilisé est rejeté sous forme de phosphates, ce qui peut nuire à l'environnement, et les normes environnementales de plus en plus sévères visent à proscrire les rejets de phosphates.In addition, the phosphoric acid usually used is released in the form of phosphates, which can harm the environment, and increasingly stringent environmental standards aim to outlaw phosphate releases.
Ainsi, un premier objet de l'invention consiste en un procédé de nettoyage d'une installation utilisée dans la préparation de la bière, ou autres boissons fermentées apparentées, comprenant les étapes de :
- a) prélavage éventuel de l'installation ;
- b) lavage de l'installation par circulation dans ladite installation d'une quantité efficace d'une formulation comprenant au moins un acide alcanesulfonique ; et
- c) rinçage de l'installation par circulation d'une solution de rinçage.
- a) possible pre-washing of the installation;
- b) washing the plant by circulating in said plant an effective amount of a formulation comprising at least one alkanesulfonic acid; and
- c) rinsing the installation by circulation of a rinsing solution.
Ainsi, le procédé de l'invention permet d'une part de réduire le nombre d'étapes de nettoyage, et d'autre part de réduire le nombre de formulations acides utilisées, de deux (acide phosphorique et acide sulfurique) à une seule formulation de nettoyage des salissures.Thus, the method of the invention makes it possible on the one hand to reduce the number of cleaning steps, and on the other hand to reduce the number of acid formulations used, from two (phosphoric acid and sulfuric acid) to a single formulation cleaning of dirt.
En outre, la formulation utilisée dans le procédé de l'invention étant moins corrosive que l'acide sulfurique, celle-ci peut être utilisée pour le nettoyage des fûts à chaud.In addition, the formulation used in the process of the invention being less corrosive than sulfuric acid, it can be used for cleaning hot drums.
Plus particulièrement, le procédé de la présente invention concerne le nettoyage des installations utilisées pour la préparation et le stockage de la bière et autres boissons fermentées apparentées.More particularly, the process of the present invention relates to the cleaning of facilities used for the preparation and storage of beer and other related fermented beverages.
Par « installation », on entend les divers éléments communément utilisés dans les brasseries, et notamment les cuves, fûts, fermenteurs, canalisations, vannes, bouteilles, cannettes, et autres, c'est-à-dire tous les éléments susceptibles d'entrer en contact avec la bière et autres liquides ou solides nécessaires à sa fabrication."Installation" means the various elements commonly used in breweries, including vats, barrels, fermenters, pipelines, valves, bottles, cans, and others, that is, all the elements likely to enter in contact with beer and other liquids or solids necessary for its manufacture.
Les matériaux des divers éléments constitutifs de l'installation sont généralement choisis parmi l'inox, l'aluminium, le cuivre, le laiton, l'acier revêtu ou non par exemple par une résine époxy, le plastique, en particulier polypropylène, polyéthylène, poly(chlorure de vinyle), le verre, et autres.The materials of the various components of the installation are generally selected from stainless steel, aluminum, copper, brass, steel coated or not, for example by an epoxy resin, plastic, in particular polypropylene, polyethylene, poly (vinyl chloride), glass, and others.
Selon un mode de réalisation préféré, les matériaux utilisés pour les installations de brasserie sont choisis parmi l'inox 304L ou 316L, l'aluminium, et l'acier revêtu de résine époxy.According to a preferred embodiment, the materials used for the brewery installations are chosen from stainless steel 304L or 316L, aluminum, and steel coated with epoxy resin.
Il doit être compris que le procédé de l'invention s'applique à l'ensemble ou seulement à une ou plusieurs parties de l'installation de fabrication de la bière ou autres boissons fermentées apparentées. Dans la présente description, le terme « installation » désigne l'ensemble de l'installation ou une ou plusieurs parties seulement de l'installation.It should be understood that the process of the invention applies to all or only one or more parts of the beer manufacturing facility or other related fermented beverages. In the present description, the term "installation" refers to the entire installation or one or more parts of the installation.
Le procédé selon l'invention comprend une éventuelle première étape de prélavage, destinée à éliminer de manière mécanique la plus grosse partie des impuretés. Le prélavage est effectué par circulation d'eau, seule ou en combinaison avec des « shots » d'une solution alcaline, de préférence diluée, par exemple une solution aqueuse d'hydroxyde de potassium ou de sodium. On entend par « shot », l'envoi dans la partie de l'installation à nettoyer d'une solution alcaline, généralement faiblement concentrée, que nous laissons agir durant un temps court. Par temps court, il est entendu une période allant de quelques secondes à plusieurs minutes, voire quelques heures.The method according to the invention comprises a possible first prewash stage, intended to mechanically remove the largest part of the impurities. The prewash is carried out by circulation of water, alone or in combination with "shots" of an alkaline solution, preferably diluted, for example an aqueous solution of potassium hydroxide or sodium hydroxide. We means "shot", sending in the part of the installation to clean with an alkaline solution, usually weakly concentrated, that we let act for a short time. In short time, it is understood a period ranging from a few seconds to several minutes or even hours.
Après l'étape de prélavage, le lavage de l'installation est réalisé par circulation d'une formulation comprenant au moins un acide alcanesulfonique.After the prewashing step, the washing of the installation is carried out by circulation of a formulation comprising at least one alkanesulfonic acid.
Dans la présente invention, on entend par acide alcanesulfonique préférentiellement les acides alcanesulfoniques comportant une chaîne hydrocarboné saturée, linéaire ou ramifiée, comportant de 1 à 4 atomes de carbone. Les acides alcanesulfoniques utilisables dans le procédé de la présente invention sont particulièrement choisis parmi l'acide méthanesulfonique, l'acide éthanesulfonique, l'acide n-propanesulfonique, l'acide iso-propanesulfonique, l'acide n-butanesulfonique, l'acide iso-butanesulfonique, l'acide sec-butanesulfonique, l'acide tert-butanesulfonique, et les mélanges de deux ou plusieurs d'entre eux en toutes proportions.In the present invention, the term "alkanesulphonic acid" is understood to mean alkanesulphonic acids comprising a saturated hydrocarbon chain, linear or branched, containing from 1 to 4 carbon atoms. Alkanesulfonic acids used in the process of the present invention are particularly selected from methanesulfonic acid, ethanesulfonic acid, n-propanesulfonic acid, iso propanesulfonic acid, n-butanesulfonic acid, iso acid -butanesulfonique, the sec-butanesulfonic acid, tert -butanesulfonique acid, and mixtures of two or more of them in any proportion.
Selon un mode de réalisation préféré, l'acide alcanesulfonique utilisé dans le procédé de la présente invention est l'acide méthanesulfonique ou l'acide éthanesulfonique, de manière tout à fait préférée l'acide utilisé est l'acide méthanesulfonique.In a preferred embodiment, the alkanesulfonic acid used in the process of the present invention is methanesulfonic acid or ethanesulfonic acid, most preferably the acid used is methanesulfonic acid.
Ainsi, la formulation de nettoyage comprenant au moins un acide alcanesulfonique mise en oeuvre dans le procédé de l'invention comprend un ou plusieurs acides alcanesulfoniques à chaîne linéaire ou ramifiée comportant de 1 à 4 atomes de carbone, et de préférence comprend au moins de l'acide méthanesulfonique (AMS).Thus, the cleaning formulation comprising at least one alkanesulfonic acid used in the process of the invention comprises one or more linear or branched chain alkanesulfonic acids comprising from 1 to 4 carbon atoms, and preferably comprises at least one carbon atom. methanesulfonic acid (AMS).
En règle générale, la formulation comprend de 0,1% à 100 % en poids d'acide alcanesulfonique, plus généralement de 0,5 % à 90 % en poids, en particulier de 0,5 % à 20 % en poids d'acide alcanesulfonique, et plus particulièrement de 0,5 % à 5 % en poids.As a rule, the formulation comprises from 0.1% to 100% by weight of alkanesulfonic acid, more generally from 0.5% to 90% by weight, in particular from 0.5% to 20% by weight of acid. alkanesulfonic acid, and more particularly from 0.5% to 5% by weight.
La formulation est généralement une formulation aqueuse qui peut être préparée sous forme de mélange concentré qui est dilué par l'utilisateur final. En variante, la formulation peut également être une formulation prête à l'emploi, c'est-à-dire qui ne nécessite pas d'être diluée. On peut par exemple utiliser de l'acide méthanesulfonique en solution à 70% en poids dans l'eau, et commercialisé par la société Arkema sous la dénomination Scaleva™, prêt à l'emploi ou dilué à l'eau dans les proportions indiquées ci-dessus.The formulation is generally an aqueous formulation that can be prepared as a concentrated mixture that is diluted by the end user. Alternatively, the formulation may also be a ready-to-use formulation, i.e., which does not need to be diluted. It is possible, for example, to use methanesulphonic acid in solution at 70% by weight in water and marketed by the Arkema under the name Scaleva ™ , ready for use or diluted with water in the proportions indicated above.
Outre le ou les acides alcanesulfoniques, la formulation de nettoyage peut éventuellement comprendre un ou plusieurs additifs, solvants, biocides et autres agents rhéologiques ou de texture, choisis parmi solvants et co-solvants, acides organiques ou minéraux (par exemple sulfurique, phosphorique, nitrique, sulfamique, citrique), agents épaississants, tensio-actifs, moussants, anti-moussants, et autres connus de l'homme du métier.In addition to the alkanesulfonic acid or acids, the cleaning formulation may optionally comprise one or more additives, solvents, biocides and other rheological or textural agents chosen from solvents and co-solvents, organic or inorganic acids (for example sulfuric, phosphoric or nitric acids). sulfamic, citric), thickening agents, surfactants, foaming agents, anti-foaming agents, and others known to those skilled in the art.
Il a été découvert que les acides alcanesulfoniques tels qu'ils viennent d'être décrits sont efficaces pour nettoyer les salissures présentes ou formées dans les installations utilisées lors de la préparation de bière et autres boissons fermentées apparentées.It has been discovered that the alkanesulfonic acids as just described are effective in cleaning the soils present or formed in facilities used in the preparation of beer and other related fermented beverages.
L'utilisation d'acides alcanesulfoniques permet ainsi d'éliminer les salissures organiques et inorganiques, telles que hydrates de carbone, graisses, protéines, minéraux inorganiques tels que carbonate de calcium, phosphate de calcium, et autres types de tartre comprenant des oxalates, sulfates, hydroxydes et/ou sulfures, combinés ou non à diverses matières organiques et/ou métaux, métalloïdes, alcalins ou alcalino-terreux, et autres résidus rencontrés dans la préparation de la bière ou autre boisson fermentée apparentée.The use of alkanesulfonic acids thus makes it possible to eliminate organic and inorganic soils, such as carbohydrates, fats, proteins, inorganic minerals such as calcium carbonate, calcium phosphate, and other types of scale comprising oxalates and sulphates. hydroxides and / or sulfides, whether or not combined with various organic materials and / or metals, metalloids, alkalis or alkaline earths, and other residues encountered in the preparation of beer or other related fermented beverages.
Les acides alcanesulfoniques sont particulièrement efficaces pour éliminer les résidus de type « pierres de bière » et « couronne d'amer » comme indiqué précédemment.Alkanesulfonic acids are particularly effective in removing "beer stone" and "bitter crown" residues as previously indicated.
Le lavage (ou nettoyage) de toute ou partie de l'installation est réalisée par circulation d'une quantité efficace d'une formulation comprenant au moins un acide alcanesulfonique, telle qu'elle vient d'être décrite.The washing (or cleaning) of all or part of the installation is carried out by circulating an effective amount of a formulation comprising at least one alkanesulfonic acid, as just described.
Par quantité efficace, on entend une quantité permettant l'élimination de toutes les salissures, qui, si elles ne sont pas correctement éliminées, pourraient favoriser le développement de bactéries. Ainsi, le procédé de l'invention permet d'éliminer tous les types de salissures, et par voie de conséquence les bactéries qui pourraient nuire à la fabrication, la conservation, la saveur, la texture, et la non-toxicité pour l'homme, de la bière ou autre boisson fermentée apparentée préparée dans l'installation et stockée dans des fûts, bouteilles, canettes et autres.By effective amount is meant an amount for the removal of all soils, which, if not properly removed, could promote the development of bacteria. Thus, the process of the invention makes it possible to eliminate all types of soiling, and consequently the bacteria that could adversely affect the manufacture, the preservation, the flavor, the texture, and the non-toxicity for humans. , beer or other related fermented drink prepared in the facility and stored in drums, bottles, cans and others.
Cette quantité peut varier dans de grandes proportions, selon le volume de l'installation à nettoyer, de la nature et de la quantité de salissures que l'on souhaite éliminer, de la température et de la pression de la formulation utilisée, et autres.This quantity can vary in large proportions, depending on the volume of the installation to be cleaned, the nature and amount of dirt that it is desired to eliminate, the temperature and pressure of the formulation used, and others.
En règle générale, une quantité efficace de la formulation acide nettoyante est mise en circulation dans l'installation, cette circulation étant établie pendant une durée suffisante pour permettre l'élimination totale des salissures.As a general rule, an effective amount of the acidic cleaning formulation is circulated in the plant, this circulation being established for a time sufficient to allow complete removal of soil.
Un test visuel de l'installation, ou encore une mesure de l'activité bactériologique au sein de l'installation selon des techniques classiques connues de l'homme du métier, permettent de déterminer la quantité efficace de formulation à utiliser et la durée de circulation de ladite formulation nécessaires à l'élimination totale des salissures.A visual test of the installation, or a measurement of the bacteriological activity within the installation according to conventional techniques known to those skilled in the art, make it possible to determine the effective amount of formulation to be used and the duration of circulation. of said formulation necessary for the total elimination of soiling.
Ainsi, la quantité de formulation et la durée de circulation seront établies pour permettre une élimination totale des salissures, tout en observant à la fois une quantité minimale de formulation (essentiellement pour des raisons économiques et environnementales) et une durée de circulation la plus courte possible (également essentiellement pour des raisons économiques).Thus, the amount of formulation and the duration of circulation will be established to allow a total elimination of soiling, while observing both a minimal amount of formulation (mainly for economic and environmental reasons) and a shortest possible circulation time (also mainly for economic reasons).
Le nettoyage acide avec la formulation comprenant au moins un acide alcanesulfonique comme indiqué précédemment peut être réalisé à toutes températures, généralement comprises entre 0°C et 100°C, plus généralement comprises entre 5°C et 40°C, typiquement entre 5°C et 20°C dans le fermenteur ou le réacteur de garde et entre 60°C et 80°C dans les récipients de conditionnement (fûts, bouteilles ou canettes) de la bière ou autre boisson fermentée apparentée.The acid cleaning with the formulation comprising at least one alkanesulfonic acid as indicated above can be carried out at all temperatures, generally between 0 ° C and 100 ° C, more generally between 5 ° C and 40 ° C, typically between 5 ° C and 20 ° C in the fermenter or guard reactor and between 60 ° C and 80 ° C in the packaging containers (drums, bottles or cans) of the beer or other related fermented beverage.
Après l'étape de lavage à l'aide de la formulation comprenant au moins un acide alcanesulfonique, l'installation est avantageusement rincée par circulation d'une solution de rinçage, par exemple à l'eau, de manière connue de l'homme du métier.After the washing step using the formulation comprising at least one alkanesulfonic acid, the installation is advantageously rinsed by circulation of a rinsing solution, for example with water, in a manner known to the man of the job.
Grâce au procédé de l'invention, le lavage d'une installation utile à la préparation de la bière ou d'autres boissons fermentées apparentées est effectué en une seule étape de lavage acide, contrairement aux techniques connues aujourd'hui. Cette unique étape de lavage acide permet d'éliminer en particulier les « pierres de bière » ainsi que les couronnes d'amer formées au cours de la fabrication desdites bières et autres boissons fermentées apparentées.Thanks to the method of the invention, the washing of a facility useful for the preparation of beer or other related fermented drinks is carried out in a single step of acid washing, unlike the techniques known today. This single stage of acid washing eliminates in particular "Beer stones" and bitter crowns formed during the manufacture of said beer and other related fermented beverages.
Selon un autre objet, la présente invention concerne l'utilisation d'une formulation comprenant au moins un acide alcanesulfonique, en particulier au moins de l'acide méthanesulfonique, pour l'élimination des salissures organiques et inorganiques, telles que hydrates de carbone, graisses, protéines, minéraux inorganiques tels que carbonate de calcium, phosphate de calcium, et autres types de tartre comprenant des oxalates, sulfates, hydroxydes et/ou sulfures, combinés ou non à diverses matières organiques et/ou métaux, métalloïdes, alcalins ou alcalino-terreux, et autres résidus rencontrés dans la préparation de la bière ou autre boisson fermentée apparentée.According to another object, the present invention relates to the use of a formulation comprising at least one alkanesulfonic acid, in particular at least methanesulphonic acid, for the removal of organic and inorganic soils, such as carbohydrates, fats , proteins, inorganic minerals such as calcium carbonate, calcium phosphate, and other types of scale comprising oxalates, sulphates, hydroxides and / or sulphides, whether or not combined with various organic materials and / or metals, metalloids, alkalis or alkaline earths earthy, and other residues encountered in the preparation of beer or other related fermented beverage.
Plus particulièrement, l'invention concerne l'utilisation d'une formulation comprenant au moins un acide alcanesulfonique, en particulier au moins de l'acide méthanesulfonique, pour l'élimination de « pierres de bière » et couronnes d'amer formées au cours de l'élaboration et/ou de la conservation de la bière.More particularly, the invention relates to the use of a formulation comprising at least one alkanesulfonic acid, in particular at least methanesulfonic acid, for the removal of "beer stones" and bitter crowns formed during the development and / or preservation of beer.
Par « autres boissons fermentées apparentées », on entend tout type de boissons telles que par exemple le vin, le cidre, le whisky, le saké, et plus généralement tout type de boissons alcoolisées dont le procédé de fabrication met en oeuvre des levures ou tout autre fermentation aérobie susceptible de dégager du gaz carbonique.By "other related fermented beverages" means any type of beverage such as for example wine, cider, whiskey, sake, and more generally any type of alcoholic beverages whose production process uses yeasts or any other aerobic fermentation capable of releasing carbon dioxide.
La présente invention est illustrée au moyens des exemples qui suivent, sans présenter aucun caractère limitatif, et qui ne peuvent être par conséquent compris comme susceptibles de restreindre la portée de l'invention telle que revendiquée.The present invention is illustrated by means of the examples which follow, without presenting any limiting character, and which can not therefore be understood as likely to restrict the scope of the invention as claimed.
Dans une cuve cylindro-conique de 74 cm x 18 cm de corps et d'une longueur de cône de 17 cm en acier inoxydable (volume 316 L), sont introduits 5 litres de moût clarifié de brasserie refroidie à température ambiante (entre 15 et 25°C).In a cylindrical-conical bowl of 74 cm x 18 cm body and a cone length of 17 cm stainless steel (volume 316 L), are introduced 5 liters of broth clarified broth cooled to room temperature (between 15 and 25 ° C).
La levure de brasserie (Saccharomyces cerevisae) est ensuite introduite en respectant la quantité nécessaire de levure vivante (50 mL de levure liquide pour 15 litres de moût) et ce afin de se placer dans des conditions industrielles.The brewer's yeast ( Saccharomyces cerevisae ) is then introduced respecting the necessary amount of live yeast (50 mL of liquid yeast for 15 liters of must) in order to be placed in industrial conditions.
La fermentation a lieu à température ambiante (entre 15 et 25 °C) pendant une durée de 6 jours. Au bout de ce laps de temps, la cuve est vidangée.The fermentation takes place at room temperature (between 15 and 25 ° C) for a period of 6 days. At the end of this time, the tank is drained.
En conformité avec la pratique industrielle, une couronne d'amer (levure et salissures organiques associées) est observée à l'interface liquide / air dans le haut de la cuve cylindro-conique.In accordance with industrial practice, a crown of bitter (yeast and associated organic fouling) is observed at the liquid / air interface in the top of the cylindro-conical tank.
La répétabilité de la formation des salissures a été évaluée sur de nombreuses fermentations pilote (une trentaine au total) et permet de garantir un niveau de salissure représentatif de la pratique et d'une reproductibilité satisfaisante.The repeatability of the formation of soils has been evaluated on many pilot fermentations (about thirty in total) and ensures a level of soiling representative of the practice and a satisfactory reproducibility.
Une étape de prélavage est réalisée par circulation de 3 fois 5 secondes d'une solution alcaline à 1,5 % d'hydroxyde de sodium (temps de pause entre les circulations : 5 minutes).A prewashing step is carried out by circulation of 3 times 5 seconds of an alkaline solution containing 1.5% of sodium hydroxide (pause time between circulations: 5 minutes).
Le nettoyage de la salissure est réalisé via la circulation d'une formulation de nettoyage dans des conditions hydrodynamiques stables et contrôlées, par l'intermédiaire d'une boule d'aspersion fixe (Marque Hacke, type M1-1 DN8) située sur la partie haute de la cuve. Plus particulièrement, le débit de circulation est de 1400 L/min et la pression d'aspersion est de 0,2 bars relatifs (1,2 bars absolus), la solution étant maintenue à température ambiante (entre 15°C et 25 °C) jusqu'à disparition totale des salissures. Toutes les 5 minutes, la circulation est interrompue afin de vérifier la disparition à l'oeil des salissures dans la cuve. Le nettoyage est estimé visuellement et le temps nécessaire pour l'obtention d'une cuve visiblement propre est ainsi établi.The cleaning of the soil is carried out via the circulation of a cleaning formulation under stable and controlled hydrodynamic conditions, via a fixed spraying ball (Brand Hacke, type M1-1 DN8) located on the part high of the tank. More particularly, the flow rate is 1400 L / min and the spraying pressure is 0.2 bar relative (1.2 bar absolute), the solution being maintained at ambient temperature (between 15 ° C and 25 ° C). ) until total disappearance of the stains. Every 5 minutes, the circulation is interrupted to check the disappearance of the eye in the tank. The cleaning is estimated visually and the time required to obtain a visibly clean tank is thus established.
Pour chaque condition expérimentale, le test est répliqué au minimum 6 fois (2 fermentations dans 3 séquences de fermentation distinctes).For each experimental condition, the test is replicated at least 6-fold (2 fermentations in 3 distinct fermentation sequences).
De plus, afin de consolider la comparaison relative des tests de nettoyage, il a été décidé de placer systématiquement dans la séquence de test, un standard de nettoyage de référence se basant sur deux cuves destinées au nettoyage par la procédure habituelle avec une solution à 1,5 % en volume d'acide phosphorique à 56 % massique.In addition, in order to consolidate the relative comparison of the cleaning tests, it was decided to systematically place in the test sequence, a standard reference cleaning system based on two tanks for cleaning by the usual procedure with a 1.5% by volume solution of phosphoric acid at 56% by mass.
Les formulations acides utilisées sont les suivantes :
- Formulation référence A : acide phosphorique (H3PO4) à 56 % massique dans l'eau (d = 1,38, soit 1,15 % massique de H3PO4 pur).
- Formulation 1 (comparatif) : 55 % acide formique dans l'eau (d = 1,195 soit 0.98 % massique d'acide formique pur).
- Formulation 2 (selon l'invention) : 1 % volume dans l'eau d'acide méthane sulfonique à 70 % massique (d = 1,35, soit 0.94 % massique en acide méthane sulfonique pur).
- Formulation reference A : phosphoric acid (H 3 PO 4 ) at 56% by weight in water (d = 1.38, ie 1.15% by weight of pure H 3 PO 4 ).
- Formulation 1 (comparative): 55% formic acid in water (d = 1.195 or 0.98% by weight of pure formic acid).
- Formulation 2 (according to the invention): 1% volume in methanesulfonic acid water at 70% by mass (d = 1.35, ie 0.94% by weight of pure methanesulphonic acid).
Le tableau 1 ci-dessous reprend les durées, exprimées en temps (minutes) supplémentaire ou inférieur, nécessaires à l'élimination visuelle totale des salissures, par rapport à un nettoyage effectué avec formulation de référence A (1,15 % massique d'acide phosphorique).
On constate que la formulation acide 2 selon l'invention permet un gain de temps de 40 minutes par rapport à une autre formulation acide (acide formique) et même de 10 minutes par rapport à la formulation de référence (acide phosphorique).It is found that the acid formulation 2 according to the invention allows a time saving of 40 minutes compared to another acid formulation (formic acid) and even 10 minutes compared to the reference formulation (phosphoric acid).
Le moût reconstitué est un moût obtenu par dilution d'un kit disponible dans le commerce pour la fabrication de bière (référence « Brewferm » type de bière : bière blanche, base froment).The reconstituted must is a must obtained by dilution of a commercially available kit for the manufacture of beer (reference "Brewferm" type of beer: white beer, wheat basis).
Le moût est reconstitué conformément aux instructions du fabricant : dilution du concentré de moût (1 L) dans 14 L d'eau froide et ajout de 750 g de sucre. Le sachet de levure lyophilisée compris dans le kit est ajouté au moût reconstitué juste avant la mise en fermentation.The must is reconstituted according to the manufacturer's instructions: dilution of must concentrate (1 L) in 14 L of cold water and addition of 750 g of sugar. The lyophilized yeast sachet included in the kit is added to the reconstituted must just before fermentation.
Contrairement au moût industriel, le niveau de salissure initial est plus faible avec du moût reconstitué et l'étape de prélavage n'est pas nécessaire ; on effectue donc directement le nettoyage acide, comme à l'étape c) de l'exemple 1.Unlike industrial must, the initial level of soiling is lower with reconstituted must and the pre-wash step is not necessary; the acid cleaning is therefore carried out directly, as in step c) of Example 1.
Comme pour le tableau 1, le tableau 2 ci-dessous reprend les durées exprimées en temps (minutes) supplémentaire ou inférieur, nécessaires à l'élimination des salissures, par rapport à la formulation de référence (1,15 % massique d'acide phosphorique).
Ici encore, on constate une diminution de la durée de nettoyage nécessaire à l'élimination des salissures, lorsqu'il est effectué avec la formulation acide selon l'invention.Here again, there is a decrease in the cleaning time required for the removal of dirt, when it is carried out with the acid formulation according to the invention.
Deux échantillons représentatifs de « pierres de bière » ont été prélevés en brasserie sur des tanks de fermentation et soumis à l'expérimentation suivante :
- pesée précise d'environ 0,5 grammes de dépôts préalablement séchés à l'air pendant 24 heures à 40°C ;
- immersion sans agitation dans la formulation test portée à température ambiante (entre 15°C et 25°C) pendant 4 heures ;
- filtration de la solution liquide et récupération du solide non dissous.
- accurate weighing of about 0.5 grams of deposits previously air dried for 24 hours at 40 ° C;
- immersion without stirring in the test formulation brought to room temperature (between 15 ° C and 25 ° C) for 4 hours;
- filtration of the liquid solution and recovery of the undissolved solid.
Ce résidu solide est séché pendant 24 heures à 40°C, puis pesé.This solid residue is dried for 24 hours at 40 ° C and weighed.
Le tableau 3 ci dessous reprend le pourcentage moyen de « pierres de bière » dissoutes sur deux échantillons en fonction de chaque formulation de nettoyage utilisée :
Formulation référence A : acide phosphorique (H3PO4) à 56 % massique dans l'eau (d = 1,38, soit 1,15 % massique de H3PO4 pur).
Formulation référence B : acide sulfurique (H2SO4) à 78 % (densité = 1,7, soit 1,32 % massique produit pur).
Formulation 1 (comparatif) : 55 % acide formique dans l'eau (d = 1,195 soit 0,98 % massique d'acide formique pur).
Formulation 2 (selon l'invention) : 1 % volume dans l'eau d'acide méthane sulfonique à 70 % massique (d = 1,35, soit 0.94 % massique en acide méthane sulfonique pur).
Formulation reference A : phosphoric acid (H 3 PO 4 ) at 56% by weight in water (d = 1.38, ie 1.15% by weight of pure H 3 PO 4 ).
Formulation reference B : sulfuric acid (H 2 SO 4 ) at 78% (density = 1.7, or 1.32% by mass pure product).
Formulation 1 (comparative): 55% formic acid in water (d = 1.195 or 0.98% by weight of pure formic acid).
Formulation 2 (according to the invention): 1% volume in methanesulfonic acid water at 70% by mass (d = 1.35, ie 0.94% by weight of pure methanesulphonic acid).
On observe que la formulation à base d'acide méthanesulfonique présente une efficacité en termes d'élimination de la couronne d'amer similaire à une formulation d'acide phosphorique, ainsi qu'une efficacité similaire à celle de l'acide sulfurique, en termes d'élimination des pierres de bière.It is observed that the methanesulfonic acid formulation has an effectiveness in terms of bitter corona removal similar to a phosphoric acid formulation, and an efficiency similar to that of sulfuric acid, in terms of elimination of beer stones.
Ainsi le procédé de l'invention permet de s'affranchir des deux étapes de nettoyages acides (phosphorique et sulfurique) préconisées jusqu'à présent, avec une seule formulation de nettoyage acide comprenant au moins un acide alcanesulfonique efficace pour l'élimination à la fois des « pierres de bière » et de la couronne d'amer.Thus, the method of the invention eliminates the two acid cleaning steps (phosphoric and sulfuric) recommended so far, with a single acid cleaning formulation comprising at least one alkanesulfonic acid effective for the elimination at a time "beer stones" and bitter crown.
On place de l'oxalate de calcium (6 g) dans 100 g d'une solution d'acide méthanesulfonique (4 g/L et 12 g/L) d'une part et dans 100 g d'une solution d'acide phosphorique (4 g/L et 12 g/L) d'autre part, pendant 24 heures à 70°C.Calcium oxalate (6 g) is placed in 100 g of a solution of methanesulphonic acid (4 g / l and 12 g / l) on the one hand and in 100 g of a phosphoric acid solution (4 g / L and 12 g / L) secondly, for 24 hours at 70 ° C.
La solution est ensuite filtrée et le filtrat est analysé pour dosage par spectrométrie ICP des ions calcium présents dans la solution.The solution is then filtered and the filtrate is analyzed for ICP spectrometry assay of the calcium ions present in the solution.
Les résultats sont présentés dans le Tableau 4 suivant :
Ces résultats montrent que l'acide méthanesulfonique est beaucoup plus efficace que l'acide phosphorique pour dissoudre l'oxalate de calcium.These results show that methanesulfonic acid is much more effective than phosphoric acid in dissolving calcium oxalate.
Claims (11)
- Process for the cleaning of an installation used in the preparation and/or the storage of beer, or any type of alcoholic drinks whose manufacturing process involve yeast or any other aerobic fermentation medium likely to release carbon dioxide, comprising the steps of:optional pre-washing of the installation;washing of the installation by circulation in said installation of an effective quantity of a formulation comprising at least one alkane sulphonic acid; andrinsing of said installation by circulation of a rinsing solution.
- Process according to Claim 1, wherein the installation comprises one or more elements chosen from among tanks, barrels, fermentors, drains, valves, bottles and beer cans.
- Process according to Claim 1 or 2, wherein the pre-washing step is carried out with an aqueous solution of sodium or potassium hydroxide.
- Process according to any one of the preceding Claims, wherein the said at least one alkane sulphonic acid is chosen from among methane sulphonic acid, ethane sulphonic acid, n-propane sulphonic acid, iso-propane sulphonic acid, n-butane sulphonic acid, iso-butane sulphonic acid, sec-butane sulphonic acid, tert-butane sulphonic acid, and mixtures of two or several of any of them, in all proportions.
- Process according to any one of the preceding Claims, wherein the cleaning formulation comprises at least methane sulphonic acid.
- Process according to any one of the preceding Claims, wherein the cleaning formulation comprises from 0,1 to 100 weight % of alkane sulphonic acid, more generally from 0,5 to 90 weight %, particularly from 0,5 to 20 weight % of alkane sulphonic acid, and more particularly from 0,5 to 5 weight % of alkane sulphonic acid.
- Process according to any one of the preceding Claims, wherein the cleaning formulation further comprises one or more rheological additives, solvents, biocides and other texture agents, selected among solvents and co-solvents, organic or inorganic acids, thickening agents, surface-active agents, foaming agents and anti-foaming agents.
- Process according to any one of the preceding Claims, wherein the acidic cleaning with said formulation comprising at least one alkane sulphonic acid is carried out at a temperature ranging between 0°C and 100°C, more generally between 5°C and 40°C, typically between 5°C and 20°C in the fermentor or the storage vessel, and between 60°C and 80°C in the packaging containers (barrels, bottles or beer cans) used for beer or any type of alcoholic drinks whose manufacturing process involve yeast or any other aerobic fermentation medium likely to release carbon dioxide.
- Process according to any one of the preceding Claims for cleaning an installation used for the preparation and/or the storage of beer, or any type of alcoholic drinks whose manufacturing process involve yeast or any other aerobic fermentation medium likely to release carbon dioxide, comprising the steps of:optional pre-washing of said installation using a diluted alkaline solution;washing of said installation by circulating in said installation a formulation comprising at least methane sulphonic acid; andrinsing said installation by circulating water.
- Use of a formulation comprising at least one alkane sulphonic acid, particularly at least methane sulphonic acid, for eliminating organic and inorganic stains, and other residues present or generated during the preparation and/or the storage of beer or any type of alcoholic drinks whose manufacturing process involve yeast or any other aerobic fermentation medium likely to release carbon dioxide.
- Use of a formulation comprising at least one alkane sulphonic acid, particularly at least methane sulphonic acid, for the elimination of beer stones and yeast rings formed during the preparation and/or the storage of beer.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL08855377T PL2217691T5 (en) | 2007-11-15 | 2008-11-12 | Acid cleaning method in the brewing industry |
| SI200831418T SI2217691T2 (en) | 2007-11-15 | 2008-11-12 | Acid cleaning method in the brewing industry |
| HRP20150392TT HRP20150392T4 (en) | 2007-11-15 | 2008-11-12 | ACID CLEANING PROCEDURE IN THE BEVERAGE INDUSTRY |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0759056A FR2923735A1 (en) | 2007-11-15 | 2007-11-15 | PROCESS FOR ACID CLEANING IN THE BRASSICOLE INDUSTRY |
| FR0759474A FR2923736B1 (en) | 2007-11-15 | 2007-11-30 | PROCESS FOR CLEANING ACID IN THE BRASSICOLE INDUSTRY |
| PCT/FR2008/052032 WO2009068810A2 (en) | 2007-11-15 | 2008-11-12 | Acid cleaning method in the brewing industry |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP2217691A2 EP2217691A2 (en) | 2010-08-18 |
| EP2217691B1 true EP2217691B1 (en) | 2015-01-14 |
| EP2217691B2 EP2217691B2 (en) | 2020-11-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP08855377.1A Active EP2217691B2 (en) | 2007-11-15 | 2008-11-12 | Acid cleaning method in the brewing industry |
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| Country | Link |
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| US (2) | US8425688B2 (en) |
| EP (1) | EP2217691B2 (en) |
| JP (3) | JP2009119445A (en) |
| CN (2) | CN101861380A (en) |
| AP (1) | AP3357A (en) |
| AR (1) | AR069332A1 (en) |
| AU (1) | AU2008328623B9 (en) |
| BR (1) | BRPI0819324A2 (en) |
| CA (1) | CA2704218C (en) |
| DK (1) | DK2217691T4 (en) |
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| ES (1) | ES2528725T5 (en) |
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| IN (1) | IN2010DN03262A (en) |
| MX (1) | MX2010004911A (en) |
| PL (1) | PL2217691T5 (en) |
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| SI (1) | SI2217691T2 (en) |
| TW (1) | TWI395812B (en) |
| WO (1) | WO2009068810A2 (en) |
| ZA (1) | ZA201002950B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2930560B1 (en) * | 2008-04-29 | 2012-08-17 | Arkema France | USE OF ALKANE-SULFONIC ACID FOR DESCALING IN THE AGRI-FOOD INDUSTRY |
| US8211239B1 (en) * | 2008-09-19 | 2012-07-03 | Birko Corporation | Method of cleaning beer kegs and other brewery processing equipment |
| TWI402110B (en) * | 2010-04-26 | 2013-07-21 | Uni President Entpr Corp | Water recovery equipment cleaning method |
| FR2961803B1 (en) * | 2010-06-29 | 2013-02-22 | Arkema France | ACID COMPOSITIONS FOR THE REMOVAL OF OXALATES |
| US9206380B2 (en) | 2013-03-14 | 2015-12-08 | Ecolab Usa Inc. | Method of generating carbonate in situ in a use solution and of buffered alkaline cleaning under an enriched CO2 atmosphere |
| US10119101B2 (en) * | 2014-04-28 | 2018-11-06 | Ecolab Usa Inc. | Method of minimizing enzyme based aerosol mist using a pressure spray system |
| FR3035403B1 (en) * | 2015-04-21 | 2017-05-19 | Arkema France | USE OF ALKANE SULFONIC ACID FOR CLEANING IN SUGAR INDUSTRIES |
| US10208274B1 (en) | 2015-07-02 | 2019-02-19 | Zee Company | Brewing vessel cleaning composition and related methods of use |
| BR102016013836A2 (en) * | 2016-06-15 | 2017-12-26 | Universidade Estadual De Campinas - Unicamp | METHODS OF OPTIMIZATION OF WASH FOR INACTIVATION OF MICRO-ORGANISMS DETERIORATING THE BREWER FERMENTATION PROCESS |
| EP3472330A1 (en) * | 2016-06-20 | 2019-04-24 | Basf Se | Process for producing ethanol from corn comprising dry-milling and adding alkanesulfonic acid to the fermented mash |
| WO2020126855A1 (en) * | 2018-12-21 | 2020-06-25 | Basf Se | Mixture comprising methanesulfonic acid and sulfuric acid |
Family Cites Families (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3036741A (en) * | 1957-06-06 | 1962-05-29 | William T Hilts | System for cleaning liquid dispensing lines |
| US3449164A (en) * | 1966-10-26 | 1969-06-10 | Nikex Nehezipari Kulkere | Chemical composition and method for the removal of beer stone |
| DE3642604A1 (en) † | 1986-12-13 | 1988-06-23 | Henkel Kgaa | USE OF SHORT-CHAIN ALKANESULPHONIC ACIDS IN CLEANING AND DISINFECTANTS |
| DE3914827C2 (en) † | 1989-05-05 | 1995-06-14 | Schuelke & Mayr Gmbh | Liquid disinfectant concentrate |
| ES2097296T3 (en) † | 1991-07-15 | 1997-04-01 | Cfpi Ind | DISINFECTANT ACID COMPOSITION WITH DETERGENT AND DESCALING CHARACTERISTICS AND PROCEDURE FOR ITS MANUFACTURE. |
| US5861366A (en) * | 1994-08-31 | 1999-01-19 | Ecolab Inc. | Proteolytic enzyme cleaner |
| JPH08289687A (en) | 1995-04-25 | 1996-11-05 | Sanyo Electric Co Ltd | Washing of line for handling fluid food/beverage |
| JP4301382B2 (en) | 2000-01-24 | 2009-07-22 | ジョンソンディバーシー株式会社 | Acid detergent for beer brewing equipment |
| DE10036607A1 (en) † | 2000-07-27 | 2002-02-14 | Henkel Ecolab Gmbh & Co Ohg | Acidic preparations for cleaning and disinfecting surfaces |
| DE10127919A1 (en) * | 2001-06-08 | 2002-12-19 | Ecolab Gmbh & Co Ohg | Washing processes, for removing mineral or starch deposits in industrial or domestic dishwashers is effected with both alkaline and acidic stages |
| EP1561801A1 (en) * | 2004-01-28 | 2005-08-10 | JohnsonDiversey Inc. | Sanitizing and cleaning composition and its use for sanitizing and/or cleaning hard surfaces |
| US7494963B2 (en) * | 2004-08-11 | 2009-02-24 | Delaval Holding Ab | Non-chlorinated concentrated all-in-one acid detergent and method for using the same |
| US8114222B2 (en) * | 2004-08-27 | 2012-02-14 | Ecolab Usa Inc. | Method for cleaning industrial equipment with pre-treatment |
| JP4455290B2 (en) | 2004-11-17 | 2010-04-21 | 花王株式会社 | Detergent composition for food manufacturing and processing equipment |
| US8450257B2 (en) | 2005-12-12 | 2013-05-28 | Vitech International, Inc. | Multipurpose, non-corrosive cleaning compositions and methods of use |
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