EP0165573B1 - Process for sterilizing packaging materials for the aseptic filling thereof with fruit juice and wine - Google Patents

Process for sterilizing packaging materials for the aseptic filling thereof with fruit juice and wine Download PDF

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Publication number
EP0165573B1
EP0165573B1 EP85107396A EP85107396A EP0165573B1 EP 0165573 B1 EP0165573 B1 EP 0165573B1 EP 85107396 A EP85107396 A EP 85107396A EP 85107396 A EP85107396 A EP 85107396A EP 0165573 B1 EP0165573 B1 EP 0165573B1
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Prior art keywords
acid
alcohol
wine
concentration
ppm
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EP85107396A
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German (de)
French (fr)
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EP0165573A2 (en
EP0165573A3 (en
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Erwin W. Dr. Wartenberg
Hong-An Dr. Duong
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Tetra Laval Holdings and Finance SA
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Tetra Laval Holdings and Finance SA
Tetra Pak Finance and Trading SA
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65BMACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
    • B65B55/00Preserving, protecting or purifying packages or package contents in association with packaging
    • B65B55/02Sterilising, e.g. of complete packages
    • B65B55/04Sterilising wrappers or receptacles prior to, or during, packaging
    • B65B55/10Sterilising wrappers or receptacles prior to, or during, packaging by liquids or gases

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  • the invention relates to a method for the sterilization of packaging materials for the aseptic filling of fruit juice and wine using sulfurous acid.
  • the invention has for its object to provide a method for the sterilization of packaging materials for the aseptic filling of fruit juice and wine using sulfurous acid, which causes a satisfactory germ killing in a short time.
  • the object is achieved in that the packaging material is treated with aqueous solutions of sulfurous acid and alcohols.
  • Figures 1 to 16 show the killing effect (reduction in the number of bacteria as a function of time) of sulphurous acid and alcohol in each case alone and of mixtures of sulphurous acid and alcohols when used against various yeasts, fungi and bacteria:
  • Aqueous mixtures (solutions) of sodium disulfite (Na 2 S 2 0 5 ) and ethanol were used as test substances, ethanol being present in a concentration between 96 and 100%. Since sulphurous acid develops its strongest germicidal effect in a strongly acidic range, the sodium disulfite used was acidified to a pH of 3.0 with citric acid after being dissolved in water.
  • the acidified, alcohol-containing Na 2 S 2 0 5 mixed solution contains not only alcohol but also sulphurous acid in various dissociation stages, the sulphurous acid being the effective antiseptic.
  • Fig. 1 shows the killing time curves of Saccharomyces cerevisiae at 22 ° C and at different H 2 S0 3 concentrations (weight as Na 2 S 2 0 5 ). Killing is quickest at a concentration of 40,000 ppm. Here a D value of D22 - 2 seconds is reached. (The D value indicates the time after which a certain number of bacteria has dropped by a power of ten at a certain temperature.)
  • the Mucor mold is even more resistant to H 2 S0 3 than Aspergillus niger, and the Mucor killing time curves at different H 2 S0 3 concentrations and at different temperatures are shown in FIGS.
  • a D value in the range of a few seconds becomes at 30,000 ppm (22 ° C) or at 10,000 ppm (60 ° C) reached.
  • Acetic acid bacteria have a fairly high resistance to sulfurous acid. As can be seen from FIGS. 10 and 11, the acetic acid bacterium Gluconobacter can only be killed slowly. Both a high concentration of H 2 S0 3 and an increase in temperature cannot significantly improve the germicidal effect. A technically usable rapid germ killing with corresponding D values in the range of a few seconds, preferably less than 3 seconds, is not achieved even at the high concentration of 100,000 ppm at room temperature. The D22 value here is still 15 seconds.
  • Acetobacter aceti shows high resistance to sulfurous acid. However, rapid killing with a Dso value of 1.7 seconds can also be achieved with this acetic acid bacterium due to the synergistic effect of the mixed solution sulfuric acid / alcohol (20,000 ppm / 15% by weight) (FIG. 14).
  • the dependence of the killing time of the lactic acid bacterium Leuconostoc dextranicum on the temperature is shown in FIG. 15.
  • the greatest kill is achieved at 60 ° C with a concentration of 10,000 ppm.
  • the Dso value here is 1.45 seconds.
  • the synergistic effect of the H 2 S0 3 alcohol mixture is also clearly expressed when other alcohols are used instead of ethanol.
  • the addition of 1-propanol (Fig. 17), 2-propanol (Fig. 18), 1-butanol (Fig. 11), 2-butanol (Fig. 20) and n-amyl alcohol (Fig. 21) to sulfurous acid contributes significantly to the strengthening of the microbicidal activity against yeasts (Saccharomyces cerevisae).
  • the alcohol 1-propanol, in combination with sulfurous acid also accelerates the killing of molds - Mucor - (Fig. 22), acetic acid bacteria - Gluconobacter (Fig. 23) and lactic acid bacteria - L. dextranicum - (Fig. 24).
  • test results described and shown clearly show a synergistic effect of sulfurous acid and alcohol in killing the germs examined.
  • the combination of sulphurous acid with alcohol enables a quick destruction of the existing germs with D-values between 1 and 2 seconds by appropriate choice of the H 2 S0 3 concentration, the alcohol content and the temperature, so that the proposed mixed solution advantageously also on an industrial scale , in particular in the sterilization of plastic-coated packaging materials for fruit juice and wine filling or in the sterilization of wine bottles.
  • Ethanol is preferably used as the alcohol, although other alcohols can also be used.
  • the sulfurous acid is preferably present in a concentration of 10,000 to 100,000, in particular 10,000 to 50,000 ppm, based on the mixture. Particularly advantageous alcohol concentrations are in the range from 10 to 30, in particular 10 to 20,% by weight, based on the mixture. Temperatures between 20 and 80, preferably 20 and 50 ° C. are suitable by the treatment according to the invention.
  • Sulfuric acid is best obtained by reacting salt-like sulfur compounds with acid.
  • Na 2 S0 5 Na 2 S0 3 is also suitable alone or in conjunction with the aforementioned substance.
  • Citric acid is preferably used as the acid for adjusting the pH.
  • the packaging material can be treated by immersion, spraying or the like with the synergistic mixed solution according to the invention. It is also possible to use that salt-like sulfur compound, e.g. B. Na 2 S 2 0 5 , which provides the sulfurous acid, to be applied separately to the packaging material and then to dissolve it by adding an acidified, aqueous alcohol solution.
  • salt-like sulfur compound e.g. B. Na 2 S 2 0 5
  • the results are summarized in the tables below.
  • the invention is of particular advantage in the case of wine packaging, since wine naturally contains sulfurous acid and alcohol. No "foreign substances" need to be used to sterilize the packaging materials, which could impair the quality of the wine.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Basic Packing Technique (AREA)

Description

Die Erfindung betrifft ein Verfahren zur Sterilisierung von Packstoffen für die aseptische Abfüllung von Fruchtsaft und Wein unter Verwendung schwefliger Säure.The invention relates to a method for the sterilization of packaging materials for the aseptic filling of fruit juice and wine using sulfurous acid.

Da Bakteriensporen in Fruchtsäften und Weinen aufgrund ungeeigneter Wachstumsbedingungen nicht zur Entwicklung kommen, ist für die aseptische Abfüllung von Wein ein Einsatz des bei anderen Getränken, z. B. Milch, üblichen Wasserstoffperoxids zur Sterilisation des Verpackungsmaterials - Flaschen, Beutel und Gefäße aus Kunststoff oder kunststoffbeschichtetem Papier - nicht erforderlich. Als Ersatz käme an sich schweflige Säure infrage, die auch bisher schon, z. B. bei der Weinvergärung und Weinabfüllung, gegen Pilzwachstum verwendet wurde. Jedoch ist die Abtötungswirkung schwefliger Säure gegen Bakterien zu gering, um eine Keimfreiheit in produktionstechnisch erwünschten, kurzen Zeiten von einigen Sekunden zu erreichen.Since bacterial spores do not develop in fruit juices and wines due to unsuitable growth conditions, the aseptic filling of wine requires the use of other beverages, e.g. As milk, conventional hydrogen peroxide for the sterilization of the packaging material - bottles, bags and containers made of plastic or plastic-coated paper - not required. As a substitute, sulfuric acid would come into question. B. was used in fermentation and bottling, against fungal growth. However, the killing effect of sulphurous acid against bacteria is too low to achieve sterility in short times of a few seconds that are technically desirable.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren zur Sterilisierung von Packstoffen für die aseptische Abfüllung von Fruchtsaft und Wein unter Verwendung schwefliger Säure anzugeben, welche in kurzer Zeit eine befriedigende Keimabtötung bewirkt.The invention has for its object to provide a method for the sterilization of packaging materials for the aseptic filling of fruit juice and wine using sulfurous acid, which causes a satisfactory germ killing in a short time.

Die Aufgabe wird erfindungsgemäß dadurch gelöst, daß man den Packstoff mit wässrigen Lösungen aus schwefliger Säure und Alkoholen behandelt.The object is achieved in that the packaging material is treated with aqueous solutions of sulfurous acid and alcohols.

Es wurde in überraschender Weise gefunden, daß eine solche Mischung synergistisch wirkt und für die in Rede stehende Getränkeverpackung und -abfüllung eine mikrobizide Wirkung hat, die diejenige von schwefliger Säure ohne Alkoholzusatz erheblich übertrifft.It has surprisingly been found that such a mixture has a synergistic effect and has a microbicidal action for the beverage packaging and bottling in question which considerably exceeds that of sulfurous acid without the addition of alcohol.

Die nachstehende Beschreibung dient im Zusammenhang mit zwei Tabellen und mehreren Figuren der weiteren Erläuterung der Erfindung.The following description is used in conjunction with two tables and several figures to further explain the invention.

Die Figuren 1 bis 16 zeigen die Abtötungswirkung (Reduzierung der Keimzahl in Abhängigkeit von der Zeit) von schwefliger Säure und Alkohol jeweils allein sowie von Mischungen aus schwefliger Säure und Alkoholen im Einsatz gegen verschiedene Hefen, Pilze und Bakterien:Figures 1 to 16 show the killing effect (reduction in the number of bacteria as a function of time) of sulphurous acid and alcohol in each case alone and of mixtures of sulphurous acid and alcohols when used against various yeasts, fungi and bacteria:

Im Verlaufe der im Zusammenhang mit der Erfindung unternommenen Untersuchung der mikrobiziden Wirkung von schwefliger Säure allein und von schwefliger Säure in Verbindung mit Alkohol wurden folgende Mikroorganismen eingesetzt:

  • Hefen (Saccharomyces cerevisiae)
  • Schrimmelpilze (Aspergillus niger und Mucor)
  • Essigbakterien (Acetobacter aceti und Gluconobacter)
  • Milchsäurebakterien (Leuconostoc dextranicum).
The following microorganisms were used in the course of the study undertaken in connection with the invention of the microbicidal action of sulphurous acid alone and of sulphurous acid in conjunction with alcohol:
  • Yeast (Saccharomyces cerevisiae)
  • Molds (Aspergillus niger and Mucor)
  • Vinegar bacteria (Acetobacter aceti and Gluconobacter)
  • Lactic acid bacteria (Leuconostoc dextranicum).

Als Testsubstanzen dienten wässrige Mischungen (Lösungen) von Natriumdisulfit (Na2S205) und Ethanol, wobei Ethanol in einer Konzentration zwischen 96 und 100 % vorlag. Da schweflige Säure in stark saurem Bereich ihre stärkste keimtötende Wirkung entfaltet, wurde das verwendete Natriumdisulfit nach Lösung in Wasser mit Zitronensäure auf einen pH-Wert von 3,0 angesäuert. Die so angesäuerte, alkoholhaltige Na2S205-Mischlösung enthält neben Alkohol schweflige Säure in verschiedenen Dissoziationsstufen, wobei die schweflige Säure das wirksame antiseptische Mittel ist.Aqueous mixtures (solutions) of sodium disulfite (Na 2 S 2 0 5 ) and ethanol were used as test substances, ethanol being present in a concentration between 96 and 100%. Since sulphurous acid develops its strongest germicidal effect in a strongly acidic range, the sodium disulfite used was acidified to a pH of 3.0 with citric acid after being dissolved in water. The acidified, alcohol-containing Na 2 S 2 0 5 mixed solution contains not only alcohol but also sulphurous acid in various dissociation stages, the sulphurous acid being the effective antiseptic.

Die keimabtötende Wirkung wurde in Abhängigkeit von der Konzentration bei verschiedenen Temperaturen untersucht:The germicidal effect was investigated depending on the concentration at different temperatures:

Fig. 1 zeigt die Abtötungszeitkurven von Saccharomyces cerevisiae bei 22°C und bei verschiedenen H2S03-Konzentrationen (Einwaage als Na2S205). Die Abtötung ist bei einer Konzentration von 40.000 ppm am schnellsten. Hier wird ein D-Wert von D22 - 2 Sekunden erreicht. (Der D-Wert gibt diejenige Zeit an, nach welcher bei einer bestimmten Temperatur eine bestimmte Keimzahl um eine Zehnerpotenz abgesunken ist.)Fig. 1 shows the killing time curves of Saccharomyces cerevisiae at 22 ° C and at different H 2 S0 3 concentrations (weight as Na 2 S 2 0 5 ). Killing is quickest at a concentration of 40,000 ppm. Here a D value of D22 - 2 seconds is reached. (The D value indicates the time after which a certain number of bacteria has dropped by a power of ten at a certain temperature.)

Die Abhängigkeit der Abtötung der Hefe S. cerevisiae von der Temperatur ist in Fig. 2 dargestellt. Bei einer einheitlichen Konzentration an Na2S205 von 10.000 ppm ergibt sich die stärkste Abtötung bei 50°C. Die dezimale Reduktionszeit beträgt hier ebenfalls ca. 2 Sekunden (D50 = 2 Sekunden).The dependence of the killing of the yeast S. cerevisiae on the temperature is shown in FIG. 2. With a uniform concentration of Na 2 S 2 0 5 of 10,000 ppm, the greatest kill results at 50 ° C. The decimal reduction time here is also approx. 2 seconds (D 50 = 2 seconds).

Die keimabtötende Wirkung der schwefligen Säure wird durch Zugabe von Alkohol (Ethanol) sprunghaft verstärkt, wie die Fig. 3 zeigt. Mit schwefliger Säure allein (10.000 ppm, 22°C) ergibt sich bei der Abtötung von S. cerevisiae ein D-Wert von D22 = 37 Sekunden. Durch Zugabe von Ethanol (15 Gew.-%) lässt sich die Abtötung erheblich beschleunigen. Der D22-Wert beträgt jetzt nur noch etwa 2 Sekunden. Wie ebenfalls aus Fig. 3 hervorgeht - vgl. die obere Kurve - zeigt Ethanol allein praktisch keine keimtötende Wirkung. Somit lässt sich der synergistische Effekt der verwendeten Mischung aus schwefliger Säure und Alkohol aus Fig. 3 deutlich ablesen.The germicidal effect of the sulfurous acid is suddenly increased by adding alcohol (ethanol), as shown in FIG. 3. With sulphurous acid alone (10,000 ppm, 22 ° C) the death of S. cerevisiae results in a D value of D 22 = 37 seconds. The addition of ethanol (15% by weight) can accelerate the killing considerably. The D22 value is now only about 2 seconds. As is also apparent from Fig. 3 - cf. the upper curve - ethanol alone shows practically no germicidal effect. The synergistic effect of the mixture of sulphurous acid and alcohol used in FIG. 3 can thus be clearly read off.

Im Vergleich mit Fig. 1 und 2 ergibt sich, daß bei Ausnutzung der gefundenen synergistischen Wirkung eine Erhöhung der Konzentration de schwefligen Säure auf 40.000 ppm (Fig. 1) bzw. der Temperatur auf 50° C (Fig. 2) nicht mehr notwendig ist.In comparison with FIGS. 1 and 2, it is found that if the synergistic effect found is used, it is no longer necessary to increase the concentration of the sulphurous acid to 40,000 ppm (FIG. 1) or the temperature to 50 ° C. (FIG. 2) .

Im Vergleich mit Hefen lassen sich die Konidien des Schimmelpilzes Aspergillus niger von schwefliger Säure leichter abtöten. Die H2S03-Konzentration und die Temperatur üben auf die Abtötung nur einen geringen Einfluß aus (Fig. 4). Bereits bei einer Konzentration von 10.000 ppm ergibt sich bei Zimmertemperatur ein D-Wert von D22 = 2,45 Sek.Compared to yeasts, the conidia of the Aspergillus niger mold from sulfurous acid are easier to kill. The H 2 S0 3 concentration and the temperature exert only a slight influence on the killing (FIG. 4). Even at a concentration of 10,000 ppm, a D value of D 22 = 2.45 seconds results at room temperature.

Die synergistische Wirkung, die sich durch Kombination von H2S03 mit Alkohol (Ethanol) ergibt, ist mit D22 = 1,8 Sek. nur schwach ausgeprägt (Fig. 5).The synergistic effect resulting from the combination of H 2 S0 3 with alcohol (ethanol) is only weakly pronounced with D 22 = 1.8 seconds (FIG. 5).

Der Schimmelpilz Mucor ist gegen H2S03 noch resistenter als Aspergillus niger. Die Abtötungszeitkurven von Mucor bei unterschiedlichen H2S03-Konzentrationen und bei verschiedenen Temperaturen sind in Fig. 6 bzw. 7 dargestellt. Ein D-Wert im Bereich von einigen Sekunden wird bei 30.000 ppm (22°C) bzw. bei 10.000 ppm (60° C) erreicht.The Mucor mold is even more resistant to H 2 S0 3 than Aspergillus niger, and the Mucor killing time curves at different H 2 S0 3 concentrations and at different temperatures are shown in FIGS. A D value in the range of a few seconds becomes at 30,000 ppm (22 ° C) or at 10,000 ppm (60 ° C) reached.

Die synergistische Wirkung des H2S03-Alkohol-Gemisches kommt auch bei Mucor deutlich zum Ausdruck (Fig. 8 und 9). Sowohl bei Zimmertemperatur (22°C) als auch bei 50° C läßt sich mit dem Alkoholzusatz eine Verbesserung der Abtötungswirkung von schwefliger Säure erzielen.The synergistic effect of the H 2 S0 3 alcohol mixture is also clearly expressed in Mucor (Fig. 8 and 9). Both at room temperature (22 ° C) and at 50 ° C, the alcohol additive can improve the killing effect of sulfuric acid.

Essigsäurebakterien weisen eine ziemlich hohe Resistenz gegen schweflige Säure auf. Wie aus Fig. 10 und 11 ersichtlich ist, läßt sich das Essigsäurebakterium Gluconobacter nur langsam abtöten. Sowohl eine hohe Konzentration von H2S03 als auch eine Temperaturerhöhung vermögen die keimabtötende Wirkung nicht wesentlich zu verbessern. Eine technisch verwertbare rasche Keimabtötung mit entsprechenden D-Werten im Bereich weniger Sekunden, vorzugsweise unter 3 Sekunden, wird sogar bei der hohen Konzentration von 100.000 ppm bei Zimmertemperatur nicht erreicht. Der D22-Wert beträgt hier immer noch 15 Sek.Acetic acid bacteria have a fairly high resistance to sulfurous acid. As can be seen from FIGS. 10 and 11, the acetic acid bacterium Gluconobacter can only be killed slowly. Both a high concentration of H 2 S0 3 and an increase in temperature cannot significantly improve the germicidal effect. A technically usable rapid germ killing with corresponding D values in the range of a few seconds, preferably less than 3 seconds, is not achieved even at the high concentration of 100,000 ppm at room temperature. The D22 value here is still 15 seconds.

Die Zugabe von Ethanol zu schwefliger Säure erweist sich bei Gluconobacter als ein entscheidender Faktor zur Verstärkung der mikrobiziden Wirkung. Eine Kombination von 30.000 ppm Na2S205 und Alkohol (30 Gew.-% Ethanol) wirkt bei Zimmertemperatur synergistisch und ermöglicht dadurch eine schnelle Abtötung mit D22 = ca. 1,6 Sek. (Fig. 12).The addition of ethanol to sulphurous acid proves to be a decisive factor in enhancing the microbicidal effect with Gluconobacter. A combination of 30,000 ppm Na 2 S 2 0 5 and alcohol (30% by weight ethanol) has a synergistic effect at room temperature and thereby enables rapid kill with D 22 = approx. 1.6 seconds (FIG. 12).

Wird de Abtötungstemperatur auf 50° C erhöht, so lässt sich ein vergleichbarer D-Wert (D50 = 1,5 Sek.) auch bei niederer Konzentration an schwefliger Säure (20.000 ppm) und geringerem Alkoholgehalt (15 Gew.-%) erreichen (Fig. 13).If the killing temperature is increased to 50 ° C, a comparable D value (D 50 = 1.5 seconds) can be achieved even with a low concentration of sulfurous acid (20,000 ppm) and a lower alcohol content (15% by weight) ( Fig. 13).

Ebenso wie Gluconobacter zeigt auch Acetobacter aceti hohe Resistenz gegen schweflige Säure. Eine schnelle Abtötung mit einem Dso-Wert von 1,7 Sek. ist jedoch auch hier bei diesem Essigsäurebakterium aufgrund der synergistischen Wirkung der Mischlösung schweflige Säure/Alkohol (20.000 ppm/15 Gew.-%) erreichbar (Fig. 14).Just like Gluconobacter, Acetobacter aceti shows high resistance to sulfurous acid. However, rapid killing with a Dso value of 1.7 seconds can also be achieved with this acetic acid bacterium due to the synergistic effect of the mixed solution sulfuric acid / alcohol (20,000 ppm / 15% by weight) (FIG. 14).

Die Abhängigkeit der Abtötungszeit des Milchsäurebakteriums Leuconostoc dextranicum von der Temperatur ist in Fig. 15 dargestellt. Die stärkste Abtötung erreicht man bei 60°C mit einer Konzentration von 10.000 ppm. Der Dso-Wert beträgt hier 1,45 Sek.The dependence of the killing time of the lactic acid bacterium Leuconostoc dextranicum on the temperature is shown in FIG. 15. The greatest kill is achieved at 60 ° C with a concentration of 10,000 ppm. The Dso value here is 1.45 seconds.

Auch bei L. dextranicum ist eine synergistische Wirkung des erfindungsgemäß eingesetzten Gemisches schweflige Säure/Alkohol deutlich feststellbar. Aus Fig. 16 geht hervor, daß die keimabtötende Wirkung der schwefligen Säure (20.000 ppm Na2S205 bei pH 3,0) durch Zugabe von Ethanol (15 Gew.-%) erheblich verstärkt wird. Es läßt sich ein D-Wert von D22 = 1,5 Sek. erreichen.With L. dextranicum, too, a synergistic effect of the sulfurous acid / alcohol mixture used according to the invention can be clearly determined. 16 shows that the germicidal effect of the sulfurous acid (20,000 ppm Na 2 S 2 0 5 at pH 3.0) is considerably increased by adding ethanol (15% by weight). A D value of D 22 = 1.5 seconds can be achieved.

Die synergistische Wirkung des H2S03-Alkohol-Gemisches kommt auch deutlich zum Ausdruck, wenn statt Ethanol andere Alkohole eingesetzt werden. Die Zugabe von 1-Propanol (Fig. 17), 2-Propanol (Fig. 18), 1-Butanol (Fig. 11), 2-Butanol (Fig. 20) und n-Amylalkohol (Fig. 21) zu schwefliger Säure trägt deutlich zur Verstärkung der mikrobiziden Wirkung gegen Hefen (Saccharomyces cerevisae) bei. Der Alkohol 1-Propanol beschleunigt ebenfalls in Kombination mit schwefliger Säure die Abtötung von Schimmelpilzen - Mucor - (Fig. 22), Essigsäurebakterien - Gluconobacter (Fig. 23) und Milchsäurebakterien - L. dextranicum - (Fig. 24).The synergistic effect of the H 2 S0 3 alcohol mixture is also clearly expressed when other alcohols are used instead of ethanol. The addition of 1-propanol (Fig. 17), 2-propanol (Fig. 18), 1-butanol (Fig. 11), 2-butanol (Fig. 20) and n-amyl alcohol (Fig. 21) to sulfurous acid contributes significantly to the strengthening of the microbicidal activity against yeasts (Saccharomyces cerevisae). The alcohol 1-propanol, in combination with sulfurous acid, also accelerates the killing of molds - Mucor - (Fig. 22), acetic acid bacteria - Gluconobacter (Fig. 23) and lactic acid bacteria - L. dextranicum - (Fig. 24).

Zusammenfassend ist festzustellen, daß sich anhand der beschriebenen und dargestellten Versuchsergebnisse eine synergistische Wirkung von schwefliger Säure und Alkohol bei der Abtötung der untersuchten Keime deutlich erkennen läßt. Die Kombination von schwefliger Säure mit Alkohol ermöglicht durch entsprechende Wahl der H2S03-Konzentration, des Alkoholgehaltes und der Temperatur eine schnelle Abtötung der vorhandenen Keime mit D-Werten zwischen 1 und 2 Sekunden, so daß die vorgeschlagene Mischlösung in vorteilhafter Weise auch großtechnisch, insbesondere bei der Sterilisierung von Kunststoffbeschichteten Packstoffen zur Fruchtsaft- und Weinabfüllung oder bei der Sterilisierung von Weinflaschen eingesetzt werden kann.In summary, it can be stated that the test results described and shown clearly show a synergistic effect of sulfurous acid and alcohol in killing the germs examined. The combination of sulphurous acid with alcohol enables a quick destruction of the existing germs with D-values between 1 and 2 seconds by appropriate choice of the H 2 S0 3 concentration, the alcohol content and the temperature, so that the proposed mixed solution advantageously also on an industrial scale , in particular in the sterilization of plastic-coated packaging materials for fruit juice and wine filling or in the sterilization of wine bottles.

Als Alkohol wird bevorzugt Ethanol verwendet, obwohl auch andere Alkohole eingesetzt werden können. Die schweflige Säure liegt vorzugsweise in einer Konzentration von 10.000 bis 100.000, insbesondere 10.000 bis 50.000 ppm bezogen auf die Mischung vor. Besonders vorteilhafte Alkoholkonzentrationen liegen im Bereich von 10 bis 30, insbesondere 10 bis 20 Gew.-% bezogen auf die Mischung. Durch erfindungsgemäße Behandlung sind Temperaturen zwischen 20 und 80, vorzugsweise 20 und 50°C geeignet. Die schweflige Säure gewinnt man am besten durch Umsetzung salzartiger Schwefelverbindungen mit Säure. Außer Na2S205 eignet sich allein oder in Verbindung mit der vorgenannten Substanz auch Na2S03. Als Säure zur Einstellung des pH-Werts verwendet man bevorzugt Zitronensäure.Ethanol is preferably used as the alcohol, although other alcohols can also be used. The sulfurous acid is preferably present in a concentration of 10,000 to 100,000, in particular 10,000 to 50,000 ppm, based on the mixture. Particularly advantageous alcohol concentrations are in the range from 10 to 30, in particular 10 to 20,% by weight, based on the mixture. Temperatures between 20 and 80, preferably 20 and 50 ° C. are suitable by the treatment according to the invention. Sulfuric acid is best obtained by reacting salt-like sulfur compounds with acid. In addition to Na 2 S 2 0 5 , Na 2 S0 3 is also suitable alone or in conjunction with the aforementioned substance. Citric acid is preferably used as the acid for adjusting the pH.

Der Packstoff kann durch Tauchen, Besprühen oder dergleichen mit der erfindungsgemäßen, synergistisch wirkenden Mischlösung behandelt werden. Dabei ist es auch möglich, diejenige salzartige Schwefelverbindung, z. B. Na2S205, welche die schweflige Säure liefert, separat auf den Packstoff aufzubringen und ihn anschließend durch Zugabe einer angesäuerten, wässrigen Alkohollösung aufzulösen. Die Ergebnisse sind in den nachstehenden Tabellen zusammengefaßt.The packaging material can be treated by immersion, spraying or the like with the synergistic mixed solution according to the invention. It is also possible to use that salt-like sulfur compound, e.g. B. Na 2 S 2 0 5 , which provides the sulfurous acid, to be applied separately to the packaging material and then to dissolve it by adding an acidified, aqueous alcohol solution. The results are summarized in the tables below.

Besonders günstig ist es, die sterilisierende Mischlösung auf den Packstoff aufzusprühen und nach Ablauf der Einwirkzeit durch Erwärmen wieder zu verdampfen.It is particularly advantageous to spray the sterilizing mixed solution onto the packaging material and to evaporate it again by heating after the exposure time has expired.

Von besonderen Vorteil ist die Erfindung bei Weinverpackungen, da Wein von Haus aus häufig schweflige Säure und Alkohol enthält. Zur Sterilisierung der Packstoffe brauchen also keine "Fremdstoffe" eingesetzt zu werden, welche die Qualität des Weines beeinträchtigen könnten.The invention is of particular advantage in the case of wine packaging, since wine naturally contains sulfurous acid and alcohol. No "foreign substances" need to be used to sterilize the packaging materials, which could impair the quality of the wine.

Abtötung von Weinschädlingen mit Schwefliger Säure in Kombination mit EthanolKilling wine pests with sulfurous acid in combination with ethanol

Figure imgb0001
Figure imgb0001

Abtötung von Weinschädlichen mit schwefliger Säure in Kombination mit Alkoholen (Propanol, Butanol,Killing wine-damaging substances with sulfurous acid in combination with alcohols (propanol, butanol, Amylalkohol) bei 22° CAmyl alcohol) at 22 ° C

Figure imgb0002
Figure imgb0002

Claims (11)

1. Method of sterilising packaging materials for the aseptic filling of fruit juice and wine, using sulphurous acid, characterised in that the packaging material is treated with aqueous solutions of sulphurous acid and
Figure imgb0003
alcohols.
2. Method according to Claim 1, characterised in that ethanol is used as the alcohol.
3. Method according to Claim 1, characterised in that butanol, propopanol and amylalcohol are used as the alcohol.
4. Method according to Claim 1 or 2, characterised in that the sulphurous acid is used in a concentration of 10,000 to 100,000 ppm in relation to the mixture.
5. Method according to Claim 4, characterised in that the sulphurous acid is used in a concentration of 10,000 to 50,000 ppm.
6. Method according to one of Claims 1 to 5, characterised in that an alcohol concentration is used amounting to 10 to 30 % by weight in relation to the mixture.
7. Method according to Claim 6, characterised in that an alcohol concentration is used amounting to 10 to 20 % by weight.
8. Method according to one of the preceding Claims, characterised in that the treatment is carried out at a temperature of between 20 and 80°C.
9. Method according to Claim 8, characterised in that the treatment is carried out at a temperature of between 20 and 50°C.
10. Method according to one of the preceding Claims, characterised in that the sulphurous acid is obtained by the reaction of salt-like sulphur compounds with acid.
11. Method according to Claim 10, characterised in that citric acid is used as the acid while Na2S205 and/or Na2S03 are used as the sulphur compound.
EP85107396A 1984-06-19 1985-06-14 Process for sterilizing packaging materials for the aseptic filling thereof with fruit juice and wine Expired EP0165573B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT85107396T ATE38809T1 (en) 1984-06-19 1985-06-14 PROCESS FOR STERILIZING PACKAGING MATERIALS FOR ASEPTIC FILLING OF FRUIT JUICE AND WINE.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19843422683 DE3422683A1 (en) 1984-06-19 1984-06-19 METHOD FOR STERILIZING PACKAGING MATERIALS FOR ASEPTICALLY FILLING FRUIT JUICE AND WINE
DE3422683 1984-06-19

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EP0165573A2 EP0165573A2 (en) 1985-12-27
EP0165573A3 EP0165573A3 (en) 1986-12-30
EP0165573B1 true EP0165573B1 (en) 1988-11-23

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EP (1) EP0165573B1 (en)
JP (1) JPS6181773A (en)
AR (1) AR240783A1 (en)
AT (1) ATE38809T1 (en)
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CA (1) CA1239768A (en)
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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8625607D0 (en) * 1986-10-25 1986-11-26 Laporte Industries Ltd Composition for treatment of bathtubs
FR2716081A1 (en) * 1994-02-11 1995-08-18 Cogia Sterilisation of fruit juice
IT1403634B1 (en) * 2011-01-17 2013-10-31 Spitaleri METHOD OF PRODUCTION OF A GRAPE-BASED ANALCOLIC DRINK AND PRODUCT OBTAINED BY THIS METHOD.
DE102013011193B3 (en) * 2013-07-04 2013-12-05 Walter Mick Method for cleaning and/or disinfection of e.g. bottles and closures before packing alcoholic extract, involves removing portion of filling material as cleaning agent, filling bottles with remaining portion and sealing bottles with closures

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB189519702A (en) * 1895-10-19 1896-02-15 Franz Hartmann An Improved Process for Manufacturing a Solution Containing Sulphurous Acid for Curative Purposes.
DE2454873C3 (en) * 1974-11-20 1979-05-10 Willibald 6363 Echzell Seibold Disinfecting cutting tools for cutting bread and baked goods
SE401913B (en) * 1976-10-07 1978-06-05 Tetra Pak Int DEVICE FOR STERILIZING A PACKAGING MATERIAL PATH
DE2807617C2 (en) * 1978-02-22 1986-10-09 Heess, Karl David Heinrich, 6840 Lampertheim Process for sterilizing beverage bottles
DE3036972C2 (en) * 1980-10-01 1986-04-03 PKL Verpackungssysteme GmbH, 4000 Düsseldorf Method for sterilizing packaging material
NZ203201A (en) * 1982-02-12 1985-01-31 Smith & Nephew Ass Sulphur dioxide-releasing composition containing hydroquinone
DE3240688A1 (en) * 1982-11-04 1984-05-30 Henkel KGaA, 4000 Düsseldorf USE OF ALKYLMONOPHOSPHONIC ACIDS AS A KILLING SUBSTANCE

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CA1239768A (en) 1988-08-02
ES8608892A1 (en) 1986-07-16
AR240783A2 (en) 1991-02-28
JPH0548111B2 (en) 1993-07-20
AU575955B2 (en) 1988-08-11
EP0165573A2 (en) 1985-12-27
JPS6181773A (en) 1986-04-25
DE3422683A1 (en) 1985-12-19
AU4370085A (en) 1986-01-02
ATE38809T1 (en) 1988-12-15
EP0165573A3 (en) 1986-12-30
AR240783A1 (en) 1991-02-28
DE3422683C2 (en) 1991-03-14
ES544310A0 (en) 1986-07-16

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