EP1551463B1 - Cork product treatment process by extraction of compounds dragged in water vapour - Google Patents

Cork product treatment process by extraction of compounds dragged in water vapour Download PDF

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Publication number
EP1551463B1
EP1551463B1 EP03784710A EP03784710A EP1551463B1 EP 1551463 B1 EP1551463 B1 EP 1551463B1 EP 03784710 A EP03784710 A EP 03784710A EP 03784710 A EP03784710 A EP 03784710A EP 1551463 B1 EP1551463 B1 EP 1551463B1
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EP
European Patent Office
Prior art keywords
cork
water vapour
stoppers
tca
treatment
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP03784710A
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German (de)
English (en)
French (fr)
Other versions
EP1551463A1 (en
Inventor
Miguel Cabral
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AMORIM AND IRMAOS SA
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AMORIM AND IRMAOS SA
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Publication of EP1551463A1 publication Critical patent/EP1551463A1/en
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Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K7/00—Chemical or physical treatment of cork
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K2240/00—Purpose of the treatment
    • B27K2240/10—Extraction of components naturally occurring in wood, cork, straw, cane or reed

Definitions

  • the present invention refers to a cork product treatment processes by extraction of compounds dragged in water vapour.
  • ROSA system The process of the invention; hereinafter referred to as ROSA system, is based on the application of water vapour to cork granules, disks, and stoppers in order to achieve its deodorization, namely eliminating all the compounds dragged in water vapour, among which the 2,4,6-trichloroanizole.
  • cork Being a highly absorptive material, cork has an enormous ability to absorb compounds present in the cork environment, particularly those that present an unpleasant flavour and/or smell. These compounds can be transferred to the products contacting the cork, which, due to said contact, will often be damaged beyond repair.
  • Cork finds one of its most significant uses as a sealing element, namely as natural cork stoppers, composite stoppers, technical stoppers, Champagne stoppers, and stoppers with a capsule element. These products are used to seal wine products, which often have an aroma delicacy that is not compatible with any unpleasant flavour transmission from the packaging materials, namely from the sealing element.
  • the ROSA system is intended to greatly reduce compounds having unpleasant aromas, and particularly the TCA, in cork products, namely in cork granules, disks, and stoppers, so that the cork products will be no longer considered the cause of the wine product contamination by the above-mentioned compounds. Only this way the alternative sealing elements will no longer have a reason to exist and the cork products will regain the rightful market place that has been theirs for centuries.
  • the strategies developed in order to solve the problem of TCA in cork products involve preventive and treatment aspects.
  • the first of these aspects aims to avoid conditions appropriated to the TCA formation or to its migration to the wine products
  • the second aspect deals with the treatment of cork products in order to remove the already existing TCA. Washing of cork products with hydrogen peroxide solution, the final treatment of these products with ozone or microwaves, the use of physical barriers, namely silicone ones, in order to prevent TCA from contacting with wine products, supercritical TCA extraction, with fluid carbon dioxide, from cork products, enzyme treatment, and cork granule treatment with water vapour are existing processes having as object the TCA removal in industrial plants.
  • Cork washing with hydrogen peroxide is a routine bleaching process used in the cork industry.
  • the washing process is carried out at an industrial scale using a drum for natural, technical, and composite stoppers.
  • Hydrogen peroxide with its oxidative properties is known to act as disinfectant, therefore contributing to diminish the microbial load in cork stoppers.
  • Microorganisms, and particularly fungi are able to produce TCA due to their metabolism in the presence of primers.
  • the peroxide washing acts as a preventive process in cork stopper contamination with TCA.
  • Unfortunately is not an effective process insofar as TCA contamination persists in cork products, despite the use of this washing process in the cork industry for the last 15 years.
  • Cork product ozonization is a process used in industry for microbial load reduction having in mind to prevent TCA production in the presence of primers. Ozonization can be simultaneous with the washing, by ozone injection into the washing water or by exposing the cork stoppers to a saturated ozone atmosphere. This process efficiency in terms of microbial load is well established, but TCA level reduction by ozone oxidative action is very doubtful. Industrial scale essays vie conducted showed no such reductions of TCA levels due to direct oxidative effect of ozone in saturated atmosphere.
  • Cortex a physical barrier between the cork stopper and the wine product is a process currently used to prevent TCA migration from the cork stopper to said wine product, under the designation Cortex.
  • This product is just a silicone barrier, with about 1 mm thick, adapted to the cork stopper base that contacts the wine in order to prevent TCA migration.
  • this small silicone disk delays the TCA migration by physical effect and not because silicone is an effective TCA barrier.
  • Cortex is not useful at all due to the fact that wine products can stay bottled longer than the time needed for TCA to migrate through the silicone disk to the wine products.
  • Another process proposed as being effective in TCA reduction is the use of enzymes, namely lacase-polifenol-oxidase.
  • This enzyme can polymerise phenols therefore preventing their metabolic conversion into anizoles by fungi action.
  • this enzyme is a good solution to prevent TCA formation, it does not act on the TCA already present and absorbed in cork products, therefore preventing its polymerisation. Consequently, the already existing TCA remains in cork products and can, therefore migrate to the wine products. Essays made in several laboratories confirm that this product is not effective in eliminating TCA.
  • cork granules treatment with water vapour in autoclave or with vapour jet in an industrial scale drum has been the current practice, either in Portugal (autoclave) or in Japan (vapour jet in an industrial scale drum).
  • autoclave both with cork granules and with cork planks does not seem to significantly reduce TCA in these products.
  • water vapour in a industrial scale drum seems to achieve a significant reduction of TCA in cork granules, but this process has the drawback that it uses a drum that prevents the continuous cork granule treatment, which is essential to the industrial scale feeding of extruding and moulding machinery used in continuous production of champagne, technical and composite stoppers.
  • EP-A-1 224 946 discloses an apparatus and process for the decontamination of cork granules in order to minimise the presence of compounds that would generate unpleasant smell.
  • the granules are fed to the apparatus and travel through it by a mixing device have a rotating shaft comprising outlet orifices for a gas in order to thoroughly mix the granules.
  • the shaft is provided with mixing blades and the decontamination is carried out by means of microwave radiation.
  • the ROSA System is a system that allows the significant extraction of compounds absorbed in cork products, dragged by water vapour, in particular TCA.
  • This system comprises two different types of apparatus. One is adapted for use with cork granules that continuously extracts said compounds, and the other one is adapted to disks and stoppers, using a drum to clean these products batch wise.
  • This apparatus comprises a stainless steel cylinder, with 2500 mm length and 250 mm diameter, having several openings, namely: four side openings (A) to the inlet of the water vapour coming from a generating source (I), which inlet that can be controlled by faucets (B); an opening (C) located on the underside of the apparatus for granule recovery after treatment; an opening (D) located on the upper side for the exhaustion of the water vapour after granule treatment.
  • a generating source I
  • faucets B
  • D located on the upper side for the exhaustion of the water vapour after granule treatment.
  • a screw propeller (K) turning about a central shaft, driven by an motor (F) that forces a rotation movement.
  • the clearance between the cylinder and the screw propeller is small so that a certain portion of the cork granules that are at a certain pitch of blades of the screw propeller can only proceed to the next pitch of blades by way of the rotation screw propeller motion.
  • the cork granule is unloaded into a feeding hopper, provided with a lock (E) that controls the amount of granules entering the system.
  • the water vapour is generated in an external boiler, the flow rate being controlled by a pressure control valve (J).
  • the system is also equipped with a temperature controller (H) and a pressure gauge (G).
  • the A type apparatus of the ROSA system uses the following operating conditions:
  • This apparatus ( Figure 2) comprises a stainless steel cylinder, located horizontally along its longitudinal axis, having in one top a lid that tightly seals by means of thread screws (A). Inside this cylinder is provided another smaller cylinder (B) in concentric arrangement regarding the first one, which surface is made of perforated plate.
  • This inner cylinder has a longitudinal opening in order to allow the loading of the cork product to be treated (disks or stoppers).
  • the inner cylinder rotates about a central shaft (C) provided with openings in its surface through which the water vapour is introduced into the apparatus.
  • the water vapour is generated in an external boiler (D), the flow rate being controlled by a pressure control valve (E).
  • the system is also equipped with a temperature controller (F) and a pressure gauge (G).
  • the outer cylinder has two further openings:
  • the lid (A) After introducing the cork product to be treated in the cylinder, the lid (A) is closed and the system is driven through the rotation movement imparted by the motor (J) and by the continuous introduction of water vapour inside the system.
  • the B type apparatus of the ROSA system uses the following operating conditions:
  • the ROSA system efficiency was assessed in several stages. First it was studied at laboratory scale, followed by pilot industrial scale tests.
  • TCA cork granules, disks and stoppers, naturally and experimentally contaminated with TCA in order to verify the TCA reduction magnitude that could be achieved by the system in this compound.
  • the TCA determination was made using the GC-MS coupled with SPME technique, after 24 hours maceration in 10% ethanol.
  • Each granule sample consists of about 2 g of granules with particle dimensions of 1-2 rom.
  • Each disk and stopper sample corresponds to a simultaneous maceration of 50 6x26 mm disks or of 50 28 x 24 mm stoppers.
  • Tables 1 and 2 The results are shown in Tables 1 and 2. In these tables it is evident the amount of TCA reduction achieved, in some Cases the presence of TCA having been determined in the water vapour condensate after distillation, where large amounts of TCA were found, proving the efficiency of the extraction system by water vapour TCA dragging.
  • Table 1 TCA before and after treatment by water vapour distillation in TCA naturally contaminated samples 10 min. 20min. 30 min 60 min.
  • Figs. 3, 4 and 5 show the achieved results.
  • Fig. 3 shows the results of 2-3 mm granules treatment in the A type apparatus, using different residence times, one "rapid” module with a treatment of about 6 minutes, and one "slow” module with a treatment of about 20 minutes.
  • Each group consists of 3 dark bars and 3 light ones, referring the same type of granule that are sampled 3 times before treatment and 3 times after treatment. TCA reductions are significant, depending however on the treatment time, being higher after a longer treatment. The average values and the corresponding standard deviations are shown in figure.
  • Fig. 4 refer to the treatment of about 40 kg of granules in the A type apparatus for 20 minutes.
  • Fig. 5 shows the results of sensorial analysis to sample pairs before and after a 20 minutes treatment. A panel of 15 trained tasters has been used and they have been asked if they would identify unpleasant aromas in the samples, and when those unpleasant aromas were found within the same pair, which sample had the most intense aroma. The results are evident with almost all of the treated samples considered clean by most of the tasters.
  • the B type apparatus was construed for the treatment of natural disks and stoppers, since the A type apparatus produced important deformations in the cork pieces, therefore preventing its intended use as sealing elements or parts of sealing elements (Fig. 7 and 8).
  • the TCA reductions achieved with this apparatus in disks were highly significant (Fig. 9) without significant changes in the visual class (Fig. 10).
  • the TCA mean reduction was 75%, while in the visual classes the reduction was 8,6% in class A and 2,3% in class B.
  • extraction system of water vapour dragged compounds is highly effective in reducing cork granules, disks, and stoppers contamination by these compounds, either using a continuous operated apparatus type for granules or using another type, batch operated, for disks and stoppers.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Forests & Forestry (AREA)
  • Closures For Containers (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Fertilizers (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Confectionery (AREA)
  • Seasonings (AREA)
EP03784710A 2002-08-13 2003-08-08 Cork product treatment process by extraction of compounds dragged in water vapour Expired - Lifetime EP1551463B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
PT10282902 2002-08-13
PT102829A PT102829B (pt) 2002-08-13 2002-08-13 Sistema e dispositivo para extrair compostos arratados pelo vapor de agua em produtos em cortica
PCT/PT2003/000010 WO2004014436A1 (en) 2002-08-13 2003-08-08 Cork product treatment system and apparatuses by extraction of compounds dragged in water vapour

Publications (2)

Publication Number Publication Date
EP1551463A1 EP1551463A1 (en) 2005-07-13
EP1551463B1 true EP1551463B1 (en) 2006-06-21

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP03784710A Expired - Lifetime EP1551463B1 (en) 2002-08-13 2003-08-08 Cork product treatment process by extraction of compounds dragged in water vapour

Country Status (8)

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EP (1) EP1551463B1 (es)
AT (1) ATE330639T1 (es)
DE (1) DE60306404T2 (es)
ES (1) ES2268459T3 (es)
MA (1) MA27383A1 (es)
PT (1) PT102829B (es)
TN (1) TNSN05029A1 (es)
WO (1) WO2004014436A1 (es)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PT104230B (pt) * 2008-10-23 2012-01-23 Amorim Isolamentos S A Processo e dispositivo para expansão de material de cortiça por acção de vapor de água saturado e/ou sobreaquecido
IT1395893B1 (it) * 2009-09-18 2012-10-26 Sugherificio Colla E Fresu S R L Turacciolo e suo metodo di realizzazione.
EP2404647B1 (en) * 2010-07-08 2013-03-27 Dartes Krup, S.L. Method for extracting organic compounds from granulated cork
PT105500A (pt) 2011-01-24 2012-07-24 Amorim & Irmaos S A Processo de aplicação de revestimento polimérico em rolhas de cortiça
ES2423255B1 (es) * 2012-03-13 2014-10-01 Universidad De Salamanca Procedimiento para la eliminación de haloanisoles y halofenoles presentes en el corcho e instalación para llevar a cabo dicha eliminación
PT108104B (pt) 2014-12-18 2021-09-16 Cork Supply Portugal S A Método de detecção de analito volátil para categorização e separação de rolhas de cortiça em função da concentração desse analito
ES2726598B2 (es) 2018-04-05 2020-06-25 Escor Processos Lda Dispositivo y procedimiento para la reduccion del tca en productos de corcho
PT115572A (pt) 2019-06-07 2020-12-07 Univ Nova De Lisboa Processo e equipamento para extração de tca de rolhas de cortiça natural com solvente orgânico líquido

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2380696A (en) * 1945-07-31 Method of sterilizing
US5941468A (en) * 1998-01-22 1999-08-24 Sterile Technology Industries, Inc. Waste treatment apparatus and method
GB2361644B (en) * 1999-11-27 2003-06-18 Robert Mayberry Marshall Waste treatment apparatus and methods
DE10101980B4 (de) * 2001-01-18 2005-02-24 Linn High Therm Gmbh Vorrichtung zur Behandlung eines Schüttguts, insbesondere von Korkgranulat

Also Published As

Publication number Publication date
DE60306404T2 (de) 2006-11-09
ES2268459T3 (es) 2007-03-16
MA27383A1 (fr) 2005-06-01
TNSN05029A1 (en) 2007-05-14
PT102829A (pt) 2004-02-27
EP1551463A1 (en) 2005-07-13
PT102829B (pt) 2005-06-30
DE60306404D1 (de) 2006-08-03
ATE330639T1 (de) 2006-07-15
WO2004014436A1 (en) 2004-02-19

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