EP0395010B1 - Method and apparatus for deodorization of cork - Google Patents

Method and apparatus for deodorization of cork Download PDF

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Publication number
EP0395010B1
EP0395010B1 EP90107858A EP90107858A EP0395010B1 EP 0395010 B1 EP0395010 B1 EP 0395010B1 EP 90107858 A EP90107858 A EP 90107858A EP 90107858 A EP90107858 A EP 90107858A EP 0395010 B1 EP0395010 B1 EP 0395010B1
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EP
European Patent Office
Prior art keywords
cork
steam
container
set forth
cooling
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
EP90107858A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0395010A1 (en
Inventor
Ichiro Konishi
Ryoichi Tajima
Tetsuo Tsutsumi
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.)
Uchiyama Manufacturing Corp
Suntory Ltd
Original Assignee
Uchiyama Manufacturing Corp
Suntory Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Uchiyama Manufacturing Corp, Suntory Ltd filed Critical Uchiyama Manufacturing Corp
Publication of EP0395010A1 publication Critical patent/EP0395010A1/en
Application granted granted Critical
Publication of EP0395010B1 publication Critical patent/EP0395010B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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 relates to a method for removing offensive odors from cork.
  • Cork has unique characteristics. It is lightweight and has a high degree of resilience. Additionally, it has excellent gas and liquid sealing properties, and it is stable against solvents such as alcohol. Furthermore, it is a hygienic material which is food-safe and not harmful to human beings, and which has no intrinsic odor.
  • cork has been widely utilized as stoppers for casings such as bottles filled with liquor such as wine, brandy or whiskey, or casings packed with various kinds of foods.
  • TCA 2,4,6-trichloroanisol
  • Cork is heated and dried at 80 °C for 6 to 8 h, after which the offensive odor causing substances are substantially evaporated.
  • TCA is specifically adsorbed by the macromolecular compounds which form cork such as cellulose, lignin and suberin, and it is difficult to remove TCA in the dried state.
  • the boiling point of TCA is 240 °C at 98.2 kPa (738.2 mmHg), and 132 °C at 3.7 kPa (28 mmHg). Therefore, in order to evaporate TCA, a heating temperature must be applied which is higher than the boiling point of TCA.
  • Cork is heated at 80 °C for 6 h, and is then left at room temperatures for about a month.
  • TCA can be removed by repeating this treatment many times. However, this method requires long periods of treatment until the TCA is entirely removed. Therefore, the production efficiency is low. (2 or 3 repetitions of the above treatment is insufficient for entirely removing TCA).
  • Cork is deodorized by being soaked in a 3 vol% solution of citric acid for 3 to 5 min.
  • the effects of this deodorization technique are retained only for a short period. That is, because cork resists the absorption of liquids, the citric acid solution cannot reach the cork interior. Therefore, the deodorizing treatment affects only the cork surface and untreated TCA within the cork is moved to the cork surface with the lapse of time. Thus the offensive odor re-occurs.
  • Cork is deodorized and sterilized by soaking it in a 1 vol% solution of hydroperoxide (H2O2).
  • H2O2 hydroperoxide
  • Cork is left and deodorized in an alcohol atmosphere at 18 to 24 °C for a month.
  • this method encounters the same problems as methods (3) and (4).
  • Cork in the grain state is washed in hot water at a temperature of 60 °C.
  • the treatment needs to be repeated 2 times.
  • TCA has a relatively strong affinity for cork, it is moved to and retained in the internal portions of the cork. According to this method, therefore, the deodorizing effect is still insufficient because the treatment affects only the cork surface.
  • TCA in the cork is extracted by a Soxhlet extractor at 45 °C for 24 hours with n-pentane.
  • TCA is entirely removed from both the surface and internal areas of the cork.
  • the equipment is very expensive and production costs become very high.
  • a certain degree of safety risk is encountered with this method.
  • DE-A-37 05 422 discusses that cork is sterilized with ozonized water or an ozonized silicone emulsion, in which the ozonized concn. is 1 mg/l at a temperature lower than 30°C.
  • the object of the present invention to provide a method for deodorizing cork by removing substances causing offensive odors, principally TCA, from the cork interior without deteriorating the cork's unique characteristics, and further to provide an apparatus for carrying out this method.
  • this object is attained with a method for deodorizing cork by removing a substance originating offensive odor from the cork comprising the steps of: supplying steam for generating a steam flow to said cork in a container with a temperature of 100°C to 130°C and a pressure of at least 101.1 kPa (760 mmHg) to thereby cause steam molecules to penetrate the internal structure of the cork thus promoting a steam distillation within the internal structure of the cork, and discharging the steam past the cork and containing the substance originating offensive odor, from said container.
  • the substance originating offensive odors may be 2,4,6-trichloroanisole which may be produced from 2,4,6-trichlorophenol or 2,4,6-trichlorphenol itself. It is preferred that the method further comprises the steps of: cutting the cork into pieces having a predetermined size, pre-heating the cut cork to a certain temperature, and maintaining the temperature and the pressure during deodorization.
  • the steam temperature is at least 100 °C; the system pressure is at least 101.1 kPa (760 mmHg).
  • the second step further comprises supplying the steam for the cork from the bottom of the container.
  • the second step may further comprise agitating the container.
  • the agitating step comprises rotating and/or oscillating the container.
  • the agitating step may also comprise stirring the cork in the container.
  • the method may further comprise the step of cooling the cork in the container.
  • the cooling step may include the steps of: maintaining the cork within the container and stopping the steam supply, thus causing a natural cooling, generating a hot atmosphere, supplying the hot atmosphere to the interior of the container after the cooling efficiency by the natural cooling has been lowered.
  • the container is maintained at a rotating and oscillating condition when the hot atmosphere is supplied thereto.
  • an apparatus for deodorizing cork by steam distillation comprising:
  • the present invention is accomplished by utilizing conventional steam distillation.
  • cork has the water resistive property to prevent water molecules from penetrating into the internal structure thereof. Therefore, though it is known that TCA on the cork surface can be washed out by water, internally contained TCA cannot be removed by water. To this point, it has been known that TCA has a characteristic which is that it can be volatilized with steam. Additionally, it has a relatively low boiling point at 3.7 kPa (28 mmHg). Therefore, if the treating temperatures are controlled to the level at which the partial pressure of TCA becomes 3.7 kPa (28 mmHg), TCA can be evaporated at relatively low temperatures. Taking the factors mentioned above into consideration, the inventors became aware that steam distillation may be effectively utilized for the deodorization of cork.
  • the steam can penerate into the internal structure of the cork for heating the internal structure so that steam distillation is caused within the internal structure for removing TCA residing in the inside of the cork.
  • cork Any kind of cork may be used and it is not limited to the field of its use or by its form.
  • cork for bottle capping, wine bottle stoppers or crown disks, for architectural use, vibration proofing or heat insulator materials may all benefit from the treatment according to the present invention.
  • the shape of the first means is not specifically limited, but for effective steam utilization, a longitudinal shape the container of which is formed with a diameter smaller than its height is most preferred.
  • any state of the cork is acceptable, but for enhancing the removal efficiency by homogenizing steam and cork, maintaining the cork in an agitated state while supplying steam to the first means is preferable.
  • moving the container per se e.g., oscillating or rolling
  • to locating an agitating means in the container of the first means to stir the inner materials are both acceptable.
  • the steam temperature is at least 100°C and the pressure of the container is at least 101 kPa (760 mmHg).
  • the partial pressure is not high enough to cause steam distillation within the internal organization of the cork.
  • the penetration of steam molecules into the internal structure of the cork may not be sufficient.
  • the steam temperature is higher than 130°C, it becomes difficult to control the temperature during the cooling process. That is, at a high steam temperature, a significant amount of steam can penetrate the internal structure.
  • the steam penetrating the internal structure of the cork may lead to a shrinkage of the cork when it is subjected to an atmospheric temperature which may result in rapid cooling. A significant magnitude of shrinkage of the cork may degradate the properties of the cork. Therefore, the temperature has to be maintained to be lower than or equal to 130°C.
  • the cork size is not limited specifically, but a smaller size is preferred because the TCA movement from within the cork to its surface becomes easier. This results in an effective removal of TCA.
  • the specific treatment temperature, the specific system pressure, the container configuration, the cork amount to be treated and other conditions for the steam distillation treatment can be selected according to the required efficiency and degree of removal of TCA.
  • the partial pressure of the TCA can be reduced by the partial pressure of the steam, and the boiling point of TCA can be lowered to about atmospheric pressure. Therefore, the deterioration of the cork can be avoided and the deodorization of the cork (removal of TCA) can be accomplished sufficiently.
  • FIG. 1 a block diagram showing the method for removing offensive odor according to the present invention is shown.
  • a given amount of cork 2 cut to a predetermined size is put into a treating container 1.
  • Purified water provided from a purified water generator 4 is supplied to a steam generator 3. Then, after steam is generated in the generator 3, it is supplied to the container 1 via a steam supply pipe 5. Steam distillation of the cork 2 is performed in the container 1, then steam is discharged from the container 1 through a steam discharge pipe 6 out of the system.
  • Steam feeding is controlled by a supply valve 7, a flow meter 8, pressure meters 9, and 10, a discharge valve 11, and a flow control valve 12.
  • Temperature sensors 13, 14 and 15 are installed in the upper, middle and lower ports of container 1, respectively. The temperature in the container 1 is monitored through these sensors by a monitor system 16, then temperature is controlled at the constant predetermined level.
  • the container 1 has an outer container 17 and an inner container 18 spaced from the outer container 17 at a constant interval as shown in Fig. 2. It may be formed as a cylinder. In this way, the container 1 is formed as a pressure proof container having a double-walled structure. This structure enables steam to be introduced into the space between the outer and the inner wall after it goes through the cork 2. Therefore, steam in the space through which the steam past the cork flows, serves for maintaining the container temperature at the desired treatment temperature and thus for reducing the heat loss in the steam Referring now to Fig. 2, when amounts of cork 2 are put into the inner container 18 by opening a lid 19, they pile on a bottom plate 20. Steam is sprayed into the interior of the container 1 through a plurality of steam pores 21 penetrating the bottom plate 20, and runs through the piled cork 2 from bottom to top.
  • a steam inlet pipe 22 is connected to the center port of the container's bottom and extends from the lower end of the outer container 17 of the container 1 to the outside of the container.
  • the lower edge of the inlet pipe 22 is connected to the steam supply pipe 5 via a first rotary joint 23.
  • Steam fluid supplied from the supply pipe 5 is supplied to the inlet pipe 22, to the inner container 18 via the steam spraying pores 21 in the bottom plate 20 of the container 1.
  • steam supplied into the inner container 18 rises through the cork 2 concurrently heating it, and is discharged from steam discharging pores 24 which penetrate the upper side wall(s) of the inner container 18 into the space 25 between the outer container 17 and the inner container 18, an outlet pipe 26 coaxially arranged surrounding the outside of the steam inlet pipe 22.
  • it is discharged from the steam discharge pipe 6 connected to the outlet pipe 26 via a second rotary joint 27.
  • Pressure and flow of steam can be controlled at a constant level by the discharge valve 11 and the flow control valve 12.
  • a central shaft 28 for rotation is located surrounding the outlet pipe 26, and is rotatably supported by a bottom portion 30a of an oscillating frame 30 formed in U-shape via a bearing 29.
  • the container 1 can be rotated against the central shaft by a rotation drive device 31 installed on the bottom portion 30a of the oscillating frame 30 composed of a motor, rotation gear, translation gear or so forth. Additionally, the container 1 can be oscillated by the oscillating frame 30. Then, by rotating with oscillation, the cork 2 and steam in the container 1 can be agitated sufficiently.
  • a pair of supporting shafts 32, and 33 are installed to an outer surface of an upper end of side portions 30b of the oscillating frame 30. These shafts 32, 33 are oscillatably supported by a pair of fixed frames 36, 37 via bearings 34, 35 to be oscillated by an oscillation drive device 38.
  • the oscillation drive device 38 is composed of a worm wheel 39 installed on the supporting shaft 33 and a motor 42 which rotatably operates a worm gear 40 via belt 41, where the worm gear 40 is engaged to gear teeth of the worm wheel 39.
  • the motor 42 is rotated in one direction the worm gear 40 and the worm wheel 39 are rotated in the same direction. This rotation slowly oscillates the oscillating frame 30 in one direction.
  • the motor 42 is rotated in the other direction, it slowly rotates the oscillating frame 30 in the other direction. In this way, the oscillating frame 30 is oscillated.
  • the steam supply pipe 5 is located through the center portion of the supporting shaft 33, connected to the oscillating frame 30 via a third rotary joint 43, and further connected to the container 1 via the first rotary joint 23.
  • the steam discharge pipe 6 is located through the center portion of the other supporting shaft 32, connected to the oscillating frame 30 via a forth rotary joint 44, and further connected to the container 1 via the second rotary joint 27.
  • a slip ring 45 is mounted on the edge of the central shaft 28 of the container 1. Signals, obtained from temperature sensors 13, 14 and 15, connected to the outside portion of the oscillating frame 30 via the slip ring 45, are input to a monitoring device 16 which is connected to the slip ring 45 (as shown in Fig. 1) allowing the temperature in the container to be effectively monitored.
  • Circular frames 46 are mounted on the top of the side portion 30b of the oscillating frame 30. Rollers 47 are installed in the inner surface of the radial frames 46 to rotate the container 1 smoothly by supporting the outer surface of the upper port of the container 1.
  • the rotation speed of the container is preferably determined as, at least, 10 rpm, and the incline angle is preferably determined as at least ⁇ 60°, though they depend on conditions such as the processing amount and the cork size.
  • the inclination angle range of the container is not strictly limited to ⁇ 60° but can be selected in any way.
  • the inclination angle of the container may be determined according to the degree of filling of the cork within the interior space of the container. Namely, the inclination angle is selected so that the cork can be distributed over the entire area of the steam path so that the steam cannot escape without contacting the cork.
  • the driving speed in rolling and agitation may be determined according to the amount of the cork filled in the container.
  • a relatively long period is required for satisfactorily cooling the internal structure of the cork. This means that if cork is immediately removed from the container to subject it to the atmosphere, a substantial magnitude of shrinkage may be caused in the cork to make it stiff and to degrade the cork properties.
  • allowing natural cooling takes a very long time.
  • supplying a hot atmosphere to the container by way of cooling may be effective.
  • rotation and oscillation of the container 1 are continued while cooling.
  • the hot atmosphere is generated in a hot atmosphere generator (not shown in the Figures), and is supplied to the container 1 by controlling the valve 7 located on the steam inlet side.
  • the hot atmosphere supplied to the container 1 can take latent heat from the surface of the cork 2 when steam is evaporated. This increases the cooling speed.
  • the penetration degree is exponentially increased according to rising of the steam temperature.
  • Cork capping plug recognized as corked was crushed by a known cork crushing machine into a grain size ordinarily used for forming compressed cork, for forming sample cork pieces. 4g of the sample cork pieces were put in a gauze bag (15 cm x 20 cm). The sample cork containing bag was put in the mid portion of the cork burden in the container 1.
  • the deodorization treatment was performed utilizing the apparatus of Fig. 2. In the treatment, the container 1 was rolled with sccessive variations of the inclination angle. The steam was flown through the container 1 across the cork in a flow rate of 20 l/h and 40 l/h. The deodorization treatment was performed for 30 min, 60 min and 90 min after reaching a predetermined condition, i.e.
  • the temperature in the container was 120 °C and the pressure was 1 kg/cm2.
  • the residual TCA amount was checked.
  • the check of residual TCA was performed by slicing the sample cork, extracting the TCA from slices by n-pentane, and measurement by gascromatograph. The result of measurement is shown in Table 4 and Fig. 3.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Forests & Forestry (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Treating Waste Gases (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
EP90107858A 1989-04-26 1990-04-25 Method and apparatus for deodorization of cork Expired - Lifetime EP0395010B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP106781/89 1989-04-26
JP10678189 1989-04-26

Publications (2)

Publication Number Publication Date
EP0395010A1 EP0395010A1 (en) 1990-10-31
EP0395010B1 true EP0395010B1 (en) 1994-02-23

Family

ID=14442447

Family Applications (1)

Application Number Title Priority Date Filing Date
EP90107858A Expired - Lifetime EP0395010B1 (en) 1989-04-26 1990-04-25 Method and apparatus for deodorization of cork

Country Status (12)

Country Link
EP (1) EP0395010B1 (es)
JP (1) JP2673382B2 (es)
AT (1) ATE101817T1 (es)
AU (1) AU630444B2 (es)
CA (1) CA2015419C (es)
DE (2) DE4013219A1 (es)
DK (1) DK0395010T3 (es)
ES (2) ES2051405T3 (es)
FR (1) FR2646372B1 (es)
GB (1) GB2230956B (es)
IT (1) IT1240633B (es)
PT (1) PT93857B (es)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2782289B1 (fr) 1998-08-11 2000-11-10 Pernod Ricard Procede de traitement de produit a base de liege utilisable pour la realisation de bouchons et bouchons comprenant un tel produit traite
FR2798879B1 (fr) * 1999-09-27 2001-10-19 Commissariat Energie Atomique Procede de traitement, et d'extraction de composes organiques du liege, par un fluide dense sous pression
ATE301026T1 (de) * 2001-11-12 2005-08-15 Inst Superior Tecnico Neue verfahren zur behandlung von korkstopfen und platten zur verringerung der fremden aromen, nämlich 2,4,6-trichoroanisole
DE10341637A1 (de) * 2003-09-10 2005-05-04 Degussa Verfahren zur Extraktion von korkhaltigem Material
US7010956B2 (en) * 2003-11-05 2006-03-14 Michael S. Head Apparatus and method for detecting an analyte
JP4504754B2 (ja) * 2004-07-21 2010-07-14 洋二 木方 コルク粉末含有リグノセルロース系成形用粉末材料およびその成形体
ES2259547B1 (es) * 2005-02-17 2007-06-01 Jose Luis Godoy Varo Metodo para la descontaminacion de corcho e instalacion para su puestaen practica.
JP4626713B2 (ja) * 2008-10-20 2011-02-09 株式会社高瀬文夫商店 木製食品容器の脱臭・脱色の処理方法
DE102009041870B4 (de) 2009-09-16 2013-02-28 Klaus-Dieter Heun Sanitärmodul
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
ES2726598B2 (es) 2018-04-05 2020-06-25 Escor Processos Lda Dispositivo y procedimiento para la reduccion del tca en productos de corcho
ES2958166A1 (es) * 2022-07-06 2024-02-02 Univ La Rioja Método de tratamiento con agua activada por plasma de materiales auxiliares de origen forestal para la conservación del vino y uso del agua activada por plasma

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE264305C (es) *
DE176526C (es) *
AT28312B (de) * 1904-06-12 1907-05-10 Hugo Gronwald Verfahren zum Sterilisieren und Konservieren von Flaschenkorken u. dgl.
DE267733C (de) * 1906-12-07 1913-11-15 Gruenzweig & Hartmann Verfahren zur Behandlung von Kork durch Hitze
DE557849C (de) * 1931-01-10 1932-08-29 Gruenzweig & Hartmann G M B H Verfahren zur Herstellung von expandiertem Korkschrot
DE689147C (de) * 1932-01-08 1940-03-12 Franz Lautenschlaeger Vorrichtung zur Sterilisation und Desinfektion von Verbandsmaterial o. dgl. mittels gespannten Dampfes
GB661453A (en) * 1949-10-04 1951-11-21 Vendo Co Steam cooker
GB993883A (en) * 1961-03-04 1965-06-02 Electrolux Ab Improvements in sterilisation autoclaves
DE1492364A1 (de) * 1963-07-18 1970-02-05 Irons Alexander S Sterilisationsverfahren und Sterilisator
SE417328B (sv) * 1978-01-16 1981-03-09 Fazer Ab Forfarande for deodorisering av kakaosmor i en tunnskiktsindustare vilket fett dessforinnan kontinuerligt homogeniserats tillsammans med avjoniserat eller destillerat vatten

Also Published As

Publication number Publication date
DE69006767T2 (de) 1994-06-01
IT9020121A1 (it) 1991-10-24
JP2673382B2 (ja) 1997-11-05
DE69006767D1 (de) 1994-03-31
ES2051405T3 (es) 1994-06-16
ES2019562A6 (es) 1991-06-16
IT9020121A0 (it) 1990-04-24
GB2230956A (en) 1990-11-07
FR2646372A1 (fr) 1990-11-02
AU630444B2 (en) 1992-10-29
FR2646372B1 (fr) 1994-02-11
AU5388190A (en) 1990-11-08
GB2230956B (en) 1992-09-09
DK0395010T3 (da) 1994-05-09
GB9009274D0 (en) 1990-06-20
JPH0347701A (ja) 1991-02-28
PT93857A (pt) 1990-11-20
PT93857B (pt) 1996-10-31
IT1240633B (it) 1993-12-17
EP0395010A1 (en) 1990-10-31
CA2015419C (en) 1999-11-16
ATE101817T1 (de) 1994-03-15
CA2015419A1 (en) 1990-10-26
DE4013219A1 (de) 1990-11-22

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