EP2033751A1 - Verfahren zur Behandlung von Kork oder eines Materials auf Korkbasis mit einem Inertgas unter einem Druck, der strikt unter 1 MPa liegt - Google Patents
Verfahren zur Behandlung von Kork oder eines Materials auf Korkbasis mit einem Inertgas unter einem Druck, der strikt unter 1 MPa liegt Download PDFInfo
- Publication number
- EP2033751A1 EP2033751A1 EP07116628A EP07116628A EP2033751A1 EP 2033751 A1 EP2033751 A1 EP 2033751A1 EP 07116628 A EP07116628 A EP 07116628A EP 07116628 A EP07116628 A EP 07116628A EP 2033751 A1 EP2033751 A1 EP 2033751A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cork
- based material
- treatment
- inert gas
- material according
- 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.)
- Granted
Links
- 239000007799 cork Substances 0.000 title claims abstract description 127
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000011261 inert gas Substances 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000011282 treatment Methods 0.000 claims abstract description 46
- 239000008187 granular material Substances 0.000 claims description 39
- 239000006184 cosolvent Substances 0.000 claims description 33
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 28
- 239000012855 volatile organic compound Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 15
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 14
- WCVOGSZTONGSQY-UHFFFAOYSA-N 2,4,6-trichloroanisole Chemical compound COC1=C(Cl)C=C(Cl)C=C1Cl WCVOGSZTONGSQY-UHFFFAOYSA-N 0.000 claims description 13
- 239000001569 carbon dioxide Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- VSMOENVRRABVKN-UHFFFAOYSA-N oct-1-en-3-ol Chemical compound CCCCCC(O)C=C VSMOENVRRABVKN-UHFFFAOYSA-N 0.000 claims description 8
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 8
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- IZUPBVBPLAPZRR-UHFFFAOYSA-N pentachlorophenol Chemical compound OC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl IZUPBVBPLAPZRR-UHFFFAOYSA-N 0.000 claims description 6
- BBABSCYTNHOKOG-UHFFFAOYSA-N 1,2,3,4,5-pentachloro-6-methoxybenzene Chemical compound COC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl BBABSCYTNHOKOG-UHFFFAOYSA-N 0.000 claims description 5
- ITXDBGLYYSJNPK-UHFFFAOYSA-N 1,2,3,5-Tetrachloro-4-methoxybenzene Chemical compound COC1=C(Cl)C=C(Cl)C(Cl)=C1Cl ITXDBGLYYSJNPK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- QCIWPAJGVAANGJ-UHFFFAOYSA-N tribromomethoxybenzene Chemical compound BrC(Br)(Br)OC1=CC=CC=C1 QCIWPAJGVAANGJ-UHFFFAOYSA-N 0.000 claims description 5
- VSMOENVRRABVKN-MRVPVSSYSA-N 1-Octen-3-ol Natural products CCCCC[C@H](O)C=C VSMOENVRRABVKN-MRVPVSSYSA-N 0.000 claims description 4
- VGVRPFIJEJYOFN-UHFFFAOYSA-N 2,3,4,6-tetrachlorophenol Chemical class OC1=C(Cl)C=C(Cl)C(Cl)=C1Cl VGVRPFIJEJYOFN-UHFFFAOYSA-N 0.000 claims description 4
- YDXQPTHHAPCTPP-UHFFFAOYSA-N 3-Octen-1-ol Natural products CCCCC=CCCO YDXQPTHHAPCTPP-UHFFFAOYSA-N 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 4
- 229960001867 guaiacol Drugs 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 235000019640 taste Nutrition 0.000 description 9
- 238000000605 extraction Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- JZABSYYZGLCMMZ-UHFFFAOYSA-N carbamic acid;2-(hydroxymethyl)-2-methylpropane-1,3-diol Chemical compound NC(O)=O.NC(O)=O.NC(O)=O.OCC(C)(CO)CO JZABSYYZGLCMMZ-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QGRPVMLBTFGQDQ-UHFFFAOYSA-N 1-chloro-2-methoxybenzene Chemical class COC1=CC=CC=C1Cl QGRPVMLBTFGQDQ-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 241000219492 Quercus Species 0.000 description 2
- 229930183415 Suberin Natural products 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- -1 lindane Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- JLPUXFOGCDVKGO-TUAOUCFPSA-N (-)-geosmin Chemical compound C1CCC[C@]2(O)[C@@H](C)CCC[C@]21C JLPUXFOGCDVKGO-TUAOUCFPSA-N 0.000 description 1
- 239000001075 (4R,4aR,8aS)-4,8a-dimethyl-1,2,3,4,5,6,7,8-octahydronaphthalen-4a-ol Substances 0.000 description 1
- XYHPPOMSLGJAAM-UHFFFAOYSA-N 2-ethyl-3-methylsulfanylpyrazine Chemical compound CCC1=NC=CN=C1SC XYHPPOMSLGJAAM-UHFFFAOYSA-N 0.000 description 1
- LFYXNXGVLGKVCJ-FBIMIBRVSA-N 2-methylisoborneol Chemical compound C1C[C@@]2(C)[C@](C)(O)C[C@@H]1C2(C)C LFYXNXGVLGKVCJ-FBIMIBRVSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UDHXJZHVNHGCEC-UHFFFAOYSA-N Chlorophacinone Chemical compound C1=CC(Cl)=CC=C1C(C=1C=CC=CC=1)C(=O)C1C(=O)C2=CC=CC=C2C1=O UDHXJZHVNHGCEC-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical class COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- JLPUXFOGCDVKGO-UHFFFAOYSA-N dl-geosmin Natural products C1CCCC2(O)C(C)CCCC21C JLPUXFOGCDVKGO-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- JLYXXMFPNIAWKQ-GNIYUCBRSA-N gamma-hexachlorocyclohexane Chemical compound Cl[C@H]1[C@H](Cl)[C@@H](Cl)[C@@H](Cl)[C@H](Cl)[C@H]1Cl JLYXXMFPNIAWKQ-GNIYUCBRSA-N 0.000 description 1
- JLYXXMFPNIAWKQ-UHFFFAOYSA-N gamma-hexachlorocyclohexane Natural products ClC1C(Cl)C(Cl)C(Cl)C(Cl)C1Cl JLYXXMFPNIAWKQ-UHFFFAOYSA-N 0.000 description 1
- 229930001467 geosmin Natural products 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 239000013529 heat transfer fluid Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229960002809 lindane Drugs 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 125000002743 phosphorus functional group Chemical group 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Images
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
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
-
- 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
- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
- B27K5/001—Heating
-
- 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 of treating cork or a cork-based material, comprising contacting the cork or the cork-based material with an inert gas at a treatment temperature of 20 to 140 ° C. C and under a pressure strictly less than 1 MPa (10 bar), a plug manufacturing process and plugs obtainable by this method.
- Cork is a natural, impervious and light material, which comes from the bark of some species of oaks, such as cork oaks, which are typically found in the countries around the Mediterranean, Europe and North Africa.
- Cork is particularly used in the manufacture of corks, which serve to plug containers such as bottles containing liquids for food, especially wine.
- Cork is an elastic material, resilient, compressible and impermeable to liquids, having at the same time a gas permeability sufficient to allow an exchange necessary for the maturation of the bottled product, and having a high coefficient of friction.
- These substances may be organic compounds such as methyl-isoborneol, geosmin, methylthio-ethylpyrazine, C8 unsaturated alcohols and ketones; chlorinated compounds such as lindane, chlorinated or non-chlorinated phenols, chlorinated or non-chlorinated anisoles, and more particularly pentachlorophenol (PCP), 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA) and pentachloroanisole, and brominated compounds such as tribromoanisole, responsible for plug or mold taste; or else p-cresol, guaiacol and octanoic acid responsible for the taste of phenol-leather-synthetic; or 1-octen-3-ol associated with mushroom taste.
- PCP pentachlorophenol
- TCA 2,4,6-trichloroanisole
- TeCA 2,3,4,6-tetrachloroani
- the cork or the cork-based material is generally subjected to treatments known in the art, in particular using carbon dioxide in the supercritical state.
- the cork by its different origins, has different mechanical and organoleptic properties, that is to say includes organic compounds responsible for said properties in different contents.
- organoleptic properties such as natural flavors.
- the aim of the invention is to satisfy this need by proposing a method of treating cork or a material based on cork, which makes it possible both to eliminate volatile organic compounds, in particular those responsible for cork taste, while at the same time preserving the mechanical properties of said cork or cork-based material, for example hydrophobicity.
- This process can be furthermore more easily implemented than the cork or cork-based processes known in the art.
- a first object of the present invention is therefore a process for treating cork or a cork-based material, comprising contacting with an inert gas at a treatment temperature of 20 to 140 ° C. under a strictly lower pressure. at 1 MPa (10 bar).
- Another object relates to a process for manufacturing stoppers using such a method for treating cork or a material based on cork.
- the invention also relates to a plug that can be obtained by the manufacturing process.
- the method of treating cork or a cork-based material comprises contacting the cork or the cork-based material with an inert gas at a treatment temperature of 20 to 140 ° C. preferably from 80 to 120 ° C, and under a pressure strictly less than 1 MPa (10 bar), preferably ranging from 0.1 to 0.4 MPa (1 to 4 bar), more preferably equal to atmospheric pressure.
- the cork or the cork-based material that can be used in the process of the invention is in particular in the form of granules preferably having a particle size of 0.1 mm up to 7 mm, plates, boards, cork washers from the casing of cork plates, natural corks from cork slabs, or cork-based corks such as "1 + 1", agglomerated or micro-agglomerated corks based on possible expansion agents.
- the particle size can be measured for example by the sieve method, at room temperature (20-25 ° C).
- Tubing is a method of making stoppers using a punch. We take a piece of cork whose thickness corresponds to the length of the cork.
- 1 + 1 is meant a stopper whose body is constituted of granules of cork agglomerated with an adhesive, while the two ends are each composed of a natural cork washer, said washers being obtained by casing a piece of cork whose thickness corresponds to that of the washers.
- the inert gas that can be used in the process according to the invention is especially chosen from carbon dioxide, nitrogen, a rare gas such as argon, and their mixtures, preferably from carbon dioxide, nitrogen and their mixtures. mixtures, and even more preferably the inert gas is carbon dioxide.
- the inert gas may be mixed with one or more so-called cosolvent compounds.
- This (s) co-solvent (s) is or are preferably chosen from water and C 1-4 alcohols such as ethanol.
- Said co-solvent or a mixture thereof is preferably added at a rate of 0 until the gas is saturated in co-solvent at the treatment temperature, which is in the range of 20 ° C to 140 ° C, better than 0.001% by weight based on the weight of the mixture inert gas + co-solvent (s) until the saturation of the gas in co-solvent (s) at the treatment temperature, and even more preferably from 0.001% by weight to 10% by weight relative to the mixture of inert gas + co-solvent (s).
- the cork or the cork-based material can be moistened by spraying water before being treated with the inert gas stream, in proportions ranging from 5% to 40%, more preferably from 15% to 25% by weight relative to the total weight of the cork.
- the duration of treatment generally ranges from 1 to 10 hours, more preferably from 2 to 4 hours.
- the process according to the invention can be carried out continuously or discontinuously, in a fixed bed or fluidized bed reactor.
- the process according to the invention carried out continuously may further comprise a step of recycling the inert gas, optionally mixed with at least one co-solvent, comprising the organic compounds extracted from cork or cork-based material, in the reactor after being subjected to a purification step, for example using activated charcoal or an absorbent substance such as bentonite, in order to eliminate the volatile organic compounds separated from the cork or the cork material, and the co-solvent (s) of the inert gas.
- a purification step for example using activated charcoal or an absorbent substance such as bentonite
- At least one exchanger may be used in order to reduce the temperature to a value below 40 ° C., preferably between 15 and 25 ° C. .
- a separation between the gas optionally mixed with at least one co-solvent and the extracted organic products can also be achieved by the addition of one or more cyclone type separators.
- Another object of the invention is the use of the method according to the invention for extracting volatile organic compounds.
- Volatile organic compounds are hydrocarbons (compounds consisting of carbon atoms and hydrogen), excluding methane, in which one or more of the atoms of hydrogen may be substituted by halogen atoms such as chlorine or fluorine, oxygenated, nitrogenous, sulfurous or phosphorus groups having a vapor pressure greater than or equal to 133 Pa at a temperature of 293.15 K. Volatile organic compounds are usually in the state of gas or vapor under normal conditions of temperature and pressure. Their Henry constant (Kh) is preferably greater than or equal to 100 Pa.m 3 / mol.
- the volatile organic compounds extracted with the process of the invention are especially (poly) chlorophenols such as pentachlorophenol (PCP), and (poly) haloanisoles such as (poly) chloroanisoles, for example 2,4,6-trichloroanisole ( TCA), 2,3,4,6-tetrachloroanisole (TeCA) and pentachloroanisole, and tribromoanisole, responsible for cork or mold taste; or p-cresol, guaiacol and octanoic acid, responsible for the taste of phenol-leather-synthetic; or 1-octen-3-ol associated with mushroom taste.
- PCP pentachlorophenol
- haloanisoles such as (poly) chloroanisoles, for example 2,4,6-trichloroanisole ( TCA), 2,3,4,6-tetrachloroanisole (TeCA) and pentachloroanisole, and tribromoanisole, responsible for cork
- a preferred embodiment of the use of the process is to extract (poly) chlorophenols such as pentachlorophenol (PCP), and (poly) haloanisoles such as (poly) chloroanisoles, for example 2,4,6-trichloroanisole ( TCA), 2,3,4,6-tetrachloroanisole (TeCA) and pentachloroanisole, and tribromoanisole.
- PCP pentachlorophenol
- haloanisoles such as (poly) chloroanisoles, for example 2,4,6-trichloroanisole ( TCA), 2,3,4,6-tetrachloroanisole (TeCA) and pentachloroanisole, and tribromoanisole.
- the invention further relates to a method for manufacturing corks or a cork-based material, comprising the method of treating cork or cork-based material as described above.
- the reactor (1) of the device is filled with cork granules (2) having a particle size ranging from 0.1 mm to 7 mm and a density ranging from 45 to 80 g / l.
- the reactor (1) has at least one of its ends, at least one filtering means such as a metal filter plate, and preferably at its two lower and upper ends (3 ') and (3 ").
- the insulated reactor (1) is heated with electric heating means or temperature control unit (UCT) and maintained at a constant temperature of 20 to 140 ° C, preferably 80 to 120 ° C.
- the heating can be achieved using an electrical resistance or a heat transfer fluid.
- the pressure in the reactor (1) is strictly less than 1 MPa (10 bar), preferably ranging from 0.1 to 0.4 MPa (1 to 4 bar), more preferably equal to atmospheric pressure. This pressure is generally regulated by a vent located on the upper part of the reactor (1) and by regulating the flow rate of the inert gas optionally mixed with at least one co-solvent
- Inert gas for example carbon dioxide or nitrogen or mixtures thereof, from a storage tank (4) is introduced via an opening valve (5), a flow control valve (6) and a flow meter (7).
- the flow rate of the inert gas preferably varies from 50 to 150 liters / minute, more preferably from 65 to 85 liters / minute.
- the inert gas is used to prevent oxidation in cork, which usually occurs when air or any other oxygen-containing mixture is used that generates Maillard reactions that produce roasted tastes. burned with cork.
- the inert gas is then heated with electric heating means (8) to the treatment temperature of from 20 to 140 ° C, preferably from 80 to 120 ° C, and optionally pressurized to a pressure less than 1 MPa (10 bar), preferably ranging from 0.1 to 0.4 MPa (1 to 4 bar).
- the inert gas is left at atmospheric pressure.
- the inert gas is mixed, for example by bubbling, before arriving in the reactor (1), with a co-solvent (9) such as water, a C 1-4 alcohol, for example ethanol, or a mixture thereof.
- a co-solvent (9) such as water
- a C 1-4 alcohol for example ethanol
- a mixture thereof may, for example, make it possible to prevent the cork granules (2) from drying out during the extraction of the volatile organic compounds, while improving the rate extraction.
- the inert gas + co-solvent mixture is further passed through an electrical heating means (10), which improves the solubility of the co-solvent in the gas, to reach a constant temperature in the range of 20 to 140 ° C, preferably 80 to 120 ° C.
- the pressure of the inert gas + cosolvent mixture is regulated via the vent (12) of the reactor to reach a pressure of less than 1 MPa (10 bar), preferably ranging from 0.1 to 0.4 MPa (1 to 4 bar).
- said mixture is left at atmospheric pressure.
- the device of the Fig. 1 further comprises an electronic control unit (11) which controls the operation of the elements (5), (6), (7), (8), (10) and (12).
- the device of the Fig. 1 does not include elements (9) and (10).
- passing a stream of inert gas optionally mixed with a co-solvent, through the cork granules (2) in the reactor (1) lasts several hours, preferably from 1 to 10 hours, better still 2 to 4 hours.
- the inert gas, optionally mixed with a co-solvent passes through the cork granules (2) in a fixed bed or in a fluidized bed.
- the inert gas makes it possible to extract undesirable volatile organic compounds, such as (poly) chlorophenols such as pentachlorophenol (PCP); (poly) haloanisoles such as (poly) chloroanisoles, for example 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA) and pentachloroanisole, and tribromoanisole; p-cresol, guaiacol, octanoic acid and 1-octen-3-ol, out of the cork granules and entrains these volatile organic compounds out of the reactor (1).
- PCP pentachlorophenol
- haloanisoles such as (poly) chloroanisoles, for example 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA) and pentachloroanisole, and tribromoanisole
- TCA 2,4,6-
- a vent (12) placed at the outlet of the reactor (1) makes it possible to regulate the pressure of the gas in the said reactor (1).
- the inert gas mixed with the co-solvent, and containing the volatile organic compounds extracted from the granules is not recycled but released into the atmosphere.
- the device comprises the same elements (1) to (12) as the device of the Fig. 1 .
- the inert gas mixed with a co-solvent, loaded with volatile organic compounds extracted from the cork granules is recycled after being passed through a cooling system (13), a separator (14) ) and a purification device (16) consisting, for example, of an activated carbon or bentonite column.
- the electronic control unit (11) of the Fig. 2 also manages the operation of the elements (13) and (15), in addition to that of the elements (5), (6), (7), (8), (10) and (12).
- the temperature of the mixture of inert gas + co-solvent charged with volatile organic compounds extracted is reduced to a value of less than 40 ° C, preferably between 15 ° C and 25 ° C, especially with the aid of the cooling system (13).
- the inert gas + co-solvent mixture charged with volatile organic compounds passes through a cyclone separating device (14) which makes a first separation between the inert gas, the co-solvent and the volatile organic compounds.
- the valve (15) draws a majority or total amount of volatile organic compounds, and a portion of the co-solvent.
- the purification device (16) completes the purification of the inert gas by absorbing any residual volatile organic compounds and the residual cosolvent.
- the combination of the elements (14) and (16) makes it possible to obtain a very good extraction rate, for example of the order of 100%, of the volatile organic compounds, and of completely purifying the inert gas, before the reintroduce into the extraction circuit.
- the device of the Fig. 2 also includes a recirculation fan (17) for recycling the inert gas into the extraction circuit.
- the content of 2,4,6-trichloroanisole contained in the cork granules was measured before and after treatment with the process according to the invention. It was measured by the method defined in the AFNOR ISO 20752: 2007 (E), edition of February 1, 2007, called cork stoppers - dosage of 2,4,6 - trichloroanisol (TCA).
- the limits of detection and quantification are respectively 0.2 and 0.5 ng / l.
- a fluidized bed reactor having a volume of about 8 liters was used.
- the reactor (1) was filled with the device of the Fig. 1 which does not include elements (9) and (10), with 104 g. cork granules (average particle size of about 1 mm), representing 18% of the volume of the reactor (1), and closed with flat filters (3 ') and (3 ").
- cork granules were treated with a stream of dry carbon dioxide gas without co-solvent, circulating at a rate of 75 l / min, at a temperature of 95.5 ° C for 5 hours, at atmospheric pressure. .
- the pellets were allowed to cool always in the presence of carbon dioxide for 45 minutes and then brought back into contact with the air.
- TCA levels are summarized in Table 1 below. ⁇ u> Table 1 ⁇ / u> TCA content (ng / l) Before treatment 3.0 After treatment 0.9
- a fluidized bed reactor having a volume of about 8 liters was used.
- the reactor (1) was filled with the device of the Fig. 1 with 100 g. of cork granules and closed with flat filters (3 ') and (3 ").
- cork granules were treated with a stream of circulating carbon dioxide gas at a rate of 75 l / min, and mixed with 0.8 liter of water at a temperature of 100 ° C for 5 hours. under atmospheric pressure.
- the granules were allowed to warm to room temperature as in Example 1 for 45 minutes and then re-contacted with air.
- TCA levels are summarized in Table 2 below. ⁇ u> Table 2 ⁇ / u> TCA content (ng / l) Before treatment 6.1 After treatment 0.5
- a fixed bed reactor having a volume of about 8 liters was used.
- the reactor (1) was filled with the device of the Fig. 1 with 600 g. of cork granules and closed with flat filters (3 ') and (3 ").
- the granules were treated with a stream of circulating carbon dioxide gas at a rate of 75 l / min, and mixed with 1.2 liters of water at a temperature of 98.5 ° C for 6 hours. under atmospheric pressure, the carbon dioxide having been in contact with demineralized water before the treatment of the cork granules.
- the granules were allowed to warm to room temperature as in Example 1 for 45 minutes and then re-contacted with air.
- TCA levels are summarized in Table 3 below. ⁇ u> Table 3 ⁇ / u> TCA content (ng / l) Before treatment 5.9 After treatment 0.4
- a fluidized bed reactor having a volume of about 8 liters was used.
- the reactor (1) was then filled with the device of the Fig. 1 , which does not include the elements (9) and (10), with these 100 g. wet cork granules.
- the granules were treated with a stream of dry carbon dioxide gas without co-solvent, flowing at a rate of 75 l / min, at a temperature of 97.5 ° C for 4 hours, at atmospheric pressure.
- the granules were allowed to warm to room temperature as in Example 1 for 45 minutes and then re-contacted with air.
- TCA levels are summarized in Table 4 below. ⁇ u> Table 4 ⁇ / u> TCA content (ng / l) Before treatment 5.9 After treatment 0.8
- a fluidized bed reactor having a volume of about 8 liters was used.
- the reactor (1) was filled with the device of the Fig. 1 with 100 g. of cork granules and closed with flat filters (3 ') and (3 ").
- cork granules were treated with a stream of circulating carbon dioxide gas at a rate of 75 l / min, and mixed with 0.8 liter of a 50/50 mixture by weight of demineralized water and water. ethanol, at a temperature of 98.5 ° C for 4 hours, at atmospheric pressure.
- the granules were allowed to warm to room temperature as in Example 1 for 45 minutes and then re-contacted with air.
- a fluidized bed reactor having a volume of about 8 liters was used.
- the reactor (1) was filled with the device of the Fig. 1 with 100 g. of cork granules and closed with flat filters (3 ') and (3 ").
- the granules were treated with a flow of nitrogen circulating at a rate of 75 l / min, and mixed with 0.8 liter of water, at a temperature of 100 ° C for 4 hours, at atmospheric pressure.
- the granules were allowed to warm to room temperature in the presence of nitrogen.
- TCA levels are summarized in Table 6 below. ⁇ u> Table 6 ⁇ / u> TCA content (ng / l) Before treatment 5.9 After treatment 0.4
- TCA levels are summarized in Table 7 below. ⁇ u> Table 7 ⁇ / u> TCA content (ng / l) Before treatment 5.9 After treatment 0.4
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
- Jellies, Jams, And Syrups (AREA)
- Paper (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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FR0757143A FR2920107B1 (fr) | 2007-08-23 | 2007-08-23 | Procede de traitement de liege ou d'un materiau a base de liege avec un gaz inerte sous une pression strictement inferieure a 1 mpa |
Publications (2)
Publication Number | Publication Date |
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EP2033751A1 true EP2033751A1 (de) | 2009-03-11 |
EP2033751B1 EP2033751B1 (de) | 2012-02-01 |
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EP07116628A Active EP2033751B1 (de) | 2007-08-23 | 2007-09-18 | Verfahren zur Behandlung von Kork oder eines Materials auf Korkbasis mit einem Inertgas unter einem Druck, der strikt unter 1 MPa liegt |
Country Status (5)
Country | Link |
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EP (1) | EP2033751B1 (de) |
AT (1) | ATE543618T1 (de) |
ES (1) | ES2383438T3 (de) |
FR (1) | FR2920107B1 (de) |
PT (1) | PT2033751E (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES2385607A1 (es) * | 2010-12-29 | 2012-07-27 | Asociación De Investigación De La Industria Agroalimentaria | Procedimiento para la adecuación organoléptica y alimentaria del corcho. |
EP2639025A1 (de) | 2012-03-13 | 2013-09-18 | Universidad de Salamanca | Verfahren und Vorrichtung zur Entfernung von Haloanisolen und Halophenolen aus Kork |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES2457098B2 (es) * | 2014-02-27 | 2014-10-02 | José Luis Godoy Varo | Procedimiento, dispositivo e instalación para la inducción de respiración controlada mediante sensores químicos |
ES2639663B2 (es) * | 2016-04-27 | 2018-02-27 | Trefinos, S.L. | Procedimiento para el tratamiento del corcho |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2597778A1 (fr) * | 1986-04-28 | 1987-10-30 | Renz Raoul Guy | Procede de traitement de bouchons en liege |
WO2003041927A1 (en) * | 2001-11-12 | 2003-05-22 | Instituto Superior Técnico | New process for treating cork stoppers or planks for the reduction of strange aromas, namely 2,4,6-trichoroanisole |
US20030118745A1 (en) * | 2001-12-26 | 2003-06-26 | Anthony Vanlandeghem | Method for preparing the surface of synthetic cork material for printing |
-
2007
- 2007-08-23 FR FR0757143A patent/FR2920107B1/fr active Active
- 2007-09-18 PT PT07116628T patent/PT2033751E/pt unknown
- 2007-09-18 AT AT07116628T patent/ATE543618T1/de active
- 2007-09-18 ES ES07116628T patent/ES2383438T3/es active Active
- 2007-09-18 EP EP07116628A patent/EP2033751B1/de active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2597778A1 (fr) * | 1986-04-28 | 1987-10-30 | Renz Raoul Guy | Procede de traitement de bouchons en liege |
WO2003041927A1 (en) * | 2001-11-12 | 2003-05-22 | Instituto Superior Técnico | New process for treating cork stoppers or planks for the reduction of strange aromas, namely 2,4,6-trichoroanisole |
US20030118745A1 (en) * | 2001-12-26 | 2003-06-26 | Anthony Vanlandeghem | Method for preparing the surface of synthetic cork material for printing |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES2385607A1 (es) * | 2010-12-29 | 2012-07-27 | Asociación De Investigación De La Industria Agroalimentaria | Procedimiento para la adecuación organoléptica y alimentaria del corcho. |
EP2639025A1 (de) | 2012-03-13 | 2013-09-18 | Universidad de Salamanca | Verfahren und Vorrichtung zur Entfernung von Haloanisolen und Halophenolen aus Kork |
Also Published As
Publication number | Publication date |
---|---|
EP2033751B1 (de) | 2012-02-01 |
PT2033751E (pt) | 2012-05-09 |
ES2383438T3 (es) | 2012-06-21 |
FR2920107A1 (fr) | 2009-02-27 |
FR2920107B1 (fr) | 2013-08-23 |
ATE543618T1 (de) | 2012-02-15 |
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