EP2974841B1 - Procede de fabrication d'un panneau de fibres - Google Patents

Procede de fabrication d'un panneau de fibres Download PDF

Info

Publication number
EP2974841B1
EP2974841B1 EP15175533.7A EP15175533A EP2974841B1 EP 2974841 B1 EP2974841 B1 EP 2974841B1 EP 15175533 A EP15175533 A EP 15175533A EP 2974841 B1 EP2974841 B1 EP 2974841B1
Authority
EP
European Patent Office
Prior art keywords
acid
wood
lignocellulose
containing material
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.)
Active
Application number
EP15175533.7A
Other languages
German (de)
English (en)
Other versions
EP2974841A1 (fr
Inventor
Andreas Geyer
Thomas Schalkhammer
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.)
Fritz Egger GmbH and Co OG
Original Assignee
Fritz Egger GmbH and Co OG
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 Fritz Egger GmbH and Co OG filed Critical Fritz Egger GmbH and Co OG
Priority to PL15175533T priority Critical patent/PL2974841T3/pl
Publication of EP2974841A1 publication Critical patent/EP2974841A1/fr
Application granted granted Critical
Publication of EP2974841B1 publication Critical patent/EP2974841B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27NMANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
    • B27N1/00Pretreatment of moulding material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27NMANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
    • B27N1/00Pretreatment of moulding material
    • B27N1/006Pretreatment of moulding material for increasing resistance to swelling by humidity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27NMANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
    • B27N1/00Pretreatment of moulding material
    • B27N1/02Mixing the material with binding agent

Definitions

  • the invention relates to a method for producing a source-reduced fiber board.
  • Wood-based materials are used, for example, in construction as an insulating, constructive or cladding element as well as flooring.
  • Wood materials are made from wood shavings, wood chips or wood fibers as well as from sawn timber or veneers of various types of wood with the addition of natural and / or synthetic binders and other additives.
  • the properties of the wood are known to be significantly determined by the moisture content of the wood. As the absorption of water increases, as a rule the wood moisture increases, the strength and dimensional stability of the wood decrease, and the susceptibility to wood-destroying microorganisms increases.
  • the protruding fibers are then mechanically torn off, whereby the flooring has optically clear damage that leads to increased and accelerated wear. Furthermore, this behavior has a crucial importance in building materials.
  • swelling in addition to increased stress, an increased internal swelling pressure can arise, which counteracts the external mechanical load and also has an influence on the load capacity of the standing under continuous load wood construction.
  • Wood generally has as builders mainly cellulose, hemicelluloses and lignin. In the cell wall polymers free hydroxyl groups are found, which can make strong hydrogen bonds with water molecules, which hold the water molecules in the cells and thereby induce swelling.
  • Wood fibers are hydrophobized with wax dispersions for the production of modified wood materials. As a result, the thickness swelling and the water absorption rate of the wood materials produced with it should be delayed.
  • a reduction of the swellable fractions in the corresponding wood products is also a known strategy.
  • the DE 102 008 056 650 A1 proposed to wood fibers with wood extraneous components such as glass, metal, ceramic and / or plastics to produce wood-based materials.
  • non-swelling shares a delayed thickness swelling of the wood panels to be achieved.
  • the EP 1 762 671 B1 describes a building board, which has a reduced swelling and shrinkage behavior and on which a waterproof final layer of polyurethane, plastic or paint or mixtures thereof is applied.
  • the EP 2 181 818 A2 describes a process for the production of wood fiber materials and wood fiber materials from wood fibers, which are obtained after plasticization of wood and which should have a reduced emission of volatile organic compounds (VOC).
  • the wood fiber materials are prepared so that the uncut and / or comminuted wood is contacted with a formulation containing at least one compound to establish a neutral to basic pH and at least one complexing agent.
  • the EP 0 139 530 A3 describes a process for the preparation of lignocellulose-containing composites, films and the like with a di- or polyisocyanate based on a binder system in which a mineral acid is used.
  • a mineral acid HNO 3 , HCl, H 2 SO 4
  • PMDI gluing agent
  • the known methods have in common that a delay of the swelling is achieved by the coating and chemical modification. This is presumably due to the fact that a shielding, occupation or substitution of the free hydroxyl groups of the cell wall polymers is carried out and the hygroscopicity is lowered. In this way, presumably the interaction between water molecules and free hydroxyl groups of the cell wall polymers is reduced, thereby achieving a reduction in the swelling rate.
  • a disadvantage of the measures described above is that this only a delay of the absorption of water is achieved.
  • the chemical modification described above increases the weight of the wood material, which can be detrimental to processing and suitability as a building material.
  • the WO 2008/028183 A1 describes a process for producing a medium density fiberboard (MDF) wherein lignocellulosic fibers are pretreated with oxalic acid or oxalic acid derivatives prior to the refining step in a type of digester.
  • MDF medium density fiberboard
  • the DE 697 10 748 T2 describes in Example 2 a process for producing an MDF board in which wood chips are treated with dilute sulfuric acid for 6 minutes at a temperature of 184 ° C and a pressure of 10 bar.
  • a disadvantage of the treatment in Vorkocher is that due to the prevailing heat, the pressure and the high degree of dissociation of the acid, the wood fibers can be severely damaged. Under these hydrolysis conditions, the cellulose contained in the wood can easily be broken down. Not only can this result in a reduction in the quality of the fiber in general, but also the structure of the fiber can be so severely damaged that the fiber material can no longer be suitable for producing a fiberboard.
  • the invention has for its object to provide an effective, cost-effective method, with the source-reduced wood materials, especially a reduced source fiber board, standard processes used in the wood industry without increased time and cost can be produced.
  • the Er may be applied to a method for producing a reduced-source fiberboard by gluing lignocellulosic material, wherein the lignocellulosic material is treated prior to gluing with an acid, wherein the treatment is carried out at a temperature of 70 to 200 ° C and a pressure of 1 to 12 bar and wherein the acid is a Brönsted acid selected from the group consisting of phosphoric acid, phosphorous acid, hypophosphorous acid and mixtures thereof, and wherein the acid is an acid having a pKa of less than 4.
  • the inventive method for producing a reduced-source fiberboard provides that the lignocellulosic material is treated prior to gluing with an acid, wherein the treatment is carried out at a temperature of 70 to 200 ° C and a pressure of 1 to 12 bar.
  • the acid according to the invention is in particular a Bronsted acid selected from the group consisting of phosphoric acid, phosphorous acid, hypophosphorous acid and phosphonic acid.
  • the swelling capacity of fiberboard can be reduced in a particularly simple and cost-effective manner if the lignocellulose-containing material before gluing under the said pressure and temperature conditions with one of these acids and / or a mixture of the acid and its salts, esters or adducts (hereinafter "acid treatment").
  • acid treatment a mixture of the acid and its salts, esters or adducts
  • the addition of the acid to the precooker or digester takes place.
  • Particularly preferred is an addition before the refiner, in particular between the digester and refiner.
  • the addition of the acid may be e.g. in a feed or discharge screw that conveys the lignocellulosic material from the precooker / digester to the refiner.
  • water is partially or completely squeezed or removed between the digester and refiner steps.
  • the acid treatment is carried out on such a pressed or dehydrated lignocellulose-containing material.
  • Such a mixture of pressed lignocellulose-containing material and acid can then be fed to the refiner.
  • reducing the swelling capacity is believed to be due to elimination of the free-standing hydroxyl groups of the cell wall polymers mediated by the acid treatment, resulting in less interaction with the water molecules and resulting in hydrophobization of the material.
  • the acid treatment can be integrated in a simple manner into the usual processes in the wood industry for the production of fiberboard, i. Complex intermediate steps (e.g., drying) or process interruptions are not required.
  • acids used according to the invention for example phosphoric acid
  • the acids used according to the invention are available inexpensively and readily available.
  • Lignocellulosic material By “lignocellulosic material” is meant any type of material containing lignocellulose.
  • Lignocellulose according to the invention contains cellulose and / or hemicellulose and lignin.
  • Cellulose is an unbranched polysaccharide consisting of several hundred to ten thousand cellobiose units. These cellobiose units, in turn, consist of two molecules of glucose linked by a ⁇ -1,4-glucosidic bond.
  • Hemicellulose is a collective name for various components of plant cell walls.
  • the hemicelluloses are branched polysaccharides with a lower chain length - usually less than 500 sugar units - which are composed of different sugar monomers.
  • Hemicellulose is composed essentially of various sugar monomers such as glucose, xylose, arabinose, galactose and mannose, which sugars may have acetyl and methyl substituted groups. They have a random, amorphous structure and are readily hydrolyzable.
  • Xylose or arabinose consist for the most part Part of sugar monomers with five carbon atoms (pentoses).
  • Mannose or galactose consist mainly of sugar monomers with six carbon atoms (hexoses).
  • Ligans are amorphous, irregularly branched aromatic macromolecules, which occur in nature as part of cell walls and there cause the lignification (lignification) of the cell. They are composed of substituted phenylpropanol units, have a lipophilic character and are insoluble in room temperature in neutral solvents such as water. Precursors of lignin are, for example, p-coumaryl alcohol, coniferyl alcohol and sinapyl alcohol. The molecular weights of lignin are usually between 10,000 and 20,000 g / mol.
  • the lignocellulosic material may be in a frayed and / or unscreened state.
  • the lignocellulose-containing material is first added in undefiberated state (for example as wood chips) and then undergoes a defibering and / or comminution (for example in the refiner) in the course of the process.
  • undefiberated state for example as wood chips
  • defibering and / or comminution for example in the refiner
  • the treatment of the lignocellulosic material may be in both defibred, partially defibred, and / or uncorrugated state.
  • the acid treatment is preferably carried out on a lignocellulose-containing material which has a water content of from 30 to 400% by weight, in particular from 40 to 200% by weight, in particular from 50 to 150, based on the total weight of the lignocellulose-containing material.
  • lignocellulose-containing material which can be used according to the invention are wood particles, for example any form of finely divided wood material, ie in particular wood chips, wood chips, OSB strands, wood fibers and / or wood flour.
  • wood particles for example any form of finely divided wood material, ie in particular wood chips, wood chips, OSB strands, wood fibers and / or wood flour.
  • the wood particles especially if they are chips, fibers or strands, substantially or completely native wood.
  • substantially herein is meant up to 80, 85, 90, 95, 98, or 99 weight percent, based on the total weight of the lignocellulosic material. Chips, fibers and / or strands of native wood have proved to be particularly suitable.
  • the lignocellulosic material may be selected from the group consisting of finely divided wood material, wood fibers, wood shavings, and wood chips.
  • wood material is understood to mean a wide variety of materials that consist of wood or contain wood, examples of wood materials are wood boards, laminates, floor coverings, worktops, table tops, pallets and / or wood shaped parts, in particular composite materials of individual wood particles may be any of cellulose products such as wood particles, especially wood shavings, finely divided wood material, wood strands, wood fibers, wood chips and / or wood veneers.Wood materials disclosed herein are particularly those based on solid wood, veneer materials, chipboard, fiber materials, fiberboard or other composites.
  • the process disclosed herein is particularly well suited for the production of pressed wood materials, in particular for the production of fiberboard.
  • a fiberboard is for example a UDF, LDF, MDF, or HDF board into consideration.
  • the fiberboard, or the preliminary or intermediate product of the fiberboard consists essentially of lignocellulose-containing material.
  • essential here means up to 80, 85, 90, 95, 98 or 99 wt .-%, based on the Total weight of the wood material.
  • the fiberboard, or the precursor or intermediate contains further additives.
  • the lignocellulosic material which is treated with acid in the process of the present invention may be different.
  • the fiberboard can be produced, for example, by comminuting cellulose-containing materials and then joining the structural elements together.
  • the precursor or intermediate can be selected, for example, from the lignocellulose-containing starting material and / or the structural elements obtained by comminution, such as, for example, the wood particles, wood chips, wood strands, wood chips, wood fibers or wood veneers.
  • source-reduced fiberboard can be produced.
  • reduced swelling is meant a reduction in swelling compared to the untreated material.
  • swelling is meant the consequences of the contact of the wood fibers with water or water vapor. In particular, a wet swelling and / or a wet expansion can occur due to the contact with water. Swelling is understood to mean swelling capacity or thickness swelling.
  • the swelling capacity can be determined according to European standard EN 317 “Particleboard and fiberboard”.
  • Thickness swelling can be determined “after water storage” or ISO 24336 "Laminate floor coverings. Determination of thickness swelling after partial immersion in water”.
  • a reduction of the swelling by at least 10%, based on the untreated material is achieved by the inventive method.
  • the swelling can be determined according to EN 317 or ISO 24336.
  • the content of the acid is 0.1 to 15% by weight, preferably 0.1 to 10% by weight, in particular 0.1, 0.2, 0.5, 1, 2, 3, 5, 7, 9, 10 or 12% by weight, based on the dry matter (atro) of the lignocellulose-containing material.
  • the acid may be used in admixture with one of its salts, esters or adducts.
  • the term "acid” includes Bronsted acids and / or Lewis acids. Examples of usable Brönsted acids described herein are, for example, mineral acids. Acids which can be used according to the invention preferably have a pK s value of less than 4, preferably less than 3.5, 3, 2.75, 2.5, 2.3 or 2. The acid can be used alone or in combination with one of its salts, esters or adducts.
  • the Brönsted acids may be selected, for example, from the group consisting of phosphoric acid, phosphorous acid, hypophosphorous acid, phosphonic acid, sulfuric acid, sulfonic acid, p-toluenesulfonic acid, benzenesulfonic acid, sulfosuccinic acid, methylsulfonic acid, methylphosphonic acid and ethylphosphonic acid or mixtures thereof.
  • the acid is selected from phosphoric acid, phosphorous acid, hypophosphorous acid and phosphonic acid and mixtures thereof. Particular preference is given to using phosphoric acid, in particular ortho- phosphoric acid.
  • a treatment with a mixture of phosphoric acid and a salt of phosphoric acid has proved to be advantageous.
  • the salts may, for example, be alkali salts, alkaline earth salts and / or ammonium salts.
  • phosphoric acid phosphorous acid, hypophosphorous acid or mixtures thereof are used. Practical experiments have shown that this can reduce the risk of strongly acidic reactions with the lignocellulose-containing material and the concomitant reduction in quality of the lignocellulose-containing fiber or of the end product.
  • Another advantage lies that the phosphoric acid is less corrosive, so that the process equipment is less stressed.
  • Phosphoric acids in the context of this invention are those which have a free HO-P group.
  • Examples of phosphoric acids which can be used according to the invention are orthophosphoric acid, phosphonic acid and / or phosphinic acid.
  • phosphoric acid is especially ortho- phosphoric acid into consideration.
  • the phosphoric acid can be used as a 10 to 85 wt .-% solution in water. If the treatment with phosphoric acid is carried out in the refiner, it is preferable to use a 50 to 85% strength by weight solution in water, in particular a 70 to 85% strength by weight solution in water.
  • salts of ortho- phosphoric acid in particular phosphates, hydrogen phosphates and / or dihydrogen phosphates are meant.
  • the salts of phosphoric acid may be, for example, their alkali salts, alkaline earth salts and / or ammonium salts or compounds. Salts of phosphoric acid which can be used according to the invention are also phosphonates and / or phosphinates.
  • Alkyl esters are particularly suitable as the phosphoric acid esters, the alkyl chain length preferably being 1 to 12 carbon atoms, preferably 1 to 10 carbon atoms, particularly preferably 1 to 5 carbon atoms and very particularly preferably 1 to 3 carbon atoms.
  • the adducts of phosphoric acid may be, for example, di-, tri- or meta-phosphates.
  • Lewis acids described herein are, for example, boron trifluoride, boron chloride, aluminum trichloride, iron (III) chloride and / or zinc chloride.
  • the addition of the acid can be done at any point in the process prior to gluing or gluing.
  • a treatment in the preheater and / or in the digester has proved to be advantageous.
  • the treatment may take place under elevated pressure (with respect to atmospheric pressure) and / or under elevated temperature (with respect to room temperature).
  • the treatment normally takes place under normal pressure and / or at a temperature of up to 100 ° C.
  • a further embodiment according to the invention provides that the treatment takes place after the digester, in particular in the intermediate stage after the digester and before the refiner or in the refiner.
  • the treatment is carried out at a temperature of 70 to 200 ° C, in particular 160 to 200 ° C. In one embodiment, the treatment may be carried out at a temperature of 120 to 180 ° C. According to the invention, the treatment is carried out at a pressure of 1 to 12 bar, in particular 2 to 10 bar. In one embodiment, the treatment may be carried out at a pressure of 6 to 9 bar.
  • the duration of the treatment may be 0.01 to 15 minutes, especially 0.3 to 5 minutes.
  • the acid is added before and / or during the crushing process in the refiner.
  • the treatment of the lignocellulosic material with the acid in a conventional refiner in the industry is usually carried out at a process temperature of 160 to 200 ° C and / or a pressure of 2 to 10 bar, in particular from 5 to 9 bar.
  • Refiner is understood to mean the machine used in the wood industry, which is used for comminution, in particular for grinding of fibers.
  • suitable refiners are disc refiners, cone refiners or cylindrical refiners. Refiner are for example in the “ Taschenbuch der Holztechnik ", Wagen1.2 / Scholz, 2nd ed. 2012, p. 235 ff , described.
  • In the refiner wood particles are treated at a process temperature of 70 to 200 ° C, in particular at 120 to 180 ° C, and / or a pressure between 1 to 10 bar, in particular at 5 to 9 bar.
  • treating is meant the processing or contacting of the lignocellulosic material (or a precursor or intermediate thereof) with the acid under the conditions described.
  • the lignocellulosic material may be present in the treatment in un-fibered, shredded and / or partially defibred state.
  • the acid is added after the precooker or digester.
  • this addition of acid takes place before the refiner, more preferably the acid is added to the still hot, lignocellulosic material that has leaked from the digester.
  • This is particularly practical in a feed or discharge screw, which conveys the lignocellulosic material from the pre-cooker or digester to the refiner.
  • the acid may be added according to another embodiment in the refiner and / or between the digester and refiner.
  • cooker is understood to mean the machine commonly used in the wood industry, which is used to soften the wood chips under the effect of temperature and excess water.
  • the common wood chips preparation for MDF production by means of a cooker and subsequent refining step is described, for example, in US Pat. Holzwerkstoffe ", Soiné, DRW-Verlag 1995, chapter 1.2.2.6 s.
  • the greater the surface area of the lignocellulose-containing material to be treated i.e., the precursor or intermediate product of the wood material
  • the surface is known to increase with decreasing particle size.
  • a higher reaction rate is achieved if the lignocellulose-containing material to be treated has a small particle size.
  • the material to be treated is brought into contact with the acid with simultaneous comminution.
  • the acid treatment takes place during the comminution of the lignocellulose-containing material (for example in the refiner).
  • the lignocellulosic material undergoes the swelling-reducing treatment, a swelling reduction is ensured down to the core of the entire wood material with low cost and process complexity and within the running of the process chain.
  • the reaction of the acid, in particular the phosphoric acid, with the surface of the lignocellulosic material may begin with the introduction of the acid in the preheater or the digester or only between the digester and the refiner and in the refiner. Due to the thermomechanical conditions in the refiner, the distribution and / or the reaction is further accelerated. By discharging water in the dryer and / or the further thermally induced drying of the nonwoven fabric during plate formation in the press, the reaction can also be driven forward become. The final reaction is often complete only after the finished plate has cooled in the warehouse.
  • Another advantage of the method according to the invention is that the diffusion process takes place here within a few minutes.
  • a further advantage is the short treatment time in Voriserrmbetude, Vorkocher and / or refiner or in between. This is generally not longer than 15 minutes, preferably 0.01 to 10 minutes, particularly preferably 0.1 to 5 minutes, in particular 0.3 to 2 minutes.
  • the inventive method is compatible with current production processes of the wood industry. It can be used within an ongoing production without significantly changing the productivity of the equipment used.
  • step a) the lignocellulosic material to be processed is preheated to the desired temperature.
  • the lignocellulose-containing material is digested in the digester under elevated pressure and at elevated temperature.
  • steps a) and / or b) take place using an excess of water.
  • the proportion of water in the mixture of water and the lignocellulose-containing material in step a) and / or b) can be from 100 to 400% by weight, in particular from 150 to 300% by weight, based on the total weight of the lignocellulose-containing material.
  • the addition of the acid may occur in step a) and / or b). Due to the increased water content in step a) and / or b), the added acid is diluted again. This may be advantageous because, according to Ostwald's law of dilution, the degree of proteolysis increases with increasing dilution. This allows a particularly effective use of the acid used.
  • the reaction of the acid is further enhanced by the increased surface area of the fiberized lignocellulosic material and / or the elevated temperature and consequent pore opening of the fibers.
  • step a) and / or b) can be problematic since exact dosing is difficult due to the considerable and sometimes fluctuating dilution. It can easily happen that either too little acid is added or too much, which then causes the reaction of the acid with the lignocellulose-containing material to proceed so strongly that it suffers from the quality of the lignocellulose-containing material and thus also the quality of the end product. Due to the dilution effect of the water present, it may also happen that not enough acid penetrates into the lignocellulosic material, which is why in turn the treatment time in step a) and / or b) must be extended.
  • step c the lignocellulosic material is fed to the refiner (step c)).
  • This phase between the digester and the refiner is referred to herein as "intermediate step bc)". It has proven to be particularly practical if the acid treatment takes place in this intermediate step bc).
  • Step bc) involves the transfer of the lignocellulosic material from the digester to the refiner, but may also include other processes, in particular intermediate storage or further processing of the lignocellulose-containing material.
  • the defibrated lignocellulose-containing material obtained from step b) becomes the refiner used in step c) by means of a feed or discharge screw fed.
  • the still hot lignocellulosic material is carried out of the digester and transported in the direction of refiner. Since the previous step a) and / or b) has an increased water content, which is not desired in the following process steps, the water from the lignocellulose-containing material is usually at least partially pressed or removed in the intermediate transport step bc).
  • the lignocellulosic material After pressing, the lignocellulosic material typically has a water content of from 50 to 200% by weight, in particular from 75 to 150% by weight, based on the total weight of the lignocellulose-containing material.
  • the acid treatment is carried out after such pressing or removal of the water, which takes place after removal from the digester.
  • the lignocellulosic material still has an elevated temperature during transport from the precooker to the refiner. This has a positive effect on the acid treatment.
  • the addition of the acid is particularly preferably carried out in intermediate step bc).
  • the addition of the acid in intermediate step bc) can be carried out by initially squeezing or removing water completely or partially and then adding the acid.
  • the acid may be added after or during at least partial squeezing or removal of the water from the lignocellulosic material.
  • the treatment time with the acid in intermediate step bc) can be 0.1 seconds to 2 minutes, preferably from 0.5 seconds to 1 minute and particularly preferably from 1 second to 30 seconds.
  • the disadvantages, as they exist in the addition in step a) and / or b) can be largely avoided by the acid addition in intermediate step bc).
  • the acid is not diluted so much, which also ensures better dosage and the risk Uncontrolled reactions can be reduced.
  • the treatment time can be reduced, which can have a positive effect on the production costs.
  • the lignocellulosic material has an increased surface area and elevated temperature such that the pores of the lignocellulosic material are at least partially opened or widened, allowing the acid to more easily diffuse into the lignocellulosic material.
  • step bc) the acid is added in intermediate step bc) or step c) and thus can remain in the lignocellulose-containing material in the further process. If the acid is added in step a) and / or b), the acid is at least partially removed by the removal or removal of the water in step c) and can then no longer be available for the reaction.
  • the acid used is a Bronsted acid selected from the group consisting of phosphoric acid, phosphorous acid, hypophosphorous acid phosphonic acid and mixtures thereof in intermediate step bc) and / or step c).
  • the acid can be used in an amount of from 0.1 to 10% by weight, based on the lignocellulose-containing material (atro).
  • Phosphoric acid is particularly preferred according to the invention as the acid.
  • the phosphoric acid can be added in admixture with one of its salts, esters or adducts in intermediate step bc) and / or step c).
  • the lignocellulose-containing material (refiner) is comminuted.
  • the acid is before and / or during the crushing process added in the refiner.
  • the treatment of the lignocellulosic material with the acid in a conventional refiner in the industry is usually carried out at a process temperature of 160 to 200 ° C and / or a pressure of 2 to 10 bar, in particular from 5 to 9 bar. These conditions allow for rapid diffusion of the acid molecules into the core of the lignocellulosic material.
  • the acid treatment can be done in each step before gluing or gluing.
  • the treatment preferably takes place in at least one of the steps a), b), bc) and / or c).
  • the acid treatment may also be carried out before or after at least one of steps a), b), c) and d). Examples of this are the feeding of the acid in feed or Austragsschnecken which carry the lignocellulosic material.
  • the acid may be added directly to the preheater, precooker and / or refiner. Most preferably, the addition of the acid is between steps b) and c), i. in intermediate step bc), and / or during step c). In a preferred embodiment, the acid is added in step bc).
  • the acid used is a Bronsted acid which is selected from the group consisting of phosphoric acid, phosphorous acid, hypophosphorous acid and phosphonic acid and mixtures thereof.
  • the acid can be used in an amount of from 0.1 to 10% by weight, based on the lignocellulose-containing material (atro).
  • Phosphoric acid is particularly preferred according to the invention as the acid.
  • the phosphoric acid may be added in admixture with one of its salts, esters or adducts.
  • step e) the lignocellulose-containing material is glued with a binder.
  • Suitable binders are in particular a melamine and / or urea resin.
  • gluing it can be understood as wholly or partially wetting with a composition that contains a binder.
  • Such compositions are also referred to by the person skilled in the art as “glue liquor”.
  • Gluing can in particular also mean the uniform distribution of the binder-containing composition on the wood particles.
  • the application of the binder-containing composition can be carried out, for example, by impregnation or spraying, in particular in a blowline.
  • a blow-line connects to the refiner.
  • surface-modifying agents which neutralize the surface and / or encapsulate the fiber can optionally also be sprayed on in the blowline.
  • the amount of the binder used in the gluing or gluing is preferably 0.1 to 20 wt .-%, in particular 1.0 to 16 wt .-%, more preferably 4.0 to 14.0 wt .-%, based on the Wood dry weight (solid resin / atro). For many applications, it is particularly practical if the binder in an amount of 0.1 to 15 wt .-% based on the dry weight of wood (solid resin / atro) is used.
  • the application of the binder can be carried out, for example, in the blowline known to the person skilled in the art.
  • the method according to the invention is suitable for a multiplicity of binder-wood particle combinations.
  • binders which can be used according to the invention are aminoplasts, phenoplasts, vinyl acetates, isocyanates, epoxy resins and / or acrylic resins.
  • Particularly preferred binders are urea-formaldehyde resin (UF), melamine-formaldehyde resin, phenol-formaldehyde resin (PF), polyvinyl acetate and / or white glue.
  • the binder used for the gluing is a system based on urea-formaldehyde resins (UF), melamine-reinforced urea-formaldehyde resins (MUF), melamine-urea-phenol-formaldehyde resins (MUPF), Phenol-formaldehyde resins (PF), polymeric diisocyanates (PMDI) and / or isocyanates used.
  • the binder is an aminoplast resin.
  • the binder used in the process of the invention may further contain hardeners.
  • the curing can also be carried out by pressing the composite material under the action of heat.
  • a drying of the glued mixture containing the lignocellulose-containing material can be carried out between the gluing (step e) and the pressing (step g).
  • step g) the mixture containing the lignocellulose-containing material is finally pressed into a fiberboard.
  • a pressing temperature of at least about 150 ° C.
  • the glued wood particles are pressed in step g) into a wood chip material.
  • a wood chip material Preferably it is in step g) is a hot pressing.
  • the press factor during hot pressing is from 2 to 10 s / mm, preferably from 3 to 6 s / mm.
  • Press factor is understood to mean in particular the residence time of the lignocellulose-containing wood chip material in seconds per millimeter thickness or thickness of the finished pressed lignocellulose-containing wood chip material in the press.
  • Suitable temperatures for the compression in step g) of the process according to the invention or one of its embodiments are temperatures of 150 ° C to 250 ° C, preferably from 160 ° C to 240 ° C, particularly preferably from 180 ° C to 230 ° C. At temperatures in these ranges, the process can be carried out particularly economically.
  • Also described herein is a fiberboard obtainable by the method of the invention or one of its embodiments and by further processing the fiber board available laminate, a floor covering, a worktop, table top or pallet.
  • the wood chips arrive for hydrothermal pretreatment in a preheating, where they are "pre-steamed” together with 1 wt .-% ortho- phosphoric acid (based on the total amount of water and wood chips) at atmospheric pressure at a temperature of up to 100 ° C.
  • the partially plasticized and modified wood chips then pass through the vibration discharge floor and a screw conveyor in the digester.
  • the pitch of the helix decreases continuously, compressing the chips into a relatively pressure-tight plug. With this plug, the seal takes place to the stove.
  • the chips are "cooked” at a vapor pressure between 6 and 10 bar at 140 to 180 ° C.
  • the chips remain about 1 to 6 minutes before being fed by a screw conveyor (discharge screw) and via the feed screw into the refiner and pulverized into fibers at a vapor pressure of 6 to 10 bar.
  • a screw conveyor discharge screw
  • further hydrophobing agents as well as surface-modifying agents which neutralize the surface or encapsulate the fiber can be sprayed on in the blowline adjoining the refiner.
  • the glued fibers now enter the dryer and are dried to the desired residual moisture.
  • the fibers on a circumferential Forming band scattered and the height of the resulting fiber mat is adjusted by calibration rollers (scalper). After precompression, the endless fiber mat is pressed in a continuous hot press at 200 ° C and 30 bar for about 3 minutes to its desired thickness.
  • the wood fiberboard thus obtained has a significantly reduced thickness swelling.
  • the wood chips arrive for hydrothermal pretreatment in a Vorierrm actuallyer, where they are "pre-damped” at atmospheric pressure of a temperature of up to 100 ° C.
  • the partially plasticized and modified woodchips then pass through the vibration discharge floor and / or a screw conveyor in the digester.
  • the pitch of the helix decreases continuously, compressing the chips into a relatively pressure-tight plug. With this plug, the seal takes place to the stove.
  • the chips are "cooked” at a vapor pressure between 6 and 10 bar at 140 to 180 ° C.
  • the chips remain about 1 to 6 minutes before being fed by a screw conveyor (discharge screw) together with ortho- phosphoric acid in an amount of 10% by weight, based on the amount of the wood material, into the refiner and at be pulverized to fibers to a vapor pressure of 6 to 10 bar.
  • a screw conveyor discharge screw
  • ortho- phosphoric acid in an amount of 10% by weight, based on the amount of the wood material
  • further hydrophobing agents as well as surface-modifying agents which neutralize the surface or encapsulate the fiber can be sprayed on in the blowline adjoining the refiner.
  • the glued fibers now enter the dryer and are dried to the desired residual moisture.
  • the fibers are scattered on a rotating forming belt and the height of the resulting fiber mat is adjusted by calibration rollers (scalper). After precompression, the endless fiber mat is pressed in a continuous hot press at 200 ° C and 30 bar for about 3 minutes to its desired thickness.
  • the wood fiberboard thus obtained has a significantly reduced thickness swelling.
  • the wood fibers were subjected to a pulping process. For this wood chips were cooked in a pre-cooker. The wood fibers were fed from the precooker to the refiner by means of a discharge screw while pressing off water. Even before the wood fibers reached the refiner, phosphoric acid was added. The wood fibers thus obtained were examined for their swelling properties. For this purpose, in a beaker, wood fibers, both the reference fibers (0% phosphoric acid) and those treated with phosphoric acid, were weighed (weighed, EW) and covered with water so that they were completely covered. The proportion of phosphoric acid is given in Table 1 as wt .-% phosphoric acid based on the total weight of wood fibers (atro).
  • the swelling was calculated as follows: WAV REFERENCE - WAV sample * 100 / WAV REFERENCE

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Wood Science & Technology (AREA)
  • Forests & Forestry (AREA)
  • Dry Formation Of Fiberboard And The Like (AREA)
  • Paper (AREA)

Claims (12)

  1. Procédé de préparation d'un panneau de fibres à gonflement réduit par encollage d'un matériau lignocellulosique, où le matériau lignocellulosique est traité avec un acide avant l'encollage, où le traitement est réalisé à une température allant de 70 à 200°C et à une pression allant de 1 à 12 bar, où l'acide est un acide de Brönsted choisi parmi le groupe consistant en l'acide phosphorique, un acide phosphoreux, un acide hypophosphoreux et leurs mélanges, et où l'acide est un acide ayant un pKa inférieur à 4.
  2. Procédé selon la revendication 1, où l'acide est mis en oeuvre en une quantité allant de 0,1 à 10% en poids, sur base du matériau lignocellulosique (atro).
  3. Procédé selon l'une quelconque des revendications précédentes, où l'acide est mis en oeuvre en mélange avec un de ses sels, esters ou adduits.
  4. Procédé selon l'une quelconque des revendications précédentes, où l'on met en oeuvre comme acide, un acide ayant un pKa inférieur à 3 ou inférieur à 2,5.
  5. Procédé selon l'une quelconque des revendications précédentes, où le traitement est réalisé à une température allant de 120 à 180°C.
  6. Procédé selon l'une quelconque des revendications précédentes, où le traitement est réalisé à une pression allant de 6 à 9 bar.
  7. Procédé selon l'une quelconque des revendications précédentes, où la durée du traitement se situe dans l'intervalle allant de 0,01 à 15 minutes, en particulier de 0,3 à 5 minutes.
  8. Procédé selon l'une quelconque des revendications précédentes, où le traitement est réalisé au cours d'une étape intermédiaire après le cuiseur et avant le raffineur.
  9. Procédé selon l'une quelconque des revendications précédentes, où le matériau lignocellulosique est présent à l'état défibré ou non défibré.
  10. Procédé selon l'une quelconque des revendications précédentes, où le matériau lignocellulosique est choisi parmi le groupe consistant en du bois finement divisé, des fibres de bois, de la sciure de bois et des copeaux de bois.
  11. Procédé selon l'une quelconque des revendications précédentes, où le procédé comprend au moins les étapes suivantes :
    a) préchauffage du matériau lignocellulosique dans un récipient de préchauffage ;
    b) décomposition du matériau lignocellulosique dans un cuiseur ;
    c) broyage du matériau lignocellulosique dans un raffineur ;
    d) traitement du matériau lignocellulosique par un acide à l'étape a), b) et/ou c) et/ou entre l'étape b) et l'étape c) ;
    e) encollage du matériau lignocellulosique avec un liant ;
    f) le cas échéant : séchage du mélange contenant le matériau lignocellulosique ;
    g) compression du mélange contenant le matériau lignocellulosique en un panneau de fibres.
  12. Procédé selon l'une quelconque des revendications précédentes, où le panneau de fibres est un panneau UDF, LDF, MDF ou HDF.
EP15175533.7A 2014-07-04 2015-07-06 Procede de fabrication d'un panneau de fibres Active EP2974841B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL15175533T PL2974841T3 (pl) 2014-07-04 2015-07-06 Sposób wytwarzania płyty pilśniowej

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102014009884.2A DE102014009884A1 (de) 2014-07-04 2014-07-04 Verfahren zur Herstellung einer Faserplatte

Publications (2)

Publication Number Publication Date
EP2974841A1 EP2974841A1 (fr) 2016-01-20
EP2974841B1 true EP2974841B1 (fr) 2019-01-09

Family

ID=53525107

Family Applications (1)

Application Number Title Priority Date Filing Date
EP15175533.7A Active EP2974841B1 (fr) 2014-07-04 2015-07-06 Procede de fabrication d'un panneau de fibres

Country Status (7)

Country Link
EP (1) EP2974841B1 (fr)
DE (1) DE102014009884A1 (fr)
ES (1) ES2710393T3 (fr)
HU (1) HUE042921T2 (fr)
PL (1) PL2974841T3 (fr)
PT (1) PT2974841T (fr)
TR (1) TR201901611T4 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102016100078B3 (de) * 2016-01-04 2017-04-13 Fritz Egger Gmbh & Co. Og Faserplatte mit erhöhter Beständigkeit gegen Pilzbefall sowie Verfahren zu deren Herstellung
CN109366677B (zh) * 2018-10-18 2021-03-05 陕西森尚建材科技有限公司 一种环保型生态植物纤维板及其制备方法

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60101004A (ja) * 1983-10-19 1985-06-05 アトランテイツク・リツチフイールド・カンパニー リグノセルロース系複合成形品の製造方法
EP0934362B1 (fr) * 1996-10-18 2002-02-27 Kronospan GmbH Traitement de matiere lignocellulosique
EP1716995B1 (fr) * 2005-04-22 2009-02-25 Georg-August-Universität Göttingen Produit à base d'acides gras et de dérivés paraffiniques pour la protection des matériaux lignocellulosiques
DE102005042658B3 (de) 2005-09-08 2007-03-01 Kronotec Ag Bauplatte, insbesondere Fußbodenpaneel
DE102006029313A1 (de) 2006-06-23 2007-12-27 Sasol Wax Gmbh Wachsdispersion aus ölhaltigen Weichwachsen, Verwendung von Weichwachsen als Hydrophobierungsmittel in Holzwerkstoffen und Verfahren zur Einbringung von Weichwachsen in Holzwerkstoffe
US20080264588A1 (en) * 2006-09-01 2008-10-30 Masood Akhtar Method of Making Medium Density Fiberboard
EP2181818A3 (fr) * 2008-10-28 2012-08-22 IHD Institut für Holztechnologie Dresden gGmbH Procédé de fabrication de matières premières en fibres de bois et matières premières en fibres de bois ayant des émissions réduites en VOC volatiles
DE102008056650A1 (de) 2008-11-10 2010-05-12 Martin Dreisman Zusammensetzung und Verfahren zur Herstellung einer Holz- oder Holzfaserplatte

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Also Published As

Publication number Publication date
HUE042921T2 (hu) 2019-07-29
PL2974841T3 (pl) 2019-05-31
DE102014009884A1 (de) 2016-01-07
TR201901611T4 (tr) 2019-02-21
EP2974841A1 (fr) 2016-01-20
ES2710393T3 (es) 2019-04-24
PT2974841T (pt) 2019-02-13

Similar Documents

Publication Publication Date Title
DE60009165T2 (de) Herstellung von hochwertigen produkten aus abfällen
EP3178622B1 (fr) Procédé de fabrication d'une plaque en matériau dérivé du bois présentant une émission réduit de composés organiques volatiles (cov)
DE69813010T2 (de) Verfahren zur herstellung von verbundwerkstoff-gegenständen aus zellulose
EP0697941B2 (fr) Procede de recuperation de copeaux et de fibres par desagregation de residus de materiaux derives du bois, de vieux meubles, de residus de production, de dechets et d'autres materiaux contenant des materiaux derives du bois
DE69710748T2 (de) Behandlung von lignocellulosematerialien
EP2974841B1 (fr) Procede de fabrication d'un panneau de fibres
EP1780243B2 (fr) Composition de liant pour matériaux à base de bois
WO2007071387A2 (fr) Fibre vegetale, element moule a base de fibres et procede de production de fibres vegetales dotees de novolak
EP2094456B1 (fr) Panneau de fibres et son procédé de fabrication
DE4327774A1 (de) Verfahren zur Herstellung von mitteldichten Holzfaserplatten (MDF)
EP2355965B1 (fr) Composition et procédé de fabrication d'un panneau de bois ou d'un panneau de fibres de bois
EP3268190B1 (fr) Procédé de fabrication d'un matériau à base de particules de bois et durcisseur employé dans ledit matériau pour aminoplaste
DE102007054123B4 (de) Verfahren zur Herstellung von Holzfaserplatten mit verringerter Formaldehydemission, hoher Feuchtebeständigkeit und Hydrolyseresistenz der Verleimung
EP3733366B1 (fr) Liant destiné à la fabrication de matériaux dérivé du bois
EP3733367B1 (fr) Matériaux dérivés du bois et compositions de liant
DE102008050428A1 (de) Verfahren zur Herstellung von mitteldichten Faserplatten (MDF) mit alkalisch härtenden Phenolformaldehydharzen
DE2744425C2 (de) Trockenverfahren zur Herstellung von Faserformkörpern aus gegenüber Stammholzmaterial unterschiedlichem pflanzlichem lignocellulosehaltigem Material, sowie Einrichtung zur Durchführung dieses Verfahren
EP2853648B1 (fr) Utilisation de particules de cuir dans des plaques en matériau bois pour la réduction des émissions de composés organiques volatiles (COV)
EP3837098B1 (fr) Matériau
EP4122662B1 (fr) Procédé de fabrication de panneau fibreux à émission réduite de cov
EP3383605B1 (fr) Panneau de fibres à résistance accrue contre toute attaque fongique, et procédé de fabrication
WO2023143963A1 (fr) Procédé de fabrication d'un panneau de fibres
DE19958756A1 (de) Verfahren zur Herstellung von mitteldichten Faserplatten (MDF)
AT526970A1 (de) Verfahren zur Herstellung eines Verbundwerkstoffs
EP3733368A1 (fr) Liant destiné à la fabrication de matériaux dérivé du bois

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

AX Request for extension of the european patent

Extension state: BA ME

17P Request for examination filed

Effective date: 20160720

RBV Designated contracting states (corrected)

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: GRANT OF PATENT IS INTENDED

RIC1 Information provided on ipc code assigned before grant

Ipc: B27N 1/00 20060101AFI20180627BHEP

Ipc: B27N 1/02 20060101ALN20180627BHEP

INTG Intention to grant announced

Effective date: 20180718

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE PATENT HAS BEEN GRANTED

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

Ref country code: AT

Ref legal event code: REF

Ref document number: 1086735

Country of ref document: AT

Kind code of ref document: T

Effective date: 20190115

REG Reference to a national code

Ref country code: CH

Ref legal event code: NV

Representative=s name: HEPP WENGER RYFFEL AG, CH

REG Reference to a national code

Ref country code: RO

Ref legal event code: EPE

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: LANGUAGE OF EP DOCUMENT: GERMAN

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 502015007578

Country of ref document: DE

REG Reference to a national code

Ref country code: PT

Ref legal event code: SC4A

Ref document number: 2974841

Country of ref document: PT

Date of ref document: 20190213

Kind code of ref document: T

Free format text: AVAILABILITY OF NATIONAL TRANSLATION

Effective date: 20190206

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2710393

Country of ref document: ES

Kind code of ref document: T3

Effective date: 20190424

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20190109

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

REG Reference to a national code

Ref country code: HU

Ref legal event code: AG4A

Ref document number: E042921

Country of ref document: HU

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190409

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190509

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190409

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190410

REG Reference to a national code

Ref country code: CH

Ref legal event code: NV

Representative=s name: SCHMAUDER AND PARTNER AG PATENT- UND MARKENANW, CH

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 502015007578

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

26N No opposition filed

Effective date: 20191010

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190109

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IT

Payment date: 20230726

Year of fee payment: 9

Ref country code: ES

Payment date: 20230825

Year of fee payment: 9

Ref country code: CH

Payment date: 20230801

Year of fee payment: 9

Ref country code: AT

Payment date: 20230726

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: PL

Payment date: 20230704

Year of fee payment: 9

Ref country code: HU

Payment date: 20230602

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: RO

Payment date: 20240625

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: PT

Payment date: 20240620

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: LU

Payment date: 20240723

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: TR

Payment date: 20240613

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20240723

Year of fee payment: 10

Ref country code: IE

Payment date: 20240724

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20240723

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: BE

Payment date: 20240723

Year of fee payment: 10

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20240723

Year of fee payment: 10