EP3900902A1 - Mineralisierung von holz oder holzwerkstoff unter verwendung von calciumacetat - Google Patents

Mineralisierung von holz oder holzwerkstoff unter verwendung von calciumacetat Download PDF

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Publication number
EP3900902A1
EP3900902A1 EP21169977.2A EP21169977A EP3900902A1 EP 3900902 A1 EP3900902 A1 EP 3900902A1 EP 21169977 A EP21169977 A EP 21169977A EP 3900902 A1 EP3900902 A1 EP 3900902A1
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EP
European Patent Office
Prior art keywords
wood
wooden material
impregnation
range
drying
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EP21169977.2A
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English (en)
French (fr)
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EP3900902B1 (de
Inventor
Thomas Volkmer
Tom Franke
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Impraegnierwerk Ag Willisau
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Impraegnierwerk Ag Willisau
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
    • B27K3/02—Processes; Apparatus
    • B27K3/0207—Pretreatment of wood before impregnation
    • B27K3/0214—Drying
    • 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
    • B27K3/02—Processes; Apparatus
    • B27K3/0278—Processes; Apparatus involving an additional treatment during or after impregnation
    • B27K3/0292—Processes; Apparatus involving an additional treatment during or after impregnation for improving fixation
    • 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
    • B27K3/36—Aliphatic compounds
    • 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
    • B27K2240/30—Fireproofing

Definitions

  • the invention relates to a method for producing a mineralized wood or mineralized wooden material. More particularly, the invention relates to mineralized wood and wooden material suitable for indoor and outdoor use and methods for making such materials.
  • fire resistance of wood or wooden material is of high importance. Accordingly, different processes have been developed to render wood or wooden material more fire resistant. These processes rely on substances which result in delayed ignition, reduced heat release rate and slower spread of flames. They act on different levels, most of the time combined: promotion of char formation at lower temperature than wood usually degrades, free-radicals trapping in the flame, dilution of combustible gases coming from wood with non-combustible gases, reduction of heat content of the volatile gases, or coating protection of the wood surface. The most commonly used fire retardants for wood products are inorganic salts, of which some can absorb moisture promoting decay and destruction of metal joints.
  • a further disadvantage of wood or wooden materials containing additives to increase fire resistance are the adverse effects of the additives, such as salt deposits, on subsequent steps involving further processing of the wood or wooden material.
  • processing of wood or wooden material containing such additives with a circular saw may lead to corrosion on the circular saw or other instruments involved in processing of the wood or wooden material as a result of the additives, including salt deposits.
  • certain process for increasing fire resistance and/or for protecting the wood employ toxic components or precursors. which may be transformed into toxic compounds upon exposure to extreme temperatures.
  • the general objective of the present invention to advance the state of the art with respect to wood protection.
  • the disadvantages of the prior art are overcome fully or partly.
  • an environmentally friendly and non-toxic method to improve the fire resistance of wood and wooden materials is provided.
  • This new method ideally also minimizes undesired swelling of the wood or wooden material upon treatment.
  • the new method would ideally lead to minimal changes in the coloration of the wood or wooden material, including after subsequent surface coating using common surface coating agents such as linseed oil.
  • toxic components and/or the generation of toxic compounds, particularly under extreme temperatures such as in a fire are avoided.
  • the invention aims at providing a method for the protection of wood and wooden materials by mineralization. This method relies on water soluble reactants penetrating the material in a stepwise fashion and reacting with each other to form water insoluble salts. These salts, often present in crystalline form, are generated in situ within the cells themselves, in the cell walls, in the pits and in the middle lamellas.
  • a further purpose of this invention is to provide mineralized products, i.e. wood or wooden material, in such a way as to allow their intended functions while also providing one or more of the following properties or functions: i) improving fire resistance, (ii) reducing flammability, (iii) minimizing weight gain upon treatment, (iv) minimizing change in coloration and color structure upon mineralization, including after subsequent surface coating of the (minarlized) wood or wooden material, (v) minimizing swelling upon exposure to humidity.
  • the general objective is achieved in a first aspect of the invention by a method comprising (i) a first impregnation step, comprising a first impregnation of wood or wooden material with an aqueous solution of potassium oxalate, (ii) a first drying step, comprising drying of the wood or wooden material, (iii) a second impregnation step, comprising a second impregnation of wood or wooden material with an aqueous solution of calcium acetate, (iv) and a second drying step, comprising drying of the wood or wooden material.
  • a first impregnation step comprising a first impregnation of wood or wooden material with an aqueous solution of potassium oxalate
  • a first drying step comprising drying of the wood or wooden material
  • a second impregnation step comprising a second impregnation of wood or wooden material with an aqueous solution of calcium acetate
  • a second drying step comprising drying of the wood or
  • halogen ions such as chloride or bromide may under extreme temperatures, i.e. under fire exposure generate toxic gases such as HCl or HBr. Therefore, the inventive method provides wood or wooden material which is safer. Additionally, calcium acetate can be used as an aqueous solution and therefore its handling is easier and safer than handling of gaseous materials. Furthermore, the generated calcium oxalate significantly improves the fire resistance of the mineralized wood or wooden material.
  • drying may be achieved by exposing the impregnated wood or wooden material to increased temperatures, for example by using hot air or an oven. Alternatively, drying may be achieved by maintaining the wood or wooden material at ambient temperature until a certain water content is reached. Additionally, or alternatively, drying may be achieved by application of an underpressure, i.e. applying a vacuum.
  • impregnation may be achieved by any suitable method, such as dipping, particularly under pressure, spraying or spreading. However, preferably, impregnation is achieved by filling an autoclave with wood or wooden material and the corresponding solution and applying a pressure. Typically, the first and second impregnation are separate impregnation steps. The intermediate drying step makes the second impregnation step significantly more efficient.
  • the concentration of potassium oxalate dissolved in the solution lies in the range of 20%-100%, preferably 90%-100% of its saturation concentration.
  • the concentration of calcium acetate dissolved in the solution may lie in the range of 1 5-90%, preferably 65-90% of its saturation concentration.
  • the saturation concentration is the maximum possibly quantity of a substance that can dissolve in the solvent, i.e. in water.
  • concentration has been found beneficial, as a calcium acetate solution with a concentration below the saturation concentration penetrates the wood or wooden material faster and deeper, i.e. the impregnation is more effective.
  • the concentration is high enough to enable sufficient generation of calcium oxalate.
  • the first and/or the second impregnation comprises a phase of overpressure during which the pressure is selected in the range of 5-10x10 5 Pa (5-10 bar), preferably 8 bar, and the temperature is selected to be in the range of 15-50 °C, preferably in the range of 15-25 °C, more preferably 20 °C.
  • the duration of the phase of overpressure in the first and/or the second impregnation step is ⁇ 1 hour, typically 1-24 h, preferably 2-8 h.
  • the first and/or the second impregnation is preceded by a vacuum phase, during which the wood or wooden material is exposed to underpressure, preferably of 1-3x10 4 Pa (100-300 mbar), preferably for 30 minutes, preferably at 20 to 60 °C.
  • underpressure refers to a pressure below atmospheric pressure, preferably to a pressure of up to 300 mbar.
  • the wood or wooden material is dried to the fiber saturation level of 20%-30%, preferably 20%-25%, more preferably 20% in the first drying step.
  • the fiber saturation level denotes the level in the drying process at which only water bound in the cell walls remains, while all other water has been removed. Drying below the fiber saturation level results in shrinkage.
  • the first and/or second drying step comprises a vacuum phase, during which the wood or wooden material is exposed to underpressure, preferably for a time period lying in the range of 30 minutes to 4 hours, more preferably 45 minutes to 3 hours, preferably at a temperature of 20-70 °C, more preferably 30-60 °C, and preferably at an underpressure of 1-3x10 4 Pa (100-300 mbar), more preferably 100-150 mbar.
  • the wood or wooden material is dried to a wood moisture of 612%, preferably 8% in the second drying step.
  • a second aspect of the invention comprises wood or wooden material which is mineralized in a method according to any of the embodiments described herein, which is characterized in that it comprises calcium oxalate deposits and is essentially free of chloride deposits, such as potassium chloride, calcium chloride or the like.
  • Essentially free of potassium chloride means that the content of chloride ions of the total salt content in the wood or wooden material is below 5%, i.e. below 1%, i.e. below 0.1 %, i.e. below 0.01 %, preferably 0%.
  • wood or wooden material which is mineralized according to the present invention contains potassium acetate deposits.
  • the molar ratio of the potassium acetate deposits and the calcium oxalate deposits is in the range of 1.5:1 to 3:1, preferably 2:1.
  • the content of calcium oxalate in the wood or wooden material which is mineralized in a method according to the present invention lies in the range of 10-20 weight percent, preferably 13-16 weight percent, more preferably 1 5-16 weight percent.
  • the wood or wooden material comprises European oak, beech or maple, mixtures thereof or consists thereof.
  • oak is used as wood or wooden material for the mineralization method described herein, wherein the content of calcium oxalate in the mineralized wood lies in the range of 12-17 weight percent, preferably 15-16 weight percent.
  • the critical heat flux as determined according to ISO 9239-1 (version of 2010-11), exceeds 10.5 kW/m 2 for mineralized oak, wherein the content of calcium oxalate lies in the range of 12-17 weight percent, preferably 15-16 weight percent.
  • the burning distance as determined according to ISO 9239-1 (version of 2010-11), lies between 100 mm and 10 mm, preferably between 30 mm and 20 mm, for mineralized oak, wherein the content of calcium oxalate lies in the range of 12-17 weight percent, preferably 15-16 weight percent.
  • the tangential swelling coefficient at 20 °C and in the presence of 65% relative humidity lies in the range of 1%-3%, preferably 2.0%-2.6%, more preferably 2.2% and 2.4%, for mineralized oak, wherein the content of calcium oxalate lies in the range of 12-17 weight percent, preferably 15-16 weight percent.
  • beech is used as wood or wooden material for the mineralization method described herein.
  • maple is used as wood or wooden material for the mineralization method described herein.
  • the mineralization with calcium oxalate is based on two separate impregnation steps.
  • the material is impregnated in an aqueous solution with potassium oxalate (C 2 O 4 K 2 ).
  • the material is dried and then impregnated with calcium acetate (Ca(CH 3 COO) 2 .).
  • the potassium oxalate already present in the material to be mineralized and the calcium acetate form calcium oxalate ⁇ CaC 2 O 4 ⁇ solid , which is practically not soluble in water, and potassium acetate as by product.
  • a molar ratio of 1:1.12 of potassium oxalate/calcium acetate was employed.
  • the molecular weight of K 2 C 2 O 4 ⁇ 6H 2 0 is 184.23 g/mol, the water solubility 38.7 g/100g H 2 O.
  • the molecular weight of Ca(CH 3 COO) 2 is 158.166 g/mol, the water solubility 34.7 g/100g in H 2 O at 20°C.
  • the potassium oxalate solution was prepared by dissolving 360 g Potassium oxalate hydrate in 1l H 2 0 and the calcium acetate solution was prepared by dissolving 309 g calcium acetate monohydrate in 1l H 2 O.
  • Calcium acetate in its anhydrous form, is a white solid at room temperature. It is a hygroscopic compound and forms solutions in water dissociating in calcium and acetate ions. It is commercially available in anhydrous and hydrous form as Ca(CH 3 COO) 2 ⁇ H 2 O. The properties will evidently depend on its hydration degree. For the tests performed calcium acetate monohydrate was employed.
  • calcium acetate and its aqueous solutions may be considered as harmless. Indeed, calcium acetate is commonly employed as food additive (E 263). Calcium acetate is therefore suited for wood impregnation and does not pose a significant danger in the event that the impregnated wood or wooden material displays residual calcium acetate.
  • Potassium oxalate is a salt of oxalic acid and is commercially available as a colorless solid. In aqueous solutions it can dissociate to form oxalate and potassium ions. Oxalate ions can be combined with calcium, magnesium, and iron ions to form less soluble or insoluble salts. Potassium oxalate is commercially available in anhydrous form or as its monohydrate. In the current experiments, the monohydrate (K 2 C 2 O 4 -H 2 0) was used. Once the oxalate anion has reacted with the cation from the calcium acetate solution, it forms a heavy soluble salt (CaC 2 O 4 ) that is retained in wood or wooden material, providing the protection effect.
  • aC 2 O 4 heavy soluble salt
  • the three hard-wood species commonly used as decorative wood for interior applications are European oak ( Quercus spp. ) , beech ( Fagus sylvatica ) and maple ( Acer spp.). They are representative species of European hardwood and grow across European countries.
  • the woods preferably used in the method according to the invention include: European oak, beech and maple.
  • European oak Quercus spp. is a hardwood belonging to the division of angiosperms. As it is characteristic for hardwoods, oak is composed by vessel elements, fibers (tracheids), parenchyma and ray cells. Vessels are arranged in a ring porous structure. Density varies from 0.43 - 0.69 - 0.96 g/cm 3 . Characteristic for oak is a high amount of water extractives (up to 12%) including a high amount of tannins. European oak heartwood ( Quercus spp. ) is classified as heavily treatable. Treatability is the ease with which a wood can be penetrated by a liquid.
  • Maple is a hardwood belonging to the division of angiosperms. As it is characteristic for hardwoods, maple is composed by vessel elements, fibers (tracheids), parenchyma and ray cells. Vessels are arranged in a non-specific pattern, resulting in a semi-porous to diffuse porous distribution. The density of maple varies from 0.53 - 0.63 - 0.79 g/cm 3 . Maple ( Acer spp. ) is classified as easily treatable.
  • the samples are placed vertically into the holding device and the burner is installed in front of the sample tilted 45°.
  • the distance of the burner from the unprotected edge of the sample is 16mm.
  • the flame has a length of 20mm.
  • the wood or wooden material obtained from mineralization may be characterized by different parameters, including the following:
  • MEE moisture excluding efficiency
  • the fiber saturation level is defined as the moisture content of wood which is determined at a theoretical relative humidity of 100%.
  • the fiber saturation point represents the wood moisture content at which the cell wall cannot increase its moisture content any further.
  • the wood moisture content is defined as the current amount of water in the wood based on the absolute dry weight of the wood.
  • the absolute dry weight of the wood (abbreviated as abs. dry) is defined as the mass which occurs after drying the wood at 103 °C until weight constancy. Weight constancy is defined as a weight change less than 0.1 % in 6 hours.
  • Moisture Content weight wood ⁇ at the current moisture conte nt ⁇ ⁇ weight abso ⁇ lute dry ⁇ weight absolute dry
  • the wood equilibrium moisture content is defined as the moisture content which occurs if the wood is exposed under stable temperature and relative humidity.
  • the parameters described above were determined for oak ( Quercuss spp .) mineralized according to the process described above (see process steps of mineralisation at an industrial level).
  • thermogravimetric analysis 245 °C
  • Critical heat flux as determined according to DIN EN ISO 9239-1 (version of 2010-11): 11.0 kW/m 2 in product direction and 11.0 kW/m 2 in direction perpendicular to the first direction
  • the mineralized oak was subjected to a modified ISO norm 11925-2 test, where the specimens were conditioned at 20 °C and 65% relative humidity instead of 23 °C and 50 % relative humidity involving exposure to an ignition source for 30 seconds. The time of burning after elimination of the ignition source was determined to be 0 seconds, as reproduced with 5 specimens).
  • the burning distance of the mineralized beech is 220 mm (length) and 160 mm (perpendicular).
  • maple Acer spp. mineralized according to the process described above (see process steps of mineralisation at an industrial level).
  • the critical heat flux of the mineralized maple is 10.0 kW/m 2 (length) and 10.5 kW/m 2 (perpendicular), as determined according to ISO 9239-1 (version of 2010-11).
  • the burning distance of the mineralized maple is 200 mm (length) and 150 mm (perpendicular).
  • a further advantage of the mineralized wood or wooden material obtained from the mineralization method outlined above is that the mineralized wood or wooden material displays remarkable color fastness.
  • the untreated wood or wooden material hardly differs from the mineralized wood or wooden material in either color or color structure.
  • mineralized wood or wooden material, particularly oak, that has been subjected to subsequent surface coating using common surface coating agents such as linseed oil also hardly differs from the respective untreated wood or wooden material in either color or color structure.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Forests & Forestry (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
EP21169977.2A 2020-04-23 2021-04-22 Mineralisierung von holz oder holzwerkstoff unter verwendung von calciumacetat Active EP3900902B1 (de)

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EP3900902B1 EP3900902B1 (de) 2024-04-17

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB244178A (en) * 1924-09-12 1925-12-14 Novocrete And Cement Products Improvements in or relating to the induration or mineralization of organic matter
NO118316B (de) * 1967-10-12 1969-12-08 Sutton Res Corp
WO2018065335A2 (en) * 2016-10-03 2018-04-12 Berner Fachhochschule - Biel Architektur, Holz Und Bau Mineralizing of wood and cellulosic materials

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB244178A (en) * 1924-09-12 1925-12-14 Novocrete And Cement Products Improvements in or relating to the induration or mineralization of organic matter
NO118316B (de) * 1967-10-12 1969-12-08 Sutton Res Corp
WO2018065335A2 (en) * 2016-10-03 2018-04-12 Berner Fachhochschule - Biel Architektur, Holz Und Bau Mineralizing of wood and cellulosic materials

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
KRAMB JASON ET AL: "Modeling of the catalytic effects of potassium and calcium on spruce wood gasification in CO2", FUEL PROCESSING TECHNOLOGY, ELSEVIER BV, NL, vol. 148, 1 March 2016 (2016-03-01), pages 50 - 59, XP029519221, ISSN: 0378-3820, DOI: 10.1016/J.FUPROC.2016.01.031 *

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