Moisture-regulating composition and support material containing the moisture-regulating composition

Abstract

The moisture regulation composition comprises 20 to 60 weight percent, on a total dry weight basis, of at least one metal-organic framework compound and 80 to 40 weight percent, on a total dry weight basis, of at least one binder material.

Description

[Technical Field]

[0001] The present invention relates to a moisture-regulating composition for regulating the relative humidity in a desired enclosed environment, or for regulating the moisture content of a product, or for regulating the relative humidity inside a package.

[0002] The present invention also relates to a support material containing a moisture-regulating composition.

[0003] The present invention further relates to a method for obtaining a support material provided together with a moisture-regulating composition. [Background technology]

[0004] Many products are manufactured or packaged with a certain level of moisture content, but these products tend to absorb moisture from the environment over time. Moisture absorption impairs the properties of the product. The sensory and physical properties of the product also deteriorate with increasing moisture content. [Overview of the Initiative]

[0005] Many products maintain their freshness, or the perception of freshness, at a desirable level of moisture content. To maintain freshness, many products should be stored under desirable relative humidity conditions.

[0006] Therefore, in order to maintain the quality of the product until its final use, it is necessary to keep the moisture content of the product at a specific level.

[0007] To optimize product characteristics until final use, it is necessary to control the moisture content of the product throughout its entire lifecycle, including shipping, distribution, storage, and product use. Maintaining product quality is essential to preserve the consumer experience and satisfaction.

[0008] For example, for products contained within a package, it is desirable to control the moisture content of the product before opening, during use, and even down to the last remaining unit of product in the package.

[0009] Numerous different packaging solutions have been proposed that provide different barrier materials to reduce moisture adsorption and achieve a desirable shelf life.

[0010] On the other hand, it is also necessary to avoid excessive drying of the product within the packaging, which would also impair the product's characteristics.

[0011] In a first aspect, the present invention provides a moisture-regulating composition comprising at least one metal-organic structural compound in a weight of 20 to 60 percent by total dry weight and at least one binder material in a weight of 80 to 40 percent by total dry weight.

[0012] A moisture-regulating composition is provided. The moisture-regulating composition of the present invention adsorbs water within a defined range of relative humidity.

[0013] In a second aspect, the present invention provides a moisture-regulating solution comprising a moisture-regulating composition comprising 20 to 60 weight percent by total dry weight of at least one metal-organic structure compound and 80 to 40 weight percent by total dry weight of at least one binder material, and a solvent in such an amount that the at least one metal-organic structure forms about 5 to about 40 percent of the total volume of the moisture-regulating solution.

[0014] A moisture-regulating solution is provided. The moisture-regulating solution of the present invention adsorbs water within a defined range of relative humidity.

[0015] In a third aspect of the present invention, the present invention provides a support material including a support material or a plastic support material, and a moisture-regulating composition comprising at least one metal-organic structural compound in a weight of 20 to 60 percent by total dry weight and at least one binder material in a weight of 80 to 40 percent by total dry weight.

[0016] The support material allows the moisture content of products positioned near the support material to be kept within a predetermined range.

[0017] According to a fourth aspect, a method is provided for preparing a support material containing a moisture-regulating composition comprising 20 to 60 weight percent by total dry weight of at least one metal-organic structural compound and 80 to 40 weight percent by total dry weight of at least one binder material, the method comprising the following steps: The process of providing support material, A step of providing an impregnation bath containing a moisture-regulating solution comprising a moisture-regulating composition comprising at least one metal-organic structural compound in a total dry weight of 20 to 60 percent and at least one binder material in a total dry weight of 80 to 40 percent, and a solvent, The process involves immersing the support material in the impregnation bath until it is impregnated with the solution in the impregnation bath, The method includes a step of drying a support material to evaporate a solvent from the support material in order to obtain a support material comprising at least one metal-organic structure that exhibits a moisture content that is in equilibrium with a vapor-water mixture characterized by a relative humidity of about 0 to 25 percent according to the corresponding sorption isotherm of at least one metal-organic structure at a temperature of 23 degrees Celsius and a pressure of 1 atmosphere.

[0018] A fifth aspect of the present invention provides a method for preparing a support material containing a moisture-regulating composition comprising 20 to 60 weight percent by total dry weight of at least one metal-organic structural compound and 80 to 40 weight percent by total dry weight of at least one binder material, the method comprising the following steps: The process of providing support material, Providing an impregnation bath containing a moisture control solution having a moisture control composition comprising at least one metal-organic framework compound of 20 to 60 weight percent based on the total dry weight and at least one binder material of 80 to 40 weight percent based on the total dry weight, and a solvent Immersing the support material into the impregnation bath until the support material is impregnated with the solution of the impregnation bath Drying the support material to evaporate the solvent therefrom so as to obtain a support material comprising at least one metal-organic framework presenting a moisture content consisting of about 0 weight percent to 25 weight percent based on the anhydrous weight of the at least one metal-organic framework

[0019] Therefore, a suitable support material can be obtained for regulating the moisture content of the product or for regulating the relative humidity of a closed environment

[0020] The moisture control composition, the moisture control solution, and the support material may be used to control the moisture content of the product and to maintain the moisture content of the product within a defined range. Thus, it is possible to maintain the quality of the product

[0021] The moisture control composition makes it possible to maintain the relative humidity within a closed environment, such as a package, within a predefined range

[0022] The moisture control composition and the moisture control solution may be used to maintain the relative humidity within a package within a defined range. Thus, it is possible to maintain the moisture content of the product packed within the package within a desired range. Thus, it is possible to maintain the quality of the product

[0023] For some products, the customer has a poor experience either when the water content of the product increases above a certain level or when the moisture content is too low. Thanks to the moisture control composition of the present invention, it is possible to maintain the moisture content of the product within a predefined range and thus to optimize the sensory stimulation characteristics of the product and the experience of the product for the consumer

[0024] By appropriately selecting the weight percentage of at least one metal-organic structure and at least one binder in the moisture-regulating composition, it is possible to adjust the moisture content of the support material or the product to a desired range.

[0025] By appropriately selecting at least one type of metal-organic structure, at least one type of binder, or both, within the moisture-regulating composition, it is possible to adjust the moisture content of a product located near a support material to a desired range.

[0026] Therefore, an undesirable increase in moisture content within the product, exceeding the desired range, is avoided.

[0027] Therefore, conversely, an undesirable decrease in the product's moisture content, falling below the desired range, is avoided.

[0028] Therefore, product deterioration is avoided, and product quality is maintained.

[0029] Similarly, by appropriately selecting the type or weight percentage of the metal-organic structure in the moisture-regulating composition, or the type or weight percentage of at least one binder, it is possible to adjust the relative humidity inside the package to a desired range.

[0030] Therefore, it is possible to obtain a package configured to maintain the relative humidity inside the package within a predetermined range. The resulting package is configured to maintain the moisture content of the product packed inside the package within a predetermined range.

[0031] The moisture-regulating composition adsorbs water within a defined relative humidity range, which is referred to below as the adsorption range. In other words, the moisture-regulating composition adsorbs water within a defined range of relative humidity, which spans from the approximate minimum threshold of relative humidity to the approximate maximum threshold of relative humidity.

[0032] The relative humidity range in which a moisture-regulating composition adsorbs water depends on the metal-organic structure(s) and / or binder(s) used within the moisture-regulating composition.

[0033] The moisture-regulating composition adsorbs only a limited amount of water below the minimum threshold of relative humidity. The moisture-regulating composition adsorbs only a limited amount of water above the maximum threshold of relative humidity.

[0034] The moisture-regulating composition adsorbs a considerable amount of water within its adsorption range, i.e., within the range of relative humidity from the minimum threshold to the maximum threshold. By selecting the type of metal-organic structure(s) and binder(s), the minimum and maximum thresholds of relative humidity are adjusted, and therefore the relative humidity values ​​within the adsorption range are adjusted.

[0035] Therefore, it is possible to adjust the moisture content of the product.

[0036] By selecting the type of metal-organic structure(s) and binder(s), it is possible to obtain a moisture-regulating composition that is tuned to adsorb a specific amount of water and water within a specific minimum and maximum threshold of relative humidity.

[0037] Therefore, by selecting the type of metal-organic structure(s) and binder(s), and using a desirable ratio of at least one metal-organic structure and at least one binder, it is possible to obtain a moisture-controlling composition characterized by the S-shape of an sorption isotherm that conforms to a desirable range of relative humidity in which the moisture-controlling composition substantially absorbs water.

[0038] By selecting the type of metal-organic structure(s) and binder(s), the relative humidity range in which the moisture-regulating composition substantially adsorbs water can be adjusted.

[0039] Therefore, by selecting the type of metal-organic structure(s) and binder(s), the moisture content of the support material containing the moisture-regulating composition, the relative humidity inside the package containing the moisture-regulating composition, or the moisture content of the product packed inside the package containing the moisture-regulating composition can be adjusted.

[0040] It is possible to control the moisture content of the product within the package, both before opening, during use, and down to the last remaining unit of product in the package. It is also possible to control the product's moisture content under conditions of varying environmental relative humidity.

[0041] Furthermore, it is possible to avoid excessive drying and excessive wetting of the product within the package.

[0042] By selecting at least one metal-organic structure(s) and one or more binders(s), it is possible to obtain a suitable moisture-regulating composition for a particular product and to maintain the moisture content of the product at a desired level.

[0043] Within the adsorption range, the moisture-regulating composition adsorbs water with an efficiency that depends on the metal-organic structure(s) used and the binder(s) used.

[0044] Within the adsorption range, the amount of water adsorbed by the moisture-regulating composition depends on the metal-organic structure(s) used and the binder(s) used.

[0045] At a defined temperature, the adsorption behavior of a compound is represented by a curve called an sorption isotherm, which shows the change in the percentage of adsorbed / desorbed water relative to the percentage of equilibrium relative humidity. The sorption isotherm is obtained at a specific temperature and pressure and shows the percentage of water adsorbed / desorbed by the moisture-controlling composition as a function of the percentage of equilibrium relative humidity.

[0046] The sorption isotherms of the moisture-regulating compositions have a curve that resembles a sigmoid pathway, i.e., an "S" shape.

[0047] The sorption isotherm of the moisture-regulating composition has a first portion consisting of zero relative humidity to a minimum threshold relative humidity. In the first portion, the moisture-regulating composition adsorbs a small amount of water, and the adsorbed water gradually increases depending on the relative humidity. The amount of adsorbed water depends on the metal-organic structure(s) and binder(s) used in the moisture-regulating composition. The value of the minimum threshold relative humidity depends on the metal-organic structure(s) and binder(s) used in the moisture-regulating composition.

[0048] The sorption isotherm of the moisture-regulating composition has a second portion consisting of a maximum threshold relative humidity range of approximately 100 percent relative humidity. In this second portion, the moisture-regulating composition adsorbs a small amount of water, and the amount of adsorbed water gradually increases depending on the relative humidity. The amount of adsorbed water depends on the metal-organic structure(s) and binder(s) used in the moisture-regulating composition. The value of the maximum threshold relative humidity also depends on the metal-organic structure(s) and binder(s) used in the moisture-regulating composition.

[0049] The sorption isotherm of the moisture-regulating composition further includes an adsorption portion comprising a minimum threshold relative humidity to a maximum threshold relative humidity. In the adsorption portion, the moisture-regulating composition adsorbs a greater amount of water than the first or second portion. In the adsorption portion, the amount of water adsorbed increases significantly depending on the relative humidity. The amount of water adsorbed depends on the metal-organic structure(s) and binder(s) used in the moisture-regulating composition.

[0050] The minimum threshold for relative humidity may be about 15–45 percent at a temperature of about 23 degrees Celsius and a pressure of 1 atmosphere. Preferably, the minimum threshold for relative humidity may be about 20–40 percent at a temperature of about 23 degrees Celsius and a pressure of 1 atmosphere.

[0051] The maximum threshold relative humidity may be about 25 to 70 percent at a temperature of about 23 degrees Celsius and a pressure of 1 atmosphere. Preferably, the maximum threshold relative humidity may be about 30 to 55 percent at a temperature of about 23 degrees Celsius and a pressure of 1 atmosphere.

[0052] The water adsorbed at the adsorption site may consist of, for example, about 5 to about 105 percent, and is expressed as the ratio of grams of water to grams of metal-organic structures (or multiple structures) with respect to the weight of the metal-organic structures (or multiple structures).

[0053] Metal-organic structures are highly efficient compounds for adsorbing water.

[0054] At least one metal-organic structure is aluminum fumarate (C 12 H6Al2O 12 ) is also acceptable.

[0055] At least one metal-organostructure may be selected from the group of chromium terephthalate metal-organostructures MIL-101(Cr), which comprises a trimer chromium(III) octahedral cluster interconnected by 1,4-benzenedicarboxylic acid and having the empirical formula [Cr3(O)X(bdc)3(H2O)2], where bdc is benzene-1,4-dicarboxylic acid and X is OH or F. In one version, the metal-organostructure MIL-101(Cr) has the general formula (Cr3O(OH)(H2O)2(bdc)3).

[0056] At least one metal-organic structure may be selected from the group of functionalized chromium terephthalate metal-organic structures, MIL-101(Cr)-X, where X represents an electron-withdrawing group (NO2, SO3H, or Cl) or an electron-donating group (NH2, or CH3).

[0057] At least one metal-organic structure may be selected from the group of amino-functionalized chromium terephthalate metal-organic structures, MIL-101(Cr)-NO2.

[0058] At least one metal-organic structure may be selected from the group of iron terephthalate metal-organic structures, MIL-101(Fe).

[0059] At least one metal-organic structure may be selected from the group of chromium-based metal-organic structures on which the soc topology Cr-soc-metal-organic-structure-1 of the chemical formula [Cr3(μ3-O)(H2O)2(TCPT)1.5Cl] is based, where TCPT is a tetratopic 3,3”,5,5”-tetrakis(4-carboxyphenyl)-p-terphenyl ligand.

[0060] At least one metal-organic structure may be selected from the group of isostructural Zr(IV)-MOFs having a rare low-symmetry 9-bonded Zr6 cluster MOF, represented as Zr(IV)-MOFs BUT-46F, BUT-46A, BUT-46W, and BUT-46B, preferably Zr(IV)-MOFs BUT-46A.

[0061] At least one metal-organic structure may be selected from the group of hybrid microporous highly bonded rare-earth metal-organic structures Y-shp-MOF-5, where "shp" refers to a square hexagonal prism.

[0062] The moisture-regulating composition may contain multiple metal-organic structure compounds selected from any one of the groups shown above.

[0063] The moisture-regulating composition or moisture-regulating solution may contain aluminum fumarate and Mil-101(Cr).

[0064] The moisture-regulating composition or moisture-regulating solution may contain aluminum fumarate and Mil-101(Fe).

[0065] The moisture-regulating composition or moisture-regulating solution may contain, based on the total weight of the metal-organic structural compounds, about 50 weight percent aluminum fumarate and about 50 weight percent Mil-101(Fe).

[0066] It is understood that any other possible metal-organic structure may be used in the moisture regulating composition or in the moisture regulating solution.

[0067] By selecting a suitable metal-organic structure(s), it is possible to adsorb water within a desired adsorption range and maintain the moisture content at a desired level.

[0068] At least one binder is a water-soluble carrier for improving the solubilization of at least one metal-organic structure.

[0069] The provision of the binder makes it possible to improve the adsorption effect. Furthermore, the presence of the binder increases the binding of the moisture regulating composition to a desired support material.

[0070] The binder improves the binding of at least one metal-organic structure on a support material or on a packaging material. The binder enables water to reach at least one metal-organic structure so as to enhance the adsorption of water from at least one metal-organic structure. The binder also avoids the adsorption ability of at least one metal-organic structure from being impaired.

[0071] At least one binder of the moisture regulating composition or the moisture regulating solution is starch ((C6H 10 O5)n-(H2O)), carboxymethyl cellulose (CMC, C6H7O2(OH)2CH2COONa), alginic acid ((C6H8O6)n), alginate, copolymer of polyacrylic acid ((C3H4O2)n), copolymer of methacrylic acid (C4H6O2), polymer and / or copolymer of maleic acid (HO2CCH=CHCO2H), polyaspartic acid ((C4H5NO3)n), hydroxyethyl cellulose (C 29 H 52 O 21 ), hydroxypropyl cellulose (C 36 H 70 O 19 ), polyvinyl alcohol (C2H 4O)x), polyvinyl alcohol-co-ethylene (EVOH, C4H8O), polyvinyl alcohol-co-vinyl acetate, polyethylene oxide ((-CH2CH2O-)n), and polyethylene oxide-co-propylene oxide may be selected from the group consisting of these.

[0072] The moisture-regulating composition or moisture-regulating solution may contain multiple binders, for example, a combination of the compounds shown above.

[0073] Providing a binder makes it possible to improve the application of at least one metal-organic structure on a support material.

[0074] At least one binder may be a water-soluble carrier for improving the solubilization of at least one metal-organic structure.

[0075] At least one binder in the moisture-regulating composition or moisture-regulating solution may be potato starch.

[0076] It is understood that any other possible binders may be used in the moisture-modulating composition or in the moisture-modulating solution.

[0077] The moisture-regulating composition may also contain aluminum fumarate and potato starch.

[0078] The moisture-regulating composition may also contain MIL-101(Cr) and potato starch.

[0079] The amount of solvent in the moisture-regulating solution is adjusted to dilute the moisture-regulating composition so that at least one metal-organic structure and at least one binder can be mixed and dispersed.

[0080] The amount of solvent in the moisture-regulating solution is adjusted to obtain a solution with a viscosity range suitable for application by coating or impregnating the support material with it.

[0081] The moisture-regulating solution may contain water as a solvent for dissolving the moisture-regulating composition in the solution.

[0082] Different solvents can also be used in the moisture-adjusting solution of the present invention.

[0083] The solvent is compatible with at least one binder and at least one metal-organic structure so as to effectively dissolve at least one binder and at least one metal-organic structure.

[0084] In some versions, the moisture-regulating solution contains at least one binder and multiple solvents for dissolving at least one metal-organic structure.

[0085] The moisture-regulating solution is advantageous in that it contains at least one metal-organic structure (or more) in an amount of approximately 5 percent to 35 percent of the total volume of the moisture-regulating solution.

[0086] In a moisture-regulating solution, at least one metal-organic structure may constitute approximately 10 percent to 30 percent of the total volume of the moisture-regulating solution.

[0087] In a moisture-regulating solution, at least one metal-organic structure may form about 15 percent to about 25 percent of the total volume of the moisture-regulating solution.

[0088] In one version, the moisture-regulating solution contains water as the solvent and is about 20 to 40 percent of the total volume of the moisture-regulating solution of aluminum fumarate as the metal-organic structure. Preferably, the moisture-regulating solution contains about 25 to 35 percent of the total volume of the moisture-regulating solution of aluminum fumarate, and most preferably, about 32 percent of the total volume of the moisture-regulating solution of aluminum fumarate.

[0089] Support materials may be used to package products in a way that maintains the product's moisture content within a predetermined range.

[0090] The support material may be used to obtain a package that allows the relative humidity inside the package and the moisture content of the product packaged inside the package to be maintained within a predetermined range. The support material may be used to obtain any component of the package. The support material of the present invention may be used to obtain different types of packages.

[0091] The support material may be packaging material used to obtain the desired product packaging.

[0092] The support material may be used to obtain packaging for tobacco-containing products.

[0093] The support material may be used to obtain packaging for heated, non-combustible tobacco-containing products.

[0094] The supporting material may include fibrous materials.

[0095] The support material may include plastic material.

[0096] The support material may be selected from the group including paper, cardboard, cloth, textiles, nonwoven materials, polymers, polymer foams, and polymer films.

[0097] The type of support material may be selected depending on the resulting package.

[0098] It is understood that other types of support materials containing moisture-regulating compositions may be used.

[0099] The supporting material may be paper having a basis weight range of approximately 20 to 200 grams per square meter.

[0100] The supporting material may be cardboard having a basis weight of approximately 180 to 300 grams per square meter.

[0101] The support material may contain a moisture-regulating composition in an amount of approximately 20 to 300 grams per square meter.

[0102] The support material may be a foamed support material. The foamed support material may be prepared from, for example, a biopolymer such as starch, protein, or cellulose.

[0103] To prepare the foamed support material, a moisture-regulating composition and at least one additional modifier are provided to be added to the support material. For example, wood pulp fibers, a starch plasticizer such as glycerol, and water may be added to the support material as modifiers.

[0104] Next, steam foaming is performed to induce the formation of a foamed support material.

[0105] Subsequently, hot press molding or steam-based extrusion molding is performed to obtain the foam material in the desired form.

[0106] A foamed support material with a density ranging from approximately 10,000 to approximately 900,000 grams per cubic meter can be obtained.

[0107] The support material may contain one or more metal-organic structures in an amount ranging from approximately 0.30 grams (±20%) to approximately 5.00 grams (±20%).

[0108] The support material may contain one or more metal-organic structures in an amount ranging from approximately 0.50 grams (±20%) to approximately 2.50 grams (±20%).

[0109] The support material may contain one or more metal-organic structures in an amount ranging from approximately 0.75 grams (±20%) to approximately 1.50 grams (±20%).

[0110] In one embodiment, the support material includes at least 1.00 gram (±20%) of a metal-organic structure(s).

[0111] The amount of metal-organic structure(s) depends on the amount of product encased in the support material, or product made by mixing the support material, and the amount of product in the resulting package.

[0112] Advantageously, the support material includes, within the package obtained by having the support material, at least one or more metal-organic structures in an amount such that the weight ratio between the support material and the product packaged within the package is 1:6 to 1:2.

[0113] Advantageously, the support material includes at least one metal-organic structure(s) in such an amount that the weight of at least one metal-organic structure(s) in the package obtained with the support material is approximately 10 percent to approximately 50 percent of the weight of the product packaged in the package.

[0114] The support material may contain approximately 1.00 gram (±20%) of aluminum fumarate.

[0115] The support material may contain approximately 1.00 gram (±20%) of MIL-101(Cr).

[0116] The support material may contain approximately 1.00 gram (±20%) of MIL-101(Fe).

[0117] The support material may contain approximately 0.50 grams (±20%) of MIL-101(Cr) and approximately 0.50 grams (±20%) of aluminum fumarate.

[0118] These amounts of moisture-regulating composition in the support enable the relative humidity to be maintained within a predetermined range, for example, in the case of cigarette packaging and the packaging of heated, non-combustible tobacco products. These amounts of moisture-regulating composition enable efficient adsorption of water.

[0119] The support material includes a moisture-regulating composition having a relative weight ratio of metal-organic structure to binder consisting of 1:4 to 3:2.

[0120] These ratios enable efficient water adsorption and allow for efficient maintenance of relative humidity within a desired range.

[0121] The support material may be impregnated with a moisture-regulating composition. A wet impregnation process or a dry impregnation process may be used.

[0122] A dry impregnation process that charges powder particles of at least one metal-organic structure based on the use of an alternating electric field for applying a moisture-regulating composition to a support material allows the at least one metal-organic structure to be deposited on all types of porous support materials, including nonwovens, textiles, paper, and foams.

[0123] The dry impregnation method makes it possible to impregnate a moisture-regulating composition in powder form into a support material.

[0124] Dry impregnation may be carried out, for example, by a high-intensity alternating electric field. Any other dry impregnation method known in the art and suitable for the support material at the time of use may be used.

[0125] Any wet impregnation method known in the field and suitable for the support material at the time of use may also be used. Impregnating the support material with a moisture-regulating composition allows for the dispersion of the moisture-regulating composition throughout the entire thickness of the support material.

[0126] The support material may include a coating layer containing a moisture-regulating composition.

[0127] The support material may comprise multiple coating layers containing a moisture-regulating composition.

[0128] The coating layer may be formed by a moisture-regulating composition.

[0129] The support material may be coated with a moisture-regulating composition that forms a coating layer on the support material. The coating layer may be formed using any method and apparatus known in the art, for example, any method of surface coating.

[0130] In this way, one surface of the support material adsorbs water in a very efficient manner.

[0131] The support material may be provided with two different coating layers containing a moisture-regulating composition, which is provided on opposing sides of the support material such that the support material is interposed between the two coating layers.

[0132] The support material may comprise a layer of at least one moisture-regulating composition having a thickness of about 10 micrometers to about 80 micrometers, preferably about 15 micrometers to 70 micrometers, and more preferably about 20 micrometers to about 60 micrometers.

[0133] The support material may be packaging material used as a packaging element of the package.

[0134] In this way, there is no need to modify the form or design of the package in order to obtain a package that adjusts the moisture content of the product it contains.

[0135] The package may comprise at least one packaging element made of a support material containing a moisture-regulating composition.

[0136] The package may comprise multiple packaging elements made of a support material containing a moisture-regulating composition.

[0137] Additionally, a support material containing the moisture-regulating composition may be added to the package, for example, by being inserted into the package.

[0138] The package preferably contains a quantity of metal-organic structure(s) ranging from approximately 0.30 to approximately 5.00 grams. More preferably, the package contains a quantity of metal-organic structure(s) ranging from approximately 0.50 to approximately 2.50 grams. The package may also contain a quantity of metal-organic structure(s) ranging from approximately 0.75 to approximately 1.50 grams.

[0139] Advantageously, the package includes at least one metal-organic structure(s) in an amount such that the weight ratio between the metal-organic structure(s) and the product packaged within the package is between 1:6 and 1:2.

[0140] Advantageously, the package comprises a quantity of metal-organic structures such that the amount of metal-organic structures(s) is at least 10 percent to 50 percent of the weight of the product packaged within the package.

[0141] The package may contain approximately 1.00 gram (±20%) of aluminum fumarate.

[0142] The package may contain approximately 1.00 gram (±20%) of MIL-101(Cr).

[0143] The package may contain approximately 1.00 gram (±20%) of MIL-101(Fe).

[0144] The package may contain approximately 0.50 grams of MIL-101(Cr) and approximately 0.50 grams (±20%) of aluminum fumarate.

[0145] The packaging may be for tobacco products or nicotine-containing products.

[0146] Products whose moisture content is regulated may be any type of product for which it is desirable to maintain a moisture content level within a predetermined range. Products whose moisture content is regulated may be any type of product for which the moisture content level is related to the product's characteristics.

[0147] Advantageously, the product has a desirable level of moisture content, consisting of about 1% to about 15% by weight, preferably about 1.5% to 10% by weight.

[0148] The product may be a "heated, non-combustible" product, a cigarette, or any type of tobacco-containing product.

[0149] The impregnation bath containing the moisture-regulating composition comprises at least one metal-organic structural compound in a weight of 20 to 60 percent by total dry weight, at least one binder material in a weight of 80 to 40 percent by total dry weight, and a solvent. The impregnation bath may further contain water as a dissolving agent.

[0150] By immersing the support material in the impregnation bath, the support material is impregnated with the solution of the impregnation bath. Thanks to the composition of the impregnation bath, after drying, it is possible to obtain a support material having at least one metal-organic structure in an area of ​​approximately 30 grams per square meter to approximately 300 grams per square meter.

[0151] The support material may be immersed in the impregnation bath solution until it is saturated with the impregnation bath.

[0152] After immersing the support material in the impregnation bath solution, the method allows the impregnated support material to be fed to a weighing roll to remove excess solution from the support material and then dry the support material.

[0153] In the drying process, the support material may be dried to obtain a support material comprising at least one metal-organic structure that exhibits a moisture content that is in equilibrium with a gas-water mixture characterized by a relative humidity of about 0 to 20 percent according to the corresponding sorption isotherm of at least one metal-organic structure at a temperature of 23 degrees Celsius and a pressure of 1 atmosphere.

[0154] In the drying process, the support material may be dried to obtain a support material comprising at least one metal-organic structure that exhibits a moisture content that is in equilibrium with a gas-water mixture characterized by a relative humidity of about 0 to 10 percent according to the corresponding sorption isotherm of at least one metal-organic structure at a temperature of 23 degrees Celsius and a pressure of 1 atmosphere.

[0155] In the drying process, the support material may be dried to obtain a support material comprising at least one metal-organic structure that exhibits a moisture content that is in equilibrium with a gas-water mixture characterized by a relative humidity of about 0 to 5 percent according to the corresponding sorption isotherm of at least one metal-organic structure at a temperature of 23 degrees Celsius and a pressure of 1 atmosphere.

[0156] The support material is dried to obtain a support material having a moisture content that, at a temperature of 23 degrees Celsius and a pressure of 1 atmosphere, is in equilibrium with a gas-water mixture having a relative humidity lower than the minimum threshold of the relative humidity of the sorption isotherm of at least one metal-organic structure.

[0157] In the drying process, the support material is dried to evaporate the solvent from the support material so that the support material comprises at least one metal-organic structure having a water content of about 0% to 20% by weight based on the water-free weight of at least one metal-organic structure.

[0158] In the drying process, the support material is dried to evaporate the solvent from the support material so that the support material comprises at least one metal-organic structure having a water content of about 0% to 10% by weight based on the water-free weight of at least one metal-organic structure.

[0159] In the drying process, the support material is dried to evaporate the solvent from the support material so that the support material comprises at least one metal-organic structure having a water content of about 0% to 5% by weight based on the water-free weight of at least one metal-organic structure.

[0160] The support material can be a web of material that is continuously supplied to the impregnation bath.

[0161] The support material can be a sheet of material supplied to the impregnation bath.

[0162] The preparation of the support material containing the moisture-regulating composition may be carried out using other methods known in the art.

[0163] The support material containing the moisture-regulating composition may be obtained by any available technique known in the art.

[0164] Adsorption, as used herein, refers to the adhesion of atoms, ions, or molecules from a gas, liquid, or dissolved solid to a surface. This process creates a film of adsorbate on the surface of the adsorbent. Absorption means the process by which a fluid (the substance to be absorbed) is dissolved by or permeates a liquid or solid (the absorbent), respectively. The term sorption encompasses both processes.

[0165] In this specification, the term "adsorption" is used to describe both "adsorption" and "absorption" processes. Similarly, in this specification, the term "adsorb" is used to describe both "adsorb" and "absorb" processes.

[0166] In this specification, the definition of "adsorption isotherm" refers to the "moisture sorption isotherm," that is, the relationship between the water content of a material in equilibrium and the equilibrium relative humidity. For each relative humidity value, the adsorption isotherm shows the corresponding water content value at a given constant temperature.

[0167] Relative humidity is the ratio of the partial pressure of water vapor to the equilibrium vapor pressure of water at a given temperature, and is usually expressed as a percentage. Relative humidity depends on the temperature and pressure of the system. Here, relative humidity is measured at a temperature of approximately 23 degrees Celsius and atmospheric pressure, i.e., 1 atmosphere. The relative humidity (RH) of a water-gas mixture is the ratio of the equilibrium vapor pressure (p*) of water on a flat surface of pure water at a given temperature. H2O ) relative to the partial pressure of water vapor in the mixture (p H2O ) Ratio: RH=p H2O / p* H2O It is defined as follows.

[0168] In this specification, the amount of water contained within a material is expressed as the "water content" or "moisture content" of the material. Moisture content is expressed as a ratio that can range from 0 (completely dry) to the value of the porosity of the material at saturation. This may be given on a volume basis or on a mass (weight) basis. In this application, this is expressed on a mass basis, i.e., moisture content is the ratio between the mass of water contained within the material and the mass of the material itself that does not contain water.

[0169] Metal-organic frameworks (MOFs) are a class of compounds consisting of clusters that coordinate with metal ions or organic ligands to form one-dimensional, two-dimensional, or three-dimensional structures containing potential spaces. Metal-organic frameworks (MOFs) provide vacancies with dimensions less than 2 nanometers, are crystalline, and are highly stable. Metal-organic frameworks are lightweight and porous materials with outstanding surface area.

[0170] The definition of "metallic organic structure without water" is used to describe a metallic organic structure in a dry state, completely free of water.

[0171] Here, "binder" refers to any compound that can bond to a metal-organic structure(s) and possible supporting material.

[0172] As used herein, the term “modifier” means any additive that can be added to a moisture-modulating composition or solution to improve properties such as the solubility of at least one metal-organic structure, the solubility of a binder, the chemical bond between the metal-organic structure and the binder, or adhesion to a supporting material.

[0173] As used herein, the term “support material” means any material that can be used as a support for a product or for preparing a package.

[0174] "Fiber-based support material" means a material containing fibers. A fiber-based support material may contain any type of fiber, such as cellulose fibers.

[0175] As used herein, the definition of "impregnation bath" means a bath that contains a solution having a solvent and compounds dissolved in the impregnation bath, and in which a support material may be immersed. The support material is impregnated with the solution of the impregnation bath and adsorbs the solution contained in the impregnation bath.

[0176] As used herein, the term “sheet” means a layered element having a width and length substantially greater than its thickness.

[0177] As used herein, the definition of “web” means a layered element having a width and length substantially greater than its thickness, and a length substantially greater than its width, and usually wound onto a reel.

[0178] A specific embodiment will be described further, for illustrative purposes only, with reference to the attached drawings. [Brief explanation of the drawing]

[0179] [Figure 1] Figure 1 shows the sorption isotherms of aluminum fumarate samples at 23 degrees Celsius and 1 atmosphere of pressure. [Figure 2]Figure 2 shows the sorption isotherms of the MIL-101 sample at 23 degrees Celsius and 1 atmosphere of pressure. [Figure 3] Figure 3 shows the percentage relative humidity over time for some of the packages prepared in the examples. [Figure 4] Figure 4 shows the percentage of moisture content over time in the sample sticks of the package from the example in Figure 3. [Modes for carrying out the invention]

[0180] Figures 1 and 2 show the sorption isotherms for aluminum fumarate and MIL-101(Cr), respectively.

[0181] Numerous compounds adsorb water under defined humidity, temperature, and pressure conditions.

[0182] For each material or compound at a set temperature, the relationship between the water content of the compound or material and the equilibrium relative humidity under equilibrium conditions can be represented graphically using a curve, or so-called moisture sorption isotherm.

[0183] A moisture sorption isotherm shows the corresponding water content value at a given constant temperature for each relative humidity value.

[0184] When temperature changes, the equilibrium conditions for temperature change, and therefore the paths of adsorption isotherms also change. Generally, as the temperature rises, the material can hold less water, and conversely, as the temperature decreases, the material can hold more water.

[0185] When the material or compound changes, the adsorption behavior also changes.

[0186] Adsorption isotherms provide a measure of water uptake by a material in response to changes in relative humidity.

[0187] Referring to Figure 1, the adsorption isotherms of aluminum fumarate obtained at 23 degrees Celsius and 1 atmosphere using a 70 milligram sample of pure aluminum fumarate have been reported.

[0188] Adsorption isotherm analysis of pure aluminum fumarate at 23 degrees Celsius and 1 atmosphere was performed in a Belsorp aqua 3 machine (MicrotracBEL Corp., Japan).

[0189] Prior to analysis, the aluminum fumarate was activated by placing the sample in a Belprep II machine (MicrotracBEL Corp., Japan) under a vacuum of 0.01 kilopascals and purging it several times with argon.

[0190] Next, the sample was heated to 200 degrees Celsius over two hours, and then held at this temperature for eight hours to reduce the water content of the sample to approximately 1 weight percent.

[0191] After cooling, the container was filled with argon and placed inside the Belsorp Aqua 3 machine.

[0192] Next, the relative humidity of the container was changed over time, and the water uptake of the aluminum fumarate sample was recorded to obtain the sorption isotherm shown in Figure 1. The measurements were performed at a laboratory temperature of 23 degrees Celsius and a pressure of 1 atmosphere.

[0193] The same procedure was repeated for a sample of pure MIL-101(Cr) to obtain the adsorption isotherm shown in Figure 2.

[0194] Referring to Figure 2, the adsorption isotherms of a 70 milligram sample of pure MIL-101(Cr) obtained at 23 degrees Celsius and 1 atmosphere are reported.

[0195] Aluminum fumarate and MIL-101(Cr) were purchased from NovoMOF, AG (Switzerland).

[0196] Figure 1 reports the percentage relative humidity on the x-axis and the percentage of water adsorption on the y-axis. Water adsorption is expressed as a weight percentage, i.e., the weight of adsorbed water divided by the weight of aluminum fumarate or MIL-101(Cr).

[0197] The adsorption isotherm of aluminum fumarate has an S-shaped path.

[0198] Referring specifically to Figure 1, the adsorption isotherm 10 of aluminum fumarate includes a first portion 11 consisting of a minimum threshold 13 from zero relative humidity to relative humidity, where aluminum fumarate adsorbs about 1 to 5 percent of water, and the amount of water adsorbed by aluminum fumarate gradually increases depending on the relative humidity.

[0199] The sorption isotherm 10 for aluminum fumarate includes a second portion 12 consisting of a maximum relative humidity threshold of 14–100 percent, where aluminum fumarate adsorbs small amounts of water in response to increasing relative humidity. In the second portion, aluminum fumarate adsorbs approximately 35–54 percent of water. The amount of water adsorbed increases gradually depending on the relative humidity.

[0200] The minimum relative humidity threshold of 13 is approximately 20 percent, and the maximum relative humidity threshold of 14 is approximately 34 percent.

[0201] The sorption isotherm 10 includes an adsorption portion 15 consisting of a minimum relative humidity threshold 13 to a maximum relative humidity threshold 14. In the adsorption portion 15, aluminum fumarate adsorbs a larger amount of water than the amount of water adsorbed in the first portion 11 or the second portion 12. In the adsorption portion 15, the amount of water adsorbed increases significantly depending on the relative humidity.

[0202] Considering the slope of the sorption isotherm 10, the slopes in the first and second parts are smaller than the slope in the adsorption part. In the adsorption part 15, the increase in water adsorbed in response to the increase in relative humidity is considerably larger than the increase in water adsorbed in response to the increase in relative humidity in the first part 11 or the second part 12.

[0203] In the adsorption portion 15, aluminum fumarate adsorbs approximately 5 to 35 percent of water.

[0204] Figure 2 reports the sorption isotherm for MIL-101(Cr), with the horizontal coordinate (x-axis) reporting the percentage of relative humidity and the vertical coordinate (y-axis) reporting the percentage of water adsorption. Water adsorption is shown as weight percentage, i.e., weight of adsorbed water / weight of aluminum fumarate or MIL-101(Cr). The sorption isotherm for MIL-101(Cr) also has an S-shaped path.

[0205] Features corresponding to the features in Figure 1 are indicated by different corresponding reference numbers for clarity.

[0206] The adsorption isotherm 20 of MIL-101(Cr) includes a first portion 21 consisting of a minimum threshold 23 from zero relative humidity to relative humidity, where MIL-101(Cr) adsorbs approximately 1 to 5 percent of water, and the amount of water adsorbed by MIL-101(Cr) has a gradual increase depending on the relative humidity.

[0207] The adsorption isotherm 20 of MIL-101(Cr) includes a second portion 22 consisting of a maximum threshold relative humidity of 24 to 100 percent relative humidity, where MIL-101(Cr) adsorbs approximately 110 to 127 percent of water, and the amount of water adsorbed has a gradual increase depending on the relative humidity.

[0208] The minimum relative humidity threshold of 23 is approximately 37 percent, and the maximum relative humidity threshold of 24 is approximately 48 percent.

[0209] The sorption isotherm 20 includes an adsorption portion 25 consisting of a minimum relative humidity threshold 23 to a maximum relative humidity threshold 24. In the adsorption portion 25, MIL-101(Cr) adsorbs more water than the amount adsorbed in the first portion 21 or the second portion 22 as the relative humidity increases. In the adsorption portion 25, the amount of water adsorbed increases significantly depending on the relative humidity.

[0210] In the adsorption section 25, MIL-101(Cr) adsorbs approximately 5 to 110 percent of water.

[0211] Both aluminum fumarate and MIL-101(Cr) show an increase in water adsorption in adsorption portions 15 and 25 with respect to each increase in relative humidity.

[0212] The adsorption portions of aluminum fumarate and MIL-101(Cr) consist of minimum and maximum thresholds for different relative humidity levels, and these thresholds depend on the specific material.

[0213] The amount of water adsorbed by aluminum fumarate and MIL-101(Cr) at the adsorption site varies depending on the specific moisture-regulating composition.

[0214] Several moisture-regulating compositions and moisture-regulating solutions have been prepared according to the present invention.

[0215] The prepared moisture-regulating composition or moisture-regulating solution is then bound to the packaging material. At least a portion of the packaging material containing the moisture-regulating composition is then inserted into a package for heat-non-combustible products, i.e., tobacco-derived products intended for use by heating rather than combustion. In addition, several porous pouches containing one or more defined amounts of metal-organic structures were prepared and similarly inserted into the heat-non-combustible product packages.

[0216] The relative humidity inside the package over time and the moisture content of the product packed inside the package were measured.

[0217] For testing, a HEETS package provided by Philip Morris International was used. The HEETS package contains 20 tobacco sticks as a heated, non-combustible product (HEETS). Also known as HeatStick, HEETS is a specially designed heated tobacco unit intended for exclusive use with an IQOS holder (manufactured by Philip Morris International). HEETS is constructed from elements including a tobacco plug, a hollow acetate tube, a polymer film filter, a cellulose acetate mouthpiece filter, and outer and mouth-end paper. In HEETS, the tobacco is heated but not combusted. Instead of smoke from tobacco combustion, an aerosol is released to the user.

[0218] To mimic the opening of a HEET package by a user intending to use the sticks contained within, the top of the outer polypropylene film and inner paper bundle was removed from the HEET package. Additionally, 10 of the 20 sticks were removed from the HEET package.

[0219] To test the behavior of some moisture-regulating products of the present invention, the moisture-regulating products were added to HEETS packages in several different ways (i.e., coated onto a sheet of cardboard inserted into the package, or impregnated onto a sheet of foam paper inserted into the package). Additionally, pure pouches containing metal-organic structures were prepared and inserted into the package.

[0220] Additionally, some reference packages containing no moisture-regulating products whatsoever were prepared and tested for comparative purposes.

[0221] In the test, the relative humidity of the prepared package was measured, as well as the moisture content of the sticks inside the package.

[0222] HEETS packaging may contain tobacco sticks having different characteristics or flavors.

[0223] For clarification, different HEETS packages without any moisture-regulating composition were compared with corresponding HEETS packages equipped with either a moisture-regulating composition or at least one metal-organic structure. In this way, a clear effect of the moisture-regulating composition or at least one metal-organic structure on the same type of HEETS package was obtained.

[0224] Additionally, a Plug and Track Hygro Button (PROGESPLUS, France) with a data logger was placed inside the HEETS package to measure the relative humidity inside the package. The packages were then each sealed in an aluminum bag.

[0225] Before placing the Hygro Button relative humidity analyzer inside the package, the button was configured using PROGESPLUS software to measure the relative humidity inside the package before the test and during the test period.

[0226] The Hygro Button, which has a built-in data logger, measures relative humidity every 5 minutes, and a graph showing relative humidity over time was extracted from the PROGESPLUS software.

[0227] The moisture content of the tobacco plug in each stick was determined using the Karl Fischer method (similar to ASTM E203-16) in conjunction with an analyzer Titrando 901 (Metrohm AG, Switzerland) and an analytical balance XP205 (Mettler Toledo, Switzerland). The moisture content of the tobacco plug in each stick was extracted using an oven by heating the sticks at 110 degrees Celsius.

[0228] The extracted vapor was transferred to a titration cell along with the airflow through a heated transfer line, and the water content was quantitatively determined by titration. Methanol was used to improve the accuracy of the analysis. The endpoint was measured by potentiometric assay, and the results were given in weight percentage.

[0229] In experimental tests, the amount of metal-organic structure is expressed in grams with two significant digits, and the value of the amount of metal-organic structure is rounded to two significant digits.

[0230] Experimental Test Examples 1, 5, 15 A HEETS package containing 20 non-combustible tobacco sticks was provided.

[0231] Ten of the 20 sticks were removed from the HEETS package. A Plug and Track Hygro Button (PROGESPLUS, France) with a data logger was placed inside the HEETS package to measure the relative humidity inside the package. The packages were then sealed individually in aluminum bags. Before placing the Hygro Button relative humidity analyzer inside the package, the button was configured using PROGESPLUS software to measure the relative humidity inside the package before the test and during the duration of the test. The Hygro Button with a built-in data logger measured the relative humidity every 5 minutes, and a graph showing the relative humidity as a function of time was extracted from the PROGESPLUS software.

[0232] The moisture content of the tobacco plug in each stick was determined using the Karl Fischer method (similar to ASTM E203-16) in conjunction with an analyzer Titrando 901 (Metrohm AG, Switzerland) and an analytical balance XP205 (Mettler Toledo, Switzerland). The moisture content of the tobacco plug in each stick was extracted using an oven by heating the sticks at 110 degrees Celsius.

[0233] Example 2 A moisture-adjusting solution was prepared containing 1.00 gram of starch, 4.70 gram of water, 0.25 gram of glycerol, and 0.50 gram of aluminum fumarate.

[0234] The aluminum fumarate was purchased from NovoMOF, AG (Switzerland).

[0235] I purchased glycerol (HOCH2CH(OH)CH2OH) from Sigma Aldrich (Switzerland).

[0236] Potato starch ((C6H 10 O5) n I purchased it from PanReac AppliChem.

[0237] 0.50 grams of aluminum fumarate were sieved and mixed with soluble potato starch. The homogeneous mixture of particles was then dissolved in distilled water to which glycerol had been pre-added.

[0238] The resulting water-adjusted solution was heated to 85 degrees Celsius in a water bath and maintained at this temperature for 45 minutes under magnetic stirring. The solution was then cooled to approximately 20-30 degrees Celsius.

[0239] Next, a moisture-regulating solution was coated onto the fibrous support material.

[0240] The fibrous support material is a low-density foamed paper with a density of 400 kilograms per cubic meter and a basis weight of 120 grams per square meter, purchased from VTT-Technical Research Centre (Finland).

[0241] The fibrous support material was coated using an EZ coater EC200, rod number 8, manufactured by Chemical Instruments Inc., yielding a layer 20 micrometers thick at a speed of 0.00635 meters per second.

[0242] The first layer was completed 30 minutes after the solution was removed from the heat source. After the solvent evaporated, the second layer coating was applied, and then, after the solvent evaporated from the second layer, the third layer coating was applied again. In this way, a layer of approximately 60 micrometers was obtained. The coating was applied to both surfaces of the supporting material.

[0243] Next, the coated support material was dried at room temperature and room temperature relative humidity. Then, to further dry the coated support material, it was placed in a Froilabo oven at 80 degrees Celsius for 3 hours. The moisture content of the packaging material after the drying process should be below the moisture content corresponding to the minimum threshold of relative humidity for aluminum fumarate on the sorption isotherm under environmental conditions (23 degrees Celsius, 1 atmosphere).

[0244] After drying, the fibrous support material was cut into smaller sheets measuring 4 cm x 6.5 cm.

[0245] Each sheet was then sealed in an aluminum bag until further analysis was performed.

[0246] To analyze the relative humidity, the top of the outer polypropylene film, the inner paper bundle, and the tops of the 10 sticks from the package were removed, and then two sheets were placed inside the HEETS package.

[0247] In this way, approximately 0.20 grams of metal-organic structures (or multiple structures) can be obtained per package of HEETS. This is shown below as Example 2.

[0248] Additionally, a Plug and Track Hygro Button (PROGESPLUS, France) with a data logger was placed inside the package to measure the relative humidity inside the package. The package was finally sealed in an aluminum bag.

[0249] Example 3 A moisture-adjusted solution was prepared according to Example 2.

[0250] Next, the moisture-regulating solution was impregnated onto the support.

[0251] Cardboard with a density of 240 grams per square meter, purchased from Invercote Lenato (Iggesund, Sweden), was used.

[0252] The cardboard was cut into sheets measuring 4 cm x 6.5 cm. The sheets were immersed in the moisture-adjusting solution and held there for 30 minutes so that the cardboard sheets would be impregnated with the solution. The sheet was obtained containing approximately 0.155 grams of aluminum fumarate.

[0253] Subsequently, the cardboard sheets were placed in an oven at 80 degrees Celsius for 3 hours to dry. The moisture content of the packaging material after the drying process should be below the moisture content corresponding to the minimum threshold of relative humidity for aluminum fumarate on the sorption isotherm under environmental conditions (23 degrees Celsius, 1 atmosphere). The dried, impregnated sheets were stored in aluminum bags until further analysis.

[0254] To analyze the relative humidity, two impregnated sheets were placed inside the HEETS packages after removing the top of the outer polypropylene film, the top of the inner paper bundle, and the top of the 10 sticks from the package, so that approximately 0.31 grams of aluminum fumarate was obtained inside each HEETS package. This is shown below as Example 3.

[0255] Additionally, a Plug and Track Hygro Button (PROGESPLUS, France) with a data logger was placed inside the HEETS package to measure the relative humidity inside the package. The package was then sealed in an aluminum bag.

[0256] Further Examples For comparison, several metal-organic structure solutions without any binder were prepared. The metal-organic structure solutions were adsorbed or inserted into porous pouches.

[0257] A porous pouch containing 1 gram of aluminum fumarate was prepared and placed in two types of HEETS packages. These samples are shown below as Examples 4 and 16, respectively.

[0258] Porous pouches containing 0.20 grams, 0.50 grams, and 1.00 gram of MIL-101 Fe were prepared, respectively. These samples are shown below as Examples 9-11.

[0259] Porous pouches containing 0.20 grams, 0.50 grams, and 1.00 grams of MIL-101 Cr were prepared, respectively. These samples are shown below as Examples 6-8. A further pouch containing 1 gram of MIL-101 Cr was prepared and shown below as Example 17, and is placed in a separate HEETS package.

[0260] A porous pouch containing multiple metal-organic structures was also prepared.

[0261] A porous pouch containing 0.50 grams of aluminum fumarate and 0.50 grams of MIL-101 Fe was also prepared. This sample is shown below as Example 18.

[0262] A porous pouch containing 0.50 grams of aluminum fumarate and 0.50 grams of MIL-101 Cr was also prepared. This sample is shown below as Example 19.

[0263] To analyze the relative humidity, each porous pouch was placed inside the HEETS package after removing the top of the outer polypropylene film, the inner paper bundle, and the top of the 10 sticks from the package.

[0264] Additionally, a Plug and Track Hygro Button (PROGESPLUS, France) with a data logger was placed inside the package to measure the relative humidity inside. The package was then sealed in an aluminum bag, which remained closed for several days. The package was kept inside the aluminum bag until the relative humidity inside the package stabilized. Usually, a few hours is sufficient.

[0265] Table 1, reported below, summarizes the packages analyzed and, for clarity, indicates the example number and adsorption method.

[0266] Relative humidity was measured in the following different HEETS packages: HEETS package containing moisture-regulating composition 3, Examples 2 and 3, HEETS package containing one or more metal-organic structures, Examples 4, 6-11, and 16-19. Examples 1, 5, and 15, in which there are no metal-organic structures at all within the HEETS package.

[0267] [Table 1]

[0268] measurement At a specific time indicated as time T0, all packages prepared according to Examples 1-19 discussed above and reported in Table 1 were opened, and the aluminum bags were placed in an artificial climate chamber at 30 degrees Celsius and 75 percent relative humidity.

[0269] Three sticks were taken from each package and sealed together with the three sticks from each example in Table 1 in an additional aluminum bag.

[0270] After 2, 4, 6, 8, 24, and 48 hours, one stick was removed from each package and sealed in an aluminum bag with other sticks from the same embodiment, and therefore from the same package, until all sticks in each package were used.

[0271] Next, all sticks were analyzed using the Karl Fischer method, and the moisture content of different sticks removed from the packages was measured, as described below. Throughout the experiment, the evolution of relative humidity within each package was recorded, as described below.

[0272] Relative humidity analysis As described above, a Plug and Track Hygro Button (PROGESPLUS, France) with a data logger was placed inside the package to measure the relative humidity inside the package. Before placing the Hygro Button relative humidity analyzer inside the package, the button was configured using PROGESPLUS software to measure the relative humidity inside the package before the test and during the duration of the test. The Hygro Button with a built-in data logger measured the relative humidity every 5 minutes, and a graph showing the relative humidity over time was extracted from the PROGESPLUS software.

[0273] The results obtained for the packages of Examples 15-19 are reported in Figure 3 and discussed below.

[0274] water content analysis The moisture content of the tobacco plug in each stick was determined using the Karl Fischer method (similar to ASTM E203-16) in conjunction with an analyzer Titrando 901 (Metrohm AG, Switzerland) and an analytical balance XP205 (Mettler Toledo, Switzerland). The water contained within the tobacco plug of each stick was extracted using an oven by heating the stick at 110 degrees Celsius.

[0275] The extracted vapor is conveyed to the titration cell together with the air stream through the heating and conveying line, and the water content is quantified by titration.

[0276] Methanol is used to improve the accuracy of the analysis.

[0277] The endpoint is measured by the potentiometric method, and the result is given as a weight percentage.

[0278] Analyze the percentage water content of each stick at each time interval to determine the adsorption capacity of the adsorbent(s) used in the examples.

[0279] The results obtained from the sticks of Examples 15 - 19 are reported in Figure 4 and discussed below.

[0280] Results Regarding the inside of the HEETS package with the use of the metal-organic framework and the HEETS package without the use of the metal-organic framework, Figure 3 shows the change in relative humidity from the moment they are sealed until they are opened and held at 30 degrees Celsius and 75 percent relative humidity for two days.

[0281] Figure 3 reports time (unit: hours [h]) on the abscissa (x-axis) and the percentage of relative humidity on the ordinate (y-axis). Curve 30 shows the change in percent relative humidity over time inside a HEETS package without a moisture regulating composition in Example 15. Curve 40 shows the change in percent relative humidity over time inside a HEETS package with a pure aluminum fumarate moisture regulating composition in Example 16. Curve 50 shows the change in percent relative humidity over time inside a HEETS package with a moisture regulating composition of 0.50 grams of aluminum fumarate and 0.50 grams of MIL 101 Fe in Example 18. Curve 60 shows the change in percent relative humidity over time inside a HEETS package with a moisture regulating composition of 0.50 grams of aluminum fumarate and 0.50 grams of MIL 101 Cr in Example 19. Curve 70 shows the change in percent relative humidity over time inside a HEETS package with a moisture regulating composition of 1.00 grams of MIL 101 Cr in Example 17. As is clear from curve 30, the level or relative humidity inside a package without any metal organic framework is higher than inside a package provided with an adsorbent material.

[0282] Upon initial opening of a package without any metal organic framework, a sharp increase in the percent relative humidity is seen.

[0283] At least packages provided with a metal organic framework have a lower level of relative humidity compared to packages without any metal organic framework. The packages of Examples 17, 18, and 19 maintain a lower level of humidity than a package without any metal organic framework even 48 hours after initial opening.

[0284] As is evident from curve 30, in the package of Example 15, the relative humidity inside the package during storage is approximately 50 percent. Once the package is opened, the relative humidity dramatically increases to 75 percent, the ambient relative humidity in the test, after about 24 hours. As is evident from curve 30, the increase in relative humidity inside the package is not linear, as the relative humidity inside the package does not immediately reach 75 percent because the cardboard and some of the packaging film remaining on the package act as a barrier, and some of the incoming water vapor is absorbed by the stick.

[0285] As is clear from Figure 3, the change in relative humidity inside the package follows an S-shaped path after the package is opened.

[0286] Analyzing curves 40, 50, 60, and 70 clearly shows the effect of metal-organic structures on relative humidity levels in both closed and open packages. Compared to the reference, packages with metal-organic structures have lower relative humidity, and the more metal-organic structures a package contains, the lower the relative humidity inside the package.

[0287] For example, the relative humidity obtained by Example 18 is intermediate between the relative humidity obtained by Examples 17 and 16.

[0288] Therefore, the relative humidity inside the package may be adjusted by selecting and mixing different metal-organic structures.

[0289] In particular, it is possible to adjust the minimum and maximum thresholds of relative humidity, and therefore the adsorption portion of the sorbation isotherm. Subsequently, it is possible to adjust the water adsorbed at the adsorption portion of the sorbation isotherm.

[0290] Similarly, the moisture content of the tobacco plugs in stick samples taken during the test at various time intervals was determined by Karl Fischer analysis. The results can be seen in Figure 4. Figure 4 reports the time (in hours [h]) on the x-axis and the percentage of moisture content of the sticks on the y-axis.

[0291] The moisture content of the cigarette plug in different embodiments reflects the relative humidity of the package in the corresponding embodiment.

[0292] In Figure 4, 80 shows a curve representing the moisture content of the cigarette plug over time in the package of Example 15, which has no metal-organic structures; 81 shows a curve representing the moisture content of the cigarette plug over time in the package of Example 16, which has 1 g of aluminum fumarate; 82 shows a curve representing the moisture content of the cigarette plug over time in the package of Example 17; 83 shows a curve representing the moisture content of the cigarette plug over time in the package of Example 18; and 84 shows a curve representing the moisture content of the cigarette plug over time in the package of Example 19.

[0293] Table 2, reported below, summarizes all the results obtained for all the examples tested.

[0294] Table 2 shows, for each example, the first column contains the amount of metal-organic structure(s), the second column contains the percentage of relative humidity inside the package before opening, and the third column contains the percentage of initial water content in the stick before opening. The fourth column reports the time required for the stick to reach a moisture content of 11 percent after the package is opened under experimental conditions. The fifth column of Table 2 reports the percentage of relative humidity inside the package after 48 hours under experimental conditions: 30 degrees Celsius, 1 atmosphere of pressure, and 75 percent relative humidity. The sixth column of Table 2 reports the percentage of moisture content inside the stick after 48 hours under experimental conditions, i.e., 30 degrees Celsius, 1 atmosphere of pressure, and 75 percent relative humidity. The results are summarized in Table 2, which is reported below.

[0295]

Table 2

[0296] Result The prepared moisture control composition exhibits a sigmoidal adsorption isotherm.

[0297] The adsorption isotherm of the prepared moisture control composition exhibits a sharp and significant increase in adsorbed water with an increase in relative humidity, i.e., after opening the package under the experimental conditions.

[0298] By selecting a metal-organic framework, or a combination of multiple metal-organic frameworks, the adsorption behavior of the moisture control composition can be adjusted to desired needs and levels of relative humidity. By selecting the metal-organic framework(s) to be used, the level of relative humidity at which the moisture control composition absorbs water, and thus the relative humidity within the package containing the moisture control composition or the water content of the product packaged within the package, is adjusted.

[0299] Thus, depending on different applications, it is possible to use a specific moisture control composition appropriate for maintaining a desired level of relative humidity within the package.

[0300] By knowing the desired level of water content of the product, it is possible to select a moisture control composition that enables maintaining the desired level of water content. It is also possible to select the supporting material and / or the amount of the supporting material used to maintain the desired level of water content.

[0301] Also, the presence of a binder(s) has been demonstrated to improve the application of the metal-organic framework(s) onto the support.

[0302] The tests also demonstrated that even a small amount of metal-organic framework(s) can effectively maintain the relative humidity within the desired range.

[0303] When HEETS sticks are manufactured and packaged, the relative humidity inside the package is approximately 8-10 percent. The moisture-regulating composition or at least one metal-organic structure of the present invention is adjusted so that the moisture content of the tobacco plug is maintained at approximately a desired level.

[0304] Different moisture-regulating compositions may be used for products having different levels of moisture content.

[0305] Therefore, depending on the different package or product whose moisture content needs to be adjusted, it is possible to select a specific moisture-controlling composition that is appropriate to maintain the desired level of relative humidity within the package and the desired level of moisture content within the product.

[0306] Therefore, depending on the product, it is possible to use a specific moisture-regulating composition that is appropriate for maintaining the desired level of moisture content within the product.

[0307] By knowing the desired moisture content level of the product, it is possible to select a moisture-regulating composition that will enable the maintenance of that desired moisture content level.

[0308] The tests also demonstrated that the moisture-regulating composition of the present invention prevents both excessive drying and excessive wetting of the product.

[0309] As is evident from Table 2, before opening, the moisture content of a cigarette plug in a package containing the moisture-regulating composition of the present invention or at least one metal-organic structure is lower than the moisture content of a cigarette plug in a corresponding package that does not contain the moisture-regulating composition of the present invention or at least one metal-organic structure.

[0310] This confirms that, even 48 hours after opening, the moisture content of the cigarette plug in a package containing the moisture-regulating composition of the present invention or at least one metal-organic structure is lower than the moisture content of the cigarette plug in a corresponding package that does not contain the moisture-regulating composition of the present invention or at least one metal-organic structure.

[0311] Using the moisture-regulating composition of the present invention or at least one metal-organic structure, the moisture content of the cigarette plug is adjusted so as to avoid excessive reduction of the moisture content.

[0312] The tests also demonstrate that water adsorption effects may be obtained by impregnating the packaging material with the moisture-regulating composition, coating the support material with the moisture-regulating composition, or applying the moisture-regulating composition to a porous pouch.

[0313] The tests also demonstrated that existing conventional HEETS packages may be improved by adding a support material to which a moisture-regulating composition is provided.

[0314] Therefore, the conventional packaging of numerous different products can be improved in a similar manner.

[0315] The tests also demonstrated that by selecting a moisture-modulating composition, it is possible to adjust the moisture content of tobacco or nicotine-containing products to a desired level, which may vary depending on the specific tobacco or nicotine-containing product.

[0316] The moisture-regulating composition acts to create an active layer that can be adjusted to absorb a specific amount of water, and above a certain minimum threshold of relative humidity.

[0317] Therefore, by selecting the correct moisture-regulating composition and a desirable mixture of metal-organic structures (multiple may be used), it is possible to obtain an adsorption isotherm having a desirable S-shape. It is possible to obtain an adsorption isotherm that is suitable for the desired moisture content of tobacco or nicotine-containing products.

[0318] Additionally, by selecting the correct moisture-modifying product and a desirable mixture of metal-organic structures, it is possible to obtain a moisture-modifying product and therefore a packaging material that does not undesirably alter the moisture content of tobacco or nicotine-containing products.

[0319] It is also possible to obtain moisture-regulating products that adsorb water at relative humidity levels higher than a minimum threshold. Furthermore, it is possible to avoid excessive drying of tobacco or nicotine-containing products during their shelf life, i.e., before initial opening.

Claims

1. A package comprising a packaging element made of a support material having a coating layer containing a moisture-regulating composition, wherein the moisture-regulating composition comprises at least one metal-organic structural compound in a total dry weight of 20 to 60 percent and at least one binder material in a total dry weight of 80 to 40 percent, and the at least one metal-organic structural compound is Aluminum fumarate (C 12 H 6 Al 2 O 12 )and, Interconnected by 1,4-benzenedicarboxylic acid, and with the chemical formula [Cr 3 (O)X(bdc) 3 (H 2 O) 2 MIL-101(Cr), a chromium terephthalate organic structure comprising a trimer chromium(III) octahedral cluster having ], wherein bdc is benzene-1,4-dicarboxylic acid and X is OH or F, A functionalized terephthalic acid chromium metal-organic framework MIL-101(Cr)-X, wherein X is an electron-withdrawing group (selected from NO 2 , SO 3 H and Cl) or an electron-donating group (selected from NH 2 and CH 3 ), and the functionalized terephthalic acid chromium metal-organic framework MIL-101(Cr)-X, The iron metal organic structure terephthalate MIL-101 (Fe) and, Chemical formula [Cr 3 (μ3-O)(H 2 A chromium-based metal-organic structure of [O)2(TCPT)1,5Cl], wherein TCPT is a tetratopic 3,3”,5,5”-tetrakis(4-carboxyphenyl)-p-terphenyl ligand, Equistructured Zr(IV)-MOFs, represented as BUT-46F, BUT-46A, BUT-46W, and BUT-46B, Y-shp-MOF-5, where "shp" in the formula refers to a square hexagonal prism, is a hybrid microporous, highly bonded rare-earth metal-organic structure Y-shp-MOF-5, Or any combination thereof, selected from the group, Furthermore, at least one binder is starch ((C 6 H 10 O 5 )n-(H 2 O)), alginic acid ((C 6 H 8 O 6 )n), alginate, polyacrylic acid copolymer ((C 3 H 4 O 2 )n), and / or maleic acid copolymer (HO 2 CCH = CHCO 2 H), polyaspartic acid ((C 4 H 5 NO 3 )n), polyvinyl alcohol-co-ethylene (EVOH, C 4 H 8 O), polyvinyl alcohol-co-vinyl acetate, polyethylene oxide ((-CH 2 CH 2 Selected from the group consisting of O-)n), or any combination thereof, A package in which the coating layer containing the moisture-regulating composition has a thickness of 10 micrometers to 80 micrometers.

2. The package according to claim 1, wherein the functionalized chromium terephthalate metal organic structure MIL-101(Cr)-X is MIL-101(Cr)-NO 2 A package that includes this.

3. The package according to claim 1, wherein the Zr(IV)-MOF includes Zr(IV)-MOF BUT-46A.

4. The package according to claim 1, wherein the at least one metal-organic structure forms between 5 percent and 40 percent of the total volume of the moisture-regulating solution.

5. The package according to claim 4, wherein the at least one metal-organic structure forms between 5 percent and 35 percent of the total volume of the moisture-regulating solution.

6. The package according to claim 4, wherein the at least one metal-organic structure forms 10 percent to 30 percent of the total volume of the moisture-regulating solution.

7. The package according to claim 4, wherein the at least one metal-organic structure forms 15 percent to 25 percent of the total volume of the moisture-regulating solution.

8. A package according to any one of claims 4 to 7, wherein the moisture adjusting solution contains a solvent, and the solvent is water.

9. A package according to claim 1, wherein the support material is a fibrous material or a plastic support material.

10. The package according to claim 9, wherein the support material is selected from the group consisting of paper, cardboard, cloth, textile, nonwoven fabric, polymer, polymer foam, and polymer film.

11. The package according to claim 9 or 10, wherein the amount of the moisture-regulating composition in the support material is between 20 grams per square meter and 300 grams per square meter.

12. The package according to claim 11, wherein the relative weight ratio between the at least one metal-organic structure and the at least one binder is 1:4 to 3:

2.

13. The package according to claim 9 or 10, wherein the moisture-regulating composition is impregnated into the support material.

14. The package according to claim 9 or 10, wherein the support material comprises a support layer made of a fibrous material or a plastic material, and the coating layer containing the moisture-regulating composition is applied on the support layer, so that the amount of the moisture-regulating composition in the support material is 20 grams per square meter to 300 grams per square meter.

15. The package according to any one of claims 9 to 14, wherein the support material is a foamed support material having a density of 10,000 grams per cubic meter to 900,000 grams per cubic meter.

16. A package according to any one of claims 1 to 15, comprising at least one metal-organic structure in an amount ranging from 0.30 grams to 5.00 grams.

17. A package according to claim 16, comprising at least one metal-organic structure in an amount ranging from 0.50 grams to 2.50 grams.

18. A package according to claim 16, comprising at least one metal-organic structure in an amount ranging from 0.75 grams to 1.50 grams.

19. The package according to claim 16, comprising at least one metal-organic structure in an amount of 1.00 gram.

20. A method for preparing packaging elements to be used in a package according to any one of claims 1 to 19, a) A step of providing the support material, b) A step of providing an impregnation bath of a moisture-regulating solution containing the moisture-regulating composition and solvent, c) The steps include: immersing the support material in the impregnation bath until it is impregnated with the solution in the impregnation bath; d) A method comprising drying the support material to evaporate the solvent from the support material to obtain a support material comprising the at least one metal-organic structure that exhibits a moisture content that is in equilibrium with a gas-water mixture characterized by relative temperatures ranging from 0 to 25 percent according to the corresponding adsorption isotherms of the at least one metal-organic structure at a temperature of 23 degrees Celsius and a pressure of 1 atmosphere.

21. A method for preparing packaging elements to be used in a package according to any one of claims 1 to 19, a1) A step of providing the support material, b1) A step of providing an impregnation bath of a moisture-regulating solution containing the moisture-regulating composition and solvent, c1) A step of immersing the support material in the impregnation bath until the support material is impregnated with the solution of the impregnation bath, d1) A method comprising drying the support material to evaporate the solvent from the support material in order to obtain a support material comprising the at least one metal-organic structure having a water content of 0 to 25 weight percent based on the water-free weight of the at least one metal-organic structure.

22. The method according to claim 20, wherein after step c) and before step d), or the method according to claim 21, wherein after step c1) and before step d1), c2) A method further comprising the step of supplying the support material impregnated with the solution of the impregnation bath to a weighing roll in order to remove excess solution from the support material.

23. The method according to any one of claims 20 to 22, wherein the support material is a web of support material that is continuously supplied to the impregnation bath.

24. A package comprising a packaging element made of a support material having a coating layer containing a moisture-regulating composition, wherein the moisture-regulating composition comprises at least one metal-organic structural compound in a weight of 20 to 60 percent by total dry weight and at least one binder material in a weight of 80 to 40 percent by total dry weight, and the at least one metal-organic structural compound is Aluminum fumarate (C 12 H 6 Al 2 O 12 )and, A functionalized chromium terephthalate metal organic structure, MIL-101(Cr)-X, wherein X is electron-withdrawing (NO 2 SO 3 (A group selected from H and Cl) or electron-donating (NH 2 and CH 3 MIL-101(Cr)-X, a functionalized chromium terephthalate organic structure, refers to a group selected from the above, The iron metal organic structure terephthalate MIL-101 (Fe) and, Chemical formula [Cr 3 (μ3-O)(H 2 A chromium-based metal-organic structure of [O)2(TCPT)1,5Cl], wherein TCPT is a tetratopic 3,3”,5,5”-tetrakis(4-carboxyphenyl)-p-terphenyl ligand, Equistructured Zr(IV)-MOF, represented as Zr(IV)-MOF BUT-46F, BUT-46A, BUT-46W, and BUT-46B, Y-shp-MOF-5, where "shp" in the formula refers to a square hexagonal prism, is a hybrid microporous, highly bonded rare-earth metal-organic structure Y-shp-MOF-5, Or any combination thereof, selected from the group, The at least one binder is carboxymethylcellulose (CMC, C 6 H 7 O 2 (OH) 2CH 2 COONa), hydroxyethylcellulose (C 29 H 52 O 21 ), hydroxypropylcellulose (C 36 H 70 O 19 ), polyvinyl alcohol ((C 2 H 4O )x), or any combination thereof, selected from the group A package in which the coating layer containing the moisture-regulating composition has a thickness of 10 micrometers to 80 micrometers.

25. The package according to claim 24, wherein the functionalized chromium terephthalate metal organic structure MIL-101(Cr)-X is MIL-101(Cr)-NO 2 A package that includes this.

26. The package according to claim 24, wherein the Zr(IV)-MOF comprises Zr(IV)-MOF BUT-46A.

27. A solvent and the package according to claim 24, wherein the at least one metal-organic structure forms 5 percent to 40 percent of the total volume of the water-adjusting solution.

28. The package according to claim 27, wherein the at least one metal-organic structure forms between 5 percent and 35 percent of the total volume of the moisture-regulating solution.

29. The package according to claim 27, wherein the at least one metal-organic structure forms 10 percent to 30 percent of the total volume of the moisture-regulating solution.

30. The package according to claim 27, wherein the at least one metal-organic structure forms 15 percent to 25 percent of the total volume of the moisture-regulating solution.

31. The package according to claim 27, wherein the moisture adjusting solution contains a solvent, and the solvent is water.

32. The package according to claim 24, wherein the support material is a fibrous material or a plastic support material.

33. The package according to claim 32, wherein the support material is selected from the group consisting of paper, cardboard, cloth, textile, nonwoven fabric, polymer, polymer foam, and polymer film.

34. The package according to claim 32 or 33, further comprising the support material in an amount of the moisture-regulating composition consisting of 20 to 300 grams per square meter.

35. The package according to claim 34, wherein the relative weight ratio between the at least one metal-organic structure and the at least one binder is 1:4 to 3:

2.

36. The package according to claim 32 or 33, wherein the moisture-regulating composition is impregnated into the support material.

37. The package according to claim 32 or 33, wherein the support material comprises a support layer made of a fibrous material or a plastic material, and a coating layer applied on the support layer and containing the moisture-regulating composition described in claim 1, wherein the amount of the moisture-regulating composition in the support material is 20 to 300 grams per square meter.

38. The package according to any one of claims 32 to 36, wherein the support material is a foamed support material having a density of 10,000 to 900,000 grams per cubic meter.

39. The package according to any one of claims 24 to 38, comprising a predetermined amount of at least one(s) metal-organic structures.

40. The package according to claim 39, wherein the predetermined amount of the at least one metal-organic structure (or more) is 0.30 to 5.00 grams.

41. The package according to claim 39, wherein the predetermined amount of the at least one metal-organic structure (or more) is 0.50 grams to 2.50 grams.

42. The package according to claim 39, wherein the predetermined amount of the at least one metal-organic structure (or more) is 0.75 grams to 1.50 grams.

43. The package according to claim 39, wherein the predetermined amount of the at least one metal-organic structure (or more) is 1.00 gram.

44. A method for preparing packaging elements to be used in the package according to any one of claims 24 to 43, e) The step of providing the support material, f) A step of providing an impregnation bath of a moisture-regulating solution containing the moisture-regulating composition and the solvent, g) A step of immersing the support material in the impregnation bath until the support material is impregnated with the solution of the impregnation bath, h) A method comprising drying the support material to evaporate the solvent from the support material to obtain a support material comprising the at least one metal-organic structure having a moisture content that is in equilibrium with a gas-water mixture characterized by a relative humidity of 0 to 25 percent according to the corresponding sorption isotherm of the at least one metal-organic structure at a temperature of 23 degrees Celsius and a pressure of 1 atmosphere.

45. A method for preparing packaging elements to be used in the package according to any one of claims 24 to 43, e1) A step of providing a support material, f1) A step of providing an impregnation bath of a moisture-regulating solution containing the moisture-regulating composition and solvent, g1) A step of immersing the support material in the impregnation bath until the support material is impregnated with the solution of the impregnation bath, h1) A method comprising the step of drying the support material to evaporate the solvent from the support material in order to obtain a support material comprising the at least one metal-organic structure having a water content of 0 to 25 weight percent based on the water-free weight of the at least one metal-organic structure.

46. The method according to claim 44, wherein after step g) and before step h), or the method according to claim 45, wherein after step g1) and before step h1), g2) A method further comprising the step of supplying the support material, which has been impregnated with the solution of the impregnation bath, to a weighing roll in order to remove excess solution from the support material.

47. The method according to any one of claims 44 to 46, wherein the support material is a web of support material that is continuously supplied to the impregnation bath.

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