Barrier composition for cellulose substrates and methods of making and using the same

Abstract

Disclosed herein is a biodegradable barrier composition for use with cellulose substrates to provide a finished product that is resistant to moisture absorption, water vapor permeability, oxygen transmission, or any combination thereof. In embodiments the barrier composition comprises pectin activated by a calcium-based medium or a food-grade organic acid. The disclosure further relates to methods of preparing a biodegradable barrier composition and methods of associating the biodegradable barrier composition with cellulose fibers to increase strength, stiffness, and / or water resistance of the cellulose fibers.

Description

Attorney Docket No. 2967050.06. WO1Customer No. 190456BARRIER COMPOSITION FOR CELLULOSE SUBSTRATES AND METHODS OF MAKING AND USING THE SAME

[0001] All patents, patent applications, and publications cited herein are hereby incorporated by reference in their entirety. The disclosures of these publications in their entireties are hereby incorporated by reference into this application in order to more fully describe the state of the art as known to those skilled therein as of the date of the invention described and claimed herein.

[0002] A portion of the disclosure of this patent document contains material that is subject to copyright protection. The copyright owner has no objection to the reproduction of the patent document or the patent disclosure, as it appears in the U. S. Patent and Trademark Office patent file or records, but otherwise reserves all copyright rights whatsoever.CROSS-REFERENCE TO RELATED APPLICATIONS

[0003] This application claims priority to U. S. Provisional Application No.63 / 748,070, entitled “BARRIER COMPOSITION FOR CELLULOSE SUBSTRATES AND METHODS OF MAKING AND USING THE SAME,” filed January 22, 2025, the contents of which is incorporated herein by reference in its entirety.FIELD OF THE DISCLOSURE

[0004] This application relates in general to a barrier composition for use with cellulose fibers and related methods; and, more specifically, to a coating for cellulose fibers configured to increase strength, stiffness, and / or water resistance of the cellulose fibers. Certain embodiments are directed to a cellulose substrate product that is resistant to liquid absorption, water vapor transmission, and oxygen transmission.Attorney Docket No. 2967050.06. WO1Customer No. 190456 BACKGROUND

[0005] This section is intended to introduce various aspects of the art, which may be associated with exemplary embodiments of the present disclosure. This discussion is believed to assist in providing a framework to facilitate a better understanding of particular aspects of the present disclosure. Accordingly, it should be understood that this section should be read in this light, and not necessarily as admissions of prior art.

[0006] Sustainable packaging has grown in popularity over recent years due to its reduced environmental impact as compared to plastics and other materials harmful to the environment. Traditional plastic packaging does not biodegrade and thus significantly contributes to pollution. These plastics often end up in landfills or littered in the ocean, wherein they may leach harmful chemicals into the environment. Moreover, producing plastics generally requires the use of non-renewable fossil fuels, the extraction of which contributes to carbon emissions.

[0007] Sustainable packaging is typically biodegradable, meaning that it may naturally decompose or break down into non-toxic components when disposed of properly, and renewable, meaning the materials / resources used can be regrown and harvested sustainably. Recycling processes are often employed such that the sustainable packaging may be reused, for example in a new sustainable packaging after being broken down and repurposed.

[0010] Sustainable packaging may be made from a variety of materials, including cellulose fibers. Cellulose fibers are long, chain-like molecules that are the main component of plant cell walls. They are made up of repeating units of glucose molecules linked together to form a tough, rigid structure. Using cellulose fibers in sustainable packaging has many advantages, including that the fibers are derived from a renewable resource, biodegradable, compostable, and generally versatile. These fibers are often used to make paper products dueAttorney Docket No. 2967050.06. WO1Customer No. 190456 in part to the cellulose fibers’ ability to provide strength and stiffness to the products. These paper products include, but are not limited to, copy paper, packaging board, cardboard, and molded fiber.

[0008] While sustainable packing made with cellulose fibers has many advantages, there are certain properties of the fibers that render them undesirable in certain applications. Cellulose fibers lack a sufficient barrier against grease, water, oxygen, and moisture transmission, which prevents these fibers from being useful as packaging products without an additive or additional layer of protection. Indeed, cellulose fibers naturally absorb liquids like water and oil or grease. When cellulose fibers that have been made into paper products are exposed to moisture, the fiber absorbs the moisture and causes the paper product to lose its strength. Paper that is used for packaging is often exposed to water and other liquids wherein it quickly loses strength, stiffness, and the ability to protect is contents.

[0009] Cellulose fiber’s tendency to absorb liquids has limited the applications of paper products made from these fibers. To prevent such negative effects, absorption-resistant barrier compositions can be used and applied to the cellulose substrate. However, existing barrier compositions are primarily composed of petroleum-derived synthetic polymers or metallized films. These petroleum-based materials raise environmental concerns due to their nonbiodegradability and challenges with recycling. Thus, there is a need for a barrier that permits a paper-based packaging material to maintain its integrity during use while also preserving the environmental sustainability of the fiber substrate such that the product remains biodegradable and compostable. The present disclosure attempts to address the limitations and deficiencies in prior solutions according to the principles and embodiments disclosed herein.SUMMARYAttorney Docket No. 2967050.06. WO1Customer No. 190456

[0010] Disclosed herein is a biodegradable barrier composition for use with cellulose substrates to provide a finished product that is resistant to moisture absorption, water vapor permeability, and oxygen transmission. In embodiments the barrier composition comprises pectin activated by a calcium-based medium or a food-grade organic acid.

[0011] In one aspect, the present disclosure relates to a multi-layered, treated substrate that is bulk water resistant, resistant to water vapor transmission, resistant to oxygen transmission, or a combination thereof. In embodiments, the treated substrate comprises: a cellulose substrate layer with a first surface; a barrier composition layer comprising pectin and a cross-linking agent, wherein the multi-layered, treated substrate is biodegradable.

[0012] In another aspect, the present disclosure relates to a barrier composition for use in creating a water-resistant cellulose substrate. In embodiments, the barrier composition comprises pectin and a cross-linking agent.

[0013] In yet another aspect, a method of associating a barrier composition with cellulose fibers is disclosed. In embodiments, the method comprises preparing the barrier composition, the barrier composition comprising pectin and a cross-linking agent, wherein the cross-linking agent comprises a calcium-based medium, a food-grade organic acid, or a combination thereof; and associating the barrier composition with the cellulose fibers.

[0014] In another embodiment, the method of associating a barrier composition with a substrate comprises applying a pectin layer to at least one surface of a substrate and applying an activator over the pectin layer, wherein the pectin layer comprises pectin and the activator layer comprises a cross-linking agent. In embodiments, the cross-linking agent comprises a calcium-based medium, a food-grade organic acid, or a combination thereof.Attorney Docket No. 2967050.06. WO1Customer No. 190456

[0015] In the various aspects and embodiments disclosed herein, the cross-linking agent can comprise a calcium-based medium, a food-grade organic acid, or a combination thereof. In embodiments, the food-grade organic acid is oxalic acid, citric acid, lactic acid, acetic acid, tartaric acid, malic acid, fumaric acid, phosphoric acid, ascorbic acid, or any combination thereof. The calcium-based medium can be calcium chloride (CaCl2), calcium acetate (Ca(C2H3O2)2), calcium sulfate (CaSC>4), calcium carbonate (CaCO3), calcium gluconate (C12H24CaO12), calcium citrate (Ca3(C6H5O7)2), calcium phosphate (Ca3(PO4)2), or any combination thereof. In certain embodiments, the concentration of pectin within the barrier composition is between about 5% and about 20%.

[0016] The foregoing has outlined rather broadly the features and technical advantages of the present disclosure in order that the detailed description of the disclosure that follows may be better understood. Additional features and advantages of the disclosure will be described hereinafter that form the subject of the claims of the disclosure.

[0017] It should be appreciated by those skilled in the art that the conception and specific embodiment disclosed may be readily utilized as a basis for modifying or designing other structures for carrying out the same purposes of the present disclosure. It also should be realized by those skilled in the art that such equivalent constructions do not depart from the spirit and scope of the disclosure as set forth in the appended claims. The novel features that are believed to be characteristic of the disclosure, both as to its organization and method of operation, together with further objects and advantages will be better understood from the following description when considered in connection with the accompanying figures. It is to be expressly understood, however, that each of the figures is provided for the purpose of illustration and description only and is not intended as a definition of the limits of the present disclosure.Attorney Docket No. 2967050.06. WO1Customer No. 190456 BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Certain illustrations, charts, or flow charts are provided to allow for a better understanding for the present invention. It is to be noted, however, that the drawings illustrate only selected embodiments of the inventions and are therefore not to be considered limiting of scope. Additional and equally effective embodiments and applications of the present invention exist.

[0012] Fig. 1 shows an elevated top perspective view a treated substrate in accordance with one embodiment.

[0013] Fig. 2 shows top perspective and exploded view of the treated substrate of Fig.1.

[0014] Fig. 3 shows a side view of a treated substrate under another embodiment. The substrate is shown with at least two barrier compositions disposed on opposite surfaces of the substrate.

[0015] Fig. 4 provides a top perspective and exploded view of the treated substrate of Fig. 3.

[0016] Fig. 5 shows a top perspective and exploded view of a treated substrate, wherein the barrier composition is created via the application of two separate layers.DETAILED DESCRIPTION

[0017] So that the manner in which the present application can be better understood, certain illustrations and figures are appended hereto. It is to be noted, however, that the drawings illustrate only selected embodiments and elements of the systems and methods described herein and are therefore not to be considered limiting in scope for the systems andAttorney Docket No. 2967050.06. WO1Customer No. 190456 methods as described herein may admit to other equally effective embodiments and applications. Various embodiments of the present disclosure will be described in detail with reference to the drawings having like reference numerals represent like parts and assemblies throughout the several views. Reference to various embodiments does not limit the scope of the disclosure, which is limited only by the scope of the claims attached hereto. Additionally, any examples set forth in this specification are not intended to be limiting and merely set forth some of the many possible embodiments for the claimed disclosure. The present disclosure may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it is therefore desired that the embodiments of the disclosure be considered in all aspects as illustrative and not restrictive. Any headings utilized in the description are for convenience only and no legal or limiting effect. Numerous objects, features, and advantages of the embodiments set forth herein will be readily apparent to those skilled in the art upon reading of the following disclosure when taken in conjunction with the accompanying drawings.Abbreviations and Definitions

[0018] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.

[0019] The singular forms “a,” “an,” and “the” include plural reference unless the context clearly dictates otherwise. The use of the word “a” or “an” when used in conjunction with the term “comprising” in the claims and / or the specification can mean “one,” but it is also consistent with the meaning of “one or more,” “at least one,” and “one or more than one.”

[0020] Wherever any of the phrases “for example,” “such as,” “including” and the like are used herein, the phrase “and without limitation” is understood to follow unless explicitlyAttorney Docket No. 2967050.06. WO1Customer No. 190456 stated otherwise. Similarly, “an example,” “exemplary” and the like are understood to be nonlimiting.

[0021] The term “substantially” allows for deviations from the descriptor that do not negatively impact the intended purpose. Descriptive terms are understood to be modified by the term “substantially” even if the word “substantially” is not explicitly recited. Therefore, for example, the phrase “wherein the lever extends vertically” means “wherein the lever extends substantially vertically” so long as a precise vertical arrangement is not necessary for the lever to perform its function.

[0022] The terms “comprising” and “including” and “having” and “involving” (and similarly “comprises,” “includes,” “has,” and “involves”) and the like are used interchangeably and have the same meaning. Specifically, each of the terms is defined consistent with the common United States patent law definition of “comprising” and is therefore interpreted to be an open term meaning “at least the following,” and is also interpreted not to exclude additional features, limitations, aspects, etc. Thus, for example, “a process involving steps a, b, and c” means that the process includes at least steps a, b, and c. Wherever the terms “a” or “an” are used, “one or more” is understood, unless such interpretation is nonsensical in context.

[0023] As used herein the term “about” is used herein to mean approximately, roughly, around, or in the region of. When the term “about” is used in conjunction with a numerical range, it modifies that range by extending the boundaries above and below the numerical values set forth. In general, the term “about” is used herein to modify a numerical value above and below the stated value by a variance of 20 percent up or down (higher or lower).

[0024] References in the specification to “one embodiment,” “an embodiment,” “an exemplary embodiment,” etc., indicates that the embodiment described can include a particular feature, structure, or characteristic, but every embodiment may not necessarily include suchAttorney Docket No. 2967050.06. WO1Customer No. 190456 feature, structure, or characteristic. Moreover, such phrases are not necessarily referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with an embodiment, it is submitted that it is within the knowledge of one skilled in the art to affect such feature, structure, or characteristic in connection with other embodiments whether or not explicitly described.

[0025] The term “sustainable,” can be used to describe products or compositions that are designed, produced, and disposed of in a manner that minimizes the product or composition’s environmental impact throughout its lifecycle or any portion thereof. In various embodiments, “sustainable” products or compositions are made from materials that are renewable, recyclable, biodegradable, compostable, or any combination thereof. The word “sustainable” can refer to manufacturing processes that prioritize energy efficiency and the reduction of carbon emissions.

[0026] The term “compostable” as used herein can mean a product that is capable of undergoing biodegradation such that the product can be broken down into non-toxic components (e.g., water, carbon dioxide, biomass, or any combination thereof) within a specified time period. Compostable can refer to a product that can be broken down in to smaller portions and processed in composting systems without leaving visible remnants. In embodiments, compostable products release negligible amounts of harmful substances (e.g., heavy metals) during composting that could harm the environment or otherwise interfere with compost quality.

[0027] “Recyclable” as used herein can refer to a product that can be processed and reused as a raw material to make new products after its initial use. In embodiments, recyclability of a product can depend on the material type, infrastructure available, and contamination levels.Attorney Docket No. 2967050.06. WO1Customer No. 190456

[0028] As used herein, the term “coat,” “associate,” “deposit,” and the like encompasses any degree, level, or amount of intake of solution or slurry into or upon a surface of a substrate, such as via saturation or dispersion with some entrained air or surface coating.

[0029] As used herein, “curing” can refer to the process of converting a liquid-applied layer or composition (such as the barrier compositions disclosed herein) into a solid. Curing can be generally achieved through thermal treatment, exposure to ambient conditions over time, or a combination thereof. Subsequent to the steps for coating substrates, processes for further treating coatings on the substrates may include heat treatment. Heat treatment initiates and / or accelerates the curing processes of the coatings and may also drive off water. Controlling the amount of heat a coated substrate is exposed to may allow for controlling curing and water loss. In embodiments, the curing process may comprise exposing the treated substrate to an oven for controlled heat treatment. In certain embodiments, substrates may pass through an oven along a series of rollers, for example. Exemplary factors that can be controlled in an oven include temperature, humidity, intensity of heating units, air speed and transport speed.

[0030] “Pectin” as used herein can refer to a naturally occurring, water-soluble polysaccharide that can be found in the cell walls of plants, particularly in fruits such as apples, citrus, and berries.

[0031] A substrate to which any of the various barrier compositions disclosed herein has been added or otherwise applied to can be referred to herein as a “treated substrate.”Description of Selected Embodiments

[0032] In various exemplary embodiments, as seen in Figs. 1-4, the present disclosure relates in general to a biodegradable barrier composition for application and use with cellulose-Attorney Docket No. 2967050.06. WO1Customer No. 190456 based substrates and treated substrates comprising the same. The disclosure further relates to methods of producing finished substrate products comprising the barrier composition disclosed herein. In specific embodiments, the barrier coating comprises pectin. In one embodiment, pectin is the primary active ingredient. Embodiments include a barrier composition formulated for use with cellulose-based packaging products to protect consumable products. Additional aspects include cellulose packaging products with an improved resistance to bulk water intrusion or absorption. In certain embodiments, the cellulose packaging products disclosed herein are resistant to bulk water absorption, water vapor transmission, oxygen transmission, or a combination thereof. In embodiments, such paper products are capable of being recycled, composted, or a combination thereof.

[0033] Fig. 1 provides an elevated top perspective view a treated substrate 100 in accordance with one embodiment. Fig. 2 shows top perspective and exploded view of the treated substrate 100 of Fig. 1. As can be seen, the treated substrate 100, 200 includes a substrate 150 with a barrier composition 110 disposed upon at least one surface thereof.

[0034] Fig. 3 shows a side view of a treated substrate 200 under another embodiment, wherein the treated substrate 200 includes a barrier composition 110, 112 disposed upon at least two surfaces. Fig. 4 provides a top perspective and exploded view of the treated substrate 200 of Fig. 3. As shown in Figs. 3 and 4, certain embodiments relate to treated substrates 200, wherein the substrate 150 comprises a first surface 152 and a second surface 154, and each of the first and second surfaces are coated with the barrier composition 110, 112. In embodiments, the barrier composition 110 associated with the first surface 152 is substantially the same as the barrier composition 112 on the second surface 154. In alternate embodiments, the barrier composition 110 associated with the first surface 152 is different from the barrier composition 112 on the second surface 154.Attorney Docket No. 2967050.06. WO1Customer No. 190456

[0035] Although Figs. 1-5 show embodiments comprising a single substrate layer 150 and up to two barrier compositions 110, 112, it should be understood that alternate embodiments can comprise any number of substrates 150 or barrier compositions 110, 112 to create a treated substrate 100, 200 with a plurality of layers.

[0036] In various embodiments the barrier composition 110, 112 is configured to enhance the resistance of a treated cellulose substate to liquid intrusion or absorption. The barrier composition 110, 112 can be configured to mitigate the absorption of liquid in cellulose fibers. In addition, in certain embodiments, the barrier composition 110, 112 is configured to increase the strength, stiffness, durability, and rigidity of a cellulose substrate during use of the same.

[0037] The barrier composition 110, 112 can be configured to be added to a finished substrate having cellulose fibers. For example, the barrier composition 110, 112 can be a homogenous mixture having flowable or viscous consistency that can be deposited on the surface of a finished product or substrate 150. One or more rollers, flow coaters, or sprayers may be used as vehicles to deposit a layer of the barrier composition 110, 112 onto the finished product or substrate. In alternative or additional embodiments, the barrier composition 110, 112 can be mixed with or added to materials or ingredients of the substrate 150 during formation of the substrate 150.

[0038] In accordance with certain embodiments, the barrier composition 110, 112 comprises any one or more of pectin and an activator.

[0039] As shown in Fig. 5, the barrier composition 110 can comprise a first layer 114 that comprises pectin (also referred to herein as a “pectin layer”) applied directly to the substrate 150, and a second layer 116 that comprises an activator (also referred to herein as an “activator layer”), which can be applied over the pectin layer 114.Attorney Docket No. 2967050.06. WO1Customer No. 190456

[0040] In embodiments, the activator comprises a cross-linking agent. The crosslinking agent can be an organic acid, a calcium-based medium, or a combination thereof. The cross-linking agent can be any cross-linking agent that is suitable for use with products designed for human consumption. The organic acid can be a food-grade organic acid. In certain embodiments, the organic acid is oxalic acid, citric acid, lactic acid, acetic acid, tartaric acid, malic acid, fumaric acid, phosphoric acid, ascorbic acid, or the like. The calcium-based medium can be any cross-linking agent that comprises calcium. Calcium-based mediums for use in forming the presently disclosed barrier composition 110, 112 can comprise any one or more of: calcium chloride (CaCl2), calcium acetate (Ca(C2H3O2)2), calcium sulfate (CaSC>4), calcium carbonate (CaCO3), calcium gluconate (C12H24CaO12), calcium citrate (Ca3(C6H5O7)2), calcium phosphate (Ca3(PO4)2), or any combination thereof.

[0041] In embodiments the barrier composition 110, 112 comprises a solution. The concentration of pectin within the barrier composition can range from about 0.5% to about 99.5%. In embodiments, the concentration of pectin within the barrier composition ranges from about 3% to about 95%. The concentration of pectin within the barrier composition 110, 112 can be about 98% or less, about 90% or less, about 80% or less, about 70% or less, about 60% or less, about 50% or less, about 40% or less, about 30% or less, about 20% or less, about 10% or less, or about 5% or less. In one embodiment, the concentration of pectin in the barrier composition 110, 112 is between about 50% and about 1%. In embodiments, the concentration of pectin within the barrier composition 110, 112 ranges from about 3.0 wt.% to about 30.0 wt.%. In certain embodiments, the final concentration of pectin within the barrier composition 110, 112 ranges from about 5.0 wt.% to about 20.0 wt.%. The concentration of pectin within the barrier composition 110, 112 can be about 5.0 wt.%, about 6.0 wt.%, about 7.0 wt.%, about 8.0 wt.%, about 9.0 wt.%, about 10.0 wt.%, about 11.0 wt.%, about 12.0 wt.%, about 13 wt.%,Attorney Docket No. 2967050.06. WO1Customer No. 190456 about 14 wt.%, about 15 wt.%, about 16 wt.%, about 17 wt.%, about 18 wt.%, about 19 wt.%, or about 20 wt.%.

[0042] In embodiments, the amount of cross-linking agent / activator in the barrier composition 110, 112, depends, at least in part, on the amount of pectin in the barrier composition 110, 112. The amount of the cross-linking agent / activator can be directly proportional to the amount of pectin within the barrier composition 110, 112. In embodiments, the ratio of pectin to activator in barrier composition 110, 112 is about 2:1, about 3:1, about 4:1, about 5:1, about 6:1, about 7:1, about 8:1, about 9:1, or about 10:1. The ratio of pectin to activator can be up to about 20: 1.

[0043] In certain embodiments, the disclosure relates to treated cellulose substrates 100, 200 for use in finished products that are resistant to water vapor transmission, oxygen transmission, or a combination thereof.

[0044] Such finished products can be a paper product as discussed herein. Non-limiting examples of such paper products include food packaging materials, food service disposable materials, and other materials that may contact food surfaces. Exemplary paper products include plates, bowls, trays, containers, wraps, cups, lids, cutlery, liners, bags, filter paper, release liners, or other storage containers, food service materials, or packaging materials used in association with food or other consumable goods. However, the present disclosure should not be limited to paper products as the barrier composition 110, 112 may be added or otherwise applied to a variety of other substrates having fibers therein. Materials to which the barrier composition 110, 112 may be added to may include, for example, wood, plywood, OSB, plastic, metals, wallboard, cardboard, medium density fiberboard (MDF), and particle board, or any material or composite material that comprises cellulose fibers or other materials prone to water absorption. In one embodiment, the “treated substrate” can be any of the variousAttorney Docket No. 2967050.06. WO1Customer No. 190456 substrates or products disclosed or otherwise referenced in U. S. Provisional Application No.63 / 713,453 for “METHODS OF ASSOCIATING AN ADDITIVE WITH CELLULOSE FIBERS,” which is incorporated by reference in its entirety.

[0045] In embodiments, the thickness of the barrier composition layer 110, 112 on the surface of the treated substrate 100, 200 can be between about 0.0001 inches to about 0.25 inches. The thickness of the barrier composition layer 110, 112 on the treated substrate 100, 200 can be between about 0.01 inches to about 0.1 inches. The thickness of the barrier composition layer 110, 112 on the treated substrate 100, 200 is about 0.001 inches, about 0.002 inches, about 0.003 inches, about 0.004 inches, about 0.005 inches, about 0.006 inches, about 0.007 inches, about 0.008 inches, about 0.009 inches, about 0.01 inches, about 0.02 inches, about 0.03 inches, about 0.04 inches, about 0.05 inches, about 0.06 inches, about 0.07 inches, about 0.08 inches, about 0.09 inches, or about 0.1 inches.

[0046] In accordance with alternate embodiments, the barrier composition 110, 112 may be mixed into or otherwise added to a paper pulp mixture to create a treated substrate. The paper pulp mixture may include dry fibers of varying lengths and qualities depending on the desired characteristics of an intended use. In certain embodiments, the dry fibers may be cellulose fibers or the like. The paper pulp mixture may be mixed with a liquid, such as water to name one example, to form a slurry. The slurry may then be processed to produce a paper product.

[0047] The barrier composition 110, 112 may be configured to mitigate the absorption of liquid in one or more cellulose fibers. In addition, when the barrier composition 110, 112 is applied to or otherwise associated with a paper product, the paper product retains strength and / or stiffness when exposed to a liquid such as water, oil, or grease.Attorney Docket No. 2967050.06. WO1Customer No. 190456

[0048] One exemplary advantage of the present disclosure may be that a food storage container associated with the barrier composition 110, 112 may maintain improved strength and stiffness when exposed to liquid, either from condensation, exposure to oil, water, or grease, or otherwise, as compared to a food storage container that lacks the barrier composition 110, 112. Further advantages that a food storage comprised of a treated substrate exhibits a product with reduced water vapor transmission and oxygen exchange between the interior of the food storage container and the outside environment.

[0049] Any of the various layers or coating described herein can be added according to an of the deposition methods disclosed herein (e.g., deposited by roll coating, flow coating, spray coating, or any other method known in the art).Methods of Preparing a Barrier Composition and Methods of Making a Treated Substrate

[0050] In another aspect, embodiments of the present disclosure relate to methods of making a barrier composition 110, 112 in accordance with the embodiments disclosed herein.

[0051] In embodiments, the method of preparing the barrier composition comprises preparing a pectin solution 114. The step of preparing a pectin solution 114 can comprise adding a required amount of pectin to a measured amount of distilled water to create a pectin mixture. The ratio of water to pectin depends on the desired concentration of pectin within the final pectin solution. The method can further comprise heating the pectin mixture to about 60° C and stirring the solution until the pectin is completely dissolved to form the pectin solution 114.

[0052] The method can further comprise preparing an activator solution 116. In embodiments, preparing the activator solution comprises adding a required amount of activatorAttorney Docket No. 2967050.06. WO1Customer No. 190456 to a measured amount of distilled water and stirring until the activator is completely dissolved to form the activator solution 116.

[0053] Preparing the barrier composition can further comprise applying the pectin solution 114 over at least one surface of a substrate 150 and applying the activator solution 116 over the previously applied pectin solution 114 and permitting the pectin solution 114 and activator solution 116 to cure and form the barrier composition 110. In another aspect, embodiments of the present disclosure relate to methods of making a treated substrate 100, 200 such as by applying the barrier composition 110, 112 to a substrate 150.

[0054] In certain embodiments, barrier compositions 110, 112 are applied to at least one surface of a substrate 150 to create a treated substrate 100, 200. The treated substrate can be further processed according to methods known to one of skill in the art to create any of the various finished products disclosed herein.

[0055] The barrier composition 110, 112 can be applied in multiple layers. The barrier composition 110, 112 can be created via a two-part application process. By way of non-limiting example, a first layer 114 comprising pectin (also referenced to herein as a “pectin layer”) can be applied directly to at least one surface of the substrate 150, and a second layer 116 comprising an activator (also referred to herein as an “activator layer”) can be applied over the pectin layer 114. The pectin layer 114 can be applied over the substrate 150 and permitted to assume a substantially even distribution across at least one surface of the substrate such that the pectin layer 114 assumes the shape of the substrate surface to which the pectin layer 114 is applied. The activator layer 116 can then be applied over the pectin layer 114, which permits the pectin layer 114 to solidify during the curing process.

[0056] In embodiments, applying barrier compositions 110, 112 to substrates includes depositing flowable or viscous layers of a homogenous mixture of the barrier composition 110,Attorney Docket No. 2967050.06. WO1Customer No. 190456 112 onto a substrate 150. For example, one or more rollers, flow coaters, or sprayers may be used as vehicles to deposit a layer of the barrier composition 110, 112 onto a surface of the substrate 150. In one example, when the substrate 150 is passed between a feed roll and a coating roller, the barrier composition 110, 112 is deposited onto the substrate 150. The thickness of the layer of the barrier composition 110, 112 deposited may be controlled by adjusting the mechanical features of the coating machine such as the distance between rollers, the speed of roller rotation, and the rate at which the barrier composition 110, 112 is applied to the substrate 150.

[0057] In one embodiment, each layer of the barrier composition 110, 112 is applied to a substrate at a rate of between about 1 to 50 grams per square meter. The barrier composition 110, 112 can be applied at a rate of between about 5 to about 20 grams per square meter. In certain embodiments, the barrier composition 110, 112 is applied about 5 grams per square meter, about 6 grams per square meter, about 7 grams per square meter, about 8 grams per square meter, about 9 grams per square meter, about 10 grams per square meter, about 11 grams per square meter, about 12 grams per square meter, about 13 grams per square meter, about 14 grams per square meter, or about 15 grams per square meter.

[0058] Following deposition of the barrier composition 110, 112, the treated substrate 100, 200 can be subjected to a curing period, for a period of time sufficient to permit the barrier composition 110, 112 to cure or dry on the at least one surface of the treated substrate 100, 200. The treated substrate can then undergo processing (e.g., cutting, final forming, stacking, packing, shipping, or a combination thereof) to form a finished product.

[0059] In embodiments, the curing period can last as little as one second. The curing period can last up to about 5 hours. The curing period can be up to about 24 hours. In certain embodiments, the curing period is less than 8 hours. The curing period can be between about 5Attorney Docket No. 2967050.06. WO1Customer No. 190456 seconds and 8 hours. In various embodiments, the duration of the curing period is about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 5 hours, about 7 hours, or about 8 hours. The curing period can be between 1 minute and 60 minutes. In embodiments, the curing period is about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, or about 60 minutes. In embodiments, the curing period is less than about 1 minute. The curing period can be about 5 seconds, about 10 seconds, about 15 seconds, about 20 seconds, about 25 seconds, about 30 seconds, about 35 seconds, about 40 seconds, about 45 seconds, about 50 seconds, about 55 seconds, or about 60 seconds.

[0060] In embodiments, application of heat can accelerate the curing period. The substrate can be cured at a temperature between about 40° C to about 200° C. The temperature of the cure period can be between about 60° C to about 150° C. In certain embodiments, the cure period temperate is about 60° C, about 65° C, about 70° C, about 75° C, about 80° C, about 85 ° C, about 90° C, about 95° C, about 100° C, about 105° C, about 110° C, about 115° C, about 120° C, about 125° C, about 130° C, about 135° C, about 140° C, about 145° C, about 150° C.

[0061] In embodiments, the barrier composition 110, 112 can be applied directly to the substrate 150 as described above. In alternate embodiments, a binding layer can be applied to the substrate 150 prior to application of the barrier composition 110, 112, wherein the binding layer is configured to promote adhesion between the substrate 150 and the barrier composition 110, 112.

[0062] The treated substrate 100, 200 can be configured to be further processed via conventional manufacturing processes to create a finished product. For example, the treated substrate 100, 200 can be cut, shaped, molded, and / or formed into a desired product.Attorney Docket No. 2967050.06. WO1Customer No. 190456

[0063] The steps of the methods disclosed herein may be performed in any order and should not be limited to a sequence as disclosed herein.

[0064] The method of treating substrate 150 with barrier composition 110, 112 may result in a treated substrate 100, 200 having increased strength, stiffness, and / or liquid resistance. Without being bound by theory, the method may result in a treated substrate 100, 200 having at least three times the strength and / or stiffness of an untreated substrate. Again, without being bound by theory, the method may result in a treated substrate 100, 200 having at least three times the strength and / or stiffness of an untreated substrate when each substrate is exposed to a liquid such as water, oil, or grease.

[0065] Since other modifications and changes varied to fit particular operating requirements and environments will be apparent to those skilled in the art, the invention is not considered limited to the example chosen for purposes of disclosure and covers all changes and modifications which do not constitute departures from the true spirit and scope of this invention. This written description provides an illustrative explanation and / or account of the present invention. It may be possible to deliver equivalent benefits using variations of the specific embodiments, without departing from the inventive concept. This description and these drawings, therefore, are to be regarded as illustrative and not restrictive.

[0066] Even though particular combinations of features are recited in the present application, these combinations are not intended to limit the disclosure of the invention. In fact, many of these features may be combined in ways not specifically recited in this application. In other words, any of the features mentioned in this application may be included in this new invention in any combination or combinations to allow the functionality required for the desired operations.Attorney Docket No. 2967050.06. WO1Customer No. 190456

[0067] No element, act, or instruction used in the present application should be construed as critical or essential to the invention unless explicitly described as such. Further, the phrase “based on” is intended to mean “based, at least in part, on” unless explicitly stated otherwise.

[0068] The invention is further described by the following non-limiting Examples.Attorney Docket No. 2967050.06. WO1Customer No. 190456 EXAMPLES

[0069] Examples are provided below to facilitate a more complete understanding of the invention. The following examples illustrate the exemplary modes of making and practicing the invention. However, the scope of the invention is not limited to specific embodiments disclosed in these Examples, which are for purposes of illustration only, since alternative methods can be utilized to obtain similar results.

[0070] In various embodiments, the present disclosure relates to a, a biodegradable barrier coating composition for application on and use with fiber-based packaging materials. In embodiments, the barrier coating comprises pectin activated by a calcium-based medium or a food-grade organic acid. While keeping the substrate recyclable and biodegradable, the coating offers improved resistance to oil and grease absorption, increased water resistance, and reduced water vapor and oxygen transmission rates across a fiber-based packing material.

[0071] Fiber-based packaging materials such as paper, paperboard, and molded fiber are becoming increasingly popular due to their renewable and biodegradable characteristics. However, these materials frequently lack the necessary barrier protection against grease, water, oxygen, and moisture transmission, which is required for many packaging applications. Conventional barrier solutions are primarily composed of petroleum-derived synthetic polymers or metallized films. While effective, these petroleum-based materials raise environmental concerns due to their non-biodegradability and difficulties with recycling. There is an increasing demand for sustainable barrier coating solutions that can ensure package integrity while preserving the fiber substrate's eco-friendliness. The subject of the current disclosure resolves this need by creating a biodegradable barrier coating formulation with naturally derived pectin as the primary active ingredient, thereby overcoming the limitations of existing petroleum-based barrier products.Attorney Docket No. 2967050.06. WO1Customer No. 190456

[0072] In embodiments, the coating comprises 5-20% pectin, a naturally occurring polysaccharide that is activated by a food-grade organic acid or calcium-based crosslinking agents. For a given percentage of pectin, a given amount of citric acid or calcium chloride is used to crosslink the pectin to create a solid pectin-based coating. This formulation satisfied grease and water resistance standards when applied to a paper substrate at a rate of 5 to 20 grams per square meter and dried at 60 to 150 °C.

[0073] In various embodiments, the coatings and protective layers described herein can be used with paper products. The coatings are formulated for application on packaging (such as packaging for food, cosmetics, and consumer goods) while maintaining recyclability and biocompatibility. Its scalable application methods enable seamless integration into existing packaging processes.

Claims

1. Attorney Docket No. 2967050.

06. WO1Customer No. 190456ClaimsWhat is claimed is:

1. A multi-layered, treated substrate that is bulk water resistant and resistant to water vapor transmission and oxygen transmission, the treated substrate comprising:a cellulose substrate layer comprising a first surface; anda barrier composition layer comprising pectin and a cross-linking agent, wherein the multilayered, treated substrate is biodegradable.

2. The treated substrate of claim 1, wherein the cross-linking agent comprises a calcium-based medium, a food-grade organic acid, or a combination thereof.

3. The treated substrate of claim 2, wherein the food-grade organic acid is oxalic acid, citric acid, lactic acid, acetic acid, tartaric acid, malic acid, fumaric acid, phosphoric acid, ascorbic acid, or any combination thereof.

4. The treated substrate of claim 2, wherein the calcium-based medium is calcium chloride (CaCl2), calcium acetate (C C^FTO?)?), calcium sulfate (CaSC>4), calcium carbonate (CaCO3), calcium gluconate (C12H24CaO12), calcium citrate (Ca3(C6H5O7)2), calcium phosphate (Ca3(PO4)2), or any combination thereof.

5. The treated substrate of claim 1, wherein the concentration of pectin within the barrier composition is between about 5% and about 20%.

6. A barrier composition for use in creating a water-resistant cellulose substrate, the barrier composition comprising pectin and a cross-linking agent.

7. The barrier composition of claim 6, wherein the cross-linking agent comprises a calcium-based medium, a food-grade organic acid, or a combination thereof.Attorney Docket No. 2967050.

06. WO1Customer No. 190456 8. The barrier composition of claim 7, wherein the food-grade organic acid is oxalic acid, citric acid, lactic acid, acetic acid, tartaric acid, malic acid, fumaric acid, phosphoric acid, ascorbic acid, or any combination thereof.

9. The barrier composition of claim 7, wherein the calcium-based medium is calcium chloride (CaCl2), calcium acetate (Ca^HsCh)?), calcium sulfate (CaSC>4), calcium carbonate (CaCO3), calcium gluconate (C12H24CaO12), calcium citrate (Ca3(C6H5O7)2), calcium phosphate (Ca3(PO4)2), or any combination thereof.

10. The barrier composition of claim 6, wherein the concentration of pectin within the barrier composition is between about 5% and about 20%.

11. A method of associating a barrier composition with cellulose fibers, the method comprising:preparing the barrier composition, the barrier composition comprising pectin and a crosslinking agent, wherein the cross-linking agent comprises a calcium-based medium, a food-grade organic acid, or a combination thereof; andassociating the barrier composition with the cellulose fibers.

12. The method of claim 11, wherein the food-grade organic acid is oxalic acid, citric acid, lactic acid, acetic acid, tartaric acid, malic acid, fumaric acid, phosphoric acid, ascorbic acid, or any combination thereof.

13. The method of claim 11, wherein the calcium-based medium is calcium chloride (CaCl2), calcium acetate (CafC^FTCh)?), calcium sulfate (CaSC>4), calcium carbonate (CaCO3), calcium gluconate (C12H24CaO12), calcium citrate (Cas^eHsO?^), calcium phosphate (Ca3(PO4)2), or any combination thereof.

14. The method of claim 11, wherein the concentration of pectin within the barrier composition is between about 5% and about 20%.

15. A method of applying a barrier composition to a substrate, the method comprising:Attorney Docket No. 2967050.

06. WO1Customer No. 190456 applying a pectin layer to at least one surface of a substrate; andapplying an activator over the pectin layer, wherein the pectin layer comprises pectin and the activator layer comprises a cross-linking agent.

16. The method of claim 15, wherein the cross-linking agent comprises a calcium -based medium, a food-grade organic acid, or a combination thereof17. The method of claim 16, wherein the food-grade organic acid is oxalic acid, citric acid, lactic acid, acetic acid, tartaric acid, malic acid, fumaric acid, phosphoric acid, ascorbic acid, or any combination thereof.

18. The method of claim 16, wherein the calcium-based medium is calcium chloride (CaCl2), calcium acetate (CafC^FTChk), calcium sulfate (CaSC>4), calcium carbonate (CaCO3), calcium gluconate (C12H24CaO12), calcium citratecalcium phosphate (Ca3(PO4)2), or any combination thereof.

19. The method of claim 15, wherein the concentration of pectin within the barrier composition is between about 5% and about 20%.

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