Squeezable fibrous based bottle containing a personal care composition

By combining a pulp molding base and fiber-based sidewalls, along with inorganic barrier and extrudable design, the problem of pulp-molded paper bottles containing and distributing viscous liquids in humid environments has been solved, resulting in extrudable fiber-based bottles with high recyclability and long shelf life.

CN122138773APending Publication Date: 2026-06-02PROCTER & GAMBLE CO

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
PROCTER & GAMBLE CO
Filing Date
2024-10-11
Publication Date
2026-06-02

AI Technical Summary

Technical Problem

Existing pulp molded paper bottles are difficult to effectively contain and dispense viscous liquid products in humid environments, and are prone to delamination and weakening of adhesion during repeated opening and closing, affecting shelf life and recyclability.

Method used

The extrudable fiber-based bottle is manufactured using a combination structure of pulp molding base and fiber-based sidewalls, combined with inorganic barrier structure and extrudable design, through wet or dry molding process. Inorganic coatings and barrier materials are used to improve moisture and oxygen barrier properties, and the bottle body is sealed by a narrow-mouth valve to control the distribution.

Benefits of technology

It enables effective containment and on-demand dispensing of viscous liquids in humid environments, maintains bottle integrity, extends shelf life, and improves product recyclability and bio-based content, meeting shelf-life requirements of 6 months to 2 years.

✦ Generated by Eureka AI based on patent content.

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Abstract

A squeezable fiber-based bottle for use with a liquid personal care composition comprising a pulp-molded base and pulp sidewalls, wherein the liquid personal care composition comprises about 14% to about 50% water; about 20% to about 70% a wetting agent; and wherein a water activity (Aw) of about 0.40 to about 0.90 is present. The pulp-molded base includes a liquid-receiving surface having orifices for dispensing a viscous liquid and a base periphery having a peripheral surface having an upper edge and a lower edge. A base barrier structure is disposed on the upper edge of the liquid-receiving surface and the base periphery. The fiber-based sidewalls have an upper edge, a lower edge, an inner surface, and an outer surface. The inner surface includes a fiber-based sidewall barrier structure. The lower edge of the fiber-based sidewall is attached to the pulp-molded base to form an impermeable seal. The impermeable seal is formed near the upper edge of the peripheral surface around the entire peripheral surface of the pulp-molded base, but not near the lower edge of the peripheral surface. The orifice for dispensing viscous fluid includes a separable slit valve disposed opposite to the liquid-containing surface. This separable slit valve is formed of plastic or other resin material.
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Description

Technical Field

[0001] A squeezable fiber-based bottle, in combination with a personal care composition having low water activity and low water content, is used for storing and dispensing viscous liquid products on demand in humid environments. In this invention, the squeezable fiber-based bottle may be recyclable. Background Technology

[0002] Since the industrial age, plastic products have been widely used in daily life. Due to their relatively low production costs and versatility, plastic packaging materials have experienced a higher growth rate in the global market compared to other packaging materials. However, most of the plastics we see on the market are made from non-renewable sources of natural crude oil. Despite continuous improvements in waste management infrastructure, plastic packaging is sometimes not recycled after use, thus leaking into the environment and potentially persisting there. Plastic pollution is prompting increasingly stringent scrutiny of plastic use and the emergence of new environmental regulations that restrict the use of plastics in packaging, especially for short-life applications.

[0003] Packaging made from natural cellulose fibers has become an area of ​​increasing interest, as part of the overall trend towards renewable and less durable raw materials. Pulp packaging also typically boasts very high recyclability. Cellulose products are often formed into films or multilayer boards using papermaking processes, or into 3D shaped objects using pulp molding methods. While pulp provides excellent structural support and a good decorative surface, its poor oxygen and moisture barrier properties, along with its poor liquid containment characteristics, lead to a loss of integrity, making individual sheets or shaped objects unsuitable for packaging liquid products. Therefore, after manufacturing cellulose products, a protective coating is usually applied to the inside to extend the shelf life of the packaged liquid product.

[0004] Liquid packaging sheets (LPBs) are typically laminated with a heat-sealable polymer (such as PE) within a structure that may include one or more barrier structures (such as EVOH, vacuum metallized alumina, etc.), or may be coated with a thin layer applied using dispersion techniques (such as spraying, roller coating, dip coating, blade coating, or curtain coating). However, such coatings present a trade-off between barrier performance and packaging recyclability. Sheets can be formed using high-speed manufacturing processes to manufacture packaging such as cartons, cans, or paper tubes. Cartons or cans are suitable for dispensing pourable liquids but not for dispensing viscous formulations (such as those used in cosmetics and personal care). Current paper tubes (including liquid sheets) require significant amounts of plastic due to the inclusion of plastic components necessary to provide reclosability and dispensing control. Furthermore, the hygroscopic nature of pulp poses additional challenges for pulp packaging applications in humid or damp environments (such as shower or bathroom applications). Liquid packaging boards typically contain high levels of adhesives (such as alkyl ketene dimer (AKD)) to increase hygroscopicity, but are susceptible to in-plane edge wicking, which is usually caused by liquid being drawn into the cut edges via capillary action. This liquid wicking leads to delamination and exposure of unbonded fiber-to-fiber bonds and / or weakening of layer-to-layer adhesions, resulting in the separation of multilayer surfaces.

[0005] Packaging made from rigid pulp molding, such as bottles, is less susceptible to edge wicking. Compared to liquid packaging sheets, pulp molding also allows for greater shape and material selection freedom. To achieve the desired liquid containment, moisture, and oxygen barrier properties, bottles can be coated with a thin plastic liner, for example, by blow molding, rotational molding, or spraying. Pulp molding pulp can also contain additives to modify the properties of the cellulose material, such as porosity, adhesiveness, or wet strength. As with paper, the inclusion of such liner, coating, and additives presents a trade-off between recyclability and barrier performance. Furthermore, high fiber content in functional accessories such as necks and closures presents challenges due to the high forming tolerances required for multiple open / close cycles and the reliability of coating integrity. Current pulp molding bottle manufacturing processes require plastic pumps to control and carefully dispense the viscous formulation because bottles are typically produced with large neck openings and rigid side panels.

[0006] The goal is to maximize the bio-based fiber content in packaging to improve bio-based renewable content and recycling rates in fiber reprocessing. It is also desirable to maximize the bio-based fiber content in packaging to create articles with varying mechanical properties across different areas of the product. For example, bottles made of plastic could be formed with rigidity relative to top loading while also including a flexible panel that the user can squeeze to dispense the product. Increasing fiber inclusions is also desired to achieve product recycling rates exceeding 95% and to flatten the bottle upon disposal, which facilitates sorting and the circular economy. Fiber-based bottles are expected to minimize plastic inclusions while offering unique design shapes, providing a reasonable shelf life of at least 6 months to 2 years, shower usability, and recyclability. Extrudable pulp fiber-based bottles are expected to be suitable for use in humid environments, maintaining integrity while containing liquid formulations, enabling on-demand dispensing, offering excellent ergonomics in use, exhibiting a reasonable shelf life, and optimizing recycling and disposal.

[0007] Because sufficiently thick barrier structures and coatings are required to maintain adequate liquid containment and a shelf life of 6 months to 2 years, placing today's liquid shampoos or other personal care formulations in squeezable fiber-based bottles limits the maximum level of fiber content. This invention identifies a method for containing liquid shampoos and other personal care products in squeezable fiber-based bottles that maximizes fiber content while maintaining a reasonable product shelf life. Summary of the Invention

[0008] This invention relates to a squeezable fiber-based bottle for use with a liquid personal care composition, the liquid personal care composition comprising: a pulp-molded base including a liquid-receiving surface having orifices for dispensing a viscous liquid, the pulp-molded base having a base periphery having peripheral surfaces including an upper edge and a lower edge, a base barrier structure disposed on the liquid-receiving surface and the upper edge of the base periphery; and a fiber-based sidewall having an upper edge, a lower edge, an outer surface, and an inner surface, the inner surface including a fiber-based sidewall barrier structure, wherein the... The lower edge of the fiber-based sidewall surrounds the entire peripheral surface of the pulp molding base and is attached near the upper edge of the peripheral surface but not near the lower edge of the peripheral surface, thereby forming an impermeable seal. The lower edge of the peripheral surface of the pulp molding base is below the liquid-containing surface, thereby allowing the squeezable fiber-based bottle to stand upright. The liquid personal care composition comprises about 14% to about 50% water; about 20% to about 70% a wetting agent; and contains about 0.40 to about 0.90 water activity (Aw). Attached Figure Description

[0009] Although claims that are specifically pointed out and clearly claimed after the specification are provided, the exemplary embodiments of the invention are believed to be better understood from the following description taken in conjunction with the accompanying drawings, wherein: Figure 1a This is a perspective view of the extrudable fiber-based bottle according to this disclosure.

[0010] Figure 1b yes Figure 1a Cross-sectional view of an extrudable fiber-based bottle.

[0011] Figure 1c It is used for Figure 1b A cross-sectional view of the pulp molding base of the bottle.

[0012] Figure 2a This is an exploded view of the bottom portion of the extrudable fiber-based bottle according to this disclosure.

[0013] Figure 2b This is a perspective view of a separable orifice valve according to this disclosure.

[0014] Figure 3a This is a cross-sectional view of the pulp molding base before the assembly of the pulp molding base barrier layer.

[0015] Figure 3b It is after the pulp molding base barrier layer is assembled. Figure 3a A cross-sectional view of the pulp molding base in the image.

[0016] Figure 3c This is a cross-sectional view showing the final assembly of the pulp molding base barrier layer.

[0017] Figure 4a This is a perspective view of an extrudable fiber-based bottle having a cylindrical tubular structure according to the present disclosure, the cylindrical tubular structure having an open end opposite to a pulp molding base.

[0018] Figure 4b Based on this disclosure Figure 4a A perspective view of an extrudable fiber-based bottle having a closed end opposite a pulp molding base.

[0019] Figure 4c Based on this disclosure Figure 4a and Figure 4b The bottom view of the extrudable fiber-based bottle is shown.

[0020] Figure 4d Based on this disclosure Figure 4b The side view of the extrudable fiber-based bottle is shown.

[0021] Figure 5aThis is a cross-sectional view of the lower portion of the squeezeable bottle according to this disclosure.

[0022] Figure 5b The cross-sectional view of the lower portion of the squeezeable bottle according to this disclosure shows the barrier structures on the inner and outer surfaces of the sidewalls.

[0023] Figure 5c The cross-sectional view of the lower portion of the squeezeable bottle according to this disclosure shows the barrier structure on the liquid-containing surface and bottom surface of the pulp molding base.

[0024] Figure 6a A perspective view of the upper edge of the sidewall of a compressible fiber-based bottle according to the present disclosure is shown, the bottle having an edge seal formed by a single folded edge protector.

[0025] Figure 6b A perspective view of the upper edge of the sidewall of a compressible fiber-based bottle according to the present disclosure is shown, the bottle having an edge seal formed by a double-folded edge protector.

[0026] Figure 6c A perspective view of the upper edge of the sidewall of a compressible fiber-based bottle according to the present disclosure is shown, the bottle having an edge seal formed by a saddle-shaped folded edge protector.

[0027] Figure 6d A perspective view of the upper edge of the sidewall of a compressible fiber-based bottle according to the present disclosure is shown, the bottle having an edge seal formed by a triple-folded edge protector.

[0028] Figure 7a The image is a perspective view of an extrudable fiber-based bottle according to the present disclosure, the bottle having an open end opposite a pulp molding base.

[0029] Figure 7b The image shows a cross-sectional view of an extrudable fiber-based bottle with a cylindrical tubular structure according to the present disclosure, the cylindrical tubular structure having an open end opposite to a pulp molding base.

[0030] Figure 7c Based on this disclosure Figure 7b The image shows a perspective view of an extrudable fiber-based bottle with a closed end opposite a pulp molding base.

[0031] Figure 7d It is used to form according to this disclosure Figures 7a to 7c A plan view of the blank for the side panel of the squeezeable bottle.

[0032] Figure 7e Based on this disclosure Figures 7a to 7c The diagram shows a cross-sectional view of the side panel of the squeezeable bottle.

[0033] Figure 8a This is a perspective view of an extrudable fiber-based bottle according to the present disclosure, the bottle having a molded side panel.

[0034] Figure 8b Based on this disclosure Figure 8a The cross-sectional view of the extrudable fiber-based bottle is shown.

[0035] Figure 8c Based on this disclosure Figure 8b The perspective view of the cross-section shown.

[0036] Figure 9a This is a perspective view of the extrudable fiber-based bottle according to this disclosure.

[0037] Figure 9b Based on this disclosure Figure 9a The cross-sectional view of the pulp molded bottle is shown.

[0038] Figure 10a The image is a perspective view of an extrudable fiber-based bottle according to the present disclosure, the bottle having an open end opposite a pulp molding base.

[0039] Figure 10b Based on this disclosure Figure 10a The cross-sectional view of the extrudable fiber-based bottle is shown.

[0040] Figure 10c Based on this disclosure Figures 10a to 10b The diagram shows a perspective view of an extrudable fiber-based bottle with a closed, sealed end opposite a pulp molding base.

[0041] Figure 10d Based on this disclosure Figure 10c The diagram shows a cross-sectional view of an extrudable fiber-based bottle with a closed, sealed end opposite a pulp molding base.

[0042] Figure 11a It is a cross-sectional view of the pulp molding base according to this disclosure.

[0043] Figure 11b This is a bottom view of the pulp molding base according to this disclosure.

[0044] Figure 12 This is an exploded perspective view of the pulp molding base according to this disclosure.

[0045] Figure 13 This is a cross-sectional view of the lower portion of the squeezeable bottle according to this disclosure.

[0046] Figure 14 This is a cross-sectional view of the lower portion of the squeezeable bottle according to this disclosure.

[0047] Figure 15This is a cross-sectional view of the lower portion of the squeezeable bottle according to this disclosure.

[0048] Figure 16 This is a graph showing the average weight change (gm / sqm / day) of a fiber-based bottle containing the liquid personal care composition of the present invention and a fiber-based bottle containing water. Detailed Implementation

[0049] The invention can be more readily understood by referring to the following detailed description of exemplary and preferred embodiments. It should be understood that the scope of the claims is not limited to the specific components, methods, conditions, apparatus, or parameters described herein, and the terminology used herein is not intended to limit the invention protected by the claims. Furthermore, as used in the specification including the appended claims, the singular forms “a,” “an,” and “the,” and “the,” also include the plural, and reference to a particular numerical value includes at least that particular value, unless the context explicitly specifies otherwise. When indicating a range of values, another embodiment includes starting from one particular value and / or ending at another particular value. Similarly, when a value is expressed as an approximation using the antecedent “about,” it should be understood that the particular value forms another embodiment. All ranges are inclusive and composable.

[0050] The purpose of this invention is to provide a compressible fiber-based bottle for liquid compositions containing 85%+ fiber content, which is resizing, capable of emptying more than 95% of the product, can be flattened during disposal, can be dispensed via a self-sealing valve, and can withstand dispensing, storage and use in humid environments.

[0051] Another object of the present invention is to provide a squeezeable bottle having a collapsible pulp sidewall, which is molded as a single component.

[0052] Another objective is to provide a squeezable bottle with collapsible molded pulp sidewalls that can be filled from the top and sealed similarly to a cosmetic tube.

[0053] Another objective is to provide a compressible pulp molded bottle that is formed as a single unit.

[0054] Another object of the present invention is to provide a removable valve that a consumer can separate from the bottle before disposing of it.

[0055] As used in this article, “pulp” is defined as a fibrous material produced by separating fibers from a sustainable source through mechanical or chemical methods and then suspending them in a fluid.

[0056] As used in this article, “fiber” is defined as a natural substance of wood or plant origin that is significantly longer than it is wide.

[0057] Unless otherwise specified, all percentages and ratios used herein are by weight of the total composition. Unless otherwise specified, all measurements are to be understood as being performed under ambient conditions, where “ambient conditions” means conditions at about 25°C, at about one atmosphere, and at about 50% relative humidity. All numerical ranges are narrower ranges including endpoints; the upper and lower limits of the ranges described are combinable to form additional ranges not explicitly described.

[0058] The compositions of the present invention may comprise, and optionally comprise, the basic components described herein, as well as optional ingredients, substantially consisting of or composed of them. As used herein, “substantially consisting of” means that the composition or component may contain additional ingredients, provided that the additional ingredients do not substantially alter the essential and novel features of the composition or method protected by the claims.

[0059] As used with respect to the composition, “apply” or “spread” means applying or spreading the composition of the present invention onto keratinized tissue such as hair.

[0060] "Dermatologically acceptable" means that the composition or component is suitable for contact with human skin tissue without undue toxicity, incompatibility, instability, allergic response, etc.

[0061] "Safe and effective amount" refers to an amount of compound or composition that is sufficient to significantly induce positive and beneficial effects.

[0062] In the context of this invention, the term "preservative effect" refers to preventing or delaying product deterioration caused by microorganisms present in the product or composition. In the context of this invention, "preservative agent" or "preservative" is a substance that prevents or delays the growth of microorganisms in a product or composition.

[0063] Although this specification concludes with a claim that specifically points out and clearly claims protection for the invention, it is believed that the invention will be better understood through the following description.

[0064] As used in this article, the term "fluid" includes both liquids and gels.

[0065] As used herein, “includes / contains” means that other steps and other components may be added without affecting the final result. This term encompasses the terms “consisting of” and “substantially consisting of”.

[0066] As used herein, “mixture” is intended to include simple combinations of substances and any compounds that may be produced by such combinations.

[0067] As used herein, unless otherwise specified, “molecular weight” refers to weight-average molecular weight. Molecular weight is measured using industry-standard methods, gel permeation chromatography (“GPC”).

[0068] Given a range of concentrations, these should be understood as the total amount of the components in the composition, or, if more than one substance falls within the range of the component definition, the total amount of all components in the composition conforms to the definition.

[0069] For example, if a composition contains 1% to 5% fatty alcohol, a composition containing 2% stearyl alcohol and 1% cetyl alcohol and no other fatty alcohols will fall within this range.

[0070] The amount of each specific ingredient or mixture thereof described below may be up to 100% (or 100%) of the total amount of ingredients in a personal care composition.

[0071] As used herein, “personal care compositions” include liquid compositions such as shampoos, shower gels, liquid hand cleansers, hair colorants, facial cleansers, and other surfactant-based liquid compositions.

[0072] As used herein, the terms “including,” “comprising,” and “containing” are intended to be non-restrictive and are understood to mean “having,” “possessing,” and “covering,” respectively.

[0073] Unless otherwise stated, all percentages, parts, and ratios are based on the total weight of the compositions of the present invention. All these weights relating to the listed ingredients are based on the content of the active substance and therefore do not include carriers or byproducts that may be contained in commercially available substances.

[0074] Unless otherwise specified, all component or composition levels refer to the active portion of the component or composition and do not include impurities, such as residual solvents or byproducts, that may be present in commercially available sources of such components or compositions.

[0075] It should be understood that each maximum numerical limit given throughout this specification includes each lower numerical limit, as such lower numerical limits are explicitly stated herein. Each minimum numerical limit given throughout this specification will include each higher numerical limit, as such higher numerical limits are explicitly stated herein. Each numerical range given throughout this specification will include each narrower numerical range falling within such a wider numerical range, as all such narrower numerical ranges are explicitly stated herein.

[0076] Figure 1 and Figure 1a An exemplary extrudable fiber-based bottle 10 is shown. The extrudable fiber-based bottle 10 includes a fiber-based sidewall 12 having an upper edge 14, a lower edge 16, an inner surface 18, and an outer surface 19. The inner surface 18 of the fiber-based sidewall 12 includes a liquid-containing material. The lower edge 16 is attached to a pulp molding base 20. Figure 1bAs shown, the pulp molding base 20 includes a liquid-containing surface 28 having a base barrier structure 40 and a hole 30 disposed at the center of the liquid-containing surface 28 for dispensing viscous liquid contained in the extrudable fiber-based bottle 10.

[0077] Figure 2a This is a unfolded view showing the lower edge 16 of the pulp molding sidewall 12, the base barrier structure 40, and the pulp molding base 20 before assembly. As shown, the pulp molding base 20 includes a base periphery having a peripheral surface 22, which has the same upper edge 24 and lower edge 26 as the upper edge 24 and lower edge 26 of the pulp molding base 20.

[0078] The pulp molding base 20 can be formed using a wet pulp molding process. This process begins with the preparation of a pulp, which involves dispersing fibers and additives in water. In this document, the terms fiber raw material, pulp raw material, and pulp are used synonymously and are completely interchangeable. As used herein, "pulp" is a fiber suspension that may consist of 0.5%–10% cellulose fibers, with the remainder being water and additives. As explained in WO2018 / 020219, a higher fiber content affects the flow characteristics of the suspension, making it difficult to transport the suspension and achieve a uniform coating on the mold. In this invention, the concentration of the fiber material in the suspension may be about 1%. In a wet molding process, the pulp is deposited onto a screen mold to form a layer by spraying or, more commonly, by immersing the mold and subsequently applying a vacuum to the back of the screen mold. In the second step, the pulp layer is pressed onto a tool comprising two mating tooling parts, one of which may have a porous wall that contacts the pulp layer and through which a vacuum can be applied to reduce the water content. Following this pressing step, the molded article is dried in a heated mold or oven. After the heating process, the water content may still be approximately 10%-20%. Subsequent pressing operations can then be performed on the article, applying heat to reduce surface roughness and porosity, and further reducing the water content to below 8%, below 5%, or below 1%. The wet-molded part has a substantially uniform wall thickness. The average wall thickness of wet-molded parts using this process can vary between 0.6 mm and 1.2 mm, and may be approximately 0.8 mm to 1.0 mm. Localized variations in thickness and density within the part may be desirable to improve assembly with other components or to provide robust support during assembly. Several established techniques exist for achieving localized variations in thickness and density in wet pulp molding processes. EP1081285 discloses the use of a split mold with multiple hollow chambers, where suction pressure can be controlled independently: this allows for variation in the amount of pulp fiber deposited in different parts of the chamber to produce thicker areas. EP1081285 also discloses areas in the mold where pulp slurry may stagnate to increase wall thickness. EP0656444 discloses the use of a mesh with different orifice sizes to control the water flow rate through different areas of the mold: this variation in flow rate results in variations in pulp deposition thickness. EP0656444 also discloses a method in which the size, spacing, and / or arrangement of discharge orifices are used to vary part thickness. WO2023104711 describes how localized variations in thickness and / or density can be achieved using localized mechanical compression, ultrasonic treatment, and / or heating. Protruding edges can be trimmed as needed after the pulp molding process.

[0079] Cellulose fibers can be wood or non-wood. Wood fibers can be long fibers from coniferous trees, such as pine, spruce, fir, and hemlock, or short fibers from hardwood trees, such as birch, eucalyptus, poplar, acacia, and oak. Non-wood plant fibers can generally be categorized into coniferous substitutes, such as cotton staple fiber and linters; flax and kenaf bast fibers; sisal; abaca; bamboo (longer fiber varieties); and hardwood substitutes, such as cereal straw, sugarcane, bagasse, bamboo (shorter fiber varieties), reeds and grasses, fine-stemmed needlegrass, kenaf (whole stem or core fiber), corn stalks, sorghum stalks, etc. Fiber formulations are typically selected to optimize dehydration and production cycle time, mechanical properties such as burst strength, and surface finish (roughness and porosity). Depending on the desired properties of the final part, fibers can include both short and long fibers. Fibers can be extracted using bleached or unbleached chemical or mechanical methods. Fibers may include recycled fibers.

[0080] The slurry may include additives for process control or functional enhancement. Typical additives for process control include retention aids, defoamers, pH adjusters, and viscosity control agents. Additives for functional enhancement include (1) fillers, such as inorganic mineral fillers; (2) adhesives, such as alkyl ketone dimers (AKD), alkenyl succinic anhydride (ASA), rosin, or lignin; (3) additives for enhancing dry strength, such as starch, amphoteric, cationic, or anionic polyacrylamide resins, enzymes, or modified polyamines; (4) additives for enhancing wet strength, such as polyamide (PAE) or polyamine epichlorohydrin, epoxide or cationic glyoxylate resins, or (5) microfibrillated cellulose (MFC) or cellulose nanocrystal (CNC) additives. In cases where a barrier structure is applied by spraying or dip coating, the present invention may include the addition of a quantity of inorganic mineral filler to the slurry to seal pores in the surface. In the present invention, the inorganic mineral filler particles may be selected from calcium carbonate and flaky kaolin or any mixture thereof.

[0081] In this invention, based on dry fiber count, the slurry may contain 0.5% to 2% AKD, possibly about 1% AKD, to provide some water resistance. In this invention, alkenyl succinic anhydride (ASA) or rosin emulsions may be used. The slurry may also contain less than 0.5% PAE or glyoxal polyacrylamide (GPAM) to provide wet strength to the final product. In this invention, based on dry fiber count, the slurry may contain 2% to 5% MFC, possibly 3% to 4% MFC, to improve surface smoothness, stiffness, burst resistance, and wet strength for barrier applications. Examples of commercially available MFCs include Curran or Fiberlean. This addition is particularly advantageous for improving the barrier effectiveness of spray or dip coatings by reducing surface porosity to prevent coating penetration.

[0082] In this invention, the pulp molding base 20 can be functionalized post-molding by vapor deposition of an inorganic barrier structure. Functionalization here should be understood as altering the properties of the molded part, such as increasing hygroscopicity or wet strength, through surface, morphological, and chemical modifications of the cellulose fibers. Suitable vapor-deposited inorganic coatings can be formed on the pulp fibers by metals or oxides and related compounds. The inorganic barrier structure can be optically opaque, translucent, or transparent, depending on the specific chemical properties applied. Typically, metal barrier structures such as aluminum will produce opaque barrier structures, while metal oxide barrier structures such as alumina or silicon dioxide will produce transparent barrier structures. In this invention, suitable inorganic coatings can be formed by vapor deposition of metals, including but not limited to aluminum, magnesium, titanium, tin, indium, silicon, carbon, gold, silver, chromium, zinc, copper, cerium, hafnium, tantalum, and diamond-like carbon. In this invention, suitable inorganic coatings can be formed by vapor deposition of metal oxides, metal nitrides, and related compounds. As used herein, metal oxides include aluminum oxide (e.g., Al2O3), aluminum carbide, aluminum nitride, magnesium oxide, titanium oxide (such as titanium dioxide, titanium oxide (3), or titanium monoxide), zinc oxide, tin oxide, yttrium oxide, or zirconium oxide (e.g., zirconium monoxide), calcium oxide, boron oxide, or metal-like oxides (such as silicon oxide, silicon carbide, and silicon nitride). Silicon oxide coatings or nitride-based coatings may also be coatings selected from the group consisting of SiOX (where x is an integer from 1 to 4) or SiOXNY (where each of x and y is an integer from 1 to 3). The barrier structure may be a single-component vapor-deposited layer comprising at least one of the above groups, or a two-component vapor-deposited layer comprising at least one combination of two components selected from the group consisting of SiOx / Al2O3, SiO / ZnO, SiO / CaO, SiO / B2O3, and CaO / Ca(OH)2. It is understood that various processes can be used to vapor-deposit metals and metal oxides. For example, chemical vapor deposition (CVD) or physical vapor deposition (PVD) processes can be used to vapor-deposit metal or metal oxide coatings. Generally, most CVD processes are suitable due to the stability of metals, metal oxides, and metal oxide precursors. In this invention, plasma-assisted CVD can be used to form vapor-deposited inorganic coatings. In this invention, atomic layer CVD can be used. In this invention, the inorganic barrier coating can have a thickness of 2 nm to 1,000 nm, a thickness of 10 nm to 200 nm, and a thickness of 20 nm to 100 nm. It has been found that this functionalization can significantly increase wet strength, improve overall moisture barrier properties, and increase contact angle while maintaining recyclability. This effect is further enhanced when these deposition processes are used in high-density pulp matrices, especially when combined with high-refined pulps, MFC, or CNC.

[0083] In this invention, the pulp molding base 20 can be molded using a wet pulp molding process with rapid dewatering and pulse drying, as disclosed by Celwise in WO2020 / 016409 and US 2021 / 0269983, which are incorporated herein by reference. It has been found that this process produces parts with higher strength and hydrophobicity compared to parts formed by conventional wet molding. Without being bound by theory, it is presumably due to the rapid dewatering enabling the cellulose fibers to quickly recombine with each other, and the high-pressure / high-temperature process enhancing lignin polymerization.

[0084] In this invention, the pulp molding base 20 can be molded using a dry molding method. According to this process, air is used as the transport medium (“airflow web”) to transport cellulose fibers and form a preform. The preform is then formed in a press at a temperature above 100°C and a pressure of at least 1 MPa. According to this process, additives such as adhesives can be sprayed in solid form or added to the cellulose fibers and / or the cellulose preform. Pulpac discloses an example of this process in SE541995, SE1851373, and SE543410. Dry molding is advantageous compared to conventional wet molding because it reduces cycle time and energy consumption by eliminating the need for drying. Parts manufactured using this method have been found to be both strong and very flexible. This is presumably due to the lower degree of hydrogen bonding between fibers. In this invention, as demonstrated by SACMI, pulp molding bases can be achieved using dry pressing with an all-metal isostatic mold to allow for a wide variety of shapes, including the ability to mold parts with undercuts, while achieving a good degree of dimensional control.

[0085] like Figure 1c As shown, the pulp molding base 20 includes a base barrier structure 40 disposed on a liquid-receiving surface 28 and a peripheral surface 22 adjacent to the upper edge 24 of the pulp molding base 20. The lower edge 16 of the fiber-based sidewall 12 is attached to the pulp molding base 20, thereby forming an impermeable seal 42. The impermeable seal 42 is formed near the upper edge 24 of the peripheral surface around the entire peripheral surface 22 of the pulp molding base 20, but not near the lower edge 26 of the peripheral surface. In this invention, the impermeable seal 42 can be formed by welding, such as by exposing the area to hot air. However, other methods of forming an impermeable seal, such as ultrasonication, are contemplated. In this invention, the lower edge 16 of the fiber-based sidewall 12 may be at least 1 mm from the lower edge 26 of the peripheral surface. The peripheral surface 22 of the pulp molding base 20 may include a flange 25 to receive the lower edge 16 of the fiber-based sidewall 12. The flange 25 may be at least 1 mm from the lower edge 26 of the peripheral surface.

[0086] like Figure 1c and Figure 2a As shown, an orifice 30 for dispensing a viscous fluid extends into a conduit 32 disposed on a bottom surface 27 of a pulp molding base 20, which is the side opposite to a liquid-containing surface 28. The conduit 32 includes a conduit opening 34 and a flexible, resilient, narrow-mouth valve 50 disposed on the conduit opening 34. The narrow-mouth valve 50 is configured to (1) allow fluid flow in response to a predetermined discharge pressure within the bottle when squeezed, and (2) automatically close to cut off the flow when the pressure decreases. Such a valve and designs of fittings using such a valve are shown in U.S. Patent Nos. 5,271,732, 5,927,446, 5,942,712, 6,545,901, and 10,287,066. The narrow-mouth valve can be selected based on the desired dispensing experience and product viscosity to adjust the sealing pressure, rupture pressure, and flow rate versus pressure curve. In this invention, the product viscosity can be between 3,000 cps and 10s. -1 Up to 30,000 cps in 10 seconds -1 Between, it can be between 5,000 cps and 10s. -1 Up to 20,000 cps in 10 seconds -1 The narrow-mouth valve 50 may be molded from a flexible, elastic material and is inert to the fluid product being packaged and dispensed. In this invention, the narrow-mouth valve 50 may be molded from liquid silicone rubber. Examples of commercially available silicone rubber grades include DC-99-525 and RBL-9525-54, sold by Dow Corning Corp. Valve 50 may include other elastomers, such as synthetic, thermosetting, or thermoplastic polymers or thermoplastic elastomers, including those based on materials such as thermoplastic propylene, ethylene, and styrene, including their halogenated counterparts. Valve 50 may also be formed as an integral structure from a flexible, tough, elastic, and resilient material membrane, as disclosed in U.S. Patent No. 10,287,066, and includes linear low-density polyethylene (LLDPE), low-density polyethylene (LDPE), LLDPE / LDPE blends, acetates, acetals, ultra-high molecular weight polyethylene (UHMW), polyesters, polyurethanes, ethylene-vinyl acetate (EVA), polypropylene, and high-density polyethylene. The separable slit valve 50 is releasably attached to the orifice 30 by snap-fit ​​or other means, such as gently adhesiveting the slit valve 50 to the pipe 32, allowing it to be easily removed from the pipe 32 by hand. The pipe opening 34 may include a lip 36 to interface with the separable slit valve 50. The separable slit valve 50 is formed of plastic or other resin material. Figure 2bAs shown, the separable slit valve 50 may include tabs 52 or other features to facilitate removal. The lower edge 26 of the peripheral surface 22 of the pulp molding base lies below the liquid-containing surface 28, the pipe opening 34, and the separable slit valve 50, thereby allowing the extrudable fiber-based bottle 10 to stand upright. The pulp molding base includes means for preventing pulp from being dispensed through the valve if pressure is accidentally applied through the sidewalls during transport or processing. This may be a closure of the pulp molding, which is dip-coated, spray-coated, or vacuum-laminated with a polymer barrier structure (not shown). In this invention, the valve can be sealed with a removable cap that is attached to a metallized laminate of the pulp molding closure using a pressure-sensitive adhesive (not shown).

[0087] It has been found that the pulp molding base 20 according to the invention is surprisingly capable of providing excellent protection for liquid formulations and maintaining integrity during use in humid environments such as bathrooms and showers, while still having a fiber content of greater than 80%, and is recyclable in the pulp stream according to PTS-RH 021:2012 Cat 2. The base barrier structure 40 disposed on the liquid-receiving surface 28 and the peripheral surface 22 near the upper edge 24 of the pulp molding base 20 can be applied to the pulp molding base 20 by spraying, dipping, or as a laminate by welding or gluing.

[0088] In the case of spraying or dipping, the base barrier structure may include a primer layer and one or more topcoat layers. The primer may be applied in the form of a polymer dispersion, which may be an aqueous polymer dispersion. The primer may be a latex dispersion, a polyvinyl alcohol dispersion, a polyhydroxyalkanoate (PHA) dispersion, or a polyolefin dispersion. An example of a polyolefin dispersion is Rhobarr, commercially available from Dow Chemical Company (DOW). ® In this invention, the primer can be a styrene acrylate, such as Joncryl commercially available from BASF. ® 4010. Typically, the thickness of the barrier structure should be as thin as possible, but thick enough to form a barrier structure between the pulp molding base and the topcoat. The average amount of primer applied to the surface of the molding base can be less than 60 g / m², less than 40 g / m², or less than 20 g / m². The base barrier structure 40 may include one or more topcoat layers, i.e., applied on top of the primer. Depending on the chemical properties, the topcoat layer may be applied immediately after the primer application, in the form of an aqueous dispersion, before drying. The topcoat layer composition may contain a polymer dispersion for producing a heat-sealable coating. The polymer dispersion may be a hydrocarbon polymer dispersion, or a synthetic hydrocarbon polymer dispersion, such as styrene acrylate latex. The topcoat layer may also contain one or more additives to enhance water barrier properties, such as waxes, MFC, or CNC. In this invention, the topcoat layer may be based on styrene acrylate, such as Joncryl commercially available from BASF.® 4030. The amount of each topcoat layer can be less than 30g / m², within the range of 6g / m² to 26g / m², or within the range of 12g / m² to 18g / m². 2 Within a certain range. Typically, more than one topcoat layer is applied to reduce the incidence of surface defects such as pinholes, spots, or cracks. After applying the primer and topcoat layers, the parts can be transferred to a heating unit, such as a hot air drying hood, to remove moisture from the coating and promote film formation by melting or partially melting the polymer in the barrier structure. In this invention, the drying temperature can be between 100°C and 150°C, or between 110°C and 120°C. After spraying and drying, the average thickness of all barrier structures can be between 10 micrometers and 100 micrometers.

[0089] In this invention, the base barrier structure 40 can be formed by a powder polymer coating to reduce emissions of volatile organic compounds (VOCs) and coating waste. In this invention, the powder may comprise a thermoplastic polymer selected from polyolefins (e.g., polyethylene or polypropylene and their copolymers). The polymer powder may also comprise water-soluble synthetic polymers such as polyvinyl alcohol, polyhydroxyalkanoates (PHAs), or polysaccharides such as cellulose. The powder particles typically have an average size of 1 pm to 200 pm, for example 5 pm to 100 pm, or for example 10 pm to 50 pm. The coating can be applied by a spraying device and then cured / melted to form a continuous film on the surface, for example according to the process described in WO2022207507, which is incorporated herein by reference. The average thickness of the film applied in this system can range from 10 micrometers to 100 micrometers.

[0090] In this invention, the base barrier structure 40 can be a layer applied by thermoforming under vacuum, such as... Figure 3a , Figure 3b and Figure 3c As shown. The barrier structure can be made of a PE laminate with a thickness of 30 to 150 micrometers, and can be between 60 and 90 micrometers before application, depending on the average final thickness of the target. In this invention, the laminate may include a P1B / LLDPE outer sealing layer, nucleated HDPE 90 / 10 Surpass ®The 167 / 640i LDPE core layer and 90% LLDPE / 10% LDPE inner sealing layer are used. The thickness of the P1B / LLDPE outer sealing layer can range from 5µm to 15µm, and it can have a mixture ratio of 15% P1B / 85% LLDPE to 25% P1B / 75% LLDPE. The nucleated HDPE 90 / 10 Surpass 167 / 640i LDPE core layer can have a thickness range from 30µm to 200mm. The thickness of the LLDPE / LDPE inner sealing layer can range from 5µm to 20µm, and it can have a mixture ratio of 95% LLDPE / 5% LDPE to 85% LLDPE / 15% LDPE. In this invention, the multilayer barrier structure can be a multilayer with a total thickness of 90µm, comprising a 5µm top layer of 15% P1B / 85% LLDPE, a 70µm core layer of nucleated HDPE 90 / 10 Surpass 167 / 640i LDPE, and a 15µm inner layer of 90% LLDPE / 10% LDPE. The barrier structure can be a biodegradable thermoplastic material selected from the group consisting of aliphatic and / or aromatic polyesters or thermoplastic starches. Examples of biodegradable laminates using a liner include those manufactured by BASF under the trade name ECOVIO. ® The products sold are binary blends of PLA and PBAT. The structure of the film lamination can be optimized and configured based on performance requirements such as barrier properties after application, adhesion to the pulp surface, and percentage of recyclable pulp.

[0091] Figure 3a A base barrier layer 40 comprising a laminate and a pulp molding base 20 is shown prior to thermoforming. Before application, the barrier structure 40 is adhered to a heating plate by pressure applied under vacuum, thereby heating the barrier structure to the molding temperature. The pulp molding base 20 is mounted on a mandrel. Once the target temperature is reached, the vacuum on the top plate is released, and the barrier structure 40 droops due to the vacuum applied to the mandrel side. The bottom mandrel can also be heated to promote adhesion between the laminate and the pulp molding base 20. Figure 3b The illustration shows the laminated state of the base barrier layer 40, which covers the liquid-receiving surface 28 including the pipe opening 34 and the peripheral surface 22 of the pulp molding base. Although in Figure 3b The diagram shows a base barrier layer 40 with a uniform wall thickness, but in reality, a thickness gradient will form depending on the amount of membrane stretching during application. It has been found that applying localized heat to the membrane, i.e., through a system such as WATTTRON, can... ® This process helps achieve a more uniform wall thickness and prevents pinholes. Depending on the required barrier properties, the average thickness of the base barrier layer 40 after application can be less than 90 micrometers, less than 75 micrometers, less than 50 micrometers, and less than 20 micrometers. Figure 3c The thermoformed pulp molding base 20 is shown, in which pipe openings 34 are cut out in the pipe 32.

[0092] Figures 4a to 4d An exemplary extrudable fiber-based bottle 110 with a cylindrical tubular structural component is shown. According to the invention, the fiber-based sidewall 112 may comprise paperboard. The paperboard is typically made of a multilayer structure consisting of multiple substrates and one or more functional layers. Figure 4a As shown, functional layer 113 may be on inner layer 118 and / or outer layer 119. An example of commercially available cardboard is Natura Barr from Stora Enso. ® Alternatively, it could be Billerud's LiquidLC. The inner coating can be an LDPE laminate to ensure good solderability and contact durability with the product. In this invention, the inner coating can be Natura from Stora Enso. ® Or Cupforma Natura ® A polymer aqueous dispersion on the plate. Dispersions such as BASF Joncryl can be used. ® Or Down Rhobarr ® The aqueous dispersion can be applied using various techniques, such as dip coating, bar coating, doctor blade coating, gravure printing, reverse roll coating, air knife coating, and forward roll coating or spray coating, followed by a drying step. The substrate of the liquid cardboard can contain lignocellulose fibers obtained through any conventional pulping process, including bleached or unbleached chemical pulping, mechanical pulping, and chemimechanical pulping. The cardboard can be made from more than one sheet (typically three sheets) and is usually in the form of a fiber web. In this invention, the cardboard can have a basis weight of 170 gsm to 350 gsm, and can have a basis weight of about 250 gsm to 280 gsm. An example of cardboard using a water-based dispersion coating is Cupforma, sold by Stora Enso. ® Natura Aqua+ and ISLA sold by Kotkamills ® Additional layers may be used, such as aluminum foil, one or more HDPE layers, thin layers produced by vapor deposition of inorganic materials, or water-dispersible nanocomposite layers that form nanosheets during drying. In this invention, cylindrical tubular structural components may have a fiber weight percentage of more than 85% of the total weight, more than 90% of the total weight, and more than 95% of the total weight.

[0093] The manufacture of an extrudable fiber-based bottle 110 comprising a cylindrical tubular structure using fiber-based sidewalls 112 is described in WO2022185176, WO2022229810, EP2007567, EP284389, and EP2630052, which are incorporated herein by reference. Based on the described process, multiple layers of sheets are assembled end-to-end into a tubular cylindrical structure, with reinforcing strips added at the assembly points, and then cut into discrete lengths. Subsequently, a pulp molding base 120 is placed in a mandrel, and an impermeable seal 142 can be heated or glued. In a subsequent step, the inner surface 118 of the tubular body is pressed against the impermeable seal 142 to complete the assembly.

[0094] Figure 5a An example of a pulp molding base 120 assembled according to this process to a cylindrical tubular structure is shown, wherein the sidewall 112 is a single-sided coated sidewall. In this configuration, a valve 150 can be assembled onto a corresponding valve seat on the liquid-receiving surface 128 of the pulp molding base 120. The valve 150 can be held in place by thermally stacking fully lined pulp discs 151 onto the lined base. The gasket coating the pulp discs can be LDPE applied by vacuum forming, or one of a heat-sealable polymer aqueous dispersion applied by spraying or dipping. In this invention, a liquid-compatible adhesive can be used for assembly. The advantage of this configuration is that, during dispensing, a natural resistance to displacement of the valve 150 is generated due to the internal liquid pressure. The sealing force of the discs against the gasketed base can still be configured to ensure that the user can easily access and remove the valve 150 by crushing the container before disposal.

[0095] In this invention, Figure 5b This illustrates a case where sidewall 112 is a double-coated sidewall, comprising an inner coating layer and an outer coating layer 113. Figure 5c The present invention is shown, which may have a pulp barrier structure 113, which, for example, completely encapsulates the pulp molding base 120 by impregnating a polymer aqueous dispersion.

[0096] An impermeable seal 142 connecting the fiber-based sidewall 112 of the connecting tubular structure and the pulp molding base 120, and an upper sealing region 129 of the fiber-based sidewall 112, may include means to prevent edge wicking to avoid catastrophic integrity failure or undesirable deformation. Edge wicking is particularly problematic in areas where liquid carton board edges are cut (“rough edges”) and exposed to water, such as when bottles are used for showering. Edge wicking of cardboard has been extensively studied, for example, liquid penetration in food service cardboard, Harju 2018, Master's Thesis. Several methods can provide edge protection, such as spraying adhesives or other hydrophobic agents, scraping, crimping, or covering cut edges with adhesive plastic strips. Edge protection methods for the upper seal 129 may employ spraying, dip coating, adding PE-PET-PE strips, or folding, as discussed below. Figures 6a to 6d As shown.

[0097] Figure 7a and Figure 7b An exemplary extrudable fiber-based bottle 210 with a conical tubular structure is shown. In this example, the fiber-based sidewalls 212 can be cut from a roll of liquid carton board as shown in the diagram. Figure 7d The blank shown is formed. Then, the fiber-based sidewalls 212 are folded and welded at the edges, as shown. Figure 7e As shown. Typical welding techniques may include hot air, ultrasonic, or adhesive bonding. The cone may then include a polymer strip 223 welded to a vertical seal 221 to protect burrs from edge wicking. The fiber-based sidewall 212 of the tubular cone may be welded to a pulp molding base 220 to produce a compressible bottle 210 including a tube 213, as shown. Figure 7c As shown. Subsequently, tube 213 can be filled and sealed, as... Figure 7c As shown. In this invention, an edge protection method can be used to apply an impermeable seal 242 between the upper edge 224 of the peripheral surface of the pulp molding base 120 and the lower edge 216 of the fiber-based sidewall. An upper seal 129 can also be formed between a first side 115 and a second side 117 of the upper edge 114 of the pulp sidewall 112. Figures 6a to 6d An example is depicted of how the first side 115 and the second side 117 of the upper edge 114 of the sealed fiber-based sidewall 112 are sealed, wherein Figure 6a A single fold is depicted; Figure 6b It depicts a double fold; Figure 6c It depicts a saddle-shaped fold; and Figure 6d It depicts a triple fold.

[0098] Figures 8a to 8cAn exemplary extrudable fiber-based bottle 310 with a pulp-molded sidewall 312 is shown. The pulp sidewall 312 can be formed from one or more components molded according to the wet molding process and liquid containment barrier application process described herein. In this invention, the fiber-based bottle sidewall 312 can be integrally formed by wet molding. The average wall thickness of the pulp sidewall 312 can be between 0.6 mm and 1.2 mm, and between 0.8 mm and 1.0 mm. In this invention, the wall thickness at the extrusion panel can be locally reduced, and can be between 0.6 mm and 0.8 mm. The wet molding of the pulp sidewall 312 can follow the same process as the aforementioned pulp molding base. In this invention, the process can include methods of rapid dehydration and induction heating to shorten cycle time. The starting pulp used to manufacture the pulp-molded sidewall 312 can consist of 1% to 10% cellulose fibers, which can be about 1%, with the remainder being water and additives. The cellulose fibers can be wood or non-wood. As previously described for pulp molding bases, fiber formulations can be optimized for dewatering and production cycle times, mechanical properties such as burst strength, and surface finish (roughness and porosity). The mechanical properties of the pulp sidewalls are particularly important for optimizing dispensing functionality. The pulp sidewall 312 can be optimized to bend when a user applies pressure, thereby reducing the volume of the bottle chamber. In this invention, the elastic modulus and geometric stiffness of the pulp sidewall 312 can be low enough to allow deformation, yet high enough to allow for some rebound upon initial use. As the contents are depleted, such as when less than 50% or possibly less than 30% of the total contents have been dispensed, the bottle walls may collapse and permanently deform, reducing the force required for dispensing. Cellulose fibers can be of different types to balance these requirements.

[0099] In this invention, the cellulose fibers forming the molded pulp sidewall 312 may include coniferous wood, bamboo, and bagasse. The length-weighted average fiber length, arithmetic mean fiber length (ISO 0.2 mm–7.0 mm), and arithmetic mean fiber width can be determined using a fiber image analyzer such as the Valmet FS5, according to TAPPI T271. Coniferous wood fibers may have a length-weighted average fiber length of approximately 2.25 mm, an arithmetic mean fiber length of approximately 1.4 mm (ISO 0.2 mm–7.0 mm), and an arithmetic mean fiber width of approximately 30 µm. Bamboo fibers may have a length-weighted average fiber length of approximately 15 mm, an arithmetic mean fiber length of approximately 1.0 mm (ISO 0.2 mm–7.0 mm), and an arithmetic mean fiber width of approximately 15 µm. Bagasse fibers may have a length-weighted average fiber length of about 1.0 mm, an arithmetic mean fiber length of about 0.6 mm (ISO 0.2 mm-7.0 mm), and an arithmetic mean fiber width of about 22 µm. In this invention, the fiber count may include 50% to 60% bamboo, 40% to 50% bagasse, and 0% to 10% coniferous wood.

[0100] Cellulose fiber slurries may also include additives for process control and / or functional enhancement. Typical additives for process control include retention aids, defoamers, pH adjusters, and slime control agents. Additives for functional enhancement include (1) fillers, such as inorganic mineral fillers, such as calcium carbonate and plate-like kaolin; (2) adhesives, such as alkyl ketone dimers (AKD), alkenyl succinic anhydride (ASA), rosin, or lignin; (3) additives for enhancing dry strength, such as starch, amphoteric, cationic, or anionic polyacrylamide resins, enzymes, and modified polyamines; (4) additives for enhancing wet strength, such as polyamide (PAE) or polyamine epichlorohydrin, epoxide or cationic glyoxylate resins, or (5) microfibrillated cellulose (MFC) or cellulose nanocrystal (CNC) additives. Fiber chemical treatments, such as the use of low eutectic solvents (DES), can enhance fiber swelling and bonding potential.

[0101] In this invention, based on a dry fiber count, the slurry may contain 0.5% to 2% AKD, and may be about 1% AKD, to provide the slurry with some excellent water resistance. The slurry may also contain 0.1% to 0.5% PAE to provide some excellent wet strength to the final product. In this invention, based on a dry fiber count, the slurry may contain 2% to 5% MFC, and may contain 3% to 4% MFC, to improve surface smoothness, stiffness, burst resistance, and wet strength for barrier applications. Examples of commercially available MFCs include Curran. ® or Fiberlean ® This addition is particularly advantageous for improving the barrier effectiveness of spray or dip coatings by reducing surface porosity to prevent coating penetration. It is also particularly beneficial for enhancing the part's resistance to mechanical stresses caused by bottle extrusion pressure. In this invention, pulp parts can be functionalized after molding via vapor deposition of the inorganic barrier structure as described above.

[0102] A pulp sidewall barrier structure 313 is disposed on the liquid-receiving surface of the inner surface 318 of the pulp sidewall. The pulp sidewall barrier structure can be applied to the molded pulp sidewall 312 by spraying or dipping. The pulp sidewall barrier structure 313 may include a primer layer and one or more topcoat layers. The primer can be applied in the form of a polymer dispersion, which may be an aqueous polymer dispersion. The primer may be a latex dispersion, a polyvinyl alcohol dispersion, a polyhydroxyalkanoate (PHA) dispersion, or a polyolefin dispersion. An example of a polyolefin dispersion is Rhobarr, commercially available from Dow Chemical Company (DOW). ® In this invention, the primer can be a styrene acrylate, such as Joncryl commercially available from BASF. ®4010. Generally, the thickness of the barrier structure should be as thin as possible, but thick enough to form a barrier structure as a topcoat layer on the inner surface of the pulp sidewall. The average amount of primer applied to the inner surface can be less than 20 g / m², and can be from 3 g / m² to 10 g / m², or from 4 g / m² to 9 g / m². The pulp sidewall barrier structure may include one or more topcoat layers, i.e., applied on top of the primer. Depending on the chemical properties, the topcoat layer can be applied immediately after the primer application, in the form of an aqueous dispersion, before drying. The topcoat layer composition may contain a polymer dispersion for producing a heat-sealable coating. The polymer dispersion may be a hydrocarbon polymer dispersion, or a synthetic hydrocarbon polymer dispersion, such as styrene acrylate latex. The topcoat layer may also contain one or more additives to enhance water barrier properties, such as waxes, MFC, or CNC. In this invention, the topcoat layer may be based on styrene acrylate, such as Joncryl commercially available from BASF. ® 4030. The amount of each topcoat layer can be less than 30 g / m², ranging from 5 g / m² to 12 g / m², or from 6 g / m² to 9 g / m². Typically, more than one topcoat layer is applied to reduce the incidence of surface defects such as pinholes, spots, or cracks. After applying the primer and topcoat layers, the extrudable fiber-based bottle can be transferred to a heating unit such as a hot air drying hood to both remove moisture from the coating and promote film formation by melting or partially melting the polymer in the barrier structure. In this invention, the drying temperature can be from 100°C to 150°C, or from 110°C to 120°C. After spraying and drying, the average thickness of all barrier structures can be between 10 micrometers and 100 micrometers.

[0103] In this invention, the barrier structure 313 of the pulp sidewall 312 can be formed by a powder polymer coating to reduce emissions of volatile organic compounds (VOCs) and coating waste. In this invention, the powder may comprise a thermoplastic polymer selected from polyolefins (e.g., polyethylene or polypropylene and their copolymers). The polymer powder may also comprise water-soluble synthetic polymers such as polyvinyl alcohol or polysaccharides such as cellulose. The powder particles typically have an average size of 1 pm to 200 pm, for example 5 pm to 100 pm, for example 10 pm to 50 pm. The coating can be applied by a spraying device and then cured / melted to form a continuous film on the surface, for example according to the process described in WO2022207507, which is incorporated herein by reference. The average thickness of the barrier structure applied in this system can range from 10 micrometers to 100 micrometers.

[0104] Figure 8a The pulp molding sidewall 312 assembled to the pulp molding base 320 is shown. This assembly can be accomplished by hot air welding, ultrasonic welding, or adhesive bonding and / or a combination thereof. Figure 8b and Figure 8cA cross-sectional view of an assembled extrudable fiber-based bottle 310 with pulp-molded sidewalls 312 is shown. This bottle has been found to have surprisingly good splash-proof performance, while also being recyclable and providing excellent liquid barrier properties. Bottle 310 is also extrudable, exhibiting good resilience from first use. During shower use, bottle 310 can soften, making it easier to squeeze while maintaining its integrity. At the end of use, the bottle can be easily crushed. Crushing causes the pulp-molded base 320 to detach from the sidewalls 312, allowing the valve 350 to be easily separated from the pulp-molded base 320. Consumers can also easily flatten the components for easy disposal.

[0105] Figure 9 illustrates another exemplary configuration of an extrudable fiber-based bottle 410 having pulp-molded sidewalls 412. In this invention, the sidewall barrier structure 413 can be a layer applied by thermal vacuum thermoforming, as previously described. Figure 3a , Figure 3b and Figure 3c This is described and depicted for the pulp molding base 20. The barrier structure 413 can be made of a PE laminate with a thickness of 30 micrometers to 150 micrometers, and can be between 60 micrometers and 90 micrometers before application, depending on the target average final thickness. In this invention, the laminate may include a P1B / LLDPE outer sealing layer, a nucleated HDPE 90 / 10 Surpass 167 / 640i LDPE core layer, and a 90% LLDPE / 10% LDPE inner sealing layer. The thickness of the P1B / LLDPE outer sealing layer can range from 5µm to 15µm, and can have a mixing ratio of 15% P1B / 85% LLDPE to 25% P1B / 75% LLDPE. The nucleated HDPE 90 / 10 Surpass 167 / 640i LDPE core layer can have a thickness range from 30µm to 200mm. The thickness of the LLDPE / LDPE internal sealing layer can range from 5µm to 20µm, and it can have a mixing ratio of 95% LLDPE / 5% LDPE to 85% LLDPE / 15% LDPE. In this invention, the multilayer barrier structure can have multiple layers with a total thickness of 90µm, comprising a 5µm top layer of 15% P1B / 85% LLDPE, a 70µm core layer of nucleated nucleated HDPE 90 / 10 Surpass 167 / 640i LDPE, and a 15µm inner layer of 90% LLDPE / 10% LDPE. The film lamination structure can be optimized and configured based on performance requirements such as barrier properties after application, adhesion to the pulp surface, and the percentage of recyclable pulp.

[0106] Prior to application, the barrier structure 413 is adhered to the heating plate by pressure applied under vacuum, thereby heating the barrier structure to the molding temperature. The pulp molding sidewall 412 is mounted on the mandrel. Once the target temperature is reached, the vacuum on the top plate is released, and the barrier structure droops due to the vacuum applied to the mandrel side. The bottom mandrel can also be heated to promote adhesion of the laminate to the pulp molding base 420. Figure 9b The illustration shows the laminated sidewall 412, which is completely covered by the barrier structure 413. The film also covers the lower edge 416 of the pulp sidewall 412 and a portion of the outer surface 419 to facilitate sealing with the pulp molding base 420. Although the base barrier structure 440 of the pulp molding base is in... Figure 9b The diagram shows a uniform wall thickness, but in reality, a thickness gradient will form depending on the amount of membrane stretching during application. It has been found that applying localized heat to the membrane, i.e., via a system such as WATTTRON, can help achieve a more uniform wall thickness and prevent pinholes. Depending on the desired barrier properties, the average thickness of the sidewall barrier structure 413 after application can be less than 90 micrometers, less than 75 micrometers, less than 50 micrometers, and ideally less than 20 micrometers.

[0107] The pulp molding base 420 can be manufactured by pulp molding. The inner surface is coated using spraying, dip coating, or by applying a layer through vacuum thermoforming. Figure 9a A pulp molding sidewall 412 assembled to a pulp molding base 420 is shown to form a liquid-tight seal. This assembly can be accomplished by hot air welding, ultrasonic welding, or adhesive bonding and / or a combination thereof.

[0108] Figure 10a and Figure 10b Another exemplary configuration of an extrudable fiber-based bottle 510 with pulp-molded sidewalls 512 is shown. In this invention, the sidewalls 512 may be molded to have two open surfaces at the upper edge 514 and the lower edge 516. A sidewall barrier structure 513 on the inner surface 518 may be coated or laminated. In this invention, the barrier structure 513 coating may be heat-sealable. The pulp-molded base 520 may be manufactured by pulp molding. The base barrier layer 540 may be applied by spraying, dip coating, or by vacuum thermoforming. The pulp-molded sidewalls 512 are assembled to the pulp-molded base 520 to form a liquid-tight seal. This assembly may be accomplished by hot air welding, ultrasonic welding, or adhesive bonding and / or combinations thereof. Figure 10a and Figure 10bThe image shows a bottle 510 assembled with a pulp molding base 520, in a transport configuration to a filling workshop. In this configuration, the bottle 510 can be filled with the desired amount of product through an opening in the upper edge 514 of the pulp sidewall 512. After filling, the first side 515 of the upper edge of the pulp sidewall can be sealed to the second side 517 of the upper edge of the pulp sidewall, forming an upper seal 529 such as a tube or bag. Figure 10c and Figure 10d As shown. The upper seal 529 can be formed by hot air welding, hot clamping, or ultrasonic molding.

[0109] Figure 11a An exemplary configuration of the lower portion of a compressible fiber-based bottle 610 is shown, featuring a mechanism that facilitates consumer separation of the valve 650 from the pulp molding base 620. Consumers may wish to separate the valve 650 from the pulp molding base 620 to reduce the non-fiber portion of the recycled paper stream. According to this configuration, the valve 650 can be sandwiched between the pulp molding base 620 and an additional molded cap 653 attached to the bottom surface 627 of the pulp molding base 620. Figure 11b As shown, the molded cap 653 may have a flap 655 that can be easily gripped by a consumer. Assembly of the molded cap 653 to the pulp molding base 620 may be performed using adhesive to form a sufficiently strong but light bond to prevent premature separation during bottle dispensing and use, yet low enough to facilitate consumer separation of the molded cap 653 before disposal. Before disposal, the consumer grasps the flap 655 and applies a twist to separate the cap 653 from the pulp molding base 620, thereby removing the valve 650.

[0110] In this invention, Figure 12 The illustration shows that the cover 753 can be removed from the pulp molding base 720 and the valve 750 via the tab 752.

[0111] Figure 13 An exemplary construction of a compressible fiber-based bottle 10 is shown, wherein the pulp molding base 120 may comprise fiber-based paperboard or cardboard. The paperboard may be made of more than one layer (typically three layers) and is typically in the form of a fiber web. In this invention, the cardboard may have a basis weight of 170 gsm to 430 gsm, and may be approximately 250 gsm to 350 gsm. Functional layers may be present on both the inner surface 128 and the outer surface 127 forming the liquid-containing portion. The innermost and outermost layers may be low-density polyethylene (LDPE) layers to ensure good sealing and liquid tightness. The liquid cardboard used may be branded under the Natura trademark. ™ 2PEBoard or Natura ™ Barr sells products from Stora Enso, a Finnish company. This invention can have both an inner and outer coating, both being polymeric aqueous dispersions, such as BASF Joncryl. ®Or Down Rhobarr ® Aqueous dispersions can be applied using a variety of techniques, such as dip coating, bar coating, doctor blade coating, gravure printing, reverse roll coating, air knife coating, and forward roll coating or spray coating, followed by a drying step. Examples of cardboard using water-based dispersion coatings are CupformaNatura Aqua+ sold by Stora Enso and ISLA sold by Kotkamills.

[0112] The pulp molding base 120 can be manufactured from a blanket, heated, and thermoformed to achieve a specific shape. The blanket can be folded, and the edges pressed together to form an impermeable seal 243. This seal can be reinforced by mechanically applying a knurling pattern. The edges 216 of the molding base 120 can also be scraped or any other solution known in the art to prevent moisture ingress. This construction is particularly advantageous for using commercially available cardboard while reinforcing the base with additional thickness to achieve a reliable impermeable seal 142 with the sidewalls 112 and base stability. The pulp molding base 120 may have a flat portion near the opening 30 to ensure reliable assembly of the pulp disc 151 via ultrasonic or heat sealing. The opening 30 can be sealed with a removable cap that uses a metallized laminate attached to the molded closure with a pressure-sensitive adhesive (not shown).

[0113] Figure 14 An exemplary configuration of a squeezable fiber-based bottle 10 is shown, wherein a membrane is applied to the outer surface 127 of a pulp molding base 120, and another membrane is applied to the inner surface 128. Figure 14 This is particularly beneficial for minimizing the risk of leakage and pinholes, while ensuring a strong bond with the pulp disc 151 via ultrasonic or heat sealing. The membrane applied to the outer surface 127 ensures the possibility of a strong seal 142 with the sidewall 112 via hot air, heat sealing, or ultrasonic waves. The membrane also ensures protection of the pulp molding base 120 from moisture absorption, thus maintaining its stability and integrity during bottle use in humid environments.

[0114] In this invention, a first film is applied to the outer surface 127 via thermal vacuum thermoforming. Subsequently, a second film is applied to the inner surface 128 via vacuum lamination. The two films can then be welded in regions 801 and 803 to completely encapsulate the pulp molding base 120, and excess film is removed in regions 802 and 804 using a cutting tool.

[0115] Figure 15 An exemplary configuration of the extrudable fiber-based bottle 10 is shown, wherein a membrane is applied to the outer surface 127 and a coating is applied to the inner surface 128 to completely encapsulate the pulp molding base 120. This configuration can be used to maximize the total fiber content. Figure 15In the process, the film is applied to the outer surface via thermal vacuum thermoforming. Then, excess film is trimmed in areas 805 and 806 using a tool. A primer (such as Joncryl) can then be applied to the inner surface 128. ® 4010) and one or more layers of coating (such as Joncryl commercialized by BASF) ® 4030). Then, the pulp disc 151 can be glued to the pulp molding base 120.

[0116] method

[0117] 1) Individual layer thickness

[0118] The thickness of the overall film / individual layer was measured by cutting a 20µm thick cross section of the film sample via a sliding slicer (e.g., Leica SM2010 R), placing it under an optical microscope in transmission light mode (e.g., Leica Diaplan), and applying imaging analysis software.

[0119] 2) thickness

[0120] The thickness (caliper / thickness) of a monolayer test sample was measured under static load using a micrometer according to pharmacopoeia method ISO 534, with modifications mentioned herein. All measurements were performed in a laboratory maintained at 23°C ± 2°C and 50% ± 2% relative humidity, with the test sample conditioned in this environment for at least 2 hours prior to testing. Thickness was measured using a micrometer equipped with a pressure foot capable of applying a stable pressure of 70 kPa ± 0.05 kPa to the test sample. The micrometer was a statically heavy instrument with readings accurate to 0.1 micrometers. A suitable instrument was the TMI digital micrometer model 49-56, or equivalent, purchased from TestingMachines Inc., New Castle, DE. The pressure foot was a flat, circular, movable surface with a diameter smaller than the test sample, capable of applying the required pressure. A suitable pressure foot diameter was 16.0 mm. The test sample was supported by a horizontal, flat reference platform, which was larger than and parallel to the surface of the pressure foot. The system was calibrated and operated according to the manufacturer's instructions. Measurements are performed on single-layer test samples taken from raw material rolls or sheets, or from finished packaging. When removing test samples from finished packaging, care is taken to avoid contaminating or deforming the sample during the process. The removed sample should be free of residual adhesive and taken from an area of ​​the packaging free of any seams or creases. Ideally, the test sample should be 200 mm in diameter. 2And it must be greater than the pressure foot. To measure thickness, first zero the micrometer relative to a horizontal, flat reference platform. Place the test sample on the platform, with the test position centered below the pressure foot. Gently lower the pressure foot at a rate of 3.0 mm per second until full pressure is applied to the test sample. Wait 5 seconds, then record the thickness of the test sample, accurate to 0.1 micrometers. Repeat this process for a total of ten replicate test samples. Calculate the arithmetic mean of all thickness measurements and report the value as "Thickness," accurate to 0.1 micrometers.

[0121] 3) Basis weight

[0122] The basis weight of the test sample is the mass (in grams) per unit area (in square meters) of a single material layer, and is measured according to the pharmacopoeia method ISO 536. The test sample is cut into blocks of known area, and the mass of the test sample is determined using an analytical balance accurate to 0.0001 g. All measurements are performed in a laboratory maintained at 23°C ± 2°C and 50% ± 2% relative humidity, and the test samples are conditioned in this environment for at least 2 hours prior to testing. Measurements are performed on test samples taken from raw material rolls or sheets, or from finished packaging. When cutting the test sample from the finished packaging, care is taken to avoid any contamination or deformation of the sample during the process. The cut sample should be free of residual adhesive and taken from an area of ​​the packaging free of any seams or creases. The test sample must be as large as possible to account for any inherent material variability. For flat samples, the dimensions of a single-layer test sample are measured using a calibrated steel ruler or equivalent from NIST. For non-flat samples, the area can be calculated using 3D data. Calculate and record the area of ​​the test sample, accurate to 0.0001 square meters. Use an analytical balance to obtain and record the mass of the test sample, accurate to 0.0001 grams. The weight of the coating can be obtained by subtracting the weight of the coated sample from the weight of the uncoated sample. Calculate and record the basis weight by dividing the mass (in grams) by the area (in square meters), accurate to 0.01 grams per square meter (gsm). Repeat this process for a total of ten replicate test samples. Calculate and report the arithmetic mean of the basis weights, accurate to 0.01 grams per square meter.

[0123] 4) Pinhole test method

[0124] This is a test method for detecting and locating any pinholes equal to or greater than 10 μm on a coated surface. Place the part to be tested on the absorbent surface with the coated side facing up. Then spread a dye penetrant solution according to ASTM F3039-23 on the test surface, applying pressure to the surface using an eyedropper or pipette and a small roller to ensure adequate contact. The dye penetrant solution should contact all areas exhibiting suspected surface abnormalities, taking care not to allow the solution to flow over the edges of the sample. Wipe away excess dye from the sample using a clean absorbent pad and carefully lift the sample. If there is no evidence of dye penetration or staining to the opposite side of the coated surface, the test passes.

[0125] 5) Bottle Leakage Test Method

[0126] This is a test method for measuring the ability of containers and closed systems to prevent leakage during storage or transportation.

[0127] Pre-treat at least three representative empty bottles of the test type at 22°C ± 3°C and 60% ± 10 RH for at least 24 hours. Prepare tap water solutions at room temperature, adding dyes such as rhodamine or toluidine to provide a permanent indication of leakage. Fill the sample with the water / dye solution to the intended filling capacity, e.g., 150 mL ± 1 mL, at laboratory ambient temperature, equipped with their respective closures (if applicable), and hermetically sealed in the storage configuration. Dry the bottle neck and shoulder area (if necessary) with a (paper) towel to ensure no product residue remains. Place the sample on a flat tray capable of holding the liquid if leakage occurs. Place some absorbent paper under the sample to facilitate leakage detection. Then store the sample at 25°C ± 3°C and 60% ± 10 RH. It is not necessary to place weights or other bottles on top of the tested sample. Alternative sample orientations during testing can be considered so that the suspected leakage area is covered by the liquid in the container. Check for liquid leakage after 24 hours, 1 week, and 2 weeks. Pay attention to any locations where leaks eventually occur.

[0128] If leakage occurs to the outside of the sample, the packaging fails the test. If no leakage occurs to the outside of the sample, the packaging passes the test.

[0129] 6) Water vapor transmission rate (WVTR) test method

[0130] Water vapor transmission rate (WVTR) is defined as the mass of water vapor that permeates through a membrane per unit time per unit area, and it is used as a parameter to measure water barrier properties. Measurements are performed according to the ASTM E96 inverted cup method. For this test, an impermeable cup (such as the “vapometer” E96 cup from Thwing-Albert Instruments) is filled with 50 g of water. The cup opening has an area of ​​3,070 mm². The cup is made of a non-corrosive material and is impermeable to water or water vapor. The flat portion of the specimen to be measured is cut into a circle slightly larger than the opening of the cup. At least three representative specimens of the material and conditions being tested should be tested. The test specimen is clamped between two gaskets and placed on the flange of the cup opening to ensure proper orientation. The specimen is then secured to the cup by tightening the open screw cap to create an impermeable seal. The cup is then weighed using a balance with a resolution of at least 0.01 g. The cup is placed on a flat tray to ensure direct water contact covering the tested specimen. The cup is then stored at 25°C ± 3°C and 60% ± 10 RH. Note that the cup should be placed in a manner that allows airflow to be unrestricted by exposed surfaces. Weigh the cup daily for at least 7 days. A steady-state condition is established when the rate of weight change of the sample remains substantially constant over at least six consecutive weight measurements. A steady-state condition is assumed when a straight line adequately fits a graph of at least six appropriately spaced points (matching periodic weight changes or exceeding 20% ​​of the 100-fold scaling sensitivity). If the weight rate is not in a steady-state condition, the storage period should be extended.

[0131] If the target part to be characterized is not flat and / or the coating is not uniform, for example, made by spray or dip coating application, the water permeability is measured on a representative flat specimen made of the same material according to the same process, and characterized as the average substrate and coating thickness matching the thickness of the target part within a tolerance of + / -20%.

[0132] The water vapor transmission rate (WVTR) of a barrier structure after thermoforming can be calculated based on water vapor permeability theory, requiring two key pieces of information. The first is the inherent barrier material characteristic of water vapor permeability coefficient varying with thickness; the second is the change in barrier thickness after thermoforming. In this study, the relationship between water vapor permeability coefficient and thickness was established using a data regression process for WVTR values, employing ASTM F1249 (AMETEK, MOCON) for different membrane sample thicknesses. The thickness distribution after thermoforming can be obtained through physical measurements from thermoformed membrane samples or prediction using a virtual thermoforming model. Once this key information is obtained, the WVTR after thermoforming can be predicted based on permeability theory. These WVTR predictions were confirmed using a modified ASTM E96 desiccant method with a custom-designed metal sample holder. The sample holder was designed to create an airtight seal between the cavity containing bentonite desiccant, the thermoformed barrier membrane, and the surrounding controlled atmosphere. Following ASTM E96, the sample was weighed repeatedly over a specified duration; the resulting graph of time (days) versus weight increase (grams) was fitted with a linear regression. The slope of the line was recorded and normalized by the area of ​​the thermoformed gasket, and recorded as WVTR.

[0133] 7) Weight reduction test method

[0134] This method is used to determine the weight loss of water through a container or individual component such as a vessel and lid. At least three representative empty samples of the test type are pretreated at 23°C ± 2°C and 60% ± 10 RH for at least 24 hours.

[0135] Then, at laboratory ambient temperature, fill the sample to its fill volume with the specified amount of tap water or another specified personal care composition, equipped with their respective closures / caps (if applicable), and hermetically seal in the storage configuration. Care should be taken with any different types of closures, such as aluminum foil with paraffin. Dry any outer surfaces (if necessary) with a (paper) towel so that no product residue remains.

[0136] For flat components, such as capping membranes, measurements are performed according to a variant of the ASTM E96 inverted cup method. For this test, an impermeable cup (such as the “vapometer” E96 cup from Thwing-Albert Instruments) is filled with 50g of water or a specified personal care composition. The cup opening has an area of ​​3,070 square millimeters. The cup is made of a non-corrosive material and is impermeable to water or water vapor. The flat portion of the specimen being measured is cut into a circle slightly larger than the cup opening. At least three representative specimens of the material and conditions being tested should be tested. The test specimen is clamped between two gaskets and placed on the cup opening flange to ensure proper orientation. The specimen is then secured to the cup by tightening the open screw cap to create an impermeable seal.

[0137] Record the weight of the filled covered container or cup using a balance with a resolution of at least 0.01 g. Then store the sample under 25°C ± 3°C, 60% ± 10 RH, or another relevant test condition. The sample should be positioned such that water or the test product is in direct contact with the sample being tested. If using an ASTM E96 cup, the cup should be positioned such that airflow is not restricted by the exposed surface. Record the weight daily for two weeks. Once the gradient stabilizes at a “steady state,” calculate the daily weight loss. Calculate the surface area of ​​the container. Calculate the weight loss and record the average daily weight loss per square meter under 25°C, 60% RH, or a relevant test condition. This test is not applicable if the weight loss does not reach a steady state, such as in cases of packaging failure with leakage.

[0138] 8) Water resistance test method

[0139] This method simulates high-volume use in a humid environment. The bottle is filled with the specified filling volume of Pantene PRO-V Repair & Protect Shampoo or another specified personal care composition to the specified filling capacity (e.g., 150g ± 1g), and then pretreated at 22°C ± 3°C and 60% ± 10 RH for at least 24 hours.

[0140] Then dispense 5g ± 1g of the contents from the bottle; immerse the package in water for 8 minutes, followed by drying for 10 minutes. This sequence of operations represents a reuse cycle. This test cycle was repeated 19 times. A minimum of 3 bottles were tested.

[0141] If no integrity or performance failure is observed in any bottle, rendering the packaging unusable after all 20 reuse cycles, then the test requirements are met.

[0142] 9) Bottle squeeze test method

[0143] This method is used to measure the force required to dispense a given amount of product from a bottle. Bottles are filled with Pantene PRO-V Repair & Protect Shampoo or another specified personal care composition to a specified filling capacity (e.g., 150 g ± 1 g) and then pretreated at 22°C ± 3°C and 60% ± 10 RH for at least 24 hours. The bottles are equipped with their respective closures to ensure no leakage.

[0144] Each bottle is then placed in a compression tester using clamps to simulate a crushing event. An example of a compression tester is the Z010TN All-round from ZwickRoell GmbH & Co. KG. The load probe has a 3 / 4-inch stainless steel ball attached to simulate a thumb pressing against the bottle panel. The bottle is placed horizontally relative to the load post with its front panel facing upwards, with the two curved aluminum supports positioned in opposite directions of the applied load, by securing one end of the bottle to one end resting on two bent aluminum supports (simulating fingers). The bottle is adjusted to ensure the load is applied at the center of the panel and midway between the neck (or bottom) and the other end of the bottle. The probe is then lowered to contact the bottle, reaching the maximum preload of 0.5 N. A balance with an accuracy of ±0.01 g and a collection plate is placed under the package to collect the product dispensed from the orifice during the crushing. The closure is opened to ensure no product leaks from the orifice before the crush test. Sometimes it is necessary to reorient the bottle.

[0145] The load is then applied to the filled bottle at a speed of 20 mm / s until a displacement of 10 mm is achieved. The probe then returns to the starting position and performs two more load cycles. The total amount of product allocated is weighed. A minimum of three bottles are tested in total.

[0146] The test is considered successful if the average product collected from each dispensing event of all test bottles is at least 1g, and all bottles survive the test without any catastrophic failures that impair bottle function (such as leakage).

[0147] 10) Recyclability in Pulp Stream Based on PTS-RH 021 CAT 2

[0148] The test was conducted using at least 250 g of a representative amount of dried material from the type of packaging to be tested, intended for consumer disposal. The first step involved separating, drying to remove, and weighing easily separable non-paper components, such as closures. The test material was reduced to a sample size of approximately 2 cm × 2 cm, and the moisture content was determined according to DIN EN ISO 287:2009-09. Approximately 50 g ± 1 g of test material was then dissociated according to DIN EN ISO 5263-1:2004-12. For this purpose, a sample with a total volume of 2,000 mL was dissociated in a standard dissociator at a consistency of 2.5% without pre-swelling. The dissociation time was 20 minutes, the speed was 3,000 rpm, and the tap water temperature was 40°C. The resulting fiber suspension was then homogenized according to ZM V / 6 / 61. For this purpose, the sample was transferred to a dispenser, diluted with tap water to a consistency of 0.5%, and homogenized for approximately 5 minutes.

[0149] Then, dissociability was tested according to Zellcheming method ZM V / 18 / 62. For this purpose, the total feedstock was sieved for 5 minutes without any other chemical additives using a Brecht-Holl fractionator with a perforated plate of 0.7 mm pore size. The residue was washed into a 2-liter tank and dehydrated through a filter inserted into a Buchner funnel. The filter was folded once and placed in an oven to dry at 105°C until constant weight. The waste was then visually inspected and weighed. The proportion of dried non-pulp components removed was also included in the calculation of the total waste content. Fiber yield was derived from the difference between the initial material (dried, 100%) and the total waste. If the total waste content did not exceed 20%, the product was rated "recyclable"; if the total waste content was between 20% and 50%, it was "recyclable, but product design improvements are warranted"; and if the total waste content exceeded 50% of the initial material input, it was "not reasonably suitable for paper recycling."

[0150] To evaluate the undisturbed paper-forming standard, the total raw material was first sieved following the Zellcheming method ZM V / 1.4 / 86. For this purpose, the total raw material was fractionated for 2 minutes using a Haindl fractionator with a 0.15 mm narrow-mouth plate. The passing fraction was then collected, referred to below as the "qualified material". Paper was then formed on a Rapid Köthen paper forming machine using the qualified material, according to DIN EN ISO 5269-2:2005-03. Two 1.8 g handmade sheets yielded approximately 60 gsm. The drying temperature was approximately 96 °C. For the paper bonding test, the dried handmade paper, along with the roll carrier and cover sheet, was sandwiched between two brass plates and placed in a drying oven where a full-surface pressure of 1.18 kPa was applied for 2 minutes. The sample was then cooled in a shaker for 10 minutes, followed by a paper bonding test and visual inspection for any optical inhomogeneities.

[0151] For the paper adhesion test, the carrier and cover sheet are slowly peeled off the handmade paper one by one. While doing so, the test operator examines for potential adhesion effects. Additionally, the surfaces of the handmade paper, cover sheet, and carrier are inspected for any damage or adhesion to the handmade paper. If no adhesion effect is observed, the product is considered "recyclable"; if some slight adhesion effect is observed with minor damage, it is "limitedly recyclable due to the stickiness of the prepared fiber material"; if adhesion effect is observed with damage, it is "non-recyclable due to the stickiness of the prepared fiber material."

[0152] Then, examine the handmade paper under transmitted light for any defects, transparent and white spots, or dirt spots from ink, coatings, paints, laminating, and adhesive particles. Additionally, evaluate whether the paper is contaminated with any dark colorants. If no or non-interfering optical inhomogeneities are observed, the product is considered "recyclable"; if interfering optical inhomogeneities are observed, the product is considered "limitedly recyclable due to the optical inhomogeneities of the fiber raw material used in its preparation"; and if unacceptable optical inhomogeneities are observed, the product is considered "non-recyclable due to the optical inhomogeneities of the fiber raw material used in its preparation".

[0153] 11) Flat pressure test

[0154] In the flat pressure test, an empty bottle is placed sideways on a plate. A vertical load of 45 N is applied to the bottle, where the diameter of the cylinder is 6 cm. The test passes if the bottle permanently deforms into a substantially flat configuration.

[0155] Personal care composition

[0156] Detergent surfactants

[0157] Personal care compositions may contain more than about 1% by weight of a surfactant system that provides cleaning properties to the composition, or more than 5% by weight of a surfactant system that enables the dissolution of scalp care active ingredients and provides a transparent appearance to the composition. Furthermore, the composition may have sufficient surfactant to achieve micellar or polymer thickening. The surfactant system comprises anionic surfactants and / or combinations of anionic surfactants and / or combinations of anionic surfactants with auxiliary surfactants selected from the group consisting of amphoteric, zwitterionic, nonionic, and mixtures thereof. Various examples and descriptions of detergency surfactants are set forth in U.S. Patent No. 8,440,605, U.S. Patent Application Publication No. 2009 / 155383, and U.S. Patent Application Publication No. 2009 / 0221463, the entire contents of which are incorporated herein by reference.

[0158] Personal care compositions may contain one or more surfactants in amounts of about 10% to about 23%, about 12% to about 21%, or about 10% to about 18% by weight.

[0159] Suitable anionic surfactants for use in the composition are alkyl sulfates and alkyl ether sulfates. Other suitable anionic surfactants are water-soluble salts of organic sulfuric acid reaction products. Other suitable anionic surfactants are reaction products of fatty acids esterified with ethanesulfonate and neutralized with sodium hydroxide. Other similar anionic surfactants are described in U.S. Patents 2,486,921, 2,486,922, and 2,396,278, the entire contents of which are incorporated herein by reference.

[0160] Exemplary anionic surfactants for use in personal care compositions include ammonium lauryl sulfate, ammonium lauryl polyoxyethylene ether sulfate, C10-15 alkyl polyoxyethylene ether sulfate, C10-15 alkyl ammonium sulfate, C11-15 alkyl ammonium sulfate, decyl ammonium sulfate, decyl polyoxyethylene ether sulfate, undecyl ammonium sulfate, undecyl polyoxyethylene ether sulfate, triethylamine lauryl sulfate, triethylamine lauryl polyoxyethylene ether sulfate, triethanolamine lauryl sulfate, triethanolamine lauryl polyoxyethylene ether sulfate, monoethanolamine lauryl sulfate, monoethanolamine lauryl polyoxyethylene ether sulfate, diethanolamine lauryl sulfate, diethanolamine lauryl polyoxyethylene ether sulfate, sodium monolaurate sulfate, sodium lauryl sulfate, sodium lauryl polyoxyethylene ether sulfate, C10-15 alkyl polyoxyethylene ether sulfate, C10-15 alkyl sulfate, C11-15 alkyl Sodium sulfate, sodium decyl sulfate, sodium decyl polyoxyethylene ether sulfate, sodium undecyl sulfate, sodium undecyl polyoxyethylene ether sulfate, potassium lauryl sulfate, potassium lauryl polyoxyethylene ether sulfate, C10-15 alkyl polyoxyethylene ether sulfate, C10-15 alkyl sulfate, C11-15 alkyl sulfate, potassium decyl sulfate, potassium decyl polyoxyethylene ether sulfate, potassium undecyl sulfate, potassium undecyl polyoxyethylene ether sulfate, sodium lauryl sarcosinate, sodium lauroyl sarcosinate, lauryl sarcosinate, cocoyl sarcosinate, ammonium cocoyl sulfate, ammonium lauroyl sulfate, sodium cocoyl sulfate, sodium lauroyl sulfate, potassium cocoyl sulfate, potassium lauryl sulfate, triethanolamine lauryl sulfate, triethanolamine lauryl sulfate, monoethanolamine cocoyl sulfate, monoethanolamine lauryl sulfate, sodium tridecylbenzenesulfonate, sodium dodecylbenzenesulfonate, sodium cocoyl hydroxyethyl sulfonate, and combinations thereof. The anionic surfactant can be sodium lauryl sulfate or sodium lauryl polyoxyethylene ether sulfate.

[0161] The compositions of the present invention may further comprise anionic surfactants selected from the group consisting of: a)R1 O(CH2CHR3O) y SO3M; b) CH3 (CH2) z CHR2 CH2 O (CH2 CHR3O) y SO3M; and c) Their mixture, Where R1 represents CH3(CH2) 10 R2 represents H or a hydrocarbon group containing 1 to 4 carbon atoms, such that the sum of the carbon atoms in z and R2 is 8, R3 is H or CH3, y is 0 to 7, when y is not zero (0), the average value of y is about 1, and M is a monovalent or divalent positively charged cation.

[0162] Suitable anionic alkyl sulfate and alkyl ether sulfate surfactants include, but are not limited to, those having branched alkyl chains, synthesized from C8 to C18 branched alcohols optionally consisting of the group consisting of: Guerbert alcohols, aldol-derived alcohols, carbonyl synthetic alcohols, FT carbonyl synthetic alcohols, and mixtures thereof. Non-limiting examples of 2-alkyl branched alcohols include: carbonyl synthetic alcohols such as 2-methyl-1-undecanol, 2-ethyl-1-decanol, 2-propyl-1-nonanol, 2-butyl-1-octanol, 2-methyl-1-dodecanol, 2-ethyl-1-undecanol, 2-propyl-1-decanol, 2-butyl-1-nonanol, 2-pentyl-1-octanol, 2-pentyl-1-heptanol, and those sold under the trade name: LIAL. ® (Sasol), ISLCHEM ® (Sasol) and NEODOL ® (Shell); and alcohols derived from Gerbert and aldol condensation, such as 2-ethyl-1-hexanol, 2-propyl-1-butanol, 2-butyl-1-octanol, 2-butyl-1-decanol, 2-pentyl-1-nonanol, 2-hexyl-1-octanol, 2-hexyl-1-decanol, and those marketed under the trade name ISOFOL ® Those sold by (Sasol) or as alcohol ethoxylates and alkoxylates under the trade name LUTENSO SOL XP ® (BASF) and LUTENSOL XL ® Those sold by BASF.

[0163] Anionic alkyl sulfates and alkyl ether sulfates may also include those synthesized from C8 to C18 branched alcohols derived from butene or propylene, under the trade name EXXAL. ™ (Exxon) and Marlipal ® (Sasol) is available for sale. This includes anionic surfactants of the subtype of tridecyl polyoxyethylene ether-n sodium sulfate (STnS), wherein n is between about 0.5 and about 3.5. Exemplary surfactants of this subtype are tridecyl polyoxyethylene ether-2 sodium sulfate and tridecyl polyoxyethylene ether-3 sodium sulfate. The compositions of the present invention may also contain sodium tridecyl sulfate.

[0164] The compositions of the present invention may further comprise anionic alkyl and alkyl ether sulfosuccinates and / or dialkyl and dialkyl ether sulfosuccinates, and mixtures thereof. The dialkyl and dialkyl ether sulfosuccinates may be C6-15 straight-chain or branched dialkyl or dialkyl ether sulfosuccinates. The alkyl moiety may be symmetrical (i.e., the same alkyl moiety) or asymmetrical (i.e., different alkyl moiety). Non-limiting examples include: disodium lauryl sulfosuccinate, disodium lauryl polyoxyethylene ether sulfosuccinate, sodium bis(tridecyl) sulfosuccinate, sodium dioctyl sulfosuccinate, sodium dihexyl sulfosuccinate, sodium dicyclohexyl sulfosuccinate, sodium dipentyl sulfosuccinate, sodium diisobutyl sulfosuccinate, straight-chain bis(tridecyl) sulfosuccinates, and mixtures thereof.

[0165] Personal care compositions may contain an auxiliary surfactant. The auxiliary surfactant may be selected from the group consisting of free amphoteric surfactants, amphoteric surfactants, nonionic surfactants, and mixtures thereof. The auxiliary surfactant may include, but is not limited to, lauramidopropyl betaine, cocamidopropyl betaine, lauramidohydroxysulfobetaine, sodium lauroamphoacetate, disodium cocoamphodiacetate, cocoamide monoethanolamide, and mixtures thereof.

[0166] The personal care composition may also contain one or more amphoteric, zwitterionic, nonionic auxiliary surfactants or mixtures thereof, in amounts of about 0.5% to about 8%, about 1.0% to about 7%, about 1.5% to about 6% by weight.

[0167] Suitable amphoteric or zwitterionic surfactants for use in the personal care compositions herein include those known for use in shampoos or other personal care cleansing agents. Non-limiting examples of suitable zwitterionic or zwitterionic surfactants are described in U.S. Patent Nos. 5,104,646 and 5,106,609, the entire contents of which are incorporated herein by reference.

[0168] Suitable amphoteric auxiliary surfactants for use in compositions include those surfactants described as derivatives of aliphatic secondary and tertiary amines, wherein the aliphatic group may be linear or branched, and wherein one of the aliphatic substituents contains about 8 to about 18 carbon atoms, and one of the aliphatic substituents contains an anionic group, such as a carboxyl group, sulfonate group, sulfate group, phosphate group, or phosphonate group. Suitable amphoteric surfactants include, but are not limited to, those selected from the group consisting of: sodium cocoaminopropionate, sodium cocoaminodipropionate, sodium cocoamphoacetate, sodium cocoamphodiacetate, sodium cocoamphohydroxypropyl sulfonate, sodium cocoamphopropionate, sodium zeinylamphopropionate, sodium laurylaminopropionate, sodium lauroylamphoacetate, sodium lauroylamphodiacetate, sodium lauroylamphohydroxypropyl sulfonate, sodium lauroylamphopropionate, sodium zeinylamphopropionate, sodium lauryliminodipropionate, and ammonium cocoaminopropionate. Ammonium cocoaminopropionate, Ammonium cocoamphoacetate, Ammonium cocoamphodiacetate, Ammonium cocoamphohydroxypropyl sulfonate, Ammonium cocoamphopropionate, Ammonium zearalenone, Ammonium laurylaminopropionate, Ammonium lauroamphoacetate, Ammonium lauroamphodiacetate, Ammonium lauroamphohydroxypropyl sulfonate, Ammonium lauroamphopropionate, Ammonium zearalenone, Ammonium lauryliminopropionate, Triethanolamine cocoaminopropionate, Triethanolamine cocoaminopropionate, Triethanolamine cocoamphoacetate, Triethanolamine cocoamphohydroxypropyl sulfonate, Ammonium cocoaminopropionate Triethanolamine sulfonate, Triethanolamine cocoamphopropionic acid, Triethanolamine zearalenone propionic acid, Triethanolamine laurylaminopropionic acid, Triethanolamine lauroylamphoacetic acid, Triethanolamine lauroylamphohydroxypropyl sulfonic acid, Triethanolamine lauroylamphopropionic acid, Triethanolamine zearalenone propionic acid, Triethanolamine lauryliminodipropionic acid, Triethanolamine cocoamphodipropionic acid, Disodium decanoylamphodiacetate, Disodium decanoylamphodipropionic acid, Disodium octanoylamphodiacetate, Disodium octanoylamphodipropionic acid, Disodium cocoamphocarboxyethylhydroxypropyl sulfonate Disodium cocoamphodiacetate, disodium cocoamphodiapropionate, disodium dicarboxyethyl cocopropanediamine, disodium lauryl polyoxyethylene ether-5-carboxyamphodiacetate, disodium lauryliminodiapropionate, disodium lauroylamphodiacetate, disodium lauroylamphodiapropionate, disodium oleylamphodiapropionate, disodium PPG-2-isodecyl alcohol polyether-7-carboxyamphodiacetate, laurylaminopropionic acid, lauroylamphodiapropionic acid, laurylaminopropylglycine, lauryl diethylenediaminoglycine, and mixtures thereof.

[0169] The composition may include a zwitterionic auxiliary surfactant, wherein the zwitterionic surfactant is a derivative of an aliphatic quaternary ammonium, phosphonium, and sulfonium compound, wherein the aliphatic group may be linear or branched, and wherein one of the aliphatic substituents contains about 8 to about 18 carbon atoms, and one of the aliphatic substituents contains an anionic group, such as a carboxyl group, sulfonate group, sulfate group, phosphate group, or phosphonate group. Amphoteric surfactants may be selected from the group consisting of: cocamidopropyl betaine, cocamidopropylamine oxide, cocamidopropyl betaine, cocamidopropyl dimethylaminohydroxypropyl hydrolyzed collagen, cocamidopropyl dimethylaminohydroxypropyl hydrolyzed collagen, cocamidopropyl hydroxysulfonyl betaine, cocamidopropyl amphoteric propionate, cocamidopropyl betaine, cocamidopropyl hydroxysulfonyl betaine, cocamidopropyl betaine, cocamidopropyl betaine, lauryl betaine, lauryl hydroxysulfonyl betaine, lauryl sulfonyl betaine, and mixtures thereof.

[0170] Nonionic surfactants suitable for use in this invention include those described in McCutcheion's "Detergents and Emulsifiers" North American edition (1986, Allured Publishing Corp.) and McCutcheion's "Functional Materials" North American edition (1992). Nonionic surfactants suitable for use in the personal care compositions of this invention include, but are not limited to, polyoxyethylene alkylphenols, polyoxyethylene alcohols, polyoxyethylene polypropylene glycol, glycerides of alkanonic acids, polyglycerides of alkanonic acids, propylene glycol esters of alkanonic acids, sorbitan esters of alkanonic acids, polyoxyethylene sorbitan esters of alkanonic acids, polyoxyethylene glycol esters of alkanonic acids, polyoxyethylene alkanonic acids, alkanolamides, N-alkylpyrrolidones, alkyl glycosides, alkyl polyglucosides, alkylamine oxides, and polyoxyethylene siloxanes.

[0171] The auxiliary surfactant may be a nonionic surfactant selected from the following alkanolamide groups: cocamide, cocamide methyl MEA, cocamide DEA, cocamide MEA, cocamide MIPA, lauramide DEA, lauramide MEA, lauramide MIPA, tetradecamide DEA, tetradecamide MEA, PEG-20 cocamide MEA, PEG-2 cocamide, PEG-3 cocamide, PEG-4 cocamide, PEG-5 cocamide, PEG-6 cocamide, PEG-7 cocamide, PEG-3 lauramide, PEG-5 lauramide, PEG-3 oleamide, PPG-2 cocamide, PPG-2 hydroxyethyl cocamide, PPG-2 hydroxyethyl isostearamide, and mixtures thereof.

[0172] Representative polyoxyethylene alcohols include those with alkyl chains in the C9-C16 range and having about 1 to about 110 alkoxy groups, including but not limited to lauryl polyoxyethylene ether-3, lauryl polyoxyethylene ether-23, cetyl polyoxyethylene ether-10, stearyl polyoxyethylene ether-10, stearyl polyoxyethylene ether-100, behenyl polyoxyethylene ether-10, and those that may be traded under the name Neodol. ® 91. Neodol ® 23. Neodol ® 25. Neodol ® 45. Neodol ® 135. Neodo ® l 67、Neodol ® PC 100, Neodol ® PC 200, Neodol ® PC 600 is obtained commercially from Shell Chemicals (Houston, Texas), as well as mixtures thereof.

[0173] It is also available for commercial purchase and can be obtained through Brij ® Polyoxyethylene fatty ethers obtained from Uniqema (Wilmington, Delaware), including but not limited to Brij ® 30. Brij ® 35. Brij ® 52. Brij ® 56. Brij ® 58. Brij ® 72. Brij ® 76. Brij ® 78. Brij ® 93. Brij ® 97. Brij ® 98. Brij ® 721, and their mixtures.

[0174] Suitable alkyl glycosides and alkyl polyglucosides can be represented by the formula (S)nOR, where S is the sugar moiety such as glucose, fructose, mannose, galactose, etc.; n is an integer from about 1 to about 1000; and R is a C8-C30 alkyl group. Examples of long-chain alcohols from which the alkyl group can be derived include decanol, lauryl alcohol, tetradecyl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, etc. Examples of these surfactants include alkyl polyglucosides, where S is the glucose moiety, R is a C8-20 alkyl group, and n is an integer from about 1 to about 9. Commercially available examples of these surfactants include those marketed under the trade name APG.® 325 CS, APG ® 600 CS and APG ® 625 CS) were purchased from Cognis (Ambler, Pa) as decyl polyglucoside and lauryl polyglucoside. Also used in this article are sucrose ester surfactants such as sucrose cocoate and sucrose lauryl ester, as well as those marketed under the trade name Triton. ™ BG-10 and Triton ™ CG-110 was purchased from The Dow Chemical Company (Houston, Tx) as an alkyl polyglucan.

[0175] Other nonionic surfactants suitable for use in this invention are glycerides and polyglycerides, including but not limited to, glyceryl monoesters, glyceryl monoesters of C12-22 saturated, unsaturated and branched fatty acids such as glyceryl oleate, glyceryl monostearate, glyceryl monopalmitate, glyceryl behenate, and mixtures thereof, and polyglycerides of C12-22 saturated, unsaturated and branched fatty acids such as polyglyceryl-4 isostearate, polyglyceryl-3 oleate, polyglyceryl-2-sesquioleate, diisostearyl triglyceride, diglyceryl monooleate, tetraglyceryl monooleate, and mixtures thereof.

[0176] Other nonionic surfactants that can be used in this article are sorbitol esters. Sorbitol esters of C12-22 saturated, unsaturated, and branched fatty acids are suitable for use in this article. These sorbitol esters typically comprise mixtures of monoesters, diesters, trimers, etc. Representative examples of suitable sorbitol esters include sorbitol monolaurate (SPAN). ® 20) Sorbitol monopalmitate (SPAN) ® 40) Sorbitol monostearate (SPAN) ® 60) Sorbitol Tristearate (SPAN) ® 65) Sorbitol monooleate (SPAN) ® 80), Sorbitol trioleate (SPAN) ® 85), and sorbitol isostearate.

[0177] Also applicable to this article are alkoxylated derivatives of sorbitol esters, including but not limited to polyoxyethylene (20) sorbitol monolaurate (Tween) esters, all purchased from Uniqema. ® 20), Polyoxyethylene (20) dehydrated sorbitan monopalmitate (Tween ® 40), Polyoxyethylene (20) dehydrated sorbitan monostearate (Tween) ®60), Polyoxyethylene (20) dehydrated sorbitan monooleate (Tween) ® 80), Polyoxyethylene (4) dehydrated sorbitol monolaurate (Tween ® 21) Polyoxyethylene (4) dehydrated sorbitan monostearate (Tween ® 61) Polyoxyethylene (5) dehydrated sorbitan monooleate (Tween ® 81), and their mixtures.

[0178] Also applicable to this article are alkylphenol ethoxylates, including but not limited to nonylphenol ethoxylates (Tergitol, purchased from The Dow Chemical Company (Houston, Tx.)). ™ NP-4, NP-6, NP-7, NP-8, NP-9, NP-10, NP-11, NP-12, NP-13, NP-15, NP-30, NP-40, NP-50, NP-55, NP-70) and octylphenol ethoxylate (Triton, purchased from The Dow Chemical Company (Houston, TX)). ™ X-15, X-35, X-45, X-114, X-100, X-102, X-165, X-305, X-405,

[0179] Also applicable to this article are tertiary alkylamine oxides, including lauryl amine oxides and cocoyl amine oxides.

[0180] Non-limiting examples of other anionic, amphoteric, amphoteric and nonionic adjunct surfactants suitable for use in personal care compositions are described in McCutcheon’s Emulsifiers and Detergents (1989 Yearbook, published by MC Publishing Co.), and in U.S. Patents 3,929,678, 2,658,072, 2,438,091 and 2,528,378, the full text of which is incorporated herein by reference.

[0181] A suitable surfactant combination contains about 0.5% to about 30%, about 1% to about 25%, and about 2% to about 20% of the average weight of alkyl branches.

[0182] The surfactant combination may have a cumulative average weight of about 7.5% to about 25%, about 10% to about 22.5%, and about 10% to about 20% of C8 to C12 alkyl chain length.

[0183] The surfactant combination may have an average C8-C12 / C13-C18 alkyl chain ratio of about 3 to about 200, about 25 to about 175.5, about 50 to about 150, or about 75 to about 125.

[0184] wetting agent

[0185] This invention may include a wetting agent. The wetting agent has an affinity for the hydrogen bonds of water molecules. Non-limiting examples of suitable wetting agents for use in this invention may include the following: amino acids and their derivatives such as proline and aspartic acid arginine, 1,3-butanediol, propylene glycol and water, as well as soft-haired pine algae extract, collagen amino acids or peptides, creatine, diglycerides, biosaccharide gum-1, glucosamine salts, glucuronides, glutamate, polyethylene glycol ethers of glycerol (e.g., glycerol polyether 20), glycerol, glycerol monopropoxylates, glycogen, hexanediol, honey and its extracts or derivatives, hydrogenated starch hydrolysate, hydrolyzed mucopolysaccharides, inositol, keratin amino acids, LAREX A-200 (purchased from Larex), glycosaminoglycans, methoxy PEG-10, methyl glucetol polyether-10 and methyl glucetol polyether-20 (both available from Amerchol in Edison, NJ), methyl glucose, 3-methyl-1,3-butanediol, N-acetyl glucosamine salts, polyethylene glycol and its derivatives (such as PEG-15 butanediol, PEG-15 butanediol, PEG-15 butanediol, PEG-15 butanediol, PEG-10 ... 4. PEG5 (Pentaerythritol, PEG6, PEG8, PEG9), pentaerythritol, 1,2-pentanediol, PPG-1 glyceryl ether, PPG-9,2-pyrrolidone-5-carboxylic acid and its salts (such as glyceryl PCA), glycoisoesters, SEACARE (purchased from Secma), sericin, sericin amino acids, sodium acetylated hyaluronic acid, sodium hyaluronate, sodium polyaspartate, sodium polyglutamate, sorbitol 20, sorbitol 6, sugars and sugar alcohols and their derivatives such as glucose, sucrose, fructose, mannose and polyglycerol sorbitol, trehalose, triglycerides, trimethylolpropane, tri(hydroxymethyl)aminomethane salts and yeast extracts and mixtures thereof, ionic salts such as sodium chloride and potassium chloride and mixtures thereof.

[0186] In this invention, the wetting agent may be a polyol selected from the group consisting of: glycerol, diglycerol, glycerin, erythritol, arabinitol, xylitol, ribitol, mannitol, sorbitol, galactitol, fucitol, maltitol, mannose, inositol, triethylene glycol, sodium pyrrolidone carboxylate (PCA), zinc PCA, and derivatives and mixtures thereof.

[0187] The composition contains a safe and effective amount of wetting agent. In particular, it may contain about 20% to about 70%; about 20% to about 50%; about 23% to about 45%; by weight of the wetting agent.

[0188] In this invention, the composition may contain two or more different wetting agents; for example, the composition may contain glycerin and xylitol.

[0189] Thickening polymer

[0190] Personal care compositions may contain a thickening polymer to increase the viscosity of the composition. Suitable thickening polymers may be used. Personal care compositions may contain about 0.05% to about 10% thickening polymer, about 0.05% to about 5% thickening polymer, about 0.05% to about 2.5% thickening polymer, and about 0.05% to about 2% thickening polymer. The thickening polymer modifier may be a polyacrylate or a polyacrylamide thickener. The thickening polymer may be an anionic thickening polymer.

[0191] Personal care compositions may contain a thickening polymer, which is a homopolymer based on acrylic acid, methacrylic acid or other related derivatives, and non-limiting examples include polyacrylates, polymethacrylates, polyethyl acrylates and polyacrylamide.

[0192] The thickening polymer may be an alkali-swellable and hydrophobically modified alkali-swellable acrylic copolymer or methacrylate copolymer. Non-limiting examples include acrylic acid / acrylonitrile copolymers, acrylate / stearyl polyoxyethylene ether-20 itaconic acid copolymers, acrylate / cetyl polyoxyethylene ether-20 itaconic acid copolymers, acrylate / aminoacrylate / C10-30 alkyl PEG-20 itaconic acid copolymers, acrylate / aminoacrylate copolymers, acrylate / stearyl polyoxyethylene ether-20 methacrylate copolymers, and acrylic acid... Ester / behenyl polyoxyethylene ether-25 methacrylate copolymer, acrylate / stearyl polyoxyethylene ether-20 methacrylate crosspolymer, acrylate / behenyl polyoxyethylene ether-25 methacrylate / HEMA crosspolymer, acrylate / vinyl neodecanoate crosspolymer, acrylate / vinyl isodecanoate crosspolymer, acrylate / palm oil alcohol polyether-25 acrylate copolymer, acrylic acid / acrylamidomethylpropane sulfonic acid copolymer, and acrylate / acrylic acid C10-C30 alkyl acrylate crosspolymer.

[0193] The thickening polymer can be a soluble crosslinked acrylic polymer, and non-limiting examples include carbomer.

[0194] The thickening polymer may be an associative polymer thickener, and non-limiting examples include: hydrophobically modified alkali-swellable emulsions, and non-limiting examples include hydrophobically modified polyacrylates; hydrophobically modified polyacrylic acid and hydrophobically modified polyacrylamide; hydrophobically modified polyethers, wherein these materials may have a hydrophobicity selected from cetyl, stearyl, oleoyl and combinations thereof.

[0195] Thickening polymers can be used in combination with polyvinylpyrrolidone, cross-linked polyvinylpyrrolidone, and derivatives. Thickening polymers can also be used in combination with polyvinyl alcohol and derivatives. Furthermore, thickening polymers can be used in combination with polyethyleneimine and derivatives.

[0196] The thickening polymer can be combined with alginate-based materials, and non-limiting examples include sodium alginate and propylene glycol alginate.

[0197] The thickening polymer can be used in combination with polyurethane polymers, and non-limiting examples include hydrophobically modified alkoxylated polyurethane polymers, including PEG-150 / decyl alcohol / SMDI copolymers, PEG-150 / stearyl alcohol / SMDI copolymers, and polyurethane-39.

[0198] Thickening polymers can be combined with associative polymer thickeners, and non-limiting examples include: hydrophobically modified cellulose derivatives; and hydrophilic portions of ethylene oxide repeating groups having about 10 to about 300, about 30 to about 200, or about 40 to about 150 repeating units. Non-limiting examples of this type include PEG-120-methylglucose dioleate, PEG-(40 or 60) sorbitol tetraoleate, PEG-150 pentaerythritol tetrastearate, PEG-55 propylene glycol oleate, and PEG-150 distearate.

[0199] Thickening polymers can be combined with cellulose and derivatives, and non-limiting examples include microcrystalline cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, methyl cellulose, ethyl cellulose; nitrocellulose; cellulose sulfate; cellulose powder; and hydrophobically modified cellulose.

[0200] The thickening polymer can be combined with guar gum and guar gum derivatives, with non-limiting examples including hydroxypropyl guar gum and hydroxypropyl guar gum hydroxypropyltrimethylammonium chloride.

[0201] Thickening polymers can be used with polyethylene oxide, polypropylene oxide, and POE-PPO copolymers.

[0202] Thickening polymers can be combined with polyalkylene glycols characterized by the following general formula:

[0203] Wherein R is hydrogen, methyl, or a mixture thereof, and further is hydrogen, and n is an integer having an average of 2,000-180,000, or 7,000-90,000, or 7,000-45,000. Non-limiting examples of this type include PEG-7M, PEG-14M, PEG-23M, PEG-25M, PEG-45M, PEG-90M, or PEG-100M.

[0204] Thickening polymers can be combined with silica, and non-limiting examples include pyrolytic silica, precipitated silica, and silica with an organosilicon surface treatment.

[0205] Thickening polymers can be combined with water-swellable clays, and non-limiting examples include synthetic lithium saponite, bentonite, montmorillonite, chlorophyllite, and lithium montmorillonite.

[0206] Thickening polymers can be combined with gums, and non-limiting examples include xanthan gum, guar gum, hydroxypropyl guar gum, gum arabic, tragacanth gum, galactomannan, long bean gum, black privet gum, and locust bean gum.

[0207] Thickening polymers can be combined with the following substances: dibenzyl sorbitol, carrageenan, pectin, agar, quince seeds, starch (from rice, corn, potatoes, wheat, etc.), starch derivatives (e.g., carboxymethyl starch, methyl hydroxypropyl starch), algal extracts, dextran, succinyl dextran, and pulleran. Non-limiting examples of thickening polymers include acrylamide / ammonium acrylate copolymers (and) polyisobutylene (and) polysorbate 20; acrylamide / sodium acryloyl dimethyl taurate copolymer / isohexadecane / polysorbate 80; ammonium acryloyl dimethyl taurate / VP copolymer; sodium acrylate / sodium acryloyl dimethyl taurate copolymer; acrylate copolymers; acrylate crosslinker-4; acrylate crosslinker-3; acrylate / behenyl polyoxyethylene ether-25 methacrylate copolymer; acrylate / acrylic acid C10-C30 alkyl ester crosslinker; acrylate / stearyl polyoxyethylene ether-20 itaconic acid copolymer; poly… Ammonium acrylate / isohexadecane / PEG-40 castor oil; carbomer, sodium carbomer, crosslinked polyvinylpyrrolidone (PVP), polyacrylamide / C13-14 isoparaffin / lauryl polyoxyethylene ether-7, polyacrylate 13 / polyisobutylene / polysorbate 20, polyacrylate crosslinked polymer-6, polyamide-3, polyquaternium-37 (and) hydrogenated polydecene (and) tridecyl polyoxyethylene ether-6, acrylamide / sodium acryloyldimethyl taurate / acrylic acid copolymer, sodium acrylate / acryloyldimethyl taurate / dimethylacrylamide, crosslinked polymer (and) isohexadecane (and) polysorbate 60, sodium polyacrylate. Exemplary commercially available thickening polymers include: ACULYN ™ 28. ACULYN ™ 33. ACULYN ™ 88. ACULYN ™ 22. ACULYN ™ Excel, Carbopol ® Aqua SF-1, Carbopol ® ETD 2020, Carbopol ® Ultrez 20, Carbopol ® Ultrez 21, Carbopol ® Ultrez 10, Carbopol ® Ultrez 30, Carbopol ® 1342, Carbopol ® Aqua SF-2 polymer, Sepigel ™ 305, Simulgel ™ 600, Sepimax Zen, Carbopol ® SMART 1000, Rheocare ® TTA, Rheomer ® SC-Plus, STRUCTURE ®PLUS, Aristoflex ® AVC, Stabylen 30, and combinations thereof.

[0208] Scalp care active ingredients

[0209] This invention may include scalp care active ingredients. These scalp care active ingredients include soluble scalp care active ingredients and scalp health agents.

[0210] a) Soluble scalp care active ingredients

[0211] Soluble scalp care active ingredients and / or anti-dandruff agents may be a material or mixture selected from the group consisting of: azoles, such as clomibazole, ketoconazole, itraconazole, econazole and neoconazole; hydroxypyridinones, such as oxymetholone (pyrrolidone ethanolamine), ciclopirox, lilopiprox and MEA-hydroxyoctyloxypyridinone; keratolytic agents, such as salicylic acid and other hydroxy acids; agaricone, such as pyraclostrobin; and metal chelating agents, such as 1,10-phenanthroline.

[0212] In this invention, the azole antimicrobial agent may be an imidazole, selected from the group consisting of: benzimidazole, benzothiazole, bifonazole, butanazole nitrate, clotrimazole, clotrimazole, kluconazole, epconazole, econazole, neoconazole, fenteconazole, fluconazole, flutriazole, isoconazole, ketoconazole, lanoconazole, metronidazole, miconazole, neconazole, omeconazole, oxiconazole nitrate, sertaconazole, thioconazole nitrate, thiaconazole, thiazole, and mixtures thereof; or the azole antimicrobial agent may be a triazole, selected from the group consisting of: terconazole, itraconazole, and mixtures thereof. The azole antimicrobial agent may be ketoconazole. Additionally, the sole antimicrobial agent may be ketoconazole.

[0213] Soluble antidandruff agents may be present in amounts of about 0.01% to 10%, about 0.1% to about 9%, about 0.25% to 8%, and about 0.5% to 6%. Soluble antidandruff agents may be surfactant-soluble, and thus may be surfactant-soluble antidandruff agents.

[0214] b) Scalp health supplement

[0215] In this invention, one or more scalp health agents may be added to provide beneficial scalp effects and / or antifungal / dandruff-reducing efficacy. This group of materials is varied and provides a broad range of beneficial effects, including moisturizing, barrier-improving, antifungal, antimicrobial, and antioxidant agents, antipruritic and sensory agents, and additional antidandruff agents such as polyvalent metal salts of pyrithione, non-limiting examples including zinc pyrithione (ZPT) and copper pyrithione, sulfur, or selenium sulfide. Such scalp health agents include, but are not limited to: vitamins E and F, salicylic acid, niacinamide, caffeine, panthenol, zinc oxide, zinc carbonate, basic zinc carbonate, glycols, glycolic acid, PCA, PEG, erythritol, glycerin, lactates, hyaluronic acid esters, allantoin and other ureas, betaine, sorbitol, glutamate, xylitol, menthol, menthyl lactate, vanillyl butyl ether, isocyclic ketones, benzyl alcohol, and compounds comprising the following structures:

[0216] R1 is selected from H, alkyl, aminoalkyl, and alkoxy; Q = H2, O, -OR1, -N(R1)2, -OPO(OR1) x -PO(OR1) x -P(OR1) x , where x = 1-2; V = NR1, O, -OPO(OR1) x -PO(OR1) x -P(OR1) x , where x = 1-2; W = H2, O; For n=0, X and Y are independently selected from H, aryl, and naphthyl groups; For n ≥ 1, X and Y = aliphatic CH2 or aromatic CH, and Z is selected from aliphatic CH2, aromatic CH, or heteroatom; A = lower alkoxy, lower alkathiol, aryl, substituted aryl, or fused aryl; and Stereochemistry can be used for labeling The position changes.

[0217] And natural extracts / oils, including peppermint oil, spearmint, argan oil, jojoba oil and aloe vera.

[0218] In this invention, the scalp care active ingredient may be in encapsulated form. In one aspect, the capsule may comprise: polyacrylamide, organosilicon, silica, polystyrene, polyurea, polyurethane, polyacrylate-based materials, gelatin, styrene-malic anhydride, polyamide, aromatic alcohols, polyvinyl alcohol, fatty alcohols, polysaccharides, waxes, hydrogenated vegetable oils, and other materials known to those skilled in the art. In one aspect, the polyurea may include cross-linked ureas, such as ureas cross-linked with formaldehyde, ureas cross-linked with glutaraldehyde, and mixtures thereof. In one aspect, the polysaccharide may include gelatin, agar, alginate, chitosan, cellulose, glycogen, hyaluronic acid, dextran, xylan, inulin, pectin, and mixtures thereof. In one aspect, the polysaccharide may be cross-linked. Suitable cross-linking agents may include calcium chloride, calcium carbonate, isocyanates, glutaraldehyde, and mixtures thereof. Typically, anti-dandruff or scalp care active ingredients can be present in encapsulated form at concentrations ranging from 1% to 5% by weight based on the total formulation weight, and even up to 50% by weight or higher, depending on the chemical properties of the material to be encapsulated and the encapsulation structure itself. In this invention, the composition may contain up to 90%, up to 10%, up to 5%, or up to 1% encapsulating material.

[0219] In this invention, the personal care composition can be transparent or clear. As used herein, the terms "clear" or "transparent" mean that the percentage of transparency (T%) of the composition at 600 nm is at least about 70% transmittance. The T% at 600 nm can be about 70% to about 100%, about 80% to about 100%, or about 90% to about 100%. In this invention, the percentage of transparency (T%) at 600 nm can be at least about 80% transmittance; the percentage of transparency (T%) at 600 nm can be at least about 90% transmittance.

[0220] In this invention, the personal care composition may be translucent or opaque. The transparency of the composition is measured by ultraviolet / visible (“UV / VIS”) spectrophotometry, and the absorption or transmission of UV / VIS light by the sample is determined using the Gretag Macbeth Colorimeter. It has been shown that a light wavelength of 600 nm is sufficient to characterize the transparency of the cleaning composition.

[0221] The personal care composition of the present invention may contain about 14% to about 50% water; or about 35% to about 50% water.

[0222] Test methods for formulation

[0223] Water activity

[0224] In this invention, water activity is measured as Aw (when on a scale of 0-1) or relative humidity -%RH (when reported as a percentage), where RH% = aw 100. The water activity (Aw) of a personal care composition is the ratio between the vapor pressure of the personal care composition itself and the vapor pressure of distilled water under the same conditions when it is in undisturbed equilibrium with the surrounding air medium.

[0225] Water activity determination

[0226] In this invention, the apparatus used for water activity determination can be: A) a Hygrolab C-1 water activity meter (purchased from Rotronic AG) equipped with temperature and humidity probes and B) a shallow disposable sample cup (purchased from Rotronic AG). In this invention, the water activity of the test material can be determined using temperature and humidity probes and the Hygrolab C-1 water activity meter (purchased from Rotronic AG). The disposable sample cup (purchased from Rotronic AG) is filled with the test material, lowered into a sample holder, and covered by the humidity and temperature probes. Using the AwE mode of the water activity meter, the water activity of the equilibrium product will be displayed as water activity (Aw) on the meter. The following conversion factor can be used to switch between units: 1.000Aw = 100%RH. Viscosity method.

[0227] The present invention may have a water activity (Aw) of about 0.40 to about 0.90; may have a water activity (Aw) of about 0.80 to about 0.87. The present invention may have a water activity (Aw) of less than about 0.80.

[0228] Viscosity Measurement

[0229] In this invention, the equipment and instruments used for viscosity measurement are: A) a disposable syringe (purchased from VWR); a rheometer (purchased from TA Instruments); and C) a 40mm parallel steel plate (purchased from TA Instruments). In this invention, the viscosity of the shampoo test material can be measured using a Discovery DHR rheometer purchased from TA Instruments (New Castle, Delaware, USA). Data collection, processing, and reporting are performed using TRIOS software version 5.1.1.46572 (purchased from TA Instruments). The instrument is configured using a parallel steel plate with a diameter of 40mm, a gap size of 1000µm, and a temperature of 25°C. A shear rate of 2.0 s⁻¹ is used. -1Data is collected by holding the flow peak for 180 seconds, and the reported viscosity is the value measured at 180 seconds. In this invention, the viscosity of the personal care composition may be from about 5,000 cps to about 20,000 cps; from about 8,000 cps to about 14,000 cps; or from about 7,000 cps to about 12,000 cps.

[0230] Example Table: Compressible Fiber-Based Bottle Packaging

[0231] Table 1

[0232] Example

[0233] Table 1 includes examples of squeezeable bottles that can be used for storing and dispensing consumer products. All bottles in these examples have a net capacity of at least 150 ml. All evaluated bottles were found to be leak-free and free of pinholes larger than 10 micrometers. The bottles were tested for fiber content, spray integrity according to a water resistance method, squeezeability according to the PTS-RH 021 / 97 cat 2 method, and resizing properties. The moisture barrier properties of the sidewalls and base of the bottles in these examples were also evaluated.

[0234] Example 1 discloses a commercially available paper tube that uses liquid cardboard as sidewalls, with welded polyethylene shoulders and a polyethylene cap featuring movable hinges. This embodiment was found to have a low fiber content and a low fiber recovery rate of less than 50% in repulping.

[0235] Examples 2-6 cover different embodiments of the invention, all of which (1) have a fiber content greater than 85%, (2) pass the extrusion test, (3) have a sidewall and base vapor transmission rate of less than 20 g / sqm / day at 25°C and 60% RH, (4) pass the water resistance test, and (5) fully pass the PTS-RH 021 / 97 cat 2 test with a fiber recovery rate of 80% or higher. Furthermore, all bottles can be flattened and extruded into near-empty containers to ensure optimal disposal while minimizing product waste residue.

[0236] Example 2 discloses an extrudable fiber-based bottle having a padded wet-molded base and sidewalls, comprising a single-layer coated liquid cardboard. The liquid cardboard is a 270 gsm pulp raw material with a 30 gsm LDPE coating. In this example, the pulp molding base 120 is molded from a pulp comprising 50% bamboo, 40% bagasse, and 10% softwood fiber portions. The pulp also contains 1% AKD added as a 10% emulsion. The pulp molding base 120 includes a base barrier structure 140 composed of a laminate from NOVA comprising nucleated HDPE. The average thickness of the laminate before and after molding is 90 micrometers and 60 micrometers, respectively. The pulp molding base 120 includes a small silicone valve 150 to facilitate dispensing. The valve is sandwiched between the pulp molding base 120 and the liquid receiving surface 128, and according to... Figure 1a The structure shown. Valve 150 is externally sealed by a removable membrane patch (not shown) to prevent accidental dispensing during dispensing and storage.

[0237] In this invention, Example 3 discloses an extrudable fiber-based bottle, which may have a sprayed wet-molded base 120 and sidewalls 112, comprising a single-layer coated liquid cardboard. A pulp molding base barrier structure 140 is applied to the liquid-containing surface 128 of the pulp molding base 120 and includes a primer and topcoat applied by spraying. The valve 150 is the same as in Example 2.

[0238] Example 4 discloses a method such as Figure 5b The extrudable fiber-based bottle shown has a padded wet-molded base 120 and sidewalls 112, including a double-coated liquid carton board. The liquid carton board is a high-barrier, double-coated liquid carton board from Stora Enso, sold under the name Natura Barr. The padded base, valve, and valve assembly are identical to those in Example 2.

[0239] Example 5 discloses an extrudable fiber-based bottle having a gasketed wet-molded base and coated wet-molded sidewalls. The sidewalls are integrally manufactured using a wet molding process with the same slurry disclosed in Example 2. The sidewalls are highly flexible and deformable. A barrier system is applied to the inner surface of the sidewalls and includes a primer and a topcoat applied by spraying. The gasketed base, valve, and valve assembly are identical to those in Example 2.

[0240] Example 6 discloses an extrudable fiber-based bottle having a gasketed wet-molded base and coated wet-molded sidewalls. Except for the base assembly, the bottle's construction is the same as in Example 5. In this invention, as... Figure 11a and Figure 11bAs shown, the valve can be clamped between the pulp molding base and the additional molding cap.

[0241] The product has been reformulated to reduce water activity and water content.

[0242] In this invention, the water activity and water content of commercially available shampoo formulations are reduced by removing any added water that is not part of the formulation (e.g., surfactants typically enter as part of an aqueous solution). Because the shampoo needs to be liquid and have a viscosity similar to commercially available shampoos (to allow for good spreadability on the hair), only flowable liquids and soluble solids are considered to replace the 29%-41% added water in commercially available cosmetic shampoos. Since it is desirable not only to reduce the water content but also to reduce the water activity (flowability) of the remaining water in the formulation, water-binding components (wetting agents) are selected. Replacing 29%-41% of the water in the shampoo with a combination of glycerin and sodium chloride yields a stable formulation with lower water content and activity. Furthermore, glycerin is known to provide a conditioning feel to hair compared to water.

[0243] Non-limiting embodiments

[0244] The personal care compositions illustrated in the following examples can be prepared using conventional formulation and mixing methods. Unless otherwise specified, all illustrative amounts are listed as a weight percentage based on the active ingredient and exclude trace materials such as diluents, preservatives, colored solutions, hypothetical ingredients, herbal medicines, etc. Unless otherwise specified, all percentages are based on weight.

[0245] Formulation Examples

[0246] Examples A and B are conventional cosmetic formulation examples with high water activity (Aw), which are included as a control comparison with Example C1, which is a formulation example of the present invention with reduced water activity (Aw).

[0247] Example description: A - Traditional shampoos with higher Aw B - Traditional anti-dandruff shampoos with higher Aw C - Lower Aw D - Lower Aw E - Lower Aw, reduces dandruff F - Lower Aw, anti-dandruff G - Lower Aw, Alternative Wetting Agent H-low Aw, sulfate-free I-lower Aw, sulfate-free

[0248] Ingredient Code :

[0249] Fiber-based bottles with lower Aw shampoo stability data

[0250] The lower water activity (Aw) shampoo formulation Example D was placed in the fiber-based bottle of Example 3, and the weight change over time was measured using the weight reduction test method #7 described above (page 26). The control group, consisting only of water, represents high water activity liquids, such as the high Aw shampoo formulation Example A. Under typical dispensing and use temperature and humidity conditions in temperate countries (ICH Region 1), the weight change of the lower Aw shampoo over time was significantly smaller. Figure 16 The chart shows that the high-Aw formulation exhibits a significant weight change in this fiber-based bottle compared to a low-Aw formulation example with a weight change of less than 10% under the same conditions.

[0251] The low weight change rate of the lower Aw formulation can be used to extend the usable shelf life of commercially available products. In this invention, as shown in Table 2 of Example 3 (II) below, this low weight change rate can be used to maximize fiber content, wherein the total coating thickness is 40 µm and the total raw material fiber % is 98%. The formulation of Example D, combined with the wall material of Example 3 (II), results in a weight loss of less than 20 g / sqm / day at 25°C and 60% RH.

[0252] Table 2

[0253] Additional Examples / Combinations

[0254] A. A squeezable fiber-based bottle in combination with a liquid personal care composition, the liquid personal care composition comprising: a pulp-molded base, the pulp-molded base including a liquid-receiving surface having orifices for dispensing a viscous liquid, the pulp-molded base having a base periphery having a peripheral surface including an upper edge and a lower edge, and a base barrier structure disposed on the liquid-receiving surface and the upper edge of the base periphery; A fiber-based sidewall having an upper edge, a lower edge, an outer surface, and an inner surface, the inner surface including a fiber-based sidewall barrier structure, wherein the lower edge of the fiber-based sidewall surrounds the entire peripheral surface of the pulp molding base and is attached near the upper edge of the peripheral surface but not near the lower edge of the peripheral surface, thereby forming an impermeable seal, the lower edge of the peripheral surface of the pulp molding base being below the liquid-containing surface, thereby allowing the compressible fiber-based bottle to stand upright; and A liquid personal care composition comprising about 14% to about 50% water; about 20% to about 70% a wetting agent; and having a water activity (Aw) of about 0.40 to about 0.90.

[0255] B. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraph A, wherein the base barrier structure has a weight reduction of less than 20 g / sqm / day at 25°C and 60% relative humidity.

[0256] C. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to B, wherein the fiber-based sidewall barrier structure has a weight reduction of less than 20 g / sqm / day at 25°C and 60% relative humidity.

[0257] D. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through C, wherein the base barrier structure includes a polymer liner.

[0258] E. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through D, wherein the base barrier structure is a water-based dispersion and contains microfibrillated cellulose (MFC) or cellulose nanocrystal (CNC) additives.

[0259] F. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through E, wherein the squeezable fiber-based bottle contains at least 85% fiber content.

[0260] G. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through F, wherein the fiber-based sidewall is a pulp molded part including a squeezable side panel.

[0261] H. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to G, wherein the orifice for dispensing the viscous fluid includes a separable slit valve.

[0262] I. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to H, wherein the separable slit valve is attached to a cap, wherein the cap is lightly attached to the bottom surface of the pulp molding base, and wherein the cap can be twisted to release the slit valve from the orifice.

[0263] J. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to I, wherein the lower edge of the fiber-based sidewall is attached near the upper edge of the peripheral surface of the pulp molding base around the entire peripheral surface and is separated from the lower edge of the peripheral surface by at least 1 mm.

[0264] K. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to J, wherein the pulp-molded sidewall is a single, integral sidewall.

[0265] L. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to K, wherein the upper edge of the integral sidewall includes a first upper edge and a second upper edge, wherein the first upper edge is attached to the second upper edge to form a seal.

[0266] M. A squeezable fiber-based bottle for use with liquid personal care compositions as described in paragraphs A through L, wherein the outer surface of the pulp-molded sidewall includes scoring lines to facilitate bidirectional folding for dispensing all viscous liquids.

[0267] N. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through M, wherein the fiber-based sidewall barrier structure includes a liner on the inner surface.

[0268] O. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to N, wherein the squeezable fiber-based bottle is capable of being crushed into a flat configuration to provide at least 95% product emptying.

[0269] P. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to O, wherein the squeezable fiber-based bottle maintains structural integrity and performance when used in a humid environment.

[0270] Q. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to P, wherein the fiber count comprises 50% to 60% bamboo, 40% to 50% bagasse, and 0% to 10% coniferous wood.

[0271] R. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through Q, wherein the fiber count comprises 50% to 60% bamboo, 35% to 50% bagasse, and up to 5% microfibrillated or nanofibrillated cellulose fibers.

[0272] S. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to R, wherein an inorganic barrier structure is applied by vapor deposition after pulp molding.

[0273] T. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through S, wherein the viscous fluid has a viscosity of 5,000 cps. -1 Up to 20,000 cps per second 10 -1 Viscosity in seconds.

[0274] U. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to T, wherein the liquid personal care composition contains about 35% to about 50% water.

[0275] V. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to U, wherein the wetting agent is about 23% to about 45%.

[0276] W. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through V, wherein the humectant is selected from the group consisting of: glycerin, amino acids, proline, aspartic acid, arginine, 1,3-butanediol, propylene glycol, and water, soft-haired pine algae extract, collagen amino acids or peptides, creatine, diglycerides, biosaccharide gum-1, glucosamine salts, glucuronides, glutamate, polyethylene glycol ethers of glycerin, glycerin, glyceryl monopropoxylate, glycogen, hexanediol, honey, hydrogenated starch hydrolysate, hydrolyzed mucopolysaccharides, inositol, keratin amino acids, glycosaminoglycans, methoxy PEG-10, methyl glucetol polyether-10 and methyl glucetol polyether-20, methyl glucose, 3-methyl-1,3-butanediol, N-acetyl glucosamine salt, polyethylene glycol, PEG4, PEG5 pentaerythritol, PEG6, PEG8, PEG 9. Pentaerythritol, 1,2-pentanediol, PPG-1 glyceryl ether, PPG-9,2-pyrrolidone-5-carboxylic acid and its salts, glyceryl PCA, glycoisoesters, sericin, sericin amino acids, sodium acetylated hyaluronic acid, sodium hyaluronate, sodium polyaspartate, sodium polyglutamate, sorbitol 20, sorbitol 6, sugars and sugar alcohols, glucose, sucrose, fructose, mannose, polyglycerol sorbitol, trehalose, triglycerides, trimethylolpropane, tri(hydroxymethyl)aminomethane salts, yeast extracts, ionic salts, sodium chloride, potassium chloride and mixtures thereof.

[0277] X. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through W, wherein the humectant is selected from the group consisting of glycerin, sodium chloride, and mixtures thereof.

[0278] Y. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to X, wherein the water activity (Aw) is about 0.80 to about 0.90.

[0279] Z. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through Y, wherein the water activity (Aw) is less than about 0.80.

[0280] AA. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through Z, wherein the liquid personal care composition contains a surfactant.

[0281] BB. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through AA, wherein the surfactant is present in amounts of about 10% to about 18%.

[0282] CC. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through BB, wherein the surfactant is selected from one or more anionic surfactants.

[0283] DD. A squeezable fiber-based bottle in combination with a liquid personal care composition as described in paragraphs A through CC, wherein the liquid personal care composition contains an amphoteric auxiliary surfactant.

[0284] EE. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to DD, wherein the amphoteric auxiliary surfactant is selected from the group consisting of: cocamidopropyl betaine, lauramide propyl betaine, and mixtures thereof.

[0285] FF. A squeezable fiber-based bottle in combination with a liquid personal care composition as described in paragraphs A through EE, wherein the liquid personal care composition contains a thickener.

[0286] GG. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through FF, wherein the liquid care composition comprises a thickener selected from the group consisting of: acrylic acid / acrylonitrile copolymer, acrylate / stearyl polyoxyethylene ether-20 itaconic acid copolymer, acrylate / cetyl polyoxyethylene ether-20 itaconic acid copolymer, acrylate / aminoacrylate / C10-30 alkyl PEG-20 itaconic acid copolymer, acrylate / aminoacrylate copolymer, acrylate / stearyl polyoxyethylene ether-20 methacrylate copolymer, etc. Acrylic ester / behenyl polyoxyethylene ether-25 methacrylate copolymer, acrylate / stearyl polyoxyethylene ether-20 methacrylate crosspolymer, acrylate / behenyl polyoxyethylene ether-25 methacrylate / HEMA crosspolymer, acrylate / vinyl neodecanoate crosspolymer, acrylate / vinyl isodecanoate crosspolymer, acrylate / palm oil alcohol polyether-25 acrylate copolymer, acrylic acid / acrylamidomethylpropane sulfonic acid copolymer, and acrylate / acrylic acid C10-C30 alkyl ester crosspolymer, and mixtures thereof.

[0287] HH. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through GG, wherein the thickener is selected from the group consisting of hydroxyethyl cellulose.

[0288] II. A squeezable fiber-based bottle in combination with a liquid personal care composition as described in paragraphs A through HH, wherein the liquid personal care composition contains sodium chloride.

[0289] JJ. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through II, wherein the liquid personal care composition contains scalp health active substances.

[0290] KK. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A through JJ, wherein the scalp health active substance is selected from the group consisting of: piroctone ethanolamine salt, zinc pyrithione, clomiphene, sulfur, and mixtures thereof.

[0291] LL. A squeezable fiber-based bottle in combination with a liquid personal care composition as described in paragraphs A to KK, wherein the personal care composition has a viscosity of about 5,000 cps to about 20,000 cps.

[0292] MM. A squeezable fiber-based bottle in combination with a liquid personal care composition as described in paragraphs A to LL, wherein the personal care composition has a viscosity of about 5,000 cps to about 20,000 cps.

[0293] NN. A squeezable fiber-based bottle for use with a liquid personal care composition as described in paragraphs A to MM, the bottle comprising a package in which the liquid personal care composition acquires water when packaged within the package, wherein the acquisition of water by the liquid personal care composition enables the realization of the physical or chemical properties of the final formulation of the liquid personal care composition.

[0294] The dimensions and values ​​disclosed herein should not be construed as strictly limited to the precise numerical values ​​cited. Rather, unless otherwise specified, each such dimension is intended to represent the stated value and the range surrounding its functional equivalent. For example, a dimension disclosed as “40 mm” is intended to represent “approximately 40 mm”.

[0295] Unless expressly excluded or otherwise limited, every reference cited herein, including any cross-references or related patents or patent applications, and any patent application or patent claiming priority to or benefiting from it, is incorporated herein by reference in its entirety. Reference to any reference is not an endorsement of it as prior art to any disclosed or protected art herein, nor is it an endorsement of any such invention, either on its own or in combination with any one or more references. Furthermore, where any meaning or definition of a term in this invention conflicts with any meaning or definition of the same term in referenced documents, the meaning or definition given to that term in this invention shall prevail.

[0296] While specific embodiments of the invention have been illustrated and described, it will be apparent to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. Therefore, it is intended that all such changes and modifications falling within the scope of the invention be covered by the appended claims.

Claims

1. A squeezable fiber-based bottle for use with a liquid personal care composition, said liquid personal care composition comprising: A pulp molding base includes a liquid-receiving surface having orifices for dispensing viscous liquid, the pulp molding base having a base periphery having a peripheral surface including an upper edge and a lower edge, and a base barrier structure disposed on the liquid-receiving surface and the upper edge of the base periphery; A fiber-based sidewall having an upper edge, a lower edge, an outer surface, and an inner surface, the inner surface including a fiber-based sidewall barrier structure, wherein the lower edge of the fiber-based sidewall surrounds the entire peripheral surface of the pulp molding base and is attached near the upper edge of the peripheral surface but not near the lower edge of the peripheral surface, thereby forming an impermeable seal, the lower edge of the peripheral surface of the pulp molding base being below the liquid-containing surface, thereby allowing the squeezable fiber-based bottle to stand upright; and a liquid personal care composition comprising 14% to 50% water, preferably 35% to 50% water; 20% to 70% a wetting agent, preferably 23% to 45% a humectant. The humectant, preferably, is selected from the group consisting of: glycerol, amino acids, proline, aspartic acid, arginine, 1,3-butanediol, propylene glycol, and water, *Pinus massoniana* extract, collagen amino acids or peptides, creatine, diglycerides, biosaccharide gum-1, glucosamine salts, glucuronides, glutamate, polyethylene glycol ethers of glycerol, glycerol, glycerol monopropoxylate, glycogen, hexanediol, honey, hydrogenated starch hydrolysate, hydrolyzed mucopolysaccharides, inositol, keratin amino acids, glycosaminoglycans, methoxy PEG-10, methyl glucetol polyether-10 and methyl glucetol polyether-20, methyl glucose, 3-methyl-1,3-butanediol, N-acetyl glucosamine salt, polyethylene glycol, PEG 4. PEG 5 pentaerythritol, PEG 6, PEG 8, PEG 9, pentaerythritol, 1,2-pentanediol, PPG-1 glyceryl ether, PPG-9,2-pyrrolidone-5-carboxylic acid and its salts, glyceryl PCA, glycoisoesters, sericin, serine, sodium acetylated hyaluronic acid, sodium hyaluronate, sodium polyaspartate, sodium polyglutamate, sorbitol 20, sorbitol 6, sugars and sugar alcohols, glucose, sucrose, fructose, mannose, polyglycerol sorbitol, trehalose, triglycerides, trimethylolpropane, tri(hydroxymethyl)aminomethane salt, yeast extract, ionic salts, sodium chloride, potassium chloride, and mixtures thereof, preferably wherein the wetting agent is selected from the group consisting of glycerol, sodium chloride, and mixtures thereof; wherein a water activity (Aw) of 0.40 to 0.90 is present, preferably wherein the water activity (Aw) is 0.80 to 0.

90.

2. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the base barrier structure has a weight reduction of less than 20 g / sqm / day at 25°C and 60% relative humidity.

3. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the fiber-based sidewall barrier structure has a weight reduction of less than 20 g / sqm / day at 25°C and 60% relative humidity.

4. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the base barrier structure comprises a polymer liner.

5. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the base barrier structure is a water-based dispersion and contains microfibrillated cellulose (MFC) or cellulose nanocrystal (CNC) additives.

6. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the extrudable fiber-based bottle contains at least 85% fiber content.

7. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the fiber-based sidewall is a pulp molded part including an extrudable side panel.

8. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the orifice for dispensing the viscous fluid includes a separable slit valve, preferably wherein the separable slit valve is attached to a cap, wherein the cap is lightly attached to the bottom surface of the pulp molding base, wherein the cap can be twisted to release the slit valve from the orifice.

9. The extrudable fiber-based bottle according to any of the preceding claims, wherein the lower edge of the fiber-based sidewall is attached near the upper edge of the peripheral surface surrounding the entire peripheral surface of the pulp molding base and is separated from the lower edge of the peripheral surface by at least 1 mm.

10. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the pulp molded sidewall is a complete one-piece sidewall, preferably wherein the upper edge of the one-piece sidewall includes a first upper edge and a second upper edge, wherein the first upper edge is attached to the second upper edge to form a seal.

11. The extrudable fiber-based bottle according to any of the preceding claims, wherein the outer surface of the pulp molded sidewall includes score lines to facilitate bidirectional folding for dispensing all viscous liquids.

12. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the fiber-based sidewall barrier structure includes a liner on the inner surface.

13. The compressible fiber-based bottle according to any one of the preceding claims, wherein the compressible fiber-based bottle is capable of being crushed into a flat configuration, thereby providing at least 95% product evacuation.

14. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the extrudable fiber-based bottle maintains structural integrity and performance when used in a humid environment.

15. The compressible fiber-based bottle according to any one of the preceding claims, wherein the fiber count comprises 50% to 60% bamboo, 40% to 50% bagasse, and 0% to 10% coniferous wood.

16. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the fiber count comprises 50% to 60% bamboo, 35% to 50% bagasse, and up to 5% microfibrillated or nanofibrillated cellulose fibers.

17. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the inorganic barrier structure is applied by vapor deposition after pulp molding.

18. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the viscous fluid has a viscosity of 5,000 cps. -1 Up to 20,000 cps per second 10 -1 Viscosity in seconds.

19. The extrudable fiber-based bottle of claim 1, wherein the water activity (Aw) is less than 0.

80.

20. The squeezable fiber-based bottle according to any one of the preceding claims, wherein the liquid personal care composition comprises a surfactant, preferably wherein the surfactant is 10% to 18%, preferably wherein the surfactant is selected from one or more anionic surfactants.

21. The squeezable fiber-based bottle according to any one of the preceding claims, wherein the liquid personal care composition comprises an amphoteric auxiliary surfactant, preferably wherein the amphoteric auxiliary surfactant is selected from the group consisting of: cocamidopropyl betaine, lauramidopropyl betaine, and mixtures thereof.

22. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the liquid personal care composition comprises a thickener, preferably wherein the thickener is selected from the group consisting of: acrylic acid / acrylonitrile copolymer, acrylate / stearyl polyoxyethylene ether-20 itaconic acid copolymer, acrylate / cetyl polyoxyethylene ether-20 itaconic acid copolymer, acrylate / aminoacrylate / C10-30 alkyl PEG-20 itaconic acid copolymer, acrylate / aminoacrylate copolymer, acrylate / stearyl polyoxyethylene ether-20 methacrylate copolymer, acrylate / behenyl polyoxyethylene ether-20 methacrylate copolymer, etc. The thickener comprises ethylene ether-25 methacrylate copolymer, acrylate / stearyl polyoxyethylene ether-20 methacrylate crosspolymer, acrylate / behenyl polyoxyethylene ether-25 methacrylate / HEMA crosspolymer, acrylate / vinyl neodecanoate crosspolymer, acrylate / vinyl isodecanoate crosspolymer, acrylate / palm oil alcohol polyether-25 acrylate copolymer, acrylic acid / acrylamidomethylpropane sulfonic acid copolymer, and acrylate / acrylic acid C10-C30 alkyl ester crosspolymer, and mixtures thereof, wherein the thickener is preferably selected from the group consisting of hydroxyethyl cellulose.

23. The squeezable fiber-based bottle according to any one of the preceding claims, wherein the liquid personal care composition comprises sodium chloride.

24. The squeezable fiber-based bottle according to any one of the preceding claims, wherein the liquid personal care composition comprises a scalp health active substance, preferably wherein the scalp health active substance is selected from the group consisting of: piroctone ethanolamine salt, zinc pyrithione, clomiphene, sulfur, and mixtures thereof.

25. The extrudable fiber-based bottle according to any one of the preceding claims, wherein the personal care composition has a viscosity of 5,000 cps to 20,000 cps.

26. A squeezable fiber-based bottle for use with a liquid personal care composition according to any one of the preceding claims, the bottle comprising a package, wherein the liquid personal care composition acquires water when packaged within the package, wherein the acquisition of water in the liquid personal care composition enables the realization of the physical or chemical properties of the final formulation of the liquid personal care composition.