Biodegradable container with personal care composition

Abstract

The present invention relates to a biodegradable container for use with a liquid personal care composition, the biodegradable container comprising: a biodegradable vessel having at least one opening and a biodegradable cap for the opening, wherein the container contains a liquid personal care composition comprising 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.

Description

Technical Field

[0001] This invention relates to a biodegradable container comprising a biodegradable vessel having at least one opening, a biodegradable cap for the opening, and a biodegradable coating having a liquid personal care composition having low water activity and low water content. The invention also relates to a method for manufacturing the container. 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 plastics 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 recyclable after use, thus leaking into the environment and potentially persisting there. Furthermore, small plastic containers (such as those used for testing or sample sizes) may be difficult to recycle due to their small size and relatively low inherent recycling value. Therefore, these containers may end up in undesirable pathways, such as incineration or landfill. 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. Fiber-based packaging also typically boasts very high recyclability. Cellulose products are often formed into films or multilayer boards using papermaking processes, or into 3D molded objects using pulp molding methods. While fibers offer excellent structural support and a pleasant decorative surface, their poor oxygen and moisture barrier properties, along with their limited liquid containment characteristics, lead to integrity failure, making individual sheets or molded 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 polymers (such as PE) that have heat-sealing properties in a structure that may include one or more barrier layers (such as EVOH, vacuum metallized alumina, etc.), or they 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 trade-offs between barrier performance, recyclability, and packaging biodegradability. In this invention, pulp vessels can be manufactured using rigid pulp molding. To achieve the desired liquid containment, moisture, and oxygen barrier properties, such vessels can be coated with a thin plastic liner or by spraying. As with paper sheets, including such liner, coating, and additives presents trade-offs between barrier performance, recyclability, and packaging biodegradability. Furthermore, including high-fiber components in functional accessories (such as necks and closures) presents challenges due to the high molding tolerance requirements from multiple open / close cycles and the reliability of coating integrity.

[0005] In this invention, packaging made from liquid cardboard and rigid pulp molding may include one or more biodegradable and / or bio-inert coatings. However, placing conventional liquid personal care formulations within such biodegradable packaging is not straightforward, as it has been historically observed that liquid products with high water content and high water activity will prematurely damage less durable biodegradable packaging to the point that a useful shelf life cannot be achieved through existing distribution and supply chains in various markets, even when the biodegradable packaging comprises multiple layers including barrier layers. Typically, when a typical commercially available liquid personal care composition (with high water content and high water activity) is placed within biodegradable packaging, the following events may occur: a) early hydrolysis of the biodegradable sealant polymer (i.e., in direct contact with the liquid product) or biodegradable primer layer leads to a significant decrease in polymer molecular weight, resulting in a weaker and more porous barrier layer; b) the weakened sealant or primer then allows moisture and water to migrate through it at a higher rate into other layers of the packaging, which may further persist within the biodegradable packaging structure. In particular, when this occurs, any metallized barrier layers present typically undergo significant corrosion and damage. This corrosion and damage can lead to even greater loss of moisture and water within the packaging; and / or c) high water content in the formulation results in a high driving force for moisture to leave the packaging to balance with the external atmosphere, leading to high total weight loss, re-drying of the internal product, and a significant increase in product viscosity, ultimately rendering the product unusable. If any or all of the above occurs, this will result in a shortened product shelf life, which may be insufficient for typical distribution systems through which consumer products move, and this can subsequently lead to a poorer product performance experience for the consumer.

[0006] Especially for liquid shampoos, while one solution could be to switch to dry shampoo, we have found that getting most consumers to immediately switch to dry shampoo can be challenging due to the change in habits (many consumers may never switch), and these solutions often require new and expensive capital investment to manufacture the product.

[0007] In order to make any further progress in manufacturing biodegradable packaging that can hold liquid personal care compositions, the present invention has found a need to understand whether such personal care formulations can actually be sufficiently modified to cause less damage to a particular type of biodegradable packaging while the product still delivers its function.

[0008] This invention relates to a combination of personal care compositions (having lower water activity and lower water content compared to currently marketed personal care compositions) with specific types of biodegradable packaging. This biodegradable packaging has sufficient moisture permeability (MVTR) barrier properties to minimize weight loss, while also passing specific types of biodegradation tests to ensure that it will not be persistent if released into the environment after use and disposal. Generally, the invention aims to match the water activity of the product to the average humidity of the product's sales environment to minimize weight loss or weight gain. In some cases, work has been done to further reduce the water activity of the product so that it can be placed within biodegradable packaging with even poorer MVTR barrier properties, where weight gain is manageable but weight loss is generally not observed. This solution enables the sale of personal care compositions (and potentially other liquid products) that still delight consumers within biodegradable packaging derived from cellulose fibers. This biodegradable packaging is less durable than today’s alternatives and still achieves a reasonable product shelf life (6 months to 2 years) to keep the product fit for consumer use, even after passing through the typical distribution system of a typical consumer goods company (from factory to distribution center to store to consumer). Summary of the Invention

[0009] The present invention relates to a biodegradable container for use with a liquid personal care composition, the biodegradable container comprising: a biodegradable vessel having at least one opening and a biodegradable cap for the opening, wherein the container contains a liquid personal care composition comprising 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. Attached Figure Description

[0010] 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 a biodegradable container according to this disclosure.

[0011] Figure 1b This is a perspective view of a biodegradable container comprising a biodegradable vessel having a fibrous body, having at least one opening and having at least one biodegradable barrier layer and a flange, the biodegradable container being filled with a disclosed personal care composition and covered by a biodegradable cap.

[0012] Figure 2 It is a perspective view of a biodegradable vessel having at least one opening and fibrous material.

[0013] Figure 3 yes Figure 1b A sectional view.

[0014] Figure 4 This is a cross-sectional view of a biodegradable container molded from pulp, which includes a biodegradable vessel having liquid-containing barrier layers on both the inner and outer surfaces and being covered by a biodegradable cap.

[0015] Figure 5 This is a cross-sectional view of a pulp-molded biodegradable container, which includes a biodegradable vessel having a liquid-containing barrier layer around all surfaces and being covered by a biodegradable cap.

[0016] Figure 6 It is a cross-sectional view of a biodegradable container including a biodegradable liquid packaging plate and a biodegradable cap.

[0017] Figure 7 This is a cross-sectional view of a pulp-molded biodegradable container, which includes a biodegradable vessel and a pulp-molded cap, having a liquid-containing barrier layer on its inner surface.

[0018] Figure 8 This is a cross-sectional view of a squeezable, biodegradable pulp molded bottle with a liquid-containing barrier layer on its inner surface.

[0019] Figure 9 This is a cross-sectional view of a squeezable, biodegradable pulp molded bottle with a liquid-containing barrier layer covering all surfaces.

[0020] Figure 10 This is a cross-sectional view of a squeezable, biodegradable pulp molded bottle following atomic layer deposition (ALD) of the metallization layer. Detailed Implementation

[0021] 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.

[0022] The compositions of the present invention may comprise, consist of, or be composed of the basic components described herein, as well as optional ingredients. As used herein, “consistently 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 characteristics of the composition or method protected by the claims.

[0023] 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.

[0024] "Dermatologically acceptable" means that the composition or component is suitable for contact with human skin tissue without undue toxicity, incompatibility, instability, allergic response, etc.

[0025] "Safe and effective amount" refers to an amount of compound or composition that is sufficient to significantly induce positive and beneficial effects.

[0026] 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.

[0027] 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.

[0028] As used in this article, the term "fluid" includes both liquids and gels.

[0029] As used herein, when used in claims, the articles including “a” and “an” should be understood to refer to one or more substances protected or described in the claims.

[0030] 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 composed of”.

[0031] As used herein, “mixture” is intended to include simple combinations of substances and any compounds that may be produced by such combinations.

[0032] 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”).

[0033] 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.

[0034] 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.

[0035] 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.

[0036] As used herein, "personal care composition" includes liquid compositions such as shampoos, body gels, liquid hand cleansers, hair colorants, facial cleansers, and other surfactant-based liquid compositions.

[0037] 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.

[0038] Unless otherwise specified, 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 included in commercially available substances.

[0039] 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.

[0040] 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.

[0041] As used herein, “biopolymer” or “bioplastic” is intended to include polymers derived from biological materials (typically plant materials).

[0042] As used herein, "biodegradable" is intended to include materials that are readily assimilated by microorganisms (such as molds, fungi, and bacteria) when buried underground or otherwise exposed to microorganisms (including exposure under conditions favorable to microbial growth), as well as materials that are "easily biodegradable," "home compostable," or "industrial compostable." When something is biodegradable, it means that the entire structure plus all major components pass one or more of the biodegradability tests listed below. A component is considered a major component if it comprises >10% by weight of the entire structure. If a polymer is deemed biodegradable after testing, it is considered to have lower durability than non-biodegradable polymers in the environment associated with the tests conducted.

[0043] As used herein, “bioinert” refers to an inorganic or inorganic-organic hybrid material that does not interact with any biological material, does not respond to any biological material, does not promote any chemical reaction or biological activity or other response of any biological material, or deteriorates it.

[0044] As used herein, “easily biodegradable” or “intrinsically biodegradable” means a material that meets the readily biodegradable or inherently biodegradable qualification level according to the OECD Chemicals Testing Guide, Method 301 B: CO2 Emissions (Modified Sturm Test) (adopted 17 July 1992).

[0045] As used in this article, “home compostable” refers to materials that meet the pass level of TÜV AUSTRIA (2012) OK compostable HOME OK-02e certification.

[0046] As used herein, “industrially compostable” refers to materials that meet the pass level of TÜV AUSTRIA (2000) OK industrial compostability certification (EN 13432: 2000).

[0047] As used herein, the term "copolymer" is intended to include polymers derived from two or more polymerizable monomers. When used in a general sense, the term "copolymer" also includes more than two different monomers, such as terpolymers. The term "copolymer" also includes random copolymers, block copolymers, and graft copolymers.

[0048] As used in this article, "lateral direction" or "CD" is intended to include the width of the membrane, which is typically perpendicular to the MD direction.

[0049] As used herein, “membrane” is intended to include sheet-like materials in which the length and width of the material far exceed its thickness. As used herein, the terms “membrane” and “sheet” are used interchangeably.

[0050] As used in this article, "longitudinal direction" or MD is intended to include the length of the membrane during its production.

[0051] As used herein, “renewable” is intended to include materials that can be produced from or derived from natural sources that are periodically (e.g., annually or annually) replenished by the action of plants (e.g., crops, edible and inedible grasses, forestry products, seaweed or algae) or microorganisms (e.g., bacteria, fungi or yeast) in 15 terrestrial, aquatic or marine ecosystems.

[0052] As used herein, “recyclable” means paper in use, including in-plant and post-consumer waste paper and paperboard, which can be processed into new paper or paperboard using methods defined in the voluntary standards for repulping and recycling corrugated fiberboard in the presence of water and water vapor to improve its performance (August 16, 2013).

[0053] As used herein, “water solubility” means the ability of a sample material of at least about 25 grams, at least about 50 grams, at least about 100 grams, or at least about 200 grams to dissolve or disperse completely in water without leaving visible solids or forming a distinct separated phase when treated at 20°C in one liter (1 L) of deionized water and thoroughly stirred at atmospheric pressure.

[0054] Conventional biodegradable containers are not formed solely from biodegradable components, or they possess relatively low mechanical stability. Therefore, the object of this invention is to provide a container formed solely from biodegradable components that, when used in conjunction with liquid personal care compositions having low water activity and low water content, exhibits high airtightness and high mechanical stability.

[0055] Figure 1bAn exemplary biodegradable container 20 with a biodegradable vessel 1 and a biodegradable cap 4 is shown. In this invention, the biodegradable cap 4 may be a biodegradable sealing film. The sealing film is flexible and optimized to provide necessary barrier properties such as MTVR, OTR, and liquid containment, as well as biodegradability. The film seals to the container flange 5, thereby isolating the interior of the container from the environment. The sealing force is optimized to be high enough to prevent liquid contents from leaking through the seal, while being low enough to ensure that a user can easily peel off the cap to access the product. In this invention, the peel force can be between 500 gf and 1000 gf, or between 700 gf and 800 gf, in a 180° peel test.

[0056] The sealing film may have a biodegradable polymer layer 6 (commonly referred to as a sealant or sealant layer or heat sealant layer) in contact with the product, which is made of a water-insoluble biodegradable polymer. In some structures, such a biodegradable polymer layer may also be suitable as a laminate between other layers, such as a paper layer and a sealant layer. The water-soluble biodegradable polymer may be a thermoplastic polymer. As used herein, a thermoplastic polymer is a polymer that melts and crystallizes or hardens upon cooling, but can be remelted upon further heating. Suitable thermoplastic polymers used herein typically have melt temperatures of 60°C to 300°C, 80°C to 250°C, or 100°C to 215°C. The molecular weight of the thermoplastic polymer is high enough to achieve entanglement between polymer molecules, but low enough, if desired, to be melt-extrudeable. Suitable thermoplastic polymers may have a weight-average molecular weight of 1000 kDa or less, 5 kDa to 800 kDa, 10 kDa to 700 kDa, or 20 kDa to 400 kDa.

[0057] Biodegradable water-insoluble polymers may include biodegradable thermoplastic materials selected from the group consisting of aliphatic and / or aromatic polyesters. Such biodegradable aromatic and / or aliphatic polyesters may be bio-produced (e.g., via large-scale bacterial fermentation) or chemically synthesized. Suitable biodegradable aliphatic and / or aromatic polyesters may be copolymers of: i) at least one aliphatic dicarboxylic acid; and / or ii) at least one aromatic dicarboxylic acid; and iii) dihydroxy compounds (diols). Examples of biodegradable aromatic and / or aliphatic polyesters include, but are not limited to: various copolyesters of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), wherein an aliphatic diacid or diol is incorporated into the polymer backbone to make such copolyesters biodegradable or compostable; and various aliphatic polyesters and copolyesters derived from diacids such as succinic acid, glutaric acid, adipic acid, sebacic acid, azelaic acid, or their derivatives (e.g., alkyl esters, acyl chlorides, or their anhydrides) and diols such as ethylene glycol, propylene glycol, 1,4-butanediol, 1,6-hexanediol, 1,4-cyclohexanediol, etc. For example, biodegradable aromatic and / or aliphatic polyesters may be selected from the group consisting of: polybutylene terephthalate (PBAT), polybutylene succinate (PBS), polybutylene adipate (PBSA), polylactic acid (PLA), polycaprolactone (PCL), polyglycolic acid (PGA), polypropylene carbonate (PPC), and any combination / mixture thereof. The aliphatic and / or aromatic polyesters used may be derived from a family of polymers called polyhydroxyalkanoates, also known as “PHAs,” which can be synthesized in fermentation plants by plants or bacteria fed with a specific substrate, such as glucose. The resulting PHAs can be made from a wide variety of copolymers. A particularly interesting group of PHA resins are homopolymers and / or copolymers containing repeating structural units of 3-hydroxybutyrate (hereinafter referred to as “P3HB”), either alone or in combination with one or more other repeating structural units. Aliphatic and / or aromatic polyesters may also include polycaprolactone. Biodegradable water-soluble polymers may include biodegradable thermoplastic materials selected from thermoplastic starches (e.g., MATER-BI from Novamont or PLANIC from Plantic / Kuraray). ® Starch can be denatured during processing to produce thermoplastic starch compositions. Thermoplastic starch compositions may also contain plasticizers. Biodegradable polymers can consist of heterogeneous blends of a variety of different biodegradable polymers—because this allows manufacturers to achieve an optimal balance of properties, such as balancing biodegradation rates and resistance to formulations contained within sealants formed from biodegradable polymers. One example may include PBAT (e.g., under the trade name ECOFLEX). ®The BASF version sold) and PLA (e.g., from Nature Works LLC, which is sold by BASF under the trade name Ecovio) ® PBAT is a blend of polymers (for sale). PBAT is typically blended with PLA to provide greater chemical resistance, hydrolysis resistance, or improved processability, while still balancing the rate of biodegradation and the temperature required to initiate biodegradation. Another example of a heterogeneous blend is PBAT blended with starch, manufactured by Novamont, which sells various grades of PBAT under the trade name Materbi. The biodegradable polymer layers of the present invention may also contain one or more additives or fillers, including but not limited to inorganic fillers, alkyd resins, nanoparticles, or renewable fillers such as cellulose (e.g., cotton, wood, hemp, cardboard), lignin, bamboo, straw, grass, kenaf, cellulose fibers, chitin, chitosan, flax, keratin, algae fillers, natural rubber, nanocrystalline starch, nanocrystalline cellulose, collagen, whey, gluten, and combinations thereof. The biodegradable polymer layer may also contain one or more other components, such as crystal nucleating agents, lubricants, plasticizers, antistatic agents, flame retardants, conductive additives, thermal insulation, crosslinking agents, antioxidants, ultraviolet absorbers, colorants, inorganic fillers, organic fillers, hydrolysis inhibitors, lubricants / release agents, expanders, antiblocking agents, anti-sticking agents, and surfactants.

[0058] Sealing films may comprise cast cellulose layers produced using a special film solution casting process. One reason for using such films is when a very strong moisture barrier layer is required, but it is difficult to apply this barrier layer directly to the heat-sealing layer inside the packaging, or directly to a paper layer that may be present on the outside of the packaging. Instead, in such cases, various biodegradable barrier-coated cellulose films are available from Futamura under its trademark Natureflex. ™ They are purchased and placed as an intermediate layer between the heat-sealing layer and any outer layer such as paper. A non-limiting example of such films is their Natureflex. ™ NM membrane is a metallized cellulose membrane with a WVTR barrier of approximately 10 g / m2.day at 38°C / 90%RH.

[0059] The capping membrane may include an inorganic barrier layer to facilitate a reduction in moisture vapor transmission rate (MVTR) throughout the structure. In many cases, the inorganic barrier layer will be vapor-deposited onto the surface of one of the biodegradable polymer layers present in the structure. In other cases, the inorganic barrier layer may be deposited on a paper layer. A metallization layer may be transferred from another metallized substrate to a paper substrate. Suitable vapor-deposited inorganic coatings may be formed from 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, as well as metal oxides (e.g., Al₂O₃ or SiO�x), metal nitrides, and related compounds. The metallization layer may be transferred from another metallized substrate to a paper substrate. The thickness of the inorganic barrier coating may be 2 nm–1,000 nm, 10 nm–200 nm, or 20 nm–100 nm. The thickness ratio of the inorganic barrier layer to the polymer layer may be from about 20 to about 20,000.

[0060] The inorganic barrier layer may comprise a nanoclay layer laid down from an aqueous nanocomposite dispersion. In this invention, the inorganic layer laid down from an aqueous coating may be a lithium montmorillonite clay layer. Further disclosures regarding lithium montmorillonite can be found in U.S. Patent Application Publication No. 2023 / 0234096 and U.S. Patent Application Publication No. 2023 / 0235510, which are incorporated herein by reference. The inorganic layer may also be a Cloisite clay layer as disclosed in U.S. Patent Application Publication No. 20220112664.

[0061] The capping film may include a biodegradable paper layer that can also be recycled in a typical paper recycling stream. The paper primarily comprises cellulose fibers and a certain amount of polymeric binders, mineral sizing agents, brighteners, surfactants, and other additives. The paper may also include recycled fibers (natural or synthetic). Non-limiting examples of paper suitable for forming biodegradable and recyclable paper layers as part of this invention include Leine Nature from Sappi. ® Paper (basic weight = 85g / m2), this paper is a glossy paper certified as "OK Home Compost"; special kraft paper from UPM with the trademark Lucent; NiklaSelect V natural fabric paper (99g / m2) from Brigli and Bergmeister, sized only on one side; PackPro 7.0 paper (80g / m2) from Brigli and Bergmeister, sized on both sides; from BillerudKorsnäs ™The paper includes Axello paper (including tough white paper from Axello, 80 g / m²), which is designed to be tougher than many other papers and therefore has some advantages in the distribution chain; and SCG Glassine paper from SCG / Prepack (58 g / m²). As shown in the table below, these papers have passed the paper recycling programs of Western Michigan University and the PTS Institute in Germany. These papers have also passed the OECD 301B biodegradability screening test, undergoing at least 60% biodegradation within 60 days.

[0062] NA - Unavailable Cellulose fibers used in papermaking can be derived from tree fibers (including cork and hardwood) as well as non-tree fibers, which typically have shorter fibers and include, but are not limited to, bamboo, grass, hemp, kenaf, flax, corn husks, cotton stalks, coffee grounds, bagasse, rice straw, wheat straw, algae, abaca, tamarisk, fine-stemmed needlegrass, milkweed fiber, pineapple leaf fiber, wood fiber, pulp fiber, etc. Some papers can be blended with a range of different fibers from various sources.

[0063] Indirect transfer of metallization onto paper

[0064] In this invention, the metallization layer may not be directly applied to the primer layer, but can be transferred from another metallized substrate to a paper structure. This is sometimes referred to as a "transfer metallization process." This is a method frequently used in the decorative industry, but there are also applications where this technique is used to form barrier layers. In this transfer metallization process, a vacuum metallization layer is first deposited onto an intermediate substrate, such as a biaxially oriented PET film, a biaxially oriented PP film, or a cellulose film, to form an intermediate structure, and then the metallization layer is transferred to the paper-based structure. Potential suppliers of these intermediate structures may include Dongguan Ruize Creative Arts New Materials Co., Ltd., Shanghai Zijiang New Material Technology Co., Ltd., or others.

[0065] The following describes how these intermediate structures are formed, as they typically contain multiple layers. Prior to vacuum metallization, the intermediate substrate is coated with a release layer that will provide good adhesion to the metallization layer subsequently deposited on top, but relatively poor adhesion to the underlying intermediate substrate. In some cases, this release layer may be formed from a polydimethylsiloxane (PDMS)-based material, but other chemicals may also be used. Vacuum metallization can be performed using the aforementioned suitable processes to deposit a suitable barrier layer. In some cases, but not always, a final primer layer is deposited on top of the metallization layer to protect it until the intermediate structure is used for a transfer process at a later time or date. Such primer coatings may also be applied later to treat the release layer with suitable surface energy / tension, making it easier to apply other coatings or laminates on top.

[0066] In the transfer process, the vacuum-metallized intermediate structure is first laminated with the paper substrate to which the vacuum-metallized layer will be transferred. This transfer process is performed using various suitable adhesives, with the selected adhesive first applied to the paper substrate. Then, in the lamination process, lamination equipment is used to bring the intermediate structure into contact with the adhesive-coated paper substrate to form a laminated structure. This adhesive forms a stronger adhesion between the metallized layer and the paper substrate than between the release layer and the intermediate substrate in the intermediate structure. The final part of the lamination process causes the laminated structure to split into two new structures at the weakest interface (now the interface between the release layer and the intermediate substrate). The two new structures are a final structure (which will be retained for further processing into packaging) and a disposable structure (which is disposed of, recycled, or reused several times later after thorough cleaning). Thus, as the laminated structure separates at its weakest interface, the vacuum-metallized layer, along with the release layer from the intermediate structure, is peeled off from the original intermediate structure and transferred to the paper substrate, forming the final structure. This final structure then consists of the paper substrate, the adhesive layer, the vacuum-metallized layer, and the release layer.

[0067] Subsequently, the final structure typically undergoes another lamination process to adhere the extruded biodegradable sealant layer to the release layer side. In some cases, an alternative to laminating the extruded biodegradable sealant layer is to directly apply the biodegradable sealant (in the form of fine polymer particles) to the final structure via methods such as emulsion coating or dry coating. At the start of this lamination process, an anchoring coating (sometimes based on polyurethane materials, but alternatively other materials) is typically applied to the top surface of the release layer to alter its surface energy before the biodegradable sealant layer attaches, ensuring good adhesion between the release layer and the biodegradable sealant layer. An example of such a polyurethane material could be the high-functionality polyurethane dispersion “TAKELAC” from Mitsui Chemicals. ™The "WPB" series of products, such as the TAKELAC WPB-341 class.

[0068] The capping film may include a biodegradable adhesive to adhere multiple layers together to form a laminate. Non-limiting examples of biodegradable adhesive layers may include biodegradable polyvinyl acetate, starch, maltodextrin, natural waxes, artificial waxes, and polyester-polyurethane blends. In this invention, the biodegradable adhesive layer may be a commercially available grade from BASF, such as Epotal 3675 or Epotal 3702 or Epotal P100ECO (which is a water-based polyester-polyurethane compostable adhesive) or Epotal 3702 (also a water-based adhesive), all of which are biodegradable and compostable. In this invention, the adhesive may be Berkshire Labels' BioTAK. ® Or Bostik 43298 Thermogrip hot melt adhesive. In this invention, the biodegradable adhesive may be water-soluble to enhance recyclability in typical paper repulping systems. Non-limiting examples of such adhesives include biodegradable and soluble grades of PVOH and polyethylene oxide.

[0069] Figure 2 An exemplary biodegradable container 20 is shown, which includes a biodegradable vessel 1 having at least one opening 3.

[0070] In this invention, the biodegradable vessel 1 can be a water-soluble biodegradable thermoplastic polymer, selected from the group consisting of aliphatic and / or aromatic polyesters or thermoplastic starches already mentioned. The biodegradable vessel 1 can be manufactured using injection molding or compression molding processes.

[0071] In this invention, the biodegradable vessel 1 may include a fibrous body 2 and at least one biodegradable barrier layer 7 (not shown).

[0072] Fiber body 2 can be made from aqueous pulp containing cellulose fibers. The method begins with the preparation of a pulp comprising fibers and additives dispersed 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, which is incorporated herein by reference, 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 is about 1%. In wet forming processes, the pulp is deposited onto a screened mold to form a layer by spraying or, more commonly, by immersing the mold and subsequently applying a vacuum behind the screen mold. In the second step, the pulp layer can be pressed onto a tool comprising two mating tooling components, one of which may have a porous wall that contacts the pulp layer and through which a vacuum can be drawn to reduce the water content. After this pressing step, the molded article is dried in a heated mold or oven. After the heated mold or oven, the water content can still be approximately 10%-20%. The article can then be subjected to subsequent pressing operations, applying heat to reduce surface roughness and porosity, and the water content can be further reduced to below 10%, below 5%, and below 1%. The average wall thickness of the wet-molded part using this method can vary between 0.6 mm and 1.2 mm, and can be approximately 0.8 mm to 1.0 mm. After the pulp molding process, protruding edges can be trimmed as needed.

[0073] Cellulose fibers can be wood or non-wood. Wood fibers can be softwood “long” fibers, such as pine, spruce, fir, and hemlock, or hardwood “short” fibers, such as birch, eucalyptus, aspen, acacia, and oak. Non-wood plant fibers can generally be categorized into softwood substitutes, such as cotton staple fibers and linters; flax, hemp, 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 breaking strength, and surface finish (roughness and porosity). Depending on the desired properties of the final product, fibers can include both short and long fibers. Fibers can be extracted using bleached or unbleached chemical or mechanical processes. Fibers may include recycled fibers.

[0074] The slurry may include additives for process control 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; (2) sizing agents, such as alkyl ketone dimers (AKD), alkenyl succinic anhydride (ASA), rosin, or lignin; (3) additives for dry strength enhancement, such as starch, amphoteric, cationic, or anionic polyacrylamide resins, enzymes, or modified polyamines; (4) additives for wet strength enhancement, such as polyamide amine (PAE) or polyamine epichlorohydrin, epoxide or cationic glyoxylate resins, or (5) microfibrillated cellulose (MFC) or cellulose nanocrystal (CNC) additives. In the case of applying a barrier layer by spraying or dip coating, the slurry may include a certain amount of inorganic mineral filler to seal pores in the surface. In this invention, the inorganic mineral filler particles may be selected from calcium carbonate and flaky kaolin or any mixture thereof.

[0075] In this invention, based on dry fiber count, the slurry may include 0.5% to 2%, and may have 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 glyoxylated polyacrylamide (GPAM) to provide wet strength to the final product. In this invention, based on dry fiber count, the slurry may include between 2% and 5%, and may be between 3% and 4%, MFC to improve surface smoothness, stiffness, burst resistance, and wet strength for barrier applications. Non-limiting 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.

[0076] In this invention, the fibrous body 2 can be functionalized after molding by vapor deposition of an inorganic barrier layer. As used herein, functionalization is intended to include 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 layer can be optically opaque, translucent, or transparent, depending on the specific chemical properties applied. Typically, metal barrier layers such as aluminum will produce opaque barrier layers, while metal oxide barrier layers such as alumina or silicon dioxide will produce transparent barrier layers. 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 layer 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–1,000 nm, a thickness of 10 nm–200 nm, and a thickness of 20 nm–100 nm. It has been found that this functionalization can significantly increase wet strength, improve bulk moisture barrier properties, and increase contact angle, while maintaining recyclability and bioinertness. This effect is further enhanced when these deposition processes are used in high-density pulp matrices, especially in conjunction with high-refined pulps, MFC, or CNC.In this invention, the fibrous body 2 can be functionalized by parchment paper treatment after molding to produce a natural hydrophobic surface with high wet strength.

[0077] In this invention, the fibrous body 2 can be molded using a wet pulp molding process with rapid dehydration 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 method produces parts with a higher degree of strength and hydrophobicity compared to parts formed by conventional wet molding. This is believed to be due to the rapid dehydration enabling the cellulose fibers to quickly re-bond each other, and the high-pressure / high-temperature process enhancing lignin polymerization.

[0078] In this invention, the fibrous body 2 can be formed using a dry molding method. According to this process, air is used as the transport medium (“airflow web”) to transport the cellulose fibers and form them into a preform. The preform is then subsequently 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 sizing agents) can be sprayed into the cellulose fibers and / or the cellulose preform via solid-phase spraying or added. Pulpac discloses examples of such processes 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 produced using this method are found to be robust yet very flexible. This is assumed to be due to the low degree of interfiber hydrogen bonding. In this invention, the pulp molding base can be achieved using dry compression molding with an all-metal isostatic mold, as demonstrated by SACMI, to allow for a wide variety of shapes, including the ability to mold parts with undercuts, while achieving a good degree of dimensional control.

[0079] Figure 3 A cross-section of an exemplary biodegradable container 20 is shown, which includes a biodegradable vessel and a biodegradable lid 4. Figure 3 As shown, the container includes a liquid-containing barrier layer 7. In this invention, the liquid-containing barrier layer 7 can be heat-sealable to form an impermeable seal with the capping film 4 while remaining peelable. The liquid-containing barrier layer 7 can be applied to the fiber body 2 by spraying, or by welding or gluing as a laminate.

[0080] In the case of spraying, the liquid-retaining barrier layer 7 may include one or more coatings or layers. In this invention, the liquid-retaining barrier may include one or more biodegradable “primer” layers, i.e., applied directly to the fibrous body 2, to promote adhesion to subsequent barrier layers and minimize application defects. The primer may be applied in the form of a polymer dispersion, may be applied in the form of an aqueous polymer dispersion, and may include one of the following components: cellulose fibers, polyvinyl alcohol (PVOH), polyvinyl alcohol copolymers, PHA, chitosan, natural gums (such as xanthan gum and carrageenan), psyllium husk, sodium alginate, maltodextrin, polysaccharides, casein, whey, agar, certain thermoplastic starch grades, and starch can be used as a primer. The primer layer may include disintegrants, plasticizers, surfactants, lubricants / stripping agents, fillers, extenders, antiblocking agents, anti-sticking agents, defoamers, or other functional ingredients. Generally, the primer layer should be as thin as possible, but thick enough to form a barrier between the fibrous body 2 and subsequent layers. The average amount of primer applied to the surface of the molded substrate can be less than 60 g / m². 2 It can be less than 40g / m 2 It can be less than 20g / m 2After applying the primer layer, the component can be transferred to a heating unit, such as a hot air drying hood, to remove moisture from the coating and to promote film formation by melting or partially melting the polymer in the barrier layer. In this invention, the drying temperature can be between 100°C and 150°C, or between 110°C and 120°C, but other temperatures are acceptable depending on the chemistry of the primer. The components of the primer can be dissolved in water and applied simultaneously as a mixture. However, this invention can apply several primer layers to reduce the incidence of surface defects such as pinholes, spots, or cracks. These different layers can have different compositions. The liquid-containing barrier layer 7 may include an inorganic barrier layer to promote a reduction in moisture permeability (MVTR) throughout the structure. The inorganic barrier layer can be applied from the vapor phase or using a transfer process onto the surface of the primer. Suitable vapor-deposited inorganic coatings can be formed from 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, as well as metal oxides (e.g., Al₂O₃ or SiO�x), metal nitrides, and related compounds. The metallization layer can be transferred from another metallized substrate to a paper substrate. The thickness of the inorganic barrier coating can be 2 nm to 1,000 nm, 10 nm to 200 nm, or 20 nm to 100 nm. Alternatively, the thickness ratio of the inorganic barrier layer to the primer layer can be about 20 to about 20,000. The inorganic barrier layer may comprise a nanoclay layer laid down by an aqueous nanocomposite dispersion. In this invention, the inorganic layer laid down by the aqueous coating may be a lithium montmorillonite clay layer. Additional disclosures regarding lithium montmorillonite can be found in U.S. Patent Application Publication No. 2023 / 0234096 and U.S. Patent Application Publication No. 2023 / 0235510, which are incorporated herein by reference. The inorganic layer may also be a Cloisite clay layer as disclosed in U.S. Patent Application Publication No. 20220112664, which is incorporated herein by reference. The liquid-containing barrier layer 7 may include one or more topcoat layers, i.e., applied on top of the primer layer to provide additional moisture and oxygen barrier functions, maintain integrity during prolonged contact with the product, and form a peelable seal with the capping film. The topcoat layer may include linseed oil, carnauba wax, and / or beeswax as taught in WO2022 / 258697, which is incorporated herein by reference. Other waxes that meet the qualifying level of the OECD 301B biodegradability screening test may be used. Examples include keratin, rapeseed wax, castor wax, candelilla wax, soybean wax, palm oil wax, and some types of biodegradable paraffin oil-based waxes. The topcoat layer may also include shellac and chitosan. The shellac coating is applied as an ethanol dispersion and dried at 90°C. The topcoat can be an inorganic-organic hybrid polymer, such as bio-ORMOCER developed by the Fraunhofer Institute for Silicate Research in Würzburg, Germany.® or ORMOCER ® These materials are hybrids between glass and polymers, and their exact chemical properties can be customized for specific applications. (Bio-ORMOCER) ® Modified to be biodegradable. ORMOCER ® and bio-ORMOCER ® Non-limiting examples include those described in U.S. Patent Nos. 2011 / 0250441 A1 and 6709757B2, which are incorporated herein by reference, in addition to German Patents DE-OS 3828098 and DE4303570, which are also incorporated herein by reference. In this invention, the bio-ORMOCER can be dried at 120°C after application. ® Leave the topcoat on for 2 to 3 minutes to allow for complete cross-linking. Due to bio-ORMOCER ® The topcoat is not heat-sealable; therefore, container 1 is sealed to capping film 4 via a biodegradable adhesive (not shown). Shellac was found to have a total surface energy of 42.2 ± 1.6 mN / m, comprising a dispersed component of 36.6 ± 0.6 mN / m and a polar component of 6.6 ± 1.0 mN / m. Chitosan was found to have a total surface energy of 48.3 ± 1.2 mN / m, comprising a dispersed component of 33.2 ± 0.6 mN / m and a polar component of 15.2 ± 0.6 mN / m. Bio-Ormocer was found to have a total surface energy of 46.6 ± 1.2 mN / m, comprising a dispersed component of 36.6 ± 0.8 mN / m and a polar component of 10.0 ± 0.4 mN / m. All of the aforementioned topcoat layer chemicals were found to be surprisingly stable for the disclosed personal care formulation. Because the thickness of the surface coating affects the recyclability and biodegradability of the packaging made from the recyclable barrier paper composite of this invention, a thinner surface coating can be used. The amount of each topcoat layer can be less than 26 g / m². 2 It can be 2g / m 2 -26g / m 2 Within the range, it can be 2g / m 2 -5g / m 2 Within the range.

[0081] In this invention, the liquid-containing barrier layer 7 can be a layer applied by thermoforming under vacuum. The barrier layer can be made of a biodegradable thermoplastic material selected from the group consisting of aliphatic and / or aromatic polyesters or thermoplastic starches already mentioned. This ensures good formability of the material and good adhesion to the sealing film. In this invention, the laminating material comprises a binary blend of PLA and PBAT sold by BASF under the trade name ECOVIOÒ. The initial thickness of the laminate is 30 to 150 micrometers, and can be between 60 and 90 micrometers before application, depending on the target average final thickness. The structure of the film laminate 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. The application method includes adhering the barrier layer to a heating plate by vacuum-applied pressure and heating the barrier layer to the forming temperature. The pulp molding cup 2 is located on a mandrel. Once the target temperature is reached, the vacuum on the top plate is released, and the barrier layer is suspended by a vacuum applied to the mandrel side. The bottom mandrel can also be heated to promote adhesion between the laminate and the pulp molding cup. While the liquid-containing barrier layer 7 is in Figure 3 The image shows a uniform wall thickness, but in reality, a thickness gradient is formed depending on the amount of membrane stretching during the application process. It has been found that applying localized heat to the membrane (i.e., via a system such as WATTTRONÒ) can help achieve a more uniform wall thickness and prevent pinholes. The average thickness of the liquid-containing barrier layer 7 after application can be less than 90 micrometers, less than 75 micrometers, less than 50 micrometers, or less than 20 micrometers, depending on the desired barrier properties.

[0082] Figure 4 A cross-section of an exemplary biodegradable container 20 is shown. The biodegradable container includes a biodegradable vessel 1 having a biodegradable liquid containment barrier layer 7 applied to an inner surface and another layer applied to an outer surface as a liquid containment barrier layer 7. We have found that this configuration is particularly suitable for improving the barrier properties of the container while maintaining its biodegradability.

[0083] Figure 5A cross-section of an exemplary biodegradable container 20 is shown, comprising a biodegradable vessel 1 and a biodegradable lid, wherein a liquid-containing barrier layer 7 is applied to the outer surface via dip coating. The liquid-containing barrier layer 7 is applied to the outer surface via dip coating and may comprise one or more coatings or layers. The coatings may comprise one or more primer layers, an inorganic barrier coating, and one or more topcoat layers. The coatings may have the same composition as those described above for spray application. Using this application method, the thickness of each coating is typically determined by its viscosity and rotational speed. This application method ensures that the container 20 is “sealed” from the product and any external moisture. This has been found to be beneficial in maintaining the integrity of the primer layer from the effects of moisture stress gradients and ultimately also prevents damage to the barrier topcoat layer.

[0084] Figure 6 A cross-section of an exemplary biodegradable container 20 is shown, comprising a biodegradable vessel 1 and a biodegradable lid, wherein the vessel 1 is made of biodegradable paperboard material 10. The paperboard material 10 typically comprises a three-layer paper structure from bleached or unbleached chemical or chemi-thermo-mechanical pulp (CTMP). The paperboard material 10 is coated on one or both sides with one or more biodegradable thermoplastic materials selected from the group consisting of aliphatic and / or aromatic polyesters or thermoplastic starches already mentioned. Several commercially available solutions with such a construction exist, such as Bioware commercialized by Huhtamaki. ® CupformaNatura, or Cupforma commercialized by Stora Enso ® Bio / 2Bio. Although these vessels are typically used for short-term storage of liquids such as drinking cups, we have found these structures to be surprisingly stable for the compositions disclosed in this invention. Vessel 1 includes a molded plate sidewall 11 joined together in a seal 13 and a molded base 12. The side base 12 may be formed from a double-sided material. In this case, the sidewall 11 may extend to form another seal with the base 12 (not shown) having a typical cup configuration.

[0085] Figure 7An exemplary biodegradable container 20 is disclosed, comprising a biodegradable vessel 1 and a biodegradable lid 14, both of which are molded from pulp. The vessel 1 and lid 14 can be two separate components, or they can be a single component connected by a movable hinge. A biodegradable liquid-containing barrier layer 7 can be applied via spraying, dipping, or lamination. This barrier layer can be applied to the inner surface of the fiber body 2, or to both the inner and outer surfaces. In this invention, both the vessel 1 and lid 14 can be sealed by radial interference. An additional biodegradable tape (not shown) can be used to ensure that the component does not decompose during transport, such as one made of cellulose acetate. In this invention, the pulp may include fibers and additives to maintain good elasticity for proper functioning of the movable hinge. In this invention, the cellulose fibers forming the molded pulp component may include cork, bamboo, and bagasse. The length-weighted average fiber length, arithmetic mean fiber length (ISO 0.2–7.0 mm), and arithmetic mean fiber width can be determined using a fiber image analyzer such as the Valmet FS5, based on TAPPI T271. Cork 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 0.2–7.0 mm), and an arithmetic mean fiber width of approximately 30 mm. 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 0.2–7.0 mm), and an arithmetic mean fiber width of approximately 15 mm. Bagasse fibers may have a length-weighted average fiber length of approximately 1.0 mm, an arithmetic mean fiber length of approximately 0.6 mm (ISO 0.2–7.0 mm), and an arithmetic mean fiber width of approximately 22 mm. In this invention, the fiber count may include between 50% and 60% bamboo, 40% and 50% bagasse, and 0% and 10% cork.

[0086] Cellulose 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 flaky kaolin; (2) sizing agents, such as alkyl ketone dimers (AKD), alkenyl succinic anhydride (ASA), rosin, or lignin; (3) additives for dry strength enhancement, such as starch, amphoteric, cationic, or anionic polyacrylamide resins, enzymes, and modified polyamines; (4) additives for wet strength enhancement, such as polyamide amine (PAE) or polyamine epichlorohydrin, epoxide or cationic acetaldehyde resins, or (5) microfibrillated cellulose (MFC) or cellulose nanocrystal (CNC) additives.

[0087] In this invention, based on dry fiber count, the pulp may include 0.5% to 2%, or about 1% AKD, to provide some excellent water resistance. The pulp may also include between 0.1% and 0.5% PAE to provide some excellent wet strength to the final product. In this invention, based on dry fiber count, the pulp may include between 2% and 5%, or between 3% and 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. In this invention, the pulp portion may be functionalized after molding by vapor deposition of an inorganic barrier layer as described above.

[0088] Figure 8 A cross-section of an exemplary biodegradable vessel 1 is disclosed, wherein this is a bottle 15 made of fibrous cellulose material obtained by wet molding. In this invention, the bottle can be grafted with an injection-molded thermoplastic starch neck 16 as described in application WO 2022 / 258707, which is incorporated herein by reference. The bottle can be bonded with a biodegradable closure using thermoplastic starch (not shown). Both the neck and the closure can be coated as described in application WO 2022 / 258697 to protect the components from formulation incompatibility, which is incorporated herein by reference. In this invention, the pulp can include fibers and additives to maintain good extrudability. In this invention, the cellulose fibers forming the molded pulp component can include cork, bamboo, and bagasse. The length-weighted average fiber length, arithmetic mean fiber length (ISO 0.2–7.0 mm), and arithmetic mean fiber width according to TAPPI T271 can be determined using a fiber image analyzer such as Valmet FS5. Cork fibers may have a length-weighted average fiber length of about 2.25 mm, an arithmetic mean fiber length of about 1.4 mm (ISO 0.2–7.0 mm), and an arithmetic mean fiber width of about 30 mm. Bamboo fibers may have a length-weighted average fiber length of about 15 mm, an arithmetic mean fiber length of about 1.0 mm (ISO 0.2–7.0 mm), and an arithmetic mean fiber width of about 15 mm. 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 0.2–7.0 mm), and an arithmetic mean fiber width of about 22 mm. In this invention, the fiber count may include between 50% and 60% bamboo, 40% and 50% bagasse, and 0% and 10% cork.

[0089] Cellulose 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 flaky kaolin; (2) sizing agents, such as alkyl ketone dimers (AKD), alkenyl succinic anhydride (ASA), rosin, or lignin; (3) additives for dry strength enhancement, such as starch, amphoteric, cationic, or anionic polyacrylamide resins, enzymes, and modified polyamines; (4) additives for wet strength enhancement, such as polyamide amine (PAE) or polyamine epichlorohydrin, epoxide or cationic acetaldehyde resins, or (5) microfibrillated cellulose (MFC) or cellulose nanocrystal (CNC) additives.

[0090] In this invention, based on dry fiber count, the pulp may include 0.5% to 2%, or about 1% AKD, to provide some excellent water resistance. The pulp may also include between 0.1% and 0.5% PAE to provide some excellent wet strength to the final product. In this invention, based on dry fiber count, the pulp may include between 2% and 5%, or between 3% and 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. In this invention, the pulp portion may be functionalized after molding by vapor deposition of an inorganic barrier layer as described above.

[0091] The bottle includes a liquid-retaining barrier layer 7 on the inner surface of the bottle 15. The liquid-retaining barrier layer 7 on the inner surface of the bottle 15 can be applied to the pulp molded bottle by spraying or dipping. In the case of spraying, the liquid-retaining barrier layer may include one or more biodegradable coatings or layers, including one or more primers and one or more topcoats, as previously disclosed.

[0092] Figure 9A cross-section of an exemplary vessel 1 is shown, wherein the vessel is a biodegradable bottle 15, and a liquid-containing barrier layer 7 is applied via dip coating to all component surfaces, the inner and outer surfaces of the biodegradable bottle 15. The liquid-containing barrier layer 7 may comprise one or more coatings or layers. The coatings may comprise one or more primer layers, an inorganic barrier coating, and one or more topcoat layers. The coatings may have the same composition as those described above for spray application. Using this application method, the thickness of each coating is typically determined by its viscosity and rotational speed. This application method ensures that the bottle is “sealed” from the product and any external moisture. This has been found to be beneficial in maintaining the integrity of the primer layer from the effects of moisture stress gradients and ultimately also prevents damage to the barrier topcoat layer.

[0093] Figure 10 A cross-section of an exemplary biodegradable vessel 1 is shown, wherein the container is a pulp bottle 17, the pulp 18 is undermolded using MFC and then processed via atomic layer deposition (ALD) after molding to provide the necessary liquid containment properties.

[0094] Packaging testing methods

[0095] 1) Individual layer thickness

[0096] 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.

[0097] 2) Thickness

[0098] 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. 2 And 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.

[0099] 3) Basis weight

[0100] 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.

[0101] 4) Substrate / Individual Layer Roughness Measurement (Sq)

[0102] Root mean square roughness (Sq) was measured using a 3D laser scanning confocal microscope, such as the Keyence VK-X200 series microscope purchased from the Keyence Corporation of America. This 3D laser scanning confocal microscope includes a VK-X200K controller and a K-X210 30 measurement unit. The instrument manufacturer's software, VK Viewer version 2.4.1.0, was used for data collection, and the manufacturer's software, Multifile Analyzer version 1.1.14.62 and VK Analyzer version 3.4.0.1, were used for data analysis. If desired, the manufacturer's image stitching software, VK Image Stitching version 2.1.0.0, was used. The manufacturer's analysis software, 15377P 22, conforms to ISO 25178. The light source used was a semiconductor laser with a wavelength of 408 nm and a power of approximately 0.95 mW. Thermal seal strength was also considered. Unless otherwise specified, test method ASTM F88-06 can be used to measure the heat seal strength of heat seals formed from various barrier paper laminates.

[0103] 5) Pinhole test method

[0104] 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 onto the test surface, applying pressure to the surface using a dropper 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 across 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.

[0105] 6) Leakage test method

[0106] This is a test method for measuring a container's ability to prevent leakage during storage or transportation.

[0107] Pre-treat at least three representative empty containers and the type of cap being tested at 22±3°C and 60%±10 RH for at least 24 hours. Prepare a tap water solution at room temperature, adding a dye 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±1 mL, at laboratory ambient temperature, equipped with their respective closures (if applicable), and hermetically sealed in the storage configuration. Dry any outer surfaces (if necessary) with a (paper) towel so that no product remains on them. Place the sample in a flat position on a 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±3°C and 60%±10 RH. It is not necessary to place any weights or other containers on top of the sample being tested. Alternative sample orientations during testing can be considered so that suspected leakage areas are covered with liquid. Check for liquid leakage after 24 hours, 1 week, and 2 weeks. Note the location of any eventual leakage. 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.

[0108] 7) Water vapor transmission rate (WVTR)

[0109] This test method is primarily based on ASTM F1249-13 under the following test conditions: the test gas temperature is 38°C (±0.56°C) and its relative humidity is 50% (±3%), or, if tropical conditions are required, the test gas temperature is set to 38°C (±0.56°C) and its relative humidity to 90% (±3%). The carrier gas is 100% N2 (dry). The equipment used to run the test is a Permatran-W water vapor permeability instrument conforming to written specification QMS 702-004. For materials outside the scope of ASTM F-1249-13 (§1.1), the water vapor transmission rate test method is not applicable. If the barrier properties of a particular substrate are too poor, especially if the coating on a paper substrate is very thin and the equipment is not properly sealed, it is impossible to measure WVTR by ASTM F1249-13. In these cases, a different test method is used, namely the ASTM E96 cup test method. However, results from the two different test methods can still be compared. For ASTM E96, if tropical conditions are required, the temperature is 38°C and the humidity is 90% relative humidity; otherwise, the humidity is sometimes 50% relative humidity. For either test method, water vapor transmission rate is reported in g / m² / day. If normalized by barrier thickness, water vapor transmission rate is reported in g.µm / m² / day.

[0110] 8) Oxygen Transmission Rate (OTR) )

[0111] This test method is primarily performed according to ASTM F1927 under the following test conditions: unless otherwise specified, the temperature of the test gas is 23°C (±0.56°C) and its relative humidity is 80% (±3%), and the concentration of the test gas is 100% O2. The carrier gas is 98% N2 and 2% H2, and the carrier gas humidity is 0%. The test gas pressure is 760 mmHg. The equipment used for this test is an Oxtran 2 / 21 oxygen permeability meter conforming to test procedure QMS 702-002. For either test method, oxygen permeability is reported in cc / m² / day. If normalized by barrier thickness, water vapor permeability is reported in cc.µm / m² / day.

[0112] 9) Weight loss test method

[0113] This method is used to determine the weight loss of water through containers or individual components such as vessels and lids. At least three representative empty samples of the test type are pretreated at 23±2°C and 60%±10 RH for at least 24 hours.

[0114] 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, which is equipped with its corresponding closure / cap (if applicable) and is hermetically sealed 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.

[0115] For flat components, such as capping films, 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 to be measured is cut into a circle slightly larger than the cup opening. At least three representative specimens of the material and condition 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.

[0116] 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 ± 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 and report the weight loss as an average of the daily weight loss per square meter at 25 °C, 60% RH, or under relevant test conditions. This test is not applicable if the weight loss does not reach a steady state, such as in the event of a packaging failure with leakage.

[0117] 10) Bottle squeeze test method

[0118] 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 fill capacity (e.g., 200 ± 1 g) and then pretreated at 22 ± 3 °C and 60% ± 10 RH for at least 24 hours. The bottles are equipped with their respective closures to ensure no leakage.

[0119] Each bottle is then placed in a compression tester using a clamp 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.

[0120] 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.

[0121] 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).

[0122] 11) Recyclability in pulp stream based on PTS-RH 021 CAT 2

[0123] 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 ± 1 g of the 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.

[0124] 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."

[0125] 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.

[0126] 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."

[0127] 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".

[0128] 12) Biodegradation screening test OECD 301B

[0129] Ideally, the biodegradability of each part and the main components of the final packaging should be tested according to test method OECD 301B.

[0130] The final packaging includes all major and minor (ink, varnish) components and is open at one end to simulate disposal after being opened by the consumer. Success / failure criteria are shown in the table below: OECD Biodegradation Test Methods and Standards

[0131] The sample should be at least 60% biodegradable within 60 days, or at least 60% biodegradable within 30 days.

[0132] Aerobic biodegradation is measured by the amount of carbon dioxide (CO2) produced by the test material, according to the standard test method defined in OECD Method 301B Test Guidelines. This test is performed according to the specified OECD test protocol, but over a period of 60 days. The polymer must achieve at least 60% biodegradation, as measured by CO2 production over 60 days in Standard Method 301B. These OECD test method guidelines are well known in the art and are cited herein as references {OECD (1992) Test No. 306: Biodegradability in Seawater, OECD Guidelines for the Testing of Chemicals, Section 3, OECD Publishing, Paris, https: / / doi.org / 10.1787 / 9789264070486-en. and OECD (1992), Test No. 301: Ready Biodegradability, OECD Guidelines for the Testing of Chemicals, Section 3, OECD Publishing, Paris, https: / / doi.org / 10.1787 / 9789264070349-en.}.

[0133] 13) OK composting INDUSTRIAL (EN 13432) test

[0134] Packaging or products bearing the OK Compost INDUSTRIAL label are guaranteed to be biodegradable in industrial composting plants. This applies to all components, inks, and additives. The sole reference point for the certification process is the harmonized EN 13432:2000 standard: Under no circumstances should any product bearing the OK Compost INDUSTRIAL logo comply with the requirements of the EU Packaging Directive (94 / 62 / EEC).

[0135] One test is a disintegration test. To pass the disintegration test, the packaging must disintegrate 90% within 12 weeks, with any remaining fragments able to pass through a 2mm sieve. The temperature must not rise above 75°C, and must be reduced to 50°C after one week. This is to simulate what would happen in a real industrial composting unit.

[0136] 14) OK Compost HOME

[0137] Because the volume of waste involved is relatively small, the temperature in garden compost heaps is significantly lower and less constant than in industrial composting environments. This is why composting in a garden is a more difficult and slower process. TÜVAUSTRIA developed OK Compost HOME to guarantee complete biodegradability according to specific requirements, even in garden compost heaps. OK Compost HOME is not based on a standard, but rather on several standards. It is important to remember that the OK Compost HOME certification process does not explicitly reference any specific standard, but rather details all the technical requirements that a product must meet to obtain certification. The disintegration test involves ensuring that disintegration occurs within 6 months at a temperature not exceeding 30°C. This is to simulate what would happen in a real home compost.

[0138] 15) Surface free energy calculation

[0139] Free surface energy and its dispersion and polar components were estimated using a high-speed optical contact angle measurement system. To calculate the free surface energy, contact angles of a series of well-characterized liquids (water, density = 1.000 kg / m³; diiodomethane, density = 3.325 kg / m³; ethylene glycol, density = 1.113 kg / m³) were used. The static contact angle of the liquid on the surface was evaluated using a fixed droplet method with a circular or elliptical fitted shape (droplet volume 2 ml). The free surface energy and its components were calculated according to the general OWRK (Owens-Wendt-Rabel-Kaelble) method. For each coating, the contact angle of each liquid on each surface was measured 4–5 times. Clean glass plates were used as reference surfaces (1 sample, 5 measurements for each liquid).

[0140] Personal care composition

[0141] Detergent surfactants

[0142] 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.

[0143] Personal care compositions may contain one or more surfactants, ranging from about 10% to about 23% by weight, from about 12% to about 21% by weight, or from about 10% to about 18% by weight.

[0144] 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.

[0145] 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.

[0146] The compositions of the present invention may further comprise anionic surfactants selected from the group consisting of: a)R1 O(CH2CHR3O) ySO3M; 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.

[0147] 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.

[0148] 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.

[0149] 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.

[0150] 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.

[0151] The personal care composition may also contain about 0.5% to about 8% by weight, about 1.0% to about 7% by weight, about 1.5% to about 6% by weight of one or more amphoteric, zwitterionic, nonionic auxiliary surfactants, or mixtures thereof.

[0152] 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.

[0153] 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.

[0154] 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.

[0155] 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.

[0156] 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.

[0157] 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.

[0158] 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.

[0159] 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.

[0160] 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.

[0161] 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.

[0162] 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.

[0163] 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,

[0164] Also applicable to this article are tertiary alkylamine oxides, including lauryl amine oxides and cocoyl amine oxides.

[0165] 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.

[0166] A suitable surfactant blend comprises about 0.5% to about 30%, about 1% to about 25%, and about 2% to about 20% of an average weight percentage of alkyl branches. The surfactant blend may have a cumulative average weight percentage of C8 to C12 alkyl chain lengths of about 7.5% to about 25%, about 10% to about 22.5%, and about 10% to about 20%. The surfactant blend 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, and about 75 to about 125.

[0167] wetting agent

[0168] 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 arginine aspartic acid, 1,3-butanediol, propylene glycol and water, as well as soft-haired pine algae extract, collagen amino acids or peptides, creatine anhydride, 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 (available from Larex), glycosaminoglycans, methoxy PEG 10, methyl glucetol polyether-10 and methyl glucetol polyether-20 (all commercially 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, PEG4, 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 glycerol PCA), Glycoisoesters, SEACARE (available from Secma), Serine, Serine, Sodium Acetyl Hyaluronic Acid, Sodium Hyaluronic Acid, Sodium Polyaspartate, Sodium Polyglutamate, Sorbitol Polyether 20, Sorbitol Polyether 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.

[0169] 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.

[0170] The composition contains a safe and effective amount of wetting agent. In particular, it may contain about 20% to about 70% by weight; about 20% to about 50% by weight; or about 23% to about 45% by weight of wetting agent.

[0171] In this invention, the composition may contain two or more different wetting agents; for example, the composition may contain glycerol and xylitol.

[0172] Thickening polymer

[0173] 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.

[0174] 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.

[0175] 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.

[0176] The thickening polymer can be a soluble crosslinked acrylic polymer, and non-limiting examples include carbomer.

[0177] 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.

[0178] 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.

[0179] The thickening polymer can be combined with alginate-based materials, and non-limiting examples include sodium alginate and propylene glycol alginate.

[0180] 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.

[0181] 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.

[0182] 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.

[0183] 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.

[0184] Thickening polymers can be used with polyethylene oxide, polypropylene oxide, and POE-PPO copolymers.

[0185] Thickening polymers can be combined with polyalkylene glycols characterized by the following general formula:

[0186] 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.

[0187] Thickening polymers can be combined with silica, and non-limiting examples include pyrolytic silica, precipitated silica, and silica with an organosilicon surface treatment.

[0188] Thickening polymers can be combined with water-swellable clays, and non-limiting examples include synthetic lithium saponite, bentonite, montmorillonite, chlorophyllite, and lithium montmorillonite.

[0189] 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.

[0190] 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, SepimaxZen, Carbopol ® SMART 1000, Rheocare ® TTA, Rheomer ® SC-Plus, STRUCTURE ® PLUS, Aristoflex ® AVC, Stabylen 30, and combinations thereof.

[0191] Scalp care active ingredients

[0192] This invention may include scalp care active ingredients. These scalp care active ingredients include soluble scalp care active ingredients and scalp health agents.

[0193] a) Soluble active ingredients for scalp care

[0194] 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.

[0195] 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.

[0196] 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.

[0197] b) Scalp health products

[0198] 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:

[0199] 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.

[0200] And natural extracts / oils, including peppermint oil, spearmint, argan oil, jojoba oil and aloe vera.

[0201] In this invention, the scalp care active ingredient may be in encapsulated form. In one aspect, the capsule may comprise: melamine, 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% encapsulation, up to 10%, up to 5%, or up to 1%.

[0202] 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.

[0203] 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.

[0204] The personal care composition of the present invention may contain about 14% to about 50% water; or may have about 35% to about 50% water.

[0205] Test methods for formulations

[0206] Water activity

[0207] In this invention, water activity is measured as Aw (when in the range of 0-1) or relative humidity -%RH (when reported as a percentage), 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.

[0208] Water activity determined

[0209] In this invention, the equipment used for determining water activity can be: A) a Hygrolab C-1 water activity meter (available from Rotronic AG) equipped with temperature and humidity probes and B) a shallow disposable sample cup (available from Rotronic AG). In this invention, the water activity of the test material can be determined using the temperature and humidity probes and the Hygrolab C-1 meter (available from Rotronic AG). The disposable sample cup (available from Rotronic AG) is filled with the test material, lowered into a sample holder, and covered by the humidity and temperature probes. Using the meter's AwE mode, the water activity of the equilibrium product will be displayed on the meter as water activity (Aw). The following conversion factor can be used to switch between units: 1.000 Aw = 100% RH. Viscosity method.

[0210] 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.

[0211] Viscosity determination

[0212] In this invention, the equipment and instruments used for viscosity determination are: A) a disposable syringe (available from VWR); a rheometer (available from TA Instruments); and C) a 40mm parallel steel plate (available from TA Instruments). In this invention, the viscosity of the shampoo test material can be determined using a Discovery DHR rheometer from TA Instruments (New Castle, Delaware, USA). Data collection, processing, and reporting are performed using TRIOS software version 5.1.1.46572 (available 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. Viscosity is measured at 2.0s. -1 Data are collected by measuring the flow peak at a shear rate maintained for 180 seconds, and the reported viscosity is the value measured at 180 seconds. In this invention, the personal care composition may have a viscosity of about 5,000 cps to about 20,000 cps; about 8,000 cps to about 14,000 cps; or about 7,000 cps to about 12,000 cps.

[0213] The product has been reformulated to reduce water activity and water content.

[0214] In this invention, to prevent premature hydrolysis of the biodegradable polymer layer on the inner side of the pulp container, the water activity and water content of the shampoo formulation must be reduced. This is achieved by modifying commercially available shampoo formulations by removing any added water that does not enter the formulation as part of another ingredient (e.g., surfactants typically enter as part of an aqueous solution). Because the shampoo needs to be a liquid with a viscosity similar to that of commercially available shampoos (to allow for good spreadability on hair), only flowable liquids and soluble solids are considered to replace the 29%-41% of added water in commercially available cosmetic shampoos. Because it is desirable not only to reduce the water content but also to reduce the water activity (reactivity) of the remaining water in the formulation, water-binding components (wetting agents) are selected. Replacing the 29%-41% water in the shampoo with a combination of both glycerin and sodium chloride produces a stable formulation with both lower water content and activity. Furthermore, glycerin is known to provide a conditioning feel on hair compared to water.

[0215] Non-limiting embodiments

[0216] 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.

[0217] Formulation Examples

[0218] Examples A and B are conventional cosmetic formulation examples with high water activity (Aw), which serve as a control comparison with Example C1, which is a formulation example of the present invention with reduced water activity (Aw).

[0219] Implementation Example Description : A-Higher Aw Traditional Shampoo B-Higher Aw Traditional Anti-Dandruff Shampoo C-lower Aw D-lower Aw E-lower Aw for dandruff F-lower Aw for dandruff G-lower Aw alternative wetting agent H-low, Aw, sulfate-free I-lower Aw, sulfate-free

[0220] Ingredient Code :

[0221] Table of biodegradable container examples with lower Aw shampoo stability data

[0222] Biodegradable containers with lower Aw shampoo stability data

[0223] The table above discloses an exemplary biodegradable container comprising a biodegradable vessel (wall material) based on this disclosure and an exemplary sealing film. The vessel is molded from wet pulp and covered with a liquid-containing barrier layer across its entire surface. The liquid-containing barrier layer is made of three distinct layers, all applied by dip coating: (1) a first layer comprising MFC, (2) a second layer comprising carnauba wax and linseed oil, and (3) a third layer comprising shellac. The sealing film is a home-compostable triple-laminated paper composite, commercially available by ParksideÒ. Neither the vessel nor the sealing film was found to have pinholes. The entire package is biodegradable. The vessel also met the minimum pass requirements for repulpingability according to PTS-RH 021 / 97 cat 2 method. Both the exemplary container and the sealing film were tested separately using the lower water activity (Aw) shampoo formulation example D and the higher water activity (Aw) shampoo, and the weight change over time was measured using method #9, the weight loss test method, as an indicator of relative stability. For both the exemplary container and the sealing film, it was found that under the same storage conditions, the weight change of the higher Aw conventional shampoo example A was significantly greater than that of the lower Aw shampoo example D.

[0224] Additional Examples / Combinations

[0225] A. A biodegradable container for use with a liquid personal care composition, said biodegradable container comprising: a) A biodegradable container having at least one opening and a biodegradable lid for the opening, wherein the container contains... b) 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.

[0226] B. A biodegradable container for use with a liquid personal care composition as described in paragraph A, wherein the biodegradable container comprises cellulose fibers and is molded from pulp.

[0227] C. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to B, wherein the biodegradable cap is a biodegradable sealing film.

[0228] D. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to C, wherein the biodegradable container includes a biodegradable liquid containment barrier layer having one or more layers and one or more coatings.

[0229] E. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through D, wherein the biodegradable vessel comprises an inorganic barrier layer applied to the cellulose fibers by vapor deposition after pulp molding.

[0230] F. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through E, wherein the biodegradable liquid containment barrier layer comprises one or more primer layers comprising a material selected from the group consisting of: cellulose fibers, polyvinyl alcohol (PVOH), polyvinyl alcohol copolymers, polyhydroxyalkanoates (PHA), polybutylene adipate succinate (PBSA), chitosan, natural gums such as xanthan gum and carrageenan, psyllium husk, sodium alginate, maltodextrin, polysaccharides, casein, whey, agar, thermoplastic starch, and mixtures thereof.

[0231] G. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through F, wherein the biodegradable liquid containment barrier layer comprises an inorganic barrier layer.

[0232] H. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through G, wherein the biodegradable liquid containment barrier layer comprises one or more topcoat layers selected from the group consisting of: linseed oil, carnauba wax, beeswax, keratin, rapeseed wax, castor wax, candelilla wax, soybean wax, palm oil wax, biodegradable paraffin oil-based waxes, shellac, chitosan, inorganic-organic hybrid polymers, and mixtures thereof.

[0233] I. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to H, wherein the free surface energy of the topcoat is between 40 mN / m and 50 mN / m, and wherein the dispersion energy component is between 32 mN / m and 37 mN / m, and the polar energy component is between 5 mN / m and 16 mN / m.

[0234] J. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to I, wherein the liquid-containing barrier layer is a thermoplastic material selected from the group consisting of aliphatic and / or aromatic polyesters or thermoplastic starches.

[0235] K. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to J, wherein the thermoplastic material is applied by thermo-vacuum thermoforming.

[0236] L. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to K, wherein the biodegradable container is made of biodegradable cardboard.

[0237] M. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to L, wherein both the biodegradable vessel and the biodegradable cap are molded from pulp.

[0238] N. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through M, wherein the biodegradable vessel and the biodegradable cap are integrally molded from pulp and include a hinge.

[0239] O. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to N, wherein the biodegradable capping comprises a sealant layer made of a water-soluble biodegradable polymer.

[0240] P. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to O, wherein the biodegradable capping membrane comprises an inorganic barrier layer.

[0241] Q. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through P, wherein the biodegradable capping film comprises cellulose.

[0242] R. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through Q, wherein the biodegradable container includes components grafted onto the biodegradable container, wherein the components are made of a biodegradable polymer.

[0243] S. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to R, wherein the biodegradable polymer is thermoplastic starch.

[0244] T. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to S, wherein the liquid personal care composition comprises about 35% to about 50% water.

[0245] U. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to T, wherein the wetting agent is from about 23% to about 45%.

[0246] V. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to U, wherein the humectant is selected from the group consisting of: glycerin, amino acids, proline, arginine aspartic acid, 1,3-butanediol, propylene glycol and water, soft-haired pine algae extract, collagen amino acids or peptides, creatine anhydride, 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, 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, glycerol PCA, glycoisoesters, serine, serine 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.

[0247] W. A biodegradable container 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, sodium chloride, and mixtures thereof.

[0248] X. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through W, wherein the water activity (Aw) is about 0.80 to about 0.90.

[0249] Y. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through X, wherein the water activity (Aw) is less than about 0.80.

[0250] Z. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through Y, wherein the liquid personal care composition comprises a surfactant.

[0251] AA. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through Z, wherein the surfactant is present in amounts of about 10% to about 18%.

[0252] BB. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through AA, wherein the surfactant is selected from one or more anionic surfactants.

[0253] CC. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through BB, wherein the liquid personal care composition comprises an amphoteric auxiliary surfactant.

[0254] DD. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through CC, wherein the amphoteric auxiliary surfactant is selected from the group consisting of cocamidopropyl betaine, lauramide propyl betaine, and mixtures thereof.

[0255] EE. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through D, wherein the liquid personal care composition contains a thickener.

[0256] FF. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through EE, wherein the liquid personal 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, 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.

[0257] GG. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through FF, wherein the thickener is selected from the group consisting of hydroxyethyl cellulose.

[0258] HH. Biodegradable containers for use with liquid personal care compositions as described in paragraphs A through GG, wherein the liquid personal care composition contains sodium chloride.

[0259] II. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through HH, wherein the liquid personal care composition contains scalp health active substances.

[0260] JJ. A biodegradable container for use with a liquid personal care composition as described in paragraphs A through II, wherein the scalp health active ingredient is selected from the group consisting of piroctone ethanolamine, zinc pyrithione, clomiphene, sulfur, and mixtures thereof.

[0261] KK. Biodegradable containers for use with liquid personal care compositions as described in paragraphs A through JJ, wherein the personal care composition has a viscosity of about 5,000 cps to about 20,000 cps.

[0262] LL. A biodegradable container for use with a liquid personal care composition as described in paragraphs A to KK, wherein the liquid personal care composition acquires water when packaged within the container, and wherein the acquisition of water by the liquid personal care composition achieves the physical or chemical properties of the final formulation of the liquid personal care composition.

[0263] 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”.

[0264] 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.

[0265] While specific embodiments of the invention have been illustrated and described by way of example, 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 biodegradable container for use with a liquid personal care composition, said biodegradable container comprising: a) A biodegradable container having at least one opening and a biodegradable cap for the opening; b) A liquid personal care composition comprising 14% to 50% water, preferably 35% to 50% water; 20% to 70% a humectant, preferably 23% to 45% a humectant, preferably wherein the humectant is selected from the group consisting of: glycerin, amino acids, proline, arginine aspartic acid, 1,3-butanediol, propylene glycol and water, soft-haired pine algae extract, collagen amino acids or peptides, creatine anhydride, 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, 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, glycerol PCA, glycoisoesters, serine, serine 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 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; The water activity (Aw) is between 0.40 and 0.90, preferably between 0.80 and 0.

90.

2. The biodegradable container according to any of the preceding claims, wherein the biodegradable vessel comprises cellulose fibers and is molded from pulp.

3. The biodegradable container according to any of the preceding claims, wherein the biodegradable cap is a biodegradable sealing film.

4. The biodegradable container according to any of the preceding claims, wherein the biodegradable vessel comprises a biodegradable liquid containment barrier layer having one or more layers and one or more coatings.

5. The biodegradable container according to any of the preceding claims, wherein the biodegradable vessel comprises an inorganic barrier layer applied to the cellulose fibers by vapor deposition after pulp molding.

6. The biodegradable container according to any of the preceding claims, wherein the biodegradable liquid containment barrier layer comprises one or more primer layers, the one or more primer layers comprising a material selected from the group consisting of: cellulose fibers, polyvinyl alcohol (PVOH), polyvinyl alcohol copolymers, polyhydroxyalkanoates (PHA), polybutylene adipate succinate (PBSA), chitosan, natural gums such as xanthan gum and carrageenan, psyllium husk, sodium alginate, maltodextrin, polysaccharides, casein, whey, agar, thermoplastic starch, and mixtures thereof.

7. The biodegradable container according to any of the preceding claims, wherein the biodegradable liquid containment barrier layer comprises an inorganic barrier layer.

8. The biodegradable container according to any of the preceding claims, wherein the biodegradable liquid containment barrier layer comprises one or more topcoat layers selected from the group consisting of: linseed oil, carnauba wax, beeswax, keratin, rapeseed wax, castor wax, candelilla wax, soybean wax, palm oil wax, biodegradable paraffin oil-based waxes, shellac, chitosan, inorganic-organic hybrid polymers, and mixtures thereof.

9. The biodegradable container according to any of the preceding claims, wherein the free surface energy of the topcoat is between 40 mN / m and 50 mN / m, and wherein the dispersion energy component is between 32 mN / m and 37 mN / m, and the polar energy component is between 5 mN / m and 16 mN / m.

10. The biodegradable container according to any of the preceding claims, wherein the liquid containment barrier layer is a thermoplastic material selected from the group consisting of aliphatic and / or aromatic polyesters or thermoplastic starches.

11. The biodegradable container according to any of the preceding claims, wherein the thermoplastic material is applied by thermo-vacuum thermoforming.

12. The biodegradable container according to any of the preceding claims, wherein the biodegradable container is made of biodegradable cardboard.

13. The biodegradable container according to any of the preceding claims, wherein both the biodegradable vessel and the biodegradable lid are molded from pulp.

14. The biodegradable container according to any of the preceding claims, wherein the biodegradable vessel and the biodegradable lid are integrally molded from pulp and include a hinge.

15. The biodegradable container according to any of the preceding claims, wherein the biodegradable cover comprises a sealant layer made of a water-soluble biodegradable polymer.

16. The biodegradable container according to any of the preceding claims, wherein the biodegradable capping membrane comprises an inorganic barrier layer.

17. The biodegradable container according to any of the preceding claims, wherein the biodegradable sealing film comprises cellulose.

18. The biodegradable container according to any of the preceding claims, wherein the biodegradable vessel comprises a component grafted to the biodegradable vessel, wherein the component is made of a biodegradable polymer.

19. The biodegradable container according to any of the preceding claims, wherein the biodegradable polymer is thermoplastic starch.

20. The biodegradable container according to any of the preceding claims, wherein the water activity (Aw) is less than 0.

80.

21. The biodegradable container according to any 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.

22. The biodegradable container according to any 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.

23. The biodegradable container according to any of the preceding claims, wherein the liquid personal care composition comprises a thickener, preferably wherein the liquid personal 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, acrylate The following are crosspolymers: 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, preferably wherein the thickener is selected from the group consisting of hydroxyethyl cellulose.

24. The biodegradable container according to any of the preceding claims, wherein the liquid personal care composition comprises sodium chloride.

25. The biodegradable container according to any 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 olamine, zinc pyrithione, clomiphene, sulfur, and mixtures thereof.

26. The biodegradable container according to any of the preceding claims, wherein the personal care composition has a viscosity of 5,000 cps to 20,000 cps.

27. A biodegradable container for use with a liquid personal care composition according to any of the preceding claims, wherein the liquid personal care composition acquires water when packaged in the container, wherein the acquisition of water by the liquid personal care composition achieves the physical or chemical properties of the final formulation of the liquid personal care composition.

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