Emollient Composition
The introduction of cocoa butter fatty acid ethyl esters addresses the limitations of natural vegetable oils by enhancing oxidative stability and skin absorption, resulting in more effective and longer-lasting personal care products.
Patent Information
- Application Number
- JP2024549561
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2022-02-28
- Filing Date
- 2023-02-28
- Publication Date
- 2025-04-10
AI Technical Summary
Natural vegetable oils used in personal care products face limitations due to oxidation and decomposition of antioxidants, leading to reduced effectiveness and a short shelf life.
The development of emollient compositions comprising a mixture of cocoa butter fatty acid ethyl esters, which are produced by esterifying cocoa butter with ethyl alcohol in the presence of a catalyst, offering improved stability and performance.
The use of cocoa butter fatty acid ethyl esters provides emollients with enhanced oxidative stability, improved skin absorption, and extended shelf life, making them suitable for a range of personal care products.
Smart Images

Figure 2025508793000001 
Figure 2025508793000002 
Figure 2025508793000003
Abstract
Description
[Technical field]
[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This application claims the benefit of U.S. Provisional Patent Application No. 63 / 268,640, filed February 28, 2022, which is incorporated by reference herein in its entirety.
[0002] The present invention relates to an emollient composition, its method of preparation, and its use in personal care products. [Background technology]
[0003] Emollients are personal care products commonly used to relieve dry skin by keeping the skin moist. Emollients can be a wide variety of ingredients ranging from synthetically derived compounds (e.g., mineral oil) to natural ingredients (e.g., vegetable oils).
[0004] Mineral oil, a by-product of petroleum refining, has long been used as a main ingredient in emollient formulations due to its low volatility and smooth texture. Like other moisturizers, mineral oil helps to lock in moisture and smooth dry and rough skin. However, because mineral oils do not easily absorb and penetrate the skin, they remain on the skin surface, where they can clog pores and cause other skin problems.
[0005] There have been many efforts in the personal care and cosmetics industry to develop bio-based and natural alternatives to mineral and vegetable oils, and they have emerged as one of the most popular alternatives. An important advantage of vegetable oils is their natural source. They are generally not harmful to the environment and more closely mimic the lipid composition of skin and hair, making them easily absorbed. They promote the protection of the skin against excessive loss of water and nutrients, without interfering with the skin's natural functions, and help moisturize and structure the underlying tissues.
[0006] Despite these desirable properties, natural vegetable oils have some inherent limitations: Oxidation of vegetable oils, along with the breakdown of antioxidants, can cause products to acquire undesirable properties or even lose their effectiveness after a relatively short shelf life.
[0007] Cocoa butter is fat derived from cocoa beans.It is widely accepted and recognized as an essential ingredient for making chocolate and confectionery.Due to its pleasant fatty acid profile and good odor on skin, cocoa butter has emerged as one of the most promising and healthy ingredients in cosmetics and personal care products.
[0008] As the demand for natural-based ingredients useful in personal care and cosmetic applications increases, it would be advantageous to have new natural-based materials with improved properties that more closely mimic the texture, appearance, stability, and properties of traditional materials for making personal care and cosmetic products. It is also desirable for such new materials to be more oxidatively stable. Summary of the Invention
[0009] The present disclosure provides an emollient composition comprising a mixture of cocoa butter fatty acid ethyl esters. A personal care formulation comprising the emollient composition is also described herein. The present disclosure further provides a method for producing a composition comprising the cocoa butter fatty acid ethyl esters. The method includes the steps of: (a) providing cocoa butter and ethyl alcohol; and (b) combining the cocoa butter and the ethyl alcohol in the presence of an esterification catalyst at an esterification temperature to obtain the cocoa butter fatty acid ethyl esters. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0010] Explanations of abbreviations and terms used in this disclosure are provided to aid in understanding and practicing the invention.
[0011] Throughout this specification, values expressed in range format should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also all individual numerical values or subranges subsumed within the range as if each numerical value and subrange were explicitly recited. For example, the range "about 0.1% to about 5%" or "about 0.1% to 5%" should be interpreted to include not only about 0.1% to about 5%, but also the individual values (e.g., 1%, 2%, 3% and 4%) and subranges (e.g., 0.1% to 0.5%, 1.1% to 2.2%, 3.3% to 4.4%) within the range recited. The statement "about X to Y" has the same meaning as "about X to about Y" unless otherwise indicated. Similarly, the statement "about X, Y, or about Z" has the same meaning as "about X, about Y, or about Z" unless otherwise indicated.
[0012] All percentages of composition or formulation components referred to herein are disclosed as weight percent (wt%) unless otherwise specified.
[0013] Unless otherwise stated, all parameter ranges disclosed are inclusive of the endpoints and all values therebetween.
[0014] When used in the specification and claims, the terms "comprise" and "comprising" and variations thereof mean that the specified features, steps or integers are included. The terms are not to be interpreted as excluding the presence of other features, steps or components.
[0015] As used herein, the singular forms "a", "an" and "the" and similar referents in the context of describing elements (particularly in the context of the claims that follow) include plural referents unless the context clearly dictates otherwise. For example, reference to "a substituent" encompasses two or more substituents in addition to a single substituent, and so forth. Unless otherwise indicated herein or clearly contradicted by the context, it is understood that any term in the singular form may include its plural counterpart, and vice versa.
[0016] As used herein, the term "or" is used to refer to a non-exclusive "or" unless otherwise indicated. The statement "at least one of A and B" has the same meaning as "A, B, or A and B."
[0017] As used herein, the terms "for example," "for instance," "such as," or "including" are meant to introduce examples that further clarify a more general subject matter. Unless otherwise specified, these examples are provided only as an aid to understanding the applications illustrated in this disclosure and are not meant to be limiting in any way.
[0018] As used herein, the term "about" can allow for a degree of variation within a value or range, for example, within 10%, within 5%, or within 1% of the specified value or within the limits of a specified range, plus or minus, and includes the exact specified value or range.
[0019] As used herein, the term "substantially" refers to a majority or majority portion, such as at least about 50%, 60%, 70%, 80%, 90%, 95%, 96%, 97%, 98%, 99%, 99.5%, 99.9%, 99.99%, or at least about 99.999% or more, or 100%.
[0020] In the methods described herein, unless a temporal or operational order is explicitly recited, acts may be performed in any order without departing from the principles of the present disclosure. Moreover, certain acts may be performed in parallel unless express "claim" language recites them separately. For example, a claimed act of doing X and a claimed act of doing Y may be performed simultaneously in a single operation, with the resulting process falling within the literal scope of the claimed process.
[0021] Representative features are presented in the following description, which may be used alone or in any combination with one or more features disclosed elsewhere in the description and / or drawings herein.
[0022] As used herein, the term "fatty acid" may refer to a molecule that includes a hydrocarbon chain and a terminal carboxylic acid group. As used herein, the carboxylic acid group of a fatty acid may be modified or esterified (e.g., COOR, where R refers to, for example, a carbon atom), such as occurs when the fatty acid is incorporated into a glyceride or another molecule. Alternatively, the carboxylic acid group may be in the form of a free fatty acid or a salt (i.e., COO" or COOH). The "tail" or hydrocarbon chain of a fatty acid may also be referred to as a fatty acid chain, a fatty acid side chain, or a fatty chain. The hydrocarbon chain of a fatty acid is typically a saturated or unsaturated aliphatic group. A fatty acid with N carbon atoms typically has a fatty acid side chain with N-1 carbons.
[0023] The term "acylglyceride" as used herein refers to a molecule having at least one glycerol moiety with at least one fatty acid residue linked via an ester bond. For example, acylglyceride can include monoacylglyceride, diacylglyceride, triacylglyceride. The group of acylglycerides can be further narrowed down by additional descriptive terms and modified to explicitly exclude or include certain subsets of acylglycerides. For example, the phrases mono- and di-acylglyceride refer to MAG (monoacylglyceride) and DAG (diacylglyceride), while the phrase non-MAG / non-DAG acylglyceride refers to the group of acylglycerides excluding MAG and DAG.
[0024] A "fatty acid residue" is a fatty acid in its acyl or esterified form.
[0025] The concentration of a particular type of fatty acid may be provided herein as a percentage of the total fatty acid content of the oil. Unless otherwise specified, such percentage is a weight percentage based on total fatty acids, including empirically calculated free and esterified fatty acids.
[0026] A "saturated" fatty acid is one that does not contain any carbon-carbon double bonds in the hydrocarbon chain. For example, stearic acid (C18:0) is a saturated fatty acid with a chain of 18 carbons with no carbon-carbon double bonds. An "unsaturated" fatty acid contains one or more carbon-carbon double bonds. For example, oleic acid (C18:1) is an unsaturated fatty acid with a chain of 18 carbons with one carbon-carbon double bond. A "polyunsaturated" fatty acid contains one or more such carbon-carbon double bonds, while a "monounsaturated" fatty acid contains only one carbon-carbon double bond. The carbon-carbon double bonds may be in one of two configurations, designated cis and trans. Naturally occurring unsaturated fatty acids are generally in the "cis" form.
[0027] Non-limiting examples of fatty acids include C14, C16 (e.g., C16:0, C16:1), C18 (e.g., C18:0, C18:1, C18:2, C18:3, C18:4), C20 (e.g., C20:0, C20:1, C20:2, C20:3, C20:4, C20:5), C22 (e.g., C22:0, C22:1, C22:2, C22:3, C22:4, C22:5, C22:6), and C24 (e.g., C24:0, C24:1, C24:2, C24:3, C24:4, C24:5, C24:6, C24:7) fatty acids. For example, the fatty acids can be myristic acid (14:0), palmitic acid (16:0), stearic or isostearic acid (18:0), oleic acid (18:1), linoleic acid (18:2), alpha-linolenic acid (18:3).
[0028] As used herein, the term "C14-C24 fatty acid" refers to a fatty acid containing 14 to 24 carbons. The C14-C24 fatty acid can be straight chain or branched chain. In some embodiments, the C14-C24 fatty acid is a C16 or C18 fatty acid.
[0029] The C14 to C24 fatty acid may be a mixture of C14 to C24 fatty acids.
[0030] The term "ethyl ester" refers to a fatty acid containing 14 to 24 carbons esterified with an ethyl group.
[0031] The fatty acid composition of an oil can be determined by methods known in the art. The American Oil Chemists' Society (AOCS) maintains analytical methods for a wide variety of tests performed on vegetable oils. Hydrolysis of oil constituents to produce free fatty acids, conversion of the free fatty acids to methyl esters, and analysis by gas-liquid chromatography (GLC) is a generally accepted standard method for determining the fatty acid composition of an oil sample. AOCS Procedure Ce 1-62 describes the procedure used.
[0032] The term "esterification or esterified" means that an ester bond is formed, including: 1) a dehydration reaction between an alcohol and an acid; 2) transesterification, the reaction of an alcohol with an ester to form a new ester; or 3) transesterification, rearrangement of a fatty acid within a triacylglycerol structure.
[0033] As used herein, "cocoa butter" refers to triacylglycerides (triglycerides or triacylglycerols) derived from a mixture of fatty acids derived from the seeds of the cocoa plant. Non-limiting examples of fatty acids in cocoa butter include C14 (e.g., C14:0), C16 (e.g., C16:0, C16:1), C18 (e.g., C18:0, C18:1, C18:2, C18:3), C20 (e.g., C20:0, C20:1), C22 (e.g., C22:0), and C24 (e.g., C24:0) fatty acids. In one embodiment, the cocoa butter has a fatty acid profile including, but not limited to, myristic acid (C14:0), palmitic acid (C16:0), palmitoleic acid (C16:1), stearic acid (C18:0), oleic acid (C18:1), linoleic acid (C18:2), alpha-linolenic acid (C18:3), arachidic acid (C20:0), paulic acid (C20:1), behenic acid (C22:0), and lignoceric acid (C24:0).
[0034] As used herein, "cocoa butter fatty acid ethyl esters" or "cocoa butter ethyl esters (CBEEs)" refers to cocoa butter fatty acids containing 14 to 24 carbons (C14 to C24 fatty acids) esterified with an ethyl group.
[0035] The term "emollient" as used herein refers to a composition or product that softens, smoothes, and moisturizes the skin by building and / or replenishing the skin barrier, repairing and filling skin cracks, and relieving roughness and redness caused by dry skin and other conditions (e.g., eczema, psoriasis). Thus, it prevents moisture loss from the skin, relieves dry skin, protects the skin, and keeps the skin healthy. Emollients may include synthetic compounds (e.g., mineral oil) and / or natural compounds (e.g., vegetable oils). Emollients may be, but are not limited to, lotions, creams, and ointments, depending on the water-to-oil ratio.
[0036] In one aspect, the emollient is a vegetable oil and / or vegetable fat such as cocoa butter. In another aspect, the emollient comprises an ester derived from cocoa butter fatty acids, including but not limited to, cocoa butter fatty acid ethyl esters. In another aspect, the emollient comprises an ester derived from cocoa butter fatty acids, including but not limited to, cocoa butter fatty acid ethyl esters.
[0037] The term "personal care formulation or personal care product" means and includes any cosmetic, hygiene, toiletry, skin care and topical care products, including, but not limited to, leave-on products (i.e., products that are left on the keratin substrate after application), rinse-off products (i.e., products that are washed or rinsed off from the keratin substrate during or within minutes of application), shampoos; hair curling and straightening products; hairstyle maintenance and hair conditioning products; lotions and creams for the nails, hands, feet, face, scalp and / or body; hair dyes; face and body make-up; nail care products; astringents; deodorants; antiperspirants; anti-acne medications; anti-aging; depilatories; colognes and fragrances; skin protection creams and lotions (such as sunscreens); skin and body cleansers; skin conditioners; skin toners; skin tightening compositions; skin tanning and whitening compositions; liquid soaps; bar soaps; bath products; and shaving products.
[0038] The texture of such personal care formulations or personal care products may be, but is not limited to, liquids, gels, sprays, emulsions (such as lotions and creams), shampoos, pomades, foams, tablets, sticks (such as lip care products), make-up, among others, any of which may be applied to the skin or hair and are typically designed to remain in contact therewith until removed, such as by rinsing with water or washing with shampoo or soap. Other forms may be gels, which may be soft, hard or squeezable. Sprays may be non-pressurized aerosols delivered from hand-pumped finger-actuated sprayers, or pressurized aerosols such as mousses, sprays or foam-forming formulations where chemical or gaseous propellants are used.
[0039] The topical formulations including the emollient compositions disclosed herein may be creams used in skin care applications.
[0040] The formulations prepared using the compositions disclosed herein generally have a white or pale white color that is considered aesthetically pleasing. In some cases, the formulations of the present invention may be further processed to produce a colored final product. In such cases, the white color is beneficial because it allows additional pigments to stand out without affecting the final color.
[0041] Furthermore, the formulation prepared using the composition disclosed herein has acceptable oil content and good spreadability, and does not leave a greasy residual feeling on skin.This texture feels comfortable to touch and apply.Furthermore, the consistency is such that good product pick-up can be achieved.Good product pick-up means that the user's fingers can collect enough product (i.e., not too much, not too little).
[0042] The compositions of the present disclosure are particularly useful in sunscreen applications. Sunscreens contain ingredients intended to block ultraviolet light from reaching the skin. The UV blockers or sunscreens can be physical or chemical salts, such as ZnO, or TiO2, or chemicals (maximum approved levels are given), such as avobenzone (3%), homosalate (15%), butyl methoxydibenzoylmethane (5%), octocrylene (10%), titanium dioxide (25%), ethylhexyl salicylate (5%), ethylhexyl methoxycinnamate (10%), bis-ethylhexyloxyphenol methoxyphenyl triazine (10%). The compositions of the present disclosure can be used with any type of UV blocker or sunscreen known in the art, or a mixture of UV blockers or sunscreens.
[0043] Emollient Composition The emollient compositions described herein comprise a mixture of cocoa butter fatty acid ethyl esters (CBEEs). In one embodiment, the CBEEs have the fatty acid ethyl ester profile shown in Table 1.
[0044] [Table 1]
[0045] In one embodiment, the CBEE comprises from about 15% to about 30%, from about 20% to about 30%, or from about 24% to about 27% palmitic acid ethyl ester.
[0046] In one embodiment, the CBEE comprises from about 25% to about 40%, from about 30% to about 40%, or from about 34% to about 37% ethyl stearate.
[0047] In one embodiment, the CBEE comprises from about 25% to about 40%, from about 30% to about 38%, or from about 31% to about 34% oleic acid ethyl ester.
[0048] In one embodiment, the CBEE comprises about 15% to about 30% palmitic acid ethyl ester, about 25% to about 40% stearate ethyl ester, and about 25% to about 40% oleic acid ethyl ester. In one embodiment, the CBEE comprises about 24% to about 27% palmitic acid ethyl ester, about 34% to about 37% stearate ethyl ester, and about 31% to about 34% oleic acid ethyl ester.
[0049] In one embodiment, the CBEE comprises about 55% to about 75%, about 60% to about 70%, about 60% to about 65%, or about 61% to about 63% saturated fatty acid ethyl esters. In one embodiment, the CBEE comprises about 62% saturated fatty acid ethyl esters.
[0050] In one embodiment, the emollient composition comprises greater than 50%, greater than 75%, greater than 90%, greater than 95%, or greater than 99% CBEE. In another embodiment, the amount of CBEE in the emollient composition ranges from about 50% to about 99%, about 75% to about 99%, about 90% to about 99%, about 95% to about 99%, about 95% to about 99%, about 95% to about 99.3%, about 95% to about 99.5%, or about 99.3% to about 99.5%. In another embodiment, the amount of CBEE in the emollient composition is about 99.3% or about 99.5.
[0051] In one embodiment, the emollient composition may be blended with other emollients, such as natural emollients, synthetic emollients, and / or petroleum-based emollients.
[0052] In one aspect, the CBEE produced by the methods described herein has a clear liquid or semi-fluid appearance and light texture. Additionally, the CBEE is non-sticky while having good spreadability, providing a smooth and silky effect. These properties make the CBEE a good candidate for applications such as personal care products and cosmetics. For example, the CBEE can be added to lotions, creams, or skin care products at a loading level of 1-15%. In another example, the CBEE can be added to anhydrous balms or sticks at a loading level of 1-30%. In yet another example, the CBEE can be added to hair care products at a loading level of 1-10%.
[0053] In another embodiment, the CBEE has a viscosity, as determined by a Brookfield viscometer, of about 19,300 MPa.s.
[0054] Personal Care Formulations The personal care formulations described herein include an emollient composition, the emollient composition comprising a mixture of cocoa butter fatty acid ethyl esters (CBEEs). In another embodiment, the CBEEs have a fatty acid ethyl ester profile as shown in Table 1.
[0055] In one embodiment, the personal care formulations described herein can contain any useful amount of the CBEE of the present disclosure. In one embodiment, the content of CBEE in the personal care formulation ranges from 1% to 100%, 10% to 50%, 15% to 45%, 20% to 40%, 22% to 38%, or 25% to 35% by weight. In one embodiment, the content of CBEE in the personal care formulation is 30% by weight.
[0056] Method for producing cocoa butter fatty acid ethyl ester The process for producing cocoa butter fatty acid ethyl esters described herein involves the esterification of cocoa butter with ethyl alcohol to obtain a mixture of esters.
[0057] In one aspect, the method includes the steps of (a) providing cocoa butter and ethyl alcohol; and (b) esterifying the cocoa butter with the ethyl alcohol in the presence of an esterification catalyst at an esterification temperature to obtain cocoa butter fatty acid ethyl esters.
[0058] The esterification of triglyceride vegetable oils is well known in the art, for example in the preparation of biodiesel. Typically, the oil is mixed with an excess of alcohol and heated to high temperature in the presence of a catalyst. The catalyst is typically, but not necessarily, a metal salt of the corresponding alcohol. The choice of reaction temperature is related to the alcohol used, and one skilled in the art will choose a temperature that balances the reaction rate with the production of undesirable by-products. In one embodiment, the esterification temperature is about 70° C., the alcohol is ethanol, and the esterification catalyst is sodium ethoxide.
[0059] In one aspect, the method may include additional steps to purify and / or modify the cocoa butter fatty acid ethyl esters. For example, the cocoa butter fatty acid ethyl esters may be desolventized under reduced pressure with nitrogen gas to remove volatiles such as solvents and ethanol. The desolventized cocoa butter fatty acid ethyl esters may be decanted with nitrogen gas, bleached with a bleaching agent, and deodorized with a deodorizing agent or process. These procedures are also well known in the art of vegetable oil refining and are referred to as "refining". These steps can be easily modified or altered depending on the impurities to be removed.
[0060] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. As used herein, each of the following terms has the meaning associated with it as defined below.
[0061] The present invention will be described in more detail by reference to the following experimental examples. These examples are provided for illustrative purposes only and are not intended to be limiting unless otherwise specified. Therefore, the present invention should not be construed as being limited to the following examples in any way, but rather as embracing any and all variations that become evident as a result of the teachings provided herein. EXAMPLES
[0062] Example 1 - Method for producing CBEE Table 2 shows the ingredients for producing CBEEs using the methods described herein.
[0063] [Table 2]
[0064] To produce the ethyl esters (i.e., CBEEs), cocoa butter was first melted and mixed with an excess of 40%-50% ethanol and 1.4% by weight (based on the total weight of cocoa butter and ethanol) of 21% sodium ethoxide catalyst dissolved in ethanol at 70°C with stirring for 120 minutes, or until esterification was complete as determined by the production of ethyl esters by high performance liquid chromatography (HPLC) analysis.
[0065] The CBEE was desolvated under nitrogen flow and reduced pressure until the volatiles present in the CBEE were less than 0.5% as measured by a volatile analyzer (scale oven). The ethanol removed from the CBEE was collected. The desolvated CBEE was decanted with nitrogen gas at 70°C to remove glycerol produced during esterification. An additional glycerol wash was used to further remove glycerol from the ethyl ester phase. The decanted CBEE was bleached with adsorbents (Sorbsil 92, PQ Corporation; and Perform 6000, Oil-Dri Fluids Purification) at 95°C under stirring. The bleached CBEE was deodorized with water at 160-165°C. Finally, the deodorized CBEE was cooled to 70°C and tocopherol (70% tocopherol in vegetable oil base, BASF Covi-Ox T70 EU (non-GM version)) was added to the cooled product.
[0066] Example 2 - Oxidation Stability of CBEE The Oxidative Stability Index (OSI) measures the relative oxidative stability of fatty materials. A sample of CBEE was heated to 110°C under a constant airflow. As the oxidative degradation of the material began, the volatile short chain fractions broke down and became entrapped in the airflow. The short chain fractions were then trapped in distilled water and detected by a conductivity probe to give the OSI reading.
[0067] Table 3 below shows the OSI for CBEE and other fatty substances. OSI values below 20 hours are generally considered unstable.
[0068] [Table 3]
[0069] As can be seen, CBEE has a significantly higher OSI than other fatty acid esters and silicones, which are traditional ingredients for making personal care products. The excellent oxidative stability makes CBEE a good candidate for making personal care products.
[0070] Example 3 - Sunscreen Solubility in CBEE The sunscreen solubility of CBEE, which measures the solubility of sunscreen in fatty materials, is shown in Table 4 below.
[0071] [Table 4]
[0072] Sunscreen solubility was determined by mixing sunscreens at various loading percentages (10-25%), heating the mixture to 70°C, and cooling the heated mixture to room temperature overnight. As observed, CBEE has comparable or better sunscreen solubility to conventional sunscreens, avobenzone and homosalate, as well as other conventional ingredients for making personal care products. The excellent oxidative stability allows CBEE to be a good candidate for making personal care products.
[0073] Example 4 - Skin Care Formulation Table 5 shows skin care formulations in which CBEE is one of the ingredients.
[0074] [Table 5]
[0075] The skin care formulation has a pH adjusted to 5.0-5.5 and the appearance of a viscous white cream. It is stable at room temperature and at 45°C for 2 months.
[0076] Example 5 - Skin Care Formulation Table 6 shows skin care formulations in which CBEE is one of the ingredients.
[0077] [Table 6]
[0078] To prepare the skin care formulation, first, tetrasodium glutamate diacetate was added to deionized water in a first vessel at room temperature with propeller mixing (300-450 rpm). In a second vessel, magnesium aluminum silicate, sclerotium gum, and glycerin were mixed and added to the first vessel at room temperature with propeller mixing (300-450 rpm). The mixture in the second vessel was then heated to 75-80°C to obtain a Phase A mixture.
[0079] In a third vessel, caprylic / capric triglyceride, isononyl isononanoate, CBEE, ethylhexyl salicylate, homosalate, ethylhexyl methoxycrylene, jojoba oil / macadamia seed oil esters (and) squalene (and) phytosteryl macadamiate (and) phytosterols, actic ceramide, tocopherol acetate, glyceryl stearate SE, potassium cetyl phosphate, and polyglycerol-3 beeswax were mixed with propeller agitation (300-450 rpm). The mixture in the third vessel was then heated to 75-80° C. Butyl methoxydibenzoylmethane was added to the mixture in the third vessel at 75-80° C. with propeller agitation (300-450 rpm) to obtain a Phase B mixture.
[0080] The Phase B mixture was added to the Phase A mixture under uniform mixing agitation (3,000-6,000 rpm) at 75-80°C until the two mixtures were uniformly blended to obtain a Phase A / B blend. The Phase A / B blend was further mixed with propeller agitation (300-450 rpm) and cooled to 55-60°C.
[0081] Citric Acid and Phenoxyethanol (and) Ethylhexylglycerin were added to the cooled Phase A / B blend at 55-60° C. under propeller agitation (300-700 rpm). Mixing was stopped when the temperature of the final mixture reached 45-50° C. to obtain the skin care formulation.
[0082] The skin care formulations have a Sun Protection Factor (SPF) of at least 13. The SPF was estimated by the DSM Sunscreen Optimizer, Broad Spectrum (USA) pass.
[0083] Example 6 - Skin Care Formulation Table 7 shows skin care formulations in which CBEE is one of the ingredients.
[0084] [Table 7]
[0085] To prepare the skin care formulation, first tetrasodium glutamate diacetate was added to deionized water in a first vessel with propeller mixing (300-700 rpm). In a second vessel, sclerotium gum and glycerin were mixed with stirring and added to the first vessel with propeller mixing (300-700 rpm). The mixture in the second vessel was then heated to 70-75°C to obtain a Phase A mixture. The Phase A mixture was uniformly mixed at 70-75°C to activate the sclerotium gum. The resulting mixture was heated to 75-80°C with uniform mixing stirring (8,000-8,500 rpm).
[0086] In a third vessel, Caprylic / Capric Triglyceride, Isononyl Isononanoate, CBEE, Ethylhexyl Salicylate, Homosalate, Jojoba Oil / Macadamia Seed Oil Ester (and) Squalene, (and) Phytosteryl Macadamiate, (and) Phytosterol, Actic Ceramide, Tocopherol Acetate, Glyceryl Stearate SE, Potassium Cetyl Phosphate, Polyglycerol-3 Beeswax, and Hectorite (and) Hydroxyethylcellulose were mixed and heated to 75-80°C. Mixing was continued until the ingredients in the mixture were homogeneously blended. Once the mixture was liquid, Butyl Methoxydibenzoylmethane was added to the mixture to minimize the heating time. Phase B mixture was thus obtained.
[0087] The Phase B mixture was added to the Phase A mixture with uniform mixing and stirring (9,000-9,500 rpm) at 70-75°C to obtain a Phase A / B blend. The Phase A / B blend was mixed with a propeller and cooled to 55-60°C with propeller stirring (300-450 rpm).
[0088] Citric acid was added to the cooled Phase A / B blend at 55-60°C and phenoxyethanol (and) ethylhexylglycerin was added with propeller agitation (500-700 rpm) at 50-55°C to obtain the Phase A / B / C blend. The citric acid diluted the emulsion and was recovered with rapid mixing.
[0089] The weight of Phase A / B / C blend is adjusted with warm water at 50-55° C. Mixing is stopped when the temperature of the final mixture reaches 45-50° C. or when the final mixture becomes solid to obtain the skin care formulation.
[0090] The skin care formulations have a Sun Protection Factor (SPF) of at least 13. The SPF was estimated by the DSM Sunscreen Optimizer, Broad Spectrum (USA) pass.
[0091] Example 7 - Skin Care Formulation Table 8 shows skin care formulations in which CBEE is one of the ingredients.
[0092] [Table 8]
[0093] To prepare the skin care formulations, deionized water was heated to 70° C. and glycerin was added to the heated deionized water with stirring (200 rpm) to obtain a Phase A mixture. Sclerotium gum was added to the Phase A mixture using a Silverson homogenizer at 5000 rpm for 5 minutes to obtain a Phase A / B blend.
[0094] CBEE, polyglycerol-3 stearate, sodium stearoyl lactylate, glyceryl stearate SE, and cetearyl alcohol were mixed and heated to 70°C to obtain a Phase C mixture. The Phase C mixture was added to the Phase A / B blend and the resulting mixture was mixed with a Silverson homogenizer at 4000 rpm for 5 minutes to obtain a Phase A / B / C blend. The Phase A / B / C blend was cooled with propeller agitation (300-600 rpm).
[0095] Benzyl alcohol (and) salicylic acid (and) glycerin (and) sorbic acid were added to the cooled Phase A / B / C blend with propeller agitation (300-600 rpm) at 50° C. The pH of the resulting skin care formulation was adjusted to 5.0-5.5 by the addition of sodium hydroxide solution.
[0096] Example 8 - Skin Care Formulation Table 9 shows skin care formulations in which CBEE is one of the ingredients.
[0097] [Table 9]
[0098] To prepare the skin care formulations, jojoba esters (saturated esters), jojoba esters (mixture of diene, monoene and saturated esters), corn (maize) starch, tocopherol, fragrance, mica (and) titanium dioxide (and) carmine were heated in a water bath to 75-80°C. The heated ingredients were mixed with CBEE preheated in an oven or water bath at 45-50°C in a rotor-stator mixer (IKA Ultra Turrax T25, S25N-25G workhead) at 6000 rpm for 1 minute until a clear homogenous phase was obtained. The mixture was poured into moulds. The moulded mixture was left at room temperature for 5 minutes and either stored in a freezer (-18°C) for 10 minutes or left at room temperature for 30 minutes before being removed from the moulds and packaged to obtain the skin care formulations.
[0099] Example 9 - Hair Care Formulation Table 10 shows hair care formulations in which CBEE is one of the ingredients.
[0100] [Table 10]
[0101] To prepare the hair care formulation, deionized water, glycerin, sclerotium gum, hydroxypropyl starch phosphate, and sodium starch octenyl succinate and hydroxypropyl starch phosphate were mixed under a Silverson homogenizer at 7000 rpm for 7 minutes to obtain a Phase A mixture.
[0102] Coconut oil and CBEE were mixed in a separate container and heated to 50° C. with slow mixing until both ingredients were completely melted to obtain Phase B mixture.
[0103] The Phase B mixture was mixed with the Phase A mixture for 10 minutes using a scraper mixing at 70 rpm to obtain a Phase A / B blend. The Phase A and Phase B mixtures could also be blended manually using a spatula followed by high shear mixing under a Silverson homogenizer at 5000-7000 rpm to obtain a Phase A / B blend. The Phase A / B blend was further mixed with a propeller mixer at low mixing (approximately 800-1200 rpm) to avoid trapping air bubbles.
[0104] Using a propeller mixer, phenoxyethanol, tocopheryl acetate, and mica were added one by one to the Phase A / B blend. Deionized water was added to make up for the water lost during the process to obtain the hair care formulation.
[0105] The hair care formulation has a pH adjusted to 4.5 to 5.5 and a viscosity of about 13500 cP.
[0106] In addition to the uses described above, the cocoa butter fatty acid ethyl esters described herein can be used as ingredients in products including, but not limited to, skin care products, sun care products, hair care products (e.g., shampoos, conditioners), makeup products, and the like.
Claims
1. An emollient composition comprising a mixture of cocoa butter fatty acid ethyl esters.
2. 10. The emollient composition of claim 1 comprising greater than 90% cocoa butter fatty acid ethyl esters.
3. 10. The emollient composition of claim 1, wherein said cocoa butter fatty acid ethyl esters have from about 60% to about 70% saturated fatty acid ethyl esters.
4. 13. A personal care formulation comprising the emollient composition of claim 1.
5. 5. The personal care formulation of claim 4, wherein the cocoa butter fatty acid ethyl ester content is from 20% to 40%.
6. 5. The personal care formulation of claim 4, further comprising one or more of sclerotium gum, glycerin, an emulsifier, a preservative, and sodium hydroxide.
7. 5. The personal care formulation of claim 4 further comprising a sunscreen.
8. 5. The personal care formulation of claim 4, further comprising one or more of a fragrance, an active, a preservative, and a colorant.
9. 5. The personal care formulation of claim 4, wherein the personal care formulation is selected from the group consisting of skin protectant creams, lotions, sunscreens, skin or body cleansers, skin conditioners, skin toners, shampoos, hair conditioners, and skin tightening compositions.
10. 1. A method for producing a composition comprising cocoa butter fatty acid ethyl esters, the method comprising: a. providing cocoa butter and ethyl alcohol; b) mixing said cocoa butter with said ethyl alcohol in the presence of an esterification catalyst at an esterification temperature to obtain said cocoa butter fatty acid ethyl esters.
11. 11. The method of claim 10, wherein the esterification temperature is about 70°C.