Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are described herein. For the purposes of the present invention, the following terms are defined below.
The term "about" as used herein refers to an amount, level, value, dimension, size, or use that may differ by up to 30%, 20%, or 10% from the amount, level, value, dimension, size, or use of a reference. The percentages used herein are by weight unless otherwise indicated.
Throughout the specification and claims which follow, unless the context requires otherwise, the word "comprise", and variations such as "comprises" and "comprising", will be understood to imply the inclusion of a stated integer or step or group of integers or steps but not the exclusion of any other integer or step or group of integers or steps.
According to the present invention, the term "cosmetic" refers to a chemical industry or fine chemical product that is spread on any part of the surface of the human body, such as skin, hair, nails, lips, teeth, etc., in order to clean, maintain, beautify, modify and change the appearance, or correct the smell of the human body, in order to maintain a good state.
Composition of lamellar liquid crystal structure
The invention relates to a composition capable of forming a liquid crystal structure based on fatty acid, glycerol laurate and potassium hydroxide, which has good thickening effect and good stability. The composition can be used for personal care products, and has excellent product use performance.
Compared with the prior art, the invention has the advantages that: without liquid crystal emulsifier and thickener, in the presence of fatty acid: 0.5-10 parts of glycerol laurate: 0.1-15 parts of potassium hydroxide: 0.01-3 parts of a composition: fatty acid: glycerol laurate (mass ratio) =3:1-1:2, fatty acid: potassium hydroxide (weight ratio) =5:1-41:1 the composition can form a large number of clear lamellar network structures (maltese cross), provide excellent viscosity and improve high temperature stability of the product.
Therefore, the invention provides a novel composition containing lamellar liquid crystal, which can prepare a lamellar liquid crystal network structure without adding a liquid crystal emulsifier and a thickening agent, has clear maltese cross pattern, and can provide good viscosity for a system and improve the stability of a product. After the product with the liquid crystal structure is smeared on the surface layer of the skin, the product has certain advantages in improving the hydration degree of the horny layer, keeping moisture for a long time, repairing the barrier function of damaged skin and even promoting the penetration of functional substances into the horny layer compared with the conventional preparation.
The present invention provides a composition having a lamellar liquid crystal structure, the composition comprising:
0.5-10% by weight of fatty acids;
0.1-15% by weight of glycerol laurate;
0.01-3 wt% potassium hydroxide; and
A carrier acceptable in the personal care product arts;
Wherein, fatty acid: the weight ratio of the glycerol laurate is 3:1-1:2;
Wherein, fatty acid: the weight ratio of potassium hydroxide is 5:1-41:1.
In the composition having a liquid crystal structure according to the present invention, the composition comprises 1 to 10 wt% of fatty acid, preferably 2 to 10 wt%, 3 to 10 wt%, 4 to 10 wt%, 5 to 10 wt%, 6 to 10 wt% of fatty acid, based on the total weight of the composition.
In the composition having a liquid crystal structure of the present invention, the fatty acid may be dodecanoic acid, tetradecanoic acid, or a combination thereof.
In the composition having a liquid crystal structure according to the present invention, the composition comprises 0.5 to 15% by weight of glycerol laurate, preferably 1 to 15% by weight, 1 to 10% by weight, 2 to 10% by weight, 5 to 10% by weight of glycerol laurate, based on the total weight of the composition.
In the composition having a liquid crystal structure according to the present invention, the composition contains 0.01 to 3 wt% of potassium hydroxide, preferably 0.1 to 3 wt%, 0.1 to 2wt% of potassium hydroxide, based on the total weight of the composition. In a preferred embodiment, the composition comprises 0.27 to 1.36 weight percent potassium hydroxide.
In a preferred embodiment, the total amount of fatty acids and glycerol laurate in the composition of the invention having a liquid crystalline structure is not less than 2% by weight, more preferably not less than 7% by weight.
In a preferred embodiment, the weight ratio of fatty acid to glycerol laurate in the composition with liquid crystal structure according to the invention is 3:1-1:2. In some embodiments, the weight ratio of fatty acid to glycerol laurate in the composition is 3:1 to 2:1. In some embodiments, the weight ratio of fatty acid to glycerol laurate in the composition is from 2:1 to 1:2.
In a preferred embodiment, the weight ratio of fatty acid to potassium hydroxide in the composition of the present invention having a liquid crystal structure is 5:1 to 41:1. In a preferred embodiment, the weight ratio of fatty acid to potassium hydroxide in the composition of the present invention having a liquid crystal structure is from 8:1 to 41:1. In some embodiments, the weight ratio of fatty acid to potassium hydroxide in the composition is from 5:1 to 10:1.
In some embodiments, the amount ratio of fatty acid to potassium hydroxide in the composition is from 10:7 to 10:1. In some embodiments, the amount ratio of fatty acid to potassium hydroxide in the composition is from 10:5 to 10:1.
In the present invention, the composition having a liquid crystal structure is disposed in an aqueous system. For example, the carrier employed in the composition may be any aqueous system known in the art, including but not limited to: deionized water and distilled water.
The invention also relates to a method for preparing a composition having a liquid crystal structure, said method comprising:
(a) Mixing fatty acid, potassium hydroxide and carrier, heating and dissolving;
(b) Adding glycerol laurate to complement the carrier;
(c) Cooling to obtain the liquid crystal structure composition.
In some embodiments, step (a) is heated to a temperature of 75-90 ℃, preferably to 80-85 ℃.
Accordingly, the present invention provides a skin care composition having a liquid crystal structure which can be obtained by a simple preparation process, and such an aqueous system prepared according to a given formulation and preparation method has a liquid crystal structure and can provide an effective moisturizing and skin care effect.
External preparation for skin
The composition with the liquid crystal structure can be used for preparing external preparations for skin. The skin external preparation is preferably a cosmetic composition including, but not limited to, products in the form of face cream, milky lotion, jelly, lotion, essence, pack, eye cream, aerosol (cleansing foam), spray, body wash, facial cleanser, and the like.
The content of the composition having a liquid crystal structure in the skin external preparation is 0.0001 to 20% by weight, preferably 0.001 to 10% by weight, more preferably 0.01 to 5% by weight.
The external skin preparation is a general concept of all ingredients commonly used outside the skin, and may be, for example, a cosmetic composition. The cosmetic composition may be basic cosmetic, facial makeup cosmetic, body cosmetic, hair care cosmetic, etc., and its dosage form is not particularly limited and may be reasonably selected according to different purposes. The cosmetic composition also contains various cosmetically acceptable medium or matrix excipients depending on dosage form and purpose.
The skin external agent comprising the composition having a liquid crystal structure may be topically applied to human skin and/or hair. The skin external preparation may further comprise a cosmetically acceptable topical carrier, which may be about 50% to about 99.99% by weight of the skin external preparation (e.g., about 80% to about 99% by weight of the skin external preparation). In a preferred embodiment of the invention, the cosmetically acceptable topical carrier comprises water. The cosmetically acceptable topical carrier may include one or more materials selected from the group consisting of moisturizers, emollients, oils, humectants, and the like. In one embodiment, the cosmetically acceptable topical carrier includes a substrate such as a nonwoven or film material.
Skin external preparations may be formulated into a variety of product types including, but not limited to, lotions, creams, gels, sticks, sprays, ointments, cleansing liquid lotions and solid soaps, shampoos and hair conditioners, hair fixatives, pastes, foams, powders, mousses, shave creams, wipes, patches, hydrogels, film-forming products, masks and skin films, films and cosmetics such as foundations and mascaras. These product types may contain several types of cosmetically acceptable topical carriers including, but not limited to, solutions, suspensions, emulsions (e.g., microemulsions and nanoemulsions), gels, solids, and liposomes.
The external skin preparation comprising the composition having a liquid crystal structure can be formulated as a solution. The solution typically comprises an aqueous or organic solvent (e.g., about 50% to about 99.99% or about 90% to about 99% of a cosmetically acceptable aqueous or organic solvent). Examples of suitable organic solvents include propylene glycol, polyethylene glycol, polypropylene glycol, glycerol, 1,2, 4-butanetriol, sorbitol esters, 1,2, 6-hexanetriol, ethanol and mixtures thereof.
The skin external preparation may be formulated as a solution containing an emollient. Such skin external preparations preferably comprise from about 2% to about 50% of one or more emollients. As used herein, "emollient" refers to a substance used to prevent or reduce dryness, for example, by preventing the loss of skin moisture through the skin. Examples of emollients include, but are not limited to, vegetable oils, mineral oils, aliphatic esters, and the like.
Lotions can be prepared from such solutions. Lotions typically contain from about 1% to about 20% (e.g., from about 5% to about 10%) of one or more emollients and from about 50% to about 90% (e.g., from about 60% to about 80%) of moisture.
Another type of product that can be formulated from solutions is a cream. A cream typically contains from about 5% to about 50% (e.g., from about 10% to about 20%) of one or more emollients and from about 45% to about 85% (e.g., from about 50% to about 75%) of moisture.
Although it is preferable that the skin external agent comprising the composition having a liquid crystal structure comprises water, the skin external agent may alternatively be anhydrous or an ointment that does not comprise water but is an organic and/or silicone solvent, grease, lipid, and wax. Ointments may contain simple bases of animal or vegetable oils or semi-solid hydrocarbons. Ointments may contain from about 2% to about 10% of one or more emollients and from about 0.1% to about 2% of one or more thickeners.
The skin external preparation can be formulated as an emulsion. If the topical carrier is an emulsion, from about 1% to about 10% (e.g., from about 2% to about 5%) of the topical carrier contains one or more emulsifying agents. The emulsifier may be nonionic, anionic or cationic. Examples of suitable emulsifiers include those commonly identified as suitable emulsifiers in the personal care and cosmetic formulations arts.
Lotions and creams can be formulated as emulsions. Typically such lotions contain from 0.5% to about 5% of one or more emulsifying agents. Such creams typically contain from about 1% to about 20% (e.g., from about 5% to about 10%) of one or more emollients; about 20% to about 80% (e.g., 30% to about 70%) water; and from about 1% to about 10% (e.g., from about 2% to about 5%) of one or more emulsifiers.
Oil-in-water and water-in-oil single emulsion skin care formulations, such as lotions and creams, are well known in the cosmetic arts and can be used in the present invention. Multiple emulsion skin external preparations (e.g., water-in-oil-in-water and oil-in-water) are also useful in the present invention. Typically, such single-phase or multiple-phase emulsions contain moisture, emollients, and emulsifiers as their essential ingredients.
The skin external agent comprising the composition having a liquid crystal structure may also be formulated as a gel (for example, an aqueous gel, an alcoholic gel, an alcohol/water gel, or an oily gel using a suitable gelling agent). Suitable gelling agents for aqueous and/or alcoholic gels include, but are not limited to, natural gums, acrylic acid and acrylate polymers and copolymers, and cellulose derivatives (e.g., hydroxymethyl cellulose and hydroxypropyl cellulose). Suitable gellants for oils (e.g., mineral oils) include, but are not limited to, hydrogenated butene/ethylene/styrene copolymers and hydrogenated ethylene/propylene/styrene copolymers. Such gels typically contain between about 0.1% and 5% by weight of such gelling agents.
External preparations for skin comprising a composition having a liquid crystal structure may also be formulated as solid preparations (e.g., wax-based sticks, bar soaps, powders, or wipes containing powders).
In addition to the above components, the skin external preparations usable in the present invention may contain various other oil-soluble substances and/or water-soluble substances which are conventionally used in skin external preparations for use on the skin and hair at levels determined in the technical field thereof.
The skin external agent of the present invention may contain additional components commonly found in skin care compositions, such as emollients, skin conditioning agents, emulsifiers, preservatives, antioxidants, fragrances, chelating agents, and the like, as long as they are physically and chemically compatible with the other components in the skin external agent and do not affect the effects of the composition having a liquid crystal structure of the present invention.
In some embodiments of the skin external preparation of the present invention, one or more preservatives may be used. Suitable preservatives include p-hydroxyacetophenone, alkyl C1-C4 p-hydroxybenzoates and phenoxyethanol. The preservative is used in an amount of about 0.5 to about 2 wt%, preferably about 0.5 to 1 wt%, based on the total weight of the composition.
In one example of the skin external agent of the present invention, one or more antioxidants may be used. Suitable antioxidants include Butylated Hydroxytoluene (BHT), ascorbyl palmitate (BHA), butylated hydroxyanisole, phenyl-alpha-naphthylamine, hydroquinone, propyl gallate, nordihydroguaiaretic acid, vitamin E or derivatives of vitamin E, vitamin C and its derivatives, calcium pantothenate, green tea extracts and mixed polyphenols, and mixtures of the foregoing. The antioxidants are used in an amount ranging from about 0.02 to 0.5 weight percent, more preferably from about 0.002 to 0.1 weight percent, based on the total weight of the composition.
In one example of the skin external agent of the present invention, one or more emollients may be used which act as lubricants to reduce flaking and improve the appearance of the skin by their ability to remain on the skin surface or in the stratum corneum. Typical emollients include fatty esters, fatty alcohols, mineral oils, polyether siloxane copolymers, and the like. Examples of suitable emollients include, without limitation, polypropylene glycol ("PPG") -15 stearyl ether, PPG-10 cetyl ether, steareth-10, oleth-8, PPG-4 lauryl ether, vitamin E acetate, lanolin, cetyl alcohol, cetostearyl alcohol ethyl hexanoate, cetostearyl alcohol, glyceryl stearate, octyl hydroxystearate, dimethylpolysiloxane, and combinations thereof. Cetyl alcohol, cetostearyl alcohol ethyl hexanoate, cetostearyl alcohol, glycerol stearate, and combinations thereof are preferred. When used, the emollient is in an amount ranging from about 0.1 to about 30 weight percent, preferably from about 1 to about 30 weight percent, based on the total weight of the composition.
In one example of the skin external agent of the present invention, one or more moisturizers may be used. Humectants, also known as humectants, help to enhance the effectiveness of emollients, reduce flaking, stimulate removal of constituent scales and enhance skin feel. Polyols may be used as humectants including, but not limited to, glycerin, polyalkylene glycols, alkylene polyols and derivatives thereof, including butylene glycol, propylene glycol, dipropylene glycol, polyglycerol, polyethylene glycol and derivatives thereof, sorbitol, hydroxypropyl sorbitol, hexylene glycol, 1, 3-dibutylene glycol, 1,2, 6-hexanetriol, ethoxylated glycerin, propoxylated glycerin and combinations thereof. When used, the humectant is present in an amount of about 0.1 to about 20 weight percent, preferably about 1 to about 15 weight percent, based on the total weight of the composition.
In one example of the skin external agent of the present invention, one or more emulsifying agents may be used. The emulsifier may be used in an effective stabilizing amount. Preferably, the emulsifier is used in an amount of about 1.0 to about 10.0 wt%, more preferably about 3.0 to about 6.0 wt%, based on the total weight of the composition. Any emulsifier that is compatible with the components of the composition may be used. Suitable emulsifiers include stearic acid, cetyl alcohol, glyceryl stearate, lecithin, stearyl alcohol, steareth-2, steareth-20, acrylic/C10-30 alkanol acrylate cross-linked polymers, and combinations thereof.
In one example of the skin external agent of the present invention, one or more pH adjusting agents may be used. The pH adjuster useful in the skin external preparation of the present invention includes tromethamine. When used, the pH adjustor is used in an amount of about 0.1 to about 2 weight percent, preferably about 0.1 to about 1 weight percent, based on the total weight of the composition.
In one embodiment of the present invention, the skin external preparation comprises acrylic/C10-30 alkanol acrylate cross-linked polymer, glycerol, p-hydroxyacetophenone, glycerol stearate and lecithin, cetyl/stearyl alcohol, cetostearyl alcohol ethyl hexanoate, tromethamine or combinations thereof.
Examples
The invention will be further illustrated by the following examples. It is noted herein that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, since many insubstantial modifications and variations will become apparent to those skilled in the art in light of the above teachings. The test methods in the following examples, in which specific conditions are not specified, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. All percentages and parts are by weight unless otherwise indicated.
The experimental materials used in the following examples are as follows:
Dodecanoic acid, trade name: the composition of the lauric acid, purchased from Fengyi oil technology (Lianyong) Inc.;
Tetradecanoic acid, trade name: myristic acid, purchased from the company of the oil science and technology of Fengyi (Liyun harbor);
hexadecanoic acid, trade name: c16-98MY, purchased from Emery Oleochemicals (M) Sdn Bhd;
octadecanoic acid, trade name: baomele stearic acid A9218, available from Talco brown (Zhangjihong Kong) Co., ltd;
Glycerol laurate, trade name: 90-L12, available from Basiff (China) Co., ltd;
Potassium hydroxide (90%), high quality flake potassium hydroxide, commercially available from wafery chemistry (chang) limited.
Example 1: preparation of lauric acid and glycerol laurate composition
Weighing 10 parts by mass of dodecanoic acid and 1.55 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until all the components are dissolved, adding 5 parts by mass of glycerol laurate, complementing the rest components to 100 by deionized water, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 2: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 1.36 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 3: preparation of hexadecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of hexadecanoic acid and 1.22 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until all the hexadecanoic acid and the potassium hydroxide are dissolved, adding 5 parts by mass of glycerol laurate, complementing the rest with deionized water to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 4: preparation of stearic acid and glycerol laurate composition
Weighing 10 parts by mass of stearic acid and 1.09 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until all the components are dissolved, adding 5 parts by mass of glycerol laurate, complementing the rest components to 100 by deionized water, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 5: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 0.66 mass part of tetradecanoic acid and 0.09 mass part of potassium hydroxide, adding into a beaker containing 75 mass parts of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 0.33 mass part of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 6: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 1.32 parts by mass of tetradecanoic acid and 0.18 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 0.66 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 7: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 2 parts by mass of tetradecanoic acid and 0.27 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 1 part by mass of glycerol laurate, complementing the rest with deionized water to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 8: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 2.66 parts by mass of tetradecanoic acid and 0.36 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 1.33 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 9: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 3.33 parts by mass of tetradecanoic acid and 0.45 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ at a rotating speed of 200rpm until the materials are completely dissolved, adding 1.66 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 10: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 4 parts by mass of tetradecanoic acid and 0.55 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 2 parts by mass of glycerol laurate, complementing the rest with deionized water to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 11: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 4.66 parts by mass of tetradecanoic acid and 0.64 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ at a rotating speed of 200rpm until the materials are completely dissolved, adding 2.33 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 12: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 5.33 parts by mass of tetradecanoic acid and 0.73 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ at a rotating speed of 200rpm until the materials are completely dissolved, adding 2.66 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 13: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 6 parts by mass of tetradecanoic acid and 0.82 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until all the materials are dissolved, adding 3 parts by mass of glycerol laurate, complementing the rest with deionized water to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 14: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 3 parts by mass of tetradecanoic acid and 0.41 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ at a rotating speed of 200rpm until all the materials are dissolved, adding 12 parts by mass of glycerol laurate, complementing the rest with deionized water to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 15: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 3.75 parts by mass of tetradecanoic acid and 0.51 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ at a rotating speed of 200rpm until all the materials are dissolved, adding 11.25 parts by mass of glycerol laurate, adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 16: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 5 parts by mass of tetradecanoic acid and 0.68 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until all the materials are dissolved, adding 10 parts by mass of glycerol laurate, complementing the rest with deionized water to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 17: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 7.5 parts by mass of tetradecanoic acid and 1.02 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ at a rotating speed of 200rpm until the materials are completely dissolved, adding 7.5 parts by mass of glycerol laurate, adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 18: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 11.25 parts by mass of tetradecanoic acid and 1.53 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ at a rotating speed of 200rpm until all the materials are dissolved, adding 3.75 parts by mass of glycerol laurate, adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 19: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 12 parts by mass of tetradecanoic acid and 1.64 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until all the materials are dissolved, adding 3 parts by mass of glycerol laurate, complementing the rest with deionized water to 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 20: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 0.27 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 21: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 0.54 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 22: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 0.91 part by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 23: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 1.09 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 24: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 1.64 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 25: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 1.91 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 26: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 2.18 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 27: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 2.46 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Example 28: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid and 2.73 parts by mass of potassium hydroxide, adding into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at 85 ℃ and a rotating speed of 200rpm until the materials are completely dissolved, adding 5 parts by mass of glycerol laurate, and adding the balance of the glycerol laurate to be 100, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Comparative example 1: preparation of tetradecanoic acid, glycerol laurate composition
Weighing 10 parts by mass of tetradecanoic acid, adding the tetradecanoic acid into a beaker containing 75 parts by mass of deionized water, mixing and stirring in a water bath kettle at a temperature of 85 ℃ and a rotation speed of 200rpm until the tetradecanoic acid is completely dissolved, adding 5 parts by mass of glycerol laurate, complementing the balance of the glycerol laurate to 100 by deionized water, and stirring for 30min; regulating the rotating speed to 100rpm, cooling and stirring, regulating the rotating speed to 50rpm after cooling to 60 ℃, continuously cooling to 40 ℃, and stopping stirring; and then preserving at room temperature for later use.
Test example: viscosity, stability and liquid crystal morphology
Viscosity meter model: RVDVS, viscosity test method: 96# rotor, 12rpm,60s.
Samples of the compositions of examples 1 to 28 and comparative example 1 of the present invention were taken, respectively, placed on a glass slide, flattened with a cover slip, then observed under the bright field of a microscope under a Leica DM2700P forward polarizing microscope (laika microscopy system company), focused until emulsion particles were clearly seen, and then observed under polarized light to see how much, whether or not the liquid crystal was apparent and the shape of the liquid crystal, and a liquid crystal image of the sample was taken at 100 times.
The results of the viscosity, stability and liquid crystal morphology of examples 1-28 and comparative example 1 are shown in the following table.
As is clear from the comparison of the results of examples 1 to 4, examples 1 and 2 had a Maltese cross liquid crystal structure under a polarizing microscope, whereas examples 3 and 4 had no Maltese cross liquid crystal structure under a polarizing microscope, i.e., a composition of lauric acid, lauric acid glyceride and potassium hydroxide could give a Maltese cross liquid crystal structure or a composition of myristic acid, lauric acid glyceride and potassium hydroxide could give a Maltese cross liquid crystal structure, i.e., the kind of fatty acid was related to the formation of the Maltese cross liquid crystal structure.
As is clear from the comparison of the results of examples 2 and 5 to 13, examples 2, 6, 7, 8, 9, 10, 11, 12 and 13 have a Maltese cross liquid crystal structure under a polarizing microscope, and example 5 has no Maltese cross liquid crystal structure under a polarizing microscope, i.e., the total amount of fatty acid and glycerol laurate is not less than 2% relative to the formation of the Maltese cross liquid crystal structure.
As is clear from comparison of the results of examples 2, 14 to 19, examples 2, 16, 17 and 18 had a maltese cross liquid crystal structure under a polarization microscope, whereas examples 14, 15 and 19 had no maltese cross liquid crystal structure under a polarization microscope, i.e. the mass ratio of fatty acid to glycerol laurate was related to the formation of maltese cross liquid crystal structure, and the mass ratio of fatty acid to glycerol laurate was 3:1 to 1:2.
As is clear from comparing the results of examples 2, 20 to 28, examples 2, 20, 21, 22, 23, 24, 25 have maltese cross liquid crystal structure under a polarizing microscope, whereas examples 26, 27, 28 have no maltese cross liquid crystal structure under a polarizing microscope, i.e. the weight ratio of fatty acid to potassium hydroxide is related to the formation of maltese cross liquid crystal structure, and the weight ratio of fatty acid to potassium hydroxide is 5:1 to 41:1.
Both example 2 and comparative example 1 had a maltese cross liquid crystal structure under a polarizing microscope, example 2 had no abnormality in stability, and comparative example 1 had delaminated, i.e., the addition of potassium hydroxide had a contributing effect on the stability of the composition.
Examples 2, 6, 7, 8, 9, 10, 11, 12 and 13 all have Maltese cross liquid crystal structures under a polarizing microscope, and stability of examples 2, 11, 12 and 13 is not abnormal, and stability of examples 6, 7, 8, 9 and 10 is layered, namely, total amount of fatty acid and glycerol laurate is related to stability of the composition, and total amount of fatty acid and glycerol laurate is equal to or more than 7%.
Example 2, example 20, example 21, example 22, example 23, example 24 and example 25 have a maltese cross liquid crystal structure under a polarizing microscope, and the stability of example 2, example 20, example 21, example 22 and example 23 is not abnormal, and the stability of example 24 and example 25 is layered, namely the weight ratio of fatty acid to potassium hydroxide is related to the stability of the composition, and the weight ratio of fatty acid to potassium hydroxide is 8:1-41:1.