CN108938439B - Liquid crystal type emulsified composition and preparation method and application thereof - Google Patents
Liquid crystal type emulsified composition and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a liquid crystal form emulsifying composition, a preparation method and application thereof. The liquid crystal emulsified composition comprises the following components in percentage by weight: liquid crystal emulsifier: 0.01-5%, preferably 0.1-3%; suspension stabilizer: 0.01-5%, preferably 0.3-4%; water-in-oil emulsifier: 0.1-5%, preferably 0.5-4%; higher aliphatic alcohol: 0.1-5%, preferably 0.5-3%; water: 30-80%, preferably 50-75%. The liquid crystal type emulsion composition disclosed by the invention is mild, free of stimulation and excellent in stability, has deep moistening and efficient moisturizing effects, can form a liquid crystal protective barrier on the surface of the skin, protects the skin from the invasion of the external environment, and effectively relieves the skin problem under the environmental pressure. In addition, the liquid crystal emulsified composition also has certain spreadability and glossiness, and can play a long-acting moisturizing and water-locking effect to make skin permanently moist and glossy.
Description
Technical Field
The invention relates to a liquid crystal form emulsifying composition, a preparation method and application thereof, belonging to the field of cosmetics.
Background
With the rapid development of cosmetic technology and the improvement of multiple preference awareness of consumers to products, various emulsification systems appear in the market, including common oil-in-water emulsification systems and water-in-oil emulsification systems, phase transition emulsification systems, microemulsion coating emulsification systems and the like. The variety of the emulsified products is more and more, and the functions are gradually diversified. However, most of the emulsified products in the market are oil-in-water systems or water-in-oil systems, and also have multiple emulsified systems of water-in-oil-in-water or oil-in-water-in-oil, which have respective advantages and disadvantages, have different skin feelings of the formulas, and have larger influence on the stability of the formulas due to the change of temperature; formulation design and production process regulation also have certain limitations, especially for a multiple emulsification system, and the limitation of the production process thereof causes that the emulsification system is still difficult to be produced in large quantities.
The oil-in-water and water-in-oil emulsifying systems have respective advantages and disadvantages, the water-in-oil system is rich in texture, high in appearance brightness, good in water resistance, easy to stick to the skin and good in moisturizing and water locking effects, and meanwhile, the moisture and brightness after the water-in-oil emulsifying system is obviously superior to that of the oil-in-water system, but the skin feeling of the prior-stage smearing is greasy and heavy than that of the oil-in-water system, and the stability of the formula is greatly influenced by the change of temperature; the difficulty of formula design and production process regulation is greater than that of an oil-in-water system. The oil-in-water system has a clear and moist skin feel at the early stage, but has poor moisturizing properties at the later stage.
Disclosure of Invention
Problems to be solved by the invention
Based on the technical problems existing in the prior art, for example: the skin feeling of the water-in-oil system is more sticky and thick than that of the oil-in-water system in the early stage, and the stability of the formula is greatly influenced by the change of temperature; poor moistening property in the later stage of the oil-in-water system, and the like. The invention firstly provides a liquid crystal form emulsifying composition. The liquid crystal type emulsified composition is mild and non-irritant, not only has deep moistening and efficient moisturizing effects, but also can form a liquid crystal protective barrier on the surface of skin to protect the skin from being damaged by the external environment, and effectively relieves the problem of the skin under the environmental pressure.
Furthermore, the invention also provides a preparation method of the liquid crystal emulsified composition, which has the advantages of easy acquisition of raw materials and simple preparation method.
Means for solving the problems
The invention provides a liquid crystal emulsified composition, which comprises the following components in parts by weight:
liquid crystal emulsifier: 0.01-5%, preferably 0.1-3%;
suspension stabilizer: 0.01-5%, preferably 0.3-4%;
water-in-oil emulsifier: 0.1-5%, preferably 0.5-4%;
higher aliphatic alcohol: 0.1-5%, preferably 0.5-3%;
water: 30-80%, preferably 50-75%.
The liquid crystal type emulsified composition according to the present invention, wherein the liquid crystal emulsifier comprises one or a combination of two or more of sucrose esters, alkyl glucosides, fatty acid polyglyceryl esters and lecithin.
The liquid crystal type emulsion composition according to the present invention, wherein the suspension stabilizer comprises a high molecular polymer, preferably, the high molecular polymer comprises: acrylic acid (ester)/C10-30 alkanol acrylate crosspolymer, acrylic acid (ester) copolymer sodium (and) lecithin, lecithin (and) sclerotium rolfsii gum (and) xanthan gum (and) pullulanase, propylene glycol laurate (and) ethyl cellulose (and) propylene glycol isostearate, isostearyl alcohol (and) butylene glycol cocoate (and) ethyl cellulose, ammonium acryloyl dimethyl taurate/VP copolymer and hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer.
The liquid crystal type emulsifying composition according to the present invention, wherein the water-in-oil emulsifier comprises one or a combination of two or more of polyglyceryl esters, silicones, fatty acid esters, ethoxylated vegetable oils, ethoxylated fatty alcohol ethers and sorbitan esters which are liquid at room temperature.
The liquid crystal type emulsified composition according to the present invention, wherein the higher aliphatic alcohol comprises an aliphatic alcohol having 16 to 24 carbon atoms; preferably, the higher fatty alcohol comprises one or a combination of two or more of cetyl alcohol, cetearyl alcohol, stearyl alcohol and behenyl alcohol.
The liquid crystal type emulsifying composition according to the present invention, wherein the weight ratio of the water-in-oil emulsifier to the liquid crystal emulsifier is 0.2-40: 1; preferably 0.5-35: 1; more preferably 1-30: 1; further preferably 5-25: 1; still more preferably 7-20: 1.
The liquid crystal type emulsion composition according to the present invention, wherein the liquid crystal type emulsion composition further comprises: one or more of grease, humectant and protective regulator;
preferably, the addition amount of the grease is 10-40%, the addition amount of the humectant is 5-10%, and the addition amount of the protective regulator is 0.1-5% by weight of the liquid crystal type emulsified composition.
The liquid crystal emulsified composition comprises one or more of semisynthetic oil, synthetic oil, animal oil, vegetable oil, mineral oil and silicone oil; and/or
The humectant comprises one or the combination of more than two of glycerol, propylene glycol, butanediol and dipropylene glycol; and/or
The protective regulator comprises one or more of antiseptic, antioxidant, perfume, pigment, chelating agent and pH regulator.
The present invention also provides a method for preparing the liquid crystal-type emulsified composition according to the present invention, which comprises a step of mixing the components of the liquid crystal-type emulsified composition.
The invention also provides the use of a liquid-crystalline emulsified composition according to the invention in cosmetics; specifically, the cosmetic comprises a skin care emulsion or a skin care cream.
ADVANTAGEOUS EFFECTS OF INVENTION
The liquid crystal type emulsion composition disclosed by the invention is mild, free of stimulation and excellent in stability, has deep moistening and efficient moisturizing effects, can form a liquid crystal protective barrier on the surface of the skin, protects the skin from the invasion of the external environment, and effectively relieves the skin problem under the environmental pressure.
In addition, the liquid crystal emulsified composition also has certain spreadability and glossiness, and can play a long-acting moisturizing and water-locking effect to make skin permanently moist and glossy.
Furthermore, the liquid crystal type emulsifying composition can stabilize the water-in-oil emulsifier in the water phase, so that the water phase and the oil phase are better connected in the using process of the product, and the product is emulsified and phase-inverted when being applied, thereby achieving the effect of long-acting and lasting skin moistening.
Furthermore, the invention also provides a preparation method of the liquid crystal form emulsified composition, the emulsifying process of the preparation method can be regulated and controlled, the raw materials are easy to obtain, the process is simple, the operation is easy, and the preparation method is suitable for industrial large-scale production.
Drawings
Fig. 1 shows the average skin moisture change rate at each time point of example 1, comparative example 2, example 6, and comparative example 10 of the present invention.
FIG. 2 shows an image at 200 times magnification under a microscope of a product of example 6 of the present invention;
FIG. 3 shows an image of the product of example 6 of the present invention under a polarizing microscope at 200 times magnification;
FIG. 4 shows an image at microscope magnification of 200 times of a product of comparative example 10 of the present invention;
FIG. 5 shows an image of a comparative example 10 product of the present invention under a polarization microscope at 200 times magnification.
Detailed Description
Various exemplary embodiments, features and aspects of the invention will be described in detail below. The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In other instances, methods, means, devices and steps which are well known to those skilled in the art have not been described in detail so as not to obscure the invention.
The invention provides a liquid crystal emulsified composition, which comprises the following components in parts by weight:
liquid crystal emulsifier: 0.01-5%, preferably 0.1-3%;
suspension stabilizer: 0.01-5%, preferably 0.3-4%;
water-in-oil emulsifier: 0.1-5%, preferably 0.5-4%;
higher aliphatic alcohol: 0.1-5%, preferably 0.5-3%;
water: 30-80%, preferably 50-75%.
The liquid crystal is a state with structure and mechanical property between liquid and crystal, and has liquid fluidity and solid molecule arrangement regularity.
Specifically, the liquid crystal emulsion composition of the present embodiment contains natural components such as a liquid crystal emulsifier, and can effectively reduce irritation and influence of the product on human skin without causing discomfort to the skin. The liquid crystal emulsified composition is mild and safe, and is suitable for various skin people. In addition, the liquid crystal emulsified composition contains a liquid crystal structure, has good affinity with the skin cuticle, is easy to stick to the skin and is absorbed by the skin; and a bionic liquid crystal film can be formed on the surface layer of the skin, so that the thickness of the skin is increased, and the sensitivity of the skin to external cold, heat and stimulus is reduced. Meanwhile, the liquid crystal structure can reduce the phenomenon of oil drop aggregation, so that the stability of the product can be improved.
In the invention, the liquid crystal emulsifier comprises one or the combination of more than two of sucrose esters, alkyl glucosides, fatty acid polyglycerol esters and lecithin. In general, the liquid crystal emulsifier of the present invention can be purchased from chemical or pharmaceutical markets.
The sucrose ester emulsifier can be, for example, an ester obtained by reacting sucrose with an edible fatty acid, and is an emulsifier in which-OH group of sucrose is a hydrophilic group and a carbon chain part of a fatty acid is a lipophilic group. The fatty acid used may be higher fatty acid such as stearic acid, palmitic acid, oleic acid, etc. The sucrose ester emulsifier of the present invention may be mono-, di-and tri-esters and mixed esters thereof obtained by reacting sucrose with stearic acid, palmitic acid and/or oleic acid, and the like.
The alkyl glucoside emulsifier of the present invention may be, for example, arachidyl alcohol glucoside or stearyl glucoside. The fatty acid polyglycerol ester emulsifier can be ester generated by reaction of polyglycerol and stearic acid and/or beeswax acid; such as polyglyceryl-6 distearate and polyglyceryl-3 beeswax, and the like. The lecithin emulsifier may be lecithin or hydrogenated lecithin, and the lecithin emulsifier is preferably used in the present invention.
In the present invention, the liquid crystal emulsifier may be added in an amount of 0.01 to 5% by weight of the liquid crystal-based emulsion composition, for example: may be 0.05%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3.5%, 4%, 4.5%, etc., preferably 0.1-3%; when the addition amount of the liquid crystal emulsifier is within the range of 0.01-5%, the prepared liquid crystal emulsified product has good stability, a liquid crystal structure is clear under a polarizing microscope, a liquid crystal protective barrier is formed on the surface of skin, the moisturizing effect is good, and emulsion droplets are fine and smooth.
By using the suspension stabilizer, the invention not only can reduce the tendency of oil drop aggregation by cooperating with the liquid crystal structure so as to improve the stability of the product, but also can suspend and stabilize the water-in-oil emulsifier added into the system at the later stage in the system. By using the suspension stabilizer, the product can better connect the water phase and the oil phase in the use process, and can be emulsified and phase-inverted when being smeared, thereby achieving the effect of long-acting and lasting skin moistening.
In the present invention, the suspension stabilizer includes a high molecular polymer. The specific components of the suspension stabilizer of the present invention are not particularly limited as long as they can be used in the fields of cosmetics, pharmaceuticals, quasi drugs, and the like. Specifically, the high molecular polymer may be acrylic acid (ester)/C10-30 alkanol acrylate crosslinked polymer, acrylic acid (ester) copolymer, etc. of Lubrizol corporation; also can be acrylic acid (ester) copolymer sodium (and) lecithin, lecithin (and) sclerotium rolfsii gum (and) xanthan gum (and) pullulanase polysaccharide, etc. of the LUCAS MEYER company; also can be EMULFREE series of raw materials of GATTEFOSSE company, comprising propylene glycol laurate (and) ethyl cellulose (and) propylene glycol isostearate, isostearyl alcohol (and) butylene glycol cocoate (and) ethyl cellulose, etc.; also available are Aristoflex Polymers from Clariant corporation, for example: acryloyl dimethyl ammonium taurate/VP copolymer, and the like; and Polymers thickening stabilizers from SEPPIC corporation, such as: one or a combination of more than two of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and the like.
In the present invention, the suspension stabilizer is added in an amount of 0.01 to 5% by weight of the liquid crystal type emulsion composition, for example: may be 0.05%, 0.1%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3.5%, 4%, 4.5%, etc., preferably 0.3-4%; when the addition amount of the suspension stabilizer is within the range of 0.01-5%, the prepared liquid crystal emulsified product has good stability, not only can suspend and stabilize emulsion droplets with a liquid crystal structure, but also can suspend and stabilize a water-in-oil emulsifier dispersed in a water phase.
The water-in-oil emulsifier of the present invention typically has a hydrophilic lipophilic balance HLB value of between 1 and 6. The water-soluble film can be stably dispersed in a water phase, so that the product can be more moistened and moisturized when in use, and has good spreadability and moisturizing and water-locking effects. The specific components of the water-in-oil emulsifier of the present invention are not particularly limited as long as the water-in-oil emulsifier is liquid at normal temperature (generally 20 to 30 ℃) which can be used in the fields of cosmetics, pharmaceuticals, quasi drugs, etc. Specifically, the water-in-oil emulsifier comprises one or more of polyglycerol esters, silicones, fatty acid esters, ethoxylated vegetable oils, ethoxylated fatty alcohol ethers and sorbitan esters.
In the present invention, the water-in-oil emulsifier is added in an amount of 0.1 to 5% by weight of the liquid crystal type emulsifying composition, for example: may be 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4.5%, etc., preferably 0.5-4%. When the addition amount of the water-in-oil emulsifier is within the range of 0.1-5%, the prepared liquid crystal emulsified product has good stability, excellent moisturizing performance, and excellent spreadability, water-moist feel, smooth feel, moist feel and the like in use.
The polyglycerin ester-based emulsifier of the present invention may be, for example, polyglycerin-3 distearate or polyglycerin-10 decaoleate. Examples of the silicone emulsifier include dimethicone PEG-10/15 crosspolymer, PEG-10 dimethicone crosspolymer, cetyl PEG/PPG-10/1 dimethicone, lauryl PEG-9 dimethicone ethyl dimethicone, and lauryl PEG-10 tris (trimethylsiloxy) silicone ethyl methicone. The fatty acid ester emulsifier may be, for example, glyceryl oleate. The ethoxylated vegetable oil emulsifier may be, for example, PEG-5 castor oil, etc. The sorbitan ester-based emulsifier may be sorbitan sesquioleate, for example. The ethoxylated fatty alcohol ether emulsifier may be, for example, oleyl polyether-2.
Preferably, in the present invention, the weight ratio of the water-in-oil emulsifier to the liquid crystal emulsifier is 0.2-40: 1; more preferably 0.5 to 35: 1; preferably 1-30: 1; further preferably 5-25: 1; more preferably 7-20:1, etc. When the ratio of the amount of the water-in-oil emulsifier to the amount of the liquid crystal emulsifier is in the range of 0.2 to 40:1, a liquid crystal type emulsified composition excellent in stability, moisture retention and the like can be further prepared.
The higher fatty alcohol can help the liquid crystal emulsifier to emulsify to form liquid crystal, and can further improve the stability of the product. Higher aliphatic alcohols generally refer to mixtures of monohydric alcohols containing six or more carbon atoms. The higher fatty alcohol of the present invention is a higher fatty alcohol which can form a liquid crystal structure together with the liquid crystal emulsifier of the present invention in water. The specific components of the higher aliphatic alcohol in the present invention are not particularly limited, and may be those usable in the fields of cosmetics, pharmaceuticals, quasi drugs, and the like. The higher aliphatic alcohol of the present invention may be a higher aliphatic alcohol having 12 or more carbon atoms, and is preferably a linear higher aliphatic alcohol having 16 to 24 carbon atoms. Such as cetyl alcohol, cetearyl alcohol, stearyl alcohol, behenyl alcohol, and the like.
In the present invention, the higher aliphatic alcohol is added in an amount of 0.1 to 5% by weight of the liquid crystal type emulsified composition, for example: may be 1%, 1.5%, 2%, 2.5%, 3.5%, 4%, 4.5%, etc., preferably 0.5-3%. When the addition amount of the higher aliphatic alcohol is in the range of 0.1 to 5%, the prepared liquid crystal emulsified composition has good stability and can also improve the viscosity.
In the present invention, the water is added in an amount of 30 to 80%, for example: may be 40%, 50%, 60%, 70%, etc., preferably 50-75%. Wherein the water can be purified water, distilled water, deionized water and the like used for reaching the cosmetic production level.
The liquid crystal-type emulsifying composition of the present invention may further include: one or more of grease, humectant and protective regulator. The oil agent is one or more of semisynthetic oil and fat, synthetic oil and fat, animal oil and fat (such as squalane), vegetable oil and fat (such as flos Potentillae chinensis (LIMNANTHES ALBA) seed oil, Butyrospermum PARKII (Butyrum PARKII) fruit fat, hydrogenated palm oil glyceride, phytosterol ester, etc.), mineral oil and silicone oil (such as polydimethylsiloxane). The humectant can be one or more of glycerol, propylene glycol, butanediol and dipropylene glycol. The protective regulator comprises cosmetic antiseptic (such as methyl paraben, phenoxyethanol, and ethylhexyl glycerin), antioxidant, perfume, pigment, chelating agent (such as EDTA-2Na), pH regulator (such as triethanolamine), etc. The specific components of the fat and oil, the humectant and the protective regulator are not particularly limited, and may be those which can be used in the fields of cosmetics, pharmaceuticals, quasi drugs and the like.
Generally speaking, the addition amount of the grease is 10-40%, the addition amount of the humectant is 5-10%, and the addition amount of the protection regulator is 0.1-5%.
In addition, the liquid crystal emulsified composition can improve local microcirculation of skin, reduce normal metabolism, has certain spreadability and glossiness, can achieve the effect of long-acting moistening and water locking, and enables the skin to be permanently moisturized and glossy.
The present invention also provides a method for preparing the liquid crystal type emulsified composition according to the present invention, comprising the step of mixing the components of the liquid crystal type emulsified composition.
Specifically, the preparation method comprises the steps of uniformly mixing the liquid crystal emulsifier, the suspension stabilizer, water and higher fatty alcohol, and then mixing the mixture with the water-in-oil emulsifier to obtain the liquid crystal emulsified composition.
Further, the preparation method comprises mixing the liquid crystal emulsifier with higher fatty alcohol, then mixing with the suspension stabilizer and water, and then mixing with the water-in-oil emulsifier to obtain the liquid crystal type emulsified composition.
According to the preparation method of the liquid crystal type emulsified composition, the emulsification process of the preparation method can be regulated and controlled, raw materials are easy to obtain, the process is simple, the operation is easy, and the preparation method is suitable for industrial large-scale production.
The invention also provides the use of a liquid-crystalline emulsified composition according to the invention in cosmetics; specifically, the cosmetic comprises a skin care emulsion or a skin care cream.
The invention also provides a preparation method of the cosmetic, which comprises the following steps:
adding water, humectant and suspension stabilizer into a container, stirring and mixing, adding antiseptic and chelating agent, stirring and heating to 75-80 deg.C;
adding liquid crystal emulsifier, higher fatty alcohol and oil into another container, stirring and heating to 75-80 deg.C, dissolving and mixing well, and keeping the temperature at 75-80 deg.C for use;
mixing the water phase and the oil phase, homogenizing for 5-10 min, stopping homogenizing, stirring, and cooling;
cooling to 40-50 deg.C, adding pH regulator and antiseptic, stirring and cooling;
cooling to 30-35 deg.C, adding water-in-oil emulsifier, homogenizing, and stirring;
quality inspection and filling: and (5) filling after the inspection is qualified to obtain the corresponding cosmetic.
Examples
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Examples 1 to 5
The skin care emulsions of examples 1-5 were prepared according to the following method, with the weight percentages of the components of examples 1-5 in table 1 below being 100% by total weight.
The skin care emulsions of examples 1-5 were prepared by the method of:
step 1), phase a (aqueous phase): adding water, humectant (glycerol), and suspension stabilizer (acryloyl dimethyl ammonium taurate/VP copolymer and acrylic acid (ester) copolymer) into container, stirring, mixing, adding antiseptic (methyl hydroxybenzoate) and chelating agent (EDTA-2Na), stirring, and heating to 75-80 deg.C;
step 2), phase B (oil phase): adding higher fatty alcohol (cetostearyl alcohol), partial oil (hydrogenated palm oil glyceride, white chinlon oil and squalane) into another container, stirring and heating to 75-80 deg.C, mixing and dissolving uniformly, adding the rest oil (shea butter, phytosterol ester and polydimethylsiloxane) and liquid crystal emulsifier (hydrogenated lecithin), keeping the temperature at 75-80 deg.C, stirring, dissolving and mixing uniformly for use;
step 3), mixing: mixing the water phase and the oil phase, homogenizing at 3000rpm for 8 min, stopping homogenizing, stirring and cooling;
step 4), phase C: cooling to 45 deg.C, adding pH regulator (triethanolamine), stirring, adding antiseptic (phenoxyethanol and ethylhexyl glycerol), stirring, and cooling;
step 5), phase D: cooling to 32 deg.C, adding water-in-oil emulsifier (lauryl PEG-10 tri (trimethylsiloxy) silicon ethyl polymethylsiloxane and polyglycerol-10 decaoleate), homogenizing, and stirring.
Step 6), quality inspection and filling: and (5) filling after the inspection is qualified.
TABLE 1
Comparative example
The skin care emulsions of comparative examples 1-5 were prepared according to the following method, with the weight percentages of the components of comparative examples 1-5 in table 2 below being 100% by total weight.
TABLE 2
Examples 6 to 10
The skin creams of examples 6-10 were prepared according to the following method, with the weight percentages of the components of examples 6-10 in Table 3 being 100% by total weight.
The skin cream of examples 6-10 was prepared by the method of:
step 1), phase a (aqueous phase): adding water, humectant (glycerol), and suspension stabilizer (acryloyl dimethyl taurate/VP copolymer and acrylic acid (ester)/C10-30 alkanol acrylate crosslinked polymer) into a container, stirring, mixing, adding antiseptic (methyl hydroxybenzoate) and chelating agent (EDTA-2Na), stirring, and heating to 75-80 deg.C;
step 2), phase B (oil phase): adding higher fatty alcohol (cetostearyl alcohol), partial oil (hydrogenated palm oil glyceride, white chinlon oil and squalane) into another container, stirring and heating to 75-80 deg.C, mixing and dissolving uniformly, adding the rest oil (shea butter, phytosterol ester and polydimethylsiloxane) and liquid crystal emulsifier (hydrogenated lecithin), keeping the temperature at 75-80 deg.C, stirring and dissolving uniformly for use;
step 3), mixing: mixing the water phase and the oil phase, homogenizing at 3000rpm for 8 min, stopping homogenizing, stirring and cooling;
step 4), phase C: cooling to 45 deg.C, adding pH regulator (triethanolamine), stirring, adding antiseptic (phenoxyethanol and ethylhexyl glycerol), stirring, and cooling;
step 5), phase D: cooling to 32 deg.C, adding water-in-oil emulsifier (polyglycerol-3 distearate and polyglycerol-10 decaoleate), homogenizing, and stirring.
Step 6), quality inspection and filling: and (5) filling after the inspection is qualified.
TABLE 3
Comparative examples 6 to 10
The skin creams of comparative examples 6-10 were prepared according to the following method, with the weight percentages of the components of comparative examples 6-10 in Table 4 below being 100% by total weight.
TABLE 4
Performance testing
First, stability test
In order to evaluate the stability of the products provided by the present invention, the products prepared in examples 1 to 10 and comparative examples 1 to 10 were respectively allowed to stand at different temperatures for a certain period of time, and the stability of the products provided by the present invention at different temperatures was measured in accordance with the test method of the industry standard QB/T1857-2013 at a temperature range of-15 to 40 ℃. The stability of the emulsions prepared in examples 1-5 and comparative examples 1-5 is shown in Table 5. The stability of the creams prepared in examples 6 to 10 and comparative examples 6 to 10 is shown in Table 6.
Stability of skin care emulsions prepared in Table 5, examples 1-5 and comparative examples 1-5
Wherein "O" is passed for stability and "X" is not passed for stability.
Stability of skin cream prepared in Table 6, examples 6-10 and comparative examples 6-10
Wherein "O" is passed for stability and "X" is not passed for stability.
As shown in Table 5, the skin care emulsions prepared in examples 1 to 5 and comparative example 2 have good stability in the experiment process of constant temperature for 3 months at the temperature ranging from-15 ℃ to 40 ℃, do not have the phenomena of serious delamination, coarseness, unstable water discharge and the like, can keep a uniform state, and the stability test is passed. The skin care emulsions prepared in comparative examples 1 and 3 to 5 exhibited increased viscosity after being maintained at-15 ℃ for 2 to 3 months, and exhibited instability such as thickening or water discharge, and the stability test did not pass. When the emulsion is kept at a high temperature of 40 ℃ for 3 months at a constant temperature, the emulsions prepared in comparative examples 1 and 3 to 5 show unstable states such as coarseness and delamination, the viscosity is also reduced, and the stability test fails.
The skin care emulsions prepared in comparative examples 1, 3, and 5 exhibited instability such as thickening or water discharge after being maintained at 25 ℃ for 2 to 3 months, and the stability test failed.
As can be seen from Table 6, the skin cream prepared in examples 6-10 and comparative example 10 has good stability in the experiment process of constant temperature for 3 months at the temperature ranging from-15 ℃ to 40 ℃, and has no phenomena of serious stratification, coarseness, unstable water discharge and the like, and can keep relatively fine, bright and stable appearance. The creams prepared in comparative examples 6, 7 and 9 show a rise in viscosity after being maintained at-15 ℃ for 2-3 months, and show instability such as coarseness or water discharge, which affects the normal use of the product. After being kept at a constant temperature of 40 ℃ for 3 months, the creams prepared in comparative examples 6 to 9 exhibited unstable states such as coarsening or delamination, and the stability test failed.
After being kept at a constant temperature of 25 ℃ for 3 months, the creams prepared in comparative examples 6 to 7 exhibited unstable states such as coarsening or delamination, and the stability test failed.
Secondly, the difference of moisture retention, use feeling and liquid crystal effect
To compare the differences between the emulsion creams provided by the present invention and the prior art, the present invention also provides the differences in moisturization, feel and liquid crystal effect of the products of example 1 and comparative example 2, and example 6 and comparative example 10, as the stability tests of comparative example 2 and comparative example 10 were able to pass, as follows:
1. moisture retention efficacy test
Randomly selecting 30 subjects with healthy skin and no skin diseases or allergy history, and selecting the appropriate area of the upper arm flexion area of the subjects as a test area. Before the test, the test area is cleaned by clear water, then is evenly wiped by alcohol and then is naturally dried for 15min, and the average skin moisture content (blank value) before the sample is not applied is measured by a skin moisture content measurer (Derma Expert-MC960 skin tester). The subjects were applied with 30. mu.L of each of 4 samples in a range of 3 cm. times.3 cm from the inner side of the forearm, and the samples were completely and uniformly applied with the fingers until after absorption. The moisture content of the skin after 30 minutes, 1 hour, 2 hours, 3 hours, 5 hours, 8 hours, and 24 hours after application was measured with a skin moisture content meter, and the moisture change rate was used as an evaluation index. The average skin moisture change rates at each time point of the 4 samples were compared and the results are shown in figure 1.
It can be seen from fig. 1 that the average skin moisture change rate at each time point using the product of example 1 was higher than that using comparative example 2, and the average skin moisture change rate at each time point after using example 6 was higher than that using comparative example 10. So that example 1 using the technique of the present invention has better moisturizing effect than comparative examples 2 and 10 than example 6.
2. Sensory skin feel evaluation
A skin-feel expert group of 20 subjects with an average age of 30 years was selected for evaluation of skin-feel. The evaluation method is that before the product is used, specific scores are given in 1-10 points for different sensory skin feeling indexes (the higher score represents the better using feeling) when the product is used, and the following steps are shown:
TABLE 7 comparison of the feeling of use of the products prepared according to the present invention with that of the comparative example
As can be seen from table 7, the skin feel differences in spreadability, water-moist feel, smooth feel and moist feel were clearly felt by the testers in examples 1 and 6 of the present invention, as compared with comparative examples 1 and 10. The embodiment of the invention is relatively easy to spread on the skin surface, has water-moist feeling which is more favored by consumers, and the product provided by the invention can improve the skin glossiness after being smeared on the skin, so that the skin is smoother and more moist.
3. Liquid crystal effect testing
FIG. 2 shows an image of a liquid crystal type emulsifying composition of example 6 of the present invention under a microscope at 200 times magnification; FIG. 3 shows an image of a liquid crystal-type emulsifying composition of example 6 of the present invention under a polarizing microscope at a magnification of 200 times; FIG. 4 shows an image at microscope magnification of 200 times of a product of comparative example 10 of the present invention; FIG. 5 shows an image of a comparative example 10 product of the present invention under a polarization microscope at 200 times magnification.
As shown in fig. 2-3, the circled area in the product of example 6 of the present invention is water-in-oil emulsifier, which can be shown to be present in the aqueous phase (external phase) without liquid crystal emulsifier encapsulation. As shown in fig. 4-5, the product of comparative example 10 did not contain a water-in-oil emulsifier, and the structure of the present application was absent. Therefore, the liquid crystal emulsified composition can stabilize the water-in-oil emulsifier in the water phase, so that the water phase and the oil phase are better connected in the using process of the product, and the product is emulsified and phase-inverted when being applied, thereby achieving the effect of long-acting and lasting skin moistening.
The liquid crystal type emulsifying composition is mild and non-irritant, has deep moistening and high-efficiency moisturizing effects due to the presence of the water-in-oil emulsifier and the liquid crystal emulsifier, can form a liquid crystal protective barrier on the surface of skin, protects the skin from being damaged by the external environment, and can effectively relieve the skin problem under the environmental pressure.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (17)
1. The liquid crystal emulsified composition is characterized by comprising the following components in parts by weight:
liquid crystal emulsifier: 0.01 to 5 percent;
suspension stabilizer: 0.01 to 5 percent;
water-in-oil emulsifier: 0.1-5%;
higher aliphatic alcohol: 0.1-5%;
water: 30-80 percent;
the water-in-oil emulsifier comprises one or the combination of more than two of polyglycerol esters, organic silicon, fatty acid esters, ethoxylated vegetable oil, ethoxylated fatty alcohol ether and sorbitan ester which are liquid at normal temperature;
the weight ratio of the water-in-oil emulsifier to the liquid crystal emulsifier is 0.5-40: 1;
mixing a liquid crystal emulsifier, a suspension stabilizer, water and higher fatty alcohol, and then mixing with a water-in-oil emulsifier to obtain the liquid crystal emulsified composition.
2. The liquid crystal-type emulsified composition according to claim 1, wherein the liquid crystal emulsifier is added in an amount of 0.1-3%, the suspension stabilizer is added in an amount of 0.3-4%, the water-in-oil emulsifier is added in an amount of 0.5-4%, the higher aliphatic alcohol is added in an amount of 0.5-3%, and the water is added in an amount of 50-75%.
3. The liquid crystal emulsified composition as claimed in claim 1, wherein the liquid crystal emulsifier comprises one or more of sucrose esters, alkyl glucosides, fatty acid polyglyceryl esters and lecithin.
4. The liquid-crystal emulsified composition as claimed in any one of claims 1 to 3, wherein the suspension stabilizer comprises a high molecular polymer.
5. The liquid-crystal emulsified composition according to claim 4, wherein the high molecular weight polymer comprises: acrylic acid (ester)/C10-30 alkanol acrylate crosspolymer, acrylic acid (ester) copolymer sodium and lecithin, lecithin and sclerotium rolfsii gum and xanthan gum and pullulanase, propylene glycol laurate and ethyl cellulose and propylene glycol isostearate, isostearyl alcohol and butylene glycol cocoate and ethyl cellulose, ammonium acryloyl dimethyl taurate/VP copolymer and hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer.
6. The liquid-crystal emulsified composition as claimed in any one of claims 1 to 3, wherein the higher aliphatic alcohol comprises an aliphatic alcohol having 16 to 24 carbon atoms.
7. The liquid crystal-type emulsified composition according to claim 6, wherein the higher fatty alcohol comprises one or a combination of two or more of cetyl alcohol, cetearyl alcohol, stearyl alcohol and behenyl alcohol.
8. The liquid-crystal emulsified composition according to any one of claims 1 to 3 wherein the weight ratio of the water-in-oil emulsifier to the liquid-crystal emulsifier is 0.5 to 35: 1.
9. the liquid crystal-type emulsifying composition according to claim 8, wherein the weight ratio of the water-in-oil emulsifier to the liquid crystal emulsifier is 1-30: 1.
10. The liquid crystal-type emulsifying composition according to claim 9, wherein the weight ratio of the water-in-oil emulsifier to the liquid crystal emulsifier is 5-25: 1.
11. The liquid crystal-type emulsifying composition according to claim 10, wherein the weight ratio of the water-in-oil emulsifier to the liquid crystal emulsifier is 7-20: 1.
12. The liquid-crystal emulsifying composition according to any one of claims 1 to 3, further comprising: one or more of grease, humectant and protective regulator.
13. The liquid crystal emulsified composition as claimed in claim 12, wherein the oil and fat is added in an amount of 10% to 40%, the humectant is added in an amount of 5% to 10%, and the protective regulator is added in an amount of 0.1% to 5% by weight of the liquid crystal emulsified composition.
14. The liquid crystal-type emulsified composition according to claim 12, wherein the oil or fat comprises one or a combination of two or more of semisynthetic oil or fat, synthetic oil or fat, animal oil or fat, vegetable oil or fat, mineral oil or fat, and silicone oil; and/or
The humectant comprises one or the combination of more than two of glycerol, propylene glycol, butanediol and dipropylene glycol; and/or
The protective regulator comprises one or more of antiseptic, antioxidant, perfume, pigment, chelating agent and pH regulator.
15. A process for the preparation of a liquid-crystal emulsified composition according to any one of claims 1 to 14, characterised in that it comprises a step of mixing the components of the liquid-crystal emulsified composition.
16. Use of a liquid-crystalline emulsified composition according to any one of claims 1 to 14 in cosmetics.
17. Use according to claim 16, characterized in that said cosmetic product comprises a skin-care emulsion or cream.
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| CN110448483B (en) * | 2019-08-12 | 2022-11-25 | 中山市博深化学有限公司 | Phase inversion emulsion and preparation method thereof |
| CN111110589A (en) * | 2019-12-12 | 2020-05-08 | 广东博然堂生物科技有限公司 | Long-acting moisturizing composition and skin care product thereof |
| CN111643376B (en) * | 2020-06-15 | 2023-04-25 | 花安堂生物科技集团有限公司 | Nanoemulsion composition and application thereof |
| CN111568782B (en) * | 2020-06-15 | 2023-02-24 | 花安堂生物科技集团有限公司 | Nanoemulsion composition capable of improving skin barrier and application thereof |
| KR102321537B1 (en) * | 2020-09-04 | 2021-11-04 | 코스맥스 주식회사 | Water-in-oil-in-water type multiple emulsion for cosmetic composition with low viscosity |
| CN113122362B (en) * | 2021-04-13 | 2023-07-07 | 中国科学院上海高等研究院 | Water-based lubricant and preparation method and application thereof |
| CN113244116B (en) * | 2021-04-27 | 2023-04-28 | 广州立白企业集团有限公司 | Structured composition and use thereof |
| CN113208940B (en) * | 2021-04-30 | 2022-12-23 | 广州市科能化妆品科研有限公司 | Refreshing and stable sun-screening composition and preparation method thereof |
| CN115381723B (en) * | 2022-08-15 | 2023-07-28 | 华东理工大学 | Multiple liquid crystal emulsion of polyol in oil-in-water, preparation method and application thereof |
| CN116570524A (en) * | 2022-10-10 | 2023-08-11 | 广州市小谭科技有限公司 | Skin cream with liquid crystal structure and preparation method thereof |
| CN115813782A (en) * | 2022-11-22 | 2023-03-21 | 广东博然堂生物科技有限公司 | Low-viscosity emulsified water aqua and preparation method thereof |
| CN115844769A (en) * | 2022-12-26 | 2023-03-28 | 上海家化联合股份有限公司 | Stable emulsion system containing oil globule composition |
| CN116059124A (en) * | 2023-03-06 | 2023-05-05 | 水羊化妆品制造有限公司 | Composition for improving gamma-aminobutyric acid irritation as well as preparation method and application thereof |
| CN116421486B (en) * | 2023-04-11 | 2024-05-28 | 晟薇药业(上海)有限公司 | Emulsifier composition, emulsified toning lotion and preparation method thereof |
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| CN105769588A (en) * | 2016-04-29 | 2016-07-20 | 辽宁向上实业有限公司 | Modified liquid crystal type emulsified liquid with natural plant substrates and method for preparing modified liquid crystal type emulsified liquid |
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Effective date of registration: 20220113 Address after: No.23, Xianke 2nd Road, Huadong Town, Huadu District, Guangzhou City, Guangdong Province, 510890 Patentee after: GUANGZHOU KENENG COSMETIC RESEARCH Co.,Ltd. Patentee after: Guangdong Danzi Group Co., Ltd; Address before: No.23, Xianke 2nd Road, Huadong Town, Huadu District, Guangzhou City, Guangdong Province, 510890 Patentee before: GUANGZHOU KENENG COSMETIC RESEARCH Co.,Ltd. Patentee before: GUANGZHOU BAIYUN LIANJIA FINE CHEMICAL PLANT Patentee before: GUANGDONG DANZ GROUP Co.,Ltd. |