CN113730288A - Liquid crystal composition and preparation method and application thereof - Google Patents

Liquid crystal composition and preparation method and application thereof Download PDF

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Publication number
CN113730288A
CN113730288A CN202110929369.0A CN202110929369A CN113730288A CN 113730288 A CN113730288 A CN 113730288A CN 202110929369 A CN202110929369 A CN 202110929369A CN 113730288 A CN113730288 A CN 113730288A
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liquid crystal
crystal composition
component
preparation
alcohol
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CN113730288B (en
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夏黎明
邬凤娟
李慧瑜
孟祥艳
徐晶
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Guangzhou Meisu Biotechnology Co ltd
Guangzhou Jnumeso Biotechnology Inc
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Guangzhou Meisu Biotechnology Co ltd
Guangzhou Jnumeso Biotechnology Inc
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/0295Liquid crystals
    • AHUMAN NECESSITIES
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/34Alcohols
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/37Esters of carboxylic acids
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/60Sugars; Derivatives thereof
    • A61K8/602Glycosides, e.g. rutin
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    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
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    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8147Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
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    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8152Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
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    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
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    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9755Gymnosperms [Coniferophyta]
    • A61K8/9767Pinaceae [Pine family], e.g. pine or cedar
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    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
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    • A61K8/9794Liliopsida [monocotyledons]
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Abstract

The invention discloses a liquid crystal composition and a preparation method and application thereof, and the preparation raw materials of the liquid crystal composition comprise glycerol, caprylic/capric triglyceride, jojoba oil, carbomer 940 and an emulsifier. The liquid crystal composition has the advantages of easily obtained raw materials, good matching of the raw materials and the content proportion thereof, uniqueness and irreplaceability. The preparation method of the liquid crystal composition is simple, the D-phase emulsification is combined with the phase inversion emulsification process, so that the prepared liquid crystal composition is uniform in particle size range of only 3-10 mu m, the liquid crystal effect is bright, the preparation effect is better than that of the traditional method, and the application value is extremely high.

Description

Liquid crystal composition and preparation method and application thereof
Technical Field
The invention belongs to the field of cosmetics, and particularly relates to a liquid crystal composition, and a preparation method and application thereof.
Background
Liquid crystals are intermediate states between liquids and solids, also known as mesomorphic states. Liquid crystals have structural order and mobility. O/W cosmetic emulsions containing liquid crystalline structures are so-called liquid crystal cosmetics, and the weak interaction between water and a surfactant in the cosmetic emulsion can enable a certain amount and a certain sequence of chaotropic liquid crystals to be formed in the emulsion, thereby having strong birefringence and being sensitive to temperature.
With the continuous improvement of the living standard of people, the requirements of people on cosmetics are continuously improved. In the related art, liquid crystal type emulsion cosmetics have excellent moisture retention, can effectively control the release rate of active substances or produce a soft and skin-friendly skin feel, and thus have extremely high market value. However, the emulsion prepared by the traditional liquid crystal preparation method has poor particle uniformity, larger particle diameter, poor liquid crystal brightness degree and less liquid crystal content, so that the use requirement of the actual liquid crystal type emulsion cosmetics cannot be met, and the generated skin care effect is poor.
Therefore, the development of a preparation method capable of efficiently obtaining a liquid crystal composition with small particle size, high particle uniformity, bright liquid crystal and high liquid crystal content is of great significance to the development and popularization of liquid crystal type emulsion cosmetics.
Disclosure of Invention
Which aims to solve at least one of the technical problems of the prior art. Compared with the liquid crystal composition produced by the traditional method, the liquid crystal composition prepared by the liquid crystal composition formula and the preparation process thereof has the advantages of better quality, small particle size, high particle uniformity, bright liquid crystal and high liquid crystal content, and has extremely important significance for developing new liquid crystal cosmetics or improving the efficacy of the liquid crystal cosmetics.
In a first aspect of the present invention, a liquid crystal composition is provided, wherein the liquid crystal composition is prepared from raw materials including glycerin, caprylic/capric triglyceride, jojoba oil, carbomer 940 and an emulsifier.
The inventor finds that the raw materials for preparing the liquid crystal composition have irreplaceability, and tests prove that the quality of the liquid crystal composition is remarkably reduced and problems such as reduced liquid crystal density, nonuniform liquid crystal density or reduced liquid crystal content occur no matter the same type of reagent is added or part of the reagents in the formula are replaced by the same type of reagent or reagents with similar functions, so that the formula has extremely strong uniqueness and irreplaceability.
According to a first aspect of the present invention, in some embodiments of the present invention, the raw materials for preparing the liquid crystal composition further comprise at least one of a cosmetic conventional adjuvant and water.
Of course, the raw materials for preparing the liquid crystal composition also include, but are not limited to: chelating agents, solubilizers, emollients, rheology modifiers, antioxidants, whitening agents, conditioning agents, soothing agents, natural perfumes/pigments and the like, which do not affect the emulsifying system itself, or functional agents.
In some preferred embodiments of the invention, the emulsifier comprises at least one of MONTANOV 202 (arachidyl alcohol/docosanol/arachidyl alcohol glucoside, also known as eicosanyl alcohol/docosanol/eicosanyl glucoside), MONTANOV 68 (cetostearyl alcohol/cetostearyl glucoside), MONTANOV 82 (cetostearyl alcohol/cocoyl glucoside), behenyl alcohol, hydrogenated lecithin, sodium stearyl glutamate, polyglycerol-10-stearate.
In some more preferred embodiments of the invention, the emulsifier is MONTANOV 202 and behenyl alcohol.
In some preferred embodiments of the present invention, the cosmetic conventional adjuvant comprises at least one of disodium EDTA, triethanolamine, phenoxyethanol, and citric acid, sodium citrate, and methylparaben.
In some more preferred embodiments of the present invention, the cosmetically conventional adjuvant is disodium EDTA, triethanolamine, and phenoxyethanol.
According to a first aspect of the invention, in some embodiments of the invention, the liquid crystal composition is made from glycerol, MONTANOV 202, caprylic/capric triglyceride, jojoba oil, behenyl alcohol, carbomer 940, disodium EDTA, triethanolamine, phenoxyethanol, and water.
In some preferred embodiments of the present invention, the liquid crystal composition is prepared from 5 to 10 parts by mass of glycerin, 1 to 2 parts by mass of MONTANOV 202, 3 to 5 parts by mass of caprylic/capric triglyceride, 3 to 5 parts by mass of jojoba oil, 1 to 2 parts by mass of behenyl alcohol, 0.1 to 0.2 part by mass of carbomer 940, 0.01 to 0.1 part by mass of disodium EDTA, 0.1 to 0.2 part by mass of triethanolamine, 0.1 to 0.2 part by mass of phenoxyethanol, and 74 to 83 parts by mass of water.
In some more preferred embodiments of the present invention, the liquid crystal composition is prepared from 5 to 10 parts by mass of glycerin, 1 to 2 parts by mass of MONTANOV 202, 5 parts by mass of caprylic/capric triglyceride, 5 parts by mass of jojoba oil, 1 to 2 parts by mass of behenyl alcohol, 0.1 to 0.2 part by mass of carbomer 940, 0.1 part by mass of disodium EDTA, 0.1 to 0.2 part by mass of triethanolamine, 0.2 part by mass of phenoxyethanol, and 75.3 to 82.4 parts by mass of water.
In a second aspect of the present invention, there is provided a method for preparing a liquid crystal composition, comprising the steps of:
injecting the mixed component B into the mixed component A to form uniform mixing;
adding the mixed component C, and homogenizing;
and adding the component D to obtain the liquid crystal composition.
According to a second aspect of the invention, in some embodiments of the invention, the component a is glycerol, water and MONTANOV 202; the component B is caprylic/capric triglyceride, jojoba oil and behenyl alcohol; the component C comprises carbomer 940, EDTA disodium and water; the component D is triethanolamine and phenoxyethanol.
According to a second aspect of the present invention, in some embodiments of the present invention, the component A, the component B and the component C are heated to be completely dissolved at 75-85 ℃ before use.
In some embodiments of the invention, the component a, component B and component C are all heated to complete dissolution at 80 ℃ prior to use.
According to the second aspect of the present invention, in some embodiments of the present invention, the homogenization conditions are 6000 to 12000rpm, and the homogenization time is 3 to 5 min.
According to a second aspect of the present invention, in some embodiments of the present invention, the particle size in the liquid crystal composition is 3 to 10 μm.
In some preferred embodiments of the present invention, the preparation method specifically comprises:
respectively stirring the component A and the component B at the temperature of 80-82 ℃ until the components are completely dissolved, and slowly injecting the component B into the component A to form uniform mixing. And slowly adding the same component C which is stirred under the condition of 80-82 ℃ until the component C is completely dissolved, stirring while adding, homogenizing at 6000-12000 rpm for 3-5 min, continuously stirring until the temperature is cooled to about 55 ℃, adding the component D, stirring until the temperature is cooled to room temperature (25-30 ℃), and thus obtaining the liquid crystal composition.
The inventor finds that the liquid crystal composition prepared by the method for preparing the liquid crystal composition has liquid crystal content and liquid crystal density which are remarkably superior to those of the liquid crystal composition prepared by the traditional method or the conventional method no matter what proportion or content of the liquid crystal composition formula is adopted.
In a third aspect of the present invention, a liquid crystal type cosmetic is provided, which comprises the liquid crystal composition according to the first aspect of the present invention or the liquid crystal composition prepared by the preparation method according to the second aspect of the present invention.
According to a third aspect of the present invention, in some embodiments of the present invention, the liquid crystal-type cosmetic further comprises an efficacy active.
In some preferred embodiments of the present invention, the efficacy of the efficacy active preferably comprises at least one of the following (1) to (4):
(1) moisture preservation;
(2) anti-aging;
(3) relieving;
(4) and (5) repairing.
According to a third aspect of the present invention, in some embodiments of the present invention, the cosmetic preferably comprises a lotion, an emulsion, a cream, a mask.
Of course, the person skilled in the art can process the cosmetic product into other forms according to the actual use requirements.
In a fourth aspect of the present invention, there is provided a use of the liquid crystal composition according to the first aspect of the present invention or the liquid crystal composition prepared by the preparation method according to the second aspect of the present invention in the preparation of cosmetics.
The invention has the beneficial effects that:
1. the liquid crystal composition has the advantages of easy acquisition of raw materials, small using amount and unique and irreplaceable property, and can stimulate the mutual enhancement effect among the raw materials.
2. The liquid crystal composition disclosed by the invention is simple in preparation method and low in preparation difficulty, and the prepared liquid crystal composition has uniform particles and bright liquid crystal effect by combining D-phase emulsification with a phase inversion emulsification process, has a better preparation effect compared with a traditional method, and has a very high application value.
3. The liquid crystal cosmetic prepared based on the liquid crystal composition has uniform emulsion particle size, and the particle size range is only 3-10 mu m, so that the using effect of the liquid crystal cosmetic can be effectively promoted.
Drawings
FIG. 1 is a 100 Ximage of a liquid crystal composition prepared using a conventional formulation, wherein A is the method of the present example and B is a conventional method;
FIG. 2 is a 500 Ximage of a liquid crystal composition prepared using a conventional formulation, wherein A is the method of the present example and B is a conventional method;
FIG. 3 is a 100 Ximage of a liquid crystal composition prepared using the formulation of example 1, wherein A is the method of the present example and B is the conventional method;
FIG. 4 is a 500 Ximage of a liquid crystal composition prepared using the formulation of example 1, wherein A is the method of the present example and B is the conventional method;
FIG. 5 shows a 100 Ximage of a liquid crystal composition prepared using the formulation of example 2, wherein A is the method of the present example and B is the conventional method;
FIG. 6 is a 500 Ximage of a liquid crystal composition prepared using the formulation of example 2, wherein A is the method of the present example and B is the conventional method;
FIG. 7 is a 100 Ximage of a liquid crystal composition prepared using the formulation of example 3, wherein A is the method of the present example and B is the conventional method;
FIG. 8 is a 500 Ximage of a liquid crystal composition prepared using the formulation of example 3, wherein A is the method of the present example and B is the conventional method;
FIG. 9 shows a 100 Ximage of a liquid crystal composition prepared using the formulation of example 4, wherein A is the method of the present example and B is the conventional method;
FIG. 10 is a 500 Ximage of a liquid crystal composition prepared using the formulation of example 4, wherein A is the method of the present example and B is the conventional method;
FIG. 11 is a drawing showing a liquid crystal composition prepared under the method of this example using the formulation of this example 5, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 12 shows a liquid crystal composition prepared under the method of this example using the formulation of this example 6, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 13 is a drawing showing a liquid crystal composition prepared under the process of this example using the formulation of this example 7, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 14 is a view showing a liquid crystal composition prepared under the process of this example using the formulation of this example 8, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 15 is a drawing showing a liquid crystal composition prepared under the process of this example using the formulation of this example 9, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 16 is a drawing showing a liquid crystal composition prepared under the method of this example using the formulation of this example 10, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 17 is a drawing showing a liquid crystal composition prepared under the process of this example using the formulation of this example 11, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 18 is a drawing showing a liquid crystal composition prepared under the process of this example using the formulation of this example 12, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 19 is a drawing showing a liquid crystal composition prepared under the process of this example using the formulation of this example 13, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 20 is a drawing showing a liquid crystal composition prepared under the process of this example using the formulation of this example 14, wherein A is 100 Ximage and B is 500 Ximage;
FIG. 21 is a liquid crystal image of liquid crystal compositions prepared by different methods after being left at high temperature for 7 days, wherein A is the formulation of example 1, B is the formulation of example 2, C is the formulation of example 4, and D is the formulation of example 9;
FIG. 22 is a liquid crystal image of liquid crystal compositions prepared by different methods after 14 days of high temperature exposure, wherein A is the formulation of example 1, B is the formulation of example 2, C is the formulation of example 4, and D is the formulation of example 9;
FIG. 23 is a liquid crystal image of liquid crystal compositions prepared by different methods after being left for 21 days at high temperature, wherein A is the formulation of example 1, B is the formulation of example 2, C is the formulation of example 4, and D is the formulation of example 9;
FIG. 24 shows liquid crystal images of liquid crystal compositions prepared by different methods after being left at high temperature for 30 days, wherein A is the formulation of example 1, B is the formulation of example 2, C is the formulation of example 4, and D is the formulation of example 9.
Detailed Description
In order to make the objects, technical solutions and technical effects of the present invention more clear, the present invention will be described in further detail with reference to specific embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The experimental materials and reagents used are, unless otherwise specified, all consumables and reagents which are conventionally available from commercial sources.
Example 1
The liquid crystal composition raw materials and the contents thereof in this example are shown in table 1.
The preparation method comprises the following steps:
respectively stirring the components A and B at 80 ℃ until the components A and B are completely dissolved, and slowly injecting the component B into the component A to form uniform mixing. And slowly adding the same component C which is stirred under the condition of 80 ℃ until the component C is completely dissolved, stirring while adding, homogenizing at 6000rpm for 5min, then continuously stirring until the temperature is cooled to about 55 ℃, adding the component D, stirring until the temperature is cooled to room temperature (25-30 ℃), and thus obtaining the liquid crystal composition.
Example 2
The liquid crystal composition raw materials and the contents thereof in this example are shown in table 1.
The preparation method comprises the following steps:
respectively stirring the components A and B at 80 ℃ until the components A and B are completely dissolved, and slowly injecting the component B into the component A to form uniform mixing. And slowly adding the same component C which is stirred under the condition of 80 ℃ until the component C is completely dissolved, stirring while adding, homogenizing at 12000rpm for 3min, then continuously stirring until the temperature is cooled to about 55 ℃, adding the component D, stirring until the temperature is cooled to room temperature (25-30 ℃), and thus obtaining the liquid crystal composition.
Example 3
The liquid crystal composition raw materials and the contents thereof in this example are shown in table 1.
The preparation method comprises the following steps:
respectively stirring the components A and B at 80 ℃ until the components A and B are completely dissolved, and slowly injecting the component B into the component A to form uniform mixing. And slowly adding the same component C which is stirred under the condition of 80 ℃ until the component C is completely dissolved, stirring while adding, homogenizing at 12000rpm for 3min, then continuously stirring until the temperature is cooled to about 55 ℃, adding the component D, stirring until the temperature is cooled to room temperature (25-30 ℃), and thus obtaining the liquid crystal composition.
Example 4
The liquid crystal composition raw materials and the contents thereof in this example are shown in table 1.
The preparation method comprises the following steps:
respectively stirring the components A and B at 80 ℃ until the components A and B are completely dissolved, and slowly injecting the component B into the component A to form uniform mixing. And slowly adding the same component C which is stirred under the condition of 80 ℃ until the component C is completely dissolved, stirring while adding, homogenizing at 12000rpm for 3min, then continuously stirring until the temperature is cooled to about 55 ℃, adding the component D, stirring until the temperature is cooled to room temperature (25-30 ℃), and thus obtaining the liquid crystal composition.
TABLE 1 raw materials and contents of liquid crystal compositions in examples 1 to 4
Figure BDA0003210725660000071
Effect comparison experiment between traditional liquid crystal preparation method and liquid crystal preparation method in this embodiment
In order to effectively illustrate the advantages of the liquid crystal preparation method in the embodiment of the present invention, the inventor adopted the same group of raw material formulations with the same content to prepare the liquid crystal composition by using the conventional liquid crystal preparation method and the liquid crystal preparation method in the embodiment, respectively.
(1) The formula of the traditional liquid crystal preparation method is as follows:
in order to remove the selectivity of the formula raw materials to the process, a formula which is suitable for the traditional liquid crystal preparation method is specially used as an experimental raw material formula, and the formula comprises the following components in percentage by weight:
the formula comprises the following components in percentage by mass: cetyl/stearyl alcohol 1%, white oil (mineral oil) 15%, M68 emulsifier (cetearyl alcohol/cetearyl glucoside) 3%, a165 emulsifier (glyceryl stearate/PEG-100 stearate) 1%, carbomer 9400.1%, glycerin 3%, disodium EDTA 0.1%, triethanolamine 0.1%, phenoxyethanol 0.2%, water 76.5%.
Experimental groups: the experimental group adopts the preparation method in the above embodiment, and the hexadecanol/octadecanol, the M68 emulsifier and a small amount of water are stirred at 80 ℃ until being completely dissolved, so as to obtain a component A; stirring white oil and A165 emulsifier at 80 deg.C until completely dissolved to obtain component B, and slowly injecting component B into component A to form uniform mixture. And slowly adding the same mixed solution of the EDTA disodium, the carbomer 940 and the water which is stirred under the condition of 80 ℃ until the EDTA disodium, the carbomer 940 and the water are completely dissolved, stirring while adding, homogenizing at 5000rpm for 5min, continuously stirring until the temperature is cooled to about 55 ℃, adding triethanolamine and phenoxyethanol, stirring until the temperature is cooled to room temperature (25-30 ℃), and thus obtaining the liquid crystal composition.
Control group: the control group adopts a traditional liquid crystal preparation method, and the preparation method comprises the following steps:
(1) preparing an oil phase solution:
and uniformly stirring the hexadecanol/octadecanol, the white oil, the M68 emulsifier and the A165 emulsifier at 75-85 ℃ to form a uniform oil phase solution.
(2) Preparing an aqueous phase solution:
mixing carbomer, glycerol and water, stirring uniformly, and heating to 75-85 ℃ to form a uniform water phase solution.
(3) Adding the water phase solution in the step (2) into the oil phase solution in the step (1), homogenizing at 4500-5500 rpm for 3-8 minutes, and keeping the temperature at 75-85 ℃.
(4) Stirring until the temperature is cooled to 45-55 ℃, adding EDTA disodium, triethanolamine and phenoxyethanol, and continuing stirring for 3-8 minutes.
(5) And stopping stirring when the temperature is reduced to 35-45 ℃ to obtain the liquid crystal composition.
The liquid crystal structures of the two sets of prepared liquid crystal compositions were observed using a microscope (Ci-POL polarization microscope, available from NIKON), the pixels in the images were analyzed using PHOTOSHOP software, and the pixels of the liquid crystal portion were calculated.
Wherein, the calculation formula of the liquid crystal content is as follows:
Figure BDA0003210725660000081
wherein, L is the liquid crystal content;
Pcpixels which are part of the image of the liquid crystal;
Pga pixel of an image.
The results are shown in FIGS. 1 and 2.
As shown in fig. 1, in the case where the magnification was 100 times, it can be seen that the liquid crystal density was higher and the uniformity was better in the experimental group than in the control group. After the amplification is further increased to 500 times, it is obvious that the content of the liquid crystal in the experimental group is higher and the brightness of the liquid crystal is higher compared with the control group, and therefore, it can be shown that under the condition of the same formula, the liquid crystal preparation method in the above embodiment can obviously prepare the liquid crystal composition with higher liquid crystal quality.
Meanwhile, according to the original description of the conventional liquid crystal preparation method (CN 111000733 a), the liquid crystal content is: 25.3% (formulation in example 21 with the best results). In order to avoid the difference of shooting devices and the difference of using the picture magnification ratio, the inventor recalculates the comparison group according to the embodiment, and finds that the liquid crystal content in the comparison group is as follows: 54.30%, the liquid crystal content in the above examples is: 73.61%, the liquid crystal content was significantly increased compared to the control.
(2) The formulation in the above example was used:
in order to further verify the effects of the conventional liquid crystal preparation method and the liquid crystal preparation method in this example, the process selectivity of the formulation raw materials was removed, and the liquid crystal composition was prepared by using the conventional liquid crystal preparation method and the liquid crystal preparation method in this example again using the 4-component formulation shown in table 1 as the experimental raw material formulation.
The traditional liquid crystal preparation method comprises the following steps:
(1) preparing an oil phase solution:
and (3) uniformly stirring the M202, the GTCC, the jojoba oil and the behenyl alcohol at 75-85 ℃ to form a uniform oil phase solution.
(2) Preparing an aqueous phase solution:
mixing carbomer, glycerol and water, stirring uniformly, and heating to 75-85 ℃ to form a uniform water phase solution.
(3) Adding the water phase solution in the step (2) into the oil phase solution in the step (1), and homogenizing at the same rotating speed and the same time as those of the embodiments 1-4, and keeping the temperature at 75-85 ℃.
(4) Stirring until the temperature is cooled to 45-55 ℃, adding EDTA disodium, triethanolamine and phenoxyethanol, and continuing stirring for 3-8 minutes.
(5) And stopping stirring when the temperature is reduced to 35-45 ℃ to obtain the liquid crystal composition.
The liquid crystal preparation method in this embodiment refers to the above embodiments 1 to 4.
The liquid crystal structures of the two sets of prepared liquid crystal compositions were observed using a microscope (Ci-POL polarization microscope, available from NIKON), the pixels in the images were analyzed using PHOTOSHOP software, and the pixels of the liquid crystal portion were calculated.
Wherein, the calculation formula of the liquid crystal content is as follows:
Figure BDA0003210725660000091
wherein, L is the liquid crystal content;
Pcpixels which are part of the image of the liquid crystal;
Pga pixel of an image.
The results are shown in Table 2 and FIGS. 3 to 10.
TABLE 2 difference in liquid crystal content and particle size in liquid crystal compositions prepared by different methods
Figure BDA0003210725660000092
Figure BDA0003210725660000101
It can be found that, in the conventional liquid crystal preparation method, the liquid crystal content of the liquid crystal composition prepared by the method is far lower than that of the liquid crystal composition prepared by the liquid crystal preparation method in the above examples, regardless of the formula. By matching the liquid crystal preparation method in the embodiment with the formula, the liquid crystal content of the prepared liquid crystal composition can reach 89.69%, and the lowest liquid crystal content is obviously different from the highest liquid crystal content obtained by the traditional liquid crystal preparation method, so that the liquid crystal preparation method in the embodiment is far superior to the existing liquid crystal preparation technology.
Liquid crystal type cosmetic based on liquid crystal composition in above embodiment
In order to effectively illustrate the applicability of the liquid crystal composition in the above examples, the inventors formulated various cosmetics based on the liquid crystal composition (examples 5 to 8), and examined the actual liquid crystal effect in cosmetics of different components and contents.
The liquid crystal type cosmetic raw materials and the contents thereof in examples 5 to 8 are shown in Table 3.
Table 3 content of liquid crystal type cosmetic raw material components based on liquid crystal compositions in the above examples
Figure BDA0003210725660000102
Figure BDA0003210725660000111
The preparation method of the liquid crystal type cosmetic in examples 5 to 8 is:
respectively stirring the components A and B at 80 ℃ until the components A and B are completely dissolved, and slowly injecting the component B into the component A to form uniform mixing. And slowly adding the same component C which is stirred under the condition of 80 ℃ until the component C is completely dissolved, stirring while adding, homogenizing at 6000-12000 rpm for 3-5 min, then continuously stirring until the temperature is cooled to about 55 ℃, adding the component D, stirring until the temperature is cooled to room temperature (25-30 ℃), and thus obtaining the liquid crystal composition.
The liquid crystal content was measured in the same manner as in the above examples.
The results are shown in Table 4 and FIGS. 11 to 14.
TABLE 4 liquid Crystal content in liquid Crystal type cosmetics in examples 5 to 8
Formulation composition Liquid Crystal content (%) Particle size range (μm)
Example 5 69.90% 3-5
Example 6 75.48% 5-10
Example 7 61.15% 3-5
Example 8 80.57% 7-9
As can be seen from fig. 11 to 14, the addition of some components has a certain influence on the liquid crystal content of the whole liquid crystal type cosmetic, which is mainly reflected in the added humectant type (the addition of 1, 3-butanediol is reflected in synergy, and the addition of 1, 2-pentanediol is reflected in antagonism), but it can be found that the liquid crystal content of the liquid crystal type cosmetic containing different humectant types is different, but the liquid crystal content can still be maintained at a high liquid crystal content level of 61.01 to 80.57%.
The inventor also prepares another group of cosmetics based on the liquid crystal composition (examples 9-14) to repeatedly verify the actual liquid crystal effect in cosmetics with different components and contents.
The liquid crystal cosmetic materials of examples 9 to 14 and the contents thereof are shown in Table 5.
Table 5 content of liquid crystal type cosmetic raw material components based on liquid crystal compositions in the above examples
Figure BDA0003210725660000112
Figure BDA0003210725660000121
Figure BDA0003210725660000131
The liquid crystal cosmetics of examples 9 to 14 were prepared in the same manner as in examples 5 to 8.
The liquid crystal content was measured in the same manner as in the above examples.
The results are shown in Table 6 and FIGS. 15 to 20.
TABLE 6 liquid Crystal content in liquid Crystal type cosmetics in examples 9 to 14
Formulation composition Liquid Crystal content (%) Particle size range (μm)
Example 9 56.08% 3-5
Example 10 50.93% 3-6
Example 11 55.74% 3-6
Example 12 55.35% 3-6
Example 13 61.73% 3-5
Example 14 58.57% 3-5
As can be seen from fig. 15 to 20, the substitution of the components in the liquid crystal composition, particularly the substitution of the thickener, has a great influence on the liquid crystal content of the entire liquid crystal type cosmetic composition based on the liquid crystal composition. It can be found that the actual liquid crystal content of the liquid crystal type cosmetic after replacing the thickener is only 50.93-61.73%, and the whole content is lower than that of examples 1-8, therefore, it can be shown that the component formula in the application has irreplaceable property, and the effect can be affected by replacing the components by similar components or the like.
Liquid crystal stability detection
To further analyze the effect of the liquid crystal compositions prepared by the liquid crystal composition preparation processes in the examples of the present invention on the functionality of liquid crystal type cosmetics, the inventors prepared the formulations in examples 1,2, 4 and 9, respectively, by the liquid crystal composition preparation methods in the examples of the present invention and the conventional liquid crystal preparation methods, respectively, and left them under high temperature extreme environment (temperature set at 48 ℃) for 7, 14, 21 and 30 days, respectively, and observed the change of liquid crystal content and density under a microscope.
The results are shown in FIGS. 21 to 24.
It can be seen that, from the formulation point of view, in 4 examples, the composition prepared from the formulation of example 2 has the best liquid crystal content under the same standing time condition, and the liquid crystal distribution and density in the visual field are better than those of other examples. From the viewpoint of the manufacturing method, it can be found that the composition produced by the conventional manufacturing method is significantly less in liquid crystal content than the method in the examples of the present invention. Moreover, it was found that the liquid crystal content of the liquid crystal composition prepared by the conventional method decreased significantly with the increase of the standing time, and particularly, the distribution and density of the liquid crystal within the visual field showed a noticeable change (decrease) after 14 days of standing, whereas the method in the examples of the present invention showed a slight decrease in the distribution within the visual field after 21 days and 30 days of standing, but the decrease was small in magnitude and insignificant in amount change as observed in the visual field, which was a negligible case.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. The liquid crystal composition is characterized in that raw materials for preparing the liquid crystal composition comprise glycerol, caprylic/capric triglyceride, jojoba oil, carbomer 940 and an emulsifier;
the emulsifier preferably comprises at least one of arachidyl alcohol/docosanol/arachidyl glucoside, cetearyl alcohol/cetearyl glucoside, cetearyl alcohol/cocoyl glucoside, behenyl alcohol, hydrogenated lecithin, sodium stearyl glutamate and polyglycerol-10-stearate.
2. The liquid crystal composition of claim 1, wherein the raw materials for preparing the liquid crystal composition further comprise at least one of cosmetic conventional adjuvants and water;
the cosmetic conventional adjuvant preferably includes at least one of disodium EDTA, triethanolamine, phenoxyethanol and citric acid, sodium citrate, and methylparaben.
3. The liquid crystal composition of any one of claims 1-2, wherein the liquid crystal composition is prepared from glycerol, arachidyl alcohol/docosanol/arachidyl alcohol glucoside, caprylic/capric triglyceride, jojoba oil, behenyl alcohol, carbomer 940, disodium EDTA, triethanolamine, phenoxyethanol, and water.
4. The liquid crystal composition of claim 3, wherein the liquid crystal composition comprises, by mass, 5 to 10 parts of glycerol, 1 to 2 parts of peanut alcohol/docosanol/peanut alcohol glucoside, 3 to 5 parts of caprylic/capric triglyceride, 3 to 5 parts of jojoba oil, 1 to 2 parts of behenyl alcohol, 0.1 to 0.2 part of carbomer 940, 0.01 to 0.1 part of disodium EDTA, 0.1 to 0.2 part of triethanolamine, 0.1 to 0.2 part of phenoxyethanol, and 74 to 83 parts of water.
5. A method for preparing a liquid crystal composition, comprising the steps of:
injecting the component B into the mixed component A;
adding the mixed component C, and homogenizing;
adding the component D to obtain a liquid crystal composition;
wherein the component A is glycerol, water and arachidonol/docosanol/arachidonol glucoside;
the component B is caprylic/capric triglyceride, jojoba oil and behenyl alcohol;
the component C comprises carbomer 940, EDTA disodium and water;
the component D is triethanolamine and phenoxyethanol.
6. The preparation method according to claim 5, wherein the component A, the component B and the component C are heated to be completely dissolved at 75-85 ℃ before use.
7. The method according to claim 5, wherein the homogenizing is carried out at 6000 to 12000rpm for 3 to 5 min.
8. The method according to claim 5, wherein the particle size of the liquid crystal composition is 3 to 10 μm.
9. A liquid crystal cosmetic, which is characterized by comprising the liquid crystal composition as defined in any one of claims 1 to 4 or the liquid crystal composition prepared by the preparation method as defined in any one of claims 5 to 8;
the liquid crystal type cosmetic preferably further contains an efficacy active substance.
10. Use of the liquid crystal composition according to any one of claims 1 to 4 or the liquid crystal composition prepared by the preparation method according to any one of claims 5 to 8 for preparing cosmetics.
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