Composite emulsifier, its preparation method and application

Abstract

The application discloses a composite emulsifier and a preparation method and application thereof, and belongs to the field of daily chemical products. The emulsifier does not contain a polyethylene glycol structure, is safe and non-toxic, and based on specific collocation of components, can form a liquid crystal structure which is still stable at a normal temperature of 35-37 DEG C of human skin after the product is applied to an emulsion, and has excellent moisturizing performance.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of daily chemical products, in particular to a composite emulsifier and its preparation method and application. BACKGROUND

[0002] Emulsifiers are often used in skin care products and cosmetics, which can form stable emulsion mixtures of incompatible components, and different emulsifiers can form different emulsion structures according to the difference in molecular structure, which mainly includes oil-in-water emulsion with oil phase as dispersed phase and water phase as continuous phase, and water-in-oil emulsion with water phase as dispersed phase and oil phase as continuous phase, corresponding to oil-in-water emulsifier and water-in-oil emulsifier. In the cream, emulsion dosage form of cosmetics, the emulsion configuration is basically oil-in-water, and the structure of the corresponding oil-in-water emulsifier is relatively simple: in the oil-water interface, the lipophilic group of the emulsifier faces the oil droplet, and the hydrophilic group faces the water phase and arranges on the surface of the oil droplet. However, after the emulsion of this configuration is applied to the skin, the water in the external phase will quickly evaporate, resulting in a rapid decrease in the moisturizing effect of the emulsion. It is found that some specific emulsifier molecules can form a layered liquid crystal structure at the oil-water interface in the emulsion system. This layered intermediate structure, which combines the properties of crystals and liquids, is similar to the liquid crystal structure of the lipid between the cells of the stratum corneum of the human skin, has better skin-friendliness, and the emulsion containing this structure has a long-lasting moisturizing effect when applied to the skin. At the same time, the layered liquid crystal structure can also preserve the active skin care ingredients in the emulsion from being oxidized by the outside world, so that they can effectively exert their efficacy.

[0003] However, the emulsifiers that can form a layered liquid crystal in the emulsion type cosmetics are quite strict in composition, and if the composition is too simple, it is difficult to achieve the ideal layered liquid crystal effect. In order to solve the problem of incomplete formation of liquid crystal structure, low stability and low formula applicability of single component emulsifiers, commercial liquid crystal emulsifiers often introduce complex components, but the liquid crystal structure formed by such products is basically stable at room temperature, and will be converted into a liquid with disordered arrangement as the temperature rises. The normal temperature of human skin is between 35-37℃, which is much higher than room temperature, so the liquid crystal structure in such products cannot exist stably on the skin surface in actual application, and does not exert the expected efficacy. On the other hand, most of the emulsifiers that can form liquid crystal structure are fatty alcohol polyoxyethylene ether emulsifiers, but such products contain polyethylene glycol structure in their molecular structure, which inevitably brings potential risk of dioxane, and long-term use may cause safety problems to human skin and health. SUMMARY

[0004] Based on the defects existing in the prior art, the purpose of the present application is to provide a composite emulsifier which does not contain a polyethylene glycol structure, is safe and non-toxic, and based on the specific collocation of components, the product can form a liquid crystal structure that is still stable at a normal human skin temperature of 35-37℃ after being applied to an emulsion, the limit temperature of experimental test can reach 45℃, and has excellent moisturizing performance.

[0005] In order to achieve the above purpose, the technical scheme adopted by the present application is:

[0006] A composite emulsifier, comprising the following components by weight:

[0007] Glycerin di-stearate 10-50 parts, polyglyceryl stearate 15-45 parts, behenyl alcohol 15-25 parts, glyceryl stearate citrate 10-20 parts, sterol 1-9 parts, and soybean glyceride 0.1-1 part.

[0008] Since the emulsifiers used in the preparation of emulsion products in the prior art are claimed to be "liquid crystal emulsifiers", but the liquid crystal structure stabilizers formed by their preparation are poor, they cannot be stably generated and maintained on the surface of human skin, and such emulsifiers often contain a polyethylene glycol structure, which has been defined as an "orange" component by some cosmetic industry organizations, indicating that these components may cause harm to human health if used for a long time, and even have a risk of causing cancer. The composite emulsifier described in the present application can effectively form a clear lamellar liquid crystal structure in the emulsion without introducing a polyethylene glycol structure component, and the structure can maintain stability at a normal human skin temperature of 35-37℃, and can maintain long-term skin care activity when used on the skin. At the same time, the product has wide applicability and can maintain the generation and stability of the liquid crystal structure in various emulsion systems of different oils, moisturizers, and thickening agents.

[0009] Meanwhile, through experimental tests, the formula composition and ratio composition of the composite emulsifier have obvious specificity, and if one component is replaced with a conventional type (for example, the behenyl alcohol is replaced with hexadecanol which is often used in conventional emulsifiers) or the addition ratio of one component is adjusted to be out of the limited range, the product may not form a liquid crystal structure in the human skin temperature range. On the other hand, since the product needs to be applied in the field of skin care cosmetics, the emulsion formed thereby needs to maintain normal use experience, and since the main role of the composite emulsifier also includes regulating the viscosity and component dispersion of the emulsion product, if the formula is not properly controlled, the product may have a high viscosity and even a grainy feeling when being applied, and cannot achieve a passing use experience. The polyglyceryl stearate is a kind of multi-hydroxy ester non-ionic surfactant, has an amphiphilic structure (both hydrophilic structure and lipophilic structure) in the molecule, and thus is used as a main emulsifier in the composite emulsifier to stabilize the water phase and oil phase components. The glycerol distearate and glycerol stearate citrate are used as co-emulsifiers, and based on the different HLB values from the main emulsifier, can effectively enhance the interface film formed by the main emulsifier, further improve the stability of the formed cream, and finally jointly act on the water-oil interface to form a stable lamellar liquid crystal structure. The behenyl alcohol in the product components mainly plays a regulating role in the formation of the liquid crystal structure, increases the order degree and stability of the liquid crystal bilayer arrangement. Meanwhile, the behenyl alcohol is an excellent emollient and can moisturize the skin and improve the moisturizing feeling of the cream. The sterol has similar properties to the cholesterol in the human cell lipid, has a special cyclopentane polyhydrogenophenanthrene structure in the molecule, has a thermodynamic affinity to the bilayer structure of the lamellar liquid crystal, has an influence on the structure and dynamic behavior of the bilayer, and can make the formed liquid crystal structure more uniform and complete.

[0010] Preferably, the polyglyceryl stearate includes polyglyceryl-10 penta stearate and polyglyceryl-6 stearate.

[0011] More preferably, the composite emulsifier includes the following components in parts by weight:

[0012] The glycerol distearate is 10-50 parts, the polyglyceryl-10 penta stearate is 10-30 parts, the polyglyceryl-6 stearate is 5-15 parts, the behenyl alcohol is 15-25 parts, the glycerol stearate citrate is 10-20 parts, the sterol is 1-9 parts, and the soybean glyceride is 0.1-1 part.

[0013] Through many experiments of the inventor, it is found that when the polyglyceryl stearate is introduced into the product in the above two compounded forms and under the compounded ratio, the product can achieve the most ideal liquid crystal structure effect.

[0014] Preferably, the sterol is at least one of phytosterols, beta-sitosterol, and cholesterols.

[0015] More preferably, the sterol is phytosterols.

[0016] More preferably, the phytosterols are at least one of soy sterol and pine-derived steryl.

[0017] The sterol is a common cosmetic additive ingredient with obvious bioactivity effects. In the compound emulsifier, the sterol is an indispensable component for the product to form a liquid crystal structure in the emulsion. When the plant-derived sterol is used, the liquid crystal structure with high moisturizing effect can effectively assist the liquid crystal in the emulsion to rapidly penetrate the skin surface and form a moisturizing barrier, and the skin care effect is better.

[0018] Preferably, the compound emulsifier comprises the following components in the weight parts per 100 parts:

[0019] polyglyceryl-10 penta stearate 14-25 parts, polyglyceryl-6 stearate 8-12 parts, behenyl alcohol 16-24 parts, glyceryl stearate citrate 12-16 parts, phytosterols 3-7 parts, soy glycerides 0.1-0.2 parts, and the rest is glyceryl distearate.

[0020] It is found through repeated verification by the inventor that when the components of the product synergistically act in the above ratio, the product can not only form a clear Maltese cross structure at room temperature, but also has more and more complete liquid crystal structure in the emulsion product when the environmental temperature reaches 37℃, which is the human skin temperature, and the product has good use experience.

[0021] More preferably, the compound emulsifier comprises the following components in the weight parts per 100 parts:

[0022] polyglyceryl-10 penta stearate 14-25 parts, polyglyceryl-6 stearate 8-12 parts, behenyl alcohol 16-24 parts, glyceryl stearate citrate 12-16 parts, phytosterols 3-7 parts, soy glycerides 0.1-0.2 parts, and the rest is glyceryl distearate.

[0023] Another object of the present application is to provide a preparation method of the compound emulsifier, comprising the following steps:

[0024] The components are heated to dissolve and uniformly mixed, then granulated, and cooled to obtain the compound emulsifier.

[0025] The processing method of the compound emulsifier product is similar to that of the conventional emulsifier product, and no special equipment and processing conditions are required, and industrial scale production can be realized.

[0026] Another object of the present application is to provide the use of the composite emulsifier in the preparation of cosmetics.

[0027] Still another object of the present application is to provide a cream, the components of which include the composite emulsifier of the present application.

[0028] The composite emulsifier of the present application, which can form a stable liquid crystal structure at the temperature of human skin, can not only generate a high-stability liquid crystal layer in the emulsion, but also make the emulsion droplets uniform, and further obtain a cream product with good use experience, as compared to other commonly used emulsifiers such as lecithin and alkyl glycoside emulsifiers.

[0029] Preferably, the mass percentage content of the composite emulsifier in the cream is 4-6 wt%.

[0030] According to the existing common cream product formula, in addition to the emulsifier, there are also synergistic emulsification components such as squalane and glycerol, thickening components, and skin care active ingredients, so the composite emulsifier of the present application can be added in a conventional amount according to the actual component composition and performance requirements, and when the above-mentioned amount is added, the comprehensive stability of the product is better.

[0031] The present application has the advantages that the present application provides a composite emulsifier, a preparation method and application thereof. The composite emulsifier does not contain polyethylene glycol structure, is safe and non-toxic, and based on the specific collocation of components, can form a stable liquid crystal structure at the normal temperature of human skin of 35-37℃ after being applied to an emulsion, and has excellent moisturizing performance. BRIEF DESCRIPTION OF DRAWINGS

[0032] Figure 1 The polarized light microscope photo of the cream prepared by the composite emulsifier of Example 1 of the present application at 25℃.

[0033] Figure 2 The polarized light microscope photo of the cream prepared by the composite emulsifier of Example 1 of the present application at 37℃.

[0034] Figure 3 The polarized light microscope photo of the cream prepared by the composite emulsifier of Example 2 of the present application at 25℃.

[0035] Figure 4 The polarized light microscope photo of the cream prepared by the composite emulsifier of Example 2 of the present application at 37℃.

[0036] Figure 5 The polarized light microscope photo of the cream prepared by the composite emulsifier of Example 3 of the present application at 25℃.

[0037] Figure 6 Polarized light microscope photograph of the cream prepared by using the composite emulsifier according to the embodiment 3 of the present application, taken at 37℃.

[0038] Figure 7 Polarized light microscope photograph of the cream prepared by using the commercial lecithin emulsifier according to the effect example 1 of the present application, taken at 25℃.

[0039] Figure 8 Polarized light microscope photograph of the cream prepared by using the commercial lecithin emulsifier according to the effect example 1 of the present application, taken at 37℃.

[0040] Figure 9 Polarized light microscope photograph of the cream prepared by using the commercial alkyl glycoside emulsifier according to the effect example 1 of the present application, taken at 25℃.

[0041] Figure 10 Polarized light microscope photograph of the cream prepared by using the commercial alkyl glycoside emulsifier according to the effect example 1 of the present application, taken at 37℃.

[0042] Figure 11 Polarized light microscope photograph of the cream prepared by using the commercial sucrose ester emulsifier according to the effect example 1 of the present application, taken at 25℃.

[0043] Figure 12 Polarized light microscope photograph of the cream prepared by using the commercial sucrose ester emulsifier according to the effect example 1 of the present application, taken at 37℃.

[0044] Figure 13 Polarized light microscope photograph of the cream prepared by using the commercial amino acid emulsifier according to the effect example 1 of the present application, taken at 25℃.

[0045] Figure 14 Polarized light microscope photograph of the cream prepared by using the commercial amino acid emulsifier according to the effect example 1 of the present application, taken at 37℃.

[0046] Figure 15 Polarized light microscope photographs of the cream prepared by using the composite emulsifier according to the embodiment 1 of the present application, taken at 25℃, 35℃, 37℃ and 45℃, respectively.

[0047] Figure 16 Test result chart of the moisturizing effect test of the cream prepared by using the composite emulsifier according to the embodiment 1 of the present application and the comparative cream prepared by using PEG-55 stearate.

[0048] Figure 17 Test result chart of the moisturizing effect test of the cream prepared by using the composite emulsifiers according to the embodiments 1 to 3 of the present application.

[0049] Figure 18Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 4 of the present invention taken at 25°C.

[0050] Figure 19 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 4 of the present invention taken at 37°C.

[0051] Figure 20 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 5 of the present invention taken at 25°C.

[0052] Figure 21 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 5 of the present invention taken at 37°C.

[0053] Figure 22 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 6 of the present invention taken at 25°C.

[0054] Figure 23 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 6 of the present invention taken at 37°C.

[0055] Figure 24 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 7 of the present invention taken at 25°C.

[0056] Figure 25 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 7 of the present invention taken at 37°C.

[0057] Figure 26 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 8 of the present invention taken at 25°C.

[0058] Figure 27 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 8 of the present invention taken at 37°C.

[0059] Figure 28 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 9 of the present invention taken at 25°C.

[0060] Figure 29 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Example 9 of the present invention taken at 37°C.

[0061] Figure 30 Polarized light microscope photograph of the cream prepared using the composite emulsifier described in Comparative Example 2 of the present invention taken at 25°C.

[0062] Figure 31Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 2, taken at 25°C.

[0063] Figure 32 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 2, taken at 37°C.

[0064] Figure 33 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 2, taken at 37°C.

[0065] Figure 34 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 3, taken at 25°C.

[0066] Figure 35 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 3, taken at 37°C.

[0067] Figure 36 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 4, taken at 25°C.

[0068] Figure 37 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 4, taken at 37°C.

[0069] Figure 38 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 5, taken at 25°C.

[0070] Figure 39 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 5, taken at 37°C.

[0071] Figure 40 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 6, taken at 25°C.

[0072] Figure 41 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 6, taken at 37°C.

[0073] Figure 42 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 7, taken at 25°C.

[0074] Figure 43 Polarized microscope photograph of the cream prepared using the composite emulsifier according to the present application Comparative Example 7, taken at 37°C.

[0075] Figure 44The radar chart of the use experience test of the cream prepared from the composite emulsifier described in Example 1 and Comparative Example 4 of the present application. DETAILED DESCRIPTION

[0076] In order to better illustrate the purposes, technical solutions and advantages of the present application, the present application will be further described below in combination with specific examples and comparative examples, which are intended to understand the content of the present application in detail, rather than limiting the present application. All other examples obtained by those of ordinary skill in the art without making creative efforts fall within the protection scope of the present application. The experimental reagents, raw materials and instruments designed in the present application and comparative examples are all common ordinary reagents, raw materials and instruments unless otherwise specified. It should be noted that in the specific embodiments of the present application, the polarizing microscope photos of each example and comparative example are actually basically taken at the same or adjacent magnification, and only the software automatically arranges more appropriate scale marks according to the photo situation when the photo is generated.

[0077] It should be noted that the terms "include", "contain" and "have" in the specification and claims of the present application and the above-mentioned drawings are intended to cover the non-exclusive inclusion. For example, a process, method, system, product or device including a series of steps or units is not limited to the listed steps or units, but can optionally also include steps or units not listed, or can optionally also include other steps or units inherent to these processes, methods, products or devices. The terms such as "first" and "second" and the like in the claims, specification and drawings of the present application are only used to distinguish one entity / operation / object from another entity / operation / object, and do not necessarily require or imply any such actual relationship or order between the entities / operations / objects.

[0078] In the present application, the technical features described in an open manner include both the closed technical solution consisting of the listed features and the open technical solution including the listed features.

[0079] In the present application, if no special description is made, the numerical range is considered to be continuous and includes the minimum value and the maximum value of the range and each value between the minimum value and the maximum value. Further, when the range refers to an integer, each integer between the minimum value and the maximum value of the range is included. In addition, when multiple ranges are provided to describe a feature or a characteristic, the ranges can be combined. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all sub-ranges therein.

[0080] The raw reagents and processing devices used in the examples and comparative examples of the present application are commercially available conventional types if not specified. The phytosterols in the examples and comparative examples of the present application are commercially available soy sterols, and the soy glycerides are commercially available products.

[0081] The present application provides a composite emulsifier comprising the following components in parts by weight:

[0082] glyceryl distearate 10-50 parts, polyglyceryl stearate 15-45 parts, behenyl alcohol 15-25 parts, glyceryl stearate citrate 10-20 parts, sterol 1-9 parts, and soy glycerides 0.1-1 part.

[0083] In a specific embodiment, the polyglyceryl stearate comprises polyglyceryl-10 penta stearate and polyglyceryl-6 stearate;

[0084] Further preferably, the composite emulsifier comprises the following components in parts by weight:

[0085] glyceryl distearate 10-50 parts, polyglyceryl-10 penta stearate 10-30 parts, polyglyceryl-6 stearate 5-15 parts, behenyl alcohol 15-25 parts, glyceryl stearate citrate 10-20 parts, sterol 1-9 parts, and soy glycerides 0.1-1 part.

[0086] In a specific embodiment, the sterol is at least one of phytosterols, β-sitosterol, and cholesterols.

[0087] Further preferably, the sterol is phytosterols.

[0088] In a specific embodiment, the composite emulsifier comprises the following components in parts by weight per 100 parts:

[0089] polyglyceryl-10 penta stearate 14-25 parts, polyglyceryl-6 stearate 8-12 parts, behenyl alcohol 16-24 parts, glyceryl stearate citrate 12-16 parts, phytosterols 3-7 parts, soy glycerides 0.1-0.2 parts, and the balance of glyceryl distearate.

[0090] Further preferably, the composite emulsifier comprises the following components in parts by weight per 100 parts:

[0091] polyglyceryl-10 penta stearate 18-20 parts, polyglyceryl-6 stearate 8-12 parts, behenyl alcohol 18-22 parts, glyceryl stearate citrate 12-14 parts, phytosterols 4-6 parts, soy glycerides 0.1-0.2 parts, and the balance of glyceryl distearate.

[0092] In an embodiment, the composite emulsifier is used in the preparation of a cream, which comprises the following components in mass percentage: the composite emulsifier 4-6%, polydimethylsiloxane 8-12%, cyclopentasiloxane 8-12%, cetyl stearyl alcohol 2-4%, 1,3-butanediol 2-4%, glycerol 2-4%, hydroxyethyl cellulose 0.1-0.5%, and the rest water.

[0093] In an embodiment, the composite emulsifier is used in the preparation of a cream, which comprises the following components in mass percentage: the composite emulsifier 4-6%, squalane 8-12%, caprylic / capric triglyceride 8-12%, cetyl stearyl alcohol 2-4%, 1,3-butanediol 2-4%, glycerol 2-4%, hydroxyethyl cellulose 0.1-0.5%, and the rest water.

[0094] In an embodiment, the composite emulsifier is used in the preparation of a cream, which comprises the following components in mass percentage: the composite emulsifier 4-6%, caprylic / capric triglyceride 15-25%, cetyl stearyl alcohol 2-4%, 1,3-butanediol 2-4%, glycerol 2-4%, hydroxyethyl cellulose 0.1-0.5%, and the rest water.

[0095] In an embodiment, the composite emulsifier is used in the preparation of a cream, which comprises the following components in mass percentage: the composite emulsifier 4-6%, behenyl alcohol 1-2%, cetyl alcohol 1-3%, hydrogenated polydecene 4-6%, glyceryl tri(ethylhexanoate) 4-6%, dimethicone 1-3%, sodium phytate 0.01-0.1%, glycerol 1-3%, isopentyldiol 4-6%, acryloyldimethyltaurine ammonium / VP copolymer 0.1-1%, and the rest water.

[0096] The application is further illustrated in the following specific examples:

[0097] Example 1

[0098] An embodiment of a composite emulsifier, a preparation method and an application thereof, the component composition of the composite emulsifier is shown in Table 1, and the preparation method of the composite emulsifier comprises the following steps:

[0099] The components are placed in a mixing pot and slowly heated to dissolve each component, mixed and stirred uniformly, and then granulated in a granulator. After cooling to room temperature, the composite emulsifier is obtained.

[0100] Examples 2-3

[0101] An embodiment of a composite emulsifier, a preparation method and an application thereof, which is different from Example 1 only in the component ratio, as shown in Table 1.

[0102] Table 1

[0103] Product Weight Parts (100 parts) Example 1 Example 2 Example 3 Polyglyceryl-10 pentastearate 19 14 24 Polyglyceryl-6 stearate 10 8 12 Behenyl alcohol 20 16 24 Glycerin stearate citrate 12 12 12 Phytosterols 5 3 7 Soybean glycerides 0.15 0.15 0.15 Glyceryl distearate Balance Balance Balance

[0104] The three composite emulsifier products of Examples 1-3 were respectively prepared into cream products according to the formulations in Table 2 as follows.

[0105] Table 2

[0106] Product Components Component Content (wt%) Compound emulsifier 6 Dimethicone 10 Cyclopentasiloxane 10 Cetearyl alcohol 2.5 1,3-Butylene glycol 3 Glycerin 3 Hydroxyethyl cellulose 0.2 Water Balance

[0107] Example 1

[0108] The cream products prepared in the above Examples 1-3 were respectively placed at 25℃ and 37℃ for 2h, and then polarized microscope photos of the products were taken by using an Olympus BX35. The results of the three products are shown in Figs. 1-3. Figures 1-2 、 Figures 3-4 and Figures 5-6 .

[0109] As can be seen from the figures, at room temperature 25℃, the cream further prepared from the composite emulsifiers of the three Examples has a large number of intact and good liquid crystal structures, and when the temperature rises to 37℃, a large number of liquid crystal structures can still be observed in the cream at this temperature, indicating that the liquid crystal structure formed by using the composite emulsifier of the present application in cosmetics has heat-resistant stability and can be generated at a temperature close to the temperature of human skin. In particular, the number of liquid crystal structures of the product of Example 1 at 37℃ is almost the same as that at 25℃, and after software statistics, the distribution density of liquid crystal structures per unit area is slightly higher than that of the other two Example products. At the same time, the emulsion droplets in the cream products prepared from the composite emulsifiers of the Examples have high uniformity.

[0110] At the same time, in order to compare the use effect of the composite emulsifier of the present application with that of the existing emulsifier products, the product of Example 1, a commercially available lecithin emulsifier (main components: stearic acid 10-30%, behenyl alcohol 10-30%, glyceryl stearate 10-30%, lecithin 20-50%, myristyl alcohol 1-10%, lauryl alcohol 1-5%, cetyl alcohol 1-5%, palmitic acid 1-5%), a commercially available alkyl glycoside emulsifier (C14-C22 alcohol 10-30%, C12-C20 alkyl glucoside 70-90%), a commercially available sucrose ester emulsifier (sucrose stearate 40-60%, octadecanol 20-30%, glyceryl stearate 20-30%) and a commercially available amino acid emulsifier were prepared into creams using a certain general cream formulation, but each commercially available emulsifier was added according to the recommended amount of the cream in the prior art, and the addition amount of other components except water was unchanged, as shown in Table 3.

[0111] Table 3

[0112] Product Components Component Content (wt%) Compound emulsifier General amount Squalane 10 Caprylic / capric triglyceride 10 Cetearyl alcohol 2.5 1,3-Butylene glycol 3 Glycerin 3 Hydroxyethyl cellulose 0.2 Water Balance

[0113] The recommended addition amount of each emulsifier in the general cream formula is as follows: the liquid crystal emulsifier prepared in Example 1 (3-6%), lecithin emulsifier (3-6%), alkyl glycoside emulsifier (1-3%), sucrose ester emulsifier (3-5%), and amino acid emulsifier (1-2%). The maximum value of the recommended addition amount (i.e., 6%, 6%, 3%, 5%, and 2%) is taken as the actual addition amount to prepare the product, and the same method is used to take a polarized light microscope photograph, and the results are shown in Figures 7-8 、 Figures 9-10 、 Figures 11-12 and Figures 13-14 Since the cream prepared from the product of Example 1 has similar results to Figures 1-2 , the results are not repeated, and the remaining Figures 7-14 It can be seen that, compared with the product of the present application, the commercially available lecithin emulsifier and the commercially available alkyl glycoside emulsifier are further prepared into creams according to the conventional addition amount, and only liquid crystal structure can be observed at 25°C in the product, but when the temperature rises to 37°C, the liquid crystal structure disappears, and the emulsion droplets of the two cream products prepared are not uniform, and there is obvious droplet difference; the cream products prepared from the commercially available sucrose ester emulsifier and the amino acid emulsifier can only observe a small amount of liquid crystal structure at 25°C, and liquid crystal structure cannot be generated at 37°C.

[0114] Further, in order to investigate the temperature range in which the composite emulsifier of the present application forms a liquid crystal structure when applied to prepare a cream, the product of Example 1 is prepared into a cream according to an outdoor use cream formula in Table 4 as follows.

[0115] The prepared product is placed at 25°C, 35°C, 37°C, and 45°C for 2h, and then the liquid crystal structure is observed according to the same method as described above.

[0116] Table 4

[0117] Product Components Component Content (wt%) Compound emulsifier 6 Caprylic / capric triglyceride 20 Cetearyl alcohol 2.5 1,3-Butylene glycol 3 Glycerin 3 Hydroxyethyl cellulose 0.2 Water Balance

[0118] The test results are shown in Figure 15 It can be seen that when the composite emulsifier of the present application is applied to prepare a cream product, even if the temperature reaches 45°C, liquid crystal structure can still be observed in the cream product, and the liquid crystal structure has high-temperature stability, that is, even if the use environment temperature is higher than the human skin temperature (for example, in the summer outdoor environment or some special working environment), the cream product can still achieve good long-acting moisturizing property.

[0119] Therefore, the cream of Table 3 above was subjected to a moisturizing effect test, and the test site was the skin of a 2x2 cm area on the inner side of the wrist of a healthy volunteer. Meanwhile, two additional test areas of the same size were set up at the same level for data collection of the blank group and sample test of the comparison group. The specific test method was as follows:

[0120] In a test environment of 22°C and 45% relative humidity, 20 mg of the cream prepared in Example 1 and the cream of the comparison group were respectively applied to the areas of Example 1 group and the comparison group, and then the initial value of the water content of the stratum corneum of the three test site of the volunteer was tested by Cutometer dual MPA 580. The real-time value of the water content of the stratum corneum of the test area was tested at 15 min, 30 min, 45 min and 60 min after application. The difference between the cream of the comparison group and the cream prepared in Example 1 was that the composite emulsifier described in Example 1 was replaced by PEG-55 stearate.

[0121] The test results were statistically analyzed and plotted into a graph as shown in Figure 16 It can be seen that the cream product prepared by the composite emulsifier described in Example 1 (labeled as liquid crystal emulsifier prepared cream) can greatly increase the water content of the stratum corneum on the skin surface at the initial use (the initial water content of the blank group without using the cream is only 42%, while the water content of the test site using the cream prepared in Example 1 reaches 58%), and the increase is much greater than that of the control product prepared by the traditional liquid crystal emulsifier containing PEG structure. Meanwhile, the water content of the test site using the comparison product (labeled as non-liquid crystal cream) is almost the same as that of the blank group after 60 min, which indicates that the product does not actually have a long-term moisturizing function. However, the cream product prepared by the composite emulsifier described in the application has a high-thermal-stability liquid crystal structure layer, so it can form a moisturizing barrier on the skin surface, and the water content of the stratum corneum after 60 min can still reach about 45%, which has a high moisturizing efficiency and a long duration. Further, the composite emulsifiers described in Examples 2 and 3 were also subjected to the same test, and the results are shown in Figure 17 It can be seen that the effects of the three products of the examples are similar, but the product of Example 1 has better durability.

[0122] Examples 4-9

[0123] One embodiment of a composite emulsifier, a preparation method and application thereof, which is different from Example 1 only in the component ratio, as shown in Table 5.

[0124] Table 5

[0125]

[0126]

[0127] Table 6

[0128]

[0129] The composite emulsifiers obtained in Examples 1-9 were prepared into creams according to the cream formula in Table 6, and then the prepared cream products were observed for liquid crystal structure according to the same method as in Effect Example 1, and it was found that the products obtained in Examples 1-3 and Figures 1-6 the results were similar, indicating that the composite emulsifiers described in the present application have little difference in the effect of forming liquid crystal structure in different systems of creams, and therefore will not be repeated here. The observation results of the cream products obtained in Examples 4-9 are shown in Figures 18-19 、 Figures 20-21 、 Figures 22-23 、 Figures 24-25 、 Figures 26-27 and Figures 28-29 . It can be seen that the products obtained in Examples 4-9 are similar to the products of Examples 1-3 at room temperature, and clear Maltese cross structures can be observed in the products, but there are certain differences in the number of liquid crystal cross structures in different products. When the temperature rises to 37°C, the number of liquid crystal cross structures in each product decreases to different extents, but overall, a certain number of liquid crystal structures are still retained in the products, and the number of liquid crystal structures in the products of Examples 7 and 9 is relatively large and the structure is more complete.

[0130] Example 10

[0131] One embodiment of a composite emulsifier and its preparation method and application, which is different from Example 1 only in that the polyglyceryl-6 stearate in the component is replaced by polyglyceryl-10 penta stearate.

[0132] The product was prepared into a cream according to the formula in Table 6 and observed for liquid crystal structure according to the method of Examples 1-9, and it was found that the liquid crystal structure in the cream at room temperature was relatively complete and the number was similar to that in Example 1, but the number decreased at 37°C, indicating that in the case of compounding polyglyceryl-6 stearate and polyglyceryl-10 penta stearate, the composite emulsifier has a better effect on forming liquid crystal structure at 37°C in the cream.

[0133] Example 11

[0134] One embodiment of a composite emulsifier and its preparation method and application, which is different from Example 1 only in that the phytosterols in the component are replaced by β-sitosterol.

[0135] The product was prepared into a cream according to the method of Example 1-9 and the liquid crystal structure was observed according to the formulation of Table 6. The results showed that the generation of liquid crystal structure in the cream was similar to that of Example 1 at room temperature, but the amount at 37°C was less, indicating that when the sterol in the complex emulsifier component is selected as a plant sterol, the generation of liquid crystal structure in the cream is best.

[0136] Comparative Examples 1-6

[0137] A complex emulsifier, its preparation method and application, which are different from Example 1 only in the component ratio, as shown in Table 7.

[0138] Table 7

[0139]

[0140]

[0141] The products of Comparative Examples 1-6 were prepared into creams according to the formulation of Table 6, and the corresponding liquid crystal structure was observed according to the method of each of the above examples. Since the product of Comparative Example 1 could not be stably applied in the cream system (oil-water separation occurred in the product), the product was unqualified and no liquid crystal structure observation was performed. The results of the remaining comparative products are shown in Figures 30-31 、 Figures 32-33 、 Figures 34-35 、 Figures 36-37 and Figures 38-39 . It can be seen that since the content of polyglyceryl stearate in the complex emulsifier of Comparative Example 2 is too high, it cannot achieve the best liquid crystal structure generation effect. Although some liquid crystal structure can still be observed in the cream at 25°C, the cross structure almost disappears at 37°C, leaving only a small amount of incomplete liquid crystal structure. The content of behenyl alcohol in the complex emulsifier of Comparative Example 3 is too low, and the prepared cream product can hardly observe liquid crystal structure at room temperature. The content of behenyl alcohol in the product of Comparative Example 4 is too high, although the product has obvious liquid crystal structure at different temperatures, but the viscosity of the product is too high, and it is difficult to evenly spread on the skin, and it is difficult to meet the use experience requirements of ordinary cream cosmetics. The product of Comparative Example 5 does not contain plant sterols, and no liquid crystal structure is observed at 37°C, indicating that plant sterols are the key component of the complex emulsifier to form heat-resistant and stable liquid crystal structure in the emulsion. However, if the content of this component is too high, as shown in the product of Comparative Example 6, the dispersion of the product components will be greatly affected, as shown in the figure, large crystalline particles appear in the product, which will cause a grainy feeling when used on the skin, and does not meet the use requirements.

[0142] Comparative Example 7

[0143] A compound emulsifier, a preparation method and application thereof, which are different from those of Example 1 only in that the polyglyceryl stearate (polyglyceryl-10 penta stearate and polyglyceryl-6 stearate) in the component is replaced by stearic acid with the same addition amount.

[0144] The prepared product is used to prepare a cream according to the formula in Table 6, and the corresponding liquid crystal structure observation is performed according to the method of each of the above examples, and the results are shown in Table 6. Figures 40-41 As can be seen from Table 6, when the polyglyceryl stearate in the compound emulsifier of the application is replaced by the conventional fatty acid ester, although a small amount of liquid crystal structure can still be observed at room temperature, no complete liquid crystal Maltese cross structure appears, which shows that the polyglyceryl stearate in the product has great significance for the integrity of the liquid crystal structure formed in the emulsion; and the cream is almost impossible to observe the liquid crystal structure at 37 DEG C.

[0145] Comparative Example 8

[0146] A compound emulsifier, a preparation method and application thereof, which are different from those of Example 1 only in that the behenyl alcohol in the component is replaced by cetyl alcohol with the same addition amount.

[0147] The prepared product is used to prepare a cream according to the formula in Table 6, and the corresponding liquid crystal structure observation is performed according to the method of each of the above examples, and the results are shown in Table 6. Figures 42-43 As can be seen from Table 6, when the polyglyceryl stearate in the compound emulsifier of the application is replaced by the conventional fatty acid ester, although a small amount of liquid crystal structure can still be observed at room temperature, no complete liquid crystal Maltese cross structure appears, which shows that the polyglyceryl stearate in the product has great significance for the integrity of the liquid crystal structure formed in the emulsion; and the cream is almost impossible to observe the liquid crystal structure at 37 DEG C.

[0148] Meanwhile, based on Comparative Examples 7 and 8, the inventors also replace other components of the compound emulsifier in Example 1 with conventional similar components to prepare comparative products, replace the sterol with a commercially available phytosterol oleate, and then prepare a cream according to the formula in Table 5 and perform liquid crystal structure observation, and the results are similar to those of Comparative Examples 7 and 8, although liquid crystal structure can be formed at room temperature, but no obvious complete liquid crystal structure can be observed at 37 DEG C, which shows that when one or several components of the compound emulsifier of the application are replaced by conventional components in existing emulsifiers, the expected effect cannot be achieved, which will not be described here.

[0149] Effect Example 2

[0150] In order to verify the use experience of the cream prepared by the composite emulsifier, the products of Example 1 and Comparative Example 4 are prepared into creams according to the formulation in Table 6, and then detected by a viscometer. At room temperature, the viscosity of the product of Example 1 is 37800 mPa.s, but the viscosity of the product of Comparative Example 4 reaches more than 100000 mPa.s, which may have a serious thick and heavy feeling when being applied;

[0151] Further, two products are tested for use. 15 volunteers with healthy skin, half male and half female, aged 20-40 years old, are used to test the two products. An appropriate amount of each product is evenly applied to the forearm and kept for 5 minutes. The use process is in a blind test mode. 15 people use two products on two forearms, but are not told the specific product formulation. Then, the absorption speed, application feeling, softness, stickiness and moisturizing degree of the products are scored and evaluated, and the average value is calculated as follows.

[0152] Absorption speed (0-5 points, 0 point for slowest absorption, 5 points for fastest absorption);

[0153] Application feeling (0-5 points, 0 point for most difficult to apply, 5 points for easiest to apply);

[0154] Softness (0-5 points, 0 point for least soft, 5 points for most soft);

[0155] Stickiness (0-5 points, 0 point for most sticky, 5 points for most refreshing);

[0156] Moisturizing degree (0-5 points, 0 point for worst moisturizing degree, 5 points for best moisturizing degree).

[0157] The test results are plotted as a radar chart as shown in Figure 44 It can be seen that the average score of each index of the product of Example 1 can be maintained at more than 3 points, and the scores of 13 out of 15 people are more than 3 points, indicating that the product has good use experience. The product of Comparative Example 4 has low absorption speed, high application difficulty and strong stickiness due to the introduction of too much behenyl alcohol, which is not suitable for use in cosmetics.

[0158] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application and do not limit the protection scope of the present application. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present application.

Claims

1. A complex emulsifier, characterized by, The composite emulsifier comprises the following components in parts by weight: glycerin distearate 10~50 parts, polyglyceryl-10 penta stearate 10~30 parts, polyglyceryl-6 stearate 5~15 parts, behenyl alcohol 15~25 parts, glyceryl stearate citrate 10~20 parts, sterol 1~9 parts, and soybean glyceride 0.1~1 part.

2. The complex emulsifier according to claim 1, wherein The sterol is at least one of phytosterol, beta-sitosterol, and cholesterin.

3. The complex emulsifier according to claim 2, wherein The sterol is phytosterol.

4. The complex emulsifier according to claim 1, wherein The composite emulsifier comprises the following components in parts by weight per 100 parts: polyglyceryl-10 penta stearate 14~25 parts, polyglyceryl-6 stearate 8~12 parts, behenyl alcohol 16~24 parts, glyceryl stearate citrate 12~16 parts, phytosterol 3~7 parts, soybean glyceride 0.1~0.2 parts, and the rest glycerin distearate.

5. The complex emulsifier according to claim 4, wherein The composite emulsifier comprises the following components in parts by weight per 100 parts: polyglyceryl-10 penta stearate 14~25 parts, polyglyceryl-6 stearate 8~12 parts, behenyl alcohol 16~24 parts, glyceryl stearate citrate 12~16 parts, phytosterol 3~7 parts, soybean glyceride 0.1~0.2 parts, and the rest glycerin distearate.

6. The method for preparing a complex emulsifier according to any one of claims 1 to 5, characterized in that, The method comprises the following steps: heating and dissolving the components and mixing them uniformly, then granulating, and cooling to obtain the composite emulsifier.

7. Use of the composite emulsifier according to any one of claims 1~5 in the preparation of a cosmetic product.

8. A cream, characterized by, The components comprise the composite emulsifier according to any one of claims 1~5.

9. The cream according to claim 8, wherein the amount of the compound is 0.01 to 5% by weight. The mass percentage of the composite emulsifier in the cream is 4~6wt%.

10. The cream according to claim 9, wherein the amount of the compound is 0.01 to 5% by weight. The cream comprises the following components in mass percentage: composite emulsifier 4~6%, dimethicone 8~12%, cyclopentasiloxane 8~12%, cetyl stearyl alcohol 2~4%, 1,3-butanediol 2~4%, glycerin 2~4%, hydroxyethyl cellulose 0.1~0.5%, and the rest water.

11. The cream of claim 9, wherein, The cream comprises the following components in mass percentage: composite emulsifier 4~6%, squalane 8~12%, caprylic / capric triglyceride 8~12%, cetyl stearyl alcohol 2~4%, 1,3-butanediol 2~4%, glycerin 2~4%, hydroxyethyl cellulose 0.1~0.5%, and the rest water.

12. The cream of claim 9, wherein, The cream comprises the following components in mass percentage: composite emulsifier 4~6%, caprylic / capric triglyceride 15~25%, cetyl stearyl alcohol 2~4%, 1,3-butanediol 2~4%, glycerin 2~4%, hydroxyethyl cellulose 0.1~0.5%, and the rest water.

13. The cream of claim 9, wherein, The cream comprises the following components in mass percentage: composite emulsifier 4~6%, behenyl alcohol 1~2%, cetyl alcohol 1~3%, hydrogenated polydecene 4~6%, glyceryl tri(ethylhexanoate) 4~6%, dimethicone 1~3%, sodium phytate 0.01~0.1%, glycerin 1~3%, isopentyldiol 4~6%, acryloyldimethyltaurine ammonium / VP copolymer 0.1~1%, and the rest water.

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