Sunscreen cosmetic composition and preparation method thereof

Abstract

The invention discloses a sunscreen cosmetic composition and a preparation method thereof. The sunscreen cosmetic composition comprises modified lignin, a compound emulsifier and water, the preparation method of the modified lignin comprises the following steps: carrying out dehydration condensation reaction on lignin and a compound as shown in a formula (I) and / or a condensation product of the compound as shown in the formula (I); the compound emulsifier is prepared from lauryl polyglycerol-3 polydimethylsilyloxyethyl polydimethylsiloxane and polyglycerol-3 polydimethylsilyloxyethyl polydimethylsiloxane, and the compound emulsifier is prepared from polyglycerol-3 polydimethylsilyloxyethyl polydimethylsiloxane; meanwhile, the adding amount of the modified lignin and the compound emulsifier is controlled, and all the components are mixed, dispersed and emulsified during preparation. Practice shows that the formula of the lignin can obtain excellent dispersion uniformity, good stability, good sunscreen effect and smooth and soft dosage form, and solves the problems existing when the lignin is used in sunscreen cosmetics at present. # imgabs0 #

Description

Technical Field

[0001] The invention relates to the field of daily chemical products, in particular to a sunscreen cosmetic composition and a preparation method thereof. Background Art

[0002] Continuous exposure of human skin to ultraviolet rays may accelerate skin aging and cause skin damage, endangering human health. In addition, effective prevention of ultraviolet rays is also helpful for skin beauty. Therefore, in modern society where the attention to skin has increased significantly, sun protection has become an indispensable part.

[0003] Lignin is a renewable natural aromatic polymer, and its current application is mainly used as fuel. Studies have shown that the unique high aromatic ring characteristics and rich functional group types of lignin give lignin certain ultraviolet absorption, antibacterial, antioxidant and other properties. At the same time, lignin has the advantages of being natural, renewable, biodegradable, and non-toxic, making lignin and its derivatives have high potential application value. However, practice has found that in the formula, it is usually difficult to ensure that lignin has appropriate dispersibility and stability, and the surface of the dosage form is not smooth, so it is difficult to apply it to sunscreen cosmetics. Summary of the invention

[0004] The object of the present invention is to overcome one or more deficiencies in the prior art and to provide a new sunscreen cosmetic composition that can reuse and exert the effects of lignin, such as UV protection, and can form a smooth surface with excellent stability.

[0005] The present invention also provides a method for preparing the sunscreen cosmetic composition.

[0006] In order to achieve the above object, a technical solution adopted by the present invention is:

[0007] A sunscreen cosmetic composition, comprising modified lignin, a composite emulsifier and water;

[0008] The preparation method of the modified lignin comprises: using the compound represented by formula (I) and / or the condensation product of the compound represented by formula (I) to carry out a dehydration condensation reaction with lignin;

[0009] R1 is selected from C 1-10 Alkyl or substituted C 1-10 alkyl;

[0010] The composite emulsifier comprises lauryl polyglyceryl-3 polydimethylsiloxyethyl dimethicone and polyglyceryl-3 polydimethylsilyl hydroxyethyl dimethicone;

[0011] In terms of mass percentage, in the sunscreen cosmetic composition, the modified lignin accounts for 0.01%-1.6%, the lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane accounts for 0.1%-2.5%, and the polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethylsiloxane accounts for 0.5%-5.5%.

[0012] In some embodiments of the present invention, the compound represented by formula (I) is prepared by hydrolyzing the compound represented by formula (II);

[0013] R1 is the same as above, R2, R3, R4 are independently selected from C 1-10 Alkoxy.

[0014] In some embodiments of the present invention, R1 is selected from n-propyl, isopropyl, n-butyl, isobutyl, n-pentyl, isopentyl, neopentyl, hexyl, heptyl, octyl, nonyl.

[0015] In some embodiments of the present invention, R2, R3, and R4 are independently selected from methoxy, ethoxy, and propoxy.

[0016] According to some preferred aspects of the present invention, the mass ratio of the compound represented by formula (II) to the lignin is 1.5-5: 1. Further, the mass ratio of the compound represented by formula (II) to the lignin can be 2: 1, 2.5: 1, 3.0: 1, 3.5: 1, 4.0: 1, etc.

[0017] In some embodiments of the present invention, the average particle size of the modified lignin is 0.5-15 μm, further 0.5-10 μm, and further 1-6 μm.

[0018] In some embodiments of the present invention, the dehydration condensation reaction is controlled to be carried out at 50-95°C, and further, for example, can be carried out at 50-60°C, 65-70°C, 75-80°C or 85-95°C.

[0019] According to a specific aspect of the present invention, in formula (I), R1 is selected from octyl.

[0020] According to a specific aspect of the present invention, the compound represented by formula (II) may be triethoxyoctylsilane, and the structural formula is as follows:

[0021] In some embodiments of the present invention, the compound represented by formula (II) is used as a raw material, and is hydrolyzed under alkaline conditions (for example, an aqueous solution of an alkali metal hydroxide, such as an aqueous solution of sodium hydroxide) and under heating conditions (the temperature may be 50-95° C.) to generate a compound represented by formula (I). Further, the silanol groups of the compound represented by formula (I) may be dehydrated and condensed to generate a silanol-containing oligosiloxane; the compound represented by formula (I) and / or the silanol-containing oligosiloxane may be dehydrated and condensed with lignin under heating conditions (the temperature may be 50-95° C.), that is, the silanol groups on the compound represented by formula (I) and / or the silanol-containing oligosiloxane may be covalently bonded with the hydroxyl groups on the surface of the lignin to form a silicon-oxygen-silicon bond;

[0022] Of course, it is also possible that the compound represented by formula (I) first forms a silicon-oxygen-silicon bond with lignin, and then the compounds represented by formula (I) on the lignin undergo a dehydration condensation reaction, or the compound represented by formula (I) on the lignin reacts with an independent compound represented by formula (I), or it is also possible that two or more compounds represented by formula (I) connected to each other on lignin react with each other, so that two or more lignins are connected together;

[0023] Meanwhile, the silanol groups on the compound represented by formula (I) may be one or two or more silanol groups reacting with the hydroxyl groups on lignin to form a bond, and the same is true for the silanol groups on the silanol-containing oligosiloxane;

[0024] That is, a silane film is formed on the surface of lignin (which may contain the compound represented by formula (I), or may contain the condensation product of the compound represented by formula (I), and of course, both may exist, and they both form silicon-oxygen-silicon bonds with lignin), and is stably present through chemical bond connection, thereby obtaining modified lignin;

[0025] The following is a further description of the process of preparing modified lignin in the present invention by taking the compound represented by formula (II) selected from triethoxyoctylsilane as an example, and the reaction route is roughly as follows:

[0026]

[0027] In the above reaction, the modified lignin after the final reaction may have one structure, two structures, or more structures coexisting. The above modified lignin 1, modified lignin 2, modified lignin 3, and modified lignin 4 are only illustrative examples, and there are other reaction connections. The reaction principle is the dehydration condensation of silanol and hydroxyl groups on lignin. As long as this reaction mechanism is met, the product obtained is one of the possible products.

[0028] According to some preferred aspects of the present invention, in the sunscreen cosmetic composition, the modified lignin accounts for 0.05%-1.5%, further 0.1%-1.4%, by mass percentage.

[0029] According to some preferred aspects of the present invention, in the sunscreen cosmetic composition, the lauryl polyglyceryl-3 polydimethylsiloxyethyl dimethicone accounts for 0.3%-2.2%, further 0.3%-1.0%, by mass percentage.

[0030] In some embodiments of the present invention, in the sunscreen cosmetic composition, the lauryl polyglyceryl-3 polydimethylsiloxyethyl dimethicone accounts for 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.3%, 1.5%, 2.0%, 2.3% or 2.4%, etc., by mass percentage.

[0031] According to some preferred aspects of the present invention, in the sunscreen cosmetic composition, the polyglyceryl-3 polydimethylsilyl hydroxyethyl polydimethicone accounts for 0.7%-5.0%, further 2.5%-3.5%, by mass percentage.

[0032] In some embodiments of the present invention, in the sunscreen cosmetic composition, the polyglyceryl-3 polydimethylsilyl hydroxyethyl polydimethicone accounts for 1%, 1.5%, 2%, 2.6%, 2.8%, 3.0%, 3.2%, 3.3%, 3.4%, 3.5%, 3.8%, 4.0%, 4.1% or 4.5%, etc., by mass percentage.

[0033] According to some preferred aspects of the present invention, the mass ratio of the lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane to the polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethylsiloxane is 1:4-8, further 1:5-7.

[0034] The sunscreen cosmetic composition of the present invention may further include inorganic sunscreen ingredients, organic sunscreen ingredients, moisturizers, preservatives, functional ingredients, and other ingredients included in conventional cosmetic compositions. The mixing amount of the ingredients is not particularly limited, and practitioners can conveniently select them within the scope that does not damage the purpose and effect of the present invention. In addition, the present invention can also be used for the manufacture of various dosage forms of cosmetics in this industry, such as oil-in-water (O / W), water-in-oil (W / O), etc., including but not limited to this.

[0035] In some embodiments of the present invention, the sunscreen cosmetic composition further comprises a combination of one or more selected from inorganic sunscreen ingredients, organic sunscreen ingredients, moisturizers, preservatives, thickeners, skin conditioners, emollients, and chelating agents.

[0036] In some embodiments of the present invention, the sunscreen cosmetic composition comprises a thickening phase, a preservative phase, an emulsified phase, a physical sunscreen phase and an aqueous phase.

[0037] Furthermore, the thickening phase comprises disteardimethylammonium hectorite and cyclohexasiloxane.

[0038] Furthermore, the preservative phase comprises caprylic acid glyceryl and caprylyl glycol.

[0039] Furthermore, the emulsified phase comprises the modified lignin, propylene glycol dicaprylate, the lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone, the polyglyceryl-3 polydimethylsilyl hydroxyethyl polydimethicone, and ethylhexylglycerin.

[0040] Furthermore, the physical sunscreen phase comprises zinc oxide.

[0041] Furthermore, the aqueous phase comprises magnesium sulfate, 1,3-propylene glycol, glycerol, 1,2-hexanediol and the water.

[0042] According to some specific aspects of the present invention, the sunscreen cosmetic composition comprises, by mass percentage:

[0043] Disteardimethylammonium hectorite 0.01%-3.00%

[0044] Cyclohexasiloxane 0.01%-20.00%

[0045] Glyceryl Caprylate 0.01%-1.00%

[0046] Caprylyl glycol 0.01%-1.00%

[0047] Modified lignin 0.01%-1.60%

[0048] Propylene glycol dicaprylate 0.01%-30.00%

[0049] Lauryl Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone 0.1%-2.5%

[0050] Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone 0.5%-5.5%

[0051] Ethylhexylglycerin 0.01%-1.00%

[0052] Zinc oxide 0.01%-25.00%

[0053] Magnesium sulfate 0.01%-3.00%

[0054] 1,3-Propanediol 0.01%-8.00%

[0055] Glycerin 0.01%-5.00%

[0056] 1,2-Hexanediol 0.01%-3.00%

[0057] Water is added in an amount such that the total amount of the sunscreen cosmetic composition is adjusted to 100%.

[0058] Furthermore, the sunscreen cosmetic composition comprises, by mass percentage:

[0059] Disteardimethylammonium hectorite 0.5%-3.00%

[0060] Cyclohexasiloxane 2%-20.00%

[0061] Glyceryl Caprylate 0.01%-0.50%

[0062] Caprylyl glycol 0.01%-0.50%

[0063] Modified lignin 0.01%-1.60%

[0064] Propylene glycol dicaprylate 10.00%-30.00%

[0065] Lauryl Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone 0.1%-2.5%

[0066] Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone 0.5%-5.5%

[0067] Ethylhexylglycerin 0.01%-0.3%

[0068] Zinc oxide 5%-25.00%

[0069] Magnesium sulfate 0.1%-2.00%

[0070] 1,3-Propanediol 1%-8.00%

[0071] Glycerin 1%-5.00%

[0072] 1,2-Hexanediol 0.01%-1.50%

[0073] The balance is water.

[0074] According to the present invention, lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone can be commercially obtained, and the commercially available product usually contains a small amount (about 0.01%-0.02% by mass) of tocopherol, and tocopherol usually has antioxidant and metabolism-improving effects, and has a positive beneficial effect on the sunscreen cosmetics of the present invention. Therefore, in the embodiments of the present invention, lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone*tocopherol can be directly used as lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone.

[0075] Another technical solution provided by the present invention is a method for preparing the sunscreen cosmetic composition described above, the preparation method comprising: mixing and emulsifying the components to prepare the sunscreen cosmetic composition.

[0076] In some embodiments of the present invention, the method for preparing the sunscreen cosmetic composition comprises:

[0077] Mix and disperse the thickening phase, the preservative phase, the emulsifying phase, and the physical sunscreen phase to obtain an oil phase;

[0078] Mixing and dispersing the components in the water phase to obtain the water phase;

[0079] The water phase is added to the oil phase for dispersion and emulsification to prepare a sunscreen cosmetic composition.

[0080] Furthermore, the above dispersion process can be carried out at 20-30°C, such as room temperature.

[0081] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art:

[0082] Based on the defects of lignin in sunscreen cosmetics such as difficulty in dispersion, poor stability, and rough surface of the dosage form after use, the inventors of the present invention innovatively provide a modified lignin, which is modified by using the compound represented by formula (I) and / or the condensation product of the compound represented by formula (I) as a surface modifier, and lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane and polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethylsiloxane as composite emulsifiers, and the modified lignin is compounded with the two emulsifiers in appropriate contents. Practice shows that the formula using lignin in the present invention can obtain excellent dispersion uniformity and good stability, and at the same time, has a good sunscreen effect and a smooth and soft dosage form, which solves the defects of lignin in sunscreen cosmetics. BRIEF DESCRIPTION OF THE DRAWINGS

[0083] Figure 1 The following are photos comparing the dosage forms of the sunscreen cosmetic compositions obtained in Example 1 of the present invention and Comparative Example 1;

[0084] Figure 2The surface comparison photographs of the sunscreen cosmetic compositions obtained in Example 1 of the present invention and Comparative Example 4 observed from the bottle mouth;

[0085] Figure 3 The following are comparison photos of the dosage form surfaces of the sunscreen cosmetic compositions obtained in Example 1 of the present invention and Comparative Example 4 observed from the bottle body;

[0086] Figure 4 These are comparative photos of the dosage form surfaces of the sunscreen cosmetic compositions obtained in Comparative Examples 5 and 6 of the present invention;

[0087] Figure 5 It is a statistical diagram of the sunscreen efficacy data of the sunscreen cosmetic compositions obtained in Examples 1-8 of the present invention and Comparative Examples 1-14;

[0088] Figure 6 This is a dosage form photo of the sunscreen cosmetic composition obtained in Example 1 of the present invention after 3 months of stability evaluation;

[0089] Figure 7 This is a dosage form photo of the sunscreen cosmetic composition obtained in Comparative Example 11 of the present invention after 3 months of stability evaluation;

[0090] Figure 8 This is a dosage form photo of the sunscreen cosmetic composition obtained in Comparative Example 12 of the present invention after 3 months of stability evaluation;

[0091] Fig. 9 This is a dosage form photo of the sunscreen cosmetic composition obtained in Comparative Example 13 of the present invention after 3 months of stability evaluation;

[0092] Fig.10 This is a dosage form photograph of the sunscreen cosmetic composition obtained in Comparative Example 14 of the present invention after 3 months of stability evaluation. DETAILED DESCRIPTION

[0093] The above scheme is further described below in conjunction with specific embodiments; it should be understood that these embodiments are used to illustrate the basic principles, main features and advantages of the present invention, and the present invention is not limited to the scope of the following embodiments; the implementation conditions adopted in the embodiments can be further adjusted according to specific requirements, and the implementation conditions not specified are usually the conditions in conventional experiments.

[0094] Unless otherwise specified in the following examples, all raw materials are commercially available or prepared by conventional methods in the art.

[0095] Disteardimethylammonium hectorite, purchased from ELEMENTIS, brand 38V CG; Cyclohexasiloxane, purchased from DOW CHEMICAL COMPANY, brand XIAMETER TMPMX-0246Cyclohexasiloxane; Caprylic acid glyceride, purchased from IOIOLEO GMBH, brand GC8; Caprylyl glycol, purchased from EVONIK, brand Octiol; Propylene glycol dicaprylate, available from OLEON NV, brand LIPIPLEX 7202Q; Lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone* tocopherol, available from SHINETSUSILICONE, brand KF-6105, lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone accounts for 99.98%; Polyglyceryl-3 polydimethylsilyl hydroxyethyl polydimethicone, available from SHIN-ETSU CHEMICAL CO., LTD, brand KF-6106; PEG-10 polydimethicone, available from SHIN-ETSU CHEMICAL CO., LTD, brand KF-6017; Lauryl PEG-10 tris(trimethylsiloxy)silylethyl polydimethicone, available from DOW CHEMICAL COMPANY, brand DOWSIL TM ES-5300 Formulation Aid; Sorbitan olive oil ester, purchased from HALLSTAR ITALIA SRL, brand name Olivem900MB; Polyglyceryl-4 oleate*Polyglyceryl-3 polyricinoleate, purchased from HALLSTAR ITALIA SRL, brand name Olivem 2090G, polyglyceryl-4 oleate accounts for 77%, polyglyceryl-3 polyricinoleate accounts for 23%; Ethylhexylglycerin, purchased from ADEKA CORPORATION, brand name ADEKA NOL GE-RF; Lignin, purchased from JUNDA, brand name SSEIF-BA OTS;

[0096] In the following, the modified lignin was prepared by the following method: 4 g of dried lignin powder was uniformly dispersed in 50 mL of sodium hydroxide aqueous solution (concentration was 0.1 mol / L) to obtain a lignin dispersion; 10 g of triethoxyoctylsilane was mixed with 90 mL of sodium hydroxide aqueous solution (concentration was 0.1 mol / L), heated and hydrolyzed at 80°C, and the hydrolyzed silane solution was slowly added dropwise to the lignin dispersion at a temperature of 60°C and magnetically stirred for 6 hours, cooled to room temperature, centrifuged (8000 rpm for 10 minutes), filtered, and dried (vacuum dried at 50°C for 12 hours), and then the modified lignin was collected, and the average particle size was measured to be about 1.0 μm.

[0097] Example 1

[0098] This example provides a sunscreen cosmetic composition and a preparation method thereof. The formula of the sunscreen cosmetic composition is shown in Table 1.

[0099] Table 1

[0100]

[0101] The preparation method of the sunscreen cosmetic composition comprises:

[0102] At room temperature, the components in the thickening phase, the preservative phase, the emulsifying phase, and the physical sunscreen phase are mixed and dispersed to obtain an oil phase;

[0103] At room temperature, the components in the water phase are mixed and dispersed to obtain a water phase;

[0104] At room temperature, the water phase was slowly added to the oil phase and emulsified by a homogenizer at a rotation speed of 4000 rpm for 10 minutes to prepare a sunscreen cosmetic composition.

[0105] Example 2

[0106] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is adjusted to 0.24%.

[0107] Example 3

[0108] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is adjusted to 0.32%.

[0109] Example 4

[0110] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is adjusted to 0.48%.

[0111] Example 5

[0112] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is adjusted to 0.56%.

[0113] Example 6

[0114] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is adjusted to 0.64%.

[0115] Example 7

[0116] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is adjusted to 0.72%.

[0117] Example 8

[0118] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is adjusted to 0.80%.

[0119] Example 9

[0120] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the content of lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone*tocopherol is 1%, and the content of polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethicone is 4%.

[0121] Example 10

[0122] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the content of lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone*tocopherol is 2%, and the content of polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethicone is 5%.

[0123] Comparative Example 1

[0124] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the modified lignin is replaced with an equal amount of unmodified lignin.

[0125] Comparative Example 2

[0126] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the amount of modified lignin added is 0.

[0127] Comparative Example 3

[0128] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is 0.004%.

[0129] Comparative Example 4

[0130] This example provides a sunscreen cosmetic composition and a preparation method thereof, which is basically the same as Example 1, except that the addition amount of modified lignin is 2.0%.

[0131] Comparative Examples 5-10

[0132] These comparative examples provide a sunscreen cosmetic composition and a preparation method thereof, which are basically the same as those in Example 1, except that the amount of emulsifier used is different, as shown in Table 2.

[0133] Table 2

[0134]

[0135] Comparative Examples 11-14

[0136] These comparative examples provide a sunscreen cosmetic composition and a preparation method thereof, which are basically the same as Example 1, except that the type of emulsifier is different, as shown in Table 3.

[0137] Table 3

[0138]

[0139]

[0140] Performance Testing

[0141] (1) Smoothness of dosage form

[0142] See also Figure 1 As shown, it is a comparison photo of the sunscreen cosmetic composition obtained in Example 1 and Comparative Example 1. It can be seen that the surface of the sunscreen cosmetic composition of Example 1 of the present invention is smooth and soft, while the surface of Comparative Example 1 is not smooth and has a rough feel.

[0143] See also Figure 2 , which shows the photographs of Example 1 and Comparative Example 4 observed from the bottle mouth. The formulation of Example 1 is smooth and stable, while the surface of Comparative Example 4 is cracked, the oil is separated, and there are multiple condensation phenomena on the surface.

[0144] See also Figure 3 As shown, the pictures of Example 1 and Comparative Example 4 observed on the bottle body are shown. Due to the excessive amount of lignin, the formula of Comparative Example 4 is cracked and the dispersion is poor, resulting in uneven color in many places of the composition and the formation of color bands.

[0145] See also Figure 4 As shown, it is a photograph showing that the formulas of Comparative Example 5 using only Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone as an emulsifier and Comparative Example 6 using only Lauryl Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone as an emulsifier cannot maintain stability.

[0146] (2) Sunscreen efficacy test (SPF 290AS in vitro test)

[0147] The sunscreen efficacy of the sunscreen cosmetic compositions obtained in Examples 1 to 8 and Comparative Examples 1 to 14 was measured. The specific measurement method is as follows:

[0148] The sunscreen cosmetic compositions obtained in the above examples and comparative examples were diluted with 1.3 mg / cm 2 After evenly applying it on a PMMA (polymethyl methacrylate) plate, the sun protection effect was measured by measuring 9 points in each unit using an SPF 290AS instrument.

[0149] The results of the above determination methods are shown in Tables 4, 5, 6 and Figure 5 .

[0150] Table 4

[0151]

[0152] Table 5

[0153]

[0154] Table 6

[0155]

[0156] As can be seen from Tables 4 and 5, the examples in which lignin modified with triethoxyoctylsilane and two emulsifiers are compounded in appropriate amounts show excellent SPF and PA values, confirming their good sunscreen effects. On the other hand, the SPF and PA values ​​of Comparative Example 1 using unmodified lignin are significantly lower than those of the examples, and Comparative Example 2 without lignin and Comparative Example 3 containing a small amount of lignin also show lower SPF and PA values. Comparative Example 4 with a high lignin content shows higher SPF and PA values. Among the two emulsifiers, Comparative Examples 5 and 6 using only one emulsifier show higher SPF and PA values, and Comparative Examples 7 to 10 using an excessive or small amount of a certain emulsifier show lower SPF and PA values ​​than the examples.

[0157] At the same time, it can be seen from the above results that there is no necessary connection between the content of emulsifier and the sun protection value. When the content of a certain emulsifier in the system changes, the sun protection value will not change regularly; when the emulsifier in the system reaches the optimal ratio, the overall dispersibility and stability of the formula will achieve good results, thereby affecting the sun protection value and resulting in a higher sun protection value; as shown in Table 6, the combination of lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethicone and polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethicone is better than other emulsifier combinations in terms of the sun protection value of modified lignin in the formula.

[0158] (3) Viscosity measurement and formulation stability evaluation

[0159] The formulation stability was evaluated by measuring the viscosity of Examples 1 to 8 and Comparative Examples 1 to 114 produced in the above-mentioned production examples.

[0160] The viscosity was measured using a Brookfield Viscometer (LV: 4 pin 6 rpm, 30 sec) on the day the formulation was completed and 3 months after the production date to observe whether the viscosity changed.

[0161] The process of high temperature (40°C), room temperature (25°C), low temperature (-5°C), cooling from high temperature to room temperature, low temperature, and then heating from low temperature to room temperature and high temperature was repeated. After the embodiment and comparative example were stored for 3 months, the viscosity after manufacturing was measured to see whether it remained unchanged. The measurement results showed that when the viscosity change exceeded 10%, the formula was unstable. The above experimental results are shown in Table 7, Table 8 and Table 9.

[0162] Note: In formula stability, o means stable and x means unstable.

[0163] Table 7

[0164]

[0165] Table 8

[0166]

[0167] Table 9

[0168]

[0169] According to Tables 7 and 8 above, Examples 1 to 10 form a viscosity formulation with low fluidity but excellent spreadability, and after 3 months, the viscosity remains similar to that after manufacture, confirming that the formulation stability is excellent. On the other hand, the viscosity of Comparative Examples 1, Comparative Examples 4 to 7, and Comparative Examples 9 to 10 decreases greatly, confirming that the formulation is unstable, and Comparative Example 2 without lignin, Comparative Example 3 containing a small amount of lignin, and Comparative Example 8 using an excess of lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane maintain appropriate viscosity and have formulation stability. In addition, Comparative Example 6, which uses lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane alone as an emulsifier, is found to have too high a viscosity and is not suitable for use.

[0170] Also, see Figures 6 to 10 As shown, Figures 6 to 10 The following are the dosage form photos of the sunscreen cosmetic compositions obtained in Example 1, Comparative Example 11, Comparative Example 12, Comparative Example 13 and Comparative Example 14 of the present invention after 3 months of stability evaluation. Figure 6 It can be seen that in Example 1 of the present invention: the surface of the material body is smooth, no particles are precipitated, and no oil stratification phenomenon occurs;

[0171] Depend on Figure 7 It can be seen that in Comparative Example 11: the surface of the material is rough, there are small particles precipitated, and there is slight oil discharge;

[0172] Depend on Figure 8 It can be seen that in Comparative Example 12, the surface of the material is rough, particles are precipitated, obvious bubbles are generated, and there is slight oil leakage;

[0173] Depend on Fig. 9It can be seen that in comparative example 13, the material body obviously produces oil and stratification occurs;

[0174] Depend on Fig.10 It can be seen that in Comparative Example 14, the surface of the material is smooth, no particles are precipitated, and there is a slight oily feeling;

[0175] Further, it can be seen from Table 9 that the combination of two emulsifiers, lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane and polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethylsiloxane, is better than other emulsifier combinations in the stability of modified lignin in the formula. In particular, it can be seen from Table 6 that the composite emulsifier combination of the present invention can have both good sunscreen effect and stability, while other emulsifier combinations are difficult to take into account both sunscreen effect and stability in the formula of the present invention using modified lignin, and even perform poorly.

[0176] In summary, according to the above-mentioned sun protection value, viscosity measurement and formula stability evaluation experimental results, it is shown that the lignin modified by the specific compound of the present invention and the specific two emulsifiers prepared in appropriate proportions are very critical to the various effects of the formula, and the present invention can ensure the good dispersibility and dispersion stability of lignin, exert good sun protection effect, and maintain appropriate viscosity for a long time.

[0177] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

[0178] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

Claims

1. A sunscreen cosmetic composition, characterized in that: The sunscreen cosmetic composition comprises modified lignin, a composite emulsifier and water; The preparation method of the modified lignin comprises: using the compound represented by formula (I) and / or the condensation product of the compound represented by formula (I) to carry out a dehydration condensation reaction with lignin; R1 is selected from C 1-10 Alkyl or substituted C 1-10 alkyl; The composite emulsifier comprises lauryl polyglyceryl-3 polydimethylsiloxyethyl dimethicone and polyglyceryl-3 polydimethylsilyl hydroxyethyl dimethicone; In terms of mass percentage, in the sunscreen cosmetic composition, the modified lignin accounts for 0.01%-1.6%, the lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane accounts for 0.1%-2.5%, and the polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethylsiloxane accounts for 0.5%-5.5%.

2. The sunscreen cosmetic composition according to claim 1, characterized in that The compound represented by formula (I) is prepared by hydrolyzing the compound represented by formula (II); R1 is the same as claim 1, R2, R3, R4 are independently selected from C 1-10 Alkoxy.

3. The sunscreen cosmetic composition according to claim 2, characterized in that: R1 is selected from n-propyl, isopropyl, n-butyl, isobutyl, n-pentyl, isopentyl, neopentyl, hexyl, heptyl, octyl, nonyl; and / or, R2, R3, R4 are independently selected from methoxy, ethoxy, propoxy.

4. The sunscreen cosmetic composition according to claim 2, characterized in that: The mass ratio of the compound represented by formula (II) to the lignin is 1.5-5:1; and / or the average particle size of the modified lignin is 0.5-15 μm, further 0.5-10 μm, and further 1-6 μm.

5. The sunscreen cosmetic composition according to claim 1, characterized in that: The dehydration condensation reaction is controlled to be carried out at 50-95°C; and / or, in formula (I), R1 is selected from octyl.

6. The sunscreen cosmetic composition according to claim 1, characterized in that: In terms of mass percentage, in the sunscreen cosmetic composition, the modified lignin accounts for 0.05%-1.5%, further 0.1%-1.4%; and / or, In the sunscreen cosmetic composition, the lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane accounts for 0.3%-2.2%, further 0.3%-1.0%, by mass percentage; and / or, In terms of percentage by mass, in the sunscreen cosmetic composition, the polyglyceryl-3 polydimethylsilyl hydroxyethyl polydimethylsiloxane accounts for 0.7%-5.0%, and further accounts for 2.5%-3.5%.

7. The sunscreen cosmetic composition according to claim 1, characterized in that: The mass ratio of the lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane to the polyglyceryl-3 polydimethylsilylhydroxyethyl polydimethylsiloxane is 1:4-8, and further 1:5-7.

8. The sunscreen cosmetic composition according to claim 1, characterized in that: The sunscreen cosmetic composition further comprises a combination of one or more selected from inorganic sunscreen ingredients, organic sunscreen ingredients, moisturizers, preservatives, thickeners, skin conditioners, emollients, and chelating agents.

9. The sunscreen cosmetic composition according to claim 1, characterized in that: The sunscreen cosmetic composition comprises a thickening phase, a preservative phase, an emulsified phase, a physical sunscreen phase and an aqueous phase; Further, the thickening phase comprises disteardimonium hectorite and cyclohexasiloxane, the preservative phase comprises caprylic acid glyceryl and caprylyl glycol, the emulsifying phase comprises the modified lignin, propylene glycol dicaprylate, the lauryl polyglyceryl-3 polydimethylsiloxyethyl polydimethylsiloxane, the polyglyceryl-3 polydimethylsilyl hydroxyethyl polydimethylsiloxane, and ethylhexylglycerin, the physical sunscreen phase comprises zinc oxide, and the aqueous phase comprises magnesium sulfate, 1,3-propylene glycol, glycerin, 1,2-hexanediol, and the water; Furthermore, in the sunscreen cosmetic composition, measured by mass percentage: Disteardimethylammonium hectorite 0.01%-3.00% Cyclohexasiloxane 0.01%-20.00% Glyceryl Caprylate 0.01%-1.00% Caprylyl glycol 0.01%-1.00% Modified lignin 0.01%-1.60% Propylene glycol dicaprylate 0.01%-30.00% Lauryl Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone 0.1%-2.5% Polyglyceryl-3 Polydimethylsiloxyethyl Dimethicone 0.5%-5.5% Ethylhexylglycerin 0.01%-1.00% Zinc oxide 0.01%-25.00% Magnesium sulfate 0.01%-3.00% 1,3-Propanediol 0.01%-8.00% Glycerin 0.01%-5.00% 1,2-Hexanediol 0.01%-3.00% Water is added in an amount such that the total amount of the sunscreen cosmetic composition is adjusted to 100%.

10. A method for preparing the sunscreen cosmetic composition according to any one of claims 1 to 9, characterized in that: The preparation method comprises: mixing and emulsifying the components to prepare the sunscreen cosmetic composition.

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