CN114732744A

CN114732744A - Oil control composition based on cationic emulsifier and flake powder

Info

Publication number: CN114732744A
Application number: CN202210278537.9A
Authority: CN
Inventors: 黄诚赟; 丛远华; 郭奕光; 贾海东
Original assignee: Shanghai Jahwa United Co Ltd
Current assignee: Shanghai Jahwa United Co Ltd
Priority date: 2022-03-17
Filing date: 2022-03-17
Publication date: 2022-07-12

Abstract

The invention provides an oil control composition based on a cationic emulsifier and a flake powder, wherein the cationic emulsifier is used in an amount of 0.1 to 10% by weight, and the weight ratio of the flake powder to the cationic emulsifier is 50:1 to 1: 100. The invention also discloses application of the oil control composition in a skin external preparation.

Description

Oil control composition based on cationic emulsifier and flake powder

Technical Field

The invention relates to the field of skin external preparations and cosmetics, in particular to an oil control composition based on a cationic emulsifier and flaky powder.

Background

Young people have active sebaceous glands and vigorous sebaceous gland secretion, so that a series of skin problems such as acne and the like easily occur, and the oil-control cosmetic has high demand. The secretion of sebaceous glands in men is more active than in women and is more likely to be disturbed by the problem of oily skin. The market research report of the intellectual research consultation in 2018 shows that the attention degrees of male consumers on the efficacies of removing acnes, controlling oil and removing blackheads are 18.5%, 12.2% and 6.8%, and the 1 st, the 3 rd and the 7 th sites of the skin care efficacy attention rate list are listed. Therefore, the development of the cosmetic with good oil control efficacy and using feeling has higher value for capturing young consumers, particularly male consumers.

The powder has instant and rapid grease adsorption capacity, can adsorb sebum instantly, can continuously adsorb the sebum secreted by the subsequent sebaceous glands within a period of time, solves the problems of gloss, greasiness and the like, and has wide application in oil control products. However, there are problems with using only powder oil control: the powder is easy to float and rub mud, and the surface tension of the powder is large, so that the powder is difficult to be uniformly mixed, and negative feelings such as dryness, tightness and the like can occur after use. Therefore, in the oil control powder of cosmetics, the powder needs to be carefully screened, and meanwhile, the formula needs to be specifically designed.

Cationic emulsifiers refer to emulsifiers having a chemical structure with cationic groups, the molecular structure of which comprises cationic groups and alkyl chains. The cationic groups mainly comprise alkyl quaternary ammonium salt, alkyl pyridinium and alkyl amine salt, and generally have good heat resistance, light resistance, acid-base tolerance, surface activity, stability and biodegradability. The cationic surfactant can form a film on the surface of skin or hair due to the unique charge property, so that the cationic surfactant has unique product use feeling and is widely applied to hair products in particular. In contrast, cationic emulsifiers are used in skin care products less because of the wide use of anionic thickeners. However, the cationic surfactant has strong absorption feeling and film-forming property, can obviously shield the greasy feeling of grease, and is particularly suitable for application in oil control products. However, the cationic emulsifier has the problem of dry skin after use, and the problem needs to be subjected to targeted formula design to improve the use feeling of the product and obtain better market competitiveness.

CN101686910 reports compounding cationic emulsifiers with toner, which has better adhesion by the charge effect of the cationic emulsifiers. The feasibility of modifying the properties of the two raw materials by compounding the cation and the toner into a composition is shown.

The present inventors have surprisingly found that compounding a cationic emulsifier with a flake can result in a composition with good oil control properties.

Disclosure of Invention

In one aspect, an oil control composition based on a cationic emulsifier and flakes is provided, wherein the cationic emulsifier is used in an amount of 0.1% to 10% by weight, and the weight ratio of flakes to cationic emulsifier is 50:1 to 1: 100.

In a preferred embodiment, the flakes in the oil control composition are selected from the group consisting of: GLASTING-HM, boron nitride, flaky barium sulfate, and flaky zinc oxide. In a preferred embodiment, the amount of flakes in the oil control composition is from 0.1% to 10% by weight. In a preferred embodiment, the cationic emulsifier in the oil control composition is TA-100. In a preferred embodiment, the cationic emulsifier is present in the oil control composition in an amount of from 1% to 5% by weight. In a preferred embodiment, the weight ratio of the platelet powder to the cationic emulsifier in the oil control composition is from 2:1 to 1: 5. In a preferred embodiment, the oil control composition of the present invention further comprises cetearyl alcohol. In a preferred embodiment, the cetearyl alcohol is present in the oil control composition in an amount of 0.1% to 10% by weight.

In another aspect, the present invention is also directed to the use of the oil control composition in a topical skin preparation. In a preferred embodiment, the external preparation for skin is selected from: face cleaning lotion, cosmetic water, lotion, cream, facial mask and gel.

Drawings

FIG. 1 shows photographs of example 4 (left), example 5 (center) and example 6 (right) after being applied to artificial leather and left for 24 hours.

FIG. 2 shows photographs of (a) artificial leather background, (b) example 12, (c) example 11, and (d) example 2 after leveling the surface of the artificial leather and standing for 60 min.

FIG. 3 shows a photograph of each sample after being smeared and left standing for 30min in the reflectance test: (a) background, (b) blank, (c) example 11, (d) example 12, (e) example 1, (f) example 13 and (g) example 2.

Detailed Description

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are described herein. For the purposes of the present invention, the following terms are defined below.

To provide a more concise description, some of the quantitative representations presented herein are not modified by the term "about". It is understood that each quantity given herein is intended to refer to the actual given value, regardless of whether the term "about" is explicitly used, and also to refer to the approximation to such given value that would reasonably be inferred by one of ordinary skill in the art, including approximations due to experimental and/or measurement conditions for such given value.

To provide a more concise description, some quantitative expressions are recited herein as a range from about an X amount to about a Y amount. It should be understood that when a range is recited, the range is not limited to the upper and lower limits recited, but includes the entire range from about the X amount to about the Y amount or any amount therebetween.

The applicant unexpectedly found that by compounding the cationic emulsifier with the flaky powder in a specific ratio, the prepared composition has good oil control performance. The cationic emulsifier can obviously improve the dispersion state of the powder, and the compounding of the flaky powder can obviously improve the use feeling of the cationic emulsifier. Moreover, the use of the cationic emulsifier in combination with the flake powder has more excellent oil-controlling properties than the use of the cationic emulsifier alone or the powder itself.

The applicant has found that there are problems with the use of powder oil control alone: the powder has the advantages of easy powder floating and mud rubbing (see test example 3), high surface tension with the powder, difficult uniform mixing (see test example 4), and possibility of negative feelings of dryness, tightness and the like after use (see test example 2). Meanwhile, the use of a cationic emulsifier alone also has a problem of dry skin feel after use (see test example 2). Therefore, in order to solve these problems, a formulation is required to improve the use feeling of the product in a targeted manner, thereby achieving better market competitiveness.

The applicants have surprisingly found that compounding a cationic emulsifier with a platelet powder results in a composition with good oil control properties. The advantages of the compounded composition are as follows:

(1) the compounding of the cationic emulsifier can obviously reduce the surface tension of the powder and the grease, so that the grease is easier to combine with the powder, and the oil control performance of the cationic emulsifier is better than that of the powder or the cationic emulsifier which is used alone (test example 4);

(2) the compounding of the cationic emulsifier can improve the dispersion state of the powder and avoid the problems of floating powder, mud rubbing and the like (test example 3);

(3) the presence of the flaky powder can improve the skin feel of the cationic emulsifier, avoid excessive dryness after use, and the related properties are superior to those of spherical powder, reticulated powder and irregular powder (test example 2).

The composition based on the cationic emulsifier and the flaky powder has excellent use feeling and oil control capability and has high practical application value in the nursing of oily skin. Furthermore, stability tests show that the compositions of the invention based on cationic emulsifiers and flakes have good stability and tunability. By investigating various powder combinations and different powder-emulsifier ratios, the method can meet the supervision requirements of national regulations on cosmetics, and is beneficial to the practical application of the technology reported by the invention in the cosmetic industry.

The applicant applied the technique reported in the present invention to a new type of oil-controlling skin-care lotion for the coming to market, which has an overall preference and a purchase probability superior to those of the Biyuquan men's clean fine moisturizing milk and the Langshi men's oil-controlling moisturizing milk in a 60-person consumer preference test, wherein the advantages of the applicant's product over the Biyuquan men's clean fine moisturizing milk in terms of the overall preference and the purchase probability are statistically different (p < 0.05). In the term of effective oil control time of consumer self-evaluation, the average of applicants' product was 4.92 hours, which is a great advantage over 4.52 hours for two races. The proportion of consumers in which the applicant's product can effectively control oil for 6-8 hours is considerably better than that of the Bieuquan competitive products (p is less than 0.05). The consumer test results show that the technology reported by the invention can bring better oil control efficacy and use feeling to the oil control product, so that the product shows better competitiveness in the competition of the cosmetic market.

In some embodiments, the oil control compositions of the present invention comprise 0.1 to 10 wt% of a cationic emulsifier. In preferred embodiments, the oil control composition of the present invention comprises from 0.1 to 5 wt%, from 0.1 to 3 wt%, or from 0.5 to 2.5 wt% of a cationic emulsifier. In a specific embodiment, the oil control composition of the present invention comprises 2.5 wt% of a cationic emulsifier. In a particular embodiment, the oil control composition of the present invention comprises 5% by weight of a cationic emulsifier.

In some embodiments, the oil control compositions of the present invention comprise 0.1 to 10 weight percent of the flake powder. In preferred embodiments, the oil control composition of the present invention comprises 0.1 to 5 wt% or 0.1 to 3 wt% of the flake powder. In a particular embodiment, the oil control composition of the present invention comprises 1% by weight of flakes. In a specific embodiment, the oil control composition of the present invention comprises 2.5 wt.%, 5 wt.%, or 10 wt.% of the flake powder.

In some embodiments, the weight ratio of the flake powder to the cationic emulsifier in the oil control composition of the present invention is from 50:1 to 1: 100. In a preferred embodiment, the weight ratio of the platelet powder to the cationic emulsifier in the oil control composition of the present invention is from 2:1 to 1: 5.

In some embodiments, other emulsifiers are also included in the oil control compositions of the present invention. In a preferred embodiment, the emulsifier is cetearyl alcohol.

In some embodiments, the oil control compositions of the present invention comprise 0.1 to 10 wt.% of other emulsifiers. In preferred embodiments, the oil control compositions of the present invention comprise 0.1 to 5 wt.%, 0.1 to 3 wt.%, or 0.1 to 2 wt.% of other emulsifiers. In a specific embodiment, the oil control composition of the present invention comprises 2% by weight cetearyl alcohol.

The oil control composition comprising a cationic emulsifier and flakes can be a topical skin agent. In some embodiments, the external preparation for skin may be an aqueous product. For example, the aqueous component may be used in an amount greater than 50 wt%, greater than 60 wt%, greater than 70 wt%, greater than 80 wt%, greater than 90 wt%, or greater than 95 wt% of the external skin preparation.

In some embodiments, an oily component may also be included in the external skin preparation. For example, the oily component may be used in an amount of 0.1 to 20% by weight, 0.5 to 15% by weight, or 2 to 10% by weight in the skin external preparation. In a specific embodiment, the oily component of the external preparation for skin comprises a volatile silicone oil. In a specific embodiment, the oily component of the external preparation for skin comprises KF-995.

It is worth mentioning that in the embodiment of the present invention, after the cationic emulsifier (e.g., TA-100) is compounded with the powder (e.g., flake powder), the dispersion of the powder can be significantly improved, and the risk of the product quality problems such as floating powder, slushing and the like occurring in the material body can be reduced. Upon compounding with cationic emulsifiers (e.g., TA-100), the dispersibility of the powders (e.g., flakes) is significantly improved. The reasons for this include: the compounding of the cationic emulsifier reduces the surface tension of the powder, the grease and the skin, and plays a vital role in improving the gloss control effect of the material body. From another perspective, the samples after addition of the powder also showed better shine inhibition than the samples using only cationic emulsifier.

The invention will be further illustrated by the following specific examples. It should be noted that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as many insubstantial modifications and variations of the invention may be made by those skilled in the art in light of the above teachings. Test methods without specifying specific conditions in the following examples are generally performed under conventional conditions or conditions recommended by the manufacturers. All percentages and parts are by weight unless otherwise indicated.

Experimental materials:

silica (silica L51): purchased from AGC Si-Tech co, Ltd;

silica (silica T30): purchased from WACKER-CHEMIE GMBH;

titanium dioxide composite powder (Look 100): from Dismann Fine chemical (Shanghai) Co., Ltd;

polymethylsilsesquioxane (PSQ): purchased from GRANT INDUSTRIES, inc;

bamboo powder: from CRODA (standing grain);

rice silk powder: purchased from CRODA (standing grain);

composite functional powder (GLASTING-HM): purchased from Chuzhou gurui mining, Limited liability company;

boron nitride (Softtouch CC 6004): purchased from pran, shanghai, biochem technologies, ltd;

barium sulfate flake (BASO4 HG): purchased from Shanghai Rainbow Jiu Enterprise development Co., Ltd;

zinc oxide (pigment grade): purchased from Merk KGaA;

flaky zinc oxide (XZ-1000 FST): shanghai hong Jiu Enterprise development Co., Ltd;

caprylic/capric triglyceride (M318): purchased from Henkel corporation;

KF-995: available from Shin-Etsu Chemical Co., Ltd;

TA-100: purchased from EVONIK corporation;

cetostearyl alcohol: purchased from Emery Oleochemicals;

p-hydroxyacetophenone: purchased from Symrise corporation;

stearic acid citric acid glyceride: purchased from dr. straettams GmbH merkurin;

polyquaternium-37: purchased from BASF corporation;

artificial leather: the leather business purchased from Chunhui, model: PVC artificial leather, naked color.

An experimental instrument:

weighing a balance: METTLER TOLEDO, PB 4002-N;

a constant-temperature water bath kettle: Shanghai-Heng scientific instruments Inc., HWS-28;

a desk-top homogenizer: POLYTRON, PT 3100D;

a desk type stirrer: IKA EUROSTAR, power control-visc;

reflection rate test equipment: cutomer dual MPH 580+ Skin-Glossimer GL 200;

constant temperature incubator at 40 ℃: MMM company, INCECLV 707, Germany;

25 ℃ constant temperature incubator: FRIOCELL707, MMM, Germany;

4 ℃ constant temperature incubator: friocell707, MMM, Germany.

Test example 1: determination of the oil and fat adsorption Capacity of different powders

In a 150ml beaker 5g of powder was weighed and the weight of the beaker was weighed and recorded. Thereafter, about 0.2g of caprylic/capric triglyceride (M318) was added and stirred with a glass rod to disperse the oil and powder uniformly. If the powder in the beaker is still dry powder or bonded powder dough, repeating the steps of adding the oil and stirring uniformly according to the condition that the oil absorption capacity of the powder is not saturated. And (3) adding the grease again into the sample forming the bonded powder dough, then reducing the bonding degree, completely scraping the powder bonded on the glass rod to the wall of the beaker according to the fact that the adsorption quantity of the powder is saturated, weighing and recording the weight of the beaker again, and considering the saturated adsorption quantity of the powder as the difference between the weight of the beaker and the weight of the beaker before adding the grease.

Note: the silica T30 bulk was very high, reducing the test amount to 2g

Table 1: oil adsorption and oil absorption per unit weight of each powder

In test example 1, the adsorption capacity of the powder of 11 for M318 was examined, and the examined powder was classified as follows according to its microstructure:

(1) flake powder: GLASTING-HM, boron nitride, flaky barium sulfate, and flaky zinc oxide;

(2) spherical powder: silica L51, silica powder PSQ;

(3) network-like agglomerated powder: silica T30;

(4) other powders: look 100, bamboo powder, rice silk powder, zinc oxide (pigment grade).

Among them, the first three powder suppliers provide scanning electron micrographs to demonstrate their microstructures. The fourth group of powder suppliers did not provide sem pictures, or sem pictures showed that the microstructure was an agglomeration of irregular particles. Table 1 summarizes the oil absorption and oil absorption per weight of the above various powders in the oil absorption test.

Of all the powders examined, silica T30 exhibited the highest oil absorption per unit weight, 968g/100g of powder, much higher than the other powders tested. The reason is that the silica T30 is prepared by vapor deposition, the powder is aggregated in a network shape, and a large number of gaps are arranged in the structure to accommodate grease, so that the oil absorption rate is extremely high. However, the network-like aggregate structure also made the skin feel extremely dry, and the relevant results were shown in test example 2.

In the flaky powder, the oil absorption rate per unit weight of the composite functional powder GLASTING-HM is the highest and is 214.0g/100g of powder, and the second powder is ranked among all the powders. The oil absorption rates per unit weight of boron nitride (Softtouch CC 6004), flaky barium sulfate (BASO4 HG) and flaky zinc oxide (XZ-1000FST) were 110.0g/100g of powder, 80.4g/100g of powder and 65.0g/100g of powder, respectively. The reason for this is that the surface of the composite functional powder GLASTING-HM is modified, the specific surface area is larger, the oil absorption rate per unit weight is improved, the surface of other flaky powder is smooth, the oil absorption capacity is weaker, but the flaky powder has a smoother skin feel, and the relevant results are shown in more detail in test example 2.

In the spherical powder, the oil absorptions per unit mass of silica L51 and silicon powder PSQ were 157.6g/100g powder and 52.0g/100g powder, respectively. The former sphere particles have hollow structures to improve the oil absorption capacity, and the latter sphere particles are smooth spheres with the lowest oil absorption capacity due to small surface area and are usually used as a slipping agent.

Among other powders, the oil absorption capacity of the powder is sequentially bamboo powder, rice silk powder, composite titanium dioxide powder hook 100 and zinc oxide (pigment grade) from large to small, and the oil absorption rate of the powder per unit weight is 192.8g/100g powder, 140.0g/100g powder, 111.6g/100g powder and 72.0g/100g powder. In the next part of the work, all the layered powders, as well as the powders with higher oil absorption among the various types of powders, were selected for more detailed examination.

Examples 1 to 10: preparation of cationic emulsions with addition of different powders

Example 1: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 178.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath kettle for heating for 30 min. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 2: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 133.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. In a 250ml beaker, 5g of GLASTING-HM and 40g of deionized water were weighed and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the body had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24 hours for later use.

Example 3: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 128.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. In a 250ml beaker, 10g of GLASTING-HM and 40g of deionized water were weighed and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk homogenizer to uniformly disperse the material, then keeping the speed of 5000rpm for homogenization, slowly adding the phase B while the mixture is hot (about 1min is finished), and keeping the mixture for homogenization for 2min to completely emulsify the material after the addition is finished. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 4: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 118.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. 20g of GLASTING-HM and 40g of deionized water were weighed in a 250ml beaker and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 5: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 118.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. Silica L5120 g and 40g of deionized water were weighed into a 250ml beaker and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 6: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 134.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath kettle for heating for 30 min. Silica T304 g and 40g of deionized water were weighed into a 250ml beaker and homogenized using a bench top homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 7: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 128.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. In a 250ml beaker, 10g of boron nitride and 40g of deionized water were weighed and homogenized using a desk homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk homogenizer to uniformly disperse the material, then keeping the speed of 5000rpm for homogenization, slowly adding the phase B while the mixture is hot (about 1min is finished), and keeping the mixture for homogenization for 2min to completely emulsify the material after the addition is finished. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24 hours for later use.

Example 8: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 128.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. 10g of flaky barium sulfate and 40g of deionized water were weighed in a 250ml beaker, and homogenized for 2min at 5000rpm using a desk homogenizer to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 9: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 128.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. 10g of zinc oxide (pigment grade) and 40g of deionized water were weighed into a 250ml beaker and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24 hours for later use.

Example 10: KF-99512 g, TA-1005 g and cetearyl alcohol 4g were weighed in a 500g beaker, sealed with a PE film and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 128.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. 10g of flaky zinc oxide and 40g of deionized water were weighed in a 250ml beaker, and the powder was uniformly dispersed by homogenizing for 2min at 5000rpm using a desk homogenizer. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Table 2: preparation of cationic emulsions with addition of different powders

In examples 1-10, ten cationic emulsions formulated with different powders were prepared, all sample formulations were formulated with 2.5% TA-100+ 2% cetearyl alcohol, emulsified oils were 6% KF-995, and 0.2% p-hydroxyacetophenone was formulated to enhance preservative performance. Wherein example 1 is a cationic emulsion base without any powder added; examples 2-4 to base the matrix emulsion was added 2.5%, 5% and 10% powdered flakes GLASTING-HM, respectively; example 5 addition of 10% silica L51 based on the matrix emulsion; example 6 the addition of 2% silica T30 based on the matrix emulsion; examples 7-10 each added 5% powder based on the cationic base emulsion, in that order boron nitride, platy barium sulfate, zinc oxide (pigment grade), and platy zinc oxide.

Test example 2: coefficient of friction test for examples 1 to 10

The friction coefficient of examples 1 to 10 on the surface of the artificial leather was measured using the slope method in the following manner:

cutting the artificial leather into a rectangle of 7cm multiplied by 15cm, placing a weight with a smooth bottom surface of 10kg above the artificial leather, standing for 24h, and taking out to compact and flatten the artificial leather. Thereafter, 1g of the sample of the example was weighed out and applied uniformly on the surface of the artificial leather, and the coating was left standing for 24 hours with the upper side facing the surface and then subjected to the test.

The device of test is fixed for one end, and the dull and stereotyped of other end liftable places artificial leather on the dull and stereotyped, adjusts the gradient of dull and stereotyped afterwards, observes the slider of placing on artificial leather and whether can slide. The slider used was a short cylindrical hollow PP slider with a diameter of 3cm, a height of 1.85cm and a weight of 2.67 g. And measuring the inclination angle of the flat plate when the sliding block just can slide by using the protractor, and calculating the friction coefficient between the artificial leather and the sliding block according to the inclination angle.

Table 3: examples 1-10 coefficient of friction against PP hollow short cylindrical slider after application to the surface of artificial leather and drying

Examples	Minimum slidable elevation angle (°)	Coefficient of friction	Remarks for note
				Blank space	14.5	0.258
1	31.4	0.610
				2	30.5	0.588
3	28.6	0.545
				4	26.8	0.505
5	33.3	0.657	Distortion of artificial leather
				6	42.3	0.908	Distortion of artificial leather
7	24.3	0.452
				8	21.9	0.402
9	31.2	0.605
				10	23.9	0.443

Table 3 summarizes the minimum elevation angle at which the slider can slide after smearing out each embodiment, and the corresponding coefficient of friction (tangent function of the minimum slidable elevation angle) in the slider experiment. The minimum slidable elevation angle of the bottom of the artificial leather relative to the PP hollow sliding block is 14.5 degrees, and the corresponding friction coefficient is 0.258. After the TA-100 emulsion without powder added is coated (example 1), the minimum slidable inclination angle is increased to 31.4 degrees, and the corresponding friction coefficient is 0.610, and the above experiment results show that the TA-100 emulsion is dry in texture after being coated, so that the friction coefficient of the surface of the artificial leather is obviously increased.

The minimum slidable elevation angles of the samples for GLASTING-HM (examples 2-4) were 30.5 °, 28.6 ° and 26.8 °, respectively, 2.5%, 5% and 10% added to the base of the TA-100 emulsion, corresponding to coefficients of friction of 0.588, 0.545 and 0.505, respectively. After the flaky GLASTING-HM powder is compounded, the friction coefficient of the surface of the artificial leather is reduced, and the reduction amplitude is increased along with the increase of the compounding amount of the powder. The experimental results show that the compounding of the flaky powder GLASTING-HM can reduce the dry and astringent feeling of the TA-100 emulsion after being smeared.

As shown in FIG. 1, after example 5 in which 10% silica L51 was added and example 6 in which 2% silica T30 was added were applied to the surface of the artificial leather and left standing for 24 hours, the artificial leather was severely twisted. It is shown that the consumer is likely to experience a negative feeling of skin tightness after using examples 5 and 6, whereas example 4 with 10% of GLASTING-HM powder added does not see a similar phenomenon. The friction coefficient measurement is affected by the distortion of the artificial leather caused by the addition of the powder, and although the test is performed by selecting a part of the artificial leather with relatively small central distortion, the test result is still affected, so that the friction coefficients of the samples of examples 5 and 6 are only used as reference.

Example 5, which was compounded with 10% silicon powder L51, had a minimum slidable inclination of 33.3 °, corresponding to a coefficient of friction of 0.657, which is slightly higher than that of example 1, to which no powder was added, indicating that silica L51 did not have a significant effect on improving the dry and astringent feel of the body. Example 6, which was compounded with 2% silica powder T30, had a minimum slip angle of 42.3 ° and a corresponding coefficient of friction of 0.908, which was further improved over example 1. It can be seen that T30 has strong oil adsorption capacity, but the skin feel is too dry, which cannot help to alleviate the problem of dry residual feel of TA-100 emulsion, but can further amplify the problem. The experimental results show that the two powders are combined with TA-100, so that the use feeling which is satisfied by consumers is difficult to obtain.

Example 7 and example 8 were compounded with 5% boron nitride and 5% barium sulfate flakes, respectively, and the minimum slidable elevation angles of the two samples were 24.3 ° and 21.9 ° in this order, which corresponds to friction coefficients of 0.452 and 0.402, which are significantly lower than those of example 1. The two powders have flat surfaces, have smaller surface areas, are lower than GLASTING-HM in oil absorption rate, but show better slip-assisting effect, and can obviously improve the use feeling of the formula if being compounded with cationic emulsion.

The powders compounded in example 9 and example 10 are both zinc oxide, the former is amorphous pigment grade powder, and the latter is regular flaky powder. The minimum slidable elevation angles of the two samples were 31.2 ° and 23.9 °, respectively, corresponding to friction coefficients of 0.605 and 0.443, respectively. The experimental results comparing the two samples show that the flaky zinc oxide shows an obvious excellent sliding assisting effect compared with the amorphous powder.

The experimental results show that the compounding of the flaky powder and the TA-100 emulsion can improve the use feeling of the emulsion matrix to a certain extent, and the powder with a smooth surface has better sliding assisting effect. Considering that the achievement of oil control efficacy is of critical importance in oil control products, the powder of the present invention is more extensively studied in the following, since it shows better performance than other powders of spherical, amorphous and network-like aggregation under the same oil absorption.

Examples 11 to 12: preparation of different GLASTING-HM slurries

Example 11: weighing 2.5g of GLASTING-HM powder and 97.5g of deionized water in a 250ml beaker, homogenizing at 5000rpm for 2min to uniformly disperse the powder, transferring the sample into a 150ml PET bottle cap with a cover, and placing the cap on the bottle cap for 24h for later use.

Example 12: weighing 5g of GLASTING-HM powder and 95g of deionized water in a 250ml beaker, homogenizing at 5000rpm for 2min to uniformly disperse the powder, transferring the sample into a 150ml PET bottle cap with a cover, and placing the cap for 24h for later use.

Table 4: raw material charge of example 11 and example 12

Examples	GLASTING-HM powder	Deionized water
			11	2.5	97.5
12	5	95

Examples 11 and 12 correspond to aqueous dispersions with GLASTING-HM addition levels of 2.5% and 5%, respectively. Since the powder was deposited in the aqueous phase, the samples of examples 11 and 12 were shaken 20 times before being used to mix them uniformly.

Test example 3: dispersibility examination of example 2, example 11 and example 12

A plurality of 3cm x 3cm areas were drawn on the artificial leather, and 100. mu.L of each of the samples of example 2, example 11 and example 12 was drawn up using a pipette gun, dropped into the corresponding area of the artificial leather, and spread uniformly. Then, the mixture was left standing for 60min to observe the dispersion of the sample on the surface of the artificial leather.

The dispersion of example 2, example 11 and example 12 on the surface of the artificial leather is shown in FIG. 2. In example 2, the powder was uniformly distributed after the troweling without the floating phenomenon. Examples 11 and 12, because of their high surface tension with respect to the artificial leather, the suspension dispersions themselves are difficult to spread evenly on the surface of the artificial leather and exist in the form of droplets. After standing for 60min, the artificial leather of example 11 and example 12 showed significant floating and uneven distribution on the surface, and the severity of floating increased with the increase of the powder content. Therefore, after TA-100 is compounded with the powder, the dispersion of the powder can be obviously improved, and the risk of product quality problems such as floating powder, mud kneading and the like of the material body is reduced.

Examples 13 and 14: preparation of oil-controlling emulsions

Example 13: KF-99512 g, TA-10010 g and cetearyl alcohol 4g were weighed in a 500g beaker, sealed with a PE film and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 173.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 14: in a 500g beaker, KF-99512 g, glyceryl stearate citrate 5g and cetearyl alcohol 4g were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 178.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath kettle for heating for 30 min. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Table 5: the amount of each raw material added in example 13 and example 14

The preparation process of the embodiment 13 and the embodiment 14 is completely the same as that of the embodiment 1, the embodiment 13 adjusts the dosage of TA-100 from 2.5 percent to 5 percent on the basis of the embodiment 1, and the embodiment 14 replaces the TA-100 with the equivalent glycerol stearate citrate.

Test example 4: oil light inhibition experiments of examples 1-2 and examples 11-14

The test was carried out in a constant temperature and humidity laboratory at a constant temperature of 20 ℃ and a constant humidity of 50%. Several 3cm by 3cm areas were drawn on the artificial leather, 5. mu.L caprylic/capric triglyceride (M318) and 100. mu.L from the corresponding example were added to the areas using a pipette and spread evenly, and left to stand for 30min to completely evaporate the water. The samples were then tested for light reflectance using a Glossimeter, and a total of four data points (two trisections of each of the two diagonals in the test area) were determined for each sample, and the average was calculated in triplicate for each test point.

Table 6: total reflectance, direct reflectance and direct reflectance ratio in the oil light suppression experiments of examples 1-2 and examples 11-14

The total reflectance, direct reflectance and direct reflectance ratios of examples 1-2 and examples 11-14 in the oil light inhibition experiment are summarized in table 6, and the sample photographs are shown in fig. 3.

The background values, i.e., the total reflectance and the direct reflectance of the artificial leather itself, were 5.27% and 52.83%, respectively. The total reflectivity and the direct reflectivity of the blank sample which is only smeared with the grease and is not smeared with the emulsion are respectively 21.13 percent and 90.37 percent, and are obviously improved compared with the background value.

The total and direct reflectivities of the samples of the spread grease and 2.5% TA-100 emulsion (example 1) were 9.92% and 76.99%, respectively, which were reduced by 53.05% and 14.81%, respectively, compared to the blank value, indicating that TA-100 has a matte finish that significantly reduces the oily feel of the oily surface even without the compounded powder.

The total and direct reflectance of the samples of the spread and 2.5% glyceryl stearate citrate emulsion (example 14) were 10.40% and 75.84%, respectively, which are reduced by 50.80% and 16.08%, respectively, compared to the blank. The oil control emulsion sold in the market usually adopts an anionic formula to obtain better absorption feeling and matte feeling, and the experimental result proves that the matte effect of the cation is slightly better than that of an anionic emulsifying system, and the oil control emulsion can be converted into an oil control product with market competitiveness by proper formula design.

The total and direct reflectivities of the samples of the spread and 5% TA-100 emulsion (example 13) were 10.32% and 72.88%, respectively, which were reduced by 51.15% and 13.82%, respectively, from the blank, with a small gap in the data associated with example 1. The possible reason is that the matte feeling of the TA-100 comes from the film forming property of the TA-100, a sample with the TA-100 content of 2.5 percent is enough to form a cationic film, and the change of the matte property is not obviously influenced by further increasing the film forming thickness by adjusting the dosage of the TA-100.

The total and direct reflectances of the greased and 2.5% GLASTING-HM powder (example 11) samples were 13.32% and 74.49%, respectively, which were a 36.97% and 17.57% reduction over the blank value, respectively. It is noted that since the surface tension of the powder dispersion and the oil phase is large, the two phases cannot be uniformly mixed, and thus the state of the artificial leather is remarkably different at different positions (see fig. 3). The total reflectivity of two points is more than 15% in the oil-light test experiment, while the total reflectivity of the other two test points is less than 11%, and the dispersion degree of data exceeds that of all the samples. At the same time, the direct reflectance ratios of the test points are also very different, with the highest value being 87.04% and the lowest value being 52.46%, the former being close to the oiled blank and the latter being close to the background.

The total and direct reflectance of the samples coated with grease and 5% GLASTING-HM powder (example 12) were 7.65% and 63.76%, respectively, which were reduced by 63.82% and 29.45%, respectively, compared to the blank. As shown in fig. 3, the uniform dispersion effect of the powder and the grease of the sample is still poor, so that the albedo and the direct reflection ratio of each test point in the test are still obviously different.

The total and direct reflectivities of the samples of the spread oil and 2.5% TA-100+ 2.5% GLASTING-HM powder (example 2) were 7.87% and 68.37%, respectively, which were reduced by 62.77% and 64.35%, respectively, compared to the blank. As shown in FIG. 3, the sample was uniformly dispersed without dusting, and no oily light was observed.

The experimental results show that after the powder is compounded with TA-100, the dispersibility of the powder is obviously improved. The reason for this is that the TA-100 formulation reduces the surface tension of the powder, oil and skin and is of great importance in improving the gloss control of the body. From another perspective, the powder added samples also exhibited better oil suppression than TA-100 alone.

Examples 15 to 19: preparation of cationic emulsions with different cationic to powder mass ratios

Example 15: in a 500g beaker, 9951 g of KF-1000.2 g, 0.2g of TA-1000.2 g and cetearyl alcohol were weighed, sealed with a PE film, and then placed in a 90 ℃ water bath and heated for 30 min. 0.4g of p-hydroxyacetophenone and 147.2g of deionized water are weighed in a 200ml beaker, 1g of polyquaternium-37 powder is slowly sprinkled in under the stirring of a cross paddle at 500rpm and kept stirring for 5min, after the macromolecular powder is completely infiltrated, the stirring speed is increased by 1000rpm and kept stirring until the macromolecular powder is completely dispersed uniformly, and then the mixture is sealed by a PE film and is placed in a 90 ℃ water bath pot to be heated for 30 min. In a 250ml beaker, 10g of GLASTING-HM and 40g of deionized water were weighed and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the body had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. After the material body is cooled to about 40 ℃, the material body is transferred into a 150ml transparent PET bottle with a cover to be covered and kept stand for 24 hours for standby.

Example 16: in a 500g beaker, 9955 g of KF, 1002 g of TA and 2g of cetostearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 147.6g of deionized water are weighed in a 200ml beaker, 1g of polyquaternium-37 powder is slowly sprinkled under the stirring of a cross paddle at 500rpm and kept stirring for 5min, after the macromolecular powder is completely infiltrated, the stirring speed is increased by 1000rpm and kept stirring until the macromolecular powder is completely dispersed uniformly, and then the mixture is sealed by a PE film and is placed in a 90 ℃ water bath kettle to be heated for 30 min. In a 250ml beaker, 2g of GLASTING-HM and 40g of deionized water were weighed and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. After the material body is cooled to about 40 ℃, the material body is transferred into a 150ml transparent PET bottle with a cover, and the bottle is sealed and kept stand for 24 hours for standby.

Example 17: in a 500g beaker, 4g of KF-99512 g, TA-1005 g and cetearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 138.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath kettle for heating for 30 min. In a 250ml beaker, 2g of GLASTING-HM and 40g of deionized water were weighed and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk homogenizer to uniformly disperse the material, then keeping the speed of 5000rpm for homogenization, slowly adding the phase B while the mixture is hot (about 1min is finished), and keeping the mixture for homogenization for 2min to completely emulsify the material after the addition is finished. After the body had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was prevented from delaminating until the body cooled to about 40 ℃ and gelled using a stand mixer with stirring at 200 rpm. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 18: KF-99512 g, TA-10010 g and cetearyl alcohol 4g were weighed in a 500g beaker, sealed with a PE film and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 131.6g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath kettle for heating for 30 min. In a 250ml beaker, 2g of GLASTING-HM and 40g of deionized water were weighed and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk type homogenizer to uniformly disperse the material, then keeping 5000rpm for homogenization, slowly adding the phase B while the phase B is hot (about 1min is finished), and keeping homogenization for 2min after the phase A is completely added to completely emulsify the material. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was stirred at 200rpm using a stand mixer to prevent the body from delaminating until the body cooled to about 40 ℃ to set. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24h for later use.

Example 19: in a 500g beaker, 99512 g of KF, 10020 g of TA and 4g of cetostearyl alcohol were weighed, sealed with a PE film, and heated in a 90 ℃ water bath for 30 min. 0.4g of p-hydroxyacetophenone and 123.4g of deionized water are weighed in a 200ml beaker, sealed by a PE film and then placed in a 90 ℃ water bath for heating for 30 min. In a 250ml beaker, 0.2g GLASTING-HM and 40g deionized water were weighed and homogenized using a bench homogenizer at 5000rpm for 2min to disperse the powder uniformly. After the phase A is heated, homogenizing at 5000rpm for 1min by using a desk homogenizer to uniformly disperse the material, then keeping the speed of 5000rpm for homogenization, slowly adding the phase B while the mixture is hot (about 1min is finished), and keeping the mixture for homogenization for 2min to completely emulsify the material after the addition is finished. After the mass had cooled to about 60 ℃, phase C was added and the powder was again homogenized at 5000rpm for 2min to completely disperse the powder. Thereafter, the body was prevented from delaminating until the body cooled to about 40 ℃ and gelled using a stand mixer with stirring at 200 rpm. And finally, transferring the material body into a 150ml transparent PET bottle with a cover, sealing and standing for 24 hours for later use.

Table 7: preparation of cationic emulsions with addition of different powders

Examples 15-19 5 parts of cationic emulsions with different cationic to powder mass ratios were prepared, with the cationic and powder respectively fixed at TA-100 and GLASTING-HM. In examples 15 to 19, the contents of cations were 0.1%, 1%, 2.5%, 5% and 10% in this order; the addition amounts of the powdered flakes GLASTING-HM were 5%, 1% and 0.1% in this order. Examples 15 and 16 were formulated with 0.5% polyquaternium-37 thickener to support the structure of the body due to the low level of cationic emulsifier. The addition amounts of the volatile silicone oil and the cetearyl alcohol are adjusted correspondingly with the adjustment of the addition amount of the cationic emulsifier.

Test example 5: stability test

In each example, 30g of the X3 material body was weighed and placed in 3 capped 50ml transparent PET bottles, and after sealing the caps, the 3 PET bottles were placed in 40 ℃, 25 ℃ and 4 ℃ incubator for 30 days. The sample was taken out after 30 days and observed for appearance after standing at room temperature for 24 hours.

Table 8 shows a summary of the stability test results for examples 2-4, examples 7-8, example 10 and examples 15-19.

TABLE 8

All samples of the cationic emulsion compounded flake powder were subjected to stability tests at 40 ℃, 25 ℃ and 4 ℃, and the stability test results of all the samples are summarized in table 8.

The cationic emulsifier and cetearyl alcohol of examples 2, 3, 4, 7, 8, 10 and 17 were added at fixed amounts of 2.5% and 2%, and the samples prepared were highly viscous emulsions having weak fluidity. The samples were white except for example 8 where the body appeared slightly gray due to the light scattering properties of the powder of flaky barium sulfate. Compared with a newly prepared sample, the stability of the samples at 40 ℃, 25 ℃ and 4 ℃ for one month is not obviously different, and the stability problems of layering, demulsification, caking, flocculation, powder agglomeration and the like do not occur.

The sample in example 15 is mainly supported by cationic emulsifier due to low addition of emulsifier, and the added amount of the added powder is high, so that the material body is in a slightly gray suspension. Example 15 no significant difference was observed in comparison to the freshly made samples after a one month stability test at 40 ℃, 25 ℃ and 4 ℃.

In example 16 and example 18, the former compound a thickener due to a cationic emulsifier, and the latter loses fluidity due to a higher addition amount of a cationic emulsion, and becomes a white soft cream. None of the two examples above showed a significant difference from the freshly prepared samples after a one month stability test at 40 ℃, 25 ℃ and 4 ℃.

Example 19 the resulting body was a relatively firm cream due to the high level of cationic emulsifier added. After the one-month stability at 40 ℃, 25 ℃ and 4 ℃ is examined, no obvious difference is found compared with a new sample.

The stability of all tested samples meets the requirements of national regulations GB/T29665 (O/W) and QB/T1857 on heat resistance and cold resistance of cosmetics. In addition, the examples with greatly different proportions show good stability in the heat-resistant and cold-resistant stability tests, which shows that the composition reported by the invention has great adjustability and is beneficial to the practical application of the technology reported by the invention in the cosmetic industry.

The cationic emulsion prepared in the above example was used for the preparation of an external preparation for skin. The skin external preparation is preferably a cosmetic composition such as a lotion, essence, gel, spray, etc. The weight percentage of the cationic emulsion in the skin external preparation is 0.0001-20% (w/w). Preferably 0.001-10% (w/w). More preferably 0.001-5% (w/w). Most preferably 0.01% to 5% (w/w).

The following are examples of specific uses of cationic emulsions in external skin preparations, and formulations and methods for preparing these dosage forms. In the tables, "-" indicates no addition.

Example 20: preparation of face cream

Example 21: preparation of the emulsion

Example 22: preparation of jelly

Example 23: preparation of essence

Example 24: preparation of facial mask

Example 25: preparation of the spray

Claims

1. An oil control composition based on a cationic emulsifier and flakes, wherein the cationic emulsifier is present in an amount of 0.1 to 10% by weight and the weight ratio of flakes to cationic emulsifier is from 50:1 to 1: 100.

2. The oil control composition of claim 1, wherein the flakes are selected from the group consisting of: GLASTING-HM, boron nitride, flaky barium sulfate, and flaky zinc oxide.

3. The oil control composition of claim 2, wherein the flakes are present in an amount of 0.1% to 10% by weight.

4. The oil control composition of claim 1, wherein the cationic emulsifier is TA-100.

5. The oil control composition of claim 4, wherein the cationic emulsifier is present in an amount of 1% to 5% by weight.

6. The oil control composition of claim 1, wherein the weight ratio of the flakes to the cationic emulsifier is from 2:1 to 1: 5.

7. The oil control composition of claim 1, wherein the composition further comprises cetearyl alcohol.

8. The oil control composition of claim 7, wherein the cetearyl alcohol is present in an amount of 0.1% to 10% by weight.

9. Use of the oil control composition of any one of claims 1-8 in an external preparation for skin.

10. The use of claim 9, wherein the external skin agent is selected from the group consisting of: cleansing milk, cosmetic water, lotion, cream, facial mask and gel.