A bentonite composition with cleaning and oil control efficacy, and a preparation method and application thereof

Abstract

The application discloses a bentonite composition with cleaning and oil control effects and a preparation method and application thereof. The preparation of the bentonite composition comprises the following steps: uniformly dispersing bentonite into an organic solvent to obtain a bentonite organic dispersion liquid, then adding the bentonite organic dispersion liquid into hot spring water, stirring to obtain a mixed dispersion liquid, removing the organic solvent in the bentonite organic dispersion liquid to obtain bentonite hot spring water; adding a hydrolyzed starch alcohol solution into the bentonite hot spring water, uniformly stirring and heating to obtain the bentonite composition. Through the synergistic interaction of the bentonite, the hydrolyzed starch and the minerals in the hot spring water, the finally obtained bentonite composition has good cleaning capacity and sustained oil control capacity.

Description

A bentonite composition with cleaning and oil-controlling effects, its preparation method and application Technical Field

[0001] This invention belongs to the field of cosmetic raw material technology, and specifically relates to a bentonite composition with cleansing and oil-controlling effects, its preparation method and application. Background Technology

[0002] Sebum is oil produced and secreted by sebaceous gland cells in the skin and then released onto the skin's surface. Excessive sebum on the skin's surface can clog pores, leading to thickened stratum corneum and skin conditions such as acne and seborrheic dermatitis. Currently, there are many types of oil-removing facial cleansers on the market, most of which are made from a combination of relatively simple surfactants and moisturizers to remove facial oil. However, because these cleansers contain a large amount of surfactants, they can leave the skin feeling tight after use. Furthermore, their oil-removing effect is only temporary and does not effectively control oil production. After a period of use, excessive oil production may actually occur, and long-term use can worsen acne-prone skin problems.

[0003] Bentonite is a non-metallic mineral whose main component is montmorillonite. It possesses excellent physicochemical properties and can be used as a purifying and decolorizing agent, binder, thixotropic agent, suspending agent, and catalyst, finding wide application in agriculture, light industry, cosmetics, and pharmaceuticals. Bentonite is rich in minerals, providing essential nutrients for human skin; it has exceptional adsorption capacity, thoroughly removing deep-seated dirt and oil, cleaning skin channels, and facilitating the absorption of trace elements and nutrients. Its unique negative charge and naturally similar pH to skin can stimulate cell vitality, improve microcirculation, and promote metabolism. However, bentonite is insoluble in water and tends to aggregate and precipitate when used in aqueous products. Furthermore, the dispersion of bentonite in a formulation is affected by dispersion time, stirring intensity, and temperature, making it inconvenient to apply in a formulation. Also, due to the physicochemical properties of bentonite, the skin may be subjected to friction from tiny particles, reducing the user experience. Additionally, when bentonite is used alone in rinse-off products, it will be rinsed off during the rinse-off process, and the duration of contact with the skin surface and the exposure dose are insufficient to support its ability to continuously absorb oil and control oil. Summary of the Invention

[0004] In order to overcome the shortcomings and deficiencies of the prior art, the primary objective of this invention is to provide a method for preparing a bentonite composition with cleaning and oil-controlling effects.

[0005] Another object of the present invention is to provide a bentonite composition with cleaning and oil-controlling effects prepared by the above method.

[0006] Another object of the present invention is to provide the application of the above-mentioned bentonite composition with cleaning and oil-controlling effects.

[0007] The objective of this invention is achieved through the following solution:

[0008] A method for preparing the above-mentioned bentonite composition with cleaning and oil-controlling effects includes the following steps:

[0009] (1) Add bentonite to an organic solvent and disperse it evenly to obtain a bentonite organic dispersion;

[0010] (2) Add the bentonite organic dispersion to hot spring water and stir until the bentonite is dispersed in the hot spring water to obtain a mixed dispersion.

[0011] (3) Remove the organic solvent from the mixed dispersion to obtain bentonite hot spring water;

[0012] (4) Add hydrolyzed starch to polyol and stir well to obtain hydrolyzed starch alcohol solution;

[0013] (5) The hydrolyzed starch alcohol solution is added to the bentonite hot spring water, heated and stirred evenly to obtain a bentonite composition with cleaning and oil control effects.

[0014] Bentonite contains a large number of polar groups, and it is easy for bentonite to agglomerate when it is directly dispersed in water. Therefore, in steps (1)-(3) of this invention, bentonite is first dissolved in an organic solvent to make the bentonite dispersed evenly in the organic solvent, and then the bentonite organic dispersion is dissolved in hot spring water, so that the dispersed bentonite is not easy to agglomerate in the hot spring water.

[0015] In some embodiments, the bentonite in step (1) has a particle size range of 2-20 μm; the bentonite accounts for 4-12% of the mass of the bentonite composition having cleaning and oil-controlling effects.

[0016] In some embodiments, the organic solvent in step (1) is at least one of ethanol and acetone; the mass ratio of the amount of the organic solvent to the amount of bentonite is 2-10:1.

[0017] In some embodiments, the uniform dispersion in step (1) refers to ultrasonic dispersion followed by stirring, wherein the power of ultrasonic dispersion is 100-300w; the time of ultrasonic dispersion is 1-6h; the stirring speed is 30-300rpm; and the stirring time is 1-6h.

[0018] In some embodiments, the hot spring water in step (2) is 46-87% by mass of the bentonite composition having cleaning and oil-controlling effects;

[0019] In some embodiments, the stirring speed in step (2) is 30-300 rpm; the stirring time is 8-24 h;

[0020] In some embodiments, step (3) of removing the organic solvent from the mixed dispersion is a rotary evaporation process, specifically, the mixed dispersion is subjected to rotary evaporation to remove the organic solvent.

[0021] In some embodiments, the temperature of the rotary evaporation process in step (3) is 20-60°C, the rotation speed is 100-500 rpm, and the evaporation time is 1-4 h.

[0022] In some embodiments, the hydrolyzed starch in step (4) is at least one of hydrolyzed corn starch, hydrolyzed wheat starch, hydrolyzed potato starch, and hydrolyzed soybean starch; the hydrolyzed starch is 4-12% by mass of the bentonite composition having cleaning and oil-controlling effects.

[0023] In some embodiments, the polyol in step (4) is at least one of 1,3-propanediol, glycerol, pentanediol, ethylene glycol, dipropylene glycol, and diethylene glycol, and the polyol is 5-30% by mass of the bentonite composition having cleaning and oil-controlling effects.

[0024] In some embodiments, the stirring speed in step (4) is 30-300 rpm; the stirring time is 0.5-5 h.

[0025] In some embodiments, the hydrolyzed starch alcohol solution in step (5) is added at a rate of 0.5-5 mL / min.

[0026] In some embodiments, the heating and stirring temperature in step (5) is 50-90°C, the heating and stirring speed is 30-300 rpm, and the heating and stirring time is 2-10 h.

[0027] A bentonite composition with cleaning and oil-controlling effects prepared by the above method.

[0028] The above-mentioned bentonite composition with cleansing and oil-controlling effects is used in the field of cosmetics preparation, especially in the preparation of cosmetics with cleansing and oil-controlling effects.

[0029] The amount of the bentonite composition with cleansing and oil-controlling effects used in cosmetics is 0.1-30% by mass.

[0030] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0031] This invention utilizes hydrolyzed starch to interact with bentonite, improving the dispersibility of bentonite in aqueous solutions and mitigating its insolubility in water and tendency to settle in aqueous applications. The resulting bentonite composition exhibits excellent stability and possesses both cleaning and oil-controlling properties. Furthermore, through the synergistic interaction of bentonite, hydrolyzed starch, and minerals from hot spring water, the final bentonite composition demonstrates both superior cleaning power and sustained oil-controlling ability. Detailed Implementation

[0032] The present invention will be further described in detail below with reference to embodiments and accompanying drawings, but the embodiments of the present invention are not limited thereto. Unless otherwise specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments used, unless otherwise specified, are all commercially available conventional products.

[0033] Example 1

[0034] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 5 μm. 8 g of bentonite was added to 40 g of anhydrous ethanol and dispersed ultrasonically (200 W) for 3 h, followed by stirring at room temperature (200 rpm) for 3 h to obtain a bentonite-ethanol dispersion. This bentonite-ethanol solution was then added to 64 g of hot spring water and stirred at room temperature (200 rpm) for 12 h to ensure complete dispersion of the bentonite in the hot spring water, resulting in a mixed dispersion. The mixed dispersion was then treated in a 45°C water bath by rotary evaporation (350 rpm) for 2 h to remove all ethanol, yielding bentonite-infused hot spring water. 8 g of hydrolyzed corn starch was added to 20 g of 1,3-propanediol and stirred at room temperature (200 rpm) for 1 h to obtain a hydrolyzed corn starch-ethanol solution. The hydrolyzed corn starch alcohol solution was added dropwise to bentonite hot spring water at a rate of 2 mL / min. After the addition was complete, the mixture was stirred at 65°C (200 rpm) for 6 hours. Finally, it was cooled to 25°C to obtain a bentonite composition with cleaning and oil-controlling effects.

[0035] In Example 1, except for anhydrous ethanol (removed by rotary evaporation), the total mass of the remaining components, including bentonite, hot spring water, hydrolyzed corn starch and 1,3-propanediol, was 100g.

[0036] Example 2

[0037] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 2μm.

[0038] By replacing 8g of bentonite with a particle size of 5μm in Example 1 with 8g of bentonite with a particle size of 2μm, while keeping the rest unchanged, a bentonite composition with cleaning and oil-controlling effects is obtained.

[0039] Example 3

[0040] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 10 μm.

[0041] By replacing 8g of bentonite with a particle size of 5μm in Example 1 with 8g of bentonite with a particle size of 10μm, while keeping the rest unchanged, a bentonite composition with cleaning and oil-controlling effects was obtained.

[0042] Example 4

[0043] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 15 μm.

[0044] By replacing 8g of bentonite with a particle size of 5μm in Example 1 with 8g of bentonite with a particle size of 15μm, while keeping the rest unchanged, a bentonite composition with cleaning and oil-controlling effects is obtained.

[0045] Example 5

[0046] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 20 μm.

[0047] By replacing 8g of bentonite with a particle size of 5μm in Example 1 with 8g of bentonite with a particle size of 20μm, while keeping the rest unchanged, a bentonite composition with cleaning and oil-controlling effects is obtained.

[0048] Example 6

[0049] In Example 1, 8g of hydrolyzed corn starch was replaced with 8g of hydrolyzed wheat starch, while the rest remained unchanged, to obtain a bentonite composition with cleaning and oil-controlling effects.

[0050] Example 7

[0051] In Example 1, 8g of hydrolyzed corn starch was replaced with 8g of hydrolyzed potato starch, while the rest remained unchanged, to obtain a bentonite composition with cleaning and oil-controlling effects.

[0052] Example 8

[0053] In Example 1, 8g of hydrolyzed corn starch was replaced with 8g of hydrolyzed soybean starch, while the rest remained unchanged, to obtain a bentonite composition with cleaning and oil-controlling effects.

[0054] Example 9

[0055] In Example 1, 8g of bentonite with a particle size of 5μm was replaced with 4g of bentonite with a particle size of 5μm, and the mass of hot spring water was appropriately adjusted to 68g so that the total mass was 100g. The rest remained unchanged, and a bentonite composition with cleaning and oil-controlling effects was obtained.

[0056] Example 10

[0057] In Example 1, 8g of bentonite with a particle size of 5μm was replaced with 12g of bentonite with a particle size of 5μm, and the mass of hot spring water was appropriately adjusted to 60g so that the total mass was 100g. The rest remained unchanged, and a bentonite composition with cleaning and oil-controlling effects was obtained.

[0058] Example 11

[0059] In Example 1, the 8g hydrolyzed corn starch was replaced with 4g hydrolyzed corn starch, and the mass of the hot spring water was appropriately adjusted to 68g so that the total mass was 100g. The rest remained unchanged, and a bentonite composition with cleaning and oil-controlling effects was obtained.

[0060] Example 12

[0061] In Example 1, 8g of hydrolyzed corn starch was replaced with 12g of hydrolyzed corn starch, and the mass of hot spring water was appropriately adjusted to 60g so that the total mass was 100g. The rest remained unchanged, and a bentonite composition with cleaning and oil-controlling effects was obtained.

[0062] Example 13

[0063] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 15 μm. 8 g of bentonite was added to 50 g of acetone and dispersed ultrasonically (100 W) for 1 hour, followed by stirring at room temperature (300 rpm) for 1 hour to obtain a bentonite-acetone solution. This bentonite-acetone solution was then added to 68 g of hot spring water and stirred at room temperature (200 rpm) for 8 hours until the bentonite was fully dispersed in the hot spring water, obtaining a mixed dispersion. This mixed dispersion was then treated by rotary evaporation (100 rpm) at 40°C for 4 hours to remove all acetone, yielding bentonite-infused hot spring water. 12 g of hydrolyzed corn starch was added to 12 g of glycerol and stirred at room temperature (50 rpm) for 3 hours to obtain a hydrolyzed corn starch alcohol solution. The hydrolyzed corn starch alcohol solution was added dropwise to bentonite hot spring water at a rate of 0.5 mL / min. After the addition was complete, the mixture was stirred at 90°C (150 rpm) for 6 hours. Finally, it was cooled to 25°C to obtain a bentonite composition with cleaning and oil-controlling effects.

[0064] In Example 13, except for anhydrous acetone (removed by rotary evaporation), the total mass of the remaining components, including bentonite, hot spring water, hydrolyzed corn starch, and glycerol, was 100g.

[0065] Comparative Example 1

[0066] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 5 μm. 8 g of bentonite was added to 40 g of anhydrous ethanol and dispersed by ultrasonication (200 W) for 3 h, followed by stirring at room temperature (200 rpm) for 3 h to obtain a bentonite ethanol solution. This bentonite ethanol solution was added to 72 g of hot spring water and stirred at room temperature (200 rpm) for 12 h to ensure complete dispersion of the bentonite in the hot spring water, obtaining a mixed dispersion. This mixed dispersion was treated by rotary evaporation (350 rpm) at 45 °C for 2 h to remove all ethanol, obtaining bentonite hot spring water. 20 g of 1,3-propanediol was added dropwise to the bentonite hot spring water at a rate of 2 mL / min. After the addition was complete, the mixture was stirred at 65 °C (200 rpm) for 6 h, and finally cooled to 25 °C to obtain the final composition.

[0067] In Comparative Example 1, the total mass of the remaining components, excluding anhydrous ethanol (removed by rotary evaporation), including bentonite, hot spring water, and 1,3-propanediol, was 100g.

[0068] The difference between Comparative Example 1 and Example 1 is that hydrolyzed corn starch was not added in Comparative Example 1.

[0069] Comparative Example 2

[0070] 8 g of hydrolyzed corn starch was added to 20 g of 1,3-propanediol and stirred at room temperature (200 rpm) for 1 h to obtain a hydrolyzed corn starch alcohol solution. The hydrolyzed corn starch alcohol solution was added dropwise to 72 g of hot spring water at a dropping rate of 2 mL / min. After the addition was complete, the mixture was stirred at 65 °C (200 rpm) for 6 h, and finally cooled to 25 °C to obtain the composition.

[0071] The difference between Comparative Example 2 and Example 1 is that no bentonite was added in Comparative Example 2.

[0072] Comparative Example 3

[0073] The 8g hydrolyzed corn starch in Example 1 was replaced with 8g corn starch, while the rest remained unchanged, to obtain the composition.

[0074] The difference between Comparative Example 3 and Example 1 is that Comparative Example 3 uses unhydrolyzed corn starch instead of hydrolyzed corn starch to obtain a composition.

[0075] Comparative Example 4

[0076] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 5 μm. 8 g of bentonite was added to 64 g of hot spring water and stirred at room temperature (200 rpm) for 12 hours to ensure complete dispersion of the bentonite in the hot spring water, thus obtaining bentonite hot spring water. 8 g of hydrolyzed corn starch and 20 g of 1,3-propanediol were added to the bentonite hot spring water, and stirring was maintained at 200 rpm for 6 hours. Finally, the mixture was cooled to 25°C to obtain the final composition.

[0077] The difference between Comparative Example 4 and Example 1 is that in Comparative Example 4, bentonite and hydrolyzed corn starch were directly added to hot spring water to obtain the composition.

[0078] Comparative Example 5

[0079] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 1 μm.

[0080] The composition was obtained by replacing 8g of bentonite with a particle size of 5μm in Example 1 with 8g of bentonite with a particle size of 1μm, while keeping the rest unchanged.

[0081] Comparative Example 6

[0082] Natural bentonite was pulverized and ground using a ball mill to obtain bentonite with a particle size of 25 μm.

[0083] The composition was obtained by replacing 8g of bentonite with a particle size of 5μm in Example 1 with 8g of bentonite with a particle size of 25μm, while keeping the rest unchanged.

[0084] Comparative Example 7

[0085] The 8g of bentonite with a particle size of 5μm in Example 1 was replaced with 15g of bentonite with a particle size of 5μm, and the mass of hot spring water was appropriately adjusted to 57g so that the total mass was 100g. The rest remained unchanged to obtain the composition.

[0086] Comparative Example 8

[0087] Zinc oxide was pulverized and ground using a ball mill to obtain zinc oxide with a particle size of 5 μm.

[0088] In Example 1, 8g of bentonite with a particle size of 5μm was replaced with 8g of zinc oxide with a particle size of 5μm, while keeping the rest unchanged, to obtain the composition.

[0089] Comparative Example 9

[0090] The composition was prepared by replacing 64g of hot spring water with 64g of deionized water in Example 1, while keeping the rest unchanged.

[0091] The difference between Comparative Example 9 and Example 1 is that Comparative Example 9 uses deionized water instead of hot spring water to obtain the composition.

[0092] Test Example 1: Storage Stability Test

[0093] After the samples of Examples 1-13 and Comparative Examples 1-8 were left to stand at 4°C, room temperature, and 45°C for one month, two months, and three months, respectively, the appearance of the samples was observed and the storage stability of the samples was tested.

[0094] Table 1. Storage stability test results of samples from Examples 1-13 and Comparative Examples 1-8

[0095]

[0096]

[0097]

[0098] Comparing Examples 1-5, Comparative Example 5, and Comparative Example 6, it is evident that different particle sizes of bentonite in the compositions result in varying storage stability of the final bentonite compositions with cleaning and oil-controlling effects. When the bentonite particle size is too small (Comparative Example 5), the electrostatic forces between bentonite molecules are greater, making them prone to aggregation. As the bentonite particle size increases, the product stability initially increases and then decreases. When the bentonite particle size is 5 μm, the product exhibits the best stability; during a three-month stability study, the product remained clear under three different conditions (4°C, room temperature, and 45°C) without any solid precipitate. When the bentonite particle size is 25 μm (Comparative Example 6), the product remained a turbid liquid with precipitate during the three-month stability study, indicating poor stability. Therefore, the bentonite particle size selected in this invention is 2-20 μm, with a preferred particle size of 5 μm (Example 1).

[0099] Comparing Examples 1 and 6-8, it is evident that different types of hydrolyzed starch in the compositions result in variations in their molecular structures, leading to differences in the interactions between the hydrolyzed starch and bentonite and hot spring water. Consequently, the storage stability of the resulting bentonite compositions with cleaning and oil-controlling effects varies. In Examples 1, 6, 7, and 8, the hydrolyzed starches in the compositions were hydrolyzed corn starch, hydrolyzed wheat starch, hydrolyzed potato starch, and hydrolyzed soybean starch, respectively. The results showed that the product of Example 1 exhibited the highest stability. During a three-month stability study, the product maintained a clear appearance under three different conditions (4°C, room temperature, and 45°C) without any solid precipitation. Therefore, in this invention, hydrolyzed corn starch was selected, resulting in the bentonite composition with the best stability exhibiting cleaning and oil-controlling effects.

[0100] Comparing Examples 1, 9, 10, and Comparative Example 7, it is evident that the amount of bentonite added affects the stability of the final product. As the amount of bentonite added increases, the product stability first increases and then decreases. When the amount of bentonite added is 8%, the product exhibits the best stability; during a three-month stability study, the product remained clear under three different conditions (4°C, room temperature, and 45°C) without any solid precipitate. When the amount of bentonite added is 15% (Comparative Example 7), the product remained a turbid liquid with precipitate during the three-month stability study, indicating poor stability. Therefore, the bentonite addition amount selected in this application is 4-12%, with a preferred addition amount of 8% (Example 1).

[0101] Comparing Examples 1, 11, and 12, it is evident that the amount of hydrolyzed starch added affects the stability of the final product. As the amount of hydrolyzed starch added increases, the product stability first increases and then decreases. When the amount of hydrolyzed starch added is 8% (Example 1), the product exhibits the best stability. During a three-month stability study, the product maintained a clear appearance under three different conditions (4°C, room temperature, and 45°C) without any solid precipitate.

[0102] Comparing Example 1 and Comparative Example 4, it can be seen that in Example 1 of the present invention, the bentonite composition with cleaning and oil-controlling effects prepared by the above process is the most stable. Under the three-month stability test, the product showed a clear appearance under three different conditions (4°C, room temperature, 45°C) and no solid precipitate was formed. In contrast, Comparative Example 4 directly mixed various raw materials, and the resulting composition had poor stability.

[0103] Comparing Example 1 and Comparative Example 1, it can be seen that, compared with the composition that only adds bentonite, the bentonite composition with cleaning and oil-controlling effects prepared by the interaction of bentonite and hydrolyzed starch in Example 1 of the present invention has better stability.

[0104] Comparing Examples 1, 6-8 and Comparative Example 3, it can be seen that, compared with unhydrolyzed corn starch, the bentonite composition prepared by hydrolyzed corn starch in Example 1 of this invention has better stability. After hydrolysis, the starch is hydrolyzed from macromolecules into small molecules, which greatly improves its solubility and allows it to interact better with bentonite.

[0105] Comparing Example 1 and Comparative Example 8, it can be seen that, compared with zinc oxide (Comparative Example 8), the bentonite in the present invention exhibits stronger interaction with hydrolyzed starch and hot spring water, resulting in a bentonite composition with better stability that has cleaning and oil-controlling effects.

[0106] Application Example 1

[0107] The facial cleanser with cleansing and oil-controlling effects provided in Application Example 1 was prepared according to the formula in Table 2.

[0108] Preparation method: Xanthan gum and sodium hyaluronate were pre-dispersed in glycerin, then added to deionized water, heated to 80°C, stirred until dissolved and uniformly transparent, and cooled to 55°C; p-hydroxyacetophenone was added to 1,3-propanediol and heated until dissolved and transparent, then added to the system and stirred evenly; cooled to 45°C, the composition of Example 1 was added to the system and stirred evenly to obtain the facial cleanser of Application Example 1.

[0109] Table 2 Application Example 1 Cleanser Formulation Table

[0110]

[0111] Application Example 2-13

[0112] The bentonite composition of Example 1 with cleaning and oil-controlling effects, which was 5% by mass in Application Example 1, was replaced with the composition of Example 2-14, which was 5% by mass, while the other components and preparation methods remained unchanged, and Application Examples 2-13 were prepared respectively.

[0113] Application Comparative Examples 1-9

[0114] The bentonite composition of Example 1 with cleaning and oil-controlling effects, which was 5% by mass in Application Example 1, was replaced with the composition of Comparative Examples 1-9, which was 5% by mass, while the other components and preparation methods remained unchanged, and Application Comparative Examples 1-9 were prepared respectively.

[0115] Blank facial cleansing base

[0116] The bentonite composition with cleaning and oil-controlling effects of Example 1, which was 5% by mass in Application Example 1, was replaced with 5% by mass of deionized water, while the other components and preparation method remained unchanged, to obtain a blank facial cleansing matrix.

[0117] Test Example 2—Cleansing Ability Test:

[0118] The samples used in this cleansing ability test were Application Examples 1-13, Comparative Examples 1-9, and a blank cleansing matrix. The testing method employed a human efficacy evaluation experiment, and the detection index was skin oil content. The test subjects were 345 healthy men or women aged 18-50 with non-sensitive skin, in a 1:1 male-to-female ratio. The test sites had no obvious damage, had not recently undergone any drug or cosmetic treatments, and had not recently taken any hormonal medications. The participants were randomly divided into 23 groups of 15 people each. The testing environment was 20-22℃ and 40%-60% RH.

[0119] Experimental steps:

[0120] (1) No products (cosmetics or topical medications) should be used on the test site for 3 days prior to the test, and the site should not come into contact with water within 3 hours. Before the test, the subject needs to clean the inside of both forearms uniformly. The cleaning method is to wipe the outside of the arm with a damp cotton towel. The forearm is exposed and placed in the test position, and the subject sits quietly in a constant temperature and humidity room for 30 minutes.

[0121] (2) The test area is marked on the inner side of the subject's forearms using a laboratory marking mold. The test area is 3cm × 3cm. Care should be taken to avoid the upper arm and wrist, and the middle test area should be selected. One area is marked on each arm, and the left and right hands are respectively designated as the sample processing area and the negative control area.

[0122] (3) Before artificial sebum modeling: The skin sebum content in the sample treatment area and the negative control area was measured respectively, and the data were recorded as T. BS .

[0123] (4) Artificial sebum modeling: Weigh 0.02g of artificial sebum, apply it evenly to the detection area, and wait 15 minutes for film formation.

[0124] (5) After artificial sebum modeling: Measure the skin sebum content in the detection area. Record the data as T. MS .

[0125] (6) Sample application: Weigh 0.01g of sample, apply it evenly to the sample treatment area after modeling, massage for 30s, then gently wipe off the sample with a damp cotton cloth and wait for 30min. At the same time, weigh an equal mass of blank cleansing matrix and treat the negative control area in the same way.

[0126] (7) After using the sample: Measure the skin oil content in the sample treatment area and the negative control area respectively, and record the data as T. S .

[0127] (8) Significance analysis: The skin oil content after sample processing and after artificial sebum modeling was tested by SPSS 24.0, α=0.05.

[0128] Among them, the skin oil content T after artificial sebum modeling MS Skin oil content T in the sample treatment area S The difference T MS -T S The larger the value, the better the cleaning ability of the sample.

[0129] Table 3. Cleaning ability test results of samples from Application Examples 1-13 and Comparative Examples 1-9

[0130]

[0131]

[0132] Comparing Application Examples 1-5, Comparative Example 5, and Comparative Example 6, it can be seen that different particle sizes of bentonite in the composition result in different oil-washing abilities in the final bentonite compositions with cleaning and oil-controlling effects. As the bentonite particle size increases, the oil-washing ability of the product first increases and then decreases. When the bentonite particle size is 5 μm, the product exhibits the best oil-washing ability, showing a highly significant difference compared to the model using artificial sebum (P<0.001). However, when the bentonite particle sizes are 1 μm and 25 μm, there is no significant difference in skin oil content before and after product use (P>0.05), indicating no oil-washing ability. Therefore, the bentonite particle size selected in this application is 2-20 μm, with a preferred particle size of 5 μm (Example 1).

[0133] Comparing Application Examples 1 and 6-8, it is evident that different types of hydrolyzed starch in the compositions result in varying grease-washing abilities in the final bentonite compositions with cleaning and oil-controlling properties. In Application Examples 1, 6, 7, and 8, the hydrolyzed starches in the compositions were hydrolyzed corn starch, hydrolyzed wheat starch, hydrolyzed potato starch, and hydrolyzed soybean starch, respectively. The results show that the product of Application Example 1 exhibits the best grease-washing ability (P<0.001). Therefore, in this invention, hydrolyzed corn starch is selected as the hydrolyzed starch, resulting in the bentonite composition with the best grease-washing ability (Example 1).

[0134] Comparing Application Examples 1, 9, and 10 with Comparative Example 7, it can be seen that the amount of bentonite added affects the grease-washing ability of the final product. As the amount of bentonite added increases, the grease-washing ability of the product first increases and then decreases. The grease-washing ability is best when the amount of bentonite added is 8% (P<0.001). When the amount of bentonite added is 15%, the excessive addition affects the interaction between bentonite, hydrolyzed starch, and hot spring water, greatly weakening the synergistic effect of the three, and causing a sharp decline in grease-washing ability. Therefore, the bentonite added in this invention is selected to be 4-12%, with a preferred addition amount of 8% (Example 1).

[0135] Comparing Application Example 1, Comparative Example 11, and Application Example 12, it can be seen that the amount of hydrolyzed starch added affects the interaction between bentonite, hydrolyzed starch, and hot spring water in the composition, ultimately affecting the grease-washing ability of the final product. As the amount of hydrolyzed starch added increases, the grease-washing ability of the product first increases and then decreases. When the amount of hydrolyzed starch added is 8% (Application Example 1), the grease-washing ability of the product is the best (P<0.001).

[0136] Comparing Application Example 1 and Application Comparative Example 4, it can be seen that the preparation of the bentonite composition affects the grease-washing effect of the final product. In Application Example 1 of the present invention, the bentonite was first pre-dispersed with ethanol, then added to hot spring water for further dispersion, and finally hydrolyzed starch alcohol solution was added. The composition with cleaning and oil-controlling effects prepared by the above process has the best grease-washing ability (P<0.001).

[0137] Comparing Application Example 1, Application Comparative Example 1, Application Comparative Example 2, and Application Comparative Example 9, it can be seen that compared to compositions that only add bentonite and hot spring water (Application Comparative Example 1), or only add hydrolyzed starch and hot spring water (Application Comparative Example 2, which has almost no oil-washing ability), or use deionized water instead of hot spring water (Application Comparative Example 9), the composition prepared in Application Example 1 of this invention, which uses bentonite, hydrolyzed starch, and hot spring water, interacts with each other, and the resulting composition with cleaning and oil-controlling effects has better oil-washing ability.

[0138] Comparing Application Example 1 and Application Comparative Example 3, it can be seen that, compared with unhydrolyzed corn starch, the hydrolyzed corn starch used in Application Example 1 of the present invention has a stronger interaction with bentonite, and the final composition with cleaning and oil-controlling effects has better oil-washing ability.

[0139] Comparing Application Example 1 and Application Comparative Example 8, it can be seen that, compared with zinc oxide (Application Comparative Example 8), the composition with cleaning and oil-controlling effects prepared by the interaction of bentonite, hydrolyzed starch, and hot spring water in Application Example 1 of this invention has better oil-washing ability.

[0140] Test Example 3—Long-lasting Oil Control Test

[0141] The oil-control test samples included Application Examples 1-13, Comparative Examples 1-9, and a blank cleansing base. The testing method employed a human efficacy evaluation experiment, and the detection index was skin sebum content. The test subjects were 360 ​​healthy individuals aged 18-45 years with oily facial skin and a forehead sebum content of not less than 150 μg / cm³. 2 The participants were male or female, with a 1:1 male-to-female ratio, without obvious injuries, recent drug or cosmetic treatments, and recent use of hormonal drugs. They were randomly divided into 23 groups of 15 people each. The testing environment was 20-22℃ and 40%-60% RH.

[0142] Experimental steps:

[0143] (1) The experimenters used the facial cleanser sample on their own. The method of use was to take 0.2g of the test sample, rub it in their hands to create foam, cleanse their face, gently massage for about 30 seconds, and then rinse with water. The experimenters used the facial cleanser sample 1-2 times a day according to their personal habits.

[0144] (3) Before using the test sample, and after using the sample for 1 week, 2 weeks and 4 weeks, the skin oil content of the experimental personnel on the forehead was tested.

[0145] Table 4 shows the long-lasting oil control test results of application examples 1-13, comparative examples 1-9, and blank cleansing bases.

[0146]

[0147]

[0148] The results show that the facial cleanser prepared with the bentonite composition of the present invention has a sustained oil-controlling effect.

[0149] Comparing Application Examples 1-5, Comparative Example 5, and Comparative Example 6, it can be seen that different particle sizes of bentonite in the composition result in different oil-controlling effects in the final bentonite compositions with cleaning and oil-controlling properties. As the bentonite particle size increases, the oil-controlling ability of the product first increases and then decreases. The product exhibits the best oil control when the bentonite particle size is 5 μm. However, the oil-controlling effect is poor when the bentonite particle sizes are 1 μm and 25 μm, respectively. Therefore, the bentonite particle size selected in this application is 2-20 μm, with a preferred particle size of 5 μm (Example 1).

[0150] Comparing Application Examples 1 and 6-8, it is evident that different types of hydrolyzed starch in the compositions result in varying oil-controlling effects in the final bentonite compositions with cleaning and oil-controlling properties. In Application Examples 1, 6, 7, and 8, the hydrolyzed starches in the compositions were hydrolyzed corn starch, hydrolyzed wheat starch, hydrolyzed potato starch, and hydrolyzed soybean starch, respectively. The results indicate that the product in Application Example 1 exhibits the best oil control. Therefore, in this invention, hydrolyzed corn starch is selected as the hydrolyzed starch, resulting in the bentonite composition with the best oil control properties (Example 1).

[0151] Comparing Application Examples 1, 9, and 10 with Comparative Example 7, it can be seen that the amount of bentonite added in the composition affects the oil control effect of the final product. As the amount of bentonite added increases, the oil control effect of the product first increases and then decreases. The oil control effect is best when the amount of bentonite added is 8%. The oil control effect is poor when the amount of bentonite added is 15% (Comparative Example 7). Therefore, the amount of bentonite added selected in this invention is 4-12%, with a preferred amount of 8% (Example 1).

[0152] Comparing Application Example 1, Comparative Example 11, and Application Example 12, it can be seen that the amount of hydrolyzed starch added to the composition affects the oil control effect of the final product. As the amount of hydrolyzed starch added increases, the oil control effect of the product first increases and then decreases. The oil control effect is best when the amount of hydrolyzed starch added is 8% (Application Example 1).

[0153] Comparing Application Example 1 and Application Comparative Example 4, it can be seen that in Application Example 1 of this application, the composition with cleaning and oil-controlling effects prepared by the above process, which is first pre-dispersed with ethanol, then added to hot spring water for further dispersion, and finally added with hydrolyzed starch alcohol solution, has the best oil control.

[0154] Comparing Application Example 1, Application Comparative Example 1, and Application Comparative Example 2, it can be seen that compared to compositions that only add bentonite (Application Comparative Example 1) or only add hydrolyzed starch (Application Comparative Example 2), the composition with cleaning and oil-controlling effects obtained by the interaction of bentonite and hydrolyzed starch in Application Example 1 of this application has better oil control.

[0155] Comparing Application Example 1 and Application Comparative Example 3, it can be seen that, compared with unhydrolyzed corn starch, the interaction between hydrolyzed corn starch treated with hydrolysis and bentonite in Application Example 1 of this application results in a bentonite composition with cleaning and oil-controlling effects that has better oil control.

[0156] Comparing Application Example 1 and Application Comparative Example 8, it can be seen that, compared to zinc oxide (Application Comparative Example 8), the bentonite composition with cleaning and oil-controlling effects prepared in Application Example 1 of this invention, which uses the interaction of bentonite and hydrolyzed starch, has better oil-controlling properties. In contrast, the use of zinc oxide weakens the oil-controlling effect of the composition, resulting in a worse oil-controlling effect.

[0157] Comparing Application Example 1, Application Comparative Example 1, Application Comparative Example 2, and Application Comparative Example 9, it can be seen that compared to compositions that only add bentonite and hot spring water (Application Comparative Example 1), or only add hydrolyzed starch and hot spring water (Application Comparative Example 2, which has almost no oil-washing ability), or use deionized water instead of hot spring water (Application Comparative Example 9), the composition prepared in Application Example 1 of this invention, which uses bentonite, hydrolyzed starch, and hot spring water, interacts with each other, and the resulting composition with a clean oil-controlling effect has better oil control.

[0158] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A method for preparing a bentonite composition with cleaning and oil-controlling effects, characterized in that... Includes the following steps: (1) Add bentonite to an organic solvent and disperse evenly to obtain a bentonite organic dispersion; (2) Add the bentonite organic dispersion to hot spring water and stir until the bentonite is dispersed in the hot spring water to obtain a mixed dispersion; (3) Remove the organic solvent from the mixed dispersion to obtain bentonite hot spring water; (4) Add hydrolyzed starch to a polyol and stir evenly to obtain a hydrolyzed starch alcohol solution; (5) Add the hydrolyzed starch alcohol solution to the bentonite hot spring water, heat and stir evenly to obtain a bentonite composition with cleaning and oil-controlling effects; The organic solvent in step (1) is at least one of ethanol and acetone; The hydrolyzed starch in step (4) is hydrolyzed corn starch, hydrolyzed wheat starch, hydrolyzed maize starch, etc. At least one of potato starch and hydrolyzed soybean starch; the bentonite in step (1) is 4-12% by mass of the bentonite composition with cleaning and oil-controlling effects; the hot spring water in step (2) is 46-87% by mass of the bentonite composition with cleaning and oil-controlling effects; the hydrolyzed starch in step (4) is 4-12% by mass of the bentonite composition with cleaning and oil-controlling effects; the polyol in step (4) is 5-30% by mass of the bentonite composition with cleaning and oil-controlling effects; the particle size range of the bentonite in step (1) is 2-20 μm; the mass ratio of the amount of organic solvent to the amount of bentonite in step (1) is 2-10:

1.

2. The method for preparing the bentonite composition with cleaning and oil-controlling effects according to claim 1, characterized in that: The polyol mentioned in step (4) is at least one of 1,3-propanediol, glycerol, pentanediol, ethylene glycol, dipropylene glycol, and diethylene glycol.

3. The method for preparing the bentonite composition with cleaning and oil-controlling effects according to claim 1, characterized in that: The uniform dispersion mentioned in step (1) refers to ultrasonic dispersion followed by stirring, wherein the power of ultrasonic dispersion is 100-300w and the time of ultrasonic dispersion is 1-6h; the stirring speed is 30-300 rpm and the stirring time is 1-6h.

4. The method for preparing the bentonite composition with cleaning and oil-controlling effects according to claim 1, characterized in that: The heating and stirring temperature in step (5) is 50-90℃, and the stirring time is 2-10h.

5. A bentonite composition with cleaning and oil-controlling effects prepared by the method according to any one of claims 1-4.

6. The application of the bentonite composition with cleansing and oil-controlling effects according to claim 5 in the preparation of cosmetics.

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