Oil beads containing amodimethicone and a method for preparing and using the same

Abstract

The application discloses an oil bead containing an amino-terminated polydimethylsiloxane and a preparation method and application thereof. The preparation method of the oil bead is that 1-10 parts of an oil phase is uniformly dispersed in 90-99 parts of an aqueous phase, and an oil bead essence is obtained through filtration, wherein the oil phase is composed of an amino-terminated polydimethylsiloxane, a castor oil / IPDI copolymer, caprylic triglyceride / capric triglyceride, ganoderma lucidum spore oil and vegetable fat. The amino-terminated polydimethylsiloxane and the castor oil / IPDI copolymer have excellent film-forming property, so that the oil phase can be stably suspended in the aqueous phase in the form of oil beads with uniform size, and a special design is not needed for a pump head in use. The oil bead prepared by using the preparation method of the oil bead is easy to apply, meanwhile, the oil-soluble active ingredients in the oil phase can be guaranteed to be fresh and active, and can be applied to the preparation of various cosmetics.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of chemical industry, and particularly relates to an oil bead containing an amino-terminated polydimethylsiloxane and a preparation method and application thereof. BACKGROUND

[0002] With the diversification of consumer demand, oil bead essence with high color value has been favored by consumers. Oil bead belongs to the wrapping technology of visual oil beads. At present, the visual particles in cosmetics on the market mainly have two types. The first type is a natural source colloid polymer such as gelatin, gum arabica, agar, calcium alginate and cellulose as a particle main body, only provides visual effect for the product, has no actual effect and is not easy to be evenly applied. The second type is a natural source colloid polymer such as gelatin, gum arabica, agar, calcium alginate and cellulose as a particle shell, can wrap emollients, active ingredients and the like, but the product must be extruded through a specially designed screen pump head when used, otherwise it is not easy to be evenly applied, the absorption and penetration of active ingredients are affected, and the stability of the oil bead is poor.

[0003] The application aims to provide an oil bead with uniform particle size and stability and a preparation method thereof. SUMMARY

[0004] The first object of the application is to provide an oil bead containing an amino-terminated polydimethylsiloxane and a preparation method thereof, and the second object of the application is to provide the application of the oil bead.

[0005] The first object of the application is achieved by an oil bead containing an amino-terminated polydimethylsiloxane, and a preparation method thereof is that 1-10 parts of an oil phase are uniformly dispersed in 90-99 parts of an aqueous phase, and an oil bead essence is obtained by filtration, wherein the oil phase is composed of an amino-terminated polydimethylsiloxane, a castor oil / IPDI copolymer, a ganoderma spore oil and a vegetable oil.

[0006] The mass percentage of each component of the oil phase is as follows: the amino-terminated polydimethylsiloxane is 0.0001-5%, the castor oil / IPDI copolymer is 0.0001-4%, the caprylic acid / capric acid triglyceride is 0.0001-1%, the ganoderma spore oil is 0.0001-20%, and the balance is the vegetable oil.

[0007] The aqueous phase is composed of the following components with the mass percentage: glycerol 1-3%, 1,3-propanediol 3-5%, carbomer 0.1-0.3%, xanthan gum 0.02-0.1%, sodium hyaluronate 0.01-0.1%, p-hydroxyacetophenone 0.1-0.6%, 1,2-hexanediol 0.2-0.7%, and the balance is deionized water.

[0008] The vegetable oil is oleyl caprylate / cupric acid ester.

[0009] The second object of the present application is achieved in that the oil beads are used in the preparation of cosmetics or skin care products.

[0010] The amino-terminated polydimethylsiloxane added in the oil phase of the present application is a compound with amino groups attached to polydimethylsiloxane, containing both hydrophilic groups and hydrophobic groups. In an aqueous system, the hydrophobic groups are arranged inwardly and the hydrophilic groups are arranged outwardly, which can make the ganoderma spore oil, coconut alcohol octanoate / oleate and other oils stably disperse in the aqueous phase, so that the oil phase is wrapped to form oil beads. The added castor oil / IPDI copolymer has excellent film-forming properties, which can make the oil beads be stably wrapped. Moreover, it is mild and non-irritating, and can be applied to various cosmetics.

[0011] The present application has the following beneficial effects: The present application can make the oil phase stably suspended in the aqueous phase in the form of oil beads with uniform size by using the excellent film-forming properties of the amino-terminated polydimethylsiloxane and the castor oil / IPDI copolymer, and the pump head does not need to be specially designed when used. The oil beads prepared by the oil bead preparation method of the present application are easy to apply, and at the same time, the activity of the oil-soluble active ingredients in the oil phase can be guaranteed, which can be applied to the preparation of various cosmetics. BRIEF DESCRIPTION OF DRAWINGS

[0012] Figure 1 Appearance of the oil beads prepared in Example 1;

[0013] Figure 2 Appearance of the oil beads prepared in Comparative Example 1;

[0014] Figure 3 Appearance of the oil beads prepared in Comparative Example 2;

[0015] Figure 4 Appearance of the oil beads prepared in Comparative Example 3;

[0016] Figure 5 Appearance of the oil beads prepared in Comparative Example 4;

[0017] Figure 6 Changes in skin moisture content before and after using the micro-bead essence of Comparative Example 1, 1 hour after use and 2 hours after use;

[0018] Figure 7 Changes in skin moisture content before and after using the micro-bead essence of Example 1, 1 hour after use and 2 hours after use. DETAILED DESCRIPTION

[0019] The technical solutions in the embodiments of the present application will be clearly and completely described below. Apparently, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all the other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the present application. If the specific conditions are not indicated in the embodiments, the conventional conditions or the conditions suggested by the manufacturers are adopted. If the manufacturers of the reagents or instruments are not indicated, the conventional products that can be purchased in the market are adopted.

[0020] The preparation method of the oil bead containing the amino-terminated polydimethylsiloxane in the present application is that 1-10 parts of an oil phase is uniformly dispersed in 90-99 parts of an aqueous phase, and an oil bead essence is obtained by filtration, wherein the oil phase is composed of amino-terminated polydimethylsiloxane, castor oil / IPDI copolymer, ganoderma spore oil and vegetable oil;

[0021] The mass percentage of each component of the oil phase is as follows: amino-terminated polydimethylsiloxane 0.0001-5%, castor oil / IPDI copolymer 0.0001-4%, caprylic acid / capric acid triglyceride 0.0001-1%, ganoderma spore oil 0.0001-20%, and the balance is vegetable oil.

[0022] The aqueous phase is composed of the following components with the mass percentage: glycerol 1-3%, 1,3-propanediol 3-5%, carbomer 0.1-0.3%, xanthan gum 0.02-0.1%, sodium hyaluronate 0.01-0.1%, p-hydroxyacetophenone 0.1-0.6%, 1,2-hexanediol 0.2-0.7%, and the balance is deionized water.

[0023] The molecular weight of the amino-terminated polydimethylsiloxane is 4000-12000 g / mol, and the amino-terminated polydimethylsiloxane TCN-620 provided by Guangzhou Tianci High-tech Materials Co., Ltd. is adopted in the present application.

[0024] The castor oil / IPDI copolymer provided by Dachanghuajia Chemical International Trade Co., Ltd. is adopted in the present application, and the trade name is Estogel M.

[0025] The specific preparation method of the oil bead is as follows:

[0026] 1) Each component of the oil phase is stirred and heated in an oil phase pot to 85-95℃ until each component is completely dissolved, and then naturally cooled to 75-80℃ for preservation to obtain the oil phase;

[0027] 2) Each component of the aqueous phase is stirred and heated in an emulsifying pot to 80-85℃ until the material is completely dissolved, and then naturally cooled to below 45℃ to obtain the aqueous phase;

[0028] 3) The water phase obtained in step 2 is stirred at a speed of 60-80 r / min by using a pneumatic lifting stirrer with a I-shaped paddle, and the oil phase obtained in step 1 is quickly added, and the stirring is continued for 10-15 min, then the stirring is maintained and the temperature is quickly reduced to below 40℃ (the oil phase is condensed by temperature shock, and is sheared into uniform oil beads by stirring), and a sample is taken for detection, and the product is filtered by using a 150-mesh filter cloth after it is qualified (the oil beads are uniformly distributed in the system, and the particle size of the oil beads is between 0.5-2 mm) to obtain oil beads containing the amino-terminated polydimethylsiloxane. The oil beads are solid oil beads, and the particle size of the oil beads is 0.5-2 mm. The particle size of the oil beads is related to the stirring speed, the stirring speed is high, the particle size is small, and even the oil beads are not formed and are directly integrated with the water phase; the stirring speed is low, and the particle size of the oil beads is large. The particle size of the oil beads is controlled to be between 0.5-2 mm, the product is beautiful, the oil beads are easy to rub and break when used, and the oil beads are easy to apply.

[0029] In the step 1, the stirring speed is 500-800 r / min.

[0030] In the step 2, the viscosity of the prepared water phase is 900-1800 mPa·s, which is measured by using a digital viscometer No. 2 rotor at a speed of 12 r / min under the condition that the temperature is 25℃ and the viscosity is 101.3 kPa.

[0031] The application also provides oil beads based on the preparation method, and the application further provides a skin care product or a cosmetic product containing the oil beads.

[0032] The amino-terminated polydimethylsiloxane is 0.0001-5%, the castor oil / IPDI copolymer is 0.0001-4%, the caprylic acid / capric acid triglyceride is 0.0001-1%, the ganoderma lucidum spore oil is 0.0001%-20%, and the balance is vegetable oil.

[0033] The glycerol is 1-3%, the 1,3 propanediol is 3-5%, the carbomer is 0.1-0.3%, the xanthan gum is 0.02-0.1%, the sodium hyaluronate is 0.01-0.1%, the p-hydroxyacetophenone is 0.1-0.6%, the 1,2-hexanediol is 0.2-0.7%, and the balance is deionized water.

[0034] Preparation of oil bead essence

[0035] 1. Raw materials

[0036] The water phase: water 89.14 parts, glycerol 3 parts, 1,3 propanediol 5 parts, carbomer 0.1 part, xanthan gum 0.03 part, sodium hyaluronate 0.05 part, p-hydroxyacetophenone 0.2 part, and 1,2-hexanediol 0.4 part.

[0037] Oil phase: 0.03 parts of amodimethicone, 0.8 parts of castor oil / IPDI copolymer, 0.2 parts of caprylic / capric triglyceride, 0.05 parts of ganoderma spore oil, 1 part of cocoyl caprylate / caprate.

[0038] 2. Preparation process of oil beads

[0039] (1) The water, glycerol, 1,3-propanediol, carbomer, xanthan gum and sodium hyaluronate in the water phase raw materials were added to an emulsifying kettle, stirred at a speed of 12 r / min using a digital viscometer No. 2 rotor, and heated to 85°C (until completely dissolved) for 20 min, then hydroxyacetophenone and 1,2-hexanediol were added, and the stirring was continued to cool to below 45°C, to obtain a water phase with a viscosity of 1500 mpa·s, ready for use.

[0040] (2) The oil phase raw materials were added to the oil phase kettle, stirred and heated to complete dissolution for 10 min, then cooled to 80°C, and the oil phase was ready for use;

[0041] (3) When the two phases reached the specified temperature, the water phase was stirred at a speed of 60 r / min using a pneumatic lifting stirrer, and the high-temperature oil phase was quickly pumped into the water phase and continued to stir for 10-15 min, then the stirring was maintained and the temperature was quickly lowered to below 40°C, the material was discharged and allowed to stand, and sampling was performed for detection, and after passing, the material was filtered through a 150-mesh filter cloth to obtain oil bead essence with uniform size and a particle size of 0.5-2 mm.

[0042] Example 2

[0043] 1. Raw materials

[0044] Water phase: water 91.24 parts, glycerol 3 parts, 1,3-propanediol 3 parts, carbomer 0.3 parts, xanthan gum 0.1 parts, sodium hyaluronate 0.1 parts, p-hydroxyacetophenone 0.6 parts, 1,2-hexanediol 0.7 parts.

[0045] Oil phase: 0.03 parts of amodimethicone, 0.03 parts of castor oil / IPDI copolymer, 0.01 parts of caprylic / capric triglyceride, 0.1 parts of ganoderma spore oil, 0.84 parts of cocoyl caprylate / caprate.

[0046] 3. Preparation process of oil beads

[0047] (1) The water, glycerol, 1,3-propanediol, carbomer, xanthan gum and sodium hyaluronate in the water phase raw materials were added to an emulsifying kettle, stirred at a speed of 12 r / min using a digital viscometer No. 2 rotor, and heated to 85°C (until completely dissolved) for 20 min, then hydroxyacetophenone and 1,2-hexanediol were added, and the stirring was continued to cool to below 45°C, to obtain a water phase with a viscosity of 1500 mpa·s, ready for use.

[0048] (2) The oil phase raw materials are added to the oil phase pot, and after stirring and heating for 10 min until completely dissolved, the temperature is lowered to 75°C to obtain the oil phase for standby;

[0049] (3) When the two phases reach the specified temperature, the water phase is stirred at a stirring speed of 60 r / min using a pneumatic lifting stirrer, and the high-temperature oil phase is quickly pumped into the water phase. After continuing to stir for 10-15 min, the stirring is maintained and the temperature is quickly lowered to below 40°C. The product is discharged and left to stand. Sampling is performed for detection. After passing, the product is filtered through a 150-mesh filter cloth to obtain oil bead essence with uniform size and a particle size of 0.5-2 mm.

[0050] Example 3

[0051] 1. Raw materials

[0052] Water phase: water 84.47 parts, glycerol 1 part, 1,3 propanediol 4 parts, carbomer 0.2 parts, xanthan gum 0.02 parts, sodium hyaluronate 0.01 parts, p-hydroxyacetophenone 0.1 parts, 1,2-hexanediol 0.2 parts.

[0053] Oil phase: amodimethicone 0.5 parts, castor oil / IPDI copolymer 0.4 parts, caprylic / capric triglyceride 0.1 parts, ganoderma spore oil 2 parts, cocoyl caprylate / caprate 7 parts.

[0054] 3. Preparation process of oil beads

[0055] (1) The water, glycerol, 1,3 propanediol, carbomer, xanthan gum, and sodium hyaluronate in the water phase raw materials are added to the emulsifying pot and stirred at a speed of 2000 r / min to heat to 85°C (until completely dissolved) for 20 min. Then, the hydroxyacetophenone and 1,2-hexanediol are added, and the stirring is continued to cool to below 45°C. The water phase with a viscosity of 900 mpa·s is obtained and is ready for use.

[0056] (2) The oil phase raw materials are added to the oil phase pot, and after stirring and heating for 12 min until completely dissolved, the temperature is lowered to 75°C to obtain the oil phase for standby;

[0057] (3) When the two phases reach the specified temperature, the water phase is stirred at a stirring speed of 60 r / min using a pneumatic lifting stirrer, and the high-temperature oil phase is quickly pumped into the water phase. After continuing to stir for 10-15 min, the stirring is maintained and the temperature is quickly lowered to below 40°C. The product is discharged and left to stand. Sampling is performed for detection. After passing, the product is filtered through a 150-mesh filter cloth to obtain oil bead essence with uniform size and a particle size of 0.5-2 mm.

[0058] Comparative Example 1

[0059] The difference between Comparative Example 1 and Example 1 is that no amodimethicone and castor oil / IPDI copolymer are added to the oil phase. The rest is the same as Example 1. The obtained oil beads are as follows:Figure 2 As shown.

[0060] Comparative Example 2

[0061] Comparative Example 2 differs from Example 1 in that the amount of carbomer in the water phase is changed from 0.1% to 0.35%, i.e. the consistency of the water phase is increased, and the rest is the same as Example 1, and the obtained oil beads are as shown in Figure 3 As shown.

[0062] Comparative Example 3

[0063] Example 3 differs from Example 1 in that the amount of carbomer is changed from 0.1% to 0.08%, i.e. the consistency is reduced, and the rest is the same as Example 1, and the obtained oil beads are as shown in Figure 4 As shown.

[0064] Comparative Example 4

[0065] Comparative Example 4 differs from Example 1 in that the stirring speed in Step 3 is increased to 100 r / min, and the rest is the same as Example 1, and the obtained oil beads are as shown in Figure 5 As shown.

[0066] Comparative Example 5

[0067] Comparative Example 5 differs from Example 1 in that the stirring speed in Step 3 is reduced to 20 r / min, and the rest is the same as Example 1.

[0068] The appearance of the oil beads obtained in Example 1 and Comparative Examples 1-5 is shown in Table 1.

[0069] Table 1 Appearance of the oil bead essence obtained in Example 1 and Comparative Examples 1-5

[0070]

[0071] Test Example 1 Stability test of the oil bead essence obtained in Example 1

[0072] 1. Heat resistance 48℃ test, take the oil bead essence obtained in Example 1, respectively placed in a transparent bottle, placed at 48℃ for 1 month, 3 parallel samples for each, observe the stability of the formula. Record the results, see Table 2.

[0073] 2. Cold resistance-18℃ test, take the oil bead essence obtained in Example 1, respectively placed in a transparent bottle, placed at-18℃ for 1 month, 3 parallel samples for each, observe the stability of the formula. Record the results, see Table 2.

[0074] Table 2 Stability of the oil bead essence obtained in Example 1

[0075] Example 1 Resistant to heat 48°C storage Oil pearl essence with 1mm or so of oil beads evenly dispersed in the water phase, not floating, not sinking accumulation, appearance novel and unique Resistant to cold -15°C storage Oil pearl essence with 1mm or so of oil beads evenly dispersed in the water phase, not floating, not sinking accumulation, appearance novel and unique

[0076] Evaluation of the moisturizing effect of the oil bead essence prepared in Example 1

[0077] Experimental method: 5 test subjects aged 25-29 years with clean faces were randomly selected, rested for 15 min at a fixed position, and then the moisture content was tested after the face was dried and stabilized for 30 min in a closed place under conditions of no air flow, direct light, and constant temperature and humidity (room temperature of 20-25°C and humidity of 40-60%). The oil beads of Comparative Example 1 and Example 1 were applied to the faces of the test subjects. The moisture content was tested before application, after application, 30 min after application, and 1 h after application. The average value of the moisture content was taken to calculate the change rate of the moisture content.

[0078] Experimental results: From the above results, it can be seen that the moisture content of the face of the test subject to which the oil bead essence of Example 1 was applied was greater than that of the test subject to which the microbead essence of Comparative Example 1 was applied. This indicates that the oil bead essence prepared in Example 1 has a better moisturizing effect. Figures 6-7 ​

Claims

1. A method for preparing oil droplets containing aminopolydimethylsiloxane, characterized in that: The preparation method comprises the following steps: uniformly dispersing an oil phase in an aqueous phase, and filtering to obtain an oil droplet essence; according to a mass ratio, the raw materials of the oil phase and the aqueous phase total 100 parts, the aqueous phase raw materials comprise 3 parts of glycerin, 5 parts of 1,3-propylene glycol, 0.1 part of carbomer, 0.03 part of xanthan gum, 0.05 part of sodium hyaluronate, 0.2 part of p-hydroxyacetophenone, 0.4 part of 1,2-hexanediol, and 89.14 parts of water; and the oil phase raw materials comprise 0.03 part of amino-terminated polydimethylsiloxane, 0.8 part of castor oil / IPDI copolymer, 0.2 part of caprylic / capric triglyceride, 0.05 part of ganoderma lucidum spore oil, and 1 part of coconut oil caprylate / caprate; the specific preparation method of the oil droplets is as follows: 1) Stir and heat the oil phase components in an oil phase pot to 85-95°C until the components are completely dissolved, then cool naturally to 80°C and keep warm to obtain the oil phase; 2) Add water, glycerin, 1,3-propylene glycol, carbomer, xanthan gum, and sodium hyaluronate from the aqueous phase ingredients to an emulsifier, stir, heat to 85°C, and maintain for 20 minutes. Then, add p-hydroxyacetophenone and 1,2-hexanediol, continue stirring, and cool naturally to below 45°C to obtain an aqueous phase with a viscosity of 1500 mPa·s. 3) The aqueous phase obtained in step 2) was stirred at 60 r / min using a pneumatic lift mixer with an I-shaped propeller. The oil phase obtained in step 1) was rapidly added and stirred for 10-15 minutes. The mixture was then rapidly cooled to below 40°C while maintaining stirring. Samples were taken for testing. If the sample passed the test, it was filtered through a 150-mesh filter cloth to obtain uniformly sized oil droplets containing aminodimethylsiloxane with a particle size of 0.5-2 mm.

2. The preparation method according to claim 1, characterized in that In step 1), the stirring speed is 500-800 r / min.

3. An oil droplet obtained based on the preparation method according to claim 1.

4. A cosmetic comprising the oil droplets according to claim 3.

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