Small-particle-size positive charge conditioning emulsion as well as preparation and hair care application thereof

Abstract

The invention relates to the field of daily chemistry, and discloses a small-particle-size positive charge conditioning emulsion and preparation and hair care application thereof, and the small-particle-size positive charge conditioning emulsion comprises low-viscosity silicone oil, a nonionic emulsifier and a small-molecule cationic quaternary ammonium salt. A small-particle-size emulsion of low-viscosity silicone oil is prepared by utilizing a small-molecular cationic conditioner which is commonly used for hair washing and caring and has conditioning and emulsifying properties, even nano-scale silicone oil is prepared, and the low-viscosity silicone oil does not have the condition that the hair feels heavy after a high-viscosity silicone oil conditioner in the prior art is applied to specific people. The emulsion has small particle size and uniform deposition, and the surface positive charges of the emulsion improve the stability of the emulsion and also improve the deposition property of the low-viscosity silicone oil to a certain extent.

Description

Technical Field

[0001] The invention relates to the field of daily chemicals, and in particular to a small-particle positive charge conditioning milk and its preparation and hair care application. Background Art

[0002] The accumulated hair damage causes the hair surface to be uneven, dull, fly-away, and with increased friction when combing. The application of conditioning ingredients can improve the hair surface condition to a certain extent. Dimethylsiloxane is a common conditioning agent in hair care products. It is deposited evenly on the hair surface through the coagulation mechanism of the shampoo system to form a thin film to improve the hair surface condition. Shampoo often uses high molecular weight or high viscosity polydimethylsiloxane, such as silicone oil with a viscosity of hundreds of thousands, as a conditioning agent. However, for people who do not need intensive hair care, such as those with sparse and flat hair, men with short hair, and those who pursue fluffy hair, excessive deposition of silicone oil with too high viscosity or molecular weight may bring superior conditioning, but at the same time, the hair may feel heavy. Summary of the invention

[0003] The object of the present invention is to provide a new method for preparing a low-viscosity silicone oil small-particle emulsion using different small-molecule cationic quaternary ammonium salts, wherein the small-molecule cationic quaternary ammonium salts include but are not limited to hexadecyltrimethylammonium chloride, stearyltrimethylammonium chloride, behenyltrimethylammonium chloride, dipalmitoyloxyethyldimethylammonium chloride, behenyltrimethylammonium methylsulfate, and dioleoylethylhydroxyethylmethylammonium methylsulfate, and the viscosity of the silicone oil includes but is not limited to 5cst, 10cst, 50cst, 350cst, 1000cst, and 12500cst.

[0004] Characterize the surface charge Zeta potential, viscosity and consistency, particle size, stability, mildness, etc. of a series of small particle size positively charged conditioning lotions. It can be used in hair care products.

[0005] Positively charged emulsions are used in shampoo, and the condensate is evenly deposited on the hair during the washing process, which improves both conditioning and hair volume, achieving a balance between light conditioning and volume, leaving the hair refreshed and free of burden. It is speculated that the positive charge on the surface of the emulsion may play a role in assisting deposition, helping to improve the uniformity and amount of deposition of low-viscosity silicone oil.

[0006] In order to solve the above technical problems, the present invention adopts the following technical solutions: The invention discloses a small-particle positively charged conditioning emulsion, which is composed of low-viscosity silicone oil, non-ionic emulsifier, small-molecule cationic quaternary ammonium salt, deionized water and preservative.

[0007] Formulating silicone oils into conditioning emulsions with small particle sizes allows for easier formulation and generally more even deposition on the hair.

[0008] Preferably, in the small-particle positively charged conditioning lotion, the mass ratio of the low-viscosity silicone oil, the nonionic emulsifier, and the small-molecule cationic quaternary ammonium salt is 30-60:3-10:1-10.

[0009] After research, it was surprisingly found that when low-viscosity silicone oil, non-ionic emulsifier, and small-molecule cationic quaternary ammonium salt are combined in a specific ratio and formed into an emulsion with water and a trace amount of preservatives, a liquid like Figure 1 The composite emulsion droplet structure shown has suitable emulsion particle size, consistency and viscosity, is highly stable, can be left at room temperature for more than one month without any change, has no stratification or precipitation, is non-toxic and non-irritating, and can be well used in cleaning products.

[0010] Preferably, the particle size of the small-particle positively charged conditioning milk is comprised between 100 nm and 1 μm.

[0011] Preferably, the viscosity of the low-viscosity silicone oil ranges from 5 cst to 12500 cst.

[0012] Preferably, the nonionic emulsifier includes one or more of laureth-3, laureth-2, laureth-10, laureth-13, oleth-16, oleth-3, oleth-20, oleth-23, and oleth-25.

[0013] Small-particle silicone oil conditioning emulsion with positive charge on the surface was prepared using different low-viscosity silicone oils (5cst, 10cst, 50cst, 350cst, 1000cst, 12500cst), non-ionic emulsifiers (laureth-3, oleth-3, oleth-20), and different small-molecule cationic quaternary ammonium salts. The particle size ranged from 100nm to 1μm.

[0014] Preferably, the small molecule cationic quaternary ammonium salt includes one or more of cetyltrimethylammonium chloride, stearyltrimethylammonium chloride, behenyltrimethylammonium chloride, dipalmitoyloxyethyldimethylammonium chloride, behenyltrimethylammonium methylsulfate, and dioleoylethylhydroxyethylmethylammonium methylsulfate; the preservative includes one or more of phenoxyethanol and sodium benzoate.

[0015] Adding different small molecule cationic quaternary ammonium salts to the emulsion can make the emulsion positively charged, which can reduce the addition of small molecule cationic conditioning agents at the back end, and can also enhance the electrostatic repulsion between emulsion particles to improve the stability of the emulsion. The liquid with positive surface charge may interact with the negatively charged hair surface during the washing process to improve the deposition of low viscosity silicone oil, and to a certain extent solve the problem that low viscosity silicone oil is difficult to deposit on hair.

[0016] Preferably, in the small-particle positively charged conditioning milk, the mass fraction of the preservative comprises 0.5% to 3%; and the mass fraction of the deionized water comprises 30% to 65%.

[0017] A method for preparing the above-mentioned small-particle positively charged conditioning milk comprises: A, adding the nonionic emulsifier, the small molecule cationic quaternary ammonium salt, and the preservative into the deionized water, heating and stirring to obtain phase A; B. heating the low-viscosity silicone oil, adding it to the phase A, and homogenizing to obtain a pre-emulsion; C. Vigorously dispersing the pre-emulsion to obtain the small-particle positively charged conditioning emulsion.

[0018] Preferably, in step C, the violent dispersion includes one or more of ultrasonic microfluidic nanodispersion and high-pressure homogenization.

[0019] Preferably, in step A, the temperature of the heating and stirring is 80°C; in step B, the heating temperature is 80°C.

[0020] An application of the above-mentioned small-particle positively charged conditioning milk is used in hair care products.

[0021] Small particle size silicone oil conditioning lotion is used in shampoo, which can improve the combing performance of slightly damaged hair and make the hair fluffy without weighing the hair down. It is also suitable for other hair care products such as conditioners, hair masks, etc.

[0022] The implementation of the present invention has the following beneficial effects: 1. Use the commonly used small molecule cationic conditioning agent for hair care, which has both conditioning and emulsifying properties, to prepare low-viscosity silicone oil small particle size emulsion, even nanometer level. Low-viscosity silicone oil does not have the heavy feeling of hair after use by certain groups of people, as the high-viscosity silicone oil conditioning agent in the existing technical solution does. The emulsion has a small particle size and uniform deposition. The positive charge on the surface of the emulsion improves the stability of the emulsion and also improves the deposition of low-viscosity silicone oil to a certain extent.

[0023] 2. Use small molecule cationic conditioners commonly used in hair care to appropriately reduce the amount of conditioners added during the formula development process, which is suitable for the development of hair care product formulas that take both conditioning and fluffy into account.

[0024] 3. The emulsion is mild and non-irritating to eyes, suitable for the development of mild and non-irritating formulas.

[0025] 4. The prepared small-particle positively charged conditioning lotion has significant conditioning properties, improves the combing properties of dry and wet hair, and increases the volume of hair. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is a schematic diagram of the structure of the small-particle positively charged conditioning lotion of the present invention.

[0027] Figure 2 This is the particle size distribution diagram of Preparation Example 5, where the red, green and blue lines represent three parallel test results of one sample respectively.

[0028] Figure 3 This is the particle size distribution diagram of Preparation Example 6, where the red, green and blue lines represent three parallel test results of one sample respectively.

[0029] Figure 4 This is the particle size distribution diagram of Preparation Example 13.

[0030] Figure 5 This is the particle size distribution diagram of Preparation Example 15.

[0031] Figure 6 This is the particle size distribution diagram of Preparation Example 19, where the red, green and blue lines represent three parallel test results of one sample, respectively.

[0032] Figure 7 This is the particle size distribution diagram of Preparation Example 20, where the red, green and blue lines represent three parallel test results of one sample, respectively.

[0033] Figure 8 This is the mildness test diagram of Preparation Example 20.

[0034] Fig. 9 This is a test schematic diagram of Example 6.

[0035] Fig.10 This is a test result diagram of Example 6. DETAILED DESCRIPTION

[0036] In order to make the objectives, technical solutions and advantages of the present invention more clear, the present invention will be further described in detail below with reference to the accompanying drawings.

[0037] Example 1 Preparation process of positively charged small particle size silicone oil conditioning lotion: (1) Add nonionic emulsifier, small molecule cationic quaternary ammonium salt and preservative into deionized water, heat to about 80°C, and stir to dissolve / disperse uniformly to obtain phase A.

[0038] (2) Heat silicone oil to 80°C, add it to phase A, and homogenize to obtain a pre-emulsion.

[0039] (3) The pre-emulsion was prepared using an ultrasonic microfluidic nanodisperser (the equipment was jointly developed with the Guangdong Provincial Laboratory of Chemistry and Fine Chemicals) or a high-pressure homogenizer to obtain a small-particle positively charged silicone oil conditioning emulsion. The structural analysis of the prepared small-particle positively charged silicone oil conditioning emulsion was performed, and the results were as follows: Figure 1 shown.

[0040] Figure 1Si in the middle refers to low-viscosity silicone oil, the orange line refers to silicone oil molecules, and N+ molecules (black and green) refer to small molecule cationic quaternary ammonium salts. Refers to the nonionic emulsifier in the present invention. It can be seen that the prepared small-particle positively charged silicone oil conditioning lotion presents a small nano droplet structure with low-viscosity silicone oil as the center, silicone oil molecules are evenly wrapped, composite small molecule cationic quaternary ammonium salt forms an outer positive charge, and finally connected to the nonionic emulsifier lipophilic segment.

[0041] Example 2 Preparation Examples (the scope of protection is not limited to the Preparation Examples) By adjusting the formula, 21 preparation examples and 3 comparative examples were compared and tested, and the results are shown in Tables 1 to 3. Among them, the small molecule cationic conditioning agents used are all commercially available products, and the active matter content is 60-100%.

[0042] Table 1

[0043] Table 2

[0044] Table 3

[0045] The Z-average particle size test conditions are: water as the dispersion medium, test temperature 25°C; the Zeta potential average value test conditions are: the sample is diluted 100 times before testing.

[0046] From Tables 1 to 3, it can be seen that different small molecule quaternary ammonium salts and different low viscosity silicone oils can be used to prepare small particle size positive charge conditioning lotions. As the content of cationic quaternary ammonium salt increases, the surface charge intensity of the conditioning lotion increases. The rheological properties of the conditioning lotion are affected by the type of small molecule cationic quaternary ammonium salt. The rheological properties of the prepared conditioning lotion are suitable for hair care products. In the same system, the viscosity of silicone oil affects the particle size of the conditioning lotion.

[0047] Example 3 Each preparation example was tested for particle size distribution, with preparation examples 5, 6, 13, 15, 19, and 20 as representatives. The results are as follows: Figures 2 to 7 It can be seen that different small molecule cationic conditioning agents and different viscosity low viscosity silicone oils can prepare nano-scale conditioning agents, proving that the preparation examples of the present invention can prepare nano-scale conditioning emulsions.

[0048] Example 4 Mildness test Taking Preparation Example 20 as an example, the CAM membrane eye irritation score (scoring method: IS) was performed using its 10% aqueous solution. The test steps are as follows: Take the chicken embryos prepared at 10 days of incubation, peel off the eggshell around the air chamber with elbow tweezers, keep the integrity of the egg membrane, and expose the white egg membrane completely; carefully remove the egg membrane with tweezers to ensure that the chicken embryo chorioallantoic membrane (hereinafter referred to as CAM membrane) is not damaged. The structure of the vascular system should be observed again to ensure its integrity; determine whether to use the reaction time method or the endpoint evaluation method according to the test substance; drip the test substance on the CAM membrane until the action time according to the test method used, and parallel 6 chicken embryos; calculate the irritation score or endpoint score of the test substance.

[0049] The results are shown in Table 4 and Figure 8 shown.

[0050] Table 4

[0051] Combining Table 4 and Figure 8 It can be seen that the Zein irritation test result of Preparation Example 20 is non-irritating.

[0052] Example 5 For example, the application of shampoo products is to select healthy hair bundles that have been cleaned and have similar properties, and ensure that the hair bundles are balanced in a constant temperature and humidity chamber for a certain period of time; use 0.6g of standard cleaning solution on both sides of the hair bundle, apply it evenly and wash it, and then perform a baseline wet hair combing test; place it in a constant temperature and humidity chamber for 3 hours and then perform a baseline dry hair combing test; use 1.2g of sample on the hair bundle, apply it evenly and wash it, and then perform a sample wet hair combing test, and place it in a constant temperature and humidity chamber for 3 hours. The sample dry hair combing test was performed. The basic formula components of the shampoo are shown in Table 5.

[0053] Table 5

[0054] As can be seen from Table 5, after adding small particle size positively charged silicone oil conditioning lotion to shampoo base, the conditioning performance of dry and wet hair is improved compared with before use; the conditioning of wet and dry hair of shampoo base containing small particle size positively charged silicone oil conditioning lotion is also significantly improved compared with 5cst silicone oil and 1000cst silicone oil with the same content of active ingredients. It is possible that the small molecule cationic quaternary ammonium salt increases the deposition amount of low viscosity silicone oil on the hair. The fluffiness test shows that after the use of Preparation Example 15 and Preparation Example 13, the fluffiness of the hair is increased by 21.97% and 14.3% respectively compared with before use, and the fluffiness of the hair can be improved after addition. The dry and wet combing properties of Applications 4, 5, and 6 are better than those of Applications 2 and 3, indicating that adding a higher content of small molecule quaternary ammonium salt can further improve the conditioning.

[0055] Example 6 Taking the blank control group and application group 5 in Table 5 as an example, an infrared spectrometer (model TENSOR II) equipped with an attenuated total reflectance (ATR) accessory was used to conduct a silicone oil deposition test, specifically including: like Fig. 9 As shown, after the hair was pressed, the ATR-IR test was used to obtain the infrared spectra of the blank hair bundle, the hair bundle after using the blank shampoo (the blank control group in Table 5), and the hair bundle containing the shampoo of Preparation Example 3 (the application group 5 in Table 5). The results are as follows Fig.10 shown.

[0056] After analysis, the positions of 800cm-1 and 1260cm-1 are stretching vibration signals of silicone oil chemical bonds. After using blank shampoo, no substances that affect the peaks at those two positions appear, while after using the shampoo containing Preparation Example 3, obvious stretching vibration signals can be seen at the positions of 800cm-1 and 1260cm-1, indicating that the application of the present invention can make silicone oil deposited on hair.

[0057] The above disclosure is only the preferred embodiment of the present invention, which certainly cannot be used to limit the scope of the present invention. Therefore, equivalent changes made according to the claims of the present invention are still within the scope of the present invention.

Claims

1. A small particle size positively charged conditioning lotion, characterized in that: The invention is composed of low-viscosity silicone oil, non-ionic emulsifier, small-molecule cationic quaternary ammonium salt, deionized water and preservative; in the small-particle positively charged conditioning emulsion, the mass ratio of the low-viscosity silicone oil, the non-ionic emulsifier and the small-molecule cationic quaternary ammonium salt is 30-60:3-10:1-10.

2. The small particle size positively charged conditioning milk according to claim 1, characterized in that: The particle size of the small-particle positively charged conditioning milk ranges from 100 nm to 1 μm.

3. The small particle size positively charged conditioning emulsion according to claim 1, characterized in that: The viscosity of the low-viscosity silicone oil ranges from 5 cst to 60000 cst.

4. The small particle size positively charged conditioning milk according to claim 1, characterized in that: The nonionic emulsifier includes one or more of laureth-3, laureth-2, laureth-10, laureth-13, oleth-16, oleth-3, oleth-20, oleth-23, and oleth-25.

5. The small particle size positively charged conditioning milk according to claim 1, characterized in that: The small molecule cationic quaternary ammonium salt includes one or more of hexadecyltrimethylammonium chloride, stearyltrimethylammonium chloride, behenyltrimethylammonium chloride, dipalmitoyloxyethyldimethylammonium chloride, behenyltrimethylammonium methylsulfate, and dioleoylethylhydroxyethylmethylammonium methylsulfate; the preservative includes one or more of phenoxyethanol and sodium benzoate.

6. The small particle size positively charged conditioning milk according to claim 1, characterized in that: In the small-particle positively charged conditioning milk, the mass fraction of the preservative is 0.5% to 3%; the mass fraction of the deionized water is 30% to 65%.

7. A method for preparing the small particle size positively charged conditioning milk according to claim 1, characterized in that: include: A, adding the nonionic emulsifier, the small molecule cationic quaternary ammonium salt, and the preservative into the deionized water, heating and stirring to obtain phase A; B. heating the low-viscosity silicone oil, adding it to the phase A, and homogenizing to obtain a pre-emulsion; C. Vigorously dispersing the pre-emulsion to obtain the small-particle positively charged conditioning emulsion.

8. The preparation method according to claim 7, characterized in that: In step C, the violent dispersion includes one or more of ultrasonic microfluidic nanodispersion and high-pressure homogenization.

9. The preparation method according to claim 7, characterized in that: In step A, the temperature of the heating and stirring is 80°C; in step B, the heating temperature is 80°C.

10. An application of the small particle size positive charge conditioning milk according to claim 1, characterized in that: Used in hair care products.

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