A small-particle positively charged conditioning lotion and its preparation and hair care application

Abstract

The present invention relates to the field of daily chemicals and discloses a small-particle positively charged conditioning emulsion, its preparation, and hair care application. The emulsion comprises a low-viscosity silicone oil, a nonionic emulsifier, and a small-molecule cationic quaternary ammonium salt. The low-viscosity silicone oil emulsion, even nanometer-sized, is prepared by utilizing a small-molecule cationic conditioning agent commonly used in hair shampooing and care, which has both conditioning and emulsifying properties. The low-viscosity silicone oil does not have the weighty feeling that high-viscosity silicone oil conditioning agents of prior art solutions can cause in certain populations. The small emulsion particle size allows for uniform deposition, and the positive charge on the emulsion surface enhances the emulsion's stability and, to a certain extent, improves the deposition properties of the low-viscosity silicone oil.

Description

Technical Field

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

[0002] Accumulated hair damage over time causes an uneven hair surface, resulting in dullness, flyaway hair, and increased combing friction. Conditioning ingredients can improve the hair's surface condition to a certain extent. Dimethicone is a common conditioning agent in hair care products. It utilizes the coagulation mechanism of the shampoo system to evenly deposit on the hair surface, forming a thin film to improve the hair's surface condition. High-molecular-weight or high-viscosity polydimethylsiloxanes, such as silicone oils with a viscosity of several hundred thousand, are often used as conditioning agents in shampoos. However, for those who don't require intensive conditioning, such as those with thinning, flat hair, men with short hair, or those seeking volume, excessive deposition of silicone oils with excessive viscosity or molecular weight, while providing superior conditioning, can also weigh down the hair. 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 cetyltrimethylammonium chloride, stearyltrimethylammonium chloride, behenyltrimethylammonium chloride, dipalmitoyloxyethyldimethylammonium chloride, behenyltrimethylammonium methylsulfate, and dioleoylethylhydroxyethylmethylammonium methylsulfate. The silicone oil viscosities include but are not limited to 5 cst, 10 cst, 50 cst, 350 cst, 1000 cst, and 12500 cst.

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

[0005] Positively charged emulsions used in shampoo improve both conditioning and volume by evenly depositing the aggregates during the cleansing process, achieving a balance of light conditioning and volume, leaving hair feeling refreshed and free of bulk. It is speculated that the positive surface charge of the emulsion may aid in the deposition of low-viscosity silicone oil, helping to increase the uniformity and amount of deposited hair.

[0006] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0007] The invention discloses a small-particle positively charged conditioning lotion, which is composed of low-viscosity silicone oil, nonionic emulsifier, small-molecule cationic quaternary ammonium salt, deionized water and preservative.

[0008] Formulating silicone oils into conditioning emulsions with small particle sizes allows for easier formulation and generally more even deposition on the hair.

[0009] 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.

[0010] After research, it was surprisingly found that when low viscosity silicone oil, nonionic emulsifier, 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 Figure 1 The composite emulsion droplet structure shown has suitable emulsion particle size, consistency and viscosity, is highly stable, can be placed at room temperature for more than one month without any change, does not stratify or precipitate, is non-toxic and non-irritating, and can be well used in cleaning products.

[0011] Preferably, the particle size of the small-particle positively charged conditioning milk is comprised between 100 nm and 1 μm.

[0012] Preferably, the viscosity of the low-viscosity silicone oil is 5 cst ~ 12500 cst.

[0013] 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.

[0014] Small-particle silicone oil conditioning emulsions with positive surface charge were 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.

[0015] 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; and the preservative includes one or more of phenoxyethanol and sodium benzoate.

[0016] Adding different small-molecule cationic quaternary ammonium salts to the emulsion imparts a positive charge, reducing the need for subsequent small-molecule cationic conditioning agents. It also enhances the electrostatic repulsion between emulsion particles, improving emulsion stability. The positively charged surface of the liquid may interact with the negatively charged hair surface during the rinsing process, improving the deposition of low-viscosity silicone oils and, to some extent, resolving the difficulty of low-viscosity silicone oils depositing on hair.

[0017] Preferably, 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%.

[0018] A method for preparing the above-mentioned small-particle positively charged conditioning milk comprises:

[0019] 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;

[0020] B. heating the low-viscosity silicone oil, adding it to the phase A, and homogenizing to obtain a pre-emulsion;

[0021] C. Vigorously dispersing the pre-emulsion to obtain the small-particle positively charged conditioning emulsion.

[0022] Preferably, in step C, the intense dispersion comprises one or more of ultrasonic microfluidic nanodispersion and high-pressure homogenization.

[0023] Preferably, in step A, the temperature of the heating and stirring is 80°C; in step B, the temperature of the heating is 80°C.

[0024] An application of the above-mentioned small-particle positively charged conditioning emulsion is used in hair care products.

[0025] Small-particle silicone oil conditioning lotion is used in shampoo to improve the combing properties of lightly damaged hair and provide volume without weighing it down. It is also suitable for other hair care products such as conditioners and hair masks.

[0026] The implementation of the present invention has the following beneficial effects:

[0027] 1. Utilizing small-molecule cationic conditioning agents commonly used in hair shampoo and conditioner, which possess both conditioning and emulsifying properties, low-viscosity silicone oil emulsions with small particle sizes, even nanometer-sized, are prepared. Low-viscosity silicone oils do not cause the weight on hair that can be felt by certain individuals with existing high-viscosity silicone oil conditioning solutions. The small particle size of the emulsion allows for uniform deposition, while the positive surface charge enhances emulsion stability and, to a certain extent, improves the deposition of the low-viscosity silicone oil.

[0028] 2. The use of small molecule cationic conditioners commonly used in hair care can appropriately reduce the amount of conditioners added during the formula development process, and is suitable for the development of hair care product formulas that take both conditioning and fluffiness into account.

[0029] 3. The emulsion is mild and non-irritating to eyes, suitable for the development of mild and non-irritating formulas.

[0030] 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

[0031] Figure 1 Schematic diagram of the structure of the small-particle positively charged conditioning lotion of the present invention.

[0032] Figure 2 This is the particle size distribution diagram of Preparation Example 5, where the red, green and blue lines represent the results of three parallel tests of one sample.

[0033] Figure 3 This is the particle size distribution diagram of Preparation Example 6, where the red, green and blue lines represent the results of three parallel tests of one sample, respectively.

[0034] Figure 4 This is the particle size distribution diagram of Preparation Example 13.

[0035] Figure 5 This is the particle size distribution diagram of Preparation Example 15.

[0036] Figure 6 This is the particle size distribution diagram of Preparation Example 19, where the red, green and blue lines represent the results of three parallel tests of one sample, respectively.

[0037] Figure 7 This is the particle size distribution diagram of Preparation Example 20, where the red, green and blue lines represent the results of three parallel tests of one sample, respectively.

[0038] Figure 8 This is the mildness test diagram of Preparation Example 20.

[0039] Figure 9 This is a test schematic diagram of Example 6.

[0040] Figure 10 This is the test result diagram of Example 6. DETAILED DESCRIPTION

[0041] In order to make the objectives, technical solutions and advantages of the present invention more clear, the present invention will be described in further detail below with reference to the accompanying drawings.

[0042] Example 1

[0043] Preparation process of positively charged small particle size silicone oil conditioning lotion:

[0044] (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.

[0045] (2) Heat silicone oil to 80°C, add it to phase A, and homogenize to obtain a pre-emulsion.

[0046] (3) The pre-emulsion was prepared using an ultrasonic microfluidic nanodisperser (equipment developed jointly 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 conducted, and the results were as follows: Figure 1 shown.

[0047] Figure 1 Si in the middle refers to low viscosity silicone oil, orange lines refer to silicone oil molecules, N+ molecules (black, green) refer to small molecule cationic quaternary ammonium salts, Refers to the nonionic emulsifier in this invention. The prepared small-particle positively charged silicone oil conditioning emulsion exhibits a structure of small nano-emulsion droplets with low-viscosity silicone oil as the core, uniformly encapsulating the silicone oil molecules, a composite small-molecule cationic quaternary ammonium salt forming an outer positive charge, and finally connecting to the lipophilic segment of the nonionic emulsifier.

[0048] Example 2

[0049] Preparation Examples (the scope of protection is not limited to the Preparation Examples)

[0050] By adjusting the formula, 21 preparation examples and 3 comparative examples were tested, and the results are shown in Tables 1 to 3. The small molecule cationic conditioning agents used were all commercially available products with an active ingredient content of 60-100%.

[0051] Table 1

[0052]

[0053] Table 2

[0054]

[0055] Table 3

[0056]

[0057] 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.

[0058] Tables 1-3 show that small-particle positively charged conditioning lotions can be prepared using various small-molecule quaternary ammonium salts and low-viscosity silicone oils. Increasing the content of the cationic quaternary ammonium salt increases the surface charge strength of the conditioning lotion. The rheological properties of the conditioning lotion are influenced by the type of small-molecule cationic quaternary ammonium salt, resulting in a lotion with rheological properties suitable for hair care products. Within the same system, silicone oil viscosity influences the particle size of the conditioning lotion.

[0059] Example 3

[0060] The particle size distribution of each preparation example was tested, 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 low viscosity silicone oils with different viscosities can all be used to prepare nano-scale conditioning agents, proving that the preparation examples of the present invention can all prepare nano-scale conditioning emulsions.

[0061] Example 4

[0062] Mildness test

[0063] Taking Preparation Example 20 as an example, a 10% aqueous solution thereof was used to evaluate the eye irritation of the CAM membrane (scoring method: IS). The test steps were as follows:

[0064] Prepare 10-day-old chick embryos and use curved forceps to peel back the eggshell surrounding the air cell, maintaining the integrity of the egg membrane and completely exposing the white membrane. Carefully remove the egg membrane with forceps, ensuring that the chick chorioallantoic membrane (CAM) is not damaged. Observe the structure of the vascular system again to ensure its integrity. Determine whether to use a reaction time method or endpoint evaluation method based on the test substance. Add the test substance dropwise to the CAM membrane until the exposure time is reached, according to the test method used, in parallel with six chick embryos. Calculate the irritation score or endpoint score for the test substance.

[0065] The results are shown in Table 4 and Figure 8 shown.

[0066] Table 4

[0067]

[0068] Combined with Table 4 and Figure 8 It can be seen that the irritation test result of Zein in Preparation Example 20 is non-irritating.

[0069] Example 5

[0070] For example, in the application of shampoo products, clean and healthy hair bundles with similar properties are screened and the hair bundles are balanced in a constant temperature and humidity chamber for a certain period of time; 0.6g of standard cleaning solution is applied to each side of the hair bundle, and after rinsing, a baseline wet hair combing test is performed; after placing in the constant temperature and humidity chamber for 3 hours, a baseline dry hair combing test is performed; 1.2g of sample is applied to the hair bundle, and after rinsing, a sample wet hair combing test is performed, and after placing in the constant temperature and humidity chamber for 3 hours, a sample wet hair combing test is performed.

[0071] The dry hair combing test was performed on the samples. The basic formula components of the shampoo are shown in Table 5.

[0072] Table 5

[0073]

[0074] Table 5 shows that the addition of a small-particle positively charged silicone oil conditioning emulsion to a shampoo base improves both wet and dry hair conditioning compared to pre-use. The shampoo base containing the small-particle positively charged silicone oil conditioning emulsion also significantly improves both wet and dry hair conditioning compared to 5 cst and 1000 cst silicone oils with the same active ingredient content. This is likely due to the small-molecule cationic quaternary ammonium salt increasing the deposition of the low-viscosity silicone oil on the hair. Fluffiness testing showed that the addition of the small-molecule cationic quaternary ammonium salt to Preparation Examples 15 and 13 increased hair volume by 21.97% and 14.3%, respectively, compared to pre-use, demonstrating that addition can improve hair volume. The dry and wet combing properties of Applications 4, 5, and 6 were significantly better than those of Applications 2 and 3, indicating that adding a higher level of the small-molecule cationic quaternary ammonium salt further enhances conditioning.

[0075] Example 6

[0076] 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:

[0077] like Figure 9 As shown, after pressing the hair, ATR-IR was used to obtain infrared spectra of the blank hair bundle, the hair bundle after using blank shampoo (blank control group in Table 5), and the hair bundle containing shampoo of Preparation Example 3 (application 5 group in Table 5). The results are as follows Figure 10 shown.

[0078] After analysis, the positions of 800cm-1 and 1260cm-1 are the stretching vibration signals of the chemical bonds of silicone oil. After using the blank shampoo, no substances that affect the peaks at those two positions appeared. However, after using the shampoo containing Preparation Example 3, obvious stretching vibration signals were seen at the positions of 800cm-1 and 1260cm-1, indicating that the application of the present invention can enable silicone oil to be deposited on hair.

[0079] The above disclosure is merely a preferred embodiment of the present invention and 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 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; the viscosity of the low-viscosity silicone oil is 5 cst to 60,000 cst; and the particle size of the small-particle positively charged conditioning emulsion is 100 nm to 1 μm.

2. The small-particle positively charged conditioning lotion 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.

3. The small particle size positively charged conditioning lotion according to claim 1, characterized in that: 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.

4. The small-particle positively charged conditioning lotion 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%.

5. A method for preparing the small-particle positively charged conditioning emulsion 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.

6. The preparation method according to claim 5, characterized in that: In step C, the intense dispersion includes one or more of ultrasonic microfluidic nanodispersion and high-pressure homogenization.

7. The preparation method according to claim 5, characterized in that: In step A, the heating and stirring temperature is 80°C; in step B, the heating temperature is 80°C.

8. A use of the small-particle positively charged conditioning emulsion according to claim 1, characterized in that: Used in hair care products.

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