Hair conditioner manufacturing method
By mixing a cationic surfactant and higher alcohol at controlled temperatures, the method stabilizes α-gel formation in hair conditioners, ensuring effective ingredient retention and improving industrial production efficiency.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- SANYO CHEM IND LTD
- Filing Date
- 2025-11-14
- Publication Date
- 2026-05-27
AI Technical Summary
Existing methods for producing α-gel hair conditioners on an industrial scale face challenges in maintaining consistent quality due to the need for precise control of heating and cooling rates, leading to variability in lamellar structure formation.
A method involving the mixing of a composition containing a cationic surfactant and a higher alcohol with a melting point of 50°C or higher with water at 5 to 45°C, eliminating the need for adjusting heating or cooling rates, thereby forming a stable α-gel structure.
This approach allows for the production of a hair conditioner with a stable α-gel that retains active ingredients longer on hair, enhancing conditioning efficacy without the need for precise temperature control, thus improving production efficiency and reducing energy consumption.
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Figure 2026087511000001_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a method for manufacturing a hair conditioner.
Background Art
[0002] As one of the cosmetics for hair, there is a hair conditioner for reducing the dryness feeling during or after hair washing using shampoo or for repairing hair damage caused by various factors. As a hair conditioner composition, it is well-known to form a gel network in which a cationic surfactant and a higher alcohol are stirred and mixed with water as a solvent, and water is contained in solid hydration crystals having a lamellar structure (Non-Patent Document 1). Such a molecular structure of the lamella is a structure in which bilayer membranes in which surfactants are regularly arranged are layered while maintaining a hexagonal crystal state, and is called "α-gel". Since α-gel retains a large amount of water between the bilayer membranes of the lamellar structure, it is possible to adjust the viscosity even when the water content is relatively high. Therefore, when the α-gel hair conditioner composition is applied to wet hair after shampooing or is diluted with water by subsequent rinsing, the viscosity reduction rate is relatively slow, and the active ingredients attached to the hair are difficult to be washed away, and the contact time between the active ingredients and the hair can be lengthened. Therefore, the hair conditioner components can be efficiently imparted to the hair.
[0003] Conventionally, when forming an α-gel by stirring and mixing a cationic surfactant and a higher alcohol with water as a solvent, heating is required in the manufacturing process, and further, adjustment of the cooling rate and the like is important. For example, since α-gel is a hydration crystal, it is known that the rate of crystal nucleus formation and crystal growth changes depending on the temperature, rate, and stirring rate during cooling (Non-Patent Document 1). It is also known that depending on the temperature at which α-gel is precipitated, the lamellar structure is formed in a vesicle shape at high temperature and in a layered shape at low temperature (Non-Patent Document 2). Therefore, it has been difficult to obtain α-gel with constant quality when scaling up on an industrial scale.
Prior Art Documents
[0004] [Non-Patent Document 1] Elucidation and control of α-gel structure formed by long-chain alkylamidoamine lactate / higher alcohol / water mixture system, C&I Commun Vol.48 No.1, 53-55 (2023) [Non-Patent Document 2] Structure of the 1-hexadecanol / octadecyltrimethylammonium chloride / water ternary system aggregate, Journal of the Chemical Society of Japan, 1989, (1) pp. 26-32 [Overview of the Initiative] [Problems that the invention aims to solve]
[0005] Therefore, the object of the present invention is to provide a manufacturing method that allows for the production of a hair conditioner with an α-gel without adjusting the heating or cooling rate. [Means for solving the problem]
[0006] The inventors, after diligently studying to solve the above problems, arrived at the present invention. The present invention relates to a method for producing a hair conditioner, comprising the step of mixing a composition (A) with a melting point of 50°C or higher with water at 5 to 45°C, wherein the composition (A) contains a cationic surfactant and a higher alcohol. [Effects of the Invention]
[0007] According to the present invention, a hair conditioner with an α-gel formed can be obtained without adjusting the heating or cooling rate. [Brief explanation of the drawing]
[0008] [Figure 1] This is a cryoscanning electron microscope image of a cross-section of hair conditioner B11 obtained in Example 11. [Figure 2]This is a cryoscanning electron microscope image of a cross-section of hair conditioner B12 obtained in Example 12. [Figure 3] This is a cryoscanning electron microscope image of a cross-section of hair conditioner B13 obtained in Example 13. [Figure 4] This is the DSC curve obtained from the DSC measurement of hair conditioner B14 in Example 14. [Figure 5] This is the DSC curve obtained from the DSC measurement of hair conditioner B16 in Example 16. [Modes for carrying out the invention]
[0009] The present invention relates to a method for producing a hair conditioner, comprising the step of mixing a composition (A) with a melting point of 50°C or higher with water at 5 to 45°C, wherein the composition (A) contains a cationic surfactant and a higher alcohol.
[0010] The melting point of composition (A) is 50°C or higher, and more preferably 50 to 100°C from the viewpoint of the stability of the α-gel formed.
[0011] The melting point of composition (A) is measured by differential scanning calorimetry (DSC) as described in JIS 7121-1987.
[0012] The composition (A) comprises a cationic surfactant and a higher alcohol. The cationic surfactant is preferably a quaternary ammonium compound having an alkyl group with 12 to 22 carbon atoms. Being a quaternary ammonium compound reduces static electricity and improves the combability of dry hair. Furthermore, the presence of alkyl groups effectively enhances the effects of the higher alcohols described later, and improves the storage stability of the hair conditioner composition. The alkyl group of the quaternary ammonium compound is preferably an alkyl group having 12 to 22 carbon atoms, and more preferably an alkyl group having 16 to 22 carbon atoms.
[0013] As the quaternary ammonium compound having an alkyl group with 12 to 22 carbon atoms, preferably, it is a compound selected from the group consisting of cetrimonium chloride, steartrimonium chloride, behentrimonium chloride, cetrimonium methosulfate, steartrimonium methosulfate, behentrimonium methosulfate, cetrimonium ethosulfate, steartrimonium ethosulfate, behentrimonium ethosulfate, and mixtures thereof.
[0014] As the higher alcohol, from the viewpoint of forming an α-gel with the higher alcohol and the cationic surfactant, preferably, it is a higher alcohol having 10 to 30 carbon atoms, and from the viewpoint of storage stability, more preferably, it is a higher alcohol having 12 to 22 carbon atoms.
[0015] Preferred specific examples of the higher alcohol include lauryl alcohol (12 carbon atoms), myristyl alcohol (14 carbon atoms), cetyl alcohol (16 carbon atoms), stearyl alcohol (18 carbon atoms), cetostearyl alcohol (16 to 18 carbon atoms), and behenyl alcohol (22 carbon atoms), etc. These may be used alone or in combination of two or more. From the viewpoint of α-gel formation, cetostearyl alcohol is more preferable.
[0016] In the composition (A), the molar ratio of the cationic surfactant to the higher alcohol (cationic surfactant: higher alcohol) is preferably 1:1 to 1:15 from the viewpoints of the conditioning effect of the hair conditioner and α-gel formation.
[0017] The composition (A) of the present invention is preferably particles obtained by heating the cationic surfactant and the higher alcohol at 75 to 120°C and uniformly dissolving them, and then cooling to 5 to 60°C.
[0018] There is no restriction on the shape of the particles, and they may be spherical particles or irregularly shaped particles. The spherical particles refer to spherical bodies with rounded corners of powder particles. The irregularly shaped particles refer to those with shapes that do not take a regular form, such as crushed, plate-like, scaly, needle-like, etc.
[0019] The median particle size of the particles based on volume is preferably 10 to 3500 μm, more preferably 100 to 3500 μm, and particularly preferably 300 to 1000 μm. The median particle size of the composition (A) based on volume can be measured by the dry method using the dry measurement unit of a laser diffraction / scattering particle size distribution measuring device (manufactured by Horiba, Ltd.; Partica LA-960V2) under the condition of compressed air: 0.30 MPa.
[0020] The median diameter of the particles based on volume can be adjusted by sieves specified in JIS Z 8801 after pulverizing the powder composition for a hair conditioner.
[0021] The manufacturing method of the hair conditioner of the present invention includes a step of mixing the composition (A) with a melting point of 50 °C or higher and water at 5 to 45 °C. The mixing temperature of the composition (A) and water is 5 to 45 °C, and more preferably 15 to 40 °C. If it is less than 5 °C, the viscosity during stirring of the conditioner deteriorates, and if it exceeds 45 °C, the composition (A) cannot form a stable lamellar structure. There is no particular limitation on the method of mixing the composition (A) and water, and they may be mixed using a known mixer, or the composition (A) and water may be put into a bag, container, etc. and mixed by hand. Examples of the mixer include a homomixer, a homodisper, a wave rotor, a homogenizer, a disperser, a paint conditioner, a ball mill, a magnetic stirrer, and a mechanical stirrer, etc. The water in question is not particularly limited and can be any water that is chemically and biologically clean. For example, distilled water, deionized water, purified water, pure water, ultrapure water, tap water, well water, and mineral water can be used. According to the manufacturing method of the present invention, an α-gel can be formed simply by mixing the composition (A) with water at 5 to 45°C, without adjusting the heating or cooling rate for α-gel formation. The conditioner obtained by the manufacturing method of the present invention forms an α-gel, and even when applied to wet hair after shampooing or diluted with water during subsequent rinsing, the rate of viscosity reduction is relatively slow. This makes it difficult for the active ingredients attached to the hair to be washed away, and the contact time between the active ingredients and the hair can be extended, allowing conditioning ingredients to be efficiently delivered to the hair.
[0022] In the step of mixing composition (A) and water at 5 to 45°C, the weight ratio of composition (A):water is preferably 1:99 to 30:70.
[0023] In the present invention, the hair conditioner may further contain one or more other hair care ingredients in addition to composition (A) and water.
[0024] Examples of other hair care ingredients include one or more of the following: cleansing agents, skin conditioners, hair styling agents, anti-dandruff agents, hair growth promoters, fragrances, sunscreen compounds, pigments, moisturizers, hydrocarbon oils, ester oils, silicone oils, film-forming agents, alpha-hydroxy acids, hair colorants, detergents, thickeners, and preservatives.
[0025] Examples of the hydrocarbon oils include paraffin, liquid paraffin, hydrogenated polyisobutene, ozokerite, squalane, pristane, ceresin, and microcrystalline wax.
[0026] Examples of the ester oils mentioned above include myristic acid esters, palmitic acid esters, stearic acid esters, lauric acid esters, linoleic acid esters, octanoic acid esters, oleic acid esters, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, lactic acid esters, malic acid esters, adipic acid esters, sebaciate esters, succinic acid esters, citrate esters, polyhydric alcohol esters, and lanolin esters.
[0027] Examples of the aforementioned humectants include glycerin, xylitol, diglycerin, dipropylene glycol (DPG), sorbitol, sodium DL-pyrrolidone carboxylate, 1,3-butylene glycol (1,3BG), propylene glycol, polyethylene glycol, polyglycerin, 1,2-propanediol, 1,3-propanediol, 1,2-butanediol, 1,4-butanediol, and maltitol.
[0028] Examples of the sunscreen compounds include benzophenone derivatives such as 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid, sodium 2-hydroxy-4-methoxybenzophenone-5-sulfonate, dihydroxymethoxybenzophenone, sodium dihydroxymethoxybenzophenone-sulfonate, 2,4-dihydroxybenzophenone, and tetrahydroxybenzophenone; paraaminobenzoic acid derivatives such as paraaminobenzoic acid, ethyl paraaminobenzoate, glyceryl paraaminobenzoate, amyl paradimethylaminobenzoate, and octyl paradimethylaminobenzoate; ethyl paramethoxycinnamate, isopropyl paramethoxycinnamate, octyl paramethoxycinnamate, and 2-ethyl paramethoxycinnamate. Examples include methoxycinnamic acid derivatives such as oxyethyl, sodium paramethoxycinnamate, potassium paramethoxycinnamate, and glyceryl mono-2-ethylhexanoate paramethoxycinnamate; salicylic acid derivatives such as octyl salicylate, phenyl salicylate, homomentyl salicylate, dipropylene glycol salicylate, ethylene glycol salicylate, myristyl salicylate, and methyl salicylate; and urocanic acid, ethyl urocanic acid, ethyl urocanic acid ester, 4-tert-butyl-4′-methoxybenzoylmethane, 2-(2′-hydroxy-5′-methylphenyl)benzotriazole, 2-phenyl-5-methylbenzoxazole, methyl anthranilate, and 2-ethylhexyl dimethoxybenzylidene dioxoimidazolidinepropionate.
[0029] According to the manufacturing method of the present invention, hair conditioner can be manufactured in a simple manner without adjusting heating or cooling temperatures. For example, a hair conditioner can be obtained by melting and mixing a solid composition (7.5 parts by weight) obtained by behentrimonium chloride (44.3 parts by weight), a cationic surfactant, and cetearyl alcohol (55.7 parts by weight), a higher alcohol, with mineral oil (4.5 parts by weight), deionized water (132 parts by weight), DPG (dipropylene glycol) (1.5 parts by weight), and sorbitol (4.5 parts by weight), mixing them in a homodisperser at 3000 rpm for 5 minutes, and letting it stand overnight to form an α-gel.
[0030] Furthermore, a hair conditioner can be obtained by melting and mixing a solid composition (7.5 parts by weight) obtained by behentrimonium chloride (44.3 parts by weight), a cationic surfactant, and cetearyl alcohol (55.7 parts by weight), a higher alcohol, along with mineral oil (4.5 parts by weight), tap water (132 parts by weight), DPG (dipropylene glycol) (1.5 parts by weight), and sorbitol (4.5 parts by weight), in a sealed container, shaking by hand for 5 minutes, and letting it stand overnight to form an α-gel. [Examples]
[0031] The present invention will be further described below with reference to examples and comparative examples, but the present invention is not limited thereto. Unless otherwise specified, % refers to weight %.
[0032] <Manufacturing Examples 1-10> Cationic surfactants and higher alcohols were weighed out in the proportions (parts by weight) shown in Table 1, heated to 115°C to dissolve uniformly, then cooled to 25°C and ground using a mill mixer. The mixture was then sieved using JIS standard sieves of 180 μm, 300 μm, 500 μm, 1 mm, and 3.35 mm to select the following particles, thereby obtaining particulate compositions A1 to A10. Compositions A1 and A5-7: Particles that do not pass through a sieve with a mesh size of 500 μm, but pass through a sieve with a mesh size of 1 mm. Compositions A2 and A9-10: Particles that do not pass through a sieve with a mesh size of 300 μm, but pass through a sieve with a mesh size of 500 μm. Composition A3: Particles that do not pass through a sieve with a mesh size of 180 μm, but pass through a sieve with a mesh size of 300 μm. Composition A4: Particles that pass through a sieve with a mesh size of 180 μm. Composition A8: Particles that do not pass through a sieve with a mesh size of 1 mm, but pass through a sieve with a mesh size of 3.35 mm.
[0033] <Median particle size based on volume> The particle size distribution was measured using a laser diffraction / scattering particle size distribution analyzer (Horiba, Ltd.; Partica LA-960V2). Using the dry measurement unit of this instrument, the volume-based median particle size was measured using the dry method under compressed air pressure of 0.30 MPa.
[0034] <Melting point> The measurement was performed using a differential scanning calorimeter (TA Instruments, DSCQ20). When the sample was heated from 20°C to 100°C at a rate of 10°C / min for the first time, the temperature at the peak of the endothermic peak that appeared at the highest temperature was defined as the melting point.
[0035] [Table 1]
[0036] <Examples 1-10> Deionized water was added to compositions A1 to A10 to make a 1% aqueous solution, and the mixture was heated in a homodisperser at 500 rpm for 1 minute at the temperatures listed in Table 2 to obtain hair conditioners B1 to B10 according to Examples 1 to 10.
[0037] <Method for confirming α-gel formation> The following measurement method was used to determine whether the dispersed particles contained in hair conditioners B1 to B10 formed an α-gel. (Method for measuring α-gel formation) The formation of the α-gel can be confirmed by the peaks obtained from wide-angle X-ray diffraction measurements of the sample. If a single, sharp peak is observed at 21.5°, it is determined that α-gel formation has occurred. If multiple peaks are observed around 21.5°, or if there are no peaks, it is determined that α-gel formation has not occurred. In Table 1, a circle (○) is indicated for samples in which α-gel formation was achieved.
[0038] [Table 2]
[0039] <Example 11> To the composition A1 obtained in Production Example 1, ion-exchanged water was added to make a 1% aqueous solution, and the mixture was mixed at 500 rpm for 1 minute using a homodisperser to obtain hair conditioner B11. A cross-section of the obtained hair conditioner B11 was cut using a cryoscanning electron microscope, and the cross-section was observed and imaged. Figure 1 shows a cryoscanning electron microscope image of the cross-section in Example 11.
[0040] <Example 12> To the composition A1 obtained in Production Example 1, ion-exchanged water was added to make a 10% aqueous solution, and the mixture was mixed with a homodisperser at 500 rpm for 1 minute to obtain hair conditioner B12. A cross-section of the obtained hair conditioner B12 was cut using a cryoscanning electron microscope, and the cross-section was observed and imaged. Figure 2 shows a cryo-scanning electron microscope image of the cross-section in Example 12.
[0041] <Example 13> To the composition A1 obtained in Production Example 1, ion-exchanged water was added to make a 30% aqueous solution, and the mixture was mixed in a homodisperser at 3000 rpm for 5 minutes to obtain hair conditioner B13. A cross-section of the obtained hair conditioner B13 was cut using a cryoscanning electron microscope, and the cross-section was observed and imaged. Figure 3 shows a cryoscanning electron microscope image of the cross-section in Example 13.
[0042] The observation conditions for the cryoscanning electron microscope in this invention were as follows. Equipment :JSM-7100F Acceleration voltage: 1.0kV Sample stage temperature: around -80°C
[0043] <Examples 14-17> Composition A1 obtained in Production Example 1, Composition A5 obtained in Production Example 5, Composition A6 obtained in Production Example 6, and Composition A7 obtained in Production Example 7 were each mixed with deionized water to make a 5% aqueous solution, and then mixed with a homodisperser at 500 rpm for 1 minute. Further mixing at 3000 rpm for 5 minutes yielded hair conditioners B14 to B17. Differential scanning calorimetry (also known as DSC measurement) was performed on the obtained hair conditioners B14 to B17.
[0044] During the first heating of the obtained hair conditioners B14-B17, an endothermic peak appeared at 73°C in each case. The endothermic peak at 73°C originated from the α-gel, confirming the formation of an α-gel. Furthermore, no endothermic peak at 56°C, which originated from the single hydrated crystals of higher alcohols, was observed.
[0045] During the second heating of the obtained hair conditioners B14-B15, an endothermic peak appeared at 73°C, originating from the α-gel. Furthermore, no endothermic peak at 56°C, originating from the single hydrated crystals of higher alcohols, was observed. Figure 4 shows the DSC curve obtained from the DSC measurement of hair conditioner B14.
[0046] During the second heating of the obtained hair conditioners B16-17, an endothermic peak appeared at 73°C, originating from the α-gel. Additionally, an endothermic peak appeared at 56°C, originating from the single hydrated crystals of the higher alcohols. Figure 5 shows the DSC curve obtained from the DSC measurement of hair conditioner B16.
[0047] The differential scanning calorimetry in this invention was performed using a differential scanning calorimeter (DA Instruments, DSCQ20). The sample was first heated from 20°C to 90°C at a rate of 10°C / min, then cooled from 90°C to 10°C at a rate of 10°C / min, and then heated again from 10°C to 90°C at a rate of 10°C / min.
[0048] Examples 1 to 17 confirmed that mixing composition (A) with water at 5 to 45°C yields a hair conditioner with an α-gel structure different from that obtained when mixed under heating. [Industrial applicability]
[0049] The present invention's method for manufacturing hair conditioner eliminates the need to adjust heating and cooling rates. Therefore, this method leads to significant improvements in production capacity through energy savings and process shortening.
Claims
1. The process includes a step of mixing a composition (A) with a melting point of 50°C or higher with water at 5 to 45°C. The composition (A) comprises a cationic surfactant and a higher alcohol. A method for manufacturing hair conditioner.
2. The manufacturing method according to claim 1, wherein the molar ratio of the cationic surfactant to the higher alcohol (catenic surfactant: higher alcohol) is 1:1 to 1:
15.
3. The production method according to claim 1, wherein the cationic surfactant is a quaternary ammonium compound having an alkyl group with 12 to 22 carbon atoms.
4. The production method according to claim 3, wherein the quaternary ammonium compound having an alkyl group having 12 to 22 carbon atoms is cetrimonium chloride, steartrimonium chloride, behentrimonium chloride, cetrimonium methosulfate, steartrimonium methosulfate, behentrimonium methosulfate, cetrimonium ethosulfate, steartrimonium ethosulfate, behentrimonium ethosulfate, or a mixture thereof.