JP2022035334A - Hair styling composition and method of producing hair styling composition - Google Patents

Abstract

To provide a hair styling composition that imparts viscosity to hair and is easy to wash off while keeping the hair cohesive, and to provide a method for producing a hair styling composition.SOLUTION: The hair styling composition comprises an oil agent and cellulose fine fibers having an average fiber diameter of 100 nm or less, the oil agent being contained therein in amount of 10% by mass or more. The method for producing a hair styling composition comprises: an oil homogenization step in which an oil agent is homogenized to make the oil agent a liquid with a uniform concentration and kept at 70 to 90 degrees Celsius; a mixing step in which the homogenized oil agent is mixed with a surfactant and cellulose fine fibers having an average fiber diameter of 100 nm or less to obtain a mixture; and an emulsification step in which an aqueous medium is mixed with the mixture obtained in the mixing step and the mixture is emulsified to obtain a water-in-oil (O/W) emulsion.SELECTED DRAWING: None

Description

The present invention relates to a hair styling composition and a method for producing a hair styling composition.

Traditionally, hair styling products such as wax have been used by consumers and the like to condition their hair. Consumers use various types of hair styling products according to, for example, their own hair quality and the condition of the day. The hair styling product contains wax or the like for imparting viscosity to give the hair a hard texture, and by adhering the wax or the like to the hair, the hair becomes cohesive and a conditioning effect is exerted. It will be. In addition, hair styling products tend to be easy to wash off, but in general, hair styling products with high viscosity have strong adhesion to hair, so it may be difficult to wash them off easily, which also has these contradictory properties. That is, it is desired to provide a hair styling product that has a viscosity but is easy to wash off.

WO2018 / 186260 Japanese Unexamined Patent Publication No. 2002-308727 Japanese Unexamined Patent Publication No. 2019-199671

Regarding the hair styling product, Patent Document 1 discloses a technique for imparting viscosity to hair, and states that the effect of improving the viscosity of hair is achieved by including a thickener in the hair styling product. As the thickener, modified cellulose nanofibers having a structure in which a predetermined functional group is bonded to a pyranose ring constituting the cellulose nanofibers are used. In this modified cellulose nanofiber, the hydroxymethyl group at the 6-position of the pyranose ring is replaced with a predetermined functional group (functional group described in paragraph [0009] of the same document) by an oxidation step and an amine modification step. , It is different from the cellulose fine fiber used in the present invention. Patent Document 2 discloses a technique relating to a cosmetic composition (hair styling product, etc.) containing fibers and capable of maintaining the adhesion of the fibers to the skin or the like. The document states that by including fibers with different properties in cosmetics, the fibers adhere well to the skin and the like, especially keratin substances, and do not peel off from the fibers over time.

The hair styling products described in these documents mention the improvement of viscosity and the maintenance of adhesiveness as the effects to be exerted, but do not pay attention to the ease of washing off, and whether or not the hair styling products are easy to wash off is not considered. It is unknown. Therefore, it is an object of the present invention to provide a hair styling composition and a method for producing a hair styling composition, which imparts viscosity to the hair and is easy to wash off while the hair is well organized.

The embodiment for solving the above-mentioned problem is shown below.
(First aspect)
It has an oil agent and cellulose fine fibers with an average fiber diameter of 100 nm or less.
The oil agent is contained in an amount of 10% by mass or more.
A hair styling composition characterized by that.

After conducting various studies to solve the above problems, the present inventor focused on the dispersibility of cellulose fine fibers. When the cellulose fine fibers are mixed with a liquid medium, the cellulose fine fibers are dispersed with each other. This is probably due to the following reasons. Cellulose fine fibers have a high aspect ratio, and the hydroxy groups of cellulose are hydrogen-bonded to each other to form a three-dimensional network structure. Therefore, the cellulose fine fibers are difficult to agglomerate and agglomerate with each other, and maintain high dispersibility in the medium. Due to this property, the hair styling composition having the cellulose fine fibers is in a state where the cellulose fine fibers are mutually dispersed in the hair styling composition. When the average fiber diameter of the cellulose fine fibers is 100 nm or less, the oil agent easily enters the voids formed by adopting the three-dimensional network structure, and therefore, the oil agent is dispersed together with the dispersion of the cellulose fine fibers. It is presumed to be.

Further, the cellulose fine fiber dispersion liquid in which the cellulose fine fibers are dispersed in the liquid medium has a viscosity. The hair styling composition of this embodiment has a viscosity due to the viscous action of the cellulose fine fibers. Further, the hair styling composition of this embodiment contains an oil agent, and the oil agent also has a viscosity. In the hair styling composition of this embodiment, the viscosity of the oily component and the viscosity of the cellulose fine fibers are combined, and the viscosity is improved as compared with the conventional hair styling composition containing no cellulose fine fibers. If the content of the oil agent is small, the viscosity is difficult to develop, but if it is contained in an amount of 10% by mass or more, the hair styling composition has an effect of imparting an excellent viscosity to the hair.

The hair to which the hair styling composition of this embodiment is attached forms a bundle with a plurality of adjacent hairs and is united. The volatile components of the hair styling composition that adhere to the hair volatilize, and the remaining components, mainly cellulose fine fibers and oils, remain attached to the hair. It is presumed that the cellulose fine fibers and the oil agent play a role in maintaining the shape of the trimmed hair. The reason for this is not clear, but probably the oil agent is dispersed together with the dispersion of the cellulose fine fibers, and even after the volatilization of the volatile components, the state in which the cellulose fine fibers are attached to the oil agent is maintained, and the cellulose fine fibers have. Due to the viscous action, the increased viscosity oil remains attached to the hair. It is presumed that the cellulose fine fibers and the oil agent intervene between the hairs forming the hair bundle to maintain the hair in a cohesive state and prevent the hair bundle from being deformed or scattered. ..

The hair styling composition of this embodiment is easy to wash off. This is presumed to be due to the following actions. In the conventional hair styling composition that does not contain cellulose fine fibers, the oil agent directly adheres to the hair. Even if the hair to which the conventional hair styling composition is attached is washed, it is not easy to wash off the hair styling composition because the oil repels water. On the other hand, the hair styling composition of this embodiment has cellulose fine fibers, and a part of the oil agent adhering to the hair is directly attached and the rest is indirectly attached via the cellulose fine fibers. ing. Cellulose fine fibers are hydrophilic and easily run off with water when washing hair. In other words, the oil agent indirectly attached to the hair by the cellulose fine fibers easily flows off by washing the hair. In the hair styling composition of this embodiment, a part of the oil agent indirectly adheres to the hair, so that it is easier to run off than the conventional hair styling composition.

(Second aspect)
Of the 100 parts by mass of the oil agent, 50 parts by mass or more is wax.
The hair styling composition of the first aspect.

The inclusion of the wax having the above concentration imparts viscosity to the hair, giving the hair an impression of having a solid feeling.

(Third aspect)
Some of the cellulose fine fibers are obtained by esterifying the hydroxy group of the cellulose fiber with a phosphoric acid.
The hair styling composition according to the first aspect or the second aspect.

The esterified cellulose fine fibers are superior in transparency as compared with the non-esterified cellulose fine fibers. For example, when the hair styling composition has a colored pigment, the cellulose fine fibers have excellent transparency, so that the hair styling composition is not easily affected by the color tone of the cellulose fine fibers, and the color tone of the colored pigment is obtained.

(Fourth aspect)
The cellulose fine fibers are contained in an amount of 0.1% by mass or more based on the solid content.
The hair styling composition according to any one of the first to third aspects.

The hair styling composition of this aspect imparts viscosity to the hair and maintains the styling shape, but has a more excellent effect of being easy to wash off.

(Fifth aspect)
The cellulose fine fibers are made from hardwood kraft pulp and / or softwood kraft pulp.
The hair styling composition according to any one of the first to fourth aspects.

The cellulose fine fiber of this embodiment has excellent strength (rigidity) of the raw material pulp and relatively few impurities generated in the process of defibration, so that it has excellent tensile strength and suppresses the change in the shape of the prepared hair. The effect of improving the cohesiveness after hair styling is achieved.

(Sixth aspect)
There is one peak value in the pseudo particle size distribution curve of the cellulose fine fibers.
The hair styling composition according to any one of the first to fifth aspects.

In the cellulose fine fibers of this embodiment, when the average fiber diameter is 100 nm or less and the peak value in the pseudo particle size distribution curve is one, the variation in fiber diameter (statistical dispersion value) is relatively small. That is, the fiber diameters of the cellulose fine fibers are close to each other. Therefore, a three-dimensional network is easily formed, and it is presumed that this formation has an excellent effect of imparting viscosity to the hair and maintaining a trimmed shape.

(7th aspect)
An oil droplet (O / W) type emulsion in water,
The hair styling composition according to any one of the first to sixth aspects.

In this embodiment, it is assumed that the cellulose fine fibers to which the oil agent is attached and the cellulose fine fibers to which the oil agent is not attached are mixed. Specifically, the hair-conditioning composition of this embodiment includes (1) cellulose fine fibers completely covered with an oil phase, (2) cellulose fine fibers completely covered with an aqueous phase, and (3) a part. Is covered with an oil phase and the rest is covered with an aqueous phase (that is, intervening between the oil phase and the aqueous phase) and has cellulose fine fibers. Then, when an external force or the like is received, the cellulose fine fibers change between the states of (1), (2), and (3). An oil-in-water (O / W) -type emulsion is generally considered to be easier to wash off than a water-in-oil (W / O) -type emulsion. In this embodiment, since the cellulose fine fibers are contained, the cellulose fine fibers are washed off when the cellulose fine fibers are to be washed off, and the oil agent adhering to the cellulose fine fibers is also easily washed off.

(8th aspect)
An oil agent homogenization process that keeps the oil agent at 70 to 90 degrees Celsius and makes it a liquid with a uniform concentration.
A mixing step of mixing a surfactant and cellulose fine fibers having an average fiber diameter of 100 nm or less with a homogenized oil to obtain a mixture.
It has an emulsification step of mixing an aqueous medium with a mixture obtained in the mixing step and emulsifying the mixture to obtain an oil droplet (O / W) type emulsion in water.
A method for producing a hair styling composition.

Since the cellulose fine fibers are mixed before the aqueous medium is mixed with the oil agent, the cellulose fine fibers are mixed with the oil agent and sufficiently dispersed. If the aqueous medium and the cellulose fine fibers are mixed in the emulsification step without going through the mixing step, most of the cellulose fine fibers are unevenly distributed in the aqueous medium, and the dispersibility tends to be uneven.

According to the present invention, there is a method for producing a hair styling composition and a hair styling composition that imparts viscosity to the hair and is easy to wash off while the hair is well organized.

The embodiment for carrying out the present invention will be described below. The embodiment of the present invention is an example of the present invention. The scope of the present invention is not limited to the scope of the present embodiment.

The hair styling composition in the present invention is characterized by containing cellulose fine fibers and an oil agent. The oil agent imparts the effect of setting the hair into a desired form.

(Oil)
The oil agent used in this embodiment refers to a liquid substance or a solid substance having incompatibility with water, and imparts viscosity and cohesiveness to hair. The oil agent is not particularly limited, and examples thereof include oily components such as wax and non-volatile oil, and one or more of the oily components such as wax and non-volatile oil are used in combination. be able to. In particular, wax is preferable from the viewpoint of imparting excellent viscosity to the hair and improving the cohesiveness. The oil agent (percentage content) may be contained in the hair styling composition in an amount of 10% by mass or more, preferably 15% by mass or more, and more preferably 20% by mass or more. If the oil (percentage content) contained in the hair styling composition is less than 10% by mass, the hair styling composition has a low viscosity and may feel watery.

The hair conditioner composition of this embodiment may be emulsified (emulsified) or non-emulsified, and the emulsion may be an oil droplet (O / W) type in water. However, a water-in-oil (W / O) type may be used, but an oil-in-water (O / W) type is particularly preferable because it has excellent wash-off property. When the hair styling composition is an oil droplet (O / W) type emulsion in water, the upper limit of the oil contained in the hair styling composition is 50% by mass, preferably 49% by mass or less. When the hair styling composition is an oil droplet (O / W) type emulsion in water and the oil agent (percentage content) exceeds 50% by mass, it becomes an oil droplet (O / W) type emulsion in water. It becomes difficult.

(Low)
Rowe imparts hair styling property to the hair styling composition, and when it is dispersed in the hair styling composition together with cellulose fine fibers, it imparts viscosity to the hair and brings about an effect of improving cohesion. The wax present in the hair styling composition is dispersible in the form of particles in an aqueous medium. In this embodiment, the wax has a melting point of 30 ° C. or higher, preferably 55 ° C. or higher, 200 ° C. or lower, preferably 120 ° C. or lower, and is in a state of solid to liquid or liquid to solid at a temperature near the melting point. It can be defined as one that changes and becomes a solid lipophilic fat compound under normal temperature and pressure.

The proportion of wax in 100 parts by mass of the oil is not particularly limited, but for example, it may be contained in an amount of 50 parts by mass or more, preferably 52 parts by mass or more, and more preferably 53 parts by mass or more. When the amount of wax is 50 parts by mass or more out of 100 parts by mass of the oil agent, the hair styling composition has an excellent viscosity and makes the hair cohesive, which is preferable.

Examples of what is used as a row are listed below, but are not limited to these. One type of wax may be used from the following, or two or more types may be selected and used in combination.

The wax used in this embodiment is not particularly limited as long as the hair styling composition is waxy, but specifically, candelilla wax, carnauba wax, sunflower seed wax, rice bran wax, wood wax, honey wax, and the like. Lanorin, hard lanorin, montan wax, hydrogenated jojoba oil, behenyl behenate, glyceryl tribehenate, selecin, paraffin wax, microcrystallin wax, fisher tropus wax, polyethylene wax, cinnamon wax, rice wax, aurikuri wax, sugar cane wax, ozokelite , Paraffin wax, polyethylene wax, wax obtained by catalytic hydrogenation of vegetable or animal oil having a linear or branched C8-C32 fatty chain can also be mentioned. Among these, beeswax and beeswax are particularly preferable because they have a strong setting force even in a small amount.

(Liquid oil)
The liquid oil can be added to the hair styling composition in order to suppress stickiness and impart good elongation. The ratio of the liquid oil content to 100 parts by mass of the oil agent is not particularly limited, but for example, it may be contained in an amount of 50 parts by mass or less, preferably 48 parts by mass or less, and more preferably 44 parts by mass or less. If the liquid oil content exceeds 50 parts by mass out of 100 parts by mass of the oil agent, the hair styling composition can be finished to have a soft viscosity, but the hair may not be well organized and stickiness may increase.

Examples of those used as liquid oils are listed below, but are not limited thereto. As the liquid oil component, one type may be used from the following, or two or more types may be selected and used in combination.

Liquid oils include liquid paraffin, ethylhexyl palmitate, macadamia nut oil, avocado oil, evening primrose oil, mink oil, rapeseed oil, cacao oil, saflower oil, persic oil, cottonseed oil, egg yolk oil, lanolin, squalane, cetanol, and stearyl alcohol. , Lauryl alcohol, cetostearyl alcohol, 1,3-butylene glycol, behenyl alcohol, lanolin alcohol, hexyldecanol, octyldodecanol, myristic acid, palmitic acid, stearic acid, isostearic acid, oleic acid, linolenic acid, linoleic acid, oxystearic acid , Undecylenic acid, lanolin fatty acid, hard lanolin fatty acid, isopropylmyristic acid, isopropylpalmitic acid, isopropylstearic acid, glycerol diethylhexanoic acid, butylstearic acid, polyoxypropylene butyl ether, polar oils such as ethyl linoleate, carboxyl-modified silicone, Carbinol-modified silicone, mercapto-modified silicone, methylstyryl-modified silicone, alkyl-modified silicone, higher fatty acid ester-modified silicone, hydrophilic special-modified silicone, higher alkoxy-modified silicone, higher fatty acid-containing silicone, fluorine-modified silicone, methylpolysiloxane, octamethyl Cyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexanesiloxane, polyoxyethylene / methylpolysiloxane copolymer, polyoxypropylene / methylpolysiloxane copolymer, poly (oxyethylene / oxypropylene) methylpolysiloxane co-weight Examples thereof include coalescence, methylhydrogenpolysiloxane, tetrahydrotetramethylcyclotetrasiloxane, methylpolysiloxane emulsion, highly polymerized methylpolysiloxane, and trimethylsiloxysilicic acid. Since the cellulosic fine fiber has a predetermined degree of water retention, it may be used as a substitute for the oil component of an alcohol-based component such as 1,3-butylene glycol which is generally added for the purpose of moisturizing. Thereby, the hair styling composition of the present embodiment can have a small amount or no oil content of the alcohol-based component, thereby preventing a decrease in the setting force. Further, liquid paraffin and ethylhexyl palmitate are particularly preferable as the liquid oil component that exhibits a glossy effect while being mixed with the cellulose fine fibers in the hair styling composition.

(Non-volatile oil)
The non-volatile oil imparts hair styling properties to the hair styling composition, and by being dispersed in the hair styling composition together with cellulose fine fibers, it has the effect of imparting viscosity to the hair and improving cohesion. Bring. Examples of the non-volatile oil include at least one selected from non-volatile hydrocarbon-based oils, non-volatile silicones, and fluorinated oils. The non-volatile hydrocarbon oil is a hydrocarbon oil composed of an ester of fatty acid and glycerol, and the fatty acid has a chain having a length different from that of C4 to C24, and these chains are linear or branched. Can be exemplified by being saturated or unsaturated with, specifically, wheat germ, sunflower, grape seed, corn, sunflower, karite, avocado, olive, soybean, sweet almond, palm, hazelnut, macadamia, jojoba, alfalfa, sesame. , Cucumber, rapeseed, Ester seed, Matsuyoigusa, Awa, barley, rye, Benibana, Jakoubara oil.

(Dispersion medium)
The hair styling composition can include an aqueous medium. The aqueous medium may be water or a lower monoalcohol having 1 to 5 carbon atoms. Further, for example, ethanol or isopropanol, a glycol having 8 or less carbon atoms, for example, propylene glycol, ethylene glycol, dipropylene glycol, a ketone having 3 or 4 carbon atoms, or an aldehyde having 2 to 4 carbon atoms may be used. good. Water, which is relatively poor in volatility, is preferable as an aqueous medium from the viewpoint that the ratio of the composition in the hair styling composition is relatively difficult to change, the composition is not easily deteriorated, and a stable state is maintained.

(Surfactant)
The surfactant can be appropriately added from the viewpoint of stabilizing the dispersibility between the compositions in the hair styling composition and improving the feel. Examples of those used as surfactants are listed below, but are not limited thereto. As the surfactant, one type may be used from the following, or two or more types may be selected and used in combination. The hydrophilicity and lipophilicity of the surfactant are not particularly limited, but in the case of an oil-in-water (O / W type) type hairdressing composition, the HLB value of the surfactant is 8 to 20, preferably 9. When it is ~ 18, the micelle is stable and preferable. The HLB value is obtained by a calculation formula of HLB value = 20 × (mass% of hydrophilic group) based on the formula weight and molecular weight of the hydrophilic group according to the Griffin method.

As the surfactant, polyoxyethylene sorbitan oleate (polysorbate 80), cetyltrimethylammonium chloride, stearyltrimethylammonium chloride, polyoxyalkylene alkyl ether, polyglycerin fatty acid ester, imidazoline type, and fatty acid amide propyl betaine can be used. In particular, polyoxyethylene sorbitan oleate (polysorbate 80) is preferable from the viewpoint of obtaining an oil droplet (O / W) type emulsion in water and a wax type emulsion in water.

The hair styling composition of this embodiment may contain a surfactant in the range of 1.0 to 10% by mass, preferably 2.0 to 8% by mass, based on the total mass. If the concentration of the surfactant in the hair styling composition is less than 1.0% by mass, the hair styling composition is difficult to emulsify, and if it exceeds 10% by mass, the composition tends to be hydrophilic and the hair becomes cohesive. It may get worse.

(Cellulose fine fiber)
The hair styling composition containing cellulose fine fibers has improved viscosity and cohesiveness of hair, and has improved ease of washing off. Conventional hair styling composition imparts viscosity and cohesiveness to hair by the effect of an oil agent, but some of them are difficult to wash off. The hair styling composition of this embodiment contains cellulose fine fibers, so that it can be easily washed off, and of course, the viscosity and cohesiveness are also improved. The cellulose fine fibers used in this embodiment have a role of increasing the hydrogen bond points of the cellulose fibers and thereby improving the strength of the molded body. Cellulose fine fibers can be obtained by defibrating (miniaturizing) the raw material pulp, and can be produced by a known treatment method such as chemical treatment or mechanical treatment.

As raw material pulp for cellulose fine fiber, for example, wood pulp made from broadleaf tree, coniferous tree, etc., non-wood pulp made from straw, bagasse, cotton, hemp, carrot fiber, etc., recovered waste paper, waste paper, etc. are used as raw materials. One type or two or more types can be selected and used from the waste paper pulp (DIP) and the like. In addition, the above-mentioned various raw materials may be in the state of a crushed material called, for example, a cellulosic powder. In recent years, the demand for hair styling composition containing organic components has been increasing, and hardwoods derived from plants other than recycled paper and wood pulp made from coniferous trees are preferred, and hardwoods are preferable.

The wood pulp is, for example, one of broad-leaved kraft pulp (LKP), coniferous kraft pulp (NKP), sulfite pulp (SP), chemical pulp such as dissolving pulp (DP), and mechanical pulp (TMP). Two or more types can be selected and used. In particular, chemical pulps such as broadleaf kraft pulp (LKP) and coniferous kraft pulp (NKP), which are wood pulps that enhance the cellulose component, are preferable, and bleached pulps are used from the viewpoint of the color of the hairdressing composition. Broad-leaved bleached kraft pulp (LBKP) and coniferous bleached kraft pulp (NBKP) are suitable because they do not easily affect the color of the hairdressing composition.

Examples of the mechanical pulp include stone ground pulp (SGP), pressurized stone ground pulp (PGW), refiner ground pulp (RGP), chemi-grand pulp (CGP), thermo-grand pulp (TGP), and ground pulp (GP). One or more of the thermomechanical pulp (TMP), chemithermomechanical pulp (CTMP), refiner mechanical pulp (RMP), bleached thermomechanical pulp (BTMP) and the like can be selected and used.

Prior to the defibration of cellulose fine fibers, it can also be pretreated by a chemical method. Pretreatment by chemical method includes, for example, hydrolysis of polysaccharide with acid (acid treatment), hydrolysis of polysaccharide with enzyme (enzyme treatment), swelling of polysaccharide with alkali (alkali treatment), oxidation of polysaccharide with oxidizing agent (acid treatment). (Oxidization treatment), reduction of polysaccharides with a reducing agent (reduction treatment), oxidation with a TEMPO catalyst (oxidation treatment), esterification with phosphoroxo acid (chemical treatment), and the like can be exemplified. Among the cellulose fine fibers, those that have been pretreated by a chemical method can be referred to as "modified cellulose fine fibers", and those that have not been pretreated by a chemical method can be referred to as "unmodified cellulose fine fibers". The modified cellulose fine fibers are, for example, those in which cellulose fibers of cellulose fine fibers are hydrolyzed (acid-treated) by acid treatment, those hydrolyzed by enzymes (enzyme treatment), and those in which polysaccharides are swollen by alkali. Examples thereof include those in which the hydroxy group of the cellulose fiber is esterified with a phosphoric acid, but the present invention is not limited thereto. When a part of the cellulose fine fibers contained in the hair styling composition of the present embodiment is the modified cellulose fine fibers, the remaining cellulose fine fibers can be said to be unmodified cellulose fine fibers. The blending ratio of the modified cellulose fine fiber and the unmodified cellulose fine fiber is not particularly limited, and is more preferably in the range of the mass of the modified cellulose fine fiber: the mass of the unmodified cellulose fine fiber = 100: 0 to 0: 100. It can be freely adjusted in the range of 80:20 to 20:80. By adjusting this blending ratio, the ease of stretching and the viscosity can be adjusted to a desired degree.

Homogeneity can be improved by subjecting to enzyme treatment, acid treatment, and oxidation treatment prior to defibration.

When the raw material pulp is subjected to enzyme treatment, acid treatment, or oxidation treatment, the hemicellulose and the amorphous region of cellulose contained in the pulp are decomposed, and as a result, the energy of the micronization treatment can be reduced, and the uniformity and dispersibility of the cellulose fiber can be improved. Can be improved. The dispersibility of the cellulose fibers contributes to, for example, improving the homogeneity of the hair styling composition. However, since the pretreatment reduces the aspect ratio of the cellulose fine fibers, it is preferable to avoid excessive pretreatment.

構造式（１）において、ａ，ｂ，ｍ，ｎは自然数である。
Ａ１，Ａ２，・・・，ＡｎおよびＡ’のうちの少なくとも１つはＯであり、残りはＲ、ＯＲ、ＮＨＲ、及び、なしのいずれかである。Ｒは、水素原子、飽和－直鎖状炭化水素基、飽和－分岐鎖状炭化水素基、飽和－環状炭化水素基、不飽和－直鎖状炭化水素基、不飽和－分岐鎖状炭化水素基、芳香族基、及びこれらの誘導基のいずれかである。αは有機物又は無機物からなる陽イオンである。このセルロース微細繊維は光透過度及び粘度が極めて高いものである。 Esterification (chemical treatment) with phosphoroxo acid is performed prior to defibration to make the fiber raw material finer, and the cellulose fine fibers produced have a large aspect ratio, excellent strength, and high light transmittance and viscosity. It becomes. Esterification with a phosphorus oxo acid can be carried out by the method described in Patent Document (Japanese Unexamined Patent Publication No. 2019-199671). The following is an example of cellulose fine fibers in which the hydroxy group of the cellulose fiber is esterified with phosphoric acid. A part of the hydroxy group of the cellulose fiber is substituted with the functional group represented by the following structural formula (1) and esterified with phosphoroxoic acid, and the amount of the functional group introduced in the structural formula (1) is 1 g of the cellulose fiber. Examples of cellulose fine fibers exceeding 2 mmоl per unit can be exemplified.
[Structural formula (1)]

In the structural formula (1), a, b, m, and n are natural numbers.
At least one of A1, A2, ..., An and A'is O, and the rest is either R, OR, NHR, and none. R is a hydrogen atom, a saturated-linear hydrocarbon group, a saturated-branched chain hydrocarbon group, a saturated-cyclic hydrocarbon group, an unsaturated-linear hydrocarbon group, an unsaturated-branched chain hydrocarbon group. , Aromatic groups, and any of these inducing groups. α is a cation composed of an organic substance or an inorganic substance. These cellulose fine fibers have extremely high light transmittance and viscosity.

The esterification reaction with phosphoric acid proceeds by adding a solution having a pH of less than 3.0 consisting of an additive containing at least one of a phosphoric acid and a phosphoric acid metal salt to the cellulose fiber, heating the fiber, and defibrating the fiber. do.

Examples of additives include phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, triammonium phosphate, ammonium pyrophosphate, ammonium polyphosphate, lithium dihydrogen phosphate, trilithium trilithium phosphate, and dihydrogen phosphate. Lithium, lithium pyrophosphate, lithium polyphosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, trisodium phosphate, sodium pyrophosphate, sodium polyphosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, triphosphate Potassium, potassium pyrophosphate, potassium polyphosphate, phosphite, sodium hydrogen phosphite, ammonium hydrogen phosphite, potassium hydrogen phosphite, sodium dihydrogen phosphite, sodium phosphite, lithium phosphite, sub Phosphoric acid compounds such as potassium phosphate, magnesium phosphite, calcium phosphite, triethyl phosphite, triphenyl phosphite, and pyrophosphoric acid can be used. Each of these additives can be used alone or in combination of two or more.

For defibration of raw pulp, for example, beaters, high-pressure homogenizers, homogenizers such as high-pressure homogenizers, stone mill type friction machines such as grinders and grinders, single-screw kneaders, multi-screw kneaders, kneader refiners, jet mills, etc. It can be done by beating the raw pulp using. However, it is preferable to use a refiner or a jet mill.

The raw pulp is defibrated so that the average fiber diameter, average fiber length, peak value of pseudo-particle size distribution, and B-type viscosity of the obtained cellulose fine fibers have the desired values or evaluations as shown below. preferable.

The average fiber diameter (average fiber width; average diameter of single fibers) of the cellulose fine fibers is preferably 100 nm or less. When the average fiber diameter of the cellulose fine fibers is in this range, the cellulose fine fibers are less likely to be entangled with each other and are dispersed, so that the hair styling composition is easily stretched and easily applied to the hair. Further, when the cellulose fine fibers having an average fiber diameter of 100 nm or less are attached to the hair, the cellulose fine fibers are relatively thin, so that it is difficult to notice that the cellulose fine fibers are attached even when the hair is viewed. .. The average fiber diameter of the cellulose fine fibers is preferably 1 to 100 nm, more preferably 2 to 90 nm, and particularly preferably 3 to 80 nm. In particular, when the average fiber diameter of the cellulose fine fibers is 1 nm or more, the fluidity of the hair styling composition is further improved, and a three-dimensional network structure between the cellulose fine fibers is easily formed. Gives and gives a natural look. If the average fiber diameter of the cellulose fine fibers exceeds 100 nm, the effect of increasing the hydrogen bond points may not be obtained, and the fibers derived from the cellulose fine fibers appear to be attached to the hair. It is more likely to give the impression that foreign matter is attached to the hair.

The average fiber diameter of the cellulose fine fibers can be adjusted by, for example, selection of raw material pulp, pretreatment, defibration and the like.

In particular, when the average fiber diameter of the cellulose fine fibers defibrated by esterification with the above-mentioned phosphorus oxo acid is within the above range, the produced cellulose fine fibers have high light transmittance. The hair styling composition containing the cellulose fine fibers is preferable because it exhibits a color tone close to the color tone of the composition contained in addition to the cellulose fine fibers. When the composition other than the cellulose fine fibers in the hair styling composition is composed of a transparent material, the color tone of the entire hair styling composition is transparent or close to transparent. Hair coated with the hair styling composition is preferable because it exhibits the original color tone of the hair. When cellulose fine fibers that have not been esterified with phosphoric acid are dispersed in purified water to prepare a dispersion liquid, the dispersion liquid exhibits a whitish color tone. However, when the cellulose fine fibers esterified with phosphorus oxo acid and defibrated are dispersed in purified water to prepare a dispersion liquid, the color tone of this dispersion liquid exhibits the color tone of the purified water itself.

The method for measuring the average fiber diameter of the cellulose fine fibers is as follows.
First, 100 ml of an aqueous dispersion of cellulose fine fibers having a solid content concentration of 0.01 to 0.1% by mass is filtered through a membrane filter made of Teflon (registered trademark), and the solvent is once with 100 ml of ethanol and three times with 20 ml of t-butanol. Replace. Next, it is freeze-dried and coated with osmium to prepare a sample. This sample is observed with an electron microscope SEM image at a magnification of 3,000 to 30,000 times depending on the width of the constituent fibers. Specifically, two diagonal lines are drawn on the observation image, and three straight lines passing through the intersections of the diagonal lines are arbitrarily drawn. Further, the width of a total of 100 fibers intersecting with these three straight lines is visually measured. Then, the median diameter of the measured value is taken as the average fiber diameter.

The average fiber length (length of the single fiber) of the cellulose fine fibers is preferably 0.01 to 1000 μm, more preferably 0.1 to 500 μm, and particularly preferably 3 to 300 μm. When the average fiber length of the cellulose fine fibers is less than 0.01 μm, it becomes difficult to form a network structure of the fibers, and as a result, the hair becomes insufficiently firm and firm. On the other hand, when the average fiber length of the cellulose fine fibers exceeds 1000 μm, the cellulose fine fibers aggregate with each other to form an agglomerate, which increases the possibility of giving the impression that foreign matter is attached to the hair.

The average fiber length of the cellulose fine fibers can be adjusted by, for example, selection of raw material pulp, pretreatment, defibration and the like.

The method for measuring the average fiber length of the cellulose fine fibers is the same as in the case of the average fiber diameter, and the length of each fiber is visually measured. The average fiber length is the medium length of the measured value.

The axial ratio (fiber length / fiber width) of the cellulose fine fibers is preferably 10 to 1000000, more preferably 20 to 500,000, and particularly preferably 30 to 100,000. When the axial ratio is less than 10, the cellulose content is substantially in the form of particles, and the viscosity and cohesiveness produced by the formation of the fiber network are poor. On the other hand, when the axial ratio exceeds 1,000,000, aggregation of fibers is likely to occur, which leads to inhibition of cellulose network formation, and aggregates of cellulose fine fibers adhering to hair are easily recognized as foreign substances.

The crystallinity of the cellulose fine fibers is 50 to 100, more preferably 60 to 90, and particularly preferably 65 to 85. If the crystallinity is less than 50, the hair may not be well organized.

The crystallinity is a value measured by an X-ray diffraction method in accordance with the "general rule of X-ray diffraction analysis" of JIS-K0131 (1996). The cellulose fine fiber has an amorphous portion and a crystalline portion, and the crystallinity means the ratio of the crystalline portion to the entire cellulose fine fiber.

The light transmittance (solid content standard 0.2% aqueous dispersion) of the cellulose fine fibers is preferably 40% or more, more preferably 60% or more, and particularly preferably 70% or more. If the light transmittance is less than 40%, the color tone of the composition other than the cellulose fine fibers in the hair styling composition is concealed. In particular, a wax-like hair styling composition that requires transparency is not preferable because it may hinder glossing. However, in the case of a hair styling composition that brings about a natural texture such as a matte tone, the light transmittance of the cellulose fine fibers is not particularly limited.

The light transmittance is a value obtained by measuring the transparency (transmittance of 350 to 880 nm light) of a 0.2% (w / v) cellulose fine fiber aqueous dispersion using a Spectrophotometer U-2910 (Hitachi, Ltd.). The dispersion medium is purified water.

The peak value in the pseudo particle size distribution curve of the cellulose fine fibers is preferably one peak. In the case of one peak, the cellulose fine fibers have high uniformity in fiber length and fiber diameter, and the dispersibility of the cellulose fine fibers contained in the hair styling composition is good. Further, with the dispersion of the cellulose fine fibers, the components other than the cellulose fine fibers in the hair styling composition, for example, the oil agent are also sufficiently dispersed.

The peak value in the pseudo particle size distribution curve of the cellulose fine fiber is measured according to ISO-13320 (2009). More specifically, a volume-based particle size distribution of cellulose fine fibers in an aqueous dispersion is investigated using a particle size distribution measuring device (a laser diffraction / scattering type particle size distribution measuring device manufactured by Seishin Enterprise Co., Ltd.). Then, the mode of the cellulose fine fibers is measured from this distribution. This mode is used as the peak value. Cellulose fine fibers preferably have a single peak in the pseudo-particle size distribution curve measured by laser diffraction in an aqueous dispersion. As described above, the cellulose fine fiber having one peak has been sufficiently finely divided, can exhibit good physical properties as the cellulose fine fiber, and the obtained hair styling composition is homogenized, which is preferable. .. The peak value of the pseudo particle size distribution of the particle size of the cellulose fine fibers that becomes the single peak is, for example, preferably 300 μm or less, more preferably 200 μm or less, and particularly preferably 100 μm or less. .. If the peak value exceeds 300 μm, the fibers are large, which may give the impression that foreign matter has adhered to the hair.

The peak value in the particle size of the cellulose fine fibers and the median diameter of the pseudo particle size distribution can be adjusted by, for example, selection of raw material pulp, pretreatment, defibration and the like.

The cellulose fine fibers obtained by defibration can be dispersed in an aqueous dispersion medium to prepare a dispersion liquid prior to preparing a hair styling composition. It is particularly preferable that the total amount of the aqueous dispersion medium is water. However, the aqueous dispersion medium may be another liquid that is partially compatible with water. As the other dispersion medium, for example, lower alcohols having 3 or less carbon atoms can be used.

In the hair styling composition containing cellulose fine fibers and an oil agent, it is presumed that the oil agent adheres to the cellulose fine fibers or stays in the voids formed by the three-dimensional network of the cellulose fine fibers. .. When the cellulose fine fibers are appropriately dispersed in the hair styling composition, the dispersibility of the oil agent becomes excellent.

(Viscosity, etc.)
When the concentration of the cellulose fine fibers is 1% by mass (w / w), the B-type viscosity of the dispersion is preferably 10 to 300,000 cP, more preferably 100 to 100,000 cP. If the B-type viscosity is less than 10 cP, the viscosity is too low, and when the hair styling composition is applied to the hair, the hair styling composition separated on the palm or the like may drip. On the other hand, when the B-type viscosity exceeds 300,000 cP, the dispersibility of the cellulose fine fibers in the hair styling composition is lowered.

In some conventional hair styling composition, a thickener is added in order to improve the viscosity. However, since the cellulose fine fibers themselves have a viscosity in the hair styling composition of the present embodiment, the hair styling composition has a sufficient viscosity even if the thickener is reduced or not added.

(Mixing ratio)
The blending ratio of the cellulose fine fibers contained in the hair styling composition is not particularly limited, but is preferably 0.1% by mass or more, more preferably 0.3% by mass or more, still more preferably 0. It is preferably 5% by mass or more. When the blending ratio of the cellulose fine fibers in the hair styling composition is 0.1% by mass or more, the cellulose fine fibers are well dispersed in the hair styling composition, and the hair styling composition has a desired viscosity.

In the hair styling composition of the present invention, since each composition is sufficiently dispersed together with the cellulose fine fibers, when a thickener is provided, uneven coating occurs even if the concentration of the thickener is relatively low. It will be difficult to do. Further, since the cellulose fine fibers and the oil agent are dispersed, the hair can be arranged into a desired shape by using a smaller amount than the coating amount used in the conventional product. Therefore, the amount of the hair styling composition used at one time can be suppressed, which is economical.

Since the hair styling composition of this embodiment contains cellulose fine fibers, it has a viscosity, is excellent in setting power of hair, and maintains the morphology of set hair. In addition, the hair styling composition of this embodiment is easy to wash off. Further, due to the excellent tensile elastic modulus of the cellulose fine fibers, the hair to which the hair styling composition is attached is reinforced, and firmness and elasticity can be obtained.

In addition to the above, preservatives, dispersion stabilizers, neutralizers, fragrances and the like can be added to the hair styling composition of this embodiment.

Examples of the preservative include hydroxybenzoic acid esters such as methylparaben, ethylparaben, propylparaben and butylparaben, 2-phenoxyethanol, 1,2-pentanediol, 1,2-hexanediol, 1,2-octanediol and the like. , 2-Alcandiols, Alkylglyceryl ethers such as 2-ethylhexyl glyceryl ethers, Salicylic acid, Sodium benzoate, Methylchloroisothiazolinone, Methylisothiazolinone, etc., Imidazolinium urea, Dehydroacetic acid, Phenols, Triclosan, Acid amides, quaternary ammonium salts, trichlorocarbanide, zincpyrythion, benzalkonium chloride, benzethonium chloride, sorbic acid, chlorhexidine, chlorhexidine gluconate, halocarban, hexachlorophen, hinokithiol, phenol, isopropylphenol, cresol, timol, para Examples thereof include chlorophenol, phenylphenol, sodium phenylphenol, phenylethyl alcohol and the like. From the viewpoint of imparting antiseptic properties, it is preferable to use 2-phenoxyethanol, 1,2-pentanediol, 1,2-hexanediol, 1,2-octanediol, and 2-ethylhexyl glyceryl ether. Further, from the viewpoint of not reducing the dispersibility of the cellulose fine fibers, those having polarity are preferable, and for example, 2-phenoxyethanol is preferable.

Dispersion stabilizers include guar gum, locust bean gum, queens seed, carrageenan, galactan, arabic gum, tara gum, tamarind, farseleran, karaya gum, trolley aoi, mannan, rice, corn, potato, wheat, xanthan gum, dextran, succinoglucan. , Curdran, hyaluronic acid, zansan gum, purulan, gellan gum, chitin, chitosan, agar, casso extract, chondroitin sulfate, casein, collagen, gelatin, albumin, soluble starch, methyl hydroxypropyl starch, methyl starch, hydroxypropyltrimonium chloride starch. , Sodium alginate, propylene glycol alginate, polyvinylpyridone, polyvinyl alcohol, vinylpyridone / vinylalcohol copolymer, polyvinylmethyl ether, polyethylene glycol, polypropylene glycol, polyoxyethylene / polyoxypropylene copolymer, methacryloyloxyethylcarboxybetaine / Alkyl methacrylate copolymer, Acrylate / Stearyl acrylate / Ethylamine methacrylate oxide copolymer, Dimethicon / Vinyl dimethicon crosspolymer, Acrylic acid / Alkyl acrylate (C10-30) copolymer, Alkyl acrylate / Diacetoneacrylamide copolymer, Alkyl acrylate / Diacetone acrylamide copolymer AMP, polyvinyl acetate partially saponified product, maleic acid copolymer, vinylpyrrolidone / dialkylaminoalkyl methacrylate copolymer, acrylic resin alkanolamine, polyester, water-dispersible polyester, polyacrylamide, polyacrylic acid Ethyl, carboxyvinyl polymer, acrylic acid / methacrylic acid ester copolymer, acrylic acid / alkyl methacrylic acid copolymer, acrylic acid / cationized methacrylic acid ester copolymer, choline chloride methacrylic acid ester polymer, cation Preferables include modified oligosaccharides, cationized dextran, guarhydroxypropyltrimonium chloride, polyethyleneimine, and cationic polymers. In particular, an acrylic acid / alkyl acrylate (C10-30) copolymer is more preferable as it does not impair the dispersion stability of the cellulose fine fibers.

As fragrances, eucalyptus extract, acetylsedrene, isoe super, isobutylquinoline, iris oil, iron, indole, ylang ylang oil, undecanal, undecenal, γ-undecalactone, estragor, eugenol, oak moss, opoponax Resinoids, orange oil, eugenol, auranthial, galactosolid, cannon, carrot seed oil, clove oil, methyl silicate, geraniol, dimethylbenzyl carvinyl acetate, styralyl acetate, sedrill acetate, telepinel acetate, p-t-butyl acetate Cyclohexyl, vetiberyl acetate, benzyl acetate, linalyl acetate, isopentyl salicylate, cyclopentadecanolide, methyl dihydrojasmonate, dihydromilsenol, jasmine absolute, jasmine lactone, cis-jasmon, citral, citronenol, citronellal, cinnamon bark oil, Cedarwood oil, sedren, sedrol, celery seed oil, thyme oil, damascon, damasenone, timole, tuberose absolute, decanal, hydroxycitroneral, α-pinene, piperitone, phenethyl alcohol, phenylacetaldehyde, petitgrain oil, hexylcinnamaldehyde, peppermint Oil, pepper oil, heliotropin, bergamot oil, benzylbenzoate, borneol, milresinoid, muskketone, methylnonylacetaldehyde, γ-methylyonone, menthol, lavender oil, D-limonen, linalol, linal, lilial, lemon oil, rose absolute, Rose oxide, rose oil and rosemary oil are preferred.

In order to keep the hair styling composition neutral, a neutralizing agent can be included in the composition of the hair styling composition, and examples of the neutralizing agent include triethanolamine.

(Example of manufacturing method of hair styling composition)
The hair styling composition of this embodiment can be produced, for example, as follows. (1) Oil agent homogenization step: The oil agent is made into a liquid having a uniform concentration while keeping the temperature at 70 to 90 degrees. (2) Mixing step: A surfactant and cellulose fine fibers having an average fiber diameter of 100 nm or less are mixed with the homogenized oil to obtain a mixture. (3) Emulsification step: An aqueous medium is mixed with the mixture obtained in the mixing step and emulsified to obtain an emulsion. (4) The obtained emulsion is used as a hair styling composition. In addition to this, the hair styling composition can be produced by the method shown below.
<Manufacturing process 1>
An example of the method for producing the hair styling composition of this embodiment is shown below. The method for producing the hair styling composition is not limited to this. (1) Put the oil in a heat-resistant container, keep the temperature at 70 to 90 degrees, and stir so that the concentration becomes uniform. (2) After that, while maintaining the temperature, an emulsifier and cellulose fine fibers are further added to the heat-resistant container, and the mixture is stirred so that the concentration of the contents becomes uniform. The cellulose fine fibers to be added may be only modified cellulose fine fibers, only unmodified cellulose fine fibers, or both modified cellulose fine fibers and unmodified cellulose fine fibers. When the cellulose fine fiber to be added contains modified cellulose fine fiber, it is better to lengthen the stirring time as compared with the case where only the unmodified cellulose fine fiber is added. The modified cellulose fine fibers may form flocs when they are initially added to a heat-resistant container, and are uniformly dispersed by sufficient stirring. This stirring operation is the same in the following manufacturing step 2. (3) Then, while maintaining the temperature, an aqueous medium is further added to the heat-resistant container, and the mixture is stirred so that the concentration of the contents becomes uniform. (4) After that, the contents of the heat-resistant container are allowed to cool to room temperature to obtain a hair styling composition. The room temperature is not particularly limited, but refers to, for example, 5 to 35 degrees.

<Manufacturing process 2>
Another example of the method for producing the hair styling composition of this embodiment is shown below. (1) Put the oil in a heat-resistant container, keep the temperature at 70 to 90 degrees, and stir so that the concentration becomes uniform. (2) After that, while maintaining the temperature, a liquid oil component is further added to the heat-resistant container, and the mixture is stirred so that the concentration of the contents becomes uniform. (3) After that, while maintaining the temperature, an emulsifier and cellulose fine fibers are further added to the heat-resistant container, and the mixture is stirred so that the concentration of the contents becomes uniform. (4) After that, while maintaining the temperature, a preservative and a fragrance are further added to the heat-resistant container, and the mixture is stirred so that the concentration of the contents becomes uniform. (4) Then, while maintaining the temperature, a neutralizing agent, a dispersion stabilizer, and an aqueous medium are further added to the heat-resistant container, and the mixture is stirred so that the concentration of the contents becomes uniform. (5) After that, the contents of the heat-resistant container are allowed to cool to room temperature to obtain a hair styling composition. The room temperature is not particularly limited, but refers to, for example, 5 to 35 degrees.

The hair styling composition of the present invention can be provided in a known state, but an emulsified one is preferable, and for example, it can be provided in the form of cream, paste, wax or the like.

The reagents and the like used to produce Test Examples 1 to 5 and Reference Example 6 were unmodified cellulose fine fibers (ELLEX-S (2% by mass) manufactured by Daio Paper Industries, Ltd., derived from broadleaf tree, ("Unmodified CNF"). Also referred to as))), modified cellulose fine fiber (ELLEX- ☆ (star) (1% by mass) manufactured by Daio Paper Industries, Ltd., derived from broadleaf tree, (also referred to as "modified CNF")), sodium carboxymethyl cellulose (CMC-Na, Daicel) Finechem Co., Ltd. Part No. 1330), Acrylic Acid / Alkyl Acrylate (C10-30) Copolymer (AQPEC HV-803ERK (CT-1) manufactured by Sumitomo Seika Co., Ltd.), Candelilla Row (manufactured by Natural Cosmetics Research Institute), Mitsurou (manufactured by Natural Cosmetics Research Institute), liquid paraffin (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.), ethylhexyl palmitate (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.), 2-ethylhexyl palmitate (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) (Manufactured by Co., Ltd.), Polysorbate 80 (manufactured by Cafe de Savon), 2-Phenoxyethanol (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.), Triethanolamine (manufactured by Hayashi Junyaku Kogyo Co., Ltd., 20 W / V%, (also "TEA") )), Perfume (manufactured by Ryohin Keikaku Co., Ltd., MUJI Essential Oil Eucalyptus 30 ml), and purified water.

Test Examples 1 to 5 and Reference Example 6 were manufactured as follows. Candelilla wax and beeswax were placed in a beaker, kept at a temperature of 80 ° C. in a water bath, and melted while stirring so that the concentration became uniform. Then, while keeping the temperature at 80 ° C., liquid paraffin and ethylhexyl palmitate were further added, and the mixture was stirred so that the concentration became uniform. Then, while keeping the temperature at 80 ° C., polysorbate 80 and one or more of unmodified cellulose fine fibers, modified cellulose fine fibers, and sodium carboxymethyl cellulose were further added, and the mixture was stirred so that the concentration became uniform. .. Then, while keeping the temperature at 80 ° C., phenoxyethanol and a fragrance were further added, and the mixture was stirred so that the concentration became uniform. Then, while keeping the temperature at 80 ° C., acrylic acid / alkyl acrylate (C10-30) copolymer, triethanolamine, and purified water were further added, and the mixture was stirred so that the concentration became uniform. After that, the beaker was taken out of the water bath and allowed to cool to room temperature.

The modified cellulose fine fiber (ELLEX® (registered trademark)-☆ (star) (1% by mass) manufactured by Daio Paper Corporation is a dispersion liquid, and the modified cellulose fine fiber may form flocs while being dispersed in the dispersion liquid. , To make the concentration uniform by adding to the beaker, it is advisable to stir sufficiently. The time to add and stir the cellulose fine fibers is the modified cellulose fine fibers (ELLEX® (registered trademark) manufactured by Daio Paper Corporation)-☆ (Star). ) (1% by mass) may be longer than the case of adding only the unmodified cellulose fine fiber (ELLEX (registered trademark) -S (2% by mass) manufactured by Daio Paper Corporation).

The compositions of Test Examples 1 to 5 and Reference Example 6 are as shown in Table 1. The concentrations of unmodified cellulose fine fibers and modified cellulose fine fibers are based on solid matter.

Ten subjects were asked to apply Test Examples 1 to 5 and Reference Example 6 to their hair, and to evaluate the following evaluation items. The evaluation items are viscosity, ease of stretching, ease of cohesion, gloss, and ease of washing off. All of Test Example 1 to Test Example 5 and Reference Example 6 were sufficiently emulsified, and separation into water and oil did not occur.

The evaluation method is as follows. First, the subject whose hair was dry applied Reference Example 6 to the hair and left it for about 8 hours, washed it off completely, and then completely dried the hair.

Next, the subject applied each of Test Example 1 to Test Example 5 to the hair and left it for the same time, washed it off completely, and then completely dried the hair. Then, with respect to the above evaluation items, whether or not the selected test example was compared with the reference example 6 was evaluated on a five-point scale.
The subjects evaluated the viscosity as 3 when the test example did not change as compared with the reference example 6, 5 when the test example felt high, and 1 when the test example felt insufficient and watery.
Regarding the ease of stretching, compared to Reference Example 6, if the test example does not change the stretchability when applied to the hair, it is 3, if it feels easy to stretch, 5 if it feels difficult to stretch, and if it feels difficult to stretch. The subject was evaluated as 1.
The subjects evaluated the ease of cohesion as 3 if the test example did not change compared to Reference Example 6, 5 if the hair felt easy to cohes, and 1 if the hair felt difficult to cohes. ..
The subjects evaluated the gloss as 3 when the test example did not change as compared with the reference example 6, 5 when the gloss was felt to be strong, and 1 when the gloss was felt to be weak.
Regarding the ease of washing off, the subjects evaluated it as 3 if the test example did not change compared to Reference Example 6, 5 if it felt easy to wash off the hair styling composition, and 1 if it felt difficult to wash off. did.
The above evaluation was performed on Test Examples 1 to 5. Table 2 shows the average value (rounded to the first decimal place) obtained by averaging the evaluation points (1 to 5 points) evaluated by 10 persons for each evaluation item of Test Example 1 to Test Example 5. Indicated.

Considering the remarkable results, Test Example 1 to Test Example 4 were evaluated higher than Reference Example 6 in terms of viscosity and ease of cohesion. Regarding the ease of washing off, Test Examples 1 to 4 were evaluated as equal to or higher than those of Reference Example 6.

(others)
The B-type viscosity of the hair styling composition is a value measured in accordance with JIS-Z8803 (2011) "Method for measuring liquid viscosity". The B-type viscosity is the resistance torque when the dispersion liquid is stirred, and the higher it is, the more energy is required for stirring. The measurement was performed at 25 ° C.
-Unless otherwise specified, JIS, TAPPI and other tests and measurement methods shown in the above specification are carried out at room temperature, particularly 25 ° C., at atmospheric pressure, especially at 1 atm.

The hair styling composition of the present invention can be used for hair.

Claims (8)

It has an oil agent and cellulose fine fibers with an average fiber diameter of 100 nm or less.
The oil agent is contained in an amount of 10% by mass or more.
A hair styling composition characterized by that. Of the 100 parts by mass of the oil agent, 50 parts by mass or more is wax.
The hair styling composition according to claim 1. Some of the cellulose fine fibers are obtained by esterifying the hydroxy group of the cellulose fiber with a phosphoric acid.
The hair styling composition according to claim 1 or 2. The cellulose fine fibers are contained in an amount of 0.1% by mass or more based on the solid content.
The hair styling composition according to any one of claims 1 to 3. The cellulose fine fibers are made from hardwood kraft pulp and / or softwood kraft pulp.
The hair styling composition according to any one of claims 1 to 4. There is one peak value in the pseudo particle size distribution curve of the cellulose fine fibers.
The hair styling composition according to any one of claims 1 to 5. An oil droplet (O / W) type emulsion in water,
The hair styling composition according to any one of the first to sixth aspects. An oil agent homogenization process that keeps the oil agent at 70 to 90 degrees Celsius and makes it a liquid with a uniform concentration.
A mixing step of mixing a surfactant and cellulose fine fibers having an average fiber diameter of 100 nm or less with a homogenized oil to obtain a mixture.
It has an emulsification step of mixing an aqueous medium with a mixture obtained in the mixing step and emulsifying the mixture to obtain an oil droplet (O / W) type emulsion in water.
A method for producing a hair styling composition.