KR102140541B1 - Liquid pigment colorant composition for artificial hair by modacrylic fiber and method for manufacturing the same - Google Patents

Abstract

Disclosed are a liquid organic and inorganic pigment colorant composition for artificial hair and a method for manufacturing the same. The method for manufacturing the liquid organic and inorganic pigment colorant composition for artificial hair comprises the steps of: a liquid polymer manufacturing step of manufacturing a liquid polymer serving as an anti-aggregation agent by dissolving modacrylic polymer powder in an organic solvent to prevent aggregation of pigment particles; a blending step of blending the liquid polymer, a pigment, a dispersant, and the organic solvent to manufacture a mixture; and a dispersion step of manufacturing a dispersion by dispersing after introducing the mixture into dispersion equipment. According to the present invention, it is possible to prevent water pollution and protect the environment.

Description

Liquid pigment colorant composition used in modacrylic for artificial hair and its manufacturing method{LIQUID PIGMENT COLORANT COMPOSITION FOR ARTIFICIAL HAIR BY MODACRYLIC FIBER AND METHOD FOR MANUFACTURING THE SAME}

The present disclosure relates to a liquid organic and inorganic pigment colorant composition used in modacrylic for artificial hair and a method for manufacturing the same.

Currently, artificial hair used in wigs is manufactured by processing synthetic resin fibers, and dyeing artificial hair using pigments so that artificial hair looks the same as human natural hair. In this regard, Korean Patent Registration No. 10-1515616 discloses a technique for dyeing artificial hair.

However, in the case of using dyes during dyeing of artificial hair, secondary wastewater is generated during processing of the fibers for artificial hair, which has a problem of causing water pollution. On the other hand, dimethyl sulfoxide, an organic solvent, usually freezes at 18°C or lower, so if dimethyl sulfoxide is included in the liquid oil and inorganic pigment colorant for artificial hair, dimethyl sulfoxide is produced during the production of liquid oil and inorganic pigment colorant for artificial hair during the spring and winter seasons. While the flowability and blackness of the colorant decreases as the freezes, and the process of mixing and spinning a resin for artificial hair and a liquid organic and inorganic pigment colorant increases the filter pressure, single yarn occurs, and the blackness of the colorant decreases. This falling issue existed.

In order to solve this problem, it is necessary to maintain the temperature of all pipes through which the liquid oil and inorganic pigment colorant for artificial hair is produced and the tank for storing the liquid oil and inorganic pigment colorant and all pipes through which the liquid oil and inorganic pigment colorant passes. In reality, the related facility cost and maintenance cost are high, so the productivity of the liquid oil and inorganic pigment colorant in spring and winter decreases, so the quality of the liquid oil and inorganic pigment colorant, radioactivity, and artificial hair within a range that does not adversely affect the resin for artificial hair There is a new need to develop a technology that facilitates production of liquid organic and inorganic pigment colorants.

The technical idea of the present disclosure is to solve the above-mentioned problems, and an object thereof is to provide a technique for developing a liquid organic and inorganic pigment colorant using an organic solvent as a solvent and containing a modacrylic polymer.

In addition, the technical idea of the present disclosure is another object to provide a technique capable of maintaining the quality of the liquid oil and inorganic pigment colorant composition for artificial hair even during the spring and winter seasons.

And, the technical idea of the present disclosure is another object to provide a technology that can reduce the facility cost and maintenance cost when manufacturing a liquid organic and inorganic pigment colorant composition for artificial hair.

The problem to be solved by the present invention is not limited to the above-described problems, and other technical problems not mentioned will be clearly understood by a person having ordinary knowledge in the technical field to which the present invention pertains from contents to be described later.

In order to achieve this object, as an embodiment of the present invention, a method of preparing a liquid oil and inorganic pigment colorant composition for artificial hair is a liquid acting as a flocculating agent by dissolving modacrylic polymer powder in an organic solvent to prevent agglomeration of the pigment particles. Liquid polymer manufacturing step for preparing a polymer; A blending step of mixing the liquid polymer, pigment, dispersant and organic solvent to prepare a stirred product; And a dispersing step of introducing and dispersing the stirring material into a dispersing equipment to prepare a dispersing material.

In addition, in the liquid polymer manufacturing step, the liquid polymer is a liquid polymer prepared by mixing 30% by weight of the modacrylic polymer powder and 70% by weight of dimethyl sulfoxide mixed with distilled water at 50-60° C. for 2-3 hours. Dimethyl sulfoxide mixed with distilled water may be prepared by mixing 3-4 wt% of distilled water and 96-97 wt% of dimethyl sulfoxide.

And, in the compounding step, the pigment is provided with carbon black, and the organic solvent is prepared by mixing 3 to 4% by weight of distilled water and the remainder of dimethyl sulfoxide, and the stirred material is 5 to 25 parts by weight of the liquid polymer, 5 to 10 parts by weight of pigment, 0.5 to 1.5 parts by weight of the dispersant and 25 to 40 parts by weight of the organic solvent, and in the dispersing step, the dispersing equipment is provided with a 3-roll mill, bead mill or basket mill, and the temperature of the dispersion during dispersion May be maintained at 20-40°C.

In addition, the method of preparing a liquid organic and inorganic pigment colorant composition for artificial hair includes a filling step of adding and stirring 1 to 5 parts by weight of an additional organic solvent to the dispersion; And an inspection step of adding 1 to 5 parts by weight of the additional organic solvent to the filler when the blackness measurement value of the filler filled in the filling step is less than a predetermined reference value; and further comprising: the additional organic solvent is dimethyl sulfoxide And acetone.

And, in the liquid polymer manufacturing step, the organic solvent may be provided at least one of dimethyl sulfoxide and acetone.

To achieve this object, as another embodiment of the present invention, the liquid oil and inorganic pigment colorant composition for artificial hair may be prepared by the method for preparing the liquid oil and inorganic pigment colorant composition for artificial hair described above.

The means for solving the above-described problems are merely exemplary and should not be construed as limiting the present invention. In addition to the exemplary embodiments described above, there may be additional embodiments described in the drawings and detailed description of the invention.

As described above, according to various embodiments of the present invention, an organic solvent such as dimethyl sulfoxide or acetone is used as a solvent, and the color of the original yarn is controlled by a liquid organic/inorganic pigment colorant composition containing a modacrylic polymer. , Since the use of dyes can be controlled selectively, it is possible to prevent water pollution caused by secondary wastewater and protect the environment by not using dyes or reducing the amount of dyes used in the process of realizing the color of the yarn for artificial hair.

In addition, by adding a certain amount of water to the dimethyl sulfoxide contained in the liquid oil and inorganic pigment colorant composition for artificial hair, the freezing point of dimethyl sulfoxide is lowered, and the liquid oil and inorganic pigment colorant for artificial hair is also used in a working environment of 7 to 8°C. It does not freeze, which has the effect of improving workability in spring and winter.

In addition, by setting the content of water added to dimethyl sulfoxide to a certain range, no trouble occurs with the modacrylic polymer contained in the liquid oil and inorganic pigment colorant for artificial hair, and to improve the flowability and blackness of the liquid oil and inorganic pigment colorant. Contribute.

In addition, as the modacrylic polymer using an organic solvent (for example, dimethyl sulfoxide, acetone, etc.) as a solvent is used as a flocculating agent, it prevents flocculation of pigment particles during dispersion and improves dispersibility. By specifying the solid content, there is an effect of excellent flowability and storage properties of the liquid oil and inorganic pigment colorant composition for artificial hair.

The effects of the present invention are not limited to the effects mentioned above, and other effects not mentioned will be clearly understood by those skilled in the art from the description of the claims.

1 is a flow chart showing a method of manufacturing a liquid oil and inorganic pigment colorant composition for artificial hair according to an embodiment of the present invention.
2 is a conceptual diagram schematically showing a stirrer used in the compounding step according to an embodiment of the present invention.

With reference to the accompanying drawings for a preferred embodiment of the present invention will be described in more detail, but for the brevity of description, the technical parts that have already been well-known will be omitted or compressed.

It should be noted that references herein to “one” or “one” embodiments of the present invention are not necessarily referring to the same embodiment, and they mean at least one. In addition, the present invention is not limited to artificial hair, and is not limited to a specific type of organic solvent.

In the following embodiments, the singular expressions include the plural expressions unless the context clearly indicates different meanings.

In the following embodiments, terms such as include or have mean that the features or components described in the specification exist, and do not preclude the possibility that one or more other features or components may be added.

When an embodiment can be implemented differently, a specific process order may be performed differently from the described order. For example, two processes described in succession may be performed substantially simultaneously, or may be performed in an order opposite to that described. That is, each step of the method described herein may be appropriately carried out in any order, unless otherwise stated on the specification or clearly contradicted by context.

A method of manufacturing a liquid oil and inorganic pigment colorant composition for artificial hair according to an embodiment of the present invention will be described in accordance with the flowchart shown in FIG. 1, but for convenience, it will be described in order.

1. Preparation step of aggregation inhibitor <S101>

In this step, a modacrylic polymer powder can be dissolved in an organic solvent to prepare a liquid polymer that acts as an aggregation inhibitor. In one embodiment, the liquid polymer prevents agglomeration of pigment particles during the dispersion step to be described later, and mixes 30% by weight of modacrylic polymer powder and 70% by weight of dimethyl sulfoxide mixed with distilled water at 50 to 60°C for 2 to 3 hours. Can be manufactured. If it is out of the above-described temperature range and time range, there is a fear that dissolution of the modacrylic polymer powder may not be smoothly performed, and the color of the liquid polymer may be reddish, so it is preferable to dissolve the modacrylic polymer within the aforementioned range. Do. In addition, in this specification, the modacrylic polymer powder is a copolymer of acrylonitrile and vinyl compound, and is obtained by copolymerizing 35 to 85% by weight of acrylonitrile and 15 to 65% by weight of vinyl chloride-based molecule or vinylidene chloride-based molecule. Means manufactured in the form.

In one embodiment, as an example of a commercially available modacrylic polymer powder, P2-3-204 (Taekwang Industry) may be used, but is not limited thereto.

In one embodiment, dimethyl sulfoxide, an organic solvent contained in the liquid polymer, is pre-mixed with distilled water, and dimethyl sulfoxide mixed with distilled water freezes at a temperature lower than the freezing point of pure dimethyl sulfoxide without water. Since dimethyl sulfoxide does not freeze even in a working environment of ~8°C, the quality and workability of the liquid oil and inorganic pigment colorant composition for artificial hair can be maintained at an excellent level.

In one embodiment, dimethyl sulfoxide mixed with distilled water may be prepared by mixing 3-4 wt% of distilled water and the balance of dimethyl sulfoxide (ie, 96-97 wt%). If the content of distilled water is less than 3% by weight and mixed with dimethyl sulfoxide, there is a concern that the quality and workability of the liquid oil and inorganic pigment colorant composition for artificial hair may deteriorate while dimethyl sulfoxide freezes during spring and winter, If the distilled water exceeds 4% by weight, the modacrylic polymer may be gelled while being entangled in water, so it is preferable that distilled water and dimethyl sulfoxide are mixed within the above-described content range.

In addition, when the modacrylic polymer is dissolved in dimethyl sulfoxide in this step, the addition of distilled water causes gelation of the modacrylic polymer and inhibits the dispersibility and flowability of the liquid organic and inorganic pigment colorant composition for artificial hair, thereby improving the blackness and overall quality. Since there is a fear of dropping, it is preferable to add modacrylic polymer powder in a state in which distilled water is premixed with dimethyl sulfoxide.

2. Mixing step <S102>

In this step, a liquid polymer, a pigment, a dispersant, and an organic solvent may be blended to prepare a stirred product. 2 is a conceptual diagram schematically showing a stirrer used in the compounding step according to an embodiment of the present invention. Referring to FIG. 2, the agitator 10 may include a housing 100, a motor 200, a first container 300, and a second container 400. The housing 100 has an inner space in which agitation is performed, and a discharge pipe 130 may be installed on one side of the housing 100 so that the agitated substance with stirring is discharged to the outside of the housing 100. The stator 110 is fixed to the inner circumferential surface of the housing 100, and the rotor 120 may be installed inside the stator 110. The rotor 120 may be coupled to the drive shaft 210 of the motor 200 to rotate in one direction when the drive shaft 210 is rotated. The motor 200 is connected to the drive shaft 210 and may provide power for the drive shaft 210 to rotate. The first container 300 is connected to the housing 100 through the first pipe 310, and the second container 400 is connected to the housing 100 through the second pipe 410.

Specifically, in this step, the liquid polymer, the dispersant, and the organic solvent are introduced into the first container 300, the pigment is introduced into the second container 400, and the motor 200 is operated to rotate the drive shaft 210 when the drive shaft 210 rotates. As the rotor 120 connected to the 210 rotates at a constant speed, shear force due to rotation occurs. That is, since a certain gap is formed between the stator 110 and the rotor 120, and a shear force is generated by rotation of the rotor 120, the agitated material passes through the gap formed between the stator 110 and the rotor 120. It can be stirred uniformly.

In addition, since the suction force is generated from each container (300, 400) toward the housing (100) by the high-speed rotation of the rotor (120), the contents introduced into the first container (300) and the contents introduced into the second container (400) are Each of the first pipe 310 and the second pipe 410 may be introduced into the housing 100. Therefore, when the pigment (eg, carbon black) composed of nanometer-scale fine powders is blended, it is possible to prevent the pigment from being scattered in the air and contaminating the work area or deteriorating workability, and when stirring, the rotor 120 ), the dispersion effect of the blend can be obtained above a certain level by high-speed rotation.

In addition, the liquid polymer serving as an anti-agglomeration agent in this step may be added in an amount of 5 to 25 parts by weight. When the content of the anti-agglomeration agent is less than 5 parts by weight, the amount of modacrylic polymer is insufficient to prevent aggregation of pigment particles during dispersion, and when the anti-aggregation agent exceeds 25 parts by weight, gelation occurs over time, and for modacrylic Since there is a problem that the storage property of the liquid organic and inorganic pigment colorant composition is lowered, the content of the liquid polymer is preferably applied within the aforementioned range.

In one embodiment, the pigment may include at least one of organic pigments and inorganic pigments. In one embodiment, the pigment is provided with carbon black, and examples of commercially available carbon black may include, but are not limited to, Mitsubishi Chemical's OIL7B or OIL31B.

In this step, the pigment may be applied in 5 to 10 parts by weight. If the content of the carbon black as a pigment is less than 5 parts by weight, the blackness of the liquid organic and inorganic pigment colorant composition for modacrylic acid is lowered, and when the pigment exceeds 10 parts by weight, aggregation of the pigment particles occurs and the entire pigment composition There is a possibility that the flowability and dispersibility decrease.

In one embodiment, the dispersant may be applied as an acid value dispersant, an amine value dispersant, or a dispersant having an acid value and an amine value at the same time. Examples of commercially available dispersants include, but are not limited to, BYK-Chemie's Disperbyk-180, Byk-9077, and the like.

In this step, the dispersant may be applied in 0.5 to 1.5 parts by weight. If the content of the dispersant is less than 0.5 parts by weight, the dispersibility decreases, and if it exceeds 1.5 parts by weight, it is preferable that the content of the dispersant is applied within the above-mentioned range because there is a possibility of trouble with the modacrylic polymer.

In addition, the organic solvent blended with the liquid polymer, the pigment, and the dispersant in this step may be prepared by mixing 3 to 4% by weight of distilled water and the remainder of dimethyl sulfoxide. The distilled water contained in the organic solvent lowers the freezing point of dimethyl sulfoxide, so the dimethyl sulfoxide does not freeze even in a working environment of 7 to 8°C, so the quality and workability of the liquid organic and inorganic pigment colorant composition for artificial hair can be maintained. If the content of distilled water in the organic solvent is less than 3% by weight, the quality and workability of the liquid oil and inorganic pigment colorant composition for artificial hair may decrease as the dimethyl sulfoxide freezes during spring and winter, and the distilled water content in the organic solvent is 4 If it exceeds weight%, the modacrylic polymer contained in the liquid polymer may gel while immersed in water.

And, in this step, the organic solvent (for example, dimethyl sulfoxide, acetone, etc.) can be applied in 25 to 40 parts by weight, but the content of the organic solvent (for example, dimethyl sulfoxide, acetone, etc.) changes the viscosity of the stirring material. It can be appropriately set in consideration.

3. Dispersion step <S103>

In this step, the dispersion may be prepared by adding and dispersing the stirred material in the dispersion equipment. In this step, the dispersing equipment may be provided as a 3-roll mill, bead mill or basket mill (eg, ring mill, rotary mill). Here, the three-roll mill is a device for homogenizing by passing the stirring material through a fine gap formed between the three rollers placed horizontally, and the draw-in roller, the middle roller, and the scraper roller adjacent to each other rotate simultaneously to the stirring material passing through the roller. Pressure and shear forces are applied. And, the basket mill (for example, the rotation mill) is a device for dispersing the compound while rotating the basket in the reverse direction and the direction of rotation of the dispersion blade installed inside the cylindrical basket, wherein the compound introduced into the basket is a basket and a dispersion blade Dispersion can be achieved quickly by rotation.

As a specific example, when dispersion is performed with a 3-roll mill, the particle size of the dispersion can be maintained at 350 nm or less by dispersing the dispersion into a 3-roll mill at least 6 times, and when dispersing with a basket mill, the rotational speed of the shaft connected to the dispersion blade inside the basket is adjusted. The particle size of the dispersion can be maintained at 350 nm or less by maintaining at 500 to 800 rpm and controlling the dispersion time to 8 to 10 hours.

And, the temperature of the dispersion can be maintained at 20 ~ 40 ℃ when dispersed in the dispersion equipment. If, when dispersing, the temperature of the dispersion exceeds 40°C, there is a concern that the blackness of the liquid oil and inorganic pigment colorant composition for artificial hair may decrease, and the use of cooling water increases rapidly and the dispersibility decreases to maintain the temperature below 20°C. When dispersing, it is desirable to keep the temperature of the dispersion within the aforementioned range.

4. Filling step <S104>

In this step, an organic solvent may be additionally added to the dispersion having been completely dispersed and stirred. In one embodiment, the additional organic solvent is the same organic solvent as the organic solvent used in step S102 and can be applied as a residual organic solvent. In this step, 1 to 5 parts by weight of the organic solvent may be added to the dispersion to form a filler.

5. Inspection step <S105>

In this step, when the blackness measurement value (eg, brightness value L) of the filling measured by the color difference meter is less than a predetermined reference value (for example, 26), 1-5 parts by weight of additional organic solvent is added to the dispersion. The blackness of the liquid organic and inorganic pigment colorant composition for artificial hair can be adjusted.

6. Filtering and conveying steps <S106>

In this step, the product that has been filled is passed through a filter having a certain particle size to remove defoaming of the product and foreign substances and finely dispersed pigments that may be present in the product, and to store the filtered liquid oil and inorganic pigment colorant composition for artificial hair that has been filtered. Can be transferred to. In addition, according to the implementation, in this step, it is also possible to filter while the product having been filled is sequentially passed through a plurality of filters having different particle sizes.

Hereinafter, the present invention will be described in more detail through specific examples. The following examples are merely examples for helping the understanding of the present invention, so the scope of the present invention is not limited or limited thereto.

1. Experiment of whether dimethyl sulfoxide mixed with water has a freezing point drop

Put the formulation made by mixing each component with the content (unit: g) listed in Table 1 below into a constant temperature chamber, lower the temperature by 1 °C from 25 °C, check the temperature at which ice crystals are generated in the formulation, and then ice at 7 °C or higher. When crystals were formed, it was evaluated that the freezing point was poor or not, and if ice crystals were formed at a temperature below 7°C, the freezing point was satisfactory. In Table 1 below, DMSO is dimethyl sulfoxide.

Experimental Example 1 Experimental Example 2 Experimental Example 3 Experimental Example 4 Distilled water 3 4 2 5 DMSO 97 96 98 95 Whether the freezing point drops Good Good Bad Good

2. Preparation of Examples and Comparative Examples

<Example 1>

3 g of distilled water and 97 g of DMSO were mixed to prepare 100 g of a dimethyl sulfoxide solution mixed with distilled water. 70 g of 100 g of the prepared dimethyl sulfoxide solution was mixed with 30 g of modacrylic polymer powder at 50 to 60° C. for 3 hours to prepare 100 g of a liquid polymer serving as an aggregation inhibitor. 15 g of the prepared liquid polymer 100 g, a solvent 30 g and a dispersant 0.5 g were added to the first container of the stirrer, and 10 g of pigment was added to the second container of the stirrer and stirred to prepare a stirred product. Here, 30 g of the solvent is 30 g of the total amount of 100 g prepared by mixing 3 g of distilled water and 97 g of DMSO.

The stirring material is put into the basket mill, the rotational speed of the shaft connected to the dispersion blade inside the basket is maintained at 500 to 800 rpm, and dispersed for 8 to 10 hours, but the temperature of the dispersion is maintained at 20 to 40°C and finally the particle size is 350 nm or less. A dispersion was obtained. 3 g of the remaining organic solvent was added to the dispersion after the dispersion was completed and stirred to make a filling. As a result of measuring the lightness value L of the filling, an additional solvent was not added as it was the same as the predetermined reference value 26. Subsequently, the filled product was passed through a 200-neck mesh, and then filtered by passing the product through a 250-neck mesh to complete a liquid oil and inorganic pigment colorant composition for artificial hair.

<Example 2>

100 g of a dimethyl sulfoxide solution mixed with distilled water was prepared by mixing 4 g of distilled water and 96 g of DMSO. 70 g of 100 g of the prepared dimethyl sulfoxide solution was mixed with 30 g of modacrylic polymer powder at 50 to 60° C. for 3 hours to prepare 100 g of a liquid polymer serving as an aggregation inhibitor. 15 g of the prepared liquid polymer 100 g, a solvent 30 g and a dispersant 0.5 g were added to the first container of the stirrer, and 10 g of pigment was added to the second container of the stirrer and stirred to prepare a stirred product. Here, 30 g of the solvent is 30 g of the total amount of 100 g prepared by mixing 4 g of distilled water and 96 g of DMSO.

The stirring material is put into the basket mill, the rotational speed of the shaft connected to the dispersion blade inside the basket is maintained at 500 to 800 rpm, and dispersed for 8 to 10 hours, but the temperature of the dispersion is maintained at 20 to 40°C or less and finally the particle size is 350 nm. The following dispersion was obtained. 3 g of the remaining organic solvent was added to the dispersion after the dispersion was completed and stirred to make a filling. As a result of measuring the lightness value L of the filling, an additional solvent was not added as it was the same as the predetermined reference value 26. Subsequently, the filled product was passed through a 200-neck mesh, and then filtered by passing the product through a 250-neck mesh to complete a liquid oil and inorganic pigment colorant composition for artificial hair.

<Comparative Example 1>

100 g of a dimethyl sulfoxide solution mixed with distilled water was prepared by mixing 2 g of distilled water and 98 g of DMSO. 70 g of 100 g of the prepared dimethyl sulfoxide solution was mixed with 30 g of modacrylic polymer powder at 50 to 60° C. for 3 hours to prepare 100 g of a liquid polymer serving as an aggregation inhibitor. 15 g of the prepared liquid polymer 100 g, a solvent 30 g and a dispersant 0.5 g were added to the first container of the stirrer, and 10 g of pigment was added to the second container of the stirrer and stirred to prepare a stirred product. Here, 30 g of the solvent is 30 g of 100 g of the total amount prepared by mixing 2 g of distilled water and 98 g of DMSO.

The stirring material is put into the basket mill, the rotational speed of the shaft connected to the dispersion blade inside the basket is maintained at 500 to 800 rpm, and dispersed for 8 to 10 hours, but the temperature of the dispersion is maintained at 20 to 40°C or less and finally the particle size is 350 nm. The following dispersion was obtained. 3 g of the remaining organic solvent was added to the dispersion after the dispersion was completed and stirred to make a filling. As a result of measuring the lightness value L of the filling, an additional solvent was not added as it was the same as the predetermined reference value 26. Subsequently, the filled product was passed through a 200-neck mesh, and then filtered by passing the product through a 250-neck mesh to complete a liquid oil and inorganic pigment colorant composition for artificial hair.

<Comparative Example 2>

5 g of distilled water and 95 g of DMSO were mixed to prepare 100 g of a dimethyl sulfoxide solution mixed with distilled water. 70 g of 100 g of the prepared dimethyl sulfoxide solution was mixed with 30 g of modacrylic polymer powder at 50 to 60° C. for 3 hours to prepare 100 g of a liquid polymer serving as an aggregation inhibitor. 15 g of the prepared liquid polymer 100 g, a solvent 30 g and a dispersant 0.5 g were added to the first container of the stirrer, and 10 g of pigment was added to the second container of the stirrer and stirred to prepare a stirred product. Here, 30 g of the solvent is 30 g of 100 g of the total amount prepared by mixing 5 g of distilled water and 95 g of DMSO.

The stirring material is put into the basket mill, the rotational speed of the shaft connected to the dispersion blade inside the basket is maintained at 500 to 800 rpm, and dispersed for 8 to 10 hours, but the temperature of the dispersion is maintained at 20 to 40°C or less and finally the particle size is 350 nm. The following dispersion was obtained. 3 g of the remaining organic solvent was added to the dispersion after the dispersion was completed and stirred to make a filling. As a result of measuring the lightness value L of the filling, an additional solvent was not added as it was the same as the predetermined reference value 26. Subsequently, the filled product was passed through a 200-neck mesh, and then filtered by passing the product through a 250-neck mesh to complete a liquid oil and inorganic pigment colorant composition for artificial hair.

3. Test and evaluation methods

Dispersibility, flowability, and blackness of the liquid oil and inorganic pigment colorant composition for artificial hair were evaluated through the methods described below, and the results are shown in Table 2.

Flow evaluation

The viscosity of each composition at 25°C (spindle NO 03, 20 rpm) was measured using a Brookfield viscometer. When the viscosity was 200 cps or less, the flowability was good, and when it exceeded 200 cps, the flowability was evaluated as poor.

Dispersibility evaluation

The particle size of each composition was measured with a Nano Particle Size Analyzer to evaluate the dispersibility as good when the particle size is 350 nm or less, and the dispersibility as bad when it exceeds 350 nm.

Blackness evaluation

After the temperature of the indoor place where the experiment is conducted is maintained at 7 to 8°C, and each pigment composition is allowed to stand for more than 24 hours in the room, using a quadrilateral APPLICATOR, coated on a blackness measuring paper such that the film thickness is 100 μm, When the L value was 26 or less, the blackness was evaluated as good by a spectrophotometer, and when the L value was larger than 26, it was evaluated as defective.

Example 1 Example 2 Comparative Example 1 Comparative Example 2 Flowability Good Good Bad Bad Dispersibility Good Good Bad Bad Blackness Good Good Bad Bad

As shown in Table 2, Examples 1 to 2 of the present invention are all good in flowability, dispersibility, and blackness, whereas in Comparative Example 1, ice crystals are generated in an environment of 7 to 8° C., resulting in flowability and distribution. It was confirmed that the acidity was lowered and the blackness was also poor. In Comparative Example 2, ice crystals did not occur in an environment of 7 to 8°C, but it was confirmed that a part of the modacrylic polymer gelled, resulting in poor flowability and dispersibility and poor blackness.

4. Preparation of further examples and comparative examples

<Example 3>

By mixing 3.3 g of distilled water and 96.7 g of DMSO, 100 g of a dimethyl sulfoxide solution mixed with distilled water was prepared. 70 g of 100 g of the prepared dimethyl sulfoxide solution was mixed with 30 g of modacrylic polymer powder at 50 to 60° C. for 3 hours to prepare 100 g of a liquid polymer serving as an aggregation inhibitor. 5 g of 100 g of the prepared liquid polymer, 40 g of solvent and 0.5 g of dispersant were added to the first container of the stirrer, and 10 g of pigment was added to the second container of the stirrer and stirred to prepare a stirred product. Here, 40 g of the solvent is taken from 40 g of the total amount of 100 g prepared by mixing 3.3 g of distilled water and 96.7 g of DMSO.

The stirring material is added to the basket mill, the rotational speed of the shaft connected to the dispersion blade inside the basket is maintained at 500 to 800 rpm, and dispersed for 8 to 10 hours. The following dispersion was obtained. 3 g of the remaining organic solvent was added to the dispersion after the dispersion was completed and stirred to make a filling. As a result of measuring the lightness value L of the filling, no additional solvent was added as it was the same as the predetermined reference value 26. Subsequently, the product through which the filling was completed was passed through a 200-neck mesh, and then filtered by passing the product through a 250-neck mesh to complete a liquid oil and inorganic pigment colorant composition for artificial hair.

<Example 4>

Except that 10 g of 100 g of liquid polymer acting as an anti-agglomerate, 35 g of solvent and 0.5 g of dispersant are added to the first container of the stirrer, and 10 g of pigment is added to the second container of the stirrer and stirred to prepare a stirred product. Was set in the same manner as in Example 3 to complete the liquid oil and inorganic pigment colorant composition for artificial hair.

<Example 5>

Except that 15 g of 100 g of liquid polymer acting as a flocculation agent, 30 g of solvent and 0.5 g of dispersant are added to the first container of the stirrer and 10 g of pigment is added to the second container of the stirrer and stirred to prepare a stirred product. Was set in the same manner as in Example 3 to complete the liquid oil and inorganic pigment colorant composition for artificial hair.

<Example 6>

Except that 20 g, 100 g of solvent, 30 g of solvent, and 0.5 g of dispersant are added to the first container of the stirrer, and 10 g of pigment is added to the second container of the stirrer and stirred to prepare a stirred product among 100 g of the liquid polymer serving as a flocculating agent. Was set in the same manner as in Example 3 to complete the liquid oil and inorganic pigment colorant composition for artificial hair.

<Example 7>

Except that 25 g, 100 g of solvent and 25 g of dispersant are added to the first container of the stirrer, and 10 g of pigment is added to the second container of the stirrer and stirred to prepare a stirred product among 100 g of the liquid polymer acting as an anti-aggregation agent. Was set in the same manner as in Example 3 to complete the liquid oil and inorganic pigment colorant composition for artificial hair.

<Comparative Example 3>

Except that 2.5 g, 100 g of solvent and 40 g of dispersant were added to the first container of the stirrer and 10 g of pigment was added to the second container of the stirrer and stirred to prepare a stirred product among the 100 g of the liquid polymer acting as an anti-agglomeration agent. The matter was set in the same manner as in Example 3 to complete the liquid oil and inorganic pigment colorant composition for artificial hair.

<Comparative Example 4>

Except that 30 g of the liquid polymer 100 g acting as a coagulant, 20 g of a solvent and 0.5 g of a dispersant are added to the first container of the stirrer, and 10 g of pigment is added to the second container of the stirrer and stirred to prepare a stirred product. Was set in the same manner as in Example 3 to complete the liquid oil and inorganic pigment colorant composition for artificial hair.

5. Additional testing and evaluation methods

Dispersion, flowability, blackness, and storage properties of the liquid oil and inorganic pigment colorant compositions for artificial hair according to Examples 3 to 7 and Comparative Examples 3 to 4 were evaluated through the methods described below, and the results are shown in Table 3. Did. The evaluation methods of dispersibility, flowability, and blackness are the same as those described above.

Zhejiang evaluation

The state of the liquid oil and inorganic pigment colorant composition for artificial hair stored at room temperature (22 to 24°C) for 2 months was visually checked, but it was confirmed whether sediment was generated or gelled in the liquid oil and inorganic pigment colorant composition for artificial hair. Therefore, when it was confirmed that sediment had occurred or gelation had occurred, the storage was evaluated as poor, and if sediment did not occur and gelation was not performed, the storage was evaluated as good.

Example 3 Example 4 Example 5 Example 6 Example 7 Comparative Example 3 Comparative Example 4 Flowability Good Good Good Good Good Good Good Dispersibility Good Good Good Good Good Bad Good Blackness Good Good Good Good Good Bad Good Zhejiang Good Good Good Good Good Good Bad

As shown in Table 3, Examples 3 to 7 of the present invention are all good in flowability, dispersibility, blackness, and storage, while Comparative Example 3 lacks the modacrylic polymer solids content and aggregates carbon black particles. It was confirmed that the dispersibility was inhibited and the blackness was also poor. In Comparative Example 4, it was confirmed that as the solid content of the modacrylic polymer was excessively contained, gelation occurred and storage was poor.

6. Blackness test according to the temperature of the dispersion during dispersion

<Experimental Example 5>

A liquid organic/inorganic pigment colorant composition for artificial hair was prepared in the same manner as in Example 5, except that the temperature of the dispersion was maintained at 20°C during dispersion. Thereafter, the blackness was evaluated in the same manner as described above, and the results are shown in Table 4.

<Experimental Example 6>

A liquid oil/inorganic pigment colorant composition for artificial hair was prepared in the same manner as in Example 5, except that the temperature of the dispersion was maintained at 30°C during dispersion. Thereafter, the blackness was evaluated in the same manner as described above, and the results are shown in Table 4.

<Experimental Example 7>

A liquid oil/inorganic pigment colorant composition for artificial hair was prepared in the same manner as in Example 5, except that the temperature of the dispersion was maintained at 40°C during dispersion. Thereafter, the blackness was evaluated in the same manner as described above, and the results are shown in Table 4.

<Experimental Example 8>

A liquid organic and inorganic pigment colorant composition for artificial hair was prepared in the same manner as in Example 5, except that the temperature of the dispersion was maintained at 50°C during dispersion. Thereafter, the blackness was evaluated in the same manner as described above, and the results are shown in Table 4.

<Experimental Example 9>

A liquid organic and inorganic pigment colorant composition for artificial hair was prepared in the same manner as in Example 5, except that the temperature of the dispersion was maintained at 10°C during dispersion. Thereafter, the blackness was evaluated in the same manner as described above, and the results are shown in Table 4.

Experimental Example 5 Experimental Example 6 Experimental Example 7 Experimental Example 8 Experimental Example 9 Blackness Good Good Good Bad Bad

As shown in Table 4, Experimental Examples 5 to 7 in which the temperature of the dispersion was maintained at 20 to 40°C during dispersion was good, whereas Experimental Example 8 in which the temperature of the dispersion exceeded 40°C was poor in blackness. As can be seen, Experimental Example 9 in which the temperature of the dispersion was less than 20° C. was confirmed to have an adverse effect on the blackness while the dispersibility was lowered.

As described above, according to various embodiments of the present invention, by adding a certain amount of water to dimethyl sulfoxide, an organic solvent contained in a liquid oil and inorganic pigment colorant composition for artificial hair, the freezing point of dimethyl sulfoxide is lowered to 7~ Even in the working environment of 8℃, the liquid oil and inorganic pigment colorant for artificial hair does not freeze, improving workability in spring and winter, and it has the effect of reducing the facility cost and maintenance cost required to maintain the temperature.

In addition, by setting the content of water added to dimethyl sulfoxide to a certain range, no trouble occurs with the modacrylic polymer contained in the pigment, and it contributes to the improvement of the flowability and blackness of the liquid organic and inorganic pigment colorant.

In addition, as the liquid polymer in which the modacrylic polymer powder is dissolved using an organic solvent (for example, dimethyl sulfoxide, acetone, etc.) as a solvent is used as a flocculating agent, the dispersion of the pigment particles is prevented during dispersion by dispersibility. Improved, the solid content of the modacrylic polymer in the liquid polymer serving as an anti-agglomeration agent is 1.5 to 7.5% by weight (for example, 1.5% by weight, 2% by weight, 3% by weight, 4% by weight, 4.5% by weight, 5 By weight%, 6% by weight, 7% by weight or 7.5% by weight), there is an effect of excellent flowability and storage properties of the liquid oil and inorganic pigment colorant composition for artificial hair.

In addition, in one embodiment of the present invention, by adding a certain amount of the modacrylic polymer of the same type as the resin used for manufacturing the artificial hair fibers in the liquid oil and inorganic pigment colorant composition for artificial hair, it is possible to prevent the aggregation of carbon particles as pigments Since it can prevent the aggregation, there is no need to add another anti-aggregation agent or a separate component.

As described above, the detailed description of the present invention has been made by examples, but since the above-described embodiments are merely described as preferred examples of the present invention, it should be understood that the present invention is limited to the above-described embodiments only. No, the scope of the present invention should be understood as the claims and the equivalent concept described below.

10: stirrer
100: housing
110: stator
120: rotor
130: discharge pipe
200: motor
210: drive shaft
300: first container
310: first pipe
400: second container
410: second pipe

Claims (6)

A liquid polymer preparation step of dissolving the modacrylic polymer powder in a first organic solvent to prevent aggregation of the pigment particles to produce a liquid polymer serving as an aggregation inhibitor;
A compounding step of mixing the liquid polymer, a pigment, a dispersant, and a second organic solvent to prepare a stirred product; And
Characterized in that it comprises; a dispersing step of introducing and dispersing the stirring material in the dispersion equipment to prepare a dispersion
Method for preparing liquid pigment colorant composition for artificial hair. According to claim 1,
In the liquid polymer manufacturing step, the liquid polymer is a liquid polymer prepared by mixing 30% by weight of the modacrylic polymer powder and 70% by weight of dimethyl sulfoxide mixed with distilled water at 50-60°C for 2-3 hours, and the distilled water Dimethyl sulfoxide mixed with is characterized by being prepared by mixing 3 to 4% by weight of distilled water and 96 to 97% by weight of dimethyl sulfoxide.
Method for preparing liquid pigment colorant composition for artificial hair. According to claim 1,
In the compounding step, the pigment is provided with carbon black, and the second organic solvent is prepared by mixing 3 to 4% by weight of distilled water and the remainder of dimethyl sulfoxide, and the stirred material is 5 to 25 parts by weight of the liquid polymer, 5 to 10 parts by weight of the pigment, 0.5 to 1.5 parts by weight of the dispersant and 25 to 40 parts by weight of the second organic solvent,
In the dispersing step, the dispersing equipment is provided with a 3-roll mill, a bead mill, or a basket mill, and when dispersing, the temperature of the dispersion is maintained at 20-40°C.
Method for preparing liquid pigment colorant composition for artificial hair. According to claim 1,
The manufacturing method of the liquid pigment colorant composition for artificial hair is
A filling step of adding and stirring 1 to 5 parts by weight of an additional organic solvent to the dispersion; And
Further comprising; when the blackness measurement value of the filler filled in the filling step is less than a predetermined reference value, an inspection step of adding 1 to 5 parts by weight of the additional organic solvent to the filler;
The additional organic solvent is characterized in that it is provided with at least one of dimethyl sulfoxide and acetone
Method for preparing liquid pigment colorant composition for artificial hair. According to claim 1,
In the liquid polymer manufacturing step, the first organic solvent is characterized in that it is provided with at least one of dimethyl sulfoxide and acetone
Method for preparing liquid pigment colorant composition for artificial hair. A liquid pigment colorant composition for artificial hair prepared by the method according to any one of claims 1 to 5.

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