KR102159014B1 - Liquid pigment colorant composition for dope dyed fiber and method for manufacturing the same - Google Patents

Abstract

Disclosed are a liquid pigment colorant composition for a dope-dyed fiber and a method for preparing the same. The method for preparing a liquid pigment colorant composition for dope-dyed fiber comprises: a solvent preparing step of preparing a solvent by dissolving sodium thiocyanate at a predetermined concentration; a blending step of preparing a stirred substance by blending a flow improving agent, a pigment, a dispersant, and the solvent; a dispersion step of preparing a dispersed substance by adding the stirred substance to a dispersion device and dispersing the stirred substance; a filling step of injecting the remaining solvent into the dispersed substance and stirring the mixture thereof; an examination step of examining a product thereof; and a transfer step of filtering and transferring the product. According to the present invention, the liquid pigment colorant composition for a dope-dyed fiber has excellent storability.

Description

Liquid pigment colorant composition for circulating dye and its manufacturing method {LIQUID PIGMENT COLORANT COMPOSITION FOR DOPE DYED FIBER AND METHOD FOR MANUFACTURING THE SAME}

The present disclosure relates to a liquid pigment colorant composition and a method for producing the same.

In general, the liquid pigment colorant composition for dyeing is a component added to the resin for dyeing. Wound yarn is a yarn produced by spinning a solution of the liquid pigment colorant composition and resin used for yarn spinning, and is a yarn that does not require a separate dyeing process because it is colored in the yarn state, and reduces environmental pollution such as wastewater generated during dyeing. It is meaningful. In this regard, Korean Patent Publication No. 10-0583365 discloses a technique for a method of manufacturing a raw yarn using a pigment.

By the way, the sodium thiocyanate aqueous solution with a sodium thiocyanate concentration of 58% (w/w) is usually 58% (w) as a solvent in the liquid pigment colorant composition for use as a raw material because sodium thiocyanate crystallizes at 16°C or lower. /w) If sodium thiocyanate aqueous solution is included, the dispersibility and flow properties of the liquid pigment colorant composition used for the original deposition are precipitated as sodium thiocyanate dissolved in the sodium thiocyanate aqueous solution is produced during the production of liquid pigment colorants for raw materials in spring or winter. In addition to the possibility of lowering the blackness, the filter pressure of the spinning device is increased during the manufacturing process of spinning yarns that are mixed and spun by mixing the resin used for spinning and the liquid pigment colorant composition used for spinning, preventing smooth spinning, For example, there was a problem of lowering the blackness).

In order to solve this problem, the temperature of the production site of the liquid pigment colorant composition for circumference, the tank for storing the liquid pigment colorant composition for circumference, and all pipes through which the liquid pigment colorant composition for circumference is passed must be maintained at 16℃ or higher. Liquid pigments used in raw materials within the range that does not adversely affect the quality, spinnability and resins used in raw materials because the productivity of the liquid pigment colorant composition for raw dyeing in spring or winter season is low due to high facility cost and maintenance cost. There is a new demand for the development of technology that facilitates the production of colorant compositions.

The technical idea of the present disclosure is to solve the above-described problems, and it is an object to develop a liquid pigment colorant composition for raw dyeing for realizing the color of acrylic fibers based on sodium thiocyanate.

In addition, the technical idea of the present disclosure is to provide a technology capable of maintaining the quality of a liquid pigment colorant composition for use in spring and fall or winter.

In addition, the technical idea of the present disclosure has another object to provide a technology capable of reducing facility cost and maintenance cost when manufacturing a liquid pigment colorant composition for use in raw materials.

The problem to be solved by the present invention is not limited to the above-described problem, and other technical problems that are not mentioned will be clearly understood by those of ordinary skill in the technical field to which the present invention belongs from the following description.

In order to achieve this object, as an embodiment of the present invention, a method for preparing a liquid pigment colorant composition for circumference comprises: a solvent preparation step of dissolving sodium thiocyanate at a constant concentration to prepare a solvent; A blending step of blending a flow improving agent, a pigment, a dispersant, and the solvent to prepare an agitated product; And a dispersion step of preparing a dispersion by introducing and dispersing the agitated product into a dispersion equipment.

In addition, in the solvent manufacturing step, the solvent is prepared by mixing 46 to 52% by weight of sodium thiocyanate with 48 to 54% by weight of distilled water, and in the blending step, the pigment is provided with carbon black, and the agitated product is 30 to 34 parts by weight of a flow improving agent, 11 to 13 parts by weight of the pigment, 0.5 to 1 parts by weight of the dispersant, and 40 to 50 parts by weight of the solvent, and in the dispersing step, the dispersing equipment is a 3-roll mill, a bead mill, or a basket It is provided with a mill, and when dispersed, the temperature of the dispersion may be maintained at 20 to 40°C.

In addition, in the stirring step, the flowability improving agent may be prepared by mixing 12% by weight of acrylic polymer, 40% by weight of sodium thiocyanate, and 48% by weight of distilled water.

In addition, a method for preparing a liquid pigment colorant composition for circulating may include a filling step of inserting and stirring 1 to 5 parts by weight of a residual solvent into the dispersion; In the case where the measurement value of the blackness of the filling material filled in the filling step is less than a predetermined reference value, an inspection step of injecting 1 to 5 parts by weight of the residual solvent into the filling material may be further included.

In order to achieve this object, as another embodiment of the present invention, the liquid pigment colorant composition for raw dyeing may be prepared by the method for preparing the liquid pigment colorant composition for raw dyeing.

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 above-described exemplary embodiments, 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, sodium thiocyanate is crystallized by setting the concentration of the sodium thiocyanate aqueous solution, which is a solvent contained in the liquid pigment colorant composition for circumference, to 46 to 52 w/w%. As the temperature is lowered, sodium thiocyanate does not precipitate even in the working environment of 5 to 10°C, which has the effect of improving workability in spring and winter. For example, if the concentration of the sodium thiocyanate aqueous solution is adjusted to 52w/w%, sodium thiocyanate does not crystallize at 10°C for 6 hours, and if the concentration of the sodium thiocyanate aqueous solution is adjusted to 46w/w%, 5 Since sodium thiocyanate does not crystallize at ℃ for 16 hours, stable work is possible even in spring and winter seasons.

In addition, according to various embodiments of the present invention, by setting the content of distilled water added in the solvent to a certain range, trouble with the acrylic polymer contained in the flowability improving agent does not occur, and the acrylic polymer is entangled in water to form a small lump. Since a hardening seed does not occur and does not gel, it contributes to the improvement of the flowability and blackness of the liquid pigment colorant composition for use.

In addition, according to various embodiments of the present invention, since the surface tension of the liquid pigment colorant composition for raw dyeing is reduced through a flow improving agent containing an acrylic polymer, a thixotropy phenomenon does not occur. Therefore, the flowability and dispersibility of the liquid pigment colorant composition for raw dyeing are improved, aggregation of pigment particles is prevented during dispersion, and the storage property of the liquid pigment colorant composition for raw dyeing is excellent.

The effects of the present invention are not limited to the effects mentioned above, and other effects that are 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 pigment colorant composition for circulating dye according to an embodiment of the present invention.
2 is a conceptual diagram schematically showing a stirrer used in the blending step according to an embodiment of the present invention.

Preferred embodiments of the present invention will be described in more detail with reference to the accompanying drawings, but technical parts that are already well-known will be omitted or compressed for conciseness of description.

It should be noted that references to "one" or "one" embodiment of the present invention in this specification are not necessarily to the same embodiment, and they mean at least one.

In the following examples, expressions in the singular include plural expressions unless the context clearly indicates otherwise.

In the following embodiments, terms such as include or have means that the features or elements described in the specification are present, and do not preclude the possibility of adding one or more other features or elements.

When a certain 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 the described order. That is, each step of the method described herein may be appropriately performed in any order unless otherwise stated in the specification or clearly contradicted by context.

A method of preparing a liquid pigment colorant composition for circulating dye according to an embodiment of the present invention will be described in accordance with the flowchart shown in FIG. 1, but will be described in order for convenience.

1. Solvent manufacturing step <S101>

In this step, sodium thiocyanate can be dissolved in a certain concentration to prepare a solvent. In one embodiment, the solvent may be prepared by mixing 46 to 52% by weight of sodium thiocyanate with 48 to 54% by weight of distilled water. That is, the sodium thiocyanate aqueous solution, which is a solvent according to an embodiment, may have a concentration range of 46 to 52 w/w%. Adjusting the concentration of the solvent can be done in a variety of ways.

For example, sodium thiocyanate powder can be dissolved in distilled water to adjust the concentration of the sodium thiocyanate aqueous solution to 46-52 w/w%, and by adding distilled water to the sodium thiocyanate aqueous solution of a specific concentration, thiocyanic acid The final concentration of the aqueous sodium solution may be adjusted to 46-52 w/w%.

In one embodiment, 50% by weight of sodium thiocyanate powder and 50% by weight of distilled water are added to the fluid mixing reactor, the temperature of the reactor is raised to 90°C, and the temperature is maintained for 6 hours, and the sodium thiocyanate aqueous solution is While measuring the concentration, distilled water may be additionally added to adjust the final concentration of the sodium thiocyanate aqueous solution to 46.6w/w%.

In another embodiment, a solvent having a concentration of 46.6w/w% may be prepared by mixing 19% by weight of distilled water at 25 to 30°C with 81% by weight of an aqueous solution of sodium thiocyanate having a concentration of 58w/w%. At this time, when the temperature of the distilled water is 16°C or less, sodium thiocyanate dissolved in the sodium thiocyanate aqueous solution may crystallize and precipitate. Therefore, mixing may be performed by maintaining the temperature of the distilled water at 25°C or higher.

In one embodiment, the solvent may include 46 to 52% by weight of sodium thiocyanate and the remainder of distilled water. As a specific example, the content of sodium thiocyanate may be provided in 46% by weight, 46.6% by weight, 47% by weight, 48% by weight, 49% by weight, 50% by weight, 51% by weight, or 52% by weight. In addition, the content of sodium thiocyanate may be in the range of one or more of the above values and one or less of the above values.

For example, the content of sodium thiocyanate in the solvent ranges from 46% to 47%, 47% to 48%, 48% to 49%, 49% to 50%, 50% by weight. It may be provided in a range of to 51% by weight, 51% to 52% by weight or 46% to 52% by weight. The sodium thiocyanate aqueous solution according to an embodiment prevents sodium thiocyanate from crystallizing from the solvent during the spring or winter season within the above range, and improves the quality of the liquid pigment colorant composition for raw dyeing and spinning efficiency of the raw yarn. Can be maintained.

If the content of sodium thiocyanate is less than 46% by weight, as the content of distilled water in the solvent increases, the flow improver to be described later may become entangled in distilled water, causing a seed phenomenon or gelation, and sodium thiocyanate is 52% by weight. If it exceeds %, sodium thiocyanate dissolved in sodium thiocyanate aqueous solution crystallizes and precipitates at a temperature higher than 10℃, so the flowability, dispersibility, and blackness of the liquid pigment colorant composition used in the spring or winter season decrease. Therefore, it is preferable that distilled water and sodium thiocyanate are mixed within the above-described content range because workability and overall quality may be deteriorated.

2. Mixing step <S102>

In this step, a flow improving agent, a pigment, a dispersant, and a solvent may be mixed to prepare an agitated product. 2 is a conceptual diagram schematically showing a stirrer used in the blending step according to an embodiment of the present invention. Referring to FIG. 2, the stirrer 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 at one side of the housing 100 so that the agitated material after 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 is coupled with the drive shaft 210 of the motor 200 to rotate in one direction when the drive shaft 210 rotates. 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 a first pipe 310, and the second container 400 is connected to the housing 100 through a second pipe 410.

Specifically, in this step, a flow improving agent, a dispersant, and a solvent are added to the first container 300 and the pigment is added to the second container 400. When the motor 200 is operated and the drive shaft 210 rotates, the drive shaft As the rotor 120 connected to the 210 rotates at a constant speed, a shear force due to rotation is generated. That is, a certain gap is formed between the stator 110 and the rotor 120, and shear force is generated by the rotation of the rotor 120, so that the agitated material passes through the gap formed between the stator 110 and the rotor 120 It can be stirred evenly.

In addition, the high-speed rotation of the rotor 120 generates a suction force from each of the containers 300 and 400 in the direction of the housing 100, so that the contents put into the first container 300 and the contents put into the second container 400 are Each of the first pipe 310 and the second pipe 410 may be introduced into the interior of the housing 100. Therefore, when a pigment made of nanometer-unit fine powder (for example, carbon black) is mixed, it is possible to prevent the pigment from contaminating the work area or deteriorating workability as the pigment is scattered in the air, and the rotor 120 ), the dispersion effect of the blend can be obtained above a certain level by high-speed rotation.

On the other hand, when mixing the flow improving agent, the pigment, the dispersant and the solvent in this step, it is possible to apply a different mixing method without using the inline mix method described above. For example, in another embodiment, a flow improving agent, a pigment, a dispersant, and a solvent may be added into a dissolver or a homomixer and stirred at a constant speed to prepare a stirred product.

And, in this step, the flow improving agent may be added in 30 to 34 parts by weight (eg, 30 parts by weight, 31 parts by weight, 32 parts by weight, 33 parts by weight, or 34 parts by weight).

If the content of the flowability improving agent is less than 30 parts by weight, it is difficult to lower the surface tension of the solvent, so the flowability of the liquid pigment colorant composition for raw dyeing decreases, and the dispersibility decreases, resulting in a decrease in blackness, and pigment particles during storage. May occur, and if the content of the flow improving agent exceeds 34 parts by weight, the viscosity of the solvent decreases and the viscosity increases, resulting in a decrease in flowability or a gelling phenomenon over time. Since the problem of lowering the storage properties of the pigment colorant composition may occur, the flowability improving agent is preferably added within the above-described content range.

In addition, in an embodiment, the flow improving agent may be prepared by mixing 12% by weight of an acrylic polymer, 40% by weight of sodium thiocyanate, and 48% by weight of distilled water. In one embodiment, the acrylic polymer may be applied as polyacrylonitrile in which an acrylonitrile monomer is polymerized. Examples of commercially available acrylonitrile monomers may include acrylonitrile manufactured by Taekwang Industrial Co., Ltd., but are not limited thereto.

If the content of the acrylic polymer contained in the flow improver exceeds 12% by weight, the viscosity may increase in the flow improver and the flowability may decrease.If the content of the acrylic polymer is less than 12% by weight, the surface tension and viscosity of the solvent It is difficult to adjust the flow rate to an appropriate level, so the effect of improving flowability may be reduced.

And, if the content of sodium thiocyanate contained in the flowability improving agent exceeds 40% by weight, sodium thiocyanate remaining unmixed with the acrylic polymer may be generated, and when it is less than 40% by weight, the acrylic polymer is contained in the flowability improving agent. There is a fear that it may not be sufficiently dissolved in

In one embodiment, the pigment may be applied as an organic or inorganic pigment, or both organic and inorganic pigments may be used. In one embodiment, the pigment is provided with carbon black, and examples of commercially available carbon black may be Mitsubishi Chemical's OIL7B or OIL31B, but are not limited thereto.

In this step, the pigment may be applied in an amount of 11 to 13 parts by weight (for example, 11 parts by weight, 12 parts by weight, or 13 parts by weight). If the content of carbon black, which is a pigment, is less than 11 parts by weight, the blackness of the liquid pigment colorant composition for raw dyeing decreases, and if the pigment exceeds 13 parts by weight, the viscosity of the liquid pigment colorant composition for raw dyeing is increased. There is a fear that the dispersibility may decrease.

In one embodiment, the dispersant may be at least one selected from the group consisting of an anionic dispersant, a cationic dispersant, an amphoteric dispersant, and a nonionic dispersant. Examples of commercially available dispersants may be BYK-Chemie's Disperbyk-184, Disperbyk 192, and the like, but are not limited thereto.

In this step, the dispersant may be applied in an amount of 0.5 to 1 parts by weight (eg, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight, or 1 part by weight). If the content of the dispersant is less than 0.5 parts by weight, the dispersibility decreases and the blackness decreases, and if the content of the dispersant exceeds 1 part by weight, the storage property may be lowered. Therefore, the content of the dispersant is preferably applied within the above-described range.

In addition, the solvent blended with the flow improving agent, the pigment, and the dispersant in this step may be prepared by mixing 46 to 52% by weight of sodium thiocyanate with the remainder of distilled water. In this step, the solvent is 40 to 50 parts by weight (for example, 40 parts by weight, 41 parts by weight, 42 parts by weight, 43 parts by weight, 44 parts by weight, 45 parts by weight, 46 parts by weight, 47 parts by weight, 48 parts by weight) , 49 parts by weight or 50 parts by weight). In this step, if the solvent is less than 40 parts by weight, the viscosity of the agitated material increases and the dispersibility decreases during the dispersion step to be described later. If it exceeds 50 parts by weight, the solvent content is relatively excessive compared to the pigment content, resulting in a low viscosity. The degree of blackness of the liquid pigment colorant composition for use in high quality may be lowered.

3. Dispersion step <S103>

In this step, the agitated material can be added to the dispersion equipment and dispersed to prepare a dispersion. In this step, the dispersion equipment may be provided with a three-roll mill, a bead mill, or a basket mill (for example, a ring mill, a rotate mill). Here, the three-roll mill is a device that homogenizes the stirring material by passing it through a fine gap formed between the three horizontally placed rollers.The draw-in roller, the middle roller, and the scraper roller adjacent to each other rotate at the same time and pressurize the agitated material passing through the roller. And shear force is applied. In addition, the basket mill (for example, a rotate mill) is a device that disperses the mixture while rotating the basket in a direction opposite to the rotation direction of the dispersion blades installed inside the cylindrical basket.The compound introduced into the basket is Dispersion can be achieved quickly by rotation.

As a specific example, in the case of dispersion by a three-roll mill, the dispersion can be added to the three-roll mill six or more times to maintain the particle size of the dispersion to be less than 350 nm, and in the case of dispersion by a basket mill, the rotation speed of the shaft connected to the dispersion blade inside the basket The particle size of the dispersion can be maintained below 350nm by maintaining at 500~800rpm and adjusting the dispersion time to 8~10 hours.

And, the temperature of the dispersion can be maintained at 20 ~ 40 ℃ when dispersed in the dispersion equipment. If the temperature of the dispersion during dispersion exceeds 40°C, there is a concern that the blackness and storage properties of the liquid pigment colorant composition used for circumference may decrease. If the temperature is less than 20°C, it is difficult to maintain the temperature and dispersibility may be impaired. It is desirable to keep the temperature of the Si dispersion within the aforementioned range.

4. Filling step <S104>

In this step, the residual solvent may be additionally added to the dispersion and stirred. In one embodiment, the residual solvent may be applied as the same as the solvent prepared in step S101. In this step, the dispersion can be made into a filler by adding 1 to 5 parts by weight of the remaining solvent.

5. Inspection step <S105>

In this step, if the blackness measurement value (for example, the brightness value L) of the packing material measured by the color difference meter is less than a predetermined reference value (for example, 25), 1 to 5 parts by weight of the remaining solvent is added to the packing material and used. The degree of blackness of the liquid pigment colorant composition can be adjusted.

6. Filtering and transfer step <S106>

In this step, the inspected filler is passed through a filter of a certain particle size to remove degassing of the product and foreign substances and finely dispersed pigments that may exist in the filler, and transfer the filtered raw pigment colorant composition to a storage tank. I can. In addition, depending on the implementation, in this step, the inspection-completed filler may be filtered while sequentially passing through a plurality of filters having different particle diameters.

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

1. Experiment for crystallization of solvent according to sodium thiocyanate concentration

Each component was added to the reactor in the amount (unit: g) shown in Table 1 to be mixed, but after raising the temperature of the reactor to 90° C., the temperature was maintained for 6 hours to prepare a solvent. After that, put the prepared solvent in a constant temperature chamber, lower the temperature by 1℃ from 25℃, and check the temperature at which sodium thiocyanate crystals precipitate in the mixture. Then, sodium thiocyanate crystallizes at a temperature of 10℃ or higher. If the crystallization was found to be poor and crystallized at a temperature below 10°C, the crystallization was evaluated as good, and the results are shown in Table 1.

Experimental Example 1 Experimental Example 2 Experimental Example 3 Experimental Example 4 Experimental Example 5 Experimental Example 6 Experimental Example 7 Experimental Example 8 Experimental Example 9 Sodium thiocyanate 46 47 48 49 50 51 52 45 53 Distilled water 54 53 52 51 50 49 48 55 47 Crystallization Good Good Good Good Good Good Good Good Bad

2. Preparation of liquid pigment colorant composition for raw dyeing

Each solvent, flowability improving agent, and dispersant were added to the first container of the stirrer, and the pigment was added to the second container of the stirrer, and stirred to prepare a stirred product in the amount (unit: g) shown in Table 2 below. Here, the solvents of Examples 1 to 5 and Comparative Examples 1 to 2 are prepared by adding 47 g of sodium thiocyanate and 53 g of distilled water into the reactor, but maintaining the temperature for 6 hours after raising the temperature of the reactor to 90°C. The solvent of Comparative Example 3 was the same as that of Experimental Example 8.

After mixing is complete, the agitated material is put into the basket mill, and the rotation speed of the shaft connected to the dispersion blade inside the basket is maintained at 500 to 800 rpm, and the dispersion is dispersed for 8 to 10 hours, but the temperature of the dispersion is kept below 40°C As a result, a dispersion having a particle size of 350 nm or less was obtained. After the dispersion was completed, 3 g of the remaining solvent was added to the dispersion and stirred to make a filler, and the lightness value L of the filler was measured. As a result, the remaining solvent was not added to the filler because it was the same as the known reference value 25. Thereafter, the inspected filler was passed through the 200-neck mesh, and the inspected filler was passed through the 250-neck mesh again and filtered to complete the raw pigment colorant composition.

ingredient Example
One Example
2 Example
3 Example 4 Example 5 Comparative example
One Comparative example
2 Comparative example
3 solvent 50 50 50 50 50 50 50 50 Flow improver 31 32 33 30 34 29 35 32 Pigment 13 12 11 13 11 14 10 12 Dispersant One 0.5 0.5 0.9 0.7 0 1.5 0.5

3. Test and evaluation method

The flowability, dispersibility, blackness, and storage properties of each liquid pigment colorant composition for raw dyeing were evaluated through the method described below, and the results are shown in Table 3.

Flowability evaluation

The viscosity of each composition was measured at 25°C (spindle NO 03, 20 rpm) using a Brookfield viscometer, and if the viscosity was 1000 cps or less, the flowability was good, and if it exceeded 1000 cps, the flowability was evaluated as poor.

Dispersion evaluation

The particle size of each composition was measured with a Nano Particle Size Analyzer. If the particle size was 350 nm or less, the dispersibility was good, and if it exceeded 350 nm, the dispersibility was evaluated as poor.

Blackness evaluation

Maintain the temperature of the indoor place where the experiment is conducted at 10℃, and after leaving each pigment composition indoors for 6 hours, apply it on the blackness measurement paper so that the thickness of the coating film becomes 100㎛ using a square applicator, and then the spectral color difference It was measured with a system, and if the L value was 25 or less, the blackness was evaluated as good, and if the L value was greater than 25, it was evaluated as defective.

Storability evaluation

Visually check the state of each raw pigment colorant composition stored in a transparent container at room temperature (22~24℃) for 2 months, but check whether a sediment has occurred in the liquid pigment colorant composition for use, and whether seeding and gelation have occurred. Thus, when it was confirmed that sediment occurred or seed phenomenon or gelation occurred, the storage property was evaluated as poor, and when no precipitate occurred and seed phenomenon and gelation were not performed, the storage property was evaluated as good.

Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Flow Good Good Good Good Good Bad Bad Bad Dispersibility Good Good Good Good Good Bad Bad Bad Blackness Good Good Good Good Good Bad Bad Bad Zhejiang Good Good Good Good Good Bad Bad Bad

As shown in Table 3, Examples 1 to 5 of the present invention have good flowability, dispersibility, blackness, and storage properties, whereas Comparative Examples 1 to 2 outside the content range of each component are liquid pigment colorants for original use. It was confirmed that the physical properties of the composition were generally poor. In Comparative Example 3, when the blackness was evaluated, sodium thiocyanate was not precipitated in an environment of 10° C., but the content of distilled water contained in the solvent was excessive, so that the acrylic polymer was seeded and gelled, and flowability and dispersibility were decreased. It was confirmed that the blackness was lowered and the storage property was poor.

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

<Experimental Example 10>

Except that the temperature of the dispersion was maintained at 20° C. during dispersion, the remaining matters were prepared in the same liquid pigment colorant composition as in Example 2. Thereafter, blackness and storage properties were evaluated in the same manner as in the above-described method, and the results are shown in Table 4.

<Experimental Example 11>

Except that the temperature of the dispersion was maintained at 30° C. during dispersion, the remaining matters were prepared in the same liquid pigment colorant composition as in Example 2. Thereafter, blackness and storage properties were evaluated in the same manner as in the above-described method, and the results are shown in Table 4.

<Experimental Example 12>

Except that the temperature of the dispersion was maintained at 40° C. during dispersion, the remaining matters were prepared in the same liquid pigment colorant composition as in Example 2. Thereafter, blackness and storage properties were evaluated in the same manner as in the above-described method, and the results are shown in Table 4.

<Experimental Example 13>

Except that the temperature of the dispersion was maintained at 50° C. during dispersion, the remaining matters were prepared in the same liquid pigment colorant composition as in Example 2. Thereafter, blackness and storage properties were evaluated in the same manner as in the above-described method, and the results are shown in Table 4.

<Experimental Example 14>

Except that the temperature of the dispersion was maintained at 10° C. during dispersion, the remaining matters were prepared in the same liquid pigment colorant composition as in Example 2. Thereafter, blackness and storage properties were evaluated in the same manner as in the above-described method, and the results are shown in Table 4.

Experimental Example 10 Experimental Example 11 Experimental Example 12 Experimental Example 13 Experimental Example 14 Blackness Good Good Good Bad Bad Zhejiang Good Good Good Bad Bad

As shown in Table 4, Experimental Examples 10 to 12 in which the temperature of the dispersion was maintained at 20 to 40°C during dispersion had good blackness and storage properties, whereas Experimental Example 13 in which the temperature of the dispersion exceeded 40°C, each component It can be seen that even if the blending of the mixture is the same as in Example 2, it can be seen that it has a negative effect on the blackness and storage properties of the liquid pigment colorant composition for circumference. It was confirmed that it had an adverse effect.

As described above, according to various embodiments of the present invention, it is possible to prepare a liquid organic and inorganic pigment colorant composition used in acrylic for fibers. In other words, it is possible to prepare a liquid pigment colorant for implementing colors with organic and inorganic pigments in an acrylic polymer using an aqueous sodium thiocyanate solution as a solvent, not a dye during textile processing.

According to various embodiments of the present invention, since the color of the raw yarn is controlled by the liquid organic and inorganic pigment colorant composition, and the use of the dye can be selectively adjusted, the dye is not used in the process of implementing the color of the original yarn or the amount of dye is reduced. It can reduce water pollution due to wastewater generated during textile processing (dyeing) and protect the environment.By adjusting the concentration of sodium thiocyanate aqueous solution, which is the main solvent, to lower the crystallization temperature, It has the advantage of reducing facility and maintenance costs, and improving the quality and stability of colorants.

According to various embodiments of the present invention, by setting the concentration of the sodium thiocyanate aqueous solution, which is a solvent contained in the liquid pigment colorant composition for circumference, to 46 to 52 w/w%, the temperature at which sodium thiocyanate is crystallized is lowered to 5 to Since sodium thiocyanate does not precipitate even in a working environment of 10°C, there is an effect of improving the productivity and workability of the liquid pigment colorant composition for use in spring and winter.

In addition, according to various embodiments of the present invention, by setting the content of distilled water added in the solvent to a certain range, troubles with the acrylic polymer contained in the flowability improving agent do not occur, and the seed phenomenon or gelation of the acrylic polymer hardening does not occur. It contributes to the improvement of the flowability and blackness of the liquid pigment colorant composition for use in raw materials, and has excellent storage properties.

Further, according to various embodiments of the present invention, since the surface tension of the solvent is reduced through the flow improving agent containing the acrylic polymer, a thixotropy phenomenon does not occur. Therefore, the flowability and dispersibility of the liquid pigment colorant composition for raw dyeing are improved, aggregation of pigment particles is prevented during dispersion, and the storage property of the liquid pigment colorant composition for raw dyeing is excellent.

In addition, in an embodiment of the present invention, by adding a certain amount of an acrylic polymer, which is the same type as the resin used for producing woven yarn, into the flowability improving agent, the surface tension of the solvent is lowered to reduce the flowability of the liquid pigment colorant composition for circulating yarn. As it can improve flowability, there is no need to add a separate component to improve flowability, and when the liquid pigment colorant for raw dyeing is mixed with the resin for raw dyeing, trouble with the resin does not occur. It is excellent in dispersibility and blackness and can prevent agglomeration of carbon black particles, which are pigments.

As described above, a detailed description of the present invention has been made by examples, but since the above-described embodiments have been described only with preferred examples of the present invention, it is understood that the present invention is limited to the above embodiments. No, the scope of the present invention should be understood in terms of the claims to be described later and their equivalent concepts.

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 (5)

A solvent preparation step of dissolving sodium thiocyanate at a constant concentration to prepare a solvent;
A blending step of blending a flow improving agent, a pigment, a dispersant, and the solvent to prepare an agitated product; And
Including; a dispersion step of preparing a dispersion by introducing and dispersing the agitated material into a dispersion equipment,
In the solvent manufacturing step, the solvent is prepared by mixing 46 to 52% by weight of sodium thiocyanate with 48 to 54% by weight of distilled water,
In the blending step, the pigment is provided with carbon black, and the agitated material is 30 to 34 parts by weight of the flow improver, 11 to 13 parts by weight of the pigment, and 0.5 to 1 parts by weight of the dispersant when the solvent is 50 parts by weight. Including,
In the dispersing step, the dispersing equipment is provided with a 3-roll mill, a bead mill, or a basket mill, and the temperature of the dispersion is maintained at 20 to 40° C. during dispersion,
In the blending step, the flow improving agent is prepared by mixing 12% by weight of acrylic polymer, 40% by weight of sodium thiocyanate, and 48% by weight of distilled water.
A method for preparing a liquid pigment colorant composition for circulating dye. delete delete The method of claim 1,
The manufacturing method of the liquid pigment colorant composition for circulating
A filling step of inserting and stirring 1 to 5 parts by weight of the remaining solvent into the dispersion;
In the case where the measurement value of the blackness of the filling material filled in the filling step is less than a predetermined reference value, an inspection step of injecting 1 to 5 parts by weight of the residual solvent into the filling material; characterized in that it further comprises
A method for preparing a liquid pigment colorant composition for circulating dye. A liquid pigment colorant composition for primitive use prepared by the method according to any one of claims 1 and 4.

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