Method for producing pigment composition

Abstract

The problem to be solved by the present invention is to provide a method for producing a pigment composition that can reduce the number of coarse particles that may be contained in the pigment composition and improve the production efficiency of the pigment composition. [Solution] The present invention relates to a method for producing a pigment composition in which a pigment is dispersed in a liquid medium by a pigment dispersing resin, by subjecting a raw material composition containing a pigment, a pigment dispersing resin, and a liquid medium to process in a dispersing machine in step 1, wherein the dispersing machine is configured to cause the raw material compositions to collide with each other.

Description

[Technical field]

[0001] The present invention relates to a method for producing a pigment composition. [Background technology]

[0002] Pigment compositions are used in various printing processes such as inkjet printing, etc. As a method for producing a pigment composition, a method is known in which a raw material composition containing a pigment component and a liquid medium is treated with a dispersing machine to obtain the pigment composition (for example, see Patent Document 1 below). [Prior art documents] [Patent documents]

[0003] [Patent Document 1] JP 2001-262038 A Summary of the Invention [Problem to be solved by the invention]

[0004] In order to obtain good ejection stability by suppressing clogging of ejection nozzles during printing, it is required that the pigment composition contains a small number of coarse particles. In order to reduce the number of coarse particles, it is effective to subject a raw material composition containing a pigment, a pigment dispersing resin and a liquid medium to a long-term dispersion treatment or to repeatedly feed the composition into a dispersing machine and treat it. However, in the above-mentioned methods, there are cases where the production efficiency of pigment compositions, inks, etc. cannot be improved.

[0005] The problem to be solved by the present invention is to provide a method for producing a pigment composition that can reduce the number of coarse particles that may be contained in the pigment composition and improve the production efficiency of the pigment composition. [Means for solving the problem]

[0006] The present invention relates to a method for producing a pigment composition in which a pigment is dispersed in a liquid medium by a pigment dispersing resin, by subjecting a raw material composition containing a pigment, a pigment dispersing resin, and a liquid medium to a step 1 of treating the raw material composition with a dispersing machine, wherein the dispersing machine is configured to collide particles of the raw material composition with each other. Effect of the Invention

[0007] According to the method for producing a pigment composition of the present invention, it is possible to reduce the number of coarse particles having a particle diameter of 1.0 μm or more that may be contained in the pigment composition, while improving the production efficiency of the pigment composition. [Brief description of the drawings]

[0008] [Figure 1] FIG. 2 is a schematic cross-sectional view showing an example of a rotor-stator type processing machine. [Diagram 2] FIG. 2 is a schematic side view showing an example of a stator in a rotor-stator type processing machine. [Diagram 3] FIG. 2 is a schematic diagram for explaining a pulverization or crushing process in a rotor-stator type processor. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0009] Hereinafter, the embodiments of the present invention will be described in detail. However, the present invention is not limited to the following embodiments, and various modifications can be made within the scope of the present invention.

[0010] In this specification, a numerical range indicated using "~" indicates a range including the numerical values ​​described before and after "~" as the minimum and maximum values, respectively. In the numerical ranges described in stages in this specification, the upper limit or lower limit of a numerical range of a certain stage can be arbitrarily combined with the upper limit or lower limit of a numerical range of another stage. In the numerical ranges described in this specification, the upper limit or lower limit of the numerical range may be replaced with a value shown in the examples. "A or B" may include either A or B, or may include both. Unless otherwise specified, the materials exemplified in this specification may be used alone or in combination of two or more types. When a plurality of substances corresponding to each component are present in the composition, the content of each component in the composition means the total amount of the plurality of substances present in the composition, unless otherwise specified. The term "process" includes not only independent processes, but also processes that cannot be clearly distinguished from other processes as long as the intended action of the process is achieved. The term "(meth)acrylic acid" is a general term for acrylic acid and the corresponding methacrylic acid, and the same applies to other similar expressions such as "(meth)acrylate."

[0011] The method for producing a pigment composition of the present invention is a method for producing a pigment composition in which a raw material composition containing a pigment, a pigment dispersion resin, and a liquid medium is treated with a dispersing machine in step 1, and the pigment is dispersed in a liquid medium by the pigment dispersion resin. In this case, the dispersing machine is characterized in that a dispersing machine having a configuration for causing the raw material compositions to collide with each other is used. According to the method for producing a pigment composition of the present invention, it is possible to reduce the number of coarse particles having a particle diameter of 1.0 μm or more that may be contained in a pigment composition in which a pigment is dispersed in a liquid medium by a pigment dispersion resin, and to improve the production efficiency of the pigment composition. When producing a pigment composition, a dispersing machine having a configuration for causing the raw material compositions to collide with a hard body can generally be used, but in order to avoid wear of the hard body during long-term use, to reduce the number of coarse particles by exhibiting excellent micronization ability, to obtain a pigment composition with excellent storage stability, or to obtain a pigment composition capable of producing printed matter with even higher print density, it is preferable to use a dispersing machine having a configuration for causing the raw material compositions to collide with each other alone or in combination with another dispersing machine.

[0012] As described above, the pigment composition refers to a pigment dispersed or dissolved in a liquid medium such as water by a pigment dispersing resin (for example, an aqueous pigment dispersion). The pigment composition may be used as a material for producing an ink, or the pigment composition itself may be used as an ink. For example, the pigment composition is preferably used for producing a printing ink or the printing ink, and more preferably used for producing an inkjet printing ink or the inkjet printing ink. When the pigment composition is used for producing an inkjet printing ink, the ratio of solid content of the pigment composition to the total amount of the pigment composition is preferably in the range of 1 mass % to 50 mass %, and more preferably in the range of 10 mass % to 30 mass %.

[0013] Among the dispersers, as a disperser having a configuration for colliding the raw material compositions with each other, it is particularly preferable to use a disperser having a configuration for colliding the raw material compositions with each other obliquely in order to simultaneously reduce the number of coarse particles in the pigment composition, reduce the dispersed particle diameter, and improve the production efficiency of the pigment composition. More specifically, by using a disperser having a configuration for colliding the raw material compositions with each other obliquely, the number of times (so-called number of passes) for repeatedly feeding the raw material composition into the disperser and processing it can be significantly reduced from the conventional approximately 10 to 30 times to preferably 1 to 8 times, more preferably 1 to 5 times, and particularly preferably 1 to 3 times. In particular, when carbon black is used as a pigment component, a pigment composition that achieves both a reduction in the number of coarse particles and a reduction in the dispersed particle diameter can be obtained with only one pass. An example of a configuration for colliding the raw material compositions with each other obliquely is an oblique collision chamber. When the disperser is used, the raw material compositions can be pressurized and sprayed from multiple directions to collide the raw material compositions with each other. An example of the oblique impingement chamber is a chamber with the device name "Starburst" manufactured by Sugino Machine Co., Ltd. The oblique impingement chamber can avoid wear of the hard body described below during long-term use and can obtain a shear force superior to that of a single nozzle chamber, and is therefore preferable for obtaining a pigment composition that exhibits excellent micronization ability, reduces the number of coarse particles, and has excellent storage stability, or for obtaining a pigment composition that can produce printed matter with even higher print density. Specifically, the dispersing machine may be manufactured by Sugino Machine Co., Ltd. under the name "Starburst."

[0014] In addition, the dispersing machine used in the present invention is preferably a so-called high-pressure homogenizer capable of applying a pressure in the range of 50 to 245 MPa when spraying the raw material composition, in order to simultaneously reduce the number of coarse particles in the pigment composition and improve the production efficiency of the pigment composition. The pressure is more preferably 80 to 200 MPa, further preferably 100 to 200 MPa, and particularly preferably 130 to 200 MPa. When the pigment component contains carbon black, a pigment composition that can be ejected by inkjet at low pressure and has excellent storage stability can be obtained, and it is easy to achieve a long life of the device and an improvement in the production volume per unit time.

[0015] The raw material composition may contain solids such as a pigment and a pigment dispersion resin, a liquid medium, and other additives. The pigment composition may contain the same type of components as the raw material composition. The solid content of the raw material composition may be 1 to 60 mass%, 10 to 50 mass%, or 15 to 40 mass%, based on the total amount of the raw material composition.

[0016] The raw material composition may be a mixture of the pigment, the pigment dispersion resin, and the liquid medium. In particular, the raw material composition may be a mixture of the pigment, the pigment dispersion resin, and the liquid medium in advance by a rotor-stator type processor or a bead mill processor prior to the step 1, which is preferable in that the number of times the raw material composition is repeatedly fed into the disperser for processing in the step 1 can be significantly reduced, and as a result, the production efficiency of the pigment composition and the ink can be significantly improved. The term "crushing" refers to, for example, a process for breaking up agglomerates. The term "cracking" refers to, for example, a process for breaking up aggregates. Prior to step 1, step 0 is a step in which the pigment, pigment dispersion resin, and liquid medium are mixed in advance using a rotor-stator type processor or a bead mill processor, and this step is also a step in which the pigment is pulverized or crushed. There is a concern that problems such as clogging of pipes may occur in the disperser when a raw material composition containing a large amount of coarse particles is treated with the disperser in step 1. Therefore, from the viewpoint of avoiding such problems, it is effective to carry out step 0 of preliminary pulverization or preliminary crushing as a pretreatment prior to the step of dispersing the pigment in a liquid medium with a pigment dispersion resin using the disperser in step 1.

[0017] Examples of the processing machine that can be used in step 0 include a rotor-stator type processing machine, a bead mill processing machine, an ultrasonic disperser, a disperser, and the like. The use of a rotor-stator type processing machine is preferred because it allows the pigment to be pulverized or disintegrated more efficiently, and as a result, a pigment composition in which the number of coarse particles is reduced can be efficiently produced.

[0018] In the rotor-stator type processor, as described below, a shear force is applied between the rotor and the stator to the raw material composition containing coarse particles, so that the coarse particles are pulverized or disintegrated. Therefore, by performing step 0 using the rotor-stator type processor and then performing step 1, the number of coarse particles in the pigment composition can be reduced more efficiently, and the number of coarse particles having a particle diameter of 1.0 μm or more can be further reduced. In addition, by performing step 1 using the rotor-stator type processor and then performing step 0, the increase in the processing time required to obtain a pigment composition having a small number of coarse particles can be suppressed, and a pigment composition having a small number of coarse particles can be obtained with good productivity. In addition, by performing step 1 using the rotor-stator type processor and then performing step 0, the number of coarse particles having a particle diameter of 0.5 μm or more can also be reduced. When evaluating the reduction rate of the number of coarse particles, the reduction rate of the number of coarse particles when a raw material composition having the same composition is pulverized or disintegrated is compared. When treating the pigment composition with various types of treating machines, the performance difference between the treating machines can be compared by using a rotation speed that is about 80% of the maximum rotation speed.

[0019] By carrying out step 0 using the rotor stator type processor and then carrying out step 1, the number of coarse particles in the pigment composition can be efficiently reduced while reducing the viscosity of the pigment composition. By carrying out step 1 after carrying out step 0 using the rotor stator type processor, the particle size of the solid content in the pigment composition obtained by the pulverization or crushing treatment can be reduced. By carrying out step 1 after carrying out step 0 using the rotor stator type processor, the pigment composition obtained by the pulverization or crushing treatment can have excellent storage stability (dispersion stability of the solid content).

[0020] By performing step 0 using the rotor-stator type processor and then step 1, a high print density can be obtained when compared under conditions where the pigment composition and the mass ratio of the pigment dispersion resin to the pigment component are the same. Also, by performing step 0 using the rotor-stator type processor and then step 1, a high adsorption rate of the pigment dispersion resin to the pigment component can be obtained.

[0021] In the present invention, it is possible to efficiently further reduce the number of coarse particles in the pigment composition by using a processing machine such as a rotor-stator type processor or a bead mill processor in step 0, using a raw material composition in which the pigment has been ground or crushed in advance, and going through step 1. In addition, by using a processing machine such as a rotor-stator type processor or a bead mill processor in step 0, using a raw material composition in which the pigment has been ground or crushed in advance, and going through step 1, it is possible to shorten the time required to produce a pigment composition having desired physical properties of the solid content (number of coarse particles, particle size, etc.).

[0022] The temperature in the treatment step using the treatment machine in the step 0 is preferably in the following range from the viewpoint of efficiently reducing the number of coarse particles, shortening the time required to obtain a pigment composition having the desired physical properties (number of coarse particles, particle diameter, etc.) of the solid content through the step 1, and promoting dissolution of the pigment dispersion resin to improve the adsorption rate of the pigment dispersion resin to the pigment component, thereby easily obtaining excellent storage stability. The temperature is preferably 25°C or higher, more preferably 30°C or higher, even more preferably 40°C or higher, particularly preferably 50°C or higher, extremely preferably 55°C or higher, and very preferably 60°C or higher. The temperature is preferably 80°C or lower, more preferably 75°C or lower, even more preferably 70°C or lower, particularly preferably 65°C or lower, and extremely preferably 60°C or lower. From these viewpoints, the temperature is preferably 25 to 80°C, more preferably 50 to 80°C, and even more preferably 60 to 80°C.

[0023] The rotor-stator type processor usable in the step 0 includes a rotor having a rotatable blade portion and a stator having a wall portion disposed on the outer periphery of the blade portion. The processor may be any of a pulverizer, a crusher, a disperser, etc. The rotor and stator may be of any shape that is commercially available, and may be used in combination with different shapes or the same shape. Since the transportability of the raw material composition, the shear rate (refining ability), the amount of heat generated during refining, etc. differ depending on the shape, a combination can be selected according to the properties of the raw material composition. Usually, a rotor with a large number of teeth is easier to refining and generates a large amount of heat.

[0024] FIG. 1 (FIG. 1(a) and FIG. 1(b)) is a schematic cross-sectional view showing an example of a rotor-stator type processor. The rotor-stator type processor 100 shown in FIG. 1 includes a central shaft 10, a rotor 20, and a stator 30. Constituent materials of the central shaft 10, the rotor 20, and the stator 30 include metal materials, ceramics, and the like.

[0025] The central shaft 10 is an elongated member that extends, for example, in the vertical direction. The central shaft 10 supports the rotor 20 and the stator 30.

[0026] The rotor 20 has an annular (e.g., circular) blade portion 22 extending in the longitudinal direction of the central axis 10 on the outer periphery of the rotor 20, and a connection portion 24 connecting the blade portion 22 and the central axis 10. The blade portion 22 can rotate around the central axis 10. The blade portion 22 has an opening (through hole) 22a penetrating the blade portion 22, and has, for example, a plurality of openings 22a at intervals (e.g., equal intervals) along the circumferential direction of the blade portion 22. The opening direction of the openings 22a may be inclined with respect to the radial direction. The end of the openings 22a on the upper side in the vertical direction may be open without any member constituting the rotor 20 being disposed therein. The number, arrangement, and shape of the openings 22a are not particularly limited.

[0027] The arrangement and shape of the blade part in the rotor of the rotor-stator type processing machine are not particularly limited. For example, the blade part is not limited to an annular member arranged on the outer periphery of the rotor, and may have a shape extending from the center to the outer periphery of the rotor. The rotor may have a plurality of blade parts extending from the center to the outer periphery of the rotor. The blade part extending from the center to the outer periphery of the rotor may have a streamlined shape.

[0028] The stator 30 has an annular (e.g., circular) wall portion 32 extending in the longitudinal direction of the central axis 10 at the outer periphery of the stator 30, and a connection portion 34 connecting the wall portion 32 and the central axis 10. The wall portion 32 is disposed on the outer periphery side of the blade portion 22 in the rotor-stator type processor 100. The wall portion 32 has an opening (through hole) 32a penetrating the wall portion 32, and has, for example, a plurality of openings 32a spaced apart (e.g., equally spaced) along the circumferential direction of the wall portion 32. The opening direction of the openings 32a may be inclined with respect to the radial direction.

[0029] The number, arrangement and shape of the openings in the wall of the stator are not particularly limited. Figure 2 is a schematic side view showing an example of a stator (wall of the stator) in a rotor-stator type processing machine. Examples of the wall of the stator include a wall having an array of openings (e.g., rectangular openings such as square openings) (Figure 2(a)), a wall having a plurality of rectangular openings arranged in a row (Figure 2(b)), and a wall having a plurality of circular (e.g., perfect circle) openings arranged in a row (Figure 2(c)). Examples of the shape of the opening include a rectangular shape (square, rectangular, etc.), a circular shape (perfect circle, ellipse, etc.), and the like.

[0030] The stator may have a plurality of annular (e.g., annular) walls extending in the longitudinal direction of the central axis at the outer periphery of the stator. For example, the stator may have the above-mentioned wall 32 as a first wall, a second wall disposed on the outer periphery of the first wall in the rotor-stator type processor, and a third wall disposed on the outer periphery of the second wall in the rotor-stator type processor. The number of walls is not particularly limited, and may be four or more.

[0031] Fig. 3 is a schematic diagram for explaining the pulverization or crushing process in the rotor-stator type processor, and is a schematic diagram showing an enlarged portion of the outer periphery of the rotor-stator type processor 100 shown in Fig. 1. In the rotor-stator type processor 100, for example, a raw material composition containing a pigment component and a liquid medium is supplied around the central axis 10, and then, as shown in Fig. 3, the raw material composition passes through the opening 22a of the blade portion 22 of the rotor 20 (flow path F1 in the figure) and reaches the space between the blade portion 22 and the wall portion 32 of the stator 30. In this space, a shear force caused by the rotational motion of the blade portion 22 is applied to the coarse particles P (solid content), so that the coarse particles P are pulverized or crushed. Thereafter, a portion of the composition containing the crushed or disintegrated particles flows out through the openings 32a of the wall 32 (flow path F2 in the figure) to the outer periphery of the wall 32, and the remainder of the composition advances further through the space between the blade portion 22 and the wall 32, where the particles are further crushed or disintegrated by shear force. As a result, the pigment component in the raw material composition containing the pigment component and a liquid medium is crushed or disintegrated by the crushing or disintegrating process of the rotor-stator type processor 100.

[0032] The shear rate (refining ability) given by the treatment section constituted by the rotor and the stator is set to 50,000 s from the viewpoints of easily efficiently reducing the number of coarse particles, easily reducing the particle size of the solid content after treatment, easily reducing the viscosity of the pigment composition, and easily obtaining excellent storage stability in the pigment composition. -1 More than 75000s is preferable. -1 More than 90,000 is preferable. -1 More preferably, 100,000s -1 More than 120,000s is particularly preferable. -1 More than 150,000s is highly preferable. -1 More than 170,000s are highly preferred -1 More preferably, the upper limit of the share rate is, for example, 400,000 s -1 may be less than or equal to 250000s -1 From these viewpoints, the share rate may be 50,000 to 400,000 s -1is preferred. -1 ] can be obtained by dividing the peripheral speed of the rotor blades [m / s] by the distance [m] between the blades and the stator wall.

[0033] The rotor-stator type processor may have a plurality of processing sections (pulverizing sections or disintegrating sections) composed of rotors and stators. By flowing the raw material composition from a processing section with a low shear rate to a processing section with a high shear rate, clogging is easily suppressed, and the number of coarse particles is easily reduced efficiently. The rotor-stator type processor may have a plurality of processing sections along a central axis extending in the vertical direction (may have a multi-stage processing section). When the rotor-stator type processor has a plurality of processing sections along the central axis, it is preferable to arrange the processing sections with a higher shear rate vertically downward from the viewpoint of easily reducing the number of coarse particles efficiently.

[0034] The rotor-stator type processor may be an in-line processor or a batch processor. In an in-line processor, the raw material composition is continuously supplied, and for example, a processor is installed in the middle of a processing path (for example, a grinding processing path and a crushing processing path, for example, a pipe), and the raw material composition can be continuously processed (grinding or crushing). In an in-line processor, the raw material composition is forced to pass through the processor in its entirety, so that the raw material composition can be uniformly processed in a short time compared to a batch processor in which only the rotor periphery is mainly processed. According to an in-line processor, the number of coarse particles can be efficiently reduced, so that clogging of the pipes of the processor used in the step 0 can be easily suppressed. In particular, the use of an in-line processor as the rotor-stator type processor can more effectively reduce the number of coarse particles having a diameter of 0.5 μm or more contained in the pigment composition finally obtained, compared to the case where a batch processor is used alone. According to an in-line processor, the viscosity of the pigment composition can be easily reduced. In an in-line processor, the raw material composition may be circulated. In a batch type processor, the raw material composition is intermittently supplied, and the raw material composition is replaced for each treatment (pulverization or crushing treatment).

[0035] Examples of rotor-stator type processors include "magic LAB" manufactured by IKA Co., Ltd. (in-line type, maximum peripheral speed: 41 m / s, maximum rotation speed: 26000 rpm); "VERSO" manufactured by Silverson Nippon Co., Ltd. (high shear in-line mixer, in-line type, maximum peripheral speed: 20 m / s, maximum rotation speed: 10000 rpm); and "L5M-A" manufactured by Silverson Nippon Co., Ltd. (batch type, maximum peripheral speed: 20 m / s, maximum rotation speed: 10000 rpm). Processors manufactured by IKA Co., Ltd. that can be used include processors equipped with a UTR module (ULTRA-TURRAX), DR module (DISPAX-REACTOR), MK module, MKO module, and CMX module. The DR module has three stages of processors (stages) consisting of rotors and stators, and the shear rate can be adjusted by the combination of rotors and stators, making it easy to efficiently reduce the number of coarse particles. For example, by using 2P / 4M / 6F processing units in this order from the top in the vertical direction, processing units with higher share rates can be arranged vertically downward.

[0036] The rotor-stator type processor preferably has a rotation speed in the range of 1,000 to 30,000 rpm, more preferably in the range of 3,000 to 25,000 rpm, and is particularly preferably in the range of 8,000 to 20,000 rpm, from the viewpoints of easily efficiently reducing the number of coarse particles, easily reducing the particle size of the solid content after treatment, easily reducing the viscosity of the pigment composition, and easily obtaining excellent storage stability of the pigment composition.

[0037] The rotor-stator type treating machine to be used has a peripheral speed in the range of preferably 5 m / s to 50 m / s, more preferably 10 m / s to 40 m / s, and is particularly preferably 15 m / s to 35 m / s, from the viewpoints of easily efficiently reducing the number of coarse particles, easily reducing the particle size of the solid content after treatment, easily reducing the viscosity of the pigment composition, and easily obtaining excellent storage stability of the pigment composition.

[0038] The raw material supplying section in the production apparatus for the pigment composition according to the present embodiment is not particularly limited as long as it can supply the raw material composition to the rotor-stator type processor. The raw material supplying section may be a pipe, a pump, or the like that supplies the raw material supplying section.

[0039] As the bead mill dispersing machine, for example, a paint shaker, a bead mill, a sand mill, a basket mill, a dyno mill, an SC mill, a nano mill, a spike mill, an agitator mill, etc. can be used.

[0040] As the pigment component, at least one selected from the group consisting of pigments and pigment derivatives can be used.

[0041] As the pigment, inorganic or organic pigments can be used. Examples of inorganic pigments include iron oxide, carbon black (e.g., carbon black produced by known methods such as contact method, furnace method, and thermal method), and titanium oxide. Examples of organic pigments include azo pigments (insoluble azo pigments (monoazo pigments, disazo pigments, pyrazolone pigments, etc.), benzimidazolone pigments, beta naphthol pigments, naphthol AS pigments, condensed azo pigments, etc.), polycyclic pigments (quinacridone pigments, perylene pigments, perinone pigments, anthraquinone pigments, dioxazine pigments, thioindigo pigments, isoindolinone pigments, isoindoline pigments, quinophthalone pigments, diketopyrrolopyrrole pigments, etc.), phthalocyanine pigments, dye chelates (basic dye chelates, acid dye chelates, etc.), nitro pigments, nitroso pigments, and aniline black. These inorganic and organic pigments can be suitably used in the production of printing inks (e.g., inkjet printing inks). The pigments may be used alone or in combination of two or more.

[0042] Examples of carbon black that can be used include #2300, #980, #960, #900, #52, #45L, #45, #40, #33, MA100, MA8, and MA7 manufactured by Mitsubishi Chemical Corporation; Regal series and Monarch series manufactured by Cabot Corporation; and Color Black FW1, Color Black series, Printex series, Special Black series, and NIPEX series manufactured by Orion Engineered Carbons Co., Ltd.

[0043] As the pigment, yellow pigments such as CI Pigment Yellow 1, 2, 12, 13, 14, 16, 17, 73, 74, 75, 83, 93, 95, 97, 98, 109, 110, 114, 120, 128, 129, 138, 150, 151, 154, 155, 174, 180, and 185 can be used.

[0044] As the pigment, magenta pigments such as CI Pigment Red 5, 7, 12, 48(Ca), 48(Mn), 57(Ca), 57:1, 112, 122, 123, 146, 149, 150, 168, 176, 184, 185, 202, 209, 213, 269, and 282 can be used.

[0045] As the pigment, cyan pigments such as CI Pigment Blue 1, 2, 3, 15, 15:1, 15:2, 15:3, 15:4, 15:6, 16, 22, 60, 63, and 66 can be used.

[0046] As the pigment, orange pigments such as CI Pigment Orange 5, 13, 16, 17, 34, 36, 43, 51, 64, and 71 can be used.

[0047] As the pigment, violet pigments such as CI Pigment Violet 1, 3, 5:1, 16, 19, 23, and 38 can be used.

[0048] As the pigment, green pigments such as CI Pigment Green 1, 4, 7, 8, 10, 17, 18, 36, 50, and 58 can be used.

[0049] As the pigment, a dry pigment (pigment in a dry powder state) or a wet pigment (pigment in a wet cake state) can be used. As the magenta pigment, a wet pigment is preferred from the viewpoint of efficiently reducing the number of coarse particles and from the viewpoint of easily shortening the time required to obtain a pigment composition having the desired physical properties of the solid content (number of coarse particles, particle diameter, etc.) through the above step 1. As the cyan pigment, a dry pigment is preferred from the viewpoint of efficiently reducing the number of coarse particles and from the viewpoint of easily shortening the time required to obtain a pigment composition having the desired physical properties of the solid content (number of coarse particles, particle diameter, etc.) through the above step 1. As the pigment, a mixture or solid solution containing two or more kinds can also be used.

[0050] As the pigment derivative, a compound in which a functional group is introduced into a pigment can be used. Examples of pigments that provide the pigment derivative include phthalocyanine pigments, azo pigments, anthraquinone pigments, quinacridone pigments, diketopyrrolopyrrole pigments, and the like. Examples of the functional group include a carboxy group, a sulfo group, an amino group, a nitro group, an acid amide group, a carbonyl group, a carbamoyl group, a phthalimide group, and a sulfonyl group. The pigment derivative can impart dispersion stability to the pigment composition or ink that can prevent the generation of coarse particles over time and the occurrence of precipitation of pigment components and the like over time.

[0051] The primary particle size of the pigment component is preferably 1.0 μm or less, and more preferably 0.01 to 0.5 μm, from the viewpoint of more effectively suppressing sedimentation of the pigment component over time. The primary particle size refers to the number average particle size measured using a transmission electron microscope (TEM).

[0052] The pigment component is preferably 1 to 50% by mass, more preferably 10 to 30% by mass, and even more preferably 15 to 25% by mass, based on the total amount of the raw material composition. In these cases, since it is easy to obtain an appropriate fluidity, efficient and uniform treatment can be performed in each process, excellent storage stability that prevents the occurrence of sedimentation of solids in the pigment composition over time is easily obtained, the occurrence of sedimentation of solids in the ink over time is easily prevented, clogging of the ink discharge nozzle at the beginning of ink discharge and the like is easily suppressed (excellent initial discharge stability is easily obtained), and clogging of the ink discharge nozzle over time is easily suppressed (excellent discharge stability over time is easily obtained).

[0053] Examples of the liquid medium include an aqueous medium (such as water), an organic solvent, etc. When a high-pressure homogenizer is used as the dispersing machine used in the present invention, it is preferable to use a high-boiling point solvent (for example, a solvent having a boiling point of 100° C. or higher) because of the high pressure applied.

[0054] Examples of water include pure water such as ion-exchanged water, ultrafiltered water, reverse osmosis water, distilled water, etc.; ultrapure water, etc. As the water, it is preferable to use water that has been sterilized by ultraviolet irradiation, addition of hydrogen peroxide, etc., from the viewpoint of easily preventing the growth of mold or bacteria when the pigment composition or ink is stored for a long period of time. The water is preferably used in an amount of 10 to 90% by mass, based on the total amount of the liquid medium contained in the pigment composition of the present invention, and is preferably used in an amount of 15 to 80% by mass in terms of producing an aqueous ink.

[0055] As the organic solvent, a water-soluble organic solvent can be used. The water-soluble organic solvent can efficiently wet the surface of the pigment component, and the resin component (e.g., a neutralized resin) dissolved in water can be easily adsorbed to the pigment component, which can shorten the time required to achieve the desired physical properties.

[0056] Examples of the water-soluble organic solvent include glycols such as ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propylene glycol, dipropylene glycol, tripropylene glycol, polyethylene glycol, and polypropylene glycol; diols such as butanediol, pentanediol, and hexanediol; glycol esters such as propylene glycol laurate; diethylene glycol ethers such as diethylene glycol monoethyl, diethylene glycol monobutyl, diethylene glycol monohexyl, and carbitol; glycol ethers such as cellosolve containing propylene glycol ether, dipropylene glycol ether, or triethylene glycol ether; alcohols (excluding glycols) such as methanol, ethanol, isopropyl alcohol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, butyl alcohol, and pentyl alcohol; lactones such as sulfolane, esters, ketones, and γ-butyrolactone; lactams such as N-(2-hydroxyethyl)pyrrolidone and 2-pyrrolidone; and glycerin and its polyalkylene oxide adducts. The water-soluble organic solvents may be used alone or in combination of two or more.

[0057] The content of the water-soluble organic solvent is preferably 10 to 500 parts by mass, more preferably 15 to 200 parts by mass, and more preferably 15 to 150 parts by mass, relative to 100 parts by mass of the pigment component contained in the raw material composition. By using a water-soluble organic solvent in the above range, the adsorption rate of the resin component to the surface of the pigment component is improved, and it is easy to obtain excellent storage stability that prevents the occurrence of precipitation of solids over time in the pigment composition, it is easy to prevent the occurrence of precipitation of solids over time in the ink, it is easy to suppress the occurrence of clogging of the ink ejection nozzle at the beginning of ink ejection (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the occurrence of clogging of the ink ejection nozzle over time (it is easy to obtain excellent ejection stability over time). Examples of water-soluble organic solvents that can improve the adsorption rate include triethylene glycol, glycerin, 2-pyrrolidone, 1-(2-hydroxyethyl)-2-pyrrolidone, dipropylene glycol, propylene glycol, and 1,5-pentanediol. Furthermore, when a high-pressure homogenizer is used in producing the pigment composition, or when an inkjet printing ink obtained using the pigment composition is applied to a thermal-type inkjet printing method described below, it is preferable to use a high-boiling point solvent having a boiling point of 100° C. or more as the organic solvent. Furthermore, using a high-boiling point solvent having a boiling point of 100° C. or more as the organic solvent is preferable in that it promotes wetting of the pigment, making it easier for the resin to be adsorbed to the pigment and improving storage stability, etc. As the high boiling point solvent, for example, glycerin, 2-pyrrolidone, 1-(2-hydroxyethyl)-2-pyrrolidone, dipropylene glycol, propylene glycol, 1,5-pentanediol, etc. can be used.

[0058] The liquid medium has a dispersion term (δD 1 ) and polar term (δP 1 ) and the hydrogen bond term (δH 1It is preferable to use a liquid medium comprising The dispersion term (δD 1 ) is preferably in the range of 12 to 24, more preferably 14 to 21, and particularly preferably 16 to 19. The polar term (ΔP 1 ) is preferably in the range of 4 to 17, more preferably 6 to 15, and particularly preferably 8 to 13. The hydrogen bond term (δH 1 ) is preferably in the range of 6 to 43, more preferably 9 to 35, and particularly preferably 9 to 30. Dispersion term (δD 1 ) and polar term (δP 1 ) and the hydrogen bond term (δH 1 ) Examples of the liquid medium that can be used include triethylene glycol, glycerin, 2-pyrrolidone, 1-(2-hydroxyethyl)-2-pyrrolidone, dipropylene glycol, propylene glycol, and 1,5-pentanediol. In addition, the dispersion term of the liquid medium (δD 1 ) and polar term (δP 1 ) and the hydrogen bond term (δH 1 ) are values ​​recorded in the computer software Hansen Solubility Parameters in Practice 4th Edition 4.1.07 (HSPiP). The dispersion term (δD 1 ) and polar term (δP 1 ) and the hydrogen bond term (δH 1 The liquid medium having the above components is preferably used in an amount of 10 to 95% by mass, and more preferably 50 to 80% by mass, based on the total amount of the liquid medium contained in the pigment composition.

[0059] The liquid medium contained in the pigment composition is preferably used in a range of 30 to 98 mass % based on the total amount of the pigment composition of the present invention, and is preferably used in a range of 60 to 95 mass % in terms of producing an aqueous ink. The liquid medium used in the pigment composition of the present invention is the above-mentioned water, the above-mentioned high boiling point solvent, the above-mentioned dispersion term (δD 1 ) and polar term (δP 1 ) and the hydrogen bond term (δH 1 In particular, when a high-pressure homogenizer is used in producing the pigment composition of the present invention, or when an inkjet printing ink obtained using the pigment composition is applied to a thermal-type inkjet printing method described below, it is preferable to use the water as the liquid medium in combination with a liquid medium having a high boiling point solvent or a dispersion term (δD 1 ) and polar term (δP 1 ) and the hydrogen bond term (δH 1 It is preferable to use the pigment in combination with a liquid medium having the above-mentioned properties, since this promotes wetting of the pigment, and as a result, the resin is easily adsorbed onto the pigment, thereby improving storage stability, etc.

[0060] From the viewpoint of easily and efficiently reducing the number of coarse particles and easily shortening the time required to obtain a pigment composition having desired physical properties of the solid content (e.g., the number of coarse particles, particle size, etc.) through step 1, it is preferable that the liquid medium satisfy at least one of the following: The liquid medium preferably contains at least one selected from the group consisting of glycols, lactams, and glycerin. The liquid medium preferably contains at least one selected from the group consisting of triethylene glycol, triethylene glycol, and dipropylene glycol. The liquid medium preferably contains at least one selected from the group consisting of N-(2-hydroxyethyl)pyrrolidone and 2-pyrrolidone. When the pigment component contains carbon black, the liquid medium preferably contains at least one selected from the group consisting of N-(2-hydroxyethyl)pyrrolidone, 2-pyrrolidone, triethylene glycol, and glycerin. When the pigment component contains a magenta pigment, the liquid medium preferably contains at least one selected from the group consisting of 2-pyrrolidone, triethylene glycol, dipropylene glycol, and glycerin. When the pigment component contains a cyan pigment, the liquid medium (a) preferably contains at least one selected from the group consisting of dipropylene glycol, N-(2-hydroxyethyl)pyrrolidone, 2-pyrrolidone, triethylene glycol, and glycerin. When the pigment component contains a yellow pigment, the liquid medium (a) preferably contains at least one selected from the group consisting of propylene glycol, N-(2-hydroxyethyl)pyrrolidone, 2-pyrrolidone, triethylene glycol, and glycerin.

[0061] The content of the water-soluble organic solvent is preferably 10 to 500 parts by mass, and more preferably 15 to 150 parts by mass, relative to 100 parts by mass of the pigment component. In these cases, it is easy to obtain excellent storage stability that prevents the occurrence of sedimentation of solids in the pigment composition over time, it is easy to prevent the occurrence of sedimentation of solids in the ink over time, it is easy to suppress the occurrence of clogging of the ink ejection nozzle at the beginning of ink ejection (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the occurrence of clogging of the ink ejection nozzle over time (it is easy to obtain excellent ejection stability over time). The liquid medium is preferably used in an amount of 30 to 98% by mass, and more preferably 60 to 95% by mass, based on the total amount of the pigment composition of the present invention, in terms of producing an aqueous ink.

[0062] The raw material composition may contain a resin component. Examples of the resin component include a pigment dispersion resin and a binder resin. As the resin component, a conventionally known resin may be used, but for example, a radical polymer may be used, and it is preferable to use a radical polymer having an aromatic cyclic structure or a heterocyclic structure. In this case, the resin component is easily adsorbed to the pigment component by the π-π interaction between the resin component and the pigment component, and excellent storage stability that prevents the occurrence of precipitation of solids over time in the pigment composition is easily obtained, the occurrence of precipitation of solids over time in the ink is easily prevented, clogging of the ink discharge nozzle at the beginning of ink discharge, etc. is easily suppressed (excellent initial discharge stability is easily obtained), and clogging of the ink discharge nozzle over time is easily suppressed (excellent discharge stability over time is easily obtained).

[0063] When a radical polymer having an anionic group is used as the resin component (e.g., pigment dispersion resin), it is preferable to use a radical polymer (neutralized product) in which a part or all of the anionic groups are neutralized with a basic compound. The resin component becomes easily dissolved in a liquid medium containing water by neutralization, and adsorption to the surface of the pigment component is promoted, making it easy to maintain a good dispersion state. As a result, it is easy to obtain excellent storage stability that prevents the occurrence of sedimentation of solids over time in the pigment composition, it is easy to prevent the occurrence of sedimentation of solids over time in the ink, it is easy to suppress the occurrence of clogging of the ink ejection nozzle at the beginning of ink ejection (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the occurrence of clogging of the ink ejection nozzle over time (it is easy to obtain excellent ejection stability over time).

[0064] Examples of the aromatic cyclic structure or heterocyclic structure include a cyclic structure introduced into a radical polymer by using a monomer having an aromatic cyclic structure or a heterocyclic structure. The aromatic cyclic structure is preferably a benzene ring structure, and more preferably a structure derived from styrene. By using a resin component that is a radical polymer having an aromatic cyclic structure or a heterocyclic structure, the adsorption of the resin component to the pigment component can be increased, and excellent storage stability that prevents the occurrence of precipitation of solids over time in the pigment composition can be easily obtained, the occurrence of precipitation of solids over time in the ink can be easily prevented, clogging of the ink discharge nozzle at the beginning of ink discharge, etc. can be easily suppressed (excellent initial discharge stability can be easily obtained), and clogging of the ink discharge nozzle over time can be easily suppressed (excellent discharge stability over time can be easily obtained).

[0065] As the radical polymer usable as the resin component, for example, a polymer obtained by radically polymerizing various monomers can be used.

[0066] As the monomer, when an aromatic cyclic structure is to be introduced into the resin component, a monomer having an aromatic cyclic structure can be used, and when a heterocyclic structure is to be introduced, a monomer having a heterocyclic structure can be used.

[0067] Examples of monomers having an aromatic ring structure include styrene, p-tert-butyldimethylsiloxystyrene, o-methylstyrene, p-methylstyrene, p-tert-butylstyrene, p-tert-butoxystyrene, m-tert-butoxystyrene, p-tert-(1-ethoxymethyl)styrene, m-chlorostyrene, p-chlorostyrene, p-fluorostyrene, α-methylstyrene, p-methyl-α-methylstyrene, vinylnaphthalene, and vinylanthracene.

[0068] Examples of the monomer having a heterocyclic structure include vinylpyridine monomers such as 2-vinylpyridine and 4-vinylpyridine.

[0069] When a polymer having both an aromatic cyclic structure and a heterocyclic structure is used as the radical polymer, a monomer having an aromatic cyclic structure and a monomer having a heterocyclic structure can be used in combination as the monomer.

[0070] The resin component is preferably a radical polymer having an aromatic ring structure, and therefore the monomer is preferably a monomer having an aromatic ring structure, more preferably at least one selected from the group consisting of styrene, α-methylstyrene, and tert-butylstyrene.

[0071] From the viewpoint of further enhancing the adsorption of the resin component to the pigment component, the content of the monomer having an aromatic cyclic structure or a heterocyclic structure is preferably 20 mass % or more, more preferably 40 mass % or more, and even more preferably 50 to 95 mass %, based on the total amount of the monomers.

[0072] As the resin component, from the viewpoint of producing a radical polymer having an acid value in the range described below, a monomer having an anionic group can be used as the monomer.

[0073] Examples of the monomer having an anionic group include monomers having an anionic group such as a carboxy group, a sulfo group, and a phosphate group. As the monomer having an anionic group, a monomer having a carboxy group is preferable, and at least one selected from the group consisting of acrylic acid and methacrylic acid is more preferable. In these cases, it is easy to obtain excellent storage stability that prevents the occurrence of precipitation of solids over time in the pigment composition, it is easy to prevent the occurrence of precipitation of solids over time in the ink, it is easy to suppress the occurrence of clogging of the ink ejection nozzle at the beginning of ink ejection (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the occurrence of clogging of the ink ejection nozzle over time (it is easy to obtain excellent ejection stability over time).

[0074] From the viewpoint of easily obtaining a radical polymer having an acid value in the range described below, the content of the monomer having an anionic group is preferably 5 to 80 mass%, more preferably 5 to 60 mass%, and even more preferably 5 to 50 mass%, based on the total amount of monomers usable for producing the resin component.

[0075] As monomers usable for producing the resin component, in addition to the above-mentioned monomers, other monomers can be used as necessary. Examples of other monomers include methyl (meth)acrylate, n-propyl (meth)acrylate, isopropyl (meth)acrylate, n-butyl (meth)acrylate, sec-butyl (meth)acrylate, tert-butyl (meth)acrylate, 2-ethylbutyl (meth)acrylate, 1,3-dimethylbutyl (meth)acrylate, hexyl (meth)acrylate, 2-ethylhexyl (meth)acrylate, octyl (meth)acrylate, ethyl (meth)acrylate, n-butyl (meth)acrylate, 2-methylbutyl (meth)acrylate, pentyl (meth)acrylate, heptyl (meth)acrylate, nonyl (meth)acrylate, 3-ethoxypropyl (meth)acrylate, 3-ethoxybutyl (meth)acrylate, and the like. Examples of the monomers include acrylate, dimethylaminoethyl (meth)acrylate, 2-hydroxyethyl (meth)acrylate, 2-hydroxybutyl (meth)acrylate, ethyl-α-(hydroxymethyl) (meth)acrylate, dimethylaminoethyl (meth)acrylate, hydroxyethyl (meth)acrylate, hydroxypropyl (meth)acrylate, phenyl (meth)acrylate, benzyl (meth)acrylate, phenylethyl (meth)acrylate, diethylene glycol (meth)acrylate, triethylene glycol (meth)acrylate, polyethylene glycol (meth)acrylate, glycerin (meth)acrylate, bisphenol A (meth)acrylate, dimethyl maleate, diethyl maleate, vinyl acetate, and the like. These monomers can be used alone or in combination of two or more. As the other monomers, such acrylates or methacrylates can be used alone, or acrylates and methacrylates can be used in combination.

[0076] The resin component may be a polymer having a linear structure formed by radical polymerization of a monomer, a polymer having a branched (grafted) structure, a polymer having a crosslinked structure, etc. The monomer sequence in each polymer is not particularly limited, and a polymer having a random sequence or a block sequence may be used.

[0077] The polymer having a crosslinked structure can be produced by using a monomer having a crosslinkable functional group as the monomer. Examples of the monomer having a crosslinkable functional group include poly(meth)acrylates of polyhydric alcohols such as ethylene glycol di(meth)acrylate, propylene glycol di(meth)acrylate, polyethylene glycol di(meth)acrylate, poly(oxyethyleneoxypropylene) glycol di(meth)acrylate, and tri(meth)acrylate of alkylene oxide adduct of glycerin; glycidyl (meth)acrylate; and divinylbenzene.

[0078] As the resin component, a polymer having a structural unit derived from the above-mentioned monomer can be used, but a polymer obtained by polymerizing only a monomer having an anionic group and a monomer having an aromatic cyclic structure or a heterocyclic structure is preferred.

[0079] As the resin component, a polymer having a structural unit derived from styrene and a structural unit derived from (meth)acrylic acid is preferred, and at least one selected from the group consisting of a styrene-(meth)acrylic acid copolymer and a styrene-(meth)acrylic acid ester-(meth)acrylic acid copolymer is more preferred. The polymer having a structural unit derived from styrene and a structural unit derived from (meth)acrylic acid preferably has an acid value in the range described below. The aromatic ring moiety in the structural unit derived from styrene is firmly adsorbed to the surface of the pigment component, and the carboxyl group in the structural unit derived from (meth)acrylic acid has good affinity with water, so that good dispersion stabilization is easily obtained. This makes it easy to obtain excellent storage stability that prevents the occurrence of sedimentation of solids over time in the pigment composition, makes it easy to prevent the occurrence of sedimentation of solids over time in the ink, makes it easy to suppress the occurrence of clogging of the ink discharge nozzle at the beginning of ink discharge (easy to obtain excellent initial discharge stability), and makes it easy to suppress the occurrence of clogging of the ink discharge nozzle over time (easy to obtain excellent discharge stability over time).

[0080] As the styrene-(meth)acrylic acid copolymer, any of styrene-acrylic acid copolymer, styrene-methacrylic acid copolymer, and styrene-acrylic acid-methacrylic acid copolymer can be used, but at least one selected from the group consisting of styrene-acrylic acid copolymer and styrene-acrylic acid-methacrylic acid copolymer is preferred. In this case, it is easy to adjust the adsorption force with the pigment component and the dispersing force in water, and as a result, it is easy to obtain excellent storage stability that prevents the occurrence of sedimentation of solids over time in the pigment composition, it is easy to prevent the occurrence of sedimentation of solids over time in the ink, it is easy to suppress the occurrence of clogging of the ink discharge nozzle at the beginning of ink discharge (it is easy to obtain excellent initial discharge stability), and it is easy to suppress the occurrence of clogging of the ink discharge nozzle over time (it is easy to obtain excellent discharge stability over time).

[0081] In the styrene-(meth)acrylic acid copolymer, the total amount of the structural units derived from styrene, the structural units derived from acrylic acid, and the structural units derived from methacrylic acid is preferably 80 to 100 mass%, more preferably 90 to 100 mass%, based on the total amount of the structural units of the styrene-(meth)acrylic acid copolymer.

[0082] The radical polymerization rate (reaction rate) of each monomer during radical polymerization is assumed to be approximately the same, and the proportion of each monomer used (feeding ratio) is assumed to be the same as the proportion of structural units derived from each monomer that constitutes the radical polymer.

[0083] The radical polymer can be produced, for example, by radically polymerizing the above-mentioned monomers by a method such as bulk polymerization, solution polymerization, suspension polymerization, or emulsion polymerization.

[0084] When producing the radical polymer, known and commonly used polymerization initiators, chain transfer agents (polymerization degree regulators), surfactants, antifoaming agents, etc. may be used as necessary.

[0085] Examples of the polymerization initiator include 2,2'-azobis(2,4-dimethylvaleronitrile), 2,2'-azobisisobutyronitrile, 1,1'-azobis(cyclohexane-1-carbonitrile), benzoyl peroxide, dibutyl peroxide, butyl peroxybenzoate, etc. The content of the polymerization initiator is preferably 0.1 to 10 mass% based on the total amount of monomers used in the production of the radical polymer.

[0086] When using a radical polymer obtained by a solution polymerization method, the resin component can be a radical polymer that has been finely divided by removing the solvent contained in the radical polymer solution obtained by the solution polymerization method, followed by drying and pulverization. When a water-soluble organic solvent and a basic compound are used in combination, the resin component that is the finely divided radical polymer is neutralized by the basic compound in the 0th step, dissolved in a liquid medium containing a water-soluble organic solvent, and adsorption to the surface of the pigment component wetted with the liquid medium proceeds. As a result, it is easy to obtain excellent storage stability that prevents the occurrence of sedimentation of solids in the pigment composition over time, it is easy to prevent the occurrence of sedimentation of solids in the ink over time, it is easy to suppress the occurrence of clogging of the ink discharge nozzle at the beginning of ink discharge (it is easy to obtain excellent initial discharge stability), and it is easy to suppress the occurrence of clogging of the ink discharge nozzle over time (it is easy to obtain excellent discharge stability over time).

[0087] The resin component is preferably classified using a mesh sieve with a mesh size (diameter) of 1 mm or less.

[0088] The acid value of the resin component (e.g., pigment dispersion resin) is preferably 60 to 300 mgKOH / g, more preferably 80 to 250 mgKOH / g, and even more preferably 100 to 200 mgKOH / g, and it is particularly preferable to use one with an acid value of 120 to 180 mgKOH / g. In these cases, the adsorption of the resin component to the pigment component can be increased, and since it is easy to obtain a moderate affinity to a liquid medium (e.g., a liquid medium containing water and a water-soluble organic solvent), it is easy to maintain a good dispersion state. Therefore, it is easy to obtain excellent storage stability that prevents the occurrence of sedimentation of solids over time in the pigment composition, it is easy to prevent the occurrence of sedimentation of solids over time in the ink, it is easy to suppress the occurrence of clogging of the ink discharge nozzle at the beginning of ink discharge (it is easy to obtain excellent initial discharge stability), and it is easy to suppress the occurrence of clogging of the ink discharge nozzle over time (it is easy to obtain excellent discharge stability over time).

[0089] The acid value is preferably an acid value derived from an anionic group such as a carboxy group, a sulfo group, or a phosphate group. The acid value is a value measured in accordance with the Japanese Industrial Standards "K0070:1992. Testing methods for acid value, saponification value, ester value, iodine value, hydroxyl value, and unsaponifiable matter of chemical products" except that tetrahydrofuran is used instead of diethyl ether as a solvent, and refers to the amount (mg) of potassium hydroxide required to completely neutralize 1 g of the resin component.

[0090] The weight average molecular weight of the resin component (for example, pigment dispersion resin) is preferably 2000 to 40000, more preferably 5000 to 30000, further preferably 5000 to 25000, preferably in the range of 6000 to 20000, and particularly preferably in the range of 8000 to 12000. In these cases, aggregation with adjacent pigment components is suppressed, and excellent storage stability that prevents the occurrence of precipitation of solids in the pigment composition over time is easily obtained, the occurrence of precipitation of solids in the ink over time is easily prevented, clogging of the ink discharge nozzle at the beginning of ink discharge is easily suppressed (excellent initial discharge stability is easily obtained), and clogging of the ink discharge nozzle over time is easily suppressed (excellent discharge stability over time is easily obtained). The "weight average molecular weight" is a value measured by GPC (gel permeation chromatography) and is a value converted into the molecular weight of polystyrene used as a standard substance.

[0091] The content of the resin component (e.g., pigment dispersion resin) is preferably 5 to 200 parts by mass, more preferably 10 to 100 parts by mass, relative to 100 parts by mass of the pigment component. This makes it easy to maintain a good dispersion state due to sufficient affinity with a liquid medium (e.g., water), and the resin component is easy to adsorb to the pigment component, so that it is easy to obtain excellent storage stability that prevents the occurrence of sedimentation of solids in the pigment composition over time, and it is easy to prevent the occurrence of sedimentation of solids in the ink over time, and it is easy to suppress the occurrence of clogging of the ink ejection nozzle at the beginning of ink ejection (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the occurrence of clogging of the ink ejection nozzle over time (it is easy to obtain excellent ejection stability over time). In addition, the amount of free resin components that are not adsorbed to the pigment component is reduced, and the ejection properties of the ink are easily improved. Furthermore, it is easy to suppress the aggregation of the pigment component due to the free resin components, and it is easy to stabilize the ink.

[0092] The raw material composition may contain a basic compound. When the resin component has an anionic group, the basic compound neutralizes the anionic group. By neutralizing the resin component with the basic compound, the affinity of the pigment component adsorbed by the resin component to the aqueous medium is increased. As a result, it is easy to reduce coarse particles, it is easy to stabilize the dispersion state of the solid content in the pigment composition, it is easy to effectively prevent the generation of coarse particles over time, and it is easy to suppress the occurrence of precipitation of the solid content over time.

[0093] As the basic compound, inorganic basic compounds, organic basic compounds, etc. can be used. As the inorganic basic compound, hydroxides of alkali metals such as potassium and sodium; carbonates of alkali metals such as potassium and sodium; hydroxides of alkaline earth metals such as calcium and barium; carbonates of calcium and barium, etc. can be mentioned. As the organic basic compound, amino alcohols such as triethanolamine, N,N-dimethanolamine, N-ethylethanolamine, dimethylethanolamine, and N-butyldiethanolamine; morpholines such as morpholine, N-methylmorpholine, and N-ethylmorpholine; piperazines such as N-(2-hydroxyethyl)piperazine and piperazine hexahydrate; and ammonium hydroxide can be mentioned. As the basic compound, alkali metal hydroxides (potassium hydroxide, sodium hydroxide, lithium hydroxide, etc.) are preferable, and potassium hydroxide is more preferable, from the viewpoint of improving the dispersion stability of the pigment component adsorbed by the resin component in the aqueous medium because they have excellent neutralization efficiency of the resin component.

[0094] When using a resin component having an anionic group, it is preferable to use a basic compound in a range in which the neutralization rate of the resin component is 80 to 120%. In this case, the affinity of the neutralized resin component to the aqueous medium is increased, and as a result, the dispersion stability of the pigment component adsorbed by the resin component in the aqueous medium is easily improved. The neutralization rate can be calculated, for example, from the following formula. Neutralization rate [%] = ((mass of basic compound [g] × 56 × 1000) / (acid value of resin component × equivalent of basic compound × mass of resin component [g])) × 100

[0095] The pigment composition according to this embodiment can be used as an ink by diluting it to a desired concentration with the above-mentioned liquid medium and / or adding additives such as a resin component (binder such as the above-mentioned acrylic resin or polyurethane resin), a drying inhibitor, a penetrating agent, a surfactant, a preservative, a viscosity adjuster, a pH adjuster, a chelating agent, a plasticizer, an antioxidant, an ultraviolet absorber, etc. After the ink is obtained, it may be subjected to a centrifugation treatment or a filtration treatment.

[0096] Examples of the ink include paints for automobiles or building materials, and printing inks such as inkjet printing ink, offset ink, gravure ink, flexo ink, and silk screen ink. When the ink is used as an inkjet printing ink, the content of the pigment component in the ink is preferably 1 to 10 mass % based on the total amount of the ink.

[0097] As the liquid medium, a water-soluble organic solvent can be used from the viewpoint of preventing the ink from drying and adjusting the viscosity or concentration of the ink to a suitable range. As the water-soluble organic solvent, the water-soluble organic solvents described above as components of the raw material composition can be used. As the water-soluble organic solvent, from the viewpoint of increasing the permeability of the ink into the recording medium, examples of the water-soluble organic solvent include lower alcohols such as ethanol and isopropyl alcohol; ethylene oxide adducts of alkyl alcohols such as ethylene glycol hexyl ether and diethylene glycol butyl ether; and propylene oxide adducts of alkyl alcohols such as propylene glycol propyl ether.

[0098] Examples of the drying inhibitor include glycerin, ethylene glycol, diethylene glycol, triethylene glycol, triethylene glycol mono-n-butyl ether, polyethylene glycol with a molecular weight of 2000 or less, propylene glycol, dipropylene glycol, tripropylene glycol, 1,3-propylene glycol, isopropylene glycol, isobutylene glycol, 1,4-butanediol, 1,3-butanediol, 1,5-pentanediol, 1,6-hexanediol, mesoerythritol, and pentaerythritol. The drying inhibitor can be the same compound as the water-soluble organic solvent used in the raw material composition. Therefore, if a water-soluble organic solvent is already used in the raw material composition, it can also function as a drying inhibitor.

[0099] The penetrant can be used for the purpose of improving the permeability into the recording medium or adjusting the dot diameter on the recording medium. Examples of the penetrant include lower alcohols such as ethanol and isopropyl alcohol; glycol monoethers of alkyl alcohols such as ethylene glycol hexyl ether, diethylene glycol butyl ether, and propylene glycol propyl ether.

[0100] The surfactant can be used to adjust the ink properties such as surface tension. The surfactant is not particularly limited, and examples thereof include various anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, etc., and at least one selected from the group consisting of anionic surfactants and nonionic surfactants is preferred. The surfactant can be used alone or in combination of two or more types.

[0101] Examples of the anionic surfactant include alkylbenzenesulfonates, alkylphenylsulfonates, alkylnaphthalenesulfonates, higher fatty acid salts, sulfates of higher fatty acid esters, sulfonates of higher fatty acid esters, sulfates and sulfonates of higher alcohol ethers, higher alkyl sulfosuccinates, polyoxyethylene alkyl ether carboxylates, polyoxyethylene alkyl ether sulfates, alkyl phosphates, polyoxyethylene alkyl ether phosphates, etc. Specific examples of these include dodecylbenzenesulfonates, isopropylnaphthalenesulfonates, monobutylphenylphenol monosulfonates, monobutylbiphenylsulfonates, dibutylphenylphenol disulfonates, etc.

[0102] Examples of nonionic surfactants include polyoxyethylene alkyl ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene fatty acid esters, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, polyoxyethylene sorbitol fatty acid esters, glycerin fatty acid esters, polyoxyethylene glycerin fatty acid esters, polyglycerin fatty acid esters, sucrose fatty acid esters, polyoxyethylene alkylamines, polyoxyethylene fatty acid amides, fatty acid alkylol amides, alkyl alkanol amides, acetylene glycol, oxyethylene adducts of acetylene glycol, polyethylene glycol polypropylene glycol block copolymers, etc. Among these, at least one selected from the group consisting of polyoxyethylene nonylphenyl ethers, polyoxyethylene octylphenyl ethers, polyoxyethylene dodecylphenyl ethers, polyoxyethylene alkyl ethers, polyoxyethylene fatty acid esters, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, fatty acid alkylol amides, acetylene glycol, oxyethylene adducts of acetylene glycol, and polyethylene glycol polypropylene glycol block copolymers is preferred.

[0103] Other surfactants that can be used include silicone surfactants such as polysiloxane oxyethylene adducts; fluorine-based surfactants such as perfluoroalkyl carboxylates, perfluoroalkyl sulfonates, and oxyethylene perfluoroalkyl ethers; and biosurfactants such as spiculisporic acid, rhamnolipid, and lysolecithin.

[0104] As the pigment composition for ink obtained by the above method, it is preferable to use one in which 20 to 60 mass % of the resin component is adsorbed onto the pigment component, based on the total amount of the resin components, because this makes it possible to obtain a pigment composition that is less likely to cause a significant increase in viscosity over time and has very excellent storage stability. Here, the mass ratio of the resin component adsorbed onto the pigment component to the total amount of the resin components [mass of the resin component adsorbed onto the pigment component / mass of the total amount of the resin components] (hereinafter abbreviated as "resin adsorption rate") refers to a value calculated by the following method. Using a particle charge meter (Spectris Corporation, product name: PCD-04), the streaming potential was measured in the range of ±2500 mV at the platinum electrode of the sample cell. The pigment composition was placed in the sample cell and titrated with a titrant (0.01 N, Poly-DADMAC). The titration of the charge amount was performed based on the potential difference (i.e., the streaming potential of the liquid) generated by the movement of the sample cell and the moving piston. The titration was terminated when the streaming potential exceeded zero (the potential became positive). The amount of dripping from the inflection point was divided by the amount of dripping when the streaming potential became zero, and the result was multiplied by 100 to obtain the resin adsorption rate. The resin adsorption rate is more preferably in the range of 20 to 50% by mass, and particularly preferably in the range of 25 to 40% by mass, in order to produce an inkjet printing ink which has very excellent storage stability since it is unlikely to cause a significant increase in viscosity over time, and which can reduce the number of coarse particles having a particle diameter of 1.0 μm or more that may be contained in the pigment composition and which can produce printed matter with high color development. EXAMPLES

[0105] The present invention will be described in more detail below with reference to examples, but the present invention is not limited to these examples.

[0106] <Preparation of styrene-acrylic acid copolymer> (Styrene-acrylic acid copolymer A) After 100 parts by mass of methyl ethyl ketone was charged into a reaction vessel equipped with a stirring device, a dropping device, and a reflux device, the inside of the reaction vessel was replaced with nitrogen while stirring. Next, the reaction vessel was heated, and a mixture of 77 parts by mass of styrene, 10 parts by mass of acrylic acid, 13 parts by mass of methacrylic acid, and 8 parts by mass of a polymerization catalyst (manufactured by Wako Pure Chemical Industries, Ltd., product name: V-59) was dropped from the dropping device over 2 hours while the reaction vessel was heated and the methyl ethyl ketone was refluxed. The temperature of the reaction vessel was kept at 80°C from the middle of the dropping. After the dropping was completed, the reaction was continued for another 25 hours at the same temperature. After the reaction was completed, the reaction vessel was allowed to cool, and then methyl ethyl ketone was added to obtain a solution with a solid content concentration of 50% by mass. Furthermore, this solution was dried and then pulverized into powder of 1 mm or less to obtain a styrene-acrylic acid copolymer A. The acid value of the styrene-acrylic acid copolymer A was 150 mgKOH / g, and the weight average molecular weight was 8800.

[0107] The weight average molecular weight is a value measured by GPC (gel permeation chromatography) and converted into the molecular weight of polystyrene used as a standard substance. The measurement was performed using the following apparatus and conditions. Liquid delivery pump: LC-9A (Shimadzu Corporation) System controller: SLC-6B (Shimadzu Corporation) Auto injector: S1L-6B (Shimadzu Corporation) Detector: RID-6A (Shimadzu Corporation) Data processing software: Sic480II Data Station (System Instruments) Column: GL-R400 (guard column) + GL-R440 + GL-R450 + GL-R400M (Hitachi Chemical Co., Ltd.) Elution solvent: THF (tetrahydrofuran) Elution flow rate: 2mL / min Column temperature: 35℃

[0108] (Styrene-acrylic acid copolymer B) Styrene-acrylic acid copolymer B was obtained in the same manner as styrene-acrylic acid copolymer A, except that the amount of styrene used was changed to 74 parts by mass, the amount of acrylic acid used was changed to 11 parts by mass, and the amount of methacrylic acid used was changed to 15 parts by mass. The acid value of styrene-acrylic acid copolymer B was 170 mgKOH / g and the weight average molecular weight was 11,000.

[0109] <Preparation of Pigment Composition> (Black pigment composition) [Example A1] First, 375 g of a black pigment (carbon black, #960, dry pigment, manufactured by Mitsubishi Chemical Corporation), 150 g of the above-mentioned styrene-acrylic acid copolymer A, 413 g of triethylene glycol, 495 g of pure water, and 68 g of a 34% by mass aqueous potassium hydroxide solution were mixed to prepare a first raw material composition (pigment concentration: 25% by mass, solid concentration: 35% by mass).

[0110] Next, in the step 0, the first raw material composition was charged into a rotor-stator type processor (manufactured by IKA Corporation, equipment name: magic LAB, 3-stage type, processing section (rotor and stator) of 2P / 4M / 6F from the top in the vertical direction, in-line type). Next, the first raw material composition was heated to 60° C. and then heated at a peripheral speed of 34 m / s (shear rate: 170,000 s -1 ), and five passes were performed at a rotation speed of 20,000 rpm to prepare a second raw material composition (slurry).

[0111] Next, in step 1, the second raw material composition was sprayed and collided at a pressure of 140 MPa using a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, oblique collision chamber) in one pass to obtain a pigment composition.

[0112] [Reference example A2] A pigment composition was obtained in the same manner as in Example A1, except that a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, oblique collision chamber) was used instead of the high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, ball collision chamber) to spray the second raw material composition at a pressure of 140 MPa and collide it against a ball, for one pass.

[0113] [Reference example A3] A pigment composition was obtained in the same manner as in Reference Example A2, except that the pressure when spraying the second raw material composition using a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, ball collision chamber) was changed from 140 MPa to 200 MPa.

[0114] [Reference example A4] First, a first raw material composition was prepared in the same manner as in Example A1.

[0115] Next, in the step 0, the first raw material composition was charged into a dispersing mixer (manufactured by EYELA, device name: MAZELA ZZ-1000 / 1000S, maximum peripheral speed: 15 m / s, maximum rotation speed: 3000 rpm). Next, the mixture was stirred for 30 minutes at a peripheral speed of 12 m / s and a rotation speed of 2400 rpm while being heated to 60° C., thereby obtaining a second raw material composition.

[0116] Next, in step 1, a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, ball collision chamber) was used to spray the second raw material composition at a pressure of 140 MPa and collide it against a ball, and a pigment composition was obtained by performing a process of one pass.

[0117] [Reference example A5] First, a first raw material composition was prepared in the same manner as in Example A1.

[0118] Next, zirconia beads (Φ0.3 mm) having a mass 20 times the mass of the pigment were added to the first raw material composition, which was then placed in a bead mill (manufactured by Imex Co., Ltd., machine name: Easy Nano RMB type, maximum peripheral speed: 15 m / s, maximum rotation speed: 2650 rpm) and stirred for 30 minutes at a peripheral speed of 12 m / s and a rotation speed of 2100 rpm while cooling to 15°C, to obtain a second raw material composition.

[0119] Next, in step 1, a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, ball collision chamber) was used to spray the second raw material composition at a pressure of 200 MPa and collide it against a ball, and a pigment composition was obtained by performing a process of one pass.

[0120] [Example A6] A pigment composition was obtained in the same manner as in Reference Example A2, except that the pressure when spraying the second raw material composition using a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, oblique collision chamber) was changed from 140 MPa to 100 MPa.

[0121] [Comparative Example A1] A mixture was prepared by mixing 50 g of black pigment (Mitsubishi Chemical Corporation, carbon black, #960, dry pigment), 20 g of the above-mentioned styrene-acrylic acid copolymer A, 55 g of triethylene glycol, and 9 g of 34% by mass potassium hydroxide aqueous solution, and then charged into a planetary mixer (Aikosha Co., Ltd., equipment name: Chemical Mixer ACM04LVTJ-B) kept at 80°C, and kneaded at a rotation speed of 80 rpm and a revolution speed of 25 rpm. After 60 minutes had elapsed since the current value of the planetary mixer reached the maximum current value, ion-exchanged water was added in 4 g increments, and kneading was continued until a total of 36 g of ion-exchanged water was added, to obtain a kneaded product. 30 g of ion-exchanged water was added to the obtained kneaded product as a dilution operation to obtain a pigment composition (pigment concentration: 25% by mass, solid content concentration: 35% by mass).

[0122] [Comparative example A2] A pigment composition was obtained in the same manner as in Example A1, except that a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, oblique collision chamber) was used instead of the high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, single nozzle chamber), and the second raw material composition similar to that used in Example A1 was passed through the single nozzle chamber at a pressure of 140 MPa in one pass.

[0123] [Comparative example A3] A pigment composition was obtained in the same manner as in Comparative Example A2, except that the pressure when spraying the second raw material composition using a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, single nozzle chamber) was changed from 140 MPa to 200 MPa.

[0124] [Comparative example A4] A pigment composition was obtained in the same manner as in Reference Example A2, except that the number of passes for spraying the second raw material composition was changed from 1 pass to 20 passes.

[0125] (Red pigment composition) [Example B1] First, 1,500 g of a red pigment (FASTOGEN SUPER MAGENTA RY WET pigment, manufactured by DIC Corporation, pigment concentration: 32 mass%, wet pigment), 95 g of the above-mentioned styrene-acrylic acid copolymer B, 356 g of triethylene glycol, and 49 g of a 34 mass% aqueous potassium hydroxide solution were mixed to prepare a first raw material composition (pigment concentration: 24 mass%, solid concentration: 28 mass%).

[0126] Next, in the step 0, the first raw material composition was charged into a rotor-stator type processor (manufactured by IKA Corporation, equipment name: magic LAB, 3-stage type, processing section (rotor and stator) of 2P / 4M / 6F from the top in the vertical direction, in-line type). Next, the first raw material composition was heated to 60° C. and then heated at a peripheral speed of 34 m / s (shear rate: 170,000 s -1), and five passes were performed at a rotation speed of 20,000 rpm to prepare a second raw material composition (slurry). Next, in step 1, the second raw material composition was sprayed and collided at a pressure of 200 MPa using a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, oblique collision chamber) in one pass to obtain a pigment composition.

[0127] [Reference example B2] A pigment composition was obtained in the same manner as in Reference Example A2, except that a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, oblique collision chamber) was used instead of the high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, ball collision chamber) to spray the second raw material composition at a pressure of 200 MPa and collide it against a ball in one pass.

[0128] [Reference example B3] First, a first raw material composition was prepared in the same manner as in Example B1.

[0129] Next, in the step 0, the first raw material composition was charged into a dispersing mixer (manufactured by EYELA, device name: MAZELA ZZ-1000 / 1000S, maximum peripheral speed: 15 m / s, maximum rotation speed: 3000 rpm). Next, the mixture was stirred for 30 minutes at a peripheral speed of 12 m / s and a rotation speed of 2400 rpm while being heated to 60° C., thereby obtaining a second raw material composition.

[0130] Next, in step 1, a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, ball collision chamber) was used to spray the second raw material composition at a pressure of 200 MPa and collide it against a ball, and a pigment composition was obtained by performing a process of one pass.

[0131] [Comparative Example B1] A mixture was prepared by mixing 50 g of a red pigment (FASTOGEN SUPER MAGENTA RY WET pigment, manufactured by DIC Corporation, dry pigment), 10 g of the above-mentioned styrene-acrylic acid copolymer B, 40 g of triethylene glycol, and 5 g of a 34% by mass potassium hydroxide aqueous solution, and then the mixture was charged into a planetary mixer (manufactured by Aikosha Seisakusho Co., Ltd., device name: chemical mixer ACM04LVTJ-B) kept at 80°C, and kneaded at a rotation speed of 80 rpm and a revolution speed of 25 rpm. After 60 minutes had elapsed since the current value of the planetary mixer reached the maximum current value, ion-exchanged water was added in 4 g increments, and kneading was continued until a total of 36 g of ion-exchanged water was added, to obtain a kneaded product. 67 g of ion-exchanged water was added to the obtained kneaded product as a dilution operation, to obtain a pigment composition (pigment concentration: 24% by mass, solid content concentration: 28% by mass).

[0132] [Comparative example B2] First, a first raw material composition was prepared in the same manner as in Example B1.

[0133] Next, in the step 0, the first raw material composition was charged into a dispersing mixer (manufactured by EYELA, device name: MAZELA ZZ-1000 / 1000S, maximum peripheral speed: 15 m / s, maximum rotation speed: 3000 rpm). Next, the mixture was stirred for 30 minutes at a peripheral speed of 12 m / s and a rotation speed of 2400 rpm while being heated to 60° C., thereby obtaining a second raw material composition.

[0134] Next, in step 1, a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, ball collision chamber) was used to spray the second raw material composition at a pressure of 200 MPa and collide it against a ball, and a pigment composition was obtained by performing a process of one pass.

[0135] Next, in the step 0, the first raw material composition was charged into a rotor-stator type processor (manufactured by IKA Corporation, equipment name: magic LAB, 3-stage type, processing section (rotor and stator) of 2P / 4M / 6F from the top in the vertical direction, in-line type). Next, the first raw material composition was heated to 60° C. and then heated at a peripheral speed of 34 m / s (shear rate: 170,000 s -1 ), and five passes were performed at a rotation speed of 20,000 rpm to prepare a second raw material composition (slurry). Next, in step 1, a high-pressure homogenizer (manufactured by Sugino Machine Co., Ltd., equipment name: Starburst, single nozzle chamber) was used to pass the second raw material composition through a single nozzle chamber at a pressure of 200 MPa for two passes, thereby obtaining a pigment composition.

[0136] <Evaluation of Pigment Composition> The pigment compositions obtained in the Examples and Comparative Examples were evaluated for the number of coarse particles, particle size, viscosity, storage stability, print density, and resin adsorption rate according to the following procedures. The results are shown in Tables 1 and 2.

[0137] (Number of coarse particles) The number of particles with a diameter of 1.0 μm or more and the number of particles with a diameter of 0.5 μm or more were measured using a particle size distribution meter (Particle Sizing Systems, Accusizer 780 APS, number counting method) according to the following procedure. The pigment composition was diluted with pure water so that the sensitivity was in the range of 1000 to 4000 particles / mL. Next, the number of particles with a diameter of 1.0 μm or more and the number of particles with a diameter of 0.5 μm or more contained in the diluted pigment composition were measured three times using the particle size distribution meter. Next, the average value of the values ​​obtained by multiplying the measured particle number by the dilution concentration was calculated as the number of coarse particles.

[0138] (Particle size) The pigment composition was placed in a cell of about 4 mL. The particle size was measured by detecting the scattered light of a laser beam using a Nanotrac particle size distribution analyzer "UPA150" manufactured by Microtrac Bell Co., Ltd., in an environment of 25°C. The particle sizes measured were the volume average particle size (Mv), number average particle size (Mn), D50, D90, and D95.

[0139] (viscosity) 1.0 mL of the pigment composition, the pigment concentration of which had been adjusted to 13%, was placed in a sample cup, and the viscosity of the pigment composition was measured in an environment of 25° C. using a TV-20 viscometer manufactured by Toki Sangyo Co., Ltd.

[0140] (Storage stability) The pigment composition was sealed in a polypropylene container and stored at 60° C. for one week. The rate of change in the volume average particle diameter (Mv), viscosity, and number of coarse particles with a diameter of 0.5 μm before and after storage was calculated. The rate of change in the volume average particle diameter (Mv), viscosity, and number of coarse particles with a diameter of 0.5 μm after storage relative to the volume average particle diameter (Mv), viscosity, and number of coarse particles with a diameter of 0.5 μm before storage was calculated. Those whose rate of change was within 10% were evaluated as having excellent storage stability, those whose rate of change was more than 10% but not more than 15% were evaluated as having good storage stability, and those whose rate of change was more than 15% were evaluated as having insufficient storage stability.

[0141] (Print density) [Preparation of inkjet recording ink] The above-mentioned pigment composition was centrifuged at 25°C, a centrifugal force of 134000G, and a residence time of 10 minutes using a batch centrifuge (manufactured by Kokusan Co., Ltd.). The supernatant was decanted to obtain a purified pigment composition. The pigment composition obtained by centrifugation was mixed with 8.0 parts by mass of 2-pyrrolidone, 8.0 parts by mass of triethylene glycol monobutyl ether, 3.0 parts by mass of glycerin, 0.5 parts by mass of Surfynol 440 (manufactured by Nissin Chemical Industry Co., Ltd.), and 47.2 parts by mass of ion-exchanged water to obtain an aqueous ink for inkjet recording. The pigment concentration in the ink obtained using the black pigment composition was 2.5% by mass, and the pigment concentration in the ink obtained using the red pigment composition was 3.5% by mass.

[0142] [Printing] The inkjet recording ink was filled into the cartridge of an inkjet printer ENVY4500 (manufactured by HP Inc.). Next, the printer was cleaned once, and then a printout was obtained by printing an image having a 100% solid area on commercially available PPC paper (sold by Otsuka Shokai, product number: 10PPCHWA4N) in plain paper / standard printing mode.

[0143] [Print Density Measurement] The 100% solid area of ​​the print was measured using X-Rite's "eXact" and the density of the print pattern was obtained as an evaluation value. The higher the evaluation value, the darker the color appears (the higher the evaluation).

[0144] (Resin adsorption rate) Using a particle charge meter (Spectris Corporation, product name: PCD-04), the streaming potential was measured in the range of ±2500 mV at the platinum electrode of the sample cell. The pigment composition was placed in the sample cell and titrated with a titrant (0.01 N, Poly-DADMAC). The titration of the charge amount was performed based on the potential difference (i.e., the streaming potential of the liquid) generated by the movement of the sample cell and the moving piston. The titration was terminated when the streaming potential exceeded zero (the potential became positive). The amount of dripping from the inflection point was divided by the amount of dripping when the streaming potential became zero, and the result was multiplied by 100 to obtain the resin adsorption rate.

[0145] [Table 1]

[0146] [Table 2] [Explanation of symbols]

[0147] 10...central shaft, 20...rotor, 22...blade portion, 22a...opening, 24...connection portion, 30...stator, 32...wall portion, 32a...opening, 34...connection portion, 100...rotor-stator type processing machine, F1, F2...flow path.

Claims

1. A method for producing a pigment composition in which a pigment is dispersed in a liquid medium by a pigment dispersing resin, by subjecting a raw material composition containing a pigment, a pigment dispersing resin, and a liquid medium to a process 1 using a dispersing machine, comprising the steps of: The raw material composition has undergone a step 0 of mixing a pigment, a pigment dispersion resin, and a liquid medium by a rotor-stator type processor; The rotor-stator type processor is an in-line or batch type processor; In the rotor-stator type processor, The share rate is 50,000 to 400,000 s −1 . The rotation speed is 1000 to 30000 rpm, and / or The peripheral speed is 5 to 50 m / s, The mixing temperature in step 0 is 50 to 80° C. The dispersing machine is a dispersing machine having a configuration for causing the raw material compositions to collide with each other, The disperser having a configuration for colliding the raw material compositions with each other is an oblique collision type disperser, The oblique collision type disperser is configured to collide the raw material compositions with each other at a pressure in the range of 50 to 200 MPa, The method for producing a pigment composition, wherein the oblique collision type disperser is an oblique collision chamber.

2. 2. The method for producing a pigment composition according to claim 1, wherein the solid content of the raw material composition is in the range of 1% by mass to 60% by mass.

3. The pigment dispersing resin contains a radical polymer having an anionic group, The acid value of the pigment dispersion resin is 60 to 300 mgKOH / g; the raw material composition further contains an alkali metal hydroxide as a basic compound that neutralizes the anionic group of the radical polymer, The following formula (1) Neutralization rate [%] = ((mass [g] of basic compound × 56 × 1000) / (acid value of pigment dispersion resin × equivalent of basic compound × mass [g] of pigment dispersion resin)) × 100 ... (1) 3. The method for producing a pigment composition according to claim 1, wherein the neutralization rate of the pigment dispersing resin defined by the formula (I) is 80 to 120%.

4. 4. The method for producing a pigment composition according to claim 1, wherein the number of times (number of passes) in which the raw material composition is repeatedly charged into a disperser having a configuration in which the raw material compositions are collided obliquely with each other is in the range of 1 to 8.

5. The method for producing a pigment composition according to any one of claims 1 to 4, wherein the pigment composition is a pigment composition for inkjet printing ink.

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