WO2021100468A1 - 顔料組成物の製造方法 - Google Patents

顔料組成物の製造方法 Download PDF

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Publication number
WO2021100468A1
WO2021100468A1 PCT/JP2020/041274 JP2020041274W WO2021100468A1 WO 2021100468 A1 WO2021100468 A1 WO 2021100468A1 JP 2020041274 W JP2020041274 W JP 2020041274W WO 2021100468 A1 WO2021100468 A1 WO 2021100468A1
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WIPO (PCT)
Prior art keywords
pigment
raw material
pigment composition
composition
easy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2020/041274
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English (en)
French (fr)
Japanese (ja)
Inventor
和香奈 内藤
尚一 保立
兼司 菅生
鳫林 秀樹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DIC Corp
Original Assignee
DIC Corp
Dainippon Ink and Chemicals Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by DIC Corp, Dainippon Ink and Chemicals Co Ltd filed Critical DIC Corp
Priority to EP20889123.4A priority Critical patent/EP4063458B1/en
Priority to CN202080077285.2A priority patent/CN114667325A/zh
Priority to JP2021558275A priority patent/JP7306475B2/ja
Priority to US17/771,881 priority patent/US20220372324A1/en
Publication of WO2021100468A1 publication Critical patent/WO2021100468A1/ja
Anticipated expiration legal-status Critical
Priority to JP2023025193A priority patent/JP7653065B2/ja
Ceased legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00Pigment pastes, e.g. for mixing in paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/006Preparation of organic pigments
    • C09B67/0063Preparation of organic pigments of organic pigments with only macromolecular substances
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/006Preparation of organic pigments
    • C09B67/0066Aqueous dispersions of pigments containing only dispersing agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0071Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
    • C09B67/0084Dispersions of dyes
    • C09B67/0091Process features in the making of dispersions, e.g. ultrasonics
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
    • C09C1/48Carbon black
    • C09C1/56Treatment of carbon black ; Purification
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
    • C09C1/48Carbon black
    • C09C1/56Treatment of carbon black ; Purification
    • C09C1/58Agglomerating, pelleting, or the like by wet methods
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding or treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding or treatment with ultrasonic vibrations
    • C09C3/045Agglomeration, granulation, pelleting
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/30Inkjet printing inks
    • C09D11/32Inkjet printing inks characterised by colouring agents
    • C09D11/322Pigment inks
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/30Inkjet printing inks
    • C09D11/32Inkjet printing inks characterised by colouring agents
    • C09D11/324Inkjet printing inks characterised by colouring agents containing carbon black
    • C09D11/326Inkjet printing inks characterised by colouring agents containing carbon black characterised by the pigment dispersant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/34Heterocyclic compounds having nitrogen in the ring
    • C08K5/3412Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
    • C08K5/3432Six-membered rings
    • C08K5/3437Six-membered rings condensed with carbocyclic rings

Definitions

  • the present invention relates to a method for producing a pigment composition.
  • the pigment composition is used in various printing such as inkjet printing.
  • a method for producing a pigment composition a method of obtaining a pigment composition by treating a raw material composition containing a pigment component and a liquid medium with a disperser is known (see, for example, Patent Document 1 below).
  • the pigment composition is required to have a small number of coarse particles from the viewpoint of suppressing clogging of the ejection nozzle during printing and obtaining good ejection stability.
  • a method in which the raw material composition containing the pigment, the pigment-dispersed resin and the liquid medium is subjected to a long-term dispersion treatment or repeatedly put into a disperser for treatment is effective.
  • the above method may not be able to improve the production efficiency of pigment compositions, inks, and the like.
  • An object to be solved by the present invention is to provide a method for producing a pigment composition, which can achieve both a reduction in the number of coarse particles that can be contained in the pigment composition and an improvement in the production efficiency of the pigment composition. ..
  • the present invention produces a pigment composition in which a pigment is dispersed in a liquid medium by a pigment-dispersed resin by going through step 1 of treating a raw material composition containing a pigment, a pigment-dispersed resin and a liquid medium with a disperser.
  • the present invention relates to a method for producing a pigment composition, wherein the disperser is a disperser having a structure in which the raw material compositions collide with each other.
  • the method for producing a pigment composition of the present invention it is possible to reduce the number of coarse particles having a particle size of 1.0 ⁇ m or more that can be contained in the pigment composition and to improve the production efficiency of the pigment composition at the same time. ..
  • FIG. 1 It is a schematic cross-sectional view which shows an example of the rotor stator type processing machine. It is a schematic side view which shows the example of the stator in the rotor stator type processing machine. It is a schematic diagram for demonstrating the crushing process or the crushing process in a rotor stator type processing machine.
  • the numerical range indicated by using “-" indicates a range including the numerical values before and after "-" as the minimum value and the maximum value, respectively.
  • the upper limit value or the lower limit value of the numerical range of one step can be arbitrarily combined with the upper limit value or the lower limit value of the numerical range of another step.
  • the upper limit value or the lower limit value of the numerical range may be replaced with the value shown in the examples.
  • “A or B” may include either A or B, or both.
  • the materials exemplified in the present specification may be used alone or in combination of two or more.
  • each component in the composition means the total amount of the plurality of substances present in the composition when a plurality of substances corresponding to each component are present in the composition, unless otherwise specified.
  • process is included in this term not only in an independent process but also in the case where the desired action of the process is achieved even if it cannot be clearly distinguished from other processes.
  • (Meta) acrylic acid is a general term for acrylic acid and methacrylic acid corresponding thereto, and is the same in other similar expressions such as "(meth) acrylate”.
  • a raw material composition containing a pigment, a pigment-dispersed resin and a liquid medium is treated with a disperser in step 1, so that the pigment is dispersed in the liquid medium by the pigment-dispersed resin.
  • This is a method for producing a pigment composition obtained.
  • the disperser is characterized by using a disperser having a structure in which the raw material compositions collide with each other.
  • the number of coarse particles having a particle size of 1.0 ⁇ m or more that can be contained in the pigment composition in which the pigment is dispersed in the liquid medium by the pigment dispersion resin can be reduced, and the pigment composition can be reduced.
  • a disperser having a structure in which the raw material composition collides with a hard body, but it is excellent in avoiding wear of the hard body when used for a long time.
  • the raw material compositions are used with each other. It is preferable to use a disperser having a configuration for colliding with each other alone or in combination with another disperser.
  • the pigment composition refers to a pigment dispersed or dissolved in a liquid medium such as water by a pigment-dispersed 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.
  • the pigment composition is preferably used, for example, for producing a printing ink or the printing ink, and more preferably for producing an inkjet printing ink or an inkjet printing ink.
  • the ratio of the solid content of the pigment composition to the total amount of the pigment composition is preferably in the range of 1% by mass to 50% by mass. More preferably, it is in the range of 10% by mass to 30% by mass.
  • the disperser having a configuration in which the raw material compositions collide with each other it is possible to use a disperser having a configuration in which the raw material compositions collide with each other in an oblique direction in the pigment composition. It is particularly preferable to reduce the number of coarse particles, reduce the particle size of the dispersed particles, and improve the production efficiency of the pigment composition. More specifically, by using a disperser having a configuration in which the raw material compositions collide with each other in an oblique direction, the number of times the raw material composition is repeatedly charged into the disperser and processed (so-called number of passes).
  • An oblique collision chamber can be mentioned as a configuration for obliquely colliding the raw material compositions with each other.
  • the disperser When the disperser is used, the raw material compositions can collide with each other by pressure-injecting the raw material compositions from a plurality of directions.
  • the oblique collision chamber include a chamber manufactured by Sugino Machine Limited with the device name "Starburst".
  • the oblique collision chamber can avoid wear of the hard body, which will be described later, when used for a long time, and can obtain a better shearing force than the single nozzle chamber. Therefore, the oblique collision chamber exhibits excellent micronizing ability and coarse particles. It is preferable to obtain a pigment composition having excellent storage stability by reducing the number of the above-mentioned substances, or to obtain a pigment composition capable of producing a printed matter having a higher print density.
  • the disperser the device name "Starburst" manufactured by Sugino Machine Limited can be used.
  • the disperser used in the present invention is a so-called high-pressure homogenizer capable of applying a pressure in the range of 50 to 245 MPa when injecting the raw material composition, that is, the number of coarse particles in the pigment composition. It is preferable in order to achieve both reduction and improvement of 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.
  • the pigment component contains carbon black, it is possible to obtain a pigment composition that can be ejected by inkjet at low pressure and has excellent storage stability, prolonging the life of the apparatus, and increasing the production amount per unit time. Easy to achieve improvement.
  • the raw material composition one containing a solid content such as a pigment or a pigment-dispersed resin and a liquid medium and further containing an additive other than these can be used.
  • the pigment composition can contain the same kind of components as the raw material composition.
  • the solid content concentration of the raw material composition may be 1 to 60% by mass, 10 to 50% by mass, or 15 to 40% by mass based on the total amount of the raw material composition.
  • the raw material composition a mixture of the pigment, the pigment-dispersed resin, and a liquid medium can be simply used.
  • the raw material composition those in which the pigment, the pigment dispersion resin and the liquid medium are previously mixed by a rotor stator type processing machine or a bead mill processing machine before the step 1 can be used.
  • the number of times the raw material composition is repeatedly put into the disperser and processed can be significantly reduced, and as a result, it is preferable in order to significantly improve the production efficiency of the pigment composition and the ink.
  • the crushing means for example, a process of crushing an integral mass. Cracking means, for example, a process of unraveling agglomerates.
  • step 0 in which the pigment, the pigment-dispersed resin, and the liquid medium are previously mixed by a rotor stator type processing machine or a bead mill processing machine before the step 1, the pigment is pulverized or crushed.
  • the raw material composition containing a large amount of coarse particles is treated with the disperser in the step 1, there is a concern that problems such as clogging of pipes may occur in the disperser. Therefore, from the viewpoint of avoiding such a problem, pre-grinding or pre-crushing is performed as a pretreatment prior to the step of dispersing the pigment in the liquid medium with the pigment dispersion resin using the disperser in step 1. It is effective to perform step 0.
  • a processing machine that can be used in the step 0 for example, a rotor stator type processing machine or a bead mill processing machine, an ultrasonic disperser, a disper, or the like can be used, and the use of the rotor stator type processing machine is a pigment. It is preferable because the pulverization or crushing of the above can be performed more efficiently, and as a result, a pigment composition having a reduced number of coarse particles can be efficiently produced.
  • the rotor stator type processing machine As described later, coarse particles are crushed or crushed by applying a shearing force to a raw material composition containing coarse particles between the rotor and the stator. Therefore, by passing through the step 0 and then the step 1 using the rotor stator type processing machine, the number of coarse particles in the pigment composition can be reduced more efficiently, and the particle size is 1.0 ⁇ m or more. The number of coarse particles can be further reduced. Further, according to the step 1 after the step 0 using the rotor stator type processing machine, the coarseness is suppressed by suppressing the increase in the treatment time for obtaining the pigment composition having a small number of coarse particles. A pigment composition having a small number of particles can be obtained with high productivity.
  • the number of coarse particles having a particle size of 0.5 ⁇ m or more can be reduced.
  • the reduction rate of the number of coarse particles when the raw material compositions having the same composition are crushed or crushed is compared.
  • the performance difference of the processing machines can be compared by using the rotation speed of about 80% of the maximum rotation speed.
  • the number of coarse particles in the pigment composition can be efficiently reduced while reducing the viscosity of the pigment composition.
  • the step 1 using the rotor stator type processing machine it is possible to reduce the particle size of the solid content in the pigment composition obtained by the pulverization treatment or the crushing treatment. ..
  • the pigment composition obtained by the pulverization treatment or the crushing treatment has excellent storage stability (dispersion stability of solid content). Gender) can be obtained.
  • step 0 after the process 0 using the rotor stator type processing machine, the comparison was made under the condition that the composition of the pigment composition and the mass ratio of the pigment-dispersed resin to the pigment component were the same. High print density can be obtained. Further, by passing through the step 0 and then the step 1 using the rotor stator type processing machine, a high adsorption rate of the pigment-dispersed resin to the pigment component can be obtained.
  • a processing machine such as a rotor stator type processing machine or a bead mill processing machine is used, and a raw material composition obtained by crushing or crushing the pigment in advance is used, and the pigment is subjected to the step 1. It is possible to efficiently further reduce the number of coarse particles in the composition. Further, in the step 0, a processing machine such as a rotor stator type processing machine or a bead mill processing machine is used, and a raw material composition obtained by crushing or crushing the pigment in advance is used, and the solid content is obtained by passing through the step 1. The time for producing a pigment composition having desired physical properties (number of coarse particles, particle size, etc.) can be shortened.
  • the temperature in the treatment step using the processing machine in the step 0 is a pigment composition having desired physical properties (number of coarse particles, particle size, etc.) of the solid content from the viewpoint of easily reducing the number of coarse particles efficiently. From the viewpoint that the time required to obtain the pigment-dispersed resin through step 1 can be easily shortened, and from the viewpoint that the adsorption rate of the pigment-dispersed resin to the pigment component can be easily improved by promoting the dissolution of the pigment-dispersed resin, and excellent storage stability can be easily obtained. Therefore, the following range is preferable.
  • the temperature is preferably 25 ° C. or higher, more preferably 30 ° C. or higher, further preferably 40 ° C. or higher, particularly preferably 50 ° C.
  • the temperature is preferably 80 ° C. or lower, more preferably 75 ° C. or lower, further 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.
  • the rotor stator type processing machine that can be used in the step 0 includes a rotor having a rotatable blade portion and a stator having a wall portion arranged on the outer peripheral side of the blade portion.
  • the processing machine may be any of a crusher, a crusher, a disperser and the like.
  • As the rotor and stator any commercially available shape can be used, and different shapes or combinations of the same shape can be used. Since there are differences in the transportability, shear rate (miniaturization ability), calorific value at the time of miniaturization, etc. of the raw material composition depending on the shape, the combination can be selected according to the properties of the raw material composition. Usually, a rotor with a large number of teeth tends to be finely divided, and the amount of heat generated increases.
  • FIG. 1 is a schematic cross-sectional view showing an example of a rotor stator type processing machine.
  • the rotor stator type processing machine 100 shown in FIG. 1 includes a central shaft 10, a rotor 20, and a stator 30.
  • Examples of the constituent materials of the central shaft 10, the rotor 20 and the stator 30 include metal materials and ceramics.
  • the central axis 10 is a long member, and extends in the vertical direction, for example.
  • the central shaft 10 supports the rotor 20 and the stator 30.
  • the rotor 20 has an annular (for example, annular) blade portion 22 extending in the longitudinal direction of the central shaft 10 on the outer peripheral portion of the rotor 20, and a connecting portion 24 for connecting the blade portion 22 and the central shaft 10. There is.
  • the blade portion 22 can rotate about the central axis 10.
  • the blade portion 22 has openings (through holes) 22a penetrating the blade portion 22, and has, for example, a plurality of openings 22a at intervals (for example, equal intervals) along the circumferential direction of the blade portion 22. ing.
  • the opening direction of the opening 22a may be inclined with respect to the radial direction.
  • the vertical end of the opening 22a may be open without the members constituting the rotor 20 being arranged.
  • the number, arrangement and shape of the openings 22a are not particularly limited.
  • the arrangement and shape of the blade portion in the rotor of the rotor stator type processing machine are not particularly limited.
  • the blade portion is not limited to the annular member arranged on the outer peripheral portion of the rotor, and may have a shape extending from the central portion of the rotor to the outer peripheral portion.
  • the rotor may have a plurality of blade portions having a shape extending from the central portion of the rotor to the outer peripheral portion.
  • the blade portion having a shape extending from the central portion to the outer peripheral portion of the rotor may have a streamlined shape.
  • the stator 30 has an annular (for example, an annular) wall portion 32 extending in the longitudinal direction of the central shaft 10 on the outer peripheral portion of the stator 30, and a connecting portion 34 connecting the wall portion 32 and the central shaft 10.
  • the wall portion 32 is arranged on the outer peripheral side of the blade portion 22 in the rotor stator type processing machine 100.
  • the wall portion 32 has openings (through holes) 32a penetrating the wall portion 32, and has, for example, a plurality of openings 32a at intervals (for example, equal intervals) along the circumferential direction of the wall portion 32. ing.
  • the opening direction of the opening 32a may be inclined with respect to the radial direction.
  • FIG. 2 is a schematic side view showing an example of a stator (wall portion of the stator) in the rotor stator type processing machine.
  • the wall portion of the stator include a wall portion (FIG. 2A) having openings arranged in an array (for example, a rectangular opening such as a square shape), and a plurality of rectangular shapes arranged in a row.
  • Examples thereof include a wall portion having an opening (FIG. 2 (b)), a wall portion having a plurality of circular (for example, a perfect circular) opening arranged in a row (FIG. 2 (c)), and the like.
  • the shape of the opening include a rectangular shape (square shape, rectangular shape, etc.), a circular shape (perfect circle shape, elliptical shape, etc.) and the like.
  • the stator may have a plurality of annular (for example, annular) wall portions extending in the longitudinal direction of the central axis at the outer peripheral portion of the stator.
  • the stator may include the above-mentioned wall portion 32 as the first wall portion, and may include a second wall portion arranged on the outer peripheral side of the first wall portion in the rotor stator type processing machine, and may include a rotor stator type.
  • a third wall portion arranged on the outer peripheral side of the second wall portion in the processing machine may be further provided.
  • the number of wall portions is not particularly limited and may be 4 or more.
  • FIG. 3 is a schematic view for explaining a crushing process or a crushing process in the rotor stator type processing machine, and is a schematic view showing a part of the outer peripheral portion of the rotor stator type processing machine 100 shown in FIG. 1 in an enlarged manner. is there.
  • the raw material composition is the blade portion of the rotor 20. It reaches the space between the blade portion 22 and the wall portion 32 of the stator 30 via the opening 22a of the 22 (flow path F1 in the drawing).
  • the coarse particles P are crushed or crushed by applying a shearing force generated by the rotational movement of the blade portion 22 to the coarse particles P (solid content).
  • a part of the composition containing the crushed or crushed particles flows out to the outer peripheral side of the wall portion 32 via the opening 32a of the wall portion 32 (flow path F2 in the figure), and the rest of the composition.
  • the particles are further crushed or crushed by the shearing force.
  • the pigment component in the raw material composition containing the pigment component and the liquid medium is crushed or crushed by the crushing treatment or the crushing treatment of the rotor stator type processing machine 100.
  • the share rate (miniaturization ability) given by the processing unit composed of the rotor and the stator has a viewpoint that the number of coarse particles can be easily reduced, a viewpoint that the particle size of the solid content after the treatment can be easily reduced, and a pigment composition.
  • reduced easily viewpoint of viscosity and, from the viewpoint of easy to obtain excellent storage stability in the pigment composition is preferably from 50000S -1 or more, more preferably 75000S -1 or more, more preferably 90000S -1 or higher, 100000S -1
  • the above is particularly preferable, 120,000s -1 or more is extremely preferable, 150,000s -1 or more is very preferable, and 170000s -1 or more is even more preferable.
  • the upper limit of the share rate may be, for example, 400,000 s -1 or less, and may be 250,000 s -1 or less. From these viewpoints, the share rate is preferably 50,000 to 400,000 s-1.
  • the share rate [s -1 ] can be obtained by dividing the peripheral speed [m / s] of the blade portion of the rotor by the distance [m] between the blade portion and the wall portion of the stator.
  • the rotor-stator type processing machine may have a plurality of processing units (crushing unit or crushing unit) composed of a rotor and a stator. By flowing the raw material composition from the processing unit having a low share rate to the processing unit having a high share rate, clogging can be easily suppressed, so that the number of coarse particles can be easily reduced.
  • the rotor stator type processing machine may have a plurality of processing units along a central axis extending in the vertical direction (may have a multi-stage processing unit).
  • the processing units having a higher share rate toward the lower side in the vertical direction from the viewpoint of easily reducing the number of coarse particles efficiently.
  • the rotor stator type processing machine may be an in-line type processing machine or a batch type processing machine.
  • the raw material composition is continuously supplied, and for example, the processing machine is installed in the middle of the processing path (for example, the crushing processing path and the crushing processing path, for example, the piping), and the raw material composition is continuously supplied. Can be processed (crushed or crushed).
  • the entire raw material composition is forcibly passed through the processing machine, so that the entire raw material composition is made uniform in a short time as compared with the batch type processing machine in which only the periphery of the rotor is processed. Easy to handle.
  • the in-line type processing machine since it is easy to efficiently reduce the number of coarse particles, it is easy to suppress the clogging of the piping of the processing machine used in the step 0.
  • using an in-line type processing machine as the rotor stator type processing machine has a diameter of 0, which is contained in the finally obtained pigment composition, as compared with the case where the batch type processing machine is used alone.
  • the number of coarse particles of 5 ⁇ m or more can be reduced more effectively.
  • the in-line processing machine it is easy to reduce the viscosity of the pigment composition.
  • the raw material composition may be circulated.
  • the raw material composition is intermittently supplied, and the raw material composition is replaced for each treatment (crushing treatment or crushing treatment).
  • the device name "magic LAB” manufactured by IKA Co., Ltd. in-line type, maximum peripheral speed: 41 m / s, maximum rotation speed: 26000 rpm
  • device name "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
  • Equipment name "L5MA” manufactured by Silverson Nippon Co., Ltd. batch type, maximum peripheral speed: 20 m / s, Maximum rotation speed: 10000 rpm) and the like.
  • a processing machine including a UTR module (ULTRA-TURRX), a DR module (DISPAX-REACTOR), an MK module, an MKO module, and a CMX module can be used.
  • the DR module has three stages of processing units (stages) composed of a rotor and a stator and the share rate can be adjusted by combining the rotor and the stator, it is easy to efficiently reduce the number of coarse particles. For example, by using the processing units of 2P / 4M / 6F in order from the upper side in the vertical direction, it is possible to arrange the processing units having a higher share rate toward the lower side in the vertical direction.
  • the rotor stator type processing machine it is preferable to use one having a rotation speed in the range of 1000 to 30,000 rpm, more preferably one in the range of 3000 to 25000 rpm, and one in the range of 8000 to 20000 rpm. From the viewpoint of easily reducing the number of coarse particles efficiently, from the viewpoint of easily reducing the particle size of the solid content after treatment, from the viewpoint of easily reducing the viscosity of the pigment composition, and excellent storage stability in the pigment composition. It is particularly preferable from the viewpoint of easily obtaining sex.
  • the rotor stator type processing machine it is preferable to use one having a peripheral speed in the range of 5 m / s to 50 m / s, and more preferably to use one having a peripheral speed in the range of 10 m / s to 40 m / s, 15 m.
  • a pigment in the range of / s to 35 m / s makes it easy to efficiently reduce the number of coarse particles, makes it easy to reduce the particle size of the solid content after treatment, and makes it easy to reduce the viscosity of the pigment composition. It is particularly preferable from the viewpoint and from the viewpoint that excellent storage stability in the pigment composition can be easily obtained.
  • the raw material supply unit in the pigment composition manufacturing apparatus according to the present embodiment is not particularly limited as long as the raw material composition can be supplied to the rotor stator type processing machine.
  • the raw material supply unit may be a pipe, a pump, or the like that supplies the raw material supply unit.
  • bead mill disperser 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 and the like can be used.
  • pigment component at least one selected from the group consisting of pigments and pigment derivatives can be used.
  • an inorganic pigment or an organic pigment can be used.
  • the inorganic pigment include iron oxide, carbon black (for example, carbon black produced by a known method such as a contact method, a furnace method, and a thermal method), titanium oxide, and the like.
  • 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, etc.).
  • Perylene pigments perinone pigments, anthraquinone pigments, dioxazine pigments, thioindigo pigments, isoindolinone pigments, isoindolin pigments, quinophthalone pigments, diketopyrrolopyrrole pigments, etc.), phthalocyanine pigments, dye chelate (basic dye type chelate, acidic dye type) Chelate etc.), nitro pigments, nitroso pigments, aniline blacks and the like.
  • These inorganic pigments and organic pigments can be suitably used for producing printing inks (for example, ink jet printing inks).
  • As the pigment one type alone or two or more types can be used in combination.
  • Carbon black includes # 2300, # 980, # 960, # 900, # 52, # 45L, # 45, # 40, # 33, MA100, MA8, MA7, etc. manufactured by Mitsubishi Chemical Corporation; Regal manufactured by Cabot Corporation. Series, Monarch series, etc .; Color Black FW1, Color Black series, Printex series, Special Black series, NIPEX series, etc. manufactured by Orion Engineered Carbons Co., Ltd. can be used.
  • C.I. I. 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, 282 and other magenta pigments can be used.
  • C.I. I. Pigment Blue 1 2, 3, 15, 15: 1, 15: 2, 15: 3, 15: 4, 15: 6, 16, 22, 60, 63, 66 and the like can be used.
  • C.I. I. Pigment Orange 5 13, 16, 17, 34, 36, 43, 51, 64, 71 and other orange pigments can be used.
  • C.I. I. Pigment Violet 1, 3, 5: 1, 16, 19, 23, 38 and other violet pigments can be used as a pigment.
  • C.I. I. Pigment Green 1 4, 7, 8, 10, 17, 18, 36, 50, 58 and other green pigments can be used.
  • a dry pigment pigment in the state of dry powder
  • a wet pigment pigment in the state of wet cake
  • the magenta pigment the time required to obtain a pigment composition having desired physical properties (number of coarse particles, particle size, etc.) of solid content through the step 1 is shortened from the viewpoint of easily reducing the number of coarse particles efficiently.
  • Wet pigments are preferable from the viewpoint of easy conversion.
  • the cyan pigment the time required to obtain a pigment composition having desired physical properties (number of coarse particles, particle size, etc.) of solid content through the step 1 is shortened from the viewpoint of easily reducing the number of coarse particles efficiently. Dry pigments are preferable from the viewpoint of easy conversion.
  • a mixture containing two or more kinds or a solid solution can also be used.
  • the pigment derivative a compound in which a functional group is introduced into the pigment can be used.
  • the pigment that gives the pigment derivative include phthalocyanine pigments, azo pigments, anthraquinone pigments, quinacridone pigments, diketopyrrolopyrrole pigments and the like.
  • 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, a sulfonyl group and the like.
  • the pigment derivative can impart dispersion stability to the pigment composition or ink, which enables prevention of generation of coarse particles over time and prevention of precipitation of pigment components and the like over time.
  • the primary particle size of the pigment component is preferably 1.0 ⁇ m or less, more preferably 0.01 to 0.5 ⁇ m, from the viewpoint of more effectively suppressing the sedimentation of the pigment component over time.
  • the primary particle size refers to the value of the number average particle size measured using a transmission electron microscope (TEM).
  • the pigment component is preferably 1 to 50% by mass, more preferably 10 to 30% by mass, still more preferably 15 to 25% by mass, based on the total amount of the raw material composition.
  • efficient and uniform treatment can be performed in each process, and excellent storage stability that prevents the occurrence of sedimentation of solids over time in the pigment composition can be achieved.
  • It is easy to obtain it is easy to prevent the occurrence of solid content in the ink over time, it is easy to suppress clogging of the ink ejection nozzle at the initial stage of ink ejection (it is easy to obtain excellent initial ejection stability), and it is easy to obtain it over time. It is easy to suppress the occurrence of clogging of the ink ejection nozzle (it is easy to obtain excellent ink ejection stability over time).
  • liquid medium examples include an aqueous medium (water, etc.), an organic solvent, and the like.
  • a high-pressure homogenizer used as the disperser 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 high pressure is applied.
  • water examples include pure water such as ion-exchanged water, ultra-filtered water, reverse osmosis water, and distilled water; ultrapure water and the like.
  • water it is preferable to use water sterilized by ultraviolet irradiation, addition of hydrogen peroxide, or the like 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 the range of 10 to 90% by mass, and the water-based ink is preferably used in the range of 15 to 80% by mass with respect to the total amount of the liquid medium contained in the pigment composition of the present invention. It is preferable in manufacturing.
  • a water-soluble organic solvent can be used as the organic solvent.
  • the water-soluble organic solvent easily wets the surface of the pigment component efficiently, and the resin component dissolved in water (for example, a resin neutralized product) is easily adsorbed on the pigment component, shortening the time required to reach the desired physical properties. It's easy to do.
  • water-soluble organic solvent examples include glycols such as ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propylene glycol, dipropylene glycol, tripropylene glycol, polyethylene glycol and polypropylene glycol; butanediol, pentanediol, hexanediol and the like.
  • Diols Diols; glycol esters such as propylene glycol laurate; diethylene glycol ethers such as diethylene glycol monoethyl, diethylene glycol monobutyl, diethylene glycol monohexyl, carbitol; cellosolves containing propylene glycol ether, dipropylene glycol ether or triethylene glycol ether, etc.
  • Glycol ethers examples include alcohols such as methanol, ethanol, isopropyl alcohol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, butyl alcohol, pentyl alcohol (excluding glycols); sulfolanes, esters, ketones, Examples thereof include lactones such as ⁇ -butyrolactone; lactams such as N- (2-hydroxyethyl) pyrrolidone and 2-pyrrolidone; glycerin and its polyalkylene oxide adduct.
  • the water-soluble organic solvent can be used alone or in combination of two or more.
  • 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 even more preferably 15 to 150 parts by mass with respect to 100 parts by mass of the pigment component contained in the raw material composition. ..
  • the water-soluble organic solvent in the above range, the adsorption rate of the resin component on the surface of the pigment component is improved, and excellent storage stability is prevented from causing the solid content to settle over time in the pigment composition. It is easy to obtain the properties, it is easy to prevent the solid content from settling over time in the ink, and it is easy to suppress the clogging of the ink ejection nozzle at the initial stage of ink ejection (it is easy to obtain excellent initial ejection stability).
  • the water-soluble organic solvent capable of improving the adsorption rate include triethylene glycol, glycerin, 2-pyrrolidone, 1- (2-hydroxyethyl) -2-pyrrolidone, dipropylene glycol, propylene glycol, 1,5. -Pentanediol and the like can be mentioned. Further, when a high-pressure homogenizer is used in producing the pigment composition, or when the inkjet printing ink obtained by using the pigment composition is applied to a thermal type inkjet printing method described later, the organic solvent is used.
  • a high boiling solvent having a boiling point of 100 ° C. or higher it is preferable to use a high boiling point solvent having a boiling point of 100 ° C. or higher as the organic solvent, because as a result of promoting the wetting of the pigment, the resin is easily adsorbed on the pigment and the storage stability and the like are improved.
  • the high boiling point solvent for example, glycerin, 2-pyrrolidone, 1- (2-hydroxyethyl) -2-pyrrolidone, dipropylene glycol, propylene glycol, 1,5-pentanediol and the like can be used.
  • the liquid medium is described below in order to obtain an ink having further excellent storage stability and easily suppressing clogging of the ink ejection nozzle at the initial stage of ink ejection and a pigment composition used for the production thereof. It is preferred to use a liquid medium having dispersed term in range and ([delta] D 1) polar term and ([delta] P 1) and a hydrogen bond (delta] H 1).
  • the dispersion term ( ⁇ D 1 ) of the liquid medium (a) is preferably in the range of 12 to 24, more preferably 14 to 21, and particularly preferably 16 to 19.
  • the polar term ( ⁇ P 1 ) of the liquid medium (a) is preferably in the range of 4 to 17, more preferably 6 to 15, and particularly preferably 8 to 13.
  • the hydrogen bond term ( ⁇ H 1 ) of the liquid medium (a) is preferably in the range of 6 to 43, more preferably 9 to 35, and particularly preferably 9 to 30.
  • the liquid medium comprising a dispersion term ([delta] D 1) and polarity term of the above range ([delta] P 1) and the hydrogen bond (delta] H 1), for example, triethylene glycol, glycerol, 2-pyrrolidone, 1- (2- Hydroxyethyl) -2-pyrrolidone, dipropylene glycol, propylene glycol, 1,5-pentanediol and the like can be used.
  • the dispersion term ([delta] D 1) and the polar term ([delta] P 1) and the hydrogen bond of the liquid medium the value of (delta] H 1) is, Hansen is a computer software Solubility Parameters in Practice 4th Edition 4.1.07 ( HSPiP) It is the value recorded in.
  • Liquid medium and a dispersion term ([delta] D 1) and polarity term of the range ([delta] P 1) and the hydrogen bond (delta] H 1) is 10 to 95 mass relative to the total amount of the liquid medium contained in the pigment composition It is preferably used in the range of%, and more preferably used in the range of 50 to 80% by mass.
  • the liquid medium contained in the pigment composition is preferably used in the range of 30 to 98% by mass, preferably in the range of 60 to 95% by mass, based on the total amount of the pigment composition of the present invention. It is preferable for producing ink.
  • the liquid medium used in the pigment composition of the present invention the water, the high point or boiling point solvent, and a the dispersion term ([delta] D 1) and the polar term ([delta] P 1) and the hydrogen bond (delta] H 1) It is preferable to use it in combination with a liquid medium or the like because the resin component such as the pigment dispersion resin is easily adsorbed on the surface of the pigment component.
  • the inkjet printing ink obtained by using the pigment composition is applied to a thermal type inkjet printing method described later.
  • the liquid medium, the water, the high point or boiling point solvent, the dispersion term ([delta] D 1) and the polar term ([delta] P 1) and the hydrogen bond (delta] H 1) and the liquid medium such as a combined use with a
  • the resin is easily adsorbed on the pigment and the storage stability and the like are improved.
  • the liquid medium shortens the time required for obtaining a pigment composition having desired physical properties (number of coarse particles, particle size, etc.) of solid content through the step 1 from the viewpoint of easily reducing the number of coarse particles efficiently. From the viewpoint of ease, it is preferable to 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.
  • the liquid medium preferably contains at least one selected from the group consisting of N- (2-hydroxyethyl) pyrrolidone, 2-pyrrolidone, triethylene glycol and glycerin.
  • the liquid medium preferably contains at least one selected from the group consisting of 2-pyrrolidone, triethylene glycol, dipropylene glycol and glycerin.
  • the liquid medium (a) contains at least one selected from the group consisting of dipropylene glycol, N- (2-hydroxyethyl) pyrrolidone, 2-pyrrolidone, triethylene glycol and glycerin. Is preferable.
  • the liquid medium (a) contains at least one selected from the group consisting of propylene glycol, N- (2-hydroxyethyl) pyrrolidone, 2-pyrrolidone, triethylene glycol and glycerin. Is preferable.
  • the content of the water-soluble organic solvent is preferably 10 to 500 parts by mass, more preferably 15 to 150 parts by mass with respect 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 solid content over time in the pigment composition, it is easy to prevent the occurrence of solid content over time in the ink, and the ink at the initial stage of ink ejection. It is easy to suppress the clogging of the ejection nozzle (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the clogging of the ink ejection nozzle over time (excellent ejection stability over time). Easy to get).
  • the liquid medium is preferably used in the range of 30 to 98% by mass with respect to the total amount of the pigment composition of the present invention, and it is preferable to use the liquid medium in the range of 60 to 95% by mass in producing a water-based ink. preferable.
  • the raw material composition can contain a resin component.
  • the resin component include pigment-dispersed resin and binder resin.
  • a resin component a conventionally known resin can be used, but for example, a radical polymer can be used, and it is preferable to use a radical polymer having an aromatic cyclic structure or a heterocyclic structure.
  • the ⁇ - ⁇ interaction between the resin component and the pigment component makes it easier for the resin component to be adsorbed on the pigment component, resulting in excellent storage stability that prevents the occurrence of sedimentation of solids over time in the pigment composition.
  • a radical polymer having an anionic group is used as a resin component (for example, a pigment-dispersed resin), a radical polymer (neutralized product) in which a part or all of the anionic group is neutralized by a basic compound is used. It is preferable to do so.
  • the resin component is easily dissolved in a liquid medium containing water, adsorption of the pigment component to the surface is promoted, and a good dispersed state is easily maintained.
  • it is easy to obtain excellent storage stability that prevents the occurrence of solid content over time in the pigment composition it is easy to prevent the occurrence of solid content over time in the ink, and the ink is ejected at the initial stage of ink ejection. It is easy to suppress the clogging of the nozzle (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the clogging of the ink ejection nozzle over time (excellent ejection stability over time).
  • Cheap cheap
  • Examples of the aromatic cyclic structure or the heterocyclic structure include a cyclic structure introduced into the radical polymer by using a monomer having an aromatic ring structure or a heterocyclic structure.
  • the aromatic cyclic structure is preferably a benzene ring structure, more preferably a styrene-derived structure.
  • radical polymer that can be used as a resin component
  • a polymer obtained by radical polymerization of various monomers can be used.
  • a monomer having an aromatic cyclic structure can be used when introducing an aromatic cyclic structure into the resin component, and when introducing a heterocyclic structure, a monomer having an aromatic cyclic structure can be used.
  • a monomer having a heterocyclic structure can be used.
  • Examples of the monomer having an aromatic cyclic structure include styrene, p-tert-butyldimethylsiloxystyrene, o-methylstyrene, p-methylstyrene, p-tert-butylstyrene, p-tert-butoxystyrene, and m-.
  • tert-butoxystyrene p-tert- (1-ethoxymethyl) styrene, m-chlorostyrene, p-chlorostyrene, p-fluorostyrene, ⁇ -methylstyrene, p-methyl- ⁇ -methylstyrene, vinylnaphthalene, vinyl Anthracen and the like can be mentioned.
  • Examples of the monomer having a heterocyclic structure include vinylpyridine-based monomers such as 2-vinylpyridine and 4-vinylpyridine.
  • the monomer When a polymer having both an aromatic cyclic structure and a heterocyclic structure is used as the radical polymer, the monomer has a monomer having an aromatic cyclic structure and a heterocyclic structure. Monomers can be used in combination.
  • a radical polymer having an aromatic cyclic structure is preferable. Therefore, as the monomer, a monomer having an aromatic cyclic structure is preferable, and at least one selected from the group consisting of styrene, ⁇ -methylstyrene and tert-butylstyrene is more preferable.
  • the content of the monomer having an aromatic cyclic structure or a heterocyclic structure is 20% by mass or more based on the total amount of the monomers from the viewpoint of further enhancing the adsorptivity of the resin component to the pigment component.
  • 40% by mass or more is more preferable, and 50 to 95% by mass is further preferable.
  • a monomer having an anionic group can be used as the monomer from the viewpoint of producing a radical polymer having an acid value in the range described later.
  • the monomer having an anionic group examples include a monomer having an anionic group such as a carboxy group, a sulfo group, and a phosphoric acid group.
  • a monomer having an anion 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.
  • 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, and the ink at the initial stage of ink ejection. It is easy to suppress the clogging of the ejection nozzle (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the clogging of the ink ejection nozzle over time (excellent ejection stability over time). Easy to get).
  • the content of the monomer having an anionic group is 5 to 80 based on the total amount of the monomers that can be used for producing the resin component from the viewpoint of easily obtaining a radical polymer having an acid value in the range described later. It is preferably by mass, more preferably 5 to 60% by mass, still more preferably 5 to 50% by mass.
  • the monomer that can be used for producing the resin component other monomers can be used, if necessary, in addition to the above-mentioned monomers.
  • examples of other monomers include methyl (meth) acrylate, n-propyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, sec-butyl (meth) acrylate, and tert-butyl ( Meta) 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,
  • 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, or the like should be used. Can be done.
  • the monomer sequence of each polymer is not particularly limited, and a polymer having a random type sequence or a block type sequence can be used.
  • a polymer having a crosslinked structure can be produced by using a monomer having a crosslinkable functional group as a monomer.
  • the monomer having a crosslinkable functional group include ethylene glycol di (meth) acrylate, propylene glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, poly (oxyethylene oxypropylene) glycol di (meth) acrylate, and the like.
  • Poly (meth) acrylates of polyhydric alcohols such as tri (meth) acrylates of glycerin alkylene oxide adducts; glycidyl (meth) acrylates; divinylbenzene and the like can be mentioned.
  • a polymer having a structural unit derived from the above-mentioned monomer can be used, but only a monomer having an anionic group and a monomer having an aromatic ring structure or a heterocyclic structure can be used.
  • a polymer obtained by polymerizing the above is preferable.
  • a polymer having a structural unit derived from styrene and a structural unit derived from (meth) acrylic acid is preferable, and a styrene- (meth) acrylic acid copolymer and a styrene- (meth) acrylic acid-based ester are used.
  • -At least one selected from the group consisting of (meth) acrylic acid copolymers is more preferable.
  • a 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 strongly adsorbed on the surface of the pigment component, and the carboxy group in the structural unit derived from (meth) acrylic acid has a good affinity with water, so that the dispersion is stabilized well. Is easy to obtain. As a result, it is easy to obtain excellent storage stability that prevents the occurrence of solid content over time in the pigment composition, it is easy to prevent the occurrence of solid content over time in the ink, and the ink is ejected at the initial stage of ink ejection. It is easy to suppress the clogging of the nozzle (it is easy to obtain excellent initial ejection stability), and it is easy to suppress the clogging of the ink ejection nozzle over time (excellent ejection stability over time). Cheap).
  • any of a styrene-acrylic acid copolymer, a styrene-methacrylic acid copolymer, and a styrene-acrylic acid-methacrylic acid copolymer can be used, but styrene- At least one selected from the group consisting of an acrylic acid copolymer and a styrene-acrylic acid-methacrylic acid copolymer is preferable.
  • the total amount of the structural unit derived from styrene, the structural unit derived from acrylic acid and the structural unit derived from methacrylic acid is the structural unit of the styrene- (meth) acrylic acid copolymer. Based on the total amount, 80 to 100% by mass is preferable, and 90 to 100% by mass is more preferable.
  • the radical polymerization rate (reaction rate) of each monomer during radical polymerization is almost the same, and the usage ratio (preparation ratio) of each monomer is a structural unit derived from each monomer constituting the radical polymer. Is considered to be the same as the ratio of.
  • the radical polymer can be produced, for example, by radically polymerizing the above-mentioned monomer by a method such as a massive polymerization method, a solution polymerization method, a suspension polymerization method, or an emulsion polymerization method.
  • a known and commonly used polymerization initiator chain transfer agent (polymerization degree adjusting agent), surfactant, defoaming agent and the like can be used, if necessary.
  • polymerization initiator examples include 2,2'-azobis (2,4-dimethylvaleronitrile), 2,2'-azobisisobutyronitrile, and 1,1'-azobis (cyclohexane-1-carbonitrile). , Benzoyl peroxide, dibutyl peroxide, butyl peroxybenzoate and the like.
  • the content of the polymerization initiator is preferably 0.1 to 10% by mass based on the total amount of the monomers used in the production of the radical polymer.
  • the radical polymer obtained by the solution polymerization method when used, as the resin component, the radical weight obtained by removing the solvent contained in the radical polymer solution obtained by the solution polymerization method, drying and pulverizing the particles into fine particles. Coalescence can be used.
  • the resin component which is a finely divided radical polymer, is used in combination with a water-soluble organic solvent and a basic compound, it is neutralized by the basic compound in the 0th step, and is a liquid medium containing the water-soluble organic solvent. The pigment component dissolved in the liquid medium and wet with the liquid medium is adsorbed on the surface.
  • a resin component classified by a mesh-like sieve having an eye size (diameter) of 1 mm or less is preferable.
  • the acid value of the resin component is preferably 60 to 300 mgKOH / g, more preferably 80 to 250 mgKOH / g, further preferably 100 to 200 mgKOH / g, and an acid value of 120 to 180 mgKOH / g is used. It is particularly preferable to do so. In these cases, the adsorptivity of the resin component to the pigment component can be enhanced, and an appropriate affinity for a liquid medium (for example, a liquid medium containing water and a water-soluble organic solvent) can be easily obtained, so that the dispersion is good. Easy to maintain state.
  • a liquid medium for example, a liquid medium containing water and a water-soluble organic solvent
  • the acid value is preferably an acid value derived from an anionic group such as a carboxy group, a sulfo group, or a phosphoric acid group.
  • an anionic group such as a carboxy group, a sulfo group, or a phosphoric acid group.
  • the acid value except that tetrahydrofuran is used as the solvent instead of diethyl ether, Japanese Industrial Standards "K0070: 1992. Test of acid value, saponification value, ester value, iodine value, hydroxyl value and unsaponifiable matter of chemical products”. It is a numerical value measured according to "Method” and refers to the amount (mg) of potassium hydroxide required to completely neutralize 1 g of the resin component.
  • the weight average molecular weight of the resin component is preferably 2000 to 40,000, more preferably 5000 to 30000, further preferably 5000 to 25000, preferably in the range of 6000 to 20000, and preferably in the range of 8000 to 12000. Is particularly preferable. In these cases, aggregation with adjacent pigment components is suppressed, it is easy to obtain excellent storage stability that prevents the occurrence of sedimentation of solids in the pigment composition over time, and sedimentation of solids in the ink over time is easy to obtain.
  • the "weight average molecular weight” is a value measured by a GPC (gel permeation chromatography) method, and is a value converted to the molecular weight of polystyrene used as a standard substance.
  • the content of the resin component is preferably 5 to 200 parts by mass, more preferably 10 to 100 parts by mass with respect to 100 parts by mass of the pigment component.
  • a liquid medium for example, water
  • the resin component is easily adsorbed on the pigment component.
  • It is easy to obtain excellent storage stability to prevent 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 initial stage of ink ejection (excellent initial ejection).
  • the raw material composition may contain a basic compound.
  • the basic compound neutralizes the anionic group when the resin component has an anionic group.
  • the affinity of the pigment component adsorbed by the resin component on the aqueous medium is enhanced.
  • it is easy to reduce coarse particles, it is easy to stabilize the dispersed state of solids in the pigment composition, it is easy to effectively prevent the generation of coarse particles over time, and it is easy to suppress the generation of sedimentation of solids over time. It's easy to do.
  • an inorganic basic compound As the basic compound, an inorganic basic compound, an organic basic compound, or the like can be used.
  • the inorganic basic compound include 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; Examples include carbonates.
  • organic basic compounds include amino alcohols such as triethanolamine, N, N-dimethanolamine, N-ethylethanolamine, dimethylethanolamine, and N-butyldiethanolamine; morpholin, N-methylmorpholin, and N-ethyl.
  • Morphorines such as morpholin; piperazine such as N- (2-hydroxyethyl) piperazine and piperazine hexahydrate; ammonium hydroxide and the like can be mentioned. Since the basic compound has excellent neutralization efficiency of the resin component, the alkali metal hydroxide (potassium hydroxide, hydroxide) can easily improve the dispersion stability of the pigment component adsorbed by the resin component in an aqueous medium. Sodium, lithium hydroxide, etc.) is preferable, and potassium hydroxide is more preferable.
  • a basic compound in a range in which the neutralization rate of the resin component is 80 to 120%.
  • the pigment composition according to the present embodiment is diluted to a desired concentration with the above-mentioned liquid medium, and / or a resin component (a binder such as the above-mentioned acrylic resin and polyurethane resin), a drying inhibitor, and a penetrant.
  • a resin component a binder such as the above-mentioned acrylic resin and polyurethane resin
  • Surfactants, preservatives, viscosity regulators, pH regulators, chelating agents, plasticizers, antioxidants, UV absorbers and other additives can be used as inks. After obtaining the ink, a centrifugation treatment or a filtration treatment may be performed.
  • the ink examples include paints for automobiles or building materials; printing inks such as inkjet printing inks, offset inks, gravure inks, flexo inks, and silk screen inks.
  • the content of the pigment component in the ink is preferably 1 to 10% by mass based on the total amount of the ink.
  • 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 within a suitable range.
  • the water-soluble organic solvent the above-mentioned water-soluble organic solvent can be used as a constituent component of the raw material composition.
  • the water-soluble organic solvent from the viewpoint of enhancing the permeability of the ink into the recording medium, 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; propylene glycol propyl ether. Such as propylene oxide adducts of alkyl alcohols and the like.
  • the anti-drying agent examples include glycerin, ethylene glycol, diethylene glycol, triethylene glycol, triethylene glycol mono-n-butyl ether, polyethylene glycol having a molecular weight of 2000 or less, propylene glycol, dipropylene glycol, tripropylene glycol, and 1,3-propylene glycol. , Isopropylene glycol, isobutylene glycol, 1,4-butanediol, 1,3-butanediol, 1,5-pentanediol, 1,6-hexanediol, mesoerythritol, pentaerythritol and the like.
  • the anti-drying agent the same compound as the above-mentioned water-soluble organic solvent used in the raw material composition can be used. Therefore, when a water-soluble organic solvent is already used in the raw material composition, it can also serve as a drying inhibitor.
  • the penetrant can be used for the purpose of improving the permeability to the recording medium or adjusting the dot diameter on the recording medium.
  • 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.
  • Surfactants can be used to adjust 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, and the like, and anionic surfactants and nonionic surfactants. At least one selected from the group consisting of sex surfactants is preferred.
  • the surfactant may be used alone or in combination of two or more.
  • anionic surfactants include alkylbenzene sulfonates, alkylphenyl sulfonates, alkylnaphthalene sulfonates, higher fatty acid salts, higher fatty acid ester sulfates, higher fatty acid ester sulfonates, and higher alcohol ether sulfates.
  • ester salts and sulfonates include ester salts and sulfonates, higher alkyl sulfosuccinates, polyoxyethylene alkyl ether carboxylates, polyoxyethylene alkyl ether sulfates, alkyl phosphates, polyoxyethylene alkyl ether phosphates and the like.
  • Nonionic surfactants include polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, glycerin fatty acid ester, and poly.
  • polyoxyethylene nonylphenyl ether polyoxyethylene octylphenyl ether, polyoxyethylene dodecylphenyl ether, polyoxyethylene alkyl ether, polyoxyethylene fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, fatty acid.
  • At least one selected from the group consisting of alkylolamide, acetylene glycol, an oxyethylene adduct of acetylene glycol, and polyethylene glycol polypropylene glycol block copolymer is preferable.
  • surfactants include silicone-based surfactants such as polysiloxane oxyethylene adducts; fluorine-based surfactants such as perfluoroalkyl carboxylic acid salts, perfluoroalkyl sulfonates, and oxyethylene perfluoroalkyl ethers; Biosurfactants such as sporic acid, ramnolipide, and lysolecithin can also be used.
  • silicone-based surfactants such as polysiloxane oxyethylene adducts
  • fluorine-based surfactants such as perfluoroalkyl carboxylic acid salts, perfluoroalkyl sulfonates, and oxyethylene perfluoroalkyl ethers
  • Biosurfactants such as sporic acid, ramnolipide, and lysolecithin can also be used.
  • the pigment composition for ink obtained by the above method it is preferable to use a pigment composition in which 20 to 60% by mass of the resin component is adsorbed on the pigment component with respect to the total amount of the resin component, which has a remarkable viscosity over time. It is preferable because a pigment composition that does not easily cause an increase and has very excellent storage stability can be obtained.
  • the mass ratio of the resin component adsorbed on the pigment component to the total amount of the resin component [mass of the resin component adsorbed on the pigment component / mass of the total amount of the resin component] (hereinafter, "resin adsorption rate" (Omitted) refers to the value calculated by the following method.
  • the flow potential in the range of ⁇ 2500 mV was measured with the platinum electrode of the sample cell.
  • the pigment composition was placed in a sample cell and titrated with a titration solution (0.01N, Poly-DADMAC). The charge amount was titrated based on the potential difference caused by the movement of the sample cell and the moving piston (that is, the flow potential of the liquid). Titration was terminated when the flow potential exceeded zero (the potential became positive). The value obtained by multiplying the value obtained by dividing the dropping amount from the inflection point by the dropping amount when the flow potential became zero by 100 was obtained as the resin adsorption rate.
  • the resin adsorption rate has excellent storage stability because it does not easily cause a significant increase in viscosity over time, and further, the number of coarse particles having a particle size of 1.0 ⁇ m or more that can be contained in the pigment composition can be determined.
  • the range is more preferably 20 to 50% by mass, and particularly preferably 25 to 40% by mass.
  • the weight average molecular weight is a value measured by a GPC (gel permeation chromatography) method, and is a value converted to the molecular weight of polystyrene used as a standard substance. The measurement was performed with the following equipment and conditions.
  • Liquid transfer pump LC-9A (manufactured by Shimadzu Corporation)
  • System controller SLC-6B (manufactured by Shimadzu Corporation)
  • Auto injector S1L-6B (manufactured by Shimadzu Corporation)
  • Detector RID-6A (manufactured by Shimadzu Corporation)
  • Data processing software Sic480II Data Station (manufactured by System Instruments)
  • Elution solvent THF (tetrahydrofuran)
  • Elution flow rate 2 mL / min Column temperature: 35 ° C
  • a styrene-acrylic acid copolymer B was obtained in the above procedure. The acid value of the styrene-acrylic acid copolymer B was 170 mgKOH / g, and the weight average molecular weight was 11000.
  • a rotor stator type processing machine manufactured by IKA Co., Ltd., equipment name: magic LAB, 3-stage type, 2P / 4M / 6F processing unit (rotor and stator), in-line type, in order from the upper part in the vertical direction).
  • a second raw material composition was prepared by performing a 5-pass treatment at a peripheral speed of 34 m / s (share rate: 170000s -1) and a rotation speed of 20000 rpm while heating at 60 ° C.
  • step 1 a process of ejecting and colliding the second raw material composition at a pressure of 140 MPa using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, oblique collision chamber).
  • a pigment composition was obtained by applying 1 pass.
  • Reference example A3 Same as Reference Example A2 except that the pressure when ejecting the second raw material composition was changed from 140 MPa to 200 MPa using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber).
  • the pigment composition was obtained by the method of.
  • the first raw material composition was prepared by the same procedure as in Example A1.
  • the first raw material composition was put into a disper mixer (manufactured by EYELA, device name: MAZELA ZZ-1000 / 1000S, maximum peripheral speed: 15 m / s, maximum rotation speed: 3000 rpm).
  • the second raw material composition was obtained by stirring at a peripheral speed of 12 m / s and a rotation speed of 2400 rpm for 30 minutes while heating at 60 ° C.
  • step 1 a process of ejecting the second raw material composition at a pressure of 140 MPa and colliding with the ball using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber). , To obtain a pigment composition.
  • a high-pressure homogenizer manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber.
  • the first raw material composition was prepared by the same procedure as in Example A1.
  • zirconia beads ( ⁇ 0.3 mm) having a mass 20 times the mass of the pigment were added to the first raw material composition, and a bead mill (manufactured by Imex Co., Ltd., device name: Easy Nano RMB type, maximum circumference) was added.
  • the second raw material composition was obtained by feeding at a speed of 15 m / s and a maximum rotation speed of 2650 rpm and stirring at a peripheral speed of 12 m / s and a rotation speed of 2100 rpm for 30 minutes while cooling at 15 ° C.
  • step 1 a process of ejecting the second raw material composition at a pressure of 200 MPa and colliding with the ball using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber). , To obtain a pigment composition.
  • a high-pressure homogenizer manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber.
  • Example A6 Reference Example A2 and reference example A2 except that the pressure when ejecting the second raw material composition was changed from 140 MPa to 100 MPa using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: starburst, oblique collision chamber). A pigment composition was obtained in the same manner.
  • a high-pressure homogenizer manufactured by Sugino Machine Limited, device name: starburst, oblique collision chamber.
  • Example A1 using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: star burst, single nozzle chamber) instead of the high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: star burst, oblique collision chamber).
  • a pigment composition was obtained in the same manner as in Example A1 except that the same second raw material composition as that used in 1 was passed through the single nozzle chamber at a pressure of 140 MPa for 1 pass. ..
  • Comparative Example A3 Same as Comparative Example A2 except that the pressure when ejecting the second raw material composition was changed from 140 MPa to 200 MPa using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, single nozzle chamber). The pigment composition was obtained by the method of.
  • Red pigment composition 1500 g of red pigment (FASTOGEN SUPER MAGENTA RY WET pigment, manufactured by DIC Corporation, pigment concentration: 32% by mass, wet pigment), 95 g of the above-mentioned styrene-acrylic acid-based copolymer B, 356 g of triethylene glycol and 34% by mass of water.
  • a first raw material composition pigment concentration: 24% by mass, solid content concentration: 28% by mass
  • a rotor stator type processing machine manufactured by IKA Co., Ltd., equipment name: magic LAB, 3-stage type, 2P / 4M / 6F processing unit (rotor and stator), in-line type, in order from the upper part in the vertical direction).
  • a second raw material composition was prepared by performing a 5-pass treatment at a peripheral speed of 34 m / s (share rate: 170000s -1) and a rotation speed of 20000 rpm while heating at 60 ° C.
  • step 1 a process of ejecting and colliding the second raw material composition at a pressure of 200 MPa using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, oblique collision chamber).
  • a pigment composition was obtained by applying 1 pass.
  • Reference example B2 instead of the high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, oblique collision chamber), a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber) is used.
  • a pigment composition was obtained in the same manner as in Reference Example A2, except that one pass was applied to the treatment of ejecting the raw material composition of No. 1 at a pressure of 200 MPa and causing it to collide with a ball.
  • the first raw material composition was put into a disper mixer (manufactured by EYELA, device name: MAZELA ZZ-1000 / 1000S, maximum peripheral speed: 15 m / s, maximum rotation speed: 3000 rpm).
  • the second raw material composition was obtained by stirring at a peripheral speed of 12 m / s and a rotation speed of 2400 rpm for 30 minutes while heating at 60 ° C.
  • step 1 a process of ejecting the second raw material composition at a pressure of 200 MPa and colliding with the ball using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber). , To obtain a pigment composition.
  • a high-pressure homogenizer manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber.
  • Example B2 First, the first raw material composition was prepared by the same procedure as in Example B1.
  • the first raw material composition was put into a disper mixer (manufactured by EYELA, device name: MAZELA ZZ-1000 / 1000S, maximum peripheral speed: 15 m / s, maximum rotation speed: 3000 rpm).
  • the second raw material composition was obtained by stirring at a peripheral speed of 12 m / s and a rotation speed of 2400 rpm for 30 minutes while heating at 60 ° C.
  • step 1 a process of ejecting the second raw material composition at a pressure of 200 MPa and colliding with the ball using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber). , To obtain a pigment composition.
  • a high-pressure homogenizer manufactured by Sugino Machine Limited, device name: Starburst, ball collision chamber.
  • a rotor stator type processing machine manufactured by IKA Co., Ltd., equipment name: magic LAB, 3-stage type, 2P / 4M / 6F processing unit (rotor and stator), in-line type, in order from the upper part in the vertical direction).
  • a second raw material composition was prepared by performing a 5-pass treatment at a peripheral speed of 34 m / s (share rate: 170000s -1) and a rotation speed of 20000 rpm while heating at 60 ° C.
  • the second raw material composition is passed through the single nozzle chamber at a pressure of 200 MPa using a high-pressure homogenizer (manufactured by Sugino Machine Limited, device name: Starburst, single nozzle chamber).
  • a pigment composition was obtained by subjecting the treatment to two passes.
  • the number of particles having a diameter of 1.0 ⁇ m or more and the number of particles having a diameter of 0.5 ⁇ m or more were measured using a particle size distribution meter (manufactured by Particle Sigmas Systems, Accuser 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 pieces / mL.
  • the number of particles having a diameter of 1.0 ⁇ m or more and the number of particles having a diameter of 0.5 ⁇ m or more contained in the diluted pigment composition were measured three times. Subsequently, the average value of the values obtained by multiplying the measured value of the number of particles by the dilution concentration was calculated as the number of coarse particles.
  • the pigment composition was placed in a cell of about 4 mL.
  • the particle size was measured by detecting scattered light of laser light in an environment of 25 ° C. using a nanotrack particle size distribution meter "UPA150" manufactured by Microtrac Bell Co., Ltd.
  • the particle size the volume average particle size (Mv), the number average particle size (Mn), D50, D90 and D95 were measured.
  • the pigment composition was sealed in a polypropylene container and then stored at 60 ° C. for 1 week. Then, the volume average particle diameter (Mv), the viscosity, and the rate of change before and after storage in the number of coarse particles having a diameter of 0.5 ⁇ m were calculated.
  • Those having a rate of change within the range of 10% can be evaluated as having excellent storage stability, those having a rate of change of more than 10% and within 15% can be evaluated as having good storage stability, and those having a rate of change exceeding 15%. It was evaluated that the storage stability was not sufficient.
  • Pigment composition obtained by centrifugation 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, and Surfinol 440 (Nisshin Chemical Industry Co., Ltd.)
  • a water-based ink for inkjet recording was obtained by mixing 0.5 parts by mass of (manufactured by the company) and 47.2 parts by mass of ion-exchanged water.
  • the pigment concentration in the ink obtained by using the black pigment composition was 2.5% by mass
  • the pigment concentration in the ink obtained by using the red pigment composition was 3.5% by mass.
  • Inkjet recording ink was filled in a cartridge of an inkjet printer ENVY4500 (manufactured by HP Inc.). Subsequently, after cleaning the printer mounted once, an image having a 100% solid part is printed on commercially available PPC paper (sold by Otsuka Shokai, product number: 10PPCHWA4N) in plain paper / standard printing mode. A printed matter was obtained by doing so.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
PCT/JP2020/041274 2019-11-21 2020-11-05 顔料組成物の製造方法 Ceased WO2021100468A1 (ja)

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CN202080077285.2A CN114667325A (zh) 2019-11-21 2020-11-05 颜料组合物的制造方法
JP2021558275A JP7306475B2 (ja) 2019-11-21 2020-11-05 顔料組成物の製造方法
US17/771,881 US20220372324A1 (en) 2019-11-21 2020-11-05 Method for producing pigment composition
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JPH1036738A (ja) * 1996-07-22 1998-02-10 Mitsubishi Pencil Co Ltd インキジェット用インキ組成物の製造方法及びインキジェット用インキ組成物
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WO2009075802A2 (en) * 2007-12-07 2009-06-18 Cabot Corporation Method of preparing a pigment composition
JP5213467B2 (ja) * 2008-01-30 2013-06-19 富士フイルム株式会社 インクジェット記録方法
JP5664027B2 (ja) 2010-08-31 2015-02-04 セイコーエプソン株式会社 インクジェット記録方法、インクジェット記録装置、及び記録物
JP5990378B2 (ja) * 2010-12-28 2016-09-14 花王株式会社 インクジェット記録用インクセット
JP2013124356A (ja) * 2011-12-16 2013-06-24 Kao Corp インクジェット記録用水系顔料分散体の製造方法
JP6083489B2 (ja) * 2014-09-02 2017-02-22 Dic株式会社 水性顔料分散体、インクジェット記録用インク及び印字物
JP2016216568A (ja) * 2015-05-18 2016-12-22 キヤノン株式会社 顔料分散体およびインクジェット用インク
JP6862692B2 (ja) * 2016-06-30 2021-04-21 Dic株式会社 水性顔料分散体の製造方法
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JPH1036738A (ja) * 1996-07-22 1998-02-10 Mitsubishi Pencil Co Ltd インキジェット用インキ組成物の製造方法及びインキジェット用インキ組成物
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