AQUEOUS PIGMENT DISPERSION AND AQUEOUS INK

Abstract

The present invention provides an aqueous pigment dispersion including at least a pigment, colloidal silica, bio-nanofibers having an average diameter of 1 nm to 100 nm and an aspect ratio of 100 or more, an anionic group-containing organic polymer compound, and also provides an aqueous ink. The bio-nanofibers are preferably cellulose nanofibers or chitosan nanofibers, and the ratio between the pigment, the colloidal silica, and the bio-nanofibers preferably satisfies (1) colloidal silica/pigment=1/100 to 20/100 or (2) colloidal silica/bio-nanofibers=1/2 to 10/1 and (3) bio-nanofibers/pigment=1/100 to 15/100.

Claims

1. An aqueous pigment dispersion comprising at least a pigment, colloidal silica, bio-nanofibers having an average diameter of 1 nm to 100 nm and an aspect ratio of 100 or more, an anionic group-containing organic polymer compound.

2. The aqueous pigment dispersion according to claim 1, wherein the bio-nanofibers are cellulose nanofibers or chitosan nanofibers.

3. The aqueous pigment dispersion according to claim 1, wherein the ratio between the pigment, the colloidal silica, and the bio-nanofibers satisfies the following: (1) colloidal silica/pigment=1/100 to 20/100 or (2) colloidal silica/bio-nanofibers=1/2 to 10/1 and (3) bio-nanofibers/pigment=1/100 to 15/100.

4. The aqueous pigment dispersion according to claim 1, wherein the anionic group-containing organic polymer compound is at least one selected from the group consisting of acrylic resins having anionic groups, polyurethane resins having anionic groups, and polysaccharide derivatives having anionic groups.

5. An aqueous ink comprising the aqueous pigment dispersion according to claim 1.

Description

EXAMPLES

[0168] The present invention is described in detail by giving examples below.

[0169] In addition, “parts” and “%” are “parts by mass” and “% by mass”, respectively, unless otherwise specified.

(Colloidal Silica)

[0170] The colloidal silica used (“Quartron PL Series” (trade name) manufactured by Fuso Chemical Co., Ltd.) is described in Table 1 below.

TABLE-US-00001 TABLE 1 Product name PL-1 PL-3 PL-3L PL-7 PL-10H Silica shape Associated Cocoon- Spherical Spherical Associated like pH (20° C.) 7.1 7.2 7.3 7.3 7.3 Specific 1.070 1.120 1.120 1.114 1.149 gravity (20/4° C.) Silica 12 19.5 19.6 23.0 23.7 concentra- tion (%) Primary 14.9 35.5 36 76.7 88.8 particle diameter/nm Secondary 38 67 56 120 212 particle diameter/nm

<Bio-Nanofibers>

[0171] The bio-nanofibers shown in Table 2 were used.

TABLE-US-00002 TABLE 2 Cellulose Cellulose Chitosan Bio-nanofiber nanofiber nanofiber nanofiber Product name Celish BiNFi-s BiNFi-s KY100G 2% cellulose chitosan Maker Daicel Sugino Sugino Machine FineChem Machine Limited Ltd. Limited Product name CEL-KY CEL-NF CHI-NF (abbreviation) Aspect ratio 160 270 430 Mode diameter 340 nm 410 nm 320 nm 80% particle 5.7 5.3 5.3 diameter/ 20% particle diameter Specific surface — 2059 cm.sup.2/cm.sup.3 1959 cm.sup.2/cm.sup.3 area Degree of 58% — — crystallization Amount of carboxyl Less than Less than — group 0.1 mmol/g 0.1 mmol/g

[0172] The average fiber diameter and aspect ratio are calculated from the results of SEM analysis. Specifically, a bio-nanofiber dispersion was cast on a wafer and observed with SEM, and fiber diameter and fiber length values of 20 or more fibers per image are read. This was performed for images of at least three regions which were not overlapped with each other, to obtain information of the fiber diameters and fiber lengths of at least 30 fibers. The average fiber diameter was calculated to two significant figures from the data of fiber diameters. The average fiber length was calculated from the data of fiber lengths, and the aspect ratio was calculated to two significant figures by aspect ratio=average fiber diameter/average fiber length.

[0173] The mode diameter and (80% particle diameter/20% particle diameter) were calculated to two significant figures from measurement values (volume basis) of 0.1% by mass of bio-nanofibers (solvent: water, temperature 25° C.) by using dynamic light scattering Nanotrac particle size analyzer UPA-150EX (manufactured by Nikkiso Co., Ltd.).

[0174] The specific surface area was calculated from particle size distribution values measured by a light scattering method using laser diffraction/scattering particle size distribution analyzer LA-960 (manufactured by Horiba, Ltd.). The measurement conditions are given below.

[0175] Measurement range: 0.01 μm to 3,000 μm, measurement method: wet method, basis of the particle diameter: volume, dispersion medium: pure water

[0176] Sample refractive index: 1.56 to 0.00i, dispersion medium refractive index: 1.333 to 0.00i

[0177] Dispersion treatment: built-in ultrasonic waves (30 W) 1 minute, circulation speed: 3, stirring speed: No

[0178] Transmittance (semiconductor laser beam) and transmittance (LED light): 80% or more

[0179] The degree of crystallization of cellulose was calculated according to a formula below from the diffraction intensity of a 002 plane at 2θ=22.6° and the diffraction intensity of an amorphous portion at 2θ-18.5° using the diffraction intensity at 2θ-4° to 32° as a baseline in a diffraction chart obtained by measurement of X-ray crystal diffraction (apparatus: RINT-2000 (manufactured by Rigaku Corporation)) at a measurement voltage of 40 kV, a measurement current of 50 mA, and a scan speed of 2°/min.

χ.sub.c=(I.sub.002c−I.sub.a)/I.sub.002c×100 [Math. 5]

[0180] (In the formula, χ.sub.c represents the degree of crystallization of type I cellulose (%), I.sub.002c represents the 002 plane diffraction intensity at 2θ=22.6°, and I.sub.a represents the amorphous portion diffraction intensity at 2θ=18.5°.)

[0181] The following compounds were used as the anionic group-containing organic polymer compound.

(Polysaccharide Derivative Having Anionic Group)

[0182] Commercial products were used.

[0183] CMC1390 (manufactured by Daicel FineChem Ltd.): sodium carboxylmethyl cellulose (etherification degree, 1.0 to 1.5)

[0184] DN-800H (manufactured by Daicel FineChem Ltd.): ammonium carboxylmethyl cellulose

[0185] DN-100L (manufactured by Daicel FineChem Ltd.): ammonium carboxylmethyl cellulose

[0186] DN-10L (manufactured by Daicel FineChem Ltd.): ammonium carboxylmethyl cellulose

(Acrylic Resin Having Anionic Group)

Production Example 101: Solution (SA-1) of Acrylic Resin Having Anionic Group

[0187] A resin A having a monomer composition ratio (styrene/methacrylic acid/acrylic acid) of 77/13/10 (mass ratio), a weight-average molecular weight of 8800, an acid value of 150 mgKOH/g, and a glass transition temperature of 107° C. was produced. Then, 87.4 parts of ion exchange water and 22 g of a 34 mass % aqueous potassium hydroxide (KOH) solution were added to 50 parts of methyl ethyl ketone (abbreviated as “MEK” hereinafter) and 50 parts of the resin A, and the resultant mixture was sufficiently stirred to prepare a resin solution. Then, MEK was removed from the resin solution at a water bath temperature of 45° C. under a reduced pressure condition of 40 hPa, thereby preparing a solution (SA-1) of an acrylic resin having an anionic group with a resin sold content of 20%.

(Polyurethane Resin Having Anionic Group)

Production Example 102: Solution (UR-1) of Polyurethane Resin Having Anionic Group

[0188] In a vessel replaced with nitrogen and provided with a thermometer, a nitrogen gas inlet tube, and a stirrer, 64.2 parts by mass of methyl ethyl ketone was added, and 18.4 parts by mass of 2,2-dimethylol propionic acid and 33.9 parts by mass of isophorone diisocyanate were mixed in the methyl ethyl ketone, followed by reaction at 80° C. for 4 hours. Four hours after, 38.2 parts by mass of methyl ethyl ketone was further supplied and the resultant mixture was cooled to 60° C. or lower, and 140.1 parts by mass of polyether polyol (“PTMG2000” polytetramethylene glycol manufactured by Mitsubishi Chemical Corporation, number-average molecular weight 1,000) and 0.01 parts by mass of dibutyltin dilaurate (hereinafter “DBTDL”) were added and continuously reacted at 80° C.

[0189] After it was confirmed that the weight-average molecular weight of the reaction product reached a range of 20,000 to 50,000, the reaction was terminated by adding 1.3 parts by mass of methanol. Next, 41.6 parts by mass of methyl ethyl ketone was added to the reaction product to prepare an organic solvent solution of urethane resin.

[0190] The carboxyl groups possessed by the urethane resin were partially or entirely neutralized by adding 15.1 parts by mass of a 50 mass % aqueous potassium hydroxide solution to the urethane resin organic solvent solution. Next, 848.5 parts by mass of water was added and sufficiently stirred to produce a mixture containing the urethane resin, methyl ethyl ketone, and water, the urethane resin being dispersed or dissolved in the water.

[0191] Next, after aging of the mixture for about 2 hours, 0.07 parts by mass of Surfynol 440 (manufactured by Air Products and Chemicals, Inc., acetylene glycol ethylene oxide adduct, nonvolatile content 100% by mass) was added to the mixture and stirred for about 20 minutes to produce a mixture, which was then distilled under a reduced pressure condition of about 1 to 50 kPa.

[0192] After it was confirmed that 144 parts by mass of methyl ethyl ketone contained in the mixture was removed, 0.03 parts by mass of Surfynol 440 (manufactured by Air Products and Chemicals, Inc.,) was added under reduced pressure, and then reduced-pressure distillation was continued. Next, after it was confirmed that 147 parts by mass of water contained in the mixture was removed, the reduced-pressure distillation was terminated.

[0193] Next, the nonvolatile content was adjusted by adding water to prepare a solution (UR-1) of a polyurethane resin having an anionic group with a resin sold content of 20% by mass.

[0194] Commercial products below were used as the pigment or the like.

(Pigment)

[0195] #960 (manufactured by Mitsubishi Chemical Corporation): carbon black

[0196] FASTOGEN Blue TGR (manufactured by DIC Corporation): C.I. Pigment Blue 15:3

[0197] FASTOGEN Super Magenta RY (manufactured by DIC Corporation): C.I. Pigment Red 122

[0198] Fast Yellow 7413 (manufactured by Sanyo Color Works, Ltd.): C.I. Pigment Yellow 74

Production Example 1: Method for Producing Ultrasonic Dispersion (US) Aqueous Black Pigment Dispersion

[0199] In a metal beaker, 20 parts of “#960” (carbon black manufactured by Mitsubishi Chemical Corporation), 20 parts of the solution (SA-1) of the anionic group-containing organic polymer compound, 5 parts of triethylene glycol, and water were added so that a total amount was 100 parts, and the resultant mixture was manually stirred. Then, ultrasonic dispersion was performed with an ultrasonic disperser (UP200St manufactured by Hielscher Company, operation frequency: 26 KHz, operation output: 160 W) for 10 minutes. After the ultrasonic dispersion treatment, 1.0 part (in terms of solid content) of bio-nanofibers “BiNFi-s 2% cellulose” (manufactured by Sugino Machine Limited, product name (abbreviation): CEL-NF), 2.0 parts (in terms of solid content) of colloidal silica “Quartron PL-3” (manufactured by Fuso Chemical Co., Ltd., product name (abbreviation): PL-3)), and pure water were added to 100 parts of the mixture so that a total amount was 250 parts, followed by manual stirring. Then, ultrasonic dispersion treatment was performed with an ultrasonic disperser (UP200St manufactured by Hielscher Company, operation frequency: 26 KHz, operation output: 160 W) for 25 minutes to produce an aqueous black pigment dispersion (corresponding to a pigment concentration of 8%).

Production Examples 2 to 4: Method for Producing Ultrasonic Dispersion (US) Aqueous Cyan Pigment Dispersion

[0200] An aqueous cyan pigment dispersion was prepared by the same method as described above except that the types and amounts of the pigment used, the anionic group-containing organic polymer compound used, the bio-nanofibers used, and the colloidal silica used were changed to those described in each of examples.

[0201] Table 3 shows examples of the amount of ultrasonic dispersion (US) aqueous pigment dispersion added.

TABLE-US-00003 TABLE 3 Production of ultrasonic dispersion (US) aqueous pigment dispersion Production Production Production Production Example 1 Example 2 Example 3 Example 4 (Black) (Cyan) (Magenta) (Yellow) Pigment Product name #960 FASTOGEN FASTOGEN Fast Yellow Blue TGR Super Magenta 7413 RY (parts) 20 20 20 20 Solution of anionic group- 20 30 30 20 containing organic polymer compound (SA-1) (parts) Triethylene glycol (parts) 5 20 20 20 Pure water Balance Balance Balance Balance Sub-total (parts) 100 100 100 100 Bio- Product name CEL-NF CEL-NF CHI-NF CEL-NF nanofiber (abbreviation) (parts) 1.0 1.0 1.0 1.0 Colloidal Product name PL-3 PL-3 PL-3 PL-3 silica (abbreviation) (parts) 2.0 2.0 2.0 1.0 Pure water Balance Balance Balance Balance Total (parts) 250 250 250 250

Preparation Example 1: Ultrasonic Dispersion (US) Aqueous Black Ink (Type 1)

[0202] First, 25 parts of pure water was added to 75 parts of the aqueous pigment dispersion (corresponding to a pigment concentration of 8%) produced in Production Example 1 and stirred by using a magnetic stirrer, and then the resultant mixture was filtered with a 1.2 μm membrane filter to produce an ultrasonic dispersion (US) aqueous black ink (Type 1) of Example 1. The physical properties and the like of the prepared ink are described in tablos below.

Preparation Example 2: Ultrasonic Dispersion (US) Aqueous Black Ink (Type 2)

[0203] First, 50 parts of separately prepared vehicle (mixing ratio by mass: 2-pyrrolidone/triethylene glycol monobutyl ether/glycerin/Surfynol 440/pure water=16/16/6/1/61) was added to 50 parts of the aqueous pigment dispersion (corresponding to a pigment concentration of 8%) produced in Production Example 1 and stirred by using a magnetic stirrer, and then the resultant mixture was filtered with a 1.2 μm membrane filter to produce an ultrasonic dispersion (US) aqueous black ink (Type 2) of Example 14. The physical properties and the like of the prepared ink are described in tables below.

[0204] An ultrasonic dispersion (US) aqueous cyan ink (Type 1) was prepared according to Preparation Example 1 or the like described above except that the type of the pigment used, the type and amount of the anionic group-containing organic polymer compound used, and the type and amount of the bio-nanofibers used were changed to those described in each of examples. The physical properties and the like of the prepared ink are described in tables below.

Production Example 5: Method for Producing Kneading Method (PLM) Aqueous Black Pigment Dispersion

[0205] In a planetary mixer (ACM04LVTJ-B, manufactured by Aicohsha Manufacturing Co., Ltd.), a mixture (50 parts of carbon black “#960” (manufactured by Mitsubishi Chemical Corporation), 10 parts of anionic group-containing organic polymer compound (resin A), 4.4 parts of a 34% aqueous potassium hydroxide solution, and 50 parts of triethylene glycol) was added, and the mixture was kneaded for 60 minutes at a jacket temperature of 60° C. and a stirring blade rotational speed of 25 rpm (number of revolutions: 80 rpm). Further, the whole of the resultant kneaded product was placed in a domestic mixer (Healthy Mix manufactured by Zojirushi Corporation), and 218.6 parts of pure water was added. After the mixer was hermetically sealed, the resultant mixture was stirred and dissolved for 20 minutes to produce 333 parts of an aqueous mixture MX. In a metal beaker, 53.33 parts of the aqueous mixture MX, 0.3 parts (in terms of solid content) of bio-nanofibers “BiNFi-s 2% cellulose” (manufactured by Sugino Machine Limited, product name (abbreviation): CEL-NF), 1.0 part (in terms of solid content) of colloidal silica “Quartron PL-10H” (manufactured by Fuso Chemical Co., Ltd., product name (abbreviation): PL-10H), and pure water were added so that a total amount was 100 parts, stirred and mixed by a homogenizer (Rotor/Stator manufactured by Silverson Machines Ltd.) at 8000 rpm for 11 minutes, and further diluted with pure water to prepare a kneading method (PLM) aqueous black pigment dispersion (corresponding to a pigment concentration of 8%).

Production Examples 6 to 8: Method for Producing Kneading Method (PLM) Aqueous Cyan Pigment Dispersion

[0206] A kneading method (PLM) aqueous cyan pigment dispersion was prepared according to the production method described above except that the types and amounts of the pigment used, the anionic group-containing organic polymer compound used, the bio-nanofibers used, and the colloidal silica used were changed to those described in each of examples. Table 4 shows examples of the amount of kneading method (PLM) aqueous pigment dispersion added.

TABLE-US-00004 TABLE 4 Production of kneading method (PLM) aqueous pigment dispersion Production Production Production Production Example 5 Example 6 Example 7 Example 8 (Black) (Cyan) (Magenta) (Yellow) Pigment Product name #960 FASTOGEN FASTOGEN Fast Yellow Blue TGR Super Magenta 7413 RY (parts) 50 50 50 50 Anionic group-containing 10 15 10 15 organic polymer compound Resin A (parts) 34% aqueous potassium 4.4 6.6 4.4 6.6 hydroxide solution Triethylene glycol (parts) 50 18.75 33.5 27.5 Pure water Balance Balance Balance Balance Aqueous mixture MX (parts) 333 333 333 333 ↓ ↓ ↓ ↓ Aqueous mixture MX (parts) 53.33 53.33 53.33 53.33 Bio-nanofiber Product name CEL-NF CHI-NF CEL-KY CHI-NF (abbreviation) (parts) 0.3 0.3 0.2 0.3 Colloidal silica Product name PL-10H PL-3 PL-7 PL-3 (abbreviation) (parts) 1.0 1.0 0.4 0.8 Anionic group- Product name — DN-800H — — containing (parts) — 0.4 — — organic polymer compound Pure water Balance Balance Balance Balance Total (parts) 100 100 100 100

Preparation Example 3: Kneading Method (PLM) Aqueous Black Ink (Type 1)

[0207] First, 12.5 parts of pure water was added to 37.5 parts of the aqueous pigment dispersion (corresponding to a pigment concentration of 8%) produced by the method of Production Example 5 and stirred by using a magnetic stirrer, and then the resultant mixture was filtered with a 1.2 μm membrane filter to produce a kneading method (PLM) aqueous black ink (Type 1) of Example 11. The physical properties and the like of the prepared ink are described in tables below.

Preparation Example 4: Kneading Method (PLM) Aqueous Black Ink (Type 2)

[0208] First, 25 parts of separately prepared vehicle (mixing ratio by mass: 2-pyrrolidone/triethylene glycol monobutyl ether/glycerin/Surfynol 440/pure water=16/16/6/1/61) was added to 25 parts of the aqueous pigment dispersion (corresponding to a pigment concentration of 8%) produced by the method of Production Example 5 and stirred by using a magnetic stirrer, and then the resultant mixture was filtered with a 1.2 μm membrane filter to produce a kneading method (PLM) aqueous black ink (Type 2) of Example 47. The physical properties and the like of the prepared ink are described in tables below.

[0209] A kneading method (PLM) aqueous cyan ink (Type 1) or the like was prepared according to Preparation Example 3 or the like described above except that the type of the pigment used, the type and amount of the anionic group-containing organic polymer compound used, and the type and amount of the bio-nanofibers used were changed to those described in each of examples. The physical properties and the like of the prepared ink are described in tables below.

(pH Measurement Method)

[0210] Measurement (ink temperature of 25° C.) was performed by using MM-60R (manufactured by DKK-TOA Corporation).

(Viscosity Measurement Method)

[0211] Measurement (ink temperature of 25° C.) was performed by using Viscometer TV-20 (manufactured by Toki Sangyo Co., Ltd.).

(Measurement Method for Average Particle Diameter)

[0212] Measurement (ink temperature of 25° C.) was performed by using a dynamic light scattering Nanotrac particle size analyzer UPA-150EX (manufactured by Nikkiso Co., Ltd.). A volume-based (Mv) median diameter (D.sub.50) was used as an average particle diameter.

(Measurement of Optical Density (O.D.) Value)

[0213] The prepared ink was applied to PPC paper by using wire bar #3. After natural drying for 24 hours, the optical density (O.D.) of a coated product was measured. Measurement was performed by using “Gretag Macbeth Spectro Scan Transmission” (United States X-Rite Inc.), and an average value obtained by measurement of a total 9 points of a 3 by 3 matrix was used as the optical density (O.D.) value of the coated product.

[0214] In addition, with respect to improvement in the optical density, the optical density (O.D.) was calculated by a formula below and evaluated based on evaluation criteria below.

(Optical density (O.D.) of sample ink)/(Optical density (O.D.) of reference ink)×100(%) [Math. 6]

(Determination Criteria)

[0215] G: Improvement of 3% or more in optical density

[0216] N: No improvement of 3% or more in optical density

(Rubfastness Test)

[0217] The prepared ink was applied to glossy paper by using wire bar #3. After natural drying for 24 hours, the coated surface was rubbed with a 45R friction block on which PPC paper for friction was wound using a Gakushin-type rubbing tester (manufactured by Daiei Kagaku Seiki Mfg. Co., Ltd.) under the conditions including a load of 200 g and a number of times of friction of 10. Then, the state of the coated surface was visually observed by three panelists and evaluated according to criteria below.

[0218] G: Three panelists evaluated that no damage occurred

[0219] N: One or more panelists evaluated that damage occurred

(Marker Resistance Test)

[0220] The prepared ink was applied to PPC paper by using wire bar #3. After natural drying for 24 hours, a boundary between an ink coated surface and an uncoated surface on the coated product was traced with a commercial fluorescent pen (Text Liner manufactured by FABER-CASTELL Company). A degree of dirt was visually observed and evaluated according to criteria below (three panelists).

[0221] G: By tracing with a fluorescent pen, no staining such as trailing or the like occurred or trailing occurred at a level with no practical problem.

[0222] N: By tracing with a fluorescent pen, significant trailing occurred and heavy staining was observed.

[0223] With respect to discharge properties and printability, an ink jet recording apparatus (ENVY4500 manufactured by Hewlett-Packard Company) having a thermal-type ink jet nozzle was filled with an aqueous ink in a constant-temperature constant-humidity chamber (room temperature 25° C., humidity 50%). Then, printing was continuously performed for 10 minutes on PPC paper as a recording material using a test print pattern (having a character part, a ruled-line part, and a solid part). After continuous printing for 10 minutes, the paper surface was visually observed by three panelists and omission or blurring of the print pattern was evaluated according to criteria below.

[0224] G: Neither omission nor blurring in the print pattern was recognized by the three panelists.

[0225] M: Omission or blurring in the print pattern was recognized by only one panelist (neither omission nor blurring in the print pattern was recognized by the other two panelists).

[0226] N: Omission or blurring in the print pattern was recognized by two or more panelists.

[0227] The ink compositions and the ink evaluation results are shown in tables below.

TABLE-US-00005 TABLE 5 Production Example 1 US Example Example Example Example Example Example Aqueous black ink (Type 1) dispersion 1 2 3 4 5 6 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Composition Black pigment Product name #960 #960 #960 #960 #960 #960 #960 (1) (parts) (solid content) 8 6 6 6 6 6 6 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing (parts) (solid content) 1.6 1.2 1.2 1.2 1.2 1.2 1.2 organic polymer Name/Product name — — — — DN-800H DN-100L CMC1390 compound (parts) (solid content) — — — — 0.15 0.15 0.1 Bio- Product name CEL-NF CEL-NF CEL-KY CEL-NF CEL-NF CEL-NF CEL-NF nanofiber (2) (abbreviation) (parts) 0.4 0.3 0.15 0.3 0.3 0.225 0.225 Colloidal Product name PL-3 PL-3 PL-7 PL-10H PL-1 PL-3 PL-7 silica (abbreviation) (3) (parts) 0.8 0.6 0.45 0.75 0.15 0.75 0.45 Triethylene glycol (parts) 2 1.5 1.5 1.5 1.5 1.5 1.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.10 0.10 0.08 0.13 0.03 0.13 0.08 (3)/(2) (solid content ratio) 2.00 2.00 3.00 2.50 0.50 3.33. 2.00 (2)/(1) (solid content ratio) 0.05 0.05 0.03 0.05 0.05 0.04 0.04 Physical pH 10.4 9.7 9.8 9.7 9.8 9.9 9.9 properties Average particle diameter D50/nm 101 89 83 88 88 87 86 Initial viscosity (mPa .Math. s) — 3.5 7.9 9.1 4.3 5.0 4.1 Optical Measured value — 1.42 1.41 1.49 1.44 1.44 1.40 density Improvement rate — 106% 105% 111% 107% 107% 104% Determination — G G G G G G Rubfastness — G G G G G G

TABLE-US-00006 TABLE 6 Comparative Comparative Example Example Example Example Example Example Example Aqueous black ink (Type 1) 7 8 9 10 11 1 2 Dispersion method (US: ultrasonic US US US US US US US dispersion method PLM: kneading method) Composition Black Product name #960 #960 #960 #960 #960 #960 #960 pigment (1) (parts) (solid content) 6 6 6 6 6 6 6 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing organic (parts) (solid content) 1.2 1.2 1.2 1.2 1.2 1.2 1.2 polymer compound Name/Product name DN-10L CMC1390 DN-800H — DN-100L — — (parts) (solid content) 0.15 0.3 0.15 — 0.15 — — Bio- Product name CEL-NF CEL-KY CEL-KY CHI-NF CHI-NF CEL-NF CHI-NF nanofiber (2) (abbreviation) (parts) 0.15 0.3 0.3 0.3 0.45 0.6 0.6 Colloidal Product name PL-3L PL-7 PL-3 PL-3 PL-10H — — silica (3) (abbreviation) (parts) 0.75 0.75 0.75 0.6 0.75 — — Triethylene glycol (parts) 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.13 0.13 0.10 0.13 — — (3)/(2) (solid content ratio) 5.00 2.50 2.50 2.00 1.67 — — (2)/(1) (solid content ratio) 0.03 0.05 0.05 0.05 0.08 0.10 0.10 Physical pH 9.8 9.7 9.7 9.7 9.9 9.8 9.8 properties Average panicle diameter D50/nm 87 84 85 87 90 79 78 Initial viscosity (mPa .Math. s) 7.6 12.3 10.8 6.2 12.8 99 or more 99 or more Optical density Measured value 1.46 1.45 1.44 1.46 1.52 1.57 1.57 Improvement rate 109% 108% 107% 109% 113% 117% 117% Determination G G G G G G G Rubfastness G G G G G G G

TABLE-US-00007 TABLE 7 Comparative Comparative Example Example Example Example Example Example Example Aqueous black ink (Type 1) 3 4 12 13 14 15 16 Dispersion method (US: ultrasonic US US US US US US US dispersion method PLM: kneading method) Composition Black pigment Product name #960 #960 #960 #960 #960 #960 #960 (1) (parts) (solid content) 6 6 6 6 6 6 6 Anionic group- Name/Product name SA-1 SA-1 UR-1 UR-1 UR-1 UR-1 UR-1 containing (parts) (solid content) 1.2 1.2 1.2 1.2 1.2 1.2 1.2 organic Name/Product name — — — — — — CMC1390 polymer (parts) (solid content) — — — — — — 0.2 compound Bio-nanofiber Product name CEL-NF CEL-NF CEL-KY CEL-KY CEL-KY (2) (abbreviation) (parts) — — 0.075 0.75 0.3 0.075 0.3 Colloidal Product name PL-10H — PL-10H PL-3L PL-3 PL-3L PL-7 silica (abbreviation) (3) (parts) 0.75 — 0.3 0.75 0.45 0.6 0.3 Triethylene glycol (parts) 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)41) (solid content ratio) 0.13 — 0.05 0.13 0.08 0.10 0.05 (3)1(2) (solid content ratio) — — 4.00 1.00 1.50 8.00 1.00 (2)/(1) (solid content ratio) — — 0.01 0.13 0.05 0.01 0.05 Physical pH 9.8 10.3 8.2 8.2 7.9 7.9 7.8 properties Average particle diameter D50/nm 88 81 132 133 120 128 131 Initial viscosity (mPa .Math. s) 2.1 1.7 3.7 35.8 15.6 4.6 3.2 Optical Measured value 0.97 1.34 1.41 1.55 1.47 1.41 1.50 density Improvement rate 72% 100% 106% 117% 110% 106% 113% Determination N (Reference) G G G G G Rubfastness N N G G G G G

TABLE-US-00008 TABLE 8 Comparative Comparative Example Example Example Example Example Aqueous black ink (Type 1) 17 18 19 5 6 Dispersion method (US: ultrasonic dispersion US US US US US method PLM: kneading method) Composition Black pigment Product name #960 #960 #960 #960 #960 (1) (parts) (solid content) 6 6 6 6 6 Anionic group- Name/Product name UR-1 UR-1 UR-1 UR-1 UR-1 containing (parts) (solid content) 1.2 1.2 1.2 1.2 1.2 organic polymer Name/Product name DN-800H DN-10L DN-100L — — compound (parts) (solid content) 0.15 0.15 0.3 — — Bio-nanofiber Product name CEL-NF CHI-NF CHI-NF — CEL-NF (2) (abbreviation) (parts) 0.15 0.225 0.3 — 0.6 Colloidal silica (3) Product name PL-3 PL-7 PL-10H — — (abbreviation) (parts) 0.75 0.75 0.75 — — Triethylene glycol (parts) 1.5 1.5 1.5 1.5 1.5 Pure water Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.13 0.13 — — (3)/(2) (solid content ratio) 5.00 3.33 2.50 — — (2)/(1) (solid content ratio) 0.03 0.04 0.05 — 0.10 Physical pH 8.3 8.3 8.3 8.9 8.4 properties Average particle diameter D50/nm 130 130 130 125 137 Initial viscosity (mPa .Math. s) 5.3 4.2 8.4 2.1 99 or more Optical density Measured value 1.50 1.45 1.54 1.33 1.53 Improvement rate 113% 109% 116% 100% 115% Determination G G G (Reference) G Rubfastness G G G N G

TABLE-US-00009 TABLE 9 Production Example 5 PLM Example Example Example Example Example Example Aqueous black ink (Type 1) dispersion 20 21 22 23 24 25 Dispersion method (US: ultrasonic PLM PLM PLM PLM PLM PLM PLM dispersion method PLM: kneading method) Composition Black Product name #960 #960 #960 #960 #960 #960 #960 pigment (1) (parts) (solid content) 8 6 6 6 6 6 6 Anionic group- Name/Product name SA-1 SA-1 Resin A Resin A Resin A Resin A Resin A containing (parts) (solid content) 1.6 1.2 1.2 1.2 1.2 1.2 12 organic Name/Product name — — — — — DN-800H DN-800H polymer compound (parts) (solid content) — — — — — 0.2 0.1 Bio-nanofiber (2) Product name CEL-NF CEL-NF CEL-KY CEL-KY CEL-KY CEL-KY CEL-NF (abbreviation) (parts) 0.3 0.225 0.3 0.075 0.6 0.3 0.45 Colloidal Product name PL-10H PL-10H PL-3 PL-101-1 PL-3L PL-3 PL-3L silica (3) (abbreviation) (parts) 1.0 0.75 0.75 0.75 0.75 0.3 1.0 Triethylene glycol (parts) 8 6 6 6 6 6 6 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.13 0.13 0.13 0.13 0.05 0.17 (3)/(2) (solid content ratio) 3.33 3.33 2.50 10.00 125 1.00 2.22 (2)/(1) (solid content ratio) 0.04 0.04 0.05 0.01 0.10 0.05 0.08 Physical pH 10.1 9.5 10.0 9.9 10.0 9.8 9.9 properties Average particle diameter D50/nm 102 88 95 96 94 94 88 Initial viscosity (mPa .Math. s) — 18.2 6.6 2.9 26.4 5.3 5.4 Optical density Measured value — 1.32 1.28 1.25 1.39 1.27 1.35 Improvement rate — 111% 107% 105% 117% 106% 114% Determination — G G G G G G Rubfastness — G G G G G G

TABLE-US-00010 TABLE 10 Comparative Comparative Example Example Example Example Aqueous black ink (Type 1) 26 27 7 8 Dispersion method (US: ultrasonic dispersion PLM PLM PLM PLM method PLM: kneading method) Composition Black pigment (1) Product name #960 #960 #960 #960 (parts) (solid content) 6 6 6 6 Anionic group- Name/Product name Resin A Resin A Resin A Resin A containing organic (parts) (solid content) 1.2 1.2 1.2 1.2 polymer compound Name/Product name DN-100L CMC1390 — — (parts) (solid content) 0.15 0.1 — — Bio- Product name CEL-NF CHI-NF CEL-NF — nanofiber (2) (abbreviation) (parts) 0.4 0.15 0.6 — Colloidal Product name PL-3 PL-3 — — silica (3) (abbreviation) (parts) 0.75 0.75 — — Triethylene glycol (parts) 6 6 6 6 Pure water Balance Balance Balance Balance Total (parts) 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.13 — — (3)/(2) (solid content ratio) 1.88 5.00 — — (2)/(1) (solid content ratio) 0.07 0.03 0.10 — Physical pH 9.9 9.9 10.0 10.1 properties Average particle diameter D50/nm 89 84 98 116 Initial viscosity (mPa .Math. s) 5.0 12.4 99 or more 1.9 Optical Measured value 1.29 1.26 1.46 1.19 density Improvement rate 109% 106% 122% 100% Determination G G G (Reference) Rubfastness G G N N

TABLE-US-00011 TABLE 11 Production Example 1 US Example Example Example Example Example Example Aqueous black ink (Type 2) dispersion 28 29 30 31 32 33 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Black pigment (1) Product name #960 #960 #960 #960 #960 #960 #960 sition (parts) (solid content) 8 4 4 4 4 4 4 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing organic (parts) (solid content) 1.6 0.8 0.8 0.8 0.8 0.8 0.8 polymer compound Name/Product name — — — — — DN-800H DN-100L (parts) (solid content) — — — — — 0.15 0.15 Bio- Product name CEL-NF CEL-NF CEL-KY CEL-KY CEL-NF CEL-NF CEL-NF nanofiber (abbreviation) (2) (parts) 0.4 0.2 0.2 0.1 0.2 0.15 0.15 Colloidal Product name PL-3 PL-3 PL-3 PL-7 PL-10H PL-1 PL-3 silica (3) (abbreviation) (parts) 0.8 0.4 0.4 0.3 0.5 0.3 0.5 2-Pyrrolidone (parts) — 8 8 8 8 8 8 Triethylene glycol monobutyl — 8 8 8 8 8 8 ether (parts) Glycerin (parts) — 3 3 3 3 3 3 Triethylene glycol (parts) 2 1 1 1 1 1 1 Surfynol 440 (parts) — 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.10 0.10 0.10 0.08 0.13 0.08 0.13 (3)/(2) (solid content ratio) 2.00 2.00 2.00 3.00 2.50 2.00 3.33 (2)/(1) (solid content ratio) 0.05 0.05 0.05 0.03 0.05 0.04 0.04 Physical pH 10.4 9.2 9.3 9.3 9.2 9.4 9.5 properties Average particle diameter D50/nm 101 88 82 82 88 89 86 Initial viscosity (mPa .Math. s) — 3.8 16.8 8.8 10.1 4.8 5.5 Optical density Measured value — 1.06 1.07 1.05 1.11 1.07 1.07 Improvement rate — 107% 108% 106% 112% 108% 108% Determination — G G G G G G Rubfastness — G G G G G G Marker resistance — G G G G G G Ink jet adaptability — G G G G G G

TABLE-US-00012 TABLE 12 Example Example Example Example Example Example Example Aqueous black ink (Type 2) 34 35 36 37 38 39 40 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Black Product name #960 #960 #960 #960 #960 #960 #960 sition pigment (1) (parts) (solid content) 4 4 4 4 4 4 4 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing organic (parts) (solid content) 0.8 0.8 0.8 0.8 0.8 0.8 0.8 polymer compound Name/Product name CMC1390 DN-10L DN-100L CMC1390 DN-800H — DN-800H (parts) (solid content) 0.1 0.15 0.2 0.2 0.2 — 0.3 Bio- Product name CEL-NF CEL-NF CEL-NF CEL-KY CEL-KY CHI-NF CHI-NF nanofibers (2) (abbreviation) (parts) 0.15 0.1 0.1 0.2 0.2 0.2 0.15 Colloidal Product name PL-7 PL-3L PL-3 PL-7 PL-3 PL-3 PL-3L silica (3) (abbreviation) (parts) 0.3 0.5 0.5 0.5 0.5 0.4 0.2 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol monobutyl 8 8 8 8 8 8 8 ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 1 1 1 1 1 1 1 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.08 0.13 0.13 0.13 0.13 0.10 0.05 (3)/(2) (solid content ratio) 2.00 5.00 5.00 2.50 2.50 2.00 1.33 (2)/(1) (solid content ratio) 0.04 0.03 0.03 0.05 0.05 0.05 0.04 Physical pH 9.4 9.2 9.2 9.2 9.1 9.2 7.8 properties Average particle diameter D50/nm 85 88 91 84 83 88 132 Initial viscosity (mPa .Math. s) 4.6 8.4 5.7 13.7 12.0 6.9 4.8 Optical Measured value 1.04 1.09 1.07 1.08 1.07 1.09 1.05 density Improvement rate 105% 110% 108% 109% 108% 110% 106% Determination G G G G G G G Rubfastness G G G G G G G Marker resistance G G G G G G G Ink jet adaptability G G G G G 0 G

TABLE-US-00013 TABLE 13 Compar- Compar- Compar- Compar- ative ative ative ative Example Example Example Example Example Example Example Aqueous black ink (Type 2) 41 9 10 11 12 42 43 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Black Product name #960 #960 #960 #960 #960 #960 #960 sition pigment (1) (parts) (solid content) 4 4 4 4 4 4 4 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 UR-1 UR-1 containing organic (parts) (solid content) 0.8 0.8 0.8 0.8 0.8 0.8 0.8 polymer Nam&Product name DN-100L — — — — — — compound (parts) (solid content) 0.15 — — — — — — Bio-nano- Product name CHI-NF CEL-NF CHI-NF CEL-NF CEL-NF fibers (2) (abbreviation) (parts) 0.3 0.4 0.4 — — 0.05 0.15 Colloidal Product name PL-10H — — PL-10H — PL-10H PL-3L silica (3) (abbreviation) (parts) 0.5 — — 0.5 — 0.2 0.5 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol monobutyl 8 8 8 8 8 8 8 ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 1 1 1 1 1 1 1 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 — — 0.13 — 0.05 0.13 (3)/(2) (solid content ratio) 1.67 — — — 4.00 3.33 — (2)/(1) (solid content ratio) 0.08 0.10 0.10 — — 0.01 0.04 Physical pH 9.4 9.3 9.3 9.3 9.3 7.8 7.8 properties Average particle diameter D50/nm 89 78 78 88 88 132 132 Intial viscosity (mPa .Math. s) 14.2 99 or more 99 or more 2.3 2.3 4.1 9.8 Optical Measured value 1.13 1.17 1.17 0.97 0.99 0.99 1.02 density Improvement rate 114% 118% 118% 98% 100% 105% 109% Determination G G G N (Reference) G G Rubfastness G G G N N G G Marker resistance M N N G G G G Ink jet adaptability G N N G G G G

TABLE-US-00014 TABLE 14 Example Example Example Example Example Example Example Aqueous black ink (Type2) 44 45 46 47 48 49 50 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Black pigment (1) Product name #960 #960 #960 #960 #960 #960 #960 sition (parts) (solid content) 4 4 4 4 4 4 4 Anionic group- Name/Product name UR-1 UR-1 UR-1 UR-1 UR-1 UR-1 UR-1 containing (parts) (solid content) 0.8 0.8 0.8 0.8 0.8 0.8 0.8 organic polymer Name/Product name — — CMC1390 DN-800H DN-100L DN-10L CMC1390 compound (parts) (solid content) — — 0.2 0.15 0.15 0.15 0.1 Bio-nano- Product name CEL-KY CEL-KY CEL-KY CEL-NF CEL-NF CHI-NF CHI-NF fibers (2) (abbreviation) (parts) 0.2 0.05 0.2 0.15 0.15 0.15 0.2 Colloidal Product name PL-3 PL-3L PL-7 PL-3 PL-3L PL-7 PL-10H silica (3) (abbreviation) (parts) 0.3 0.4 0.2 0.5 0.5 0.5 0.5 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol monobutyl 8 8 8 8 8 8 8 ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 1 1 1 1 1 1 1 Surfynol 440 (parts) 0.6 0.5 0.5 0.5 0.6 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.08 0.10 0.05 0.13 0.13 0.13 0.13 (3)/(2) (solid content ratio) 1.50 8.00 1.00 3.33 3.33 3.33 2.50 (2)/(1) (solid content ratio) 0.05 0.01 0.05 0.04 0.04 0.04 0.05 Physical pH 7.5 7.5 7.4 7.9 7.8 7.9 7.9 properties Average particle diameter D60/nm 119 128 130 132 133 130 131 Initial viscosity (mPa .Math. s) 17.3 5.1 3.6 5.9 5.6 4.7 11.1 Optical Measured value 1.03 0.99 1.06 1.05 1.06 1.02 1.07 density Improvement rate 110% 105% 112% 112% 113% 109% 114% Determination G G G G G G G Rubfastness G G G G G G G Marker resistance G G G G G G G Ink jet adaptability G G G G G G M

TABLE-US-00015 TABLE 15 Compar- Compar- Production ative ative Example 5 Example Example Example PLM Example Example Example Aqueous black ink (Type 2) 51 13 14 dispersion 52 53 54 Dispersion method (US: ultrasonic US US US PLM PLM PLM PLM dispersion method PLM: kneading method) Compo- Black pigment (1) Product name #960 #960 #960 #960 #960 #960 #960 sition (parts) (solid content) 4 4 4 8 4 4 4 Anionic group- Name/Product name UR-1 UR-1 UR-1 SA-1 SA-1 Resin A Resin A containing organic (parts) (solid content) 0.8 0.8 0.8 1.6 0.8 0.8 0.8 polymer compound Name/Product name DN-100L — — — — — — (parts) (solid content) 0.3 — — — — — — Bio-nano- Product name CHI-NF — CEL-NF CEL-NF CEL-NF CEL-KY CEL-KY fibers (2) (abbreviation) (parts) 0.2 — 0.4 0.3 0.15 0.2 0.05 Colloidal Product name PL-10H — — PL-10H PL-10H PL-3 PL-10H silica (3) (abbreviation) (parts) 0.5 — — 1 0.5 0.5 0.5 2-Pyrrolidone (parts) 8 8 8 — 8 8 8 Triethylene glycol monobutyl 8 8 8 — 8 8 8 ether (parts) Glycerin (parts) 3 3 3 — 3 3 3 Triethylene glycol (parts) 1 1 1 8 4 4 4 Surfynol 440 (parts) 0.5 0.5 0.5 — 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 — — 0.13 0.13 0.13 0.13 (3)/(2) (solid content ratio) 2.50 — — 3.33 3.33 2.50 10.00 (2)/(1) (solid content ratio) 0.05 — 0.10 — 0.04 0.05 0.01 Physical pH 7.9 7.8 8.0 10.4 9.0 9.5 9.4 properties Average particle diameter D50/nm 131 133 138 101 87 96 97 Initial viscosity (mPa .Math. s) 9.3 2.3 99 or more — 20.2 7.3 3.2 Optical Measured value 1.08 0.94 1.07 — 1.04 1.01 0.99 density Improvement rate 115% 100% 114% — 111% 107% 105% Determination G (Reference) G — G G G Rubfastness G N G — G G G Marker resistance G G N — G G G Ink jet adaptability G G N — G G G

TABLE-US-00016 TABLE 16 Example Example Example Example Example Example Example Aqueous black ink (Type 2) 55 56 57 58 59 60 61 Dispersion method (US: ultrasonic dispersion PLM PLM PLM PLM PLM PLM PLM method PLM: kneading method) Compo- Black pigment (1) Product name #960 #960 #960 #960 #960 #960 #960 sition (parts) (solid content) 4 4 4 4 4 4 4 Anionic group- Name/Product name Resin A Resin A Resin A Resin A Resin A Resin A Resin A containing (parts) (solid content) 0.8 0.8 0.8 0.8 0.8 0.8 0.8 organic polymer Name/Product name — CMC1390 DN-800H DN-800H DN-100L DN-10L CMC1390 compound (parts) (solid content) — 0.2 0.2 0.15 0.15 0.15 0.1 Bio-nano- Product name CEL-KY CEL-KY CEL-KY CEL-NF CEL-NF CHI-NF CHI-NF fibers (2) (abbreviation) 0.4 0.2 0.2 0.15 0.15 0.15 0.15 (parts) Colloidal Product name PL-3L PL-7 PL-3 PL-3L PL-3 PL-10H PL-3 silica (3) (abbreviation) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 (parts) 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol monobutyl 8 8 8 8 8 8 8 ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 4 4 4 4 4 4 4 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.13 0.13 0.13 0.13 0.13 0.13 (3)/(2) (solid content ratio) 1.25 2.50 2.50 3.33 3.33 3.33 3.33 (2)/(1) (solid content ratio) 0.10 0.05 0.05 0.04 0.04 0.04 0.04 Physical pH 9.5 9.4 9.3 9.4 9.4 9.5 9.4 properties Average particle diameter D50/nm 93 94 95 89 89 87 85 Initial viscosity (mPa .Math. s) 29.3 6.9 5.9 6.0 5.6 4.7 13.8 Optical Measured value 1.10 1.01 1.00 1.07 1.02 1.00 1.05 density Improvement rate 117% 107% 106% 114% 109% 106% 112% Determination G G G G G G G Rubfastness G G G G G G G Marker resistance G G G G G G G Ink jet adaptability M G G G G G M

TABLE-US-00017 TABLE 17 Comparative Comparative Example Example Aqueous black ink (Type 2) 15 16 Dispersion method (US: ultrasonic dispersion method PLM PLM PLM: kneading method) Composition Black pigment (1) Product name #960 #960 (parts) (solid content) 4 4 Anionic group- Name/Product name Resin A Resin A containing organic (parts) (solid content) 0.8 0.8 polymer Name/Product name — — compound (parts) (solid content) — — Bio-nanofibers (2) Product name CEL-NF — (abbreviation) (parts) 0.4 — Colloidal silica (3) Product name — — (abbreviation) — — (Parts) 2-Pyrrolidone (parts) 8 8 Triethylene glycol monobutyl ether (parts) 8 8 Glycerin (parts) 3 3 Triethylene glycol (parts) 4 4 Surfynol 440(parts) 0.5 0.5 Pure water Balance Balance Total (parts) 100 100 (3)/(1) (solid content ratio) — — (3)/(2) (solid content ratio) — — (2)/(1) (solid content ratio) 0.10 — Physical pH 9.5 9.5 properties Average particle diameter D50/nm 97 97 Initial viscosity (mPa .Math. s) 99 or more 2.8 Optical density Measured value 1.15 0.94 Improvement rate 122% 100% Determination G (Reference) Rubfastness N N Marker resistance N G Ink jet adaptability N G

TABLE-US-00018 TABLE 18 Production Example 2 US Example Example Example Example Example Example Aqueous cyan ink (Type 1) dispersion 62 63 64 65 66 67 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment (1) name Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR (parts) 8 6 6 6 6 6 6 (solid content) Anionic Name/ SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 group- Product name containing (parts) 2.4 1.8 1.8 1.8 1.8 1.8 1.8 organic (solid content) polymer Name/ — — — — CMC1390 DN-800H DN-10L compound Product name (parts) — — — — 0.2 0.15 0.15 (solid content) Bio-nano- Product name CEL-NF CEL-NF CEL-NF CEL-KY CEL-KY CEL-NF CEL-NF fibers (2) (abbreviation) (parts) 0.4 0.3 0.3 0.1 0.2 0.15 0.15 Colloidal Product name PL-3 PL-3 PL-10H PL-3 PL-10H PL-1 PL-3 slice (3) (abbreviation) (parts) 0.8 0.6 0.2 0.3 0.225 0.3 0.75 Triethylene glycol (parts) 8 6 6 6 6 6 6 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.10 0.10 0.03 0.05 0.04 0.05 0.13 (3)/(2) (solid content ratio) 2.00 2.00 0.67 3.00 1.13 2.00 5.00 (2)/(1) (solid content ratio) 0.05 0.05 0.05 0.02 0.03 0.03 0.03 Physical pH 9.8 9.2 9.2 9.5 9.3 9.7 9.8 properties Average particle 99 94 95 96 97 92 93 diameter D50/nm Initial viscosity (mPa .Math. s) — 4.1 8.9 4.7 7.8 7.1 7.1 Optical Measured value — 1.23 1.28 1.21 1.26 1.26 1.23 density Improvement rate — 105% 109% 103% 107% 107% 105% Determination — G G G G G G Rubfastness — G G G G G G

TABLE-US-00019 TABLE 19 Compar- Compar- ative ative Example Example Example Example Example Example Example Aqueous cyan ink (Type 1) 68 69 70 17 18 71 72 Dispersion method (US: ultrasonic US US US US US US US dispersion method PLM: kneading method) Compo- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment name Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR (1) (parts) 6 6 6 6 6 6 6 (solid content) Anionic- Name/Product SA-1 SA-1 SA-1 SA-1 SA-1 UR-1 UR-1 group name containing (parts) 1.8 1.8 1.8 1.8 1.8 1.8 1.8 organic (solid content) polymer Name/Product DN-100L CMC1390 DN-100L — — — — compound name (parts) (solid content) 0.2 0.1 0.1 — — — — Bio-nano- Product name CEL-NF CHI-NF CHI-NF — — CEL-NF CEL-KY fibers (2) (abbreviation) (parts) 0.1 0.15 0.45 — — 0.6 0.15 Colloidal Product name PL-10H PL-3L PL-10H PL-10H — PL-3 PL-7 silica (3) (abbreviation) (parts) 0.3 0.5 0.6 0.5 — 0.3 0.225 Triethylene glycol (parts) 6 6 6 6 6 6 6 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.05 0.08 0.10 0.08 — 0.05 0.04 (3)/(2) (solid content ratio) 3.00 3.33 1.33 — — 0.50 1.50 (2)/(1) (solid content ratio) 0.02 0.03 0.08 — — 0.10 0.03 Physical pH 9.5 9.5 9.5 9.5 9.6 8.7 8.7 properties Average particle 95 95 95 93 91 122 101 diameter D50/nm Initial viscosity (mPa .Math. s) 7.5 8.7 10.5 2.0 1.8 6.9 8.1 Optical Measured value 1.27 1.26 1.28 1.02 1.17 1.22 1.19 density Improvement rate 108% 107% 109% 87% 100% 109% 106% Determination G G G N (Reference) G G Rubfastness G G G N N G G

TABLE-US-00020 TABLE 20 Compar- Compar- Production ative ative Example 6 Example Example Example Example Example PLM Example Aqueous cyan ink (Type 1) 73 74 75 19 20 dispersion 76 Dispersion method (US: US US US US US PLM PLM ultrasonic dispersion method PLM: kneading method) Compo- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment (1) name Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR (parts) 6 6 6 6 6 8 6 (solid content) Anionic Name/ UR-1 UR-1 UR-1 UR-1 UR-1 Resin A Resin A group- Product name containing (parts) 1.8 1.8 1.8 1.8 1.8 2.4 1.8 organic (solid content) polymer Name/Product name DN-800H DN-10L CMC1390 — — DN-800H ON-800H compound (parts) 0.15 0.09 0.1 — — 0.4 0.3 (solid content) Bio-nano- Product name CEL-NF CEL-NF CHI-NF CEL-NF — CHI-NF CEL-NF fibers (2) (abbreviation) (parts) 0.15 0.45 0.15 0.4 — 0.3 0.225 Colloidal Product name PL-10H PL-3L PL-10H — — PL-3 PL-3 silica (3) (abbreviation) (parts) 0.3 0.75 0.45 — — 1.0 0.75 Triethylene glycol (parts) 6 6 6 6 6 3 2.25 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.05 0.13 0.08 — — 0.13 0.13 (3)/(2) (solid content ratio) 2.00 1.67 3.00 — — 3.33 3.33 (2)/(1) (solid content ratio) 0.03 0.08 0.03 0.07 — 0.04 0.04 Physical pH 8.6 8.8 8.7 8.7 8.3 9.9 9.7 properties Average particle 127 121 122 118 118 95 92 diameter D50/nm Initial viscosity (mPa .Math. s) 16.8 11.1 5.2 99 or more 8.7 — 8.9 Optical Measured value 1.25 1.24 1.19 1.32 1.12 — 1.24 density Improvement rate 112% 111% 106% 118% 100% — 107% Determination G G G G (Reference) — G Rubfastness G G G G N — G

TABLE-US-00021 TABLE 21 Example Example Example Example Example Example Aqueous cyan ink (Type 1) 77 78 79 80 81 82 Dispersion method (US: ultrasonic PLM PLM PLM PLM PLM PLM dispersion method PLM kneading method) Compo- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment name Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR (1) (parts) 6 6 6 6 6 6 (solid content) Anionic Name/Product name Resin A Resin A Resin A Resin A Resin A Resin AA group- (parts) 1.8 1.8 1.8 1.8 1.8 1.8 containing (solid content) organic Name/Product DN-100L DN-100L — — DN-800H CMC1390 polymer name compound (parts) 0.15 0.15 — — 0.2 0.1 (solid content) Bio-nano- Product name CEL-NF CHI-NF CEL-KY CEL-KY CEL-KY CEL-KY fibers (2) (abbreviation) (parts) 0.15 0.3 0.2 0.09 0.2 0.1 Colloidal Product name PL-10H PL-10H PL-3 PL-10H PL-3L PL-3 silica (3) (abbreviation) (parts) 0.3 0.5 1.0 0.3 0.5 0.75 Triethyne glycol (parts) 2.25 2.25 2.25 2.25 2.25 2.25 Pure water Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.05 0.08 0.17 0.05 0.08 0.13 (3)/(2) (solid content ratio) 2.00 1.67 5.00 3.33 2.50 7.50 (2)/(1) (solid content ratio) 0.03 0.05 0.03 0.02 0.03 0.02 Physical pH 9.8 9.2 9.8 9.8 9.6 9.6 properties Average particle 93 96 92 92 93 93 diameter D50/nm Initial viscosity (mPa .Math. s) 7.0 14.5 6.0 3.5 23.0 13.4 Optical Measured value 1.23 1.26 1.21 1.20 1.21 1.21 density Improvement rate 106% 108% 104% 103% 104% 104% Determination G G G G G G Rubfastness G G G G G G

TABLE-US-00022 TABLE 22 Comparative Comparative Example Example Aqueous cyan ink (Type1) 21 22 Dispersion method (US: ultrasonic dispersion PLM PLM method PLM: kneading method) Composition Cyan pigment Product name FASTOGEN Blue FASTOGEN Blue (1) TGR TGR (parts) (solid content) 6 6 Anionic group- Name/Product name Resin A Resin A containing (parts) (solid content) 1.8 1.8 organic Name/Product name — — polymer (parts) (solid content) — — compound Bio-nanofibers Product name CEL-NF — (2) (abbreviation) (parts) 0.6 — Colloidal silica Product name — — (3) (abbreviation) (parts) — — Triethylene glycol (parts) 2.25 2.25 Pure water Balance Balance Total (parts) 100 100 (3)/(1) (solid content ratio) — — (3)/(2) (solid content ratio) — — (2)/(1) (solid content ratio) 0.10 — Physical pH 9.8 9.9 properties Average particle diameter D50/nm 91 89 Initial viscosity (mPa .Math. s) 99 or more 1.5 Optical density Measured value 1.37 1.16 Improvement rate 118% 100% Determination G (Reference) Rubfastness G N

TABLE-US-00023 TABLE 23 Production Example 2 US Example Example Example Example Example Example Aqueous cyan ink (Type 2) dispersion 83 84 85 86 87 88 Dispersion method (US: ultrasonic US US US US US US US dispersion method PLM: kneading method) Compo- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment (1) name Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR (parts) 8 4 4 4 4 4 4 (solid content) Anionic Name/ SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 group- Product name containing (parts) 2.4 1.2 1.2 1.2 1.2 1.2 1.2 organic (solid content) polymer Name/ — — — — CMC1390 DN-800H DN-800H compound Product name (parts) — — — — 0.2 0.2 0.15 (solid content) Bio-nano- Product name CEL-NF CEL-NF CEL-NF CEL-KY CEL-KY CEL-KY CEL-NF fibers (2) (abbreviation) (parts) 0.4 0.2 0.15 0.1 0.2 0.2 0.15 Colloidal Product name PL-3 PL-3 PL-10H PL-3 PL-10H PL-7 PL-1 silica (3) (abbreviation) (parts) 0.8 0.4 0.2 0.3 0.15 0.2 0.3 2-Pyrrolidone (parts) — 8 8 8 8 8 8 Triethylene glycol — 8 8 8 8 8 8 monobutyl ether (parts) Glycerin (parts) — 3 3 3 3 3 3 Triethylene glycol (parts) 8 4 4 4 4 4 4 Surfynol 440 (parts) — 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.10 0.10 0.05 0.08 0.04 0.05 0.08 (3)/(2) (solid content ratio) 2.00 2.00 1.33 3.00 0.75 1.00 2.00 (2)/(1) (solid content ratio) 0.05 0.05 0.04 0.03 0.05 0.05 0.04 Physical pH 9.8 8.8 8.8 9.0 8.9 8.9 9.2 properties Average particle diameter D50/nm 99 95 95 95 96 96 92 Initial viscosity (mPa .Math. s) — 4.5 9.8 5.1 8.8 9.7 7.9 Optical Measured value — 1.04 1.08 1.02 1.06 1.04 1.06 density Improvement rate — 107% 111% 105% 109% 107% 109% Determination — G G G G G G Rubfastness — G G G G G G Marker resistance — G G G G G G Ink jet adaptability — G G G G G G

TABLE-US-00024 TABLE 24 Compar- Compar- ative ative Example Example Example Example Example Example Example Aqueous cyan ink (Type 2) 89 90 91 92 23 24 93 Dispersion method (US: ultrasonic US US US US US US US dispersion method PLM: kneading method) Compo- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment (1) name Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR (parts) (solid 4 4 4 4 4 4 4 content) Anionic Name/Product SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 UR-1 group- name containing (parts) 1.2 1.2 1.2 1.2 1.2 1.2 1.2 organic (solid content) polymer Name/Product DN-10L DN-100L CMC1390 DN-100L — — — compound name (parts) 0.15 0.2 0.1 0.15 — — — (solid content) Bio-nano- Product name CEL-NF CEL-NF CHI-NF CHI-NF — — CEL-NF fibers (2) (abbreviation) (Parts) 0.15 0.1 0.15 0.3 — — 0.15 Colloidal Product name PL-3 PL-10H PL-3L PL-10H PL-10H — PL-3 silica (3) (abbreviation) (parts) 0.5 0.3 0.5 0.5 0.5 — 0.5 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol 8 8 8 8 8 8 8 monobutyt ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 4 4 4 4 4 4 4 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.08 0.13 0.13 0.13 0.13 (3)/(2) (solid content ratio) 3.33 3.00 3.33 1.67 — — 3.33 (2)/(1) (solid content ratio) 0.04 0.03 0.04 0.08 — — 0.04 Physical pH 9.3 9.0 9.0 9.0 9.0 9.0 8.3 properties Average particle 93 95 95 95 93 93 122 diameter D50/nm Initial viscosity (mPa .Math. s) 7.8 8.3 9.8 11.7 2.2 2.1 7.7 Optical Measured value 1.04 1.07 1.06 1.08 0.97 0.97 1.02 density Improvement rate 107% 110% 109% 111% 100% 100% 109% Determination G G G G N (Reference) G Rubfastness G G G G N N G Marker resistance G G G G G G G Ink jet adaptability G G G G G G G

TABLE-US-00025 TABLE 25 Compar- Compar- ative ative Example Example Example Example Example Example Aqueous cyan ink (Type 2) 94 95 96 97 25 26 Dispersion method (US: ultrasonic dispersion US US US US US US method PLM: kneading method) Compo- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment (1) name Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR (parts) (solid 4 4 4 4 4 4 content) Anionic Name/Product UR-1 UR-1 UR-1 UR-1 UR-1 UR-1 group- name containing (parts) 0.8 1.2 1.2 1.2 1.2 1.2 organic (solid content) polymer Name/Product name — DN-800H DN-10L CMC1390 — — compound (parts) (solid content) — 0.15 0.15 0.1 — — Bio- Product name CEL-KY CEL-NF CEL-NF CHI-NF CEL-NF — nanofibers (2) (abbreviation) (parts) 0.2 0.15 0.15 0.15 0.4 — Colloidal Product name PL-7 PL-10H PL-3L PL-10H — — silica (3) (abbreviation) (parts) 0.2 0.3 0.5 0.5 — — 2-Pyrrolidone (parts) 8 8 8 8 8 8 Triethylene glycol 8 8 8 8 8 8 monobutyl ether (parts) Glycerin (parts) 3 3 3 3 3 3 Triethylene glycol (parts) 4 4 4 4 4 4 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.05 0.08 0.13 0.13 — — (3)/(2) (solid content ratio) 1.00 2.00 3.33 3.33 — — (2)/(1) (solid content ratio) 0.05 0.04 0.04 0.04 0.10 — Physical pH 8.3 82 8.4 8.3 8.3 8.3 properties Average particle diameter D50/nm 101 127 121 122 118 118 Initial viscosity (mPa .Math. s) 8.9 18.8 12.4 5.8 99 or more 8.7 Optical Measured value 1.00 1.05 1.04 1.00 1.11 0.94 density Improvement rate 106% 112% 111% 106% 118% 100% Determination G G G G G (Reference) Rubfastness G G G G G N Marker resistance G G G G N G Ink jet adaptability G M G G N G

TABLE-US-00026 TABLE 26 Production Example 6 PLM Example Example Example Example Example Example Aqueous cyan ink (Type 2) dispersion 98 99 100 101 102 103 Dispersion method PLM PLM PLM PLM PLM PLM PLM (US: ultrasonic dispersion method PLM: kneading method) Compos- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN ition pigment (1) name Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR Blue TGR (parts) 8 4 4 4 4 4 4 (solid content) Anionic Name/ Resin A Resin A Resin A Resin A Resin A Resin A Resin A group- Product name containing (parts) 2.4 1.2 1.2 1.2 1.2 1.2 1.2 organic (solid content) polymer Name/Product DN-800H DN-8001-1 DN-100L CMC1390 DN-100L — — compound name (parts) 0.4 0.2 0.15 0.1 0.15 — — (solid content) Bio- Product name CHI-NF CEL-NF CEL-NF CEL-NF CHI-NF CEL-KY CEL-KY nano- (abbreviation) fibers (2) (parts) 0.3 0.15 0.2 0.15 0.3 0.2 0.15 Colloidal Product name PL-3 PL-3 PL-10H PL-3L PL-10H PL-3 PL-10H silica (3) (abbreviation) (parts) 1.0 0.5 0.3 0.5 0.5 0.75 0.3 2-Pyrrolidone (parts) — 8 8 8 8 8 8 Triethylene glycol — 8 8 8 8 8 8 monobutyl ether (parts) Glycerin (parts) — 3 3 3 3 3 3 Triethylene glycol (parts) 3 1.5 1.5 1.5 1.5 1.5 1.5 Surfynol 440 (parts) — 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.13 0.08 0.13 0.13 0.19 0.08 (3)/(2) (solid content ratio) 3.33 3.33 1.50 3.33 1.67 3.75 2.00 (2)/(1) (solid content ratio) 0.04 0.04 0.05 0.04 0.08 0.05 0.04 Physical pH 9.9 92 9.3 9.0 8.8 9.3 9.3 properties Average particle 95 92 93 96 96 92 92 diameter D50/nm Initial viscosity (mPa .Math. s) — 9.9 7.9 9.1 16.1 6.6 3.9 Optical Measured value — 1.03 1.02 1.01 1.04 1.00 0.99 density Improvement rate — 107% 106% 105% 108% 104% 103% Determination — G G G G G G Rubfastness — G G G G G G Marker resistance — G G G G G G Ink jet adaptability — G G G M G G

TABLE-US-00027 TABLE 27 Compa- Compa- rative rative Example Example Example Example Aqueous cyan ink (Type 2) 104 105 27 28 Dispersion method PLM PLM PLM PLM (US: ultrasonic dispersion method PLM: kneading method) Compo- Cyan Product FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment (1) name Blue TGR Blue TGR Blue TGR Blue TGR (parts) (solid content) 4 4 4 4 Anionic Name/Product name Resin A Resin A Resin A Resin A group- (parts) (solid content) 1.2 1.2 1.2 1.2 containing Name/Product name DN-800H CMC1390 — — organic polymer (parts) (solid content) 0.2 0.1 — — compound Bio- Product name CEL-KY CEL-KY CEL-NF — nanofibers (abbreviation) (2) (parts) 0.2 0.1 0.4 — Colloidal Product name PL-3L PL-3 — — silica (3) (abbreviation) (parts) 0.5 0.5 — — 2-Pyrrolidone (parts) 8 8 8 8 Triethylene glycol 8 8 8 8 monobutyl ether (parts) Glycerin (parts) 3 3 3 3 Triethylene glycol (parts) 1.5 1.5 1.5 1.5 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Total (parts) 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.13 — — (3)/(2) (solid content ratio) 2.50 5.00 — — (2)/(1) (solid content ratio) 0.05 0.03 0.10 — Physical pH 9.1 9.1 9.3 9.3 properties Average particle diameter D50/nm 93 93 91 91 Initial viscosity (mPa .Math. s) 25.6 14.8 99 or more 2.5 Optical Measured value 0.99 0.99 1.13 0.96 density Improvement rate 103% 103% 118% 100% Determination G G G (Reference) Rubfastness G G G N Marker resistance G G N G Ink jet adaptability M G N G

TABLE-US-00028 TABLE 28 Production Example 3 US Example Example Example Example Example Example Aqueous magenta ink (Type 1) dispersion 106 107 108 109 110 111 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Magenta Product name FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment Super Super Super Super Super Super Super (1) Magenta Magenta Magenta Magenta Magenta Magenta Magenta RY RY RY RY RY RY RY (parts) (solid content) 8 6 6 6 6 6 6 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing (parts) (solid content) 2.4 1.8 1.8 1.8 1.8 1.8 1.8 organic polymer Name/Product name — — — CMC1390 DN-800H DN-800H DN-100L compound (parts) (solid content) — — — 0.15 0.15 0.3 0.15 Bio-nanofibers Product name CHI-NF CEL-NF CEL-NF CEL-KY CEL-KY CEL-NF CEL-NF (2) (abbreviation) (parts) 0.4 0.3 0.075 0.45 0.1 0.15 0.2 Colloidal silica Product name PL-3 PL-3 PL-10H PL-1 PL-10H PL-1 PL-3 (3) (abbreviation) (parts) 0.8 0.6 0.3 0.3 0.3 0.3 0.15 Triethylene glycol (parts) 8 6 6 6 6 6 6 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.10 0.10 0.05 0.05 0.05 0.05 0.03 (3)/(2) (solid content ratio) 2.00 2.00 4.00 0.67 3.00 2.00 0.75 (2)/(1) (solid content ratio) 0.05 0.05 0.01 0.08 0.02 0.03 0.03 Physical pH 9.9 9.2 9.2 9.7 9.7 9.7 9.8 properties Average particle diameter D50/nm 96 95 95 110 109 92 93 Initial viscosity (mPa .Math. s) — 2.9 14.5 11.9 8.8 8.3 8.4 Optical density Measured value — 1.19 1.21 1.31 1.30 1.22 1.23 Improvement rate — 103% 105% 114% 113% 106% 107% Determination — G G G G G G Rubfastness — G G G G G G

TABLE-US-00029 TABLE 29 Comparative Comparative Example Example Example Example Example Example Example Aqueous magenta ink (Type 1) 112 29 30 113 114 115 116 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Magenta Product name FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment Super Super Super Super Super Super Super (1) Magenta Magenta Magenta Magenta Magenta Magenta Magenta RY RY RY RY RY RY RY (parts) (solid content) 6 6 6 6 6 6 6 Anionic group- Name/Product name SA-1 SA-1 SA-1 UR-1 UR-1 UR-1 UR-1 containing (parts) (solid content) 1.8 1.8 1.8 1.8 1.8 1.8 1.8 organic polymer Name/Product name DN-10L — — — — DN-800H DN-10L compound (parts) (solid content) 0.3 — — — — 0.15 0.15 Bio-nanofibers Product name CHI-NF CEL-NF — CEL-NF CEL-KY CEL-NF CEL-NF (2) (abbreviation) (parts) 0.075 0.6 — 0.075 0.15 0.3 0.3 Colloidal silica Product name PL-3 — — PL-3 PL-7 PL-10H PL-7 (3) (abbreviation) (parts) 0.45 — — 0.45 0.15 0.45 0.225 Triethylene glycol (parts) 6 6 6 6 6 6 6 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.08 — — 0.08 0.03 0.08 0.04 (3)/(2) (solid content ratio) 6.00 — — 6.00 1.00 1.50 0.75 (2)/(1) (solid content ratio) 0.01 0.10 — 0.01 0.03 0.05 0.05 Physical pH 9.5 9.5 10.1 8.8 8.4 8.5 8.9 properties Average particle diameter D50/nm 95 93 104 102 108 107 101 Initial viscosity (mPa .Math. s) 6.5 99 or more 1.4 6.9 11.0 8.4 8.0 Optical density Measured value 1.19 1.31 1.15 1.18 1.23 1.19 1.19 Improvement rate 103% 114% 100% 105% 110% 106% 106% Determination G G (Reference) G G G G Rubfastness G G N G G G G

TABLE-US-00030 TABLE 30 Production Comparative Comparative Example 7 Example Example Example PLM Example Example Example Aqueous magenta ink (Type 1) 117 31 32 dispersion 118 119 120 Dispersion method (US: ultrasonic dispersion US US US PLM PLM PLM PLM method PLM: kneading method) Compo- Magenta Product name FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment Super Super Super Super Super Super Super (1) Magenta Magenta Magenta Magenta Magenta Magenta Magenta RY RY RY RY RY RY RY (parts) (solid content) 6 6 6 6 6 6 6 Anionic group- Name/Product name UR-1 UR-1 UR-1 Resin A Resin A Resin A Resin A containing (parts) (solid content) 1.8 1.8 1.8 1.6 1.2 1.2 1.2 organic polymer Name/Product name CMC1390 — — — — — CMC1390 compound (parts) (solid content) 0.2 — — — — — 0.1 Bio-nanofibers Product name CHI-NF CEL-KY CEL-KY CEL-KY CEL-KY (2) (abbreviation) (parts) 0.15 — — 0.2 0.15 0.2 0.1 Colloidal silica Product name PL-10H PL-10H — PL-7 PL-7 PL-1 PL-10H (3) (abbreviation) (parts) 0.5 0.3 — 0.4 0.3 0.3 0.5 Triethylene glycol (parts) 6 6 6 5.4 4.05 4.05 4.05 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.08 0.05 — 0.05 0.05 0.05 0.08 (3)/(2) (solid content ratio) 3.33 — — 2.00 2.00 1.50 5.00 (2)/(1) (solid content ratio) 0.03 — — 0.03 0.03 0.03 0.02 Physical pH 7.8 8.8 8.8 10.3 9.7 9.7 9.7 properties Average particle diameter D50/nm 102 98 98 101 101 104 103 Initial viscosity (mPa .Math. s) 7.0 2.0 2.0 — 3.5 8.0 16.9 Optical density Measured value 1.16 1.12 1.12 — 1.16 1.17 1.21 Improvement rate 104% 100% 100% — 104% 105% 108% Determination G N (Reference) — G G G Rubfastness G N N — G G G

TABLE-US-00031 TABLE 31 Comparative Example Example Example Example Aqueous magenta ink (Type 1) 121 122 123 33 Dispersion method (US: ultrasonic dispersion method PLM PLM PLM PLM PLM: kneading method) Composition Magenta Product name FASTOGEN FASTOGEN FASTOGEN FASTOGEN pigment (1) Super Super Super Super Magenta RY Magenta RY Magenta RY Magenta RY (parts) (solid content) 6 6 6 6 Anionic Name/Product name Resin A Resin A Resin A Resin A group- (parts) (solid content) 1.2 1.2 1.2 1.2 containing Name/Product name — DN-100L CMC1390 — organic (parts) (solid content) — 0.15 0.1 — polymer compound Bio- Product name CEL-NF CEL-NF CHI-NF nanofibers (2) (abbreviation) (parts) 0.15 0.2 0.15 — Colloidal Product name PL-3 PL-10H PL-3 — silica (3) (abbreviation) (parts) 0.4 0.3 0.5 — Triethylene glycol (parts) 4.05 4.05 4.05 4.05 Pure water Balance Balance Balance Balance Total (parts) 100 100 100 100 (3)/(1) (solid content ratio) 0.07 0.05 0.08 — (3)/(2) (solid content ratio) 2.67 1.50 3.33 — (2)/(1) (solid content ratio) 0.03 0.03 0.03 — Physical pH 9.2 9.8 9.5 10.0 properties Average particle diameter D50/nm 96 93 96 101 Initial viscosity (mPa .Math. s) 14.5 10.1 8.0 1.5 Optical Measured value 1.16 1.19 1.18 1.12 density Improvement rate 104% 106% 105% 100% Determination G G G (Reference) Rubfastness G G G N

TABLE-US-00032 TABLE 32 Production Example 3 US Example Example Example Example Example Example Aqueous magenta ink (Type 2) dispersion 124 125 126 127 128 129 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Magenta Product name FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment Super Super Super Super Super Super Super (1) Magenta Magenta Magenta Magenta Magenta Magenta Magenta RY RY RY RY RY RY RY (parts) (solid content) 8 4 4 4 4 4 4 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing (parts) (solid content) 2.4 1.2 1.2 1.2 1.2 1.2 1.2 organic polymer Name/Product name — — — — CMC1390 DN-800H DN-800H compound (parts) (solid content) — — — — 0.2 0.2 0.15 Bio-nanofibers Product name CHI-NF CEL-NF CEL-NF CEL-KY CEL-KY CEL-KY CEL-NF (2) (abbreviation) (parts) 0.4 0.2 0.15 0.1 0.1 0.1 0.15 Colloidal silica Product name PL-3 PL-3 PL-10H PL-3 PL-1 PL-10H PL-1 (3) (abbreviation) (parts) 0.8 0.4 0.2 0.3 0.3 0.3 0.3 2-Pyrrolidone (parts) — 8 8 8 8 8 8 Triethylene glycol monobutyl — 8 8 8 8 8 8 ether (parts) Glycerin (parts) — 3 3 3 3 3 3 Triethylene glycol (parts) 8 4 4 4 4 4 4 Surfynol 440 (parts) — 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.10 0.10 0.05 0.08 0.08 0.08 0.08 (3)/(2) (solid content ratio) 2.00 2.00 1.33 3.00 3.00 3.00 2.00 (2)/(1) (solid content ratio) 0.05 0.05 0.04 0.03 0.03 0.03 0.04 Physical pH 9.9 8.8 8.8 9.1 9.2 9.2 9.2 properties Average particle diameter D50/nm 96 95 95 110 110 109 92 Initial viscosity (mPa .Math. s) — 3.3 16.1 10.9 13.2 9.8 9.1 Optical density Measured value — 0.90 0.91 0.96 0.98 0.98 0.92 Improvement rate — 103% 105% 110% 114% 113% 106% Determination — G G G G G G Rubfastness — G G G G G G Marker resistance — G G G G G G Ink jet adaptability — G M G G G G

TABLE-US-00033 TABLE 33 Comparative Comparative Example Example Example Example Example Example Example Aqueous magenta ink (Type 2) 130 131 132 34 35 133 134 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Magenta Product name FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment Super Super Super Super Super Super Super (1) Magenta Magenta Magenta Magenta Magenta Magenta Magenta RY RY RY RY RY RY RY (parts) (solid content) 4 4 4 4 4 4 4 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 UR-1 UR-1 containing (parts) (solid content) 1.2 1.2 1.2 1.2 1.2 1.2 1.2 organic polymer Name/Product name DN-100L DN-10L DN-100L — — — — compound (parts) (solid content) 0.2 0.1 0.15 — — — — Bio-nanofibers Product name CEL-NF CHI-NF CHI-NF CEL-NF — CEL-NF CEL-KY (2) (abbreviation) (parts) 0.2 0.2 0.25 0.4 — 0.05 0.1 Colloidal silica Product name PL-3 PL-3 PL-10H — — PL-3 PL-7 (3) (abbreviation) (parts) 0.5 0.4 0.2 — — 0.4 0.2 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol monobutyl 8 8 8 8 8 8 8 ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 4 4 4 4 4 4 4 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.13 0.10 0.05 — — 0.10 0.05 (3)/(2) (solid content ratio) 2.50 2.00 0.80 — — 8.00 2.00 (2)/(1) (solid content ratio) 0.05 0.05 0.06 0.10 — 0.01 0.03 Physical pH 9.3 9.0 8.8 9.0 9.0 8.4 8.0 properties Average particle diameter D50/nm 93 95 95 93 93 102 108 Initial viscosity (mPa .Math. s) 9.3 7.2 17.8 99 or more 2.1 7.7 12.2 Optical density Measured value 0.93 0.90 0.92 0.99 0.87 0.86 0.90 Improvement rate 107% 103% 106% 114% 100% 105% 110% Determination G G G G (Reference) G G Rubfastness G G G G N G G Marker resistance G G G N G G G Ink jet adaptability G G M N G G G

TABLE-US-00034 TABLE 34 Production Comparative Comparative Example 7 Example Example Example Example Example PLM Example Aqueous magenta ink (Type 2) 135 136 137 36 37 dispersion 138 Dispersion method (US: ultrasonic dispersion US US US US US PLM PLM method PLM: kneading method) Compo- Magenta Product name FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment Super Super Super Super Super Super Super (1) Magenta Magenta Magenta Magenta Magenta Magenta Magenta RY RY RY RY RY RY RY (parts) (solid content) 4 4 4 4 4 8 4 Anionic group- Name/Product name UR-1 UR-1 UR-1 UR-1 UR-1 Resin A Resin A containing (parts) (solid content) 1.2 1.2 1.2 1.2 1.2 1.6 0.8 organic polymer Name/Product name DN-800H DN-10L CMC1390 — — — — compound (parts) (solid content) 0.15 0.1 0.2 — — — — Bio-nanofibers Product name CEL-NF CEL-NF CHI-NF CEL-KY CEL-KY (2) (abbreviation) (parts) 0.15 0.15 0.1 — — 0.2 0.1 Colloidal silica Product name PL-10H PL-7 PL-10H PL-10H — PL-7 PL-7 (3) (abbreviation) (parts) 0.2 0.3 0.5 0.2 — 0.4 0.2 2-Pyrrolidone (parts) 8 8 8 8 8 — 8 Triethylene glycol monobutyl 8 8 8 8 8 — 8 ether (parts) Glycerin (parts) 3 3 3 3 3 — 3 Triethylene glycol (parts) 4 4 4 4 4 5.4 2.7 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 — 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.05 0.08 0.13 0.05 — 0.05 0.05 (3)/(2) (solid content ratio) 1.33 2.00 5.00 — — 2.00 2.00 (2)/(1) (solid content ratio) 0.04 0.04 0.03 — — 0.03 0.03 Physical pH 8.1 8.5 7.4 8.4 8.4 10.3 9.2 properties Average particle diameter D50/nm 107 101 102 98 98 101 101 Initial viscosity (mPa .Math. s) 9.3 9 7.8 2.2 2.2 — 3.8 Optical density Measured value 0.87 0.87 0.85 0.82 0.82 — 0.88 Improvement rate 106% 106% 104% 100% 100% — 104% Determination G G G N (Reference) — G Rubfastness G G G N N — G Marker resistance G G G G G — G Ink jet adaptability G G G G G — G

TABLE-US-00035 TABLE 35 Comparative Example Example Example Example Example Example Example Aqueous magenta ink (Type 2) 139 140 141 142 143 144 38 Dispersion method (US: ultrasonic dispersion PLM PLM PLM PLM PLM PLM PLM method PLM: kneading method) Compo- Magenta Product name FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN FASTOGEN sition pigment Super Super Super Super Super Super Super (1) Magenta Magenta Magenta Magenta Magenta Magenta Magenta RY RY RY RY RY RY RY (parts) (solid content) 4 4 4 4 4 4 4 Anionic group- Name/Product name Resin A Resin A Resin A Resin A Resin A Resin A Resin A containing (parts) (solid content) 0.8 0.8 0.8 0.8 0.8 0.8 0.8 organic polymer Name/Product name — CMC1390 — DN-800H DN-100L CMC1390 — compound (parts) (solid content) — 0.1 — 0.15 0.15 0.1 — Bio-nanofibers Product name CEL-KY CEL-KY CEL-NF CEL-NF CEL-NF CHI-NF (2) (abbreviation) (parts) 0.2 0.1 0.15 0.1 0.2 0.15 — Colloidal silica Product name PL-1 PL-10H PL-3 PL-7 PL-10H PL-3 — (3) (abbreviation) (parts) 0.3 0.5 0.4 0.2 0.3 0.5 — 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol monobutyl 8 8 8 8 8 8 8 ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 2.7 2.7 2.7 2.7 2.7 2.7 2.7 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.08 0.13 0.10 0.05 0.08 0.13 — (3)/(2) (solid content ratio) 1.50 5.00 2.67 2.00 1.50 3.33 — (2)/(1) (solid content ratio) 0.05 0.03 0.04 0.03 0.05 0.04 — Physical pH 9.2 9.2 8.8 9.2 9.3 9.0 9.3 properties Average particle diameter D50/nm 104 103 96 92 93 96 91 Initial viscosity (mPa .Math. s) 8.8 18.9 16.1 9.8 11.3 8.8 2.6 Optical density Measured value 0.89 0.92 0.88 0.88 0.90 0.89 0.85 Improvement rate 105% 108% 104% 104% 106% 105% 100% Determination G G G G G G (Reference) Rubfastness G G G G G G N Marker resistance G G G G G G G Ink jet adaptability G G M G M G G

TABLE-US-00036 TABLE 36 Production Example 4 US Example Example Example Example Example Example Aqueous yellow ink (Type 1) dispersion 145 146 147 148 149 150 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Yellow Product name Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow sition pigment (1) 7413 7413 7413 7413 7413 7413 7413 (parts) (solid content) 8 6 6 6 6 6 6 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing (parts) (solid content) 1.6 1.2 1.2 1.2 1.2 1.2 1.2 organic polymer Name/Product name — — CMC1390 DN-800H DN-10L CMC1390 DN-800H compound (parts) (solid content) — — 0.15 0.15 0.09 0.3 0.09 Bio-nanofibers Product name CEL-NF CEL-NF CEL-KY CEL-KY CEL-KY CEL-NF CEL-NF (2) (abbreviation) (parts) 0.4 0.3 0.15 0.15 0.09 0.3 0.45 Colloidal silica Product name PL-3 PL-3 PL-10H PL-1 PL-3 PL-7 PL-10H (3) (abbreviation) (parts) 0.4 0.3 0.3 0.09 0.75 0.45 0.3 Triethylene glycol (parts) 8 6 6 6 6 6 6 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.05 0.05 0.05 0.02 0.13 0.08 0.05 (3)/(2) (solid content ratio) 1.00 1.00 2.00 0.60 8.33 1.50 0.67 (2)/(1) (solid content ratio) 0.05 0.05 0.03 0.03 0.02 0.05 0.08 Physical pH 9.9 9.5 9.3 9.0 9.2 9.2 9.0 properties Average particle diameter D50/nm 99 106 112 120 119 109 110 Initial viscosity (mPa .Math. s) — 2.4 17.6 15.8 10.1 4.9 2.4 Optical density Measured value — 1.29 1.24 1.25 1.27 1.33 1.33 Improvement rate — 110% 106% 107% 108% 113% 113% Determination — G G G G G G Rubfastness — G G G G G G

TABLE-US-00037 TABLE 37 Production Comparative Example 8 Example Example Example Example Example PLM Example Aqueous yellow ink (Type 1) 151 152 153 154 39 dispersion 155 Dispersion method (US: ultrasonic dispersion US US US US US PLM PLM method PLM: kneading method) Compo- Yellow Product name Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow sition pigment (1) 7413 7413 7413 7413 7413 7413 7413 (parts) (solid content) 6 6 6 6 6 8 6 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 Resin A Resin A containing (parts) (solid content) 1.2 1.2 1.2 1.2 1.2 2.4 1.8 organic polymer Name/Product name — CMC1390 DN-800H DN-800H — — — compound (parts) (solid content) — 0.15 0.15 0.3 — — — Bio-nanofibers Product name CHI-NF CHI-NF CHI-NF CHI-NF — CHI-NF CEL-NF (2) (abbreviation) (parts) 0.15 0.15 0.25 0.3 — 0.3 0.225 Colloidal silica Product name PL-3 PL-7 PL-7 PL-1 — PL-3 PL-3 (3) (abbreviation) (parts) 0.45 0.3 0.2 0.3 — 0.8 0.6 Triethylene glycol (parts) 6 6 6 6 6 4.4 3.3 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.08 0.05 0.03 0.05 — 0.10 0.10 (3)/(2) (solid content ratio) 3.00 2.00 0.80 1.00 — 2.67 2.67 (2)/(1) (solid content ratio) 0.03 0.03 0.04 0.05 — 0.04 0.04 Physical pH 9.6 9.5 9.1 9.3 9.5 10.1 9.7 properties Average particle diameter D50/nm 110 113 101 110 90 86 82 Initial viscosity (mPa .Math. s) 10.6 17.0 17.8 11.3 1.5 — 2.8 Optical density Measured value 1.28 1.24 1.31 1.27 1.17 — 1.09 Improvement rate 109% 106% 112% 108% 100% — 106% Determination G G G G (Reference) — G Rubfastness G G G G N — —

TABLE-US-00038 TABLE 38 Example Example Example Example Example Example Example Aqueous yellow ink (Type 1) 156 157 158 159 160 161 162 Dispersion method (US: ultrasonic dispersion PLM PLM PLM PLM PLM PLM PLM method PLM: kneading method) Compo- Yellow Product name Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow sition pigment (1) 7413 7413 7413 7413 7413 7413 7413 (parts) (solid content) 6 6 6 6 6 6 6 Anionic group- Name/Product name Resin A Resin A Resin A Resin A Resin A Resin A Resin A containing (parts) (solid content) 1.8 1.8 1.8 1.8 1.8 1.8 1.8 organic polymer Name/Product name — CMC1390 — — DN-100L DN-10L DN-800H compound (parts) (solid content) — 0.09 — — 0.15 0.3 0.09 Bio-nanofibers Product name CEL-NF CEL-NF CEL-KY CEL-KY CEL-NF CHI-NF CHI-NF (2) (abbreviation) (parts) 0.15 0.15 0.15 0.09 0.15 0.09 0.15 Colloidal silica Product name PL-10H PL-3 PL-7 PL-3 PL-7 PL-10H PL-10H (3) (abbreviation) (parts) 0.15 0.5 0.1 0.3 0.4 0.15 0.9 Triethylene glycol (parts) 3.3 3.3 3.3 3.3 3.3 3.3 3.3 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.03 0.08 0.02 0.05 0.07 0.03 0.15 (3)/(2) (solid content ratio) 1.00 3.33 0.67 3.33 2.67 1.67 6.00 (2)/(1) (solid content ratio) 0.03 0.03 0.03 0.02 0.03 0.02 0.03 Physical pH 9.7 9.7 9.8 9.8 9.7 9.7 9.7 properties Average particle diameter D50/nm 82 82 78 67 82 82 82 Initial viscosity (mPa .Math. s) 14.5 9.8 14.0 3.9 7.9 6.5 8.9 Optical density Measured value 1.17 1.10 1.10 1.09 1.15 1.13 1.19 Improvement rate 114% 107% 107% 106% 112% 109% 115% Determination G G G G G G G Rubfastness G G G G G G G

TABLE-US-00039 TABLE 39 Comparative Comparative Example Example Aqueous yellow ink (Type 1) 40 41 Dispersion method (US: ultrasonic dispersion PLM PLM method PLM: kneading method) Composition Yellow Product name Fast Yellow 7413 Fast Yellow 7413 pigment (1) (parts) (solid content) 6 6 Anionic Name/Product name Resin A Resin A group- (parts) (solid content) 1.8 1.8 containing Name/Product name — — organic (parts) (solid content) — — polymer compound Bio- Product name — — nanofibers (abbreviation) (2) (parts) — — Colloidal Product name PL-10H — silica (3) (abbreviation) (parts) 0.5 — Triethylene glycol (parts) 3.3 3.3 Pure water Balance Balance Total (parts) 100 100 (3)/(1) (solid content ratio) 0.08 — (3)/(2) (solid content ratio) — — (2)/(1) (solid content ratio) — — Physical pH 9.7 10.1 properties Average particle diameter D50/nm 82 76 Initial viscosity (mPa .Math. s) 2.4 1.6 Optical Measured value 1.22 1.03 density Improvement rate 119% 100% Determination N (Reference) Rubfastness N N

TABLE-US-00040 TABLE 40 Production Example 4 US Example Example Example Example Example Example Aqueous yellow ink (Type 2) dispersion 163 164 165 166 167 168 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Yellow Product name Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow sition pigment (1) 7413 7413 7413 7413 7413 7413 7413 (parts) (solid content) 8 4 4 4 4 4 4 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing (parts) (solid content) 1.6 0.8 0.8 0.8 0.8 0.8 0.8 organic polymer Name/Product name — — CMC1390 DN-800H DN-10L CMC1390 DN-800H compound (parts) (solid content) — — 0.1 0.1 0.1 0.2 0.2 Bio-nanofibers Product name CEL-NF CEL-NF CEL-KY CEL-KY CEL-KY CEL-NF CEL-NF (2) (abbreviation) (parts) 0.4 0.2 0.1 0.1 0.1 0.2 0.2 Colloidal silica Product name PL-3 PL-3 PL-10H PL-1 PL-3 PL-7 PL-10H (3) (abbreviation) (parts) 0.4 0.2 0.2 0.3 0.5 0.4 0.2 2-Pyrrolidone (parts) — 8 8 8 8 8 8 Triethylene glycol monobutyl — 8 8 8 8 8 8 ether (parts) Glycerin (parts) — 3 3 3 3 3 3 Triethylene glycol (parts) 8 4 4 4 4 4 4 Surfynol 440 (parts) — 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.05 0.05 0.05 0.08 0.13 0.10 0.05 (3)/(2) (solid content ratio) 1.00 1.00 2.00 3.00 5.00 2.00 1.00 (2)/(1) (solid content ratio) 0.05 0.05 0.03 0.03 0.03 0.05 0.05 Physical pH 9.9 9.0 8.9 8.6 8.8 8.8 8.6 properties Average particle diameter D50/nm 99 106 112 120 119 109 110 Initial viscosity (mPa .Math. s) — 2.7 19.5 17.6 11.2 5.4 2.7 Optical density Measured value — 1.07 1.03 1.04 1.05 1.10 1.10 Improvement rate — 110% 106% 107% 108% 113% 113% Determination — G G G G G G Rubfastness — G G G G G G Marker resistance — G G G G G G Ink jet adaptability — G M M G G G

TABLE-US-00041 TABLE 41 Example Example Example Example Example Example Example Aqueous yellow ink (Type 2) 169 170 171 172 173 174 175 Dispersion method (US: ultrasonic dispersion US US US US US US US method PLM: kneading method) Compo- Yellow Product name Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow sition pigment (1) 7413 7413 7413 7413 7413 7413 7413 (parts) (solid content) 4 4 4 4 4 4 4 Anionic group- Name/Product name SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 SA-1 containing (parts) (solid content) 0.8 0.8 0.8 0.8 0.8 0.8 0.8 organic polymer Name/Product name DN-10L — CMC1390 DN-100L DN-10L DN-800H DN-800H compound (parts) (solid content) 0.2 — 0.1 0.15 0.2 0.1 0.2 Bio-nanofibers Product name CEL-NF CHI-NF CHI-NF CHI-NF CHI-NF CHI-NF CHI-NF (2) (abbreviation) (parts) 0.2 0.15 0.15 0.15 0.1 0.25 0.3 Colloidal silica Product name PL-10H PL-7 PL-7 PL-7 PL-10H PL-7 PL-1 (3) (abbreviation) (parts) 0.2 0.2 0.3 0.2 0.3 0.2 0.3 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol monobutyl 8 8 8 8 8 8 8 ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 4 4 4 4 4 4 4 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.05 0.05 0.08 0.05 0.08 0.05 0.08 (3)/(2) (solid content ratio) 1.00 1.33 2.00 1.33 3.00 0.80 1.00 (2)/(1) (solid content ratio) 0.05 0.04 0.04 0.04 0.03 0.06 0.08 Physical pH 8.8 9.1 9.0 8.7 8.6 8.7 8.9 properties Average particle diameter D50/nm 133 110 113 108 106 101 110 Initial viscosity (mPa .Math. s) 19.9 11.8 18.9 5.1 11.2 19.8 12.5 Optical density Measured value 1.08 1.06 1.03 1.03 1.03 1.09 1.05 Improvement rate 111% 109% 106% 106% 106% 112% 108% Determination G G G G G G G Rubfastness G G G G G G G Marker resistance G G G G G G G Ink jet adaptability M G M G G M G

TABLE-US-00042 TABLE 42 Produciton Comparative Example 8 Example PLM Example Example Example Example Example Aqueous yellow ink (Type 2) 42 dispersion 175 176 177 178 179 Dispersion method (US: ultrasonic dispersion US PLM PLM PLM PLM PLM PLM method PLM: kneading method) Compo- Yellow Product name Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow sition pigment (1) 7413 7413 7413 7413 7413 7413 7413 (parts) (solid content) 4 8 4 4 4 4 4 Anionic group- Name/Product name SA-1 Resin A Resin A Resin A Resin A Resin A Resin A containing (parts) (solid content) 0.8 2.4 1.2 1.2 1.2 1.2 1.2 organic polymer Name/Product name — — — — DN-800H CMC1390 — compound (parts) (solid content) — — — — 0.15 0.1 — Bio-nanofibers Product name — CHI-NF CEL-NF CEL-NF CEL-NF CEL-NF CEL-KY (2) (abbreviation) (parts) — 0.3 0.15 0.15 0.15 0.15 0.2 Colloidal silica Product name — PL-3 PL-3 PL-10H PL-1 PL-3 PL-7 (3) (abbreviation) (parts) — 0.8 0.4 0.2 0.3 0.5 0.1 2-Pyrrolidone (parts) 8 — 8 8 8 8 8 Triethylene glycol monobutyl 8 — 8 8 8 8 8 ether (parts) Glycerin (parts) 3 — 3 3 3 3 3 Triethylene glycol (parts) 4 4.4 2.2 2.2 2.2 2.2 2.2 Surfynol 440 (parts) 0.5 — 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) — — 0.10 0.05 0.08 0.13 0.03 (3)/(2) (solid content ratio) — — 2.67 1.33 2.00 3.33 0.50 (2)/(1) (solid content ratio) — 0.04 0.04 0.04 0.04 0.04 0.05 Physical pH 8.6 10.1 9.2 9.2 9.2 9.2 9.3 properties Average particle diameter D50/nm 97 86 82 82 82 82 78 Initial viscosity (mPa .Math. s) 2.8 — 3.1 16.1 8.4 10.9 15.6 Optical density Measured value 0.97 — 0.91 0.98 0.91 0.92 0.92 Improvement rate 100% — 106% 114% 106% 107% 107% Determination (Reference) — G G G G G Rubfastness N — G G G G G Marker resistance N — G G G G G Ink jet adaptability G — G M G G G

TABLE-US-00043 TABLE 43 Comparative Comparative Example Example Example Example Example Example Example Aqueous yellow ink (Type 2) 180 181 182 183 184 43 44 Dispersion method (US: ultrasonic dispersion PLM PLM PLM PLM PLM PLM PLM method PLM: kneading method) Compo- Yellow Product name Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow Fast Yellow sition pigment (1) 7413 7413 7413 7413 7413 7413 7413 (parts) (solid content) 4 4 4 4 4 4 4 Anionic group- Name/Product name Resin A Resin A Resin A Resin A Resin A Resin A Resin A containing (parts) (solid content) 1.2 1.2 1.2 1.2 1.2 1.2 1.2 organic polymer Name/Product name — CMC1390 DN-100L DN-10L DN-800H — — compound (parts) (solid content) — 0.1 0.15 0.2 0.1 — — Bio-nanofibers Product name CEL-KY CEL-KY CEL-NF CHI-NF CHI-NF (2) (abbreviation) (parts) 0.1 0.1 0.15 0.1 0.25 — — Colloidal silica Product name PL-3 PL-1 PL-7 PL-10H PL-10H PL-10H — (3) (abbreviation) (parts) 0.3 0.3 0.4 0.2 0.2 0.5 — 2-Pyrrolidone (parts) 8 8 8 8 8 8 8 Triethylene glycol monobutyl 8 8 8 8 8 8 8 ether (parts) Glycerin (parts) 3 3 3 3 3 3 3 Triethylene glycol (parts) 2.2 2.2 2.2 2.2 2.2 2.2 2.2 Surfynol 440 (parts) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Pure water Balance Balance Balance Balance Balance Balance Balance Total (parts) 100 100 100 100 100 100 100 (3)/(1) (solid content ratio) 0.08 0.08 0.10 0.05 0.05 0.13 — (3)/(2) (solid content ratio) 3.00 3.00 2.67 2.00 0.80 — — (2)/(1) (solid content ratio) 0.03 0.03 0.04 0.03 0.06 — — Physical pH 9.3 9.2 9.2 9.2 9.2 9.2 9.2 properties Average particle diameter D50/nm 67 79 82 82 82 82 82 Initial viscosity (mPa .Math. s) 4.3 19.6 8.8 7.2 9.9 2.7 2.7 Optical density Measured value 0.91 0.95 0.96 0.94 0.99 1.02 0.86 Improvement rate 106% 110% 112% 109% 115% 119% 100% Determination G G G G G N (Reference) Rubfastness G G G G G N N Marker resistance G G G G G G G Ink jet adaptability G M G G G G G

AQUEOUS PIGMENT DISPERSION AND AQUEOUS INK

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C09D11/38

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