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Patent US5990227 - Ink set - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsDisclosed herein is an ink-jet recording process which comprises applying a first liquid at least containing a water-soluble resin having at least one carboxyl group or anhydride thereof, or sulfonic group per molecule to a recording medium and then applying an ink at least comprising water, an organic...http://www.google.com/patents/US5990227?utm_source=gb-gplus-sharePatent US5990227 - Ink setAdvanced Patent SearchPublication numberUS5990227 APublication typeGrantApplication numberUS 08/801,368Publication dateNov 23, 1999Filing dateFeb 19, 1997Priority dateJul 17, 1992Fee statusPaidAlso published asCA2100202A1, CA2100202C, DE69315004D1, DE69315004T2, EP0581135A1, EP0581135B1, US5623294Publication number08801368, 801368, US 5990227 A, US 5990227A, US-A-5990227, US5990227 A, US5990227AInventorsYoshihisa Takizawa, Makoto Aoki, Yutaka KurabayashiOriginal AssigneeCanon Kabushiki KaishaExport CitationBiBTeX, EndNote, RefManPatent Citations (23), Referenced by (10), Classifications (45), Legal Events (4) External Links: USPTO, USPTO Assignment, EspacenetInk set
US 5990227 AAbstract
Disclosed herein is an ink-jet recording process which comprises applying a first liquid at least containing a water-soluble resin having at least one carboxyl group or anhydride thereof, or sulfonic group per molecule to a recording medium and then applying an ink at least comprising water, an organic solvent, a dye, an alkali-soluble resin and an alkali to the portions where the first liquid has adhered, thereby forming an image. An ink set and an instrument for use in such a process are also disclosed.
1. An ink set for ink-jet recording having a first, a second, a third and a fourth ink independently, each of the inks having a different color from each other, and being selected from the group consisting of a black ink and three color inks of yellow, magenta and cyan, wherein(1) the first ink contains a water-soluble resin having at least one carboxyl group or anhydride thereof, or sulfonic group in a molecule thereof, and the first ink's pH (pH1) ranges from pH 1 to 6; (2) the second ink's pH (pH2) ranges from pH 4 to 8, and the second ink contains(a) a water-soluble resin having at least one carboxyl group or anhydride thereof, or sulfonic group in a molecule thereof, or (b) an alkali-soluble resin and an alkali; (3) the third ink contains an alkali-soluble resin and an alkali, and the third ink's pH (pH3) ranges from pH 6 to 10; (4) the fourth ink contains an alkali-soluble resin and an alkali and the fourth ink's pH (pH4) ranges from pH 8 to 13; and the pHs of the first, second, third and fourth inks satisfy the relationship of pH1 <pH2 <pH3 <pH4. 2. The ink set according to claim 1, wherein the water-soluble resin is a naturally-occurring or a synthetic water-soluble resin which has at least one carboxyl group or anhydride thereof, or sulfonic group in a molecule, or a mixture thereof.
3. The ink set according to claim 1, wherein the water-soluble resin is a polymer obtained by using, as a monomer, at least one of acrylic acid, methacrylic acid, itaconic acid, maleic acid and maleic anhydride, or a copolymer synthesized from at least one of said monomers and at least one of hydrophilic monomers having a hydrophilic group including a hydroxyl, amide, amino, ether, pyrrolidone or ethyleneimine group in a molecule.
4. The ink set according to claim 1, wherein the alkali-soluble resin is a copolymer of a hydrophilic monomer unit end a hydrophobic monomer.
5. The ink set according to claim 1, wherein the water-soluble resin has a weight average molecular weight of from 1,000 to 500,000.
6. The ink set according to claim 1, wherein the alkali-soluble resin has a weight average molecular weight of from 1,000 to 100,000.
This application is a division of application Ser. No. 08/092,219 filed Jul. 16, 1993 now U.S. Pat. No. 5,623,294.
As means for solving the above-described problems, Japanese Patent Application Laid-Open No. 55-65269 discloses the use of inks comprising a compound capable of enhancing their penetrability, such as a surfactant, and Japanese Patent Application Laid-Open No. 55-66976 discloses the use of inks comprising, as a principal component, a volatile solvent. However, the former method has involved a disadvantage that although the penetrability of the inks into recording paper is improved, and the bleeding can be prevented to some extent, the image density and the brightness of images are lowered because the inks penetrate deeply in the recording paper together with coloring matter. In addition, since the wettability to the surface of the recording paper is also improved, the inks tend to spread, resulting in reduction of resolution and occurrence of feathering. Therefore, such a method has not been preferred. In particular, this problem is noticeable when black-colored characters are expressed. On the other hand, the latter method is liable to cause clogging due to the evaporation of the solvent in a nozzle of a recording head in addition to the above-described disadvantages. Such a method has therefore not been preferred.
The present invention has been completed with the foregoing circumstances in view and has as a first object the provision of an ink set, a color ink-jet recording process and a recording apparatus, which can achieve sufficient image density even in recording on plain paper, and make it possible to conduct recording high in image quality in which evenness of image density is high and in particular, bleeding in a color image is prevented.
In the twelfth aspect of the present invention, there is provided an ink-jet recording process comprising at least using yellow, magenta, cyan and black inks and ejecting the inks on a recording material to record a color image onto the recording material, wherein the inks of different colors are different in pH from one another, and when at least two inks of the different colors are mixed, at least a part of the compositions of the inks mixed deposits, or the viscosity of at least one ink increases.
In the thirteenth aspect of the present invention, there is provided an ink-jet recording process comprising using yellow, magenta, cyan and black inks and ejecting the inks on a recording material to record a color image onto the recording material, wherein the inks completely satisfy the following conditions:
The present invention is composed of the above-described three aspects.
As a method of applying the first liquid to the recording medium, it is considered to apply the first liquid to the whole surface of the recording paper by a sprayer, roller or the like. However, the application is preferably carried out by an ink-jet system by which the first liquid can be applied selectively and evenly only to portions where the ink will be applied subsequently. In the case where the first liquid is applied by the ink-jet system, it is necessary to apply the first liquid in advance to at least portions where the ink is to applied. No particular limitation is imposed on the sizes of drops of the first liquid and the ink or the diameters of their dots formed on the recording paper. However, when the dot diameter of the first liquid is larger than that of the recording ink, the desired effect is achieved to a greater extent.
A head 13 is formed by bonding of a glass, ceramic or plastic plate or the like having a groove 14 through which an ink is passed, to a heating head 15, which is used for thermal recording and has a heating resistor (the drawing shows a head to which, however, the invention is not limited). The heating head 15 is composed of a protective film 16 made of silicon oxide or the like, aluminum electrodes 17-1 and 17-2, a heating resistor layer 18 made of nichrome or the like, a heat accumulating layer 19, and a substrate 20 made of alumina or the like having a good heat radiating property.
Now, upon application of electric signals to the electrodes 17-1, 17-2, the heating head 15 rapidly generates heat at the region shown by n to form bubbles in the ink 21 which is in contact with this region. The meniscus 23 of the ink is projected by the action of the pressure thus produced, and the ink 21 is ejected from the orifice 22 to a recording material 25 in the form of recording droplets 24. FIG. 3 schematically illustrates a multi-head composed of an array of a number of heads as shown in FIG. 1. The multi-head is formed by closely bonding a glass plate or the like 27 having a number of channels 26 to a heating head 28 similar to the head as illustrated in FIG. 1.
FIG. 5 illustrates an exemplary ink cartridge 45 in which an ink fed to the head through an ink-feeding member, for example, a tube is contained. Here, reference numeral 40 designates an ink container portion containing the ink to be fed, as exemplified by a bag for the ink. One end thereof is provided with a stopper 42 made of rubber. A needle (not illustrated) may be inserted into this stopper 42 so that the ink in the bag 40 for the ink can be fed to the head. Reference numeral 44 indicates an ink absorbing member for receiving a waste ink.
In the case where the color recording process according to the first aspect of the present invention is carried out, for example, a recording apparatus in which five recording heads, each of which has been illustrated in FIG. 3, are arranged on a carriage, is used. An example thereof is illustrated in FIG. 7. Reference numerals 81, 82, 83 and 84 indicate recording heads for ejecting inks of yellow, magenta, cyan and black colors, respectively. Reference numeral 85 designates a head for ejection of the first liquid. The heads are arranged in the above-described recording apparatus and serve to eject the recording inks of the different colors according to recording signals. Before the ejection of the inks, the first liquid is applied in advance to at least portions of recording paper where the recording inks of the different colors are to applied thereto. FIG. 7 shows the case where the five recording heads have been used. However, the present invention is not limited thereto. As shown in FIG. 8, preference is given even to the case where the flow paths of the yellow, magenta, cyan and black inks and the first liquid are separately provided in one recording head.
First of all, the following respective components were mixed into solutions, and the resultant solutions were then filtered under pressure through a membrane filter (Fluoropore Filter, trade name: product of Sumitomo Electric Industries, Ltd.) having a pore size of 0.22 μm, thereby obtaining first liquids A through G.
______________________________________(A)    Methyl vinyl ether-maleic                    1 part  anhydride copolymer  (Mw = 20,000)  Diethylene glycol 20 parts  Water              79 parts  pH = 4.8(B)    Polyacrylic acid (Mw = 10,000)                     5 parts  Diethylene glycol 21 parts  Water             74 parts  pH = 3.1(C     ) Acrylic acid-itaconic acid                    10 parts  copolymer (Mw = 8,000)  Diethylene glycol 40 parts  Water             50 parts  pH = 2.2(D)    Pectinic acid     3 parts  Diethylene glycol 30 parts  Water             67 parts  pH = 4.2(E)    Methyl vinyl ether-maleic                     7 parts  anhydride copolymer  (Mw = 67,000)  Diethylene glycol 15 parts  Water             78 parts  pH = 2.5______________________________________
______________________________________(1)Yellow:   Styrene-acrylic acid copolymer                         3 parts     (Mw = 10,000)     Sodium hydroxide     0.5 part     C.I. Direct Yellow 86                         2 parts     Diethylene glycol   30 parts     Water               64.5 partsMagenta:  Styrene-acrylic acid copolymer                          3 parts     (Mw = 10,000)     Sodium hydroxide    0.5 part     C.I. Acid Red 35    3 parts     Diethylene glycol   30 parts     Water               63.5 partsCyan:     Styrene-acrylic acid copolymer                          3 parts     (Mw = 10,000)     Sodium hydroxide    0.5 part     C.I. Direct Blue 199                         2 parts     Diethylene glycol   30 parts     Water               64.5 partsBlack:    Styrene-acrylic acid copolymer                         3 parts     (Mw = 10,000)     Sodium hydroxide    0.5 part     C.I. Food Black 2   2 parts     Diethylene glycol   30 parts     Water               64.5 parts(2)Yellow:   Styrene-maleic acid copolymer                         1 part     (Mw = 30,000)     Aqueous ammonia     0.5 part     C.I. Direct Yellow 86                         2 parts     Diethylene glycol   30 parts     Water               66.5 partsMagenta:  Styrene-maleic acid copolymer                         1 part     (Mw = 30,000)     Aqueous ammonia     0.5 part     C.I. Acid Red 35    3 part     Diethylene glycol   30 parts     Water               65.5 partsCyan:     Styrene-maleic acid copolymer                         1 part     (Mw = 30,000)     Aqueous ammonia     0.5 part     C.I. Direct Blue 199                         2 parts     Diethylene glycol   30 parts     Water               66.5 partsBlack:    Styrene-maleic acid copolymer                         1 part     (Mw = 30,000)     Aqueous ammonia     0.5 part     C.I. Food Black 2   2 parts     Diethylene glycol   30 parts     Water               66.5 parts(3)Yellow:    Isobutylene-maleic anhydride                         2 parts     copolymer (Mw = 20,000)     Sodium hydroxide    0.5 part     C.I. Direct Yellow 86                         2 parts     Diethylene glycol   30 parts     Water               65.5 partsMagenta:  Isobutylene-maleic anhydride                         2 parts     copolymer (Mw = 20,000)     Sodium hydroxide    0.5 part     C.I. Acid Red 35    3 parts     Diethylene glycol   30 parts     Water               64.5 partsCyan:     Isobutylene-maleic anhydride                         2 parts     copolymer (Mw = 20,000)     Sodium hydroxide    0.5 part     C.I. Direct Blue 199                         2 parts     Diethylene glycol   30 parts     Water               65.5 partsBlack:    Isobutylene-maleic anhydride                         2 parts     copolymer (Mw = 20,000)     Sodium hydroxide    0.5 part     C.I. Food Black 2   2 parts     Diethylene glycol   30 parts     Water               65.5 parts(4)Yellow:   Styrene-acrylic acid-acrylic                         1 part     ester copolymer (Mw = 100,000)     Sodium hydroxide    0.3 part     C.I. Direct Yellow 86                         2 parts     Diethylene glycol   30 parts     Water               66.7 partsMagenta:  Styrene-acrylic acid-acrylic                         1 part     ester copolymer (Mw= 100,000)     Sodium hydroxide    0.3 part     C.I. Acid Red 35    3 parts     Diethylene glycol   30 parts     Water               65.7 partsCyan:     Styrene-acrylic acid-acrylic                         1 part     ester copolymer (Mw = 100,000)     Sodium hydroxide    0.3 part     C.I. Direct Blue 199                         2 parts     Diethylene glycol   30 parts     Water               66.7 partsBlack:    Styrene-acrylic acid-acrylic                         1 part     ester copolymer (Mw = 10,000)     Sodium hydroxide    0.3 part     C.I. Food Black 2   2 parts     Diethylene glycol   30 parts     Water               66.7 parts(5)Yellow:   Styrene-maleic acid copolymer                         5 parts     (Mw = 1,600)     Sodium hydroxide    2.5 parts     C.I. Direct Yellow 86                         2 parts     Diethylene glycol   20 parts     Water               70.5 partsMagenta:  Styrene-maleic acid copolymer                         5 parts     (Mw = 1,600)     Sodium hydroxide    2.5 parts     C.I. Acid Red 35    3 parts     Diethylene glycol   20 parts     Water               69.5 partsCyan:     Styrene-maleic acid copolymer                         5 parts     (Mw = 1,600)     Sodium hydroxide    2.5 parts     C.I. Direct Blue 199                         2 parts     Diethylene glycol   20 parts     Water               70.5 partsBlack:     Styrene-maleic acid copolymer                         5 parts     (Mw = 1,600)     Sodium hydroxide    2.5 parts     C.I. Food Black 2   2 parts     Diethylene glycol   20 parts     Water               70.5 parts______________________________________
Recording was conducted in the same manner as in Examples 1 to 10 except that a liquid in which the methyl vinyl ether-maleic anhydride copolymer was omitted from the first liquid in (A) was used as a first liquid and liquids with the styrene-acrylic acid copolymer omitted from the respective inks in (1) were used as inks.
Recording was conducted in the same manner as in Examples 1 to 10 except that a liquid in which the methyl vinyl ether-maleic anhydride copolymer was omitted from the first liquid in (A) was used as a first liquid and the inks in (1) were used as inks.
Recording was conducted in the same manner as in Examples 1 to 10 except that the first liquid in (A) was used as a first liquid and liquids in which the styrene-acrylic acid copolymer was omitted from the respective inks in (1) were used as inks.
TABLE 1______________________________________First     Ink      Record  Resistance Rub-offliquid      set      density                       to bleeding                                  resistance______________________________________Ex. 1  (A)    (1)      A     A          AEx. 2      (B)               (2)                     A          A          AEx. 3      (C)               (3)                     A          A          AEx. 4      (D)               (4)                     A          A          AEx. 5      (E)               (5)                     A          A          AEx. 6      (F)               (1)                     A          A          AEx. 7      (G)               (1)                     A          A          AEx. 8      (A)               (2)                     A          A          AEx. 9      (A)               (3)                     A          A          AEx. 10    (A)       (4)                     A          A          AComp.      *1        *1                      C   C             AEx. 1Comp.      *1        *1                      C   C             AEx. 2Comp.      *1        *1                      C         C          AEx. 3______________________________________ *1: Described in the text.
First of all, the following respective components were mixed into solutions, and the resultant solutions were then filtered under pressure through a membrane filter (Fluoropore Filter, trade name: product of Sumitomo Electric Industries, Ltd.) having a pore size of 0.22 μm, thereby obtaining sets of inks (6) through (9) of yellow, magenta and cyan colors and sets of inks (10) through (12) of yellow, magenta, cyan and black colors.
______________________________________(6)Yellow:   Acrylic acid-itaconic acid                               2 parts     copolymer (Mw = 5,000)                                    2 partsct Yellow 86                                        30 partscol                                                    66 partsMagenta:  Styrene-monoethyl maleate                                3 parts                              copolymer                                         0.2 part                                         3 parts35                                        30 partscol                                                    63.8 partsCyan:       C.I. Direct Blue 199                                     2 parts                                        30 partscol                                                    68 parts(7)Yellow:   Methyl vinyl ether-maleic                                3 parts                    anhydride copolymer (Mw = 2,000)                                     2 partst Yellow 86                                        30 partscol                                                    65 partsMagenta:  Styrene-maleic acid copolymer                            3 parts                    (Mw = 1,000)                                       0 .2 part e                   C.I. Acid Red 35                                           3 parts                                         30 parts                                                     63.8 partsCyan:       Styrene-acrylic acid copolymer                            3 parts                    (Mw = 3,000)                      Sodium hydroxide                                          0.5 part                                       2 parts Blue 199                                         30 partsl                                                     64.5 parts(8)Yellow:   Styrene-maleic acid copolymer                            1 part                                   (Mw = 90,000)                                            0.5 part                                      2 partst Yellow 86                    Diethylene glycol                                         30 parts                                                     66.5 partsMagenta:  Acrylic acid-itaconic acid                                 1 part                                   copolymer (Mw = 80,000)                                           3 parts5                    Diethylene glycol                                         30 parts                         Water                                                     66 partsCyan:       Polyacrylic acid                    1 part                                   (Mw = 400,000)                                       2 parts Blue 199                    Diethylene glycol                                         30 parts                                                     67 parts(9)Yellow:   Carboxymethylated starch                                 13 parts                                     2 partst Yellow 86                                        30 partsol                    Water                                                    55 partsMagenta:  Styrene-maleic acid polymer                            13 parts                      copolymer (Mw = 3,000)                                         0.2 part                                          3 parts5                    Diethylene glycol                                        30 parts                                                    53.8 partsCyan:       Styrene-acrylic acid copolymer                          13 parts                                  (Mw = 10,000)                                          0.5 part                    C.I. Direct Blue 199                                      2 parts                                        30 partscol                                                    54.5 parts(10)Yellow:   Pectinic acid                           2 parts                    C.I. Direct Yellow 86                                     2 parts                                        30 partscol                                                    66 partsMagenta:  Methyl vinyl ether-maleic                                 2 parts                                  anhydride copolymer (Mw = 5,000)                    C.I. Acid Red 35                                          3 parts                                        30 partsol                    Water                                                   65 partsCyan:       Isobutylene-maleic anhydride                             2 parts                                 copolymer (Mw = 2,000)                                        0.3 part                    C.I. Direct Blue 199                                     2 parts                                       30 partscol                                                   65.7 partsBlack:     Isobutylene-maleic anhydride                            2 parts          copolymer (Mw = 20,000)                    Sodium hydroxide                                         0.5 part                                        2 partsk 2                                       30 partsol                                                   65.5 parts(11)Yellow:   Polyacrylic acid                    1 part                                 (Mw = 100,000)                                    2 partst Yellow 86                                       30 partsol                                                   67 partsMagenta:  Methyl vinyl ether-anhydrous                             2 parts                       monoethyl maleate copolymer                                 (Mw = 10,000)                                         3 parts5                                       30 partsol                    Water                                                   65 partsCyan:       Styrene-acrylic acid copolymer                           2 parts                    (Mw = 10,000)                                         0.3 part                                      2 partslue 199                                        30 parts                    Water                                                    66.7 partsBlack:     Styrene-acrylic acid-acrylic                             2 parts                                ester (Mw = 50,000)                                         0.5 part                                         2 parts2                  Diethylene glycol                                        30 parts                                                    65.5 parts(12)Yellow:   Polyitaconic acid                2 parts                                (Mw = 16,000)                    C.I. Direct Yellow 86                                     2 parts                                        20 partsl                                                    75 partsMagenta:  Acrylic acid-methacrylic acid                             4 parts                      (Mw = 5,600)                    C.I. Acid Red 35                                          3 parts                      Diethylene glycol                                        20 parts                       Water                                                    73 partsCyan:       Styrene-maleic acid copolymer                            5 parts         (Mw = 1,600)                    Sodium hydroxide                                         1.5 part                                      2 partslue 199                   Diethylene glycol                                        20 parts                                                    71.5 partsBlack:     Styrene-maleic acid copolymer                            4 parts      (Mw = 7,600)                   Sodium hydroxide                                          2.5 part                                         2 parts 2         Diethylene glycol                                        20 parts          Water                                     71.5______________________________________                         parts
Recording was conducted in the same manner as in Examples 11 to 17 except that liquids in which the methyl vinyl ether-maleic anhydride copolymer, the styrene-maleic acid copolymer or the styrene-acrylic acid copolymer was omitted from the inks of their corresponding colors in (7) were used in an ink set.
Recording was conducted in the same manner as in Examples 11 to 17 except that liquids in which the methyl vinyl ether-maleic anhydride copolymer or the styrene-maleic acid copolymer was omitted from the inks of their corresponding colors in (7) were used in an ink set.
Recording was conducted in the same manner as in Examples 11 to 17 except that liquids in which the methyl vinyl ether-maleic anhydride copolymer or the styrene-acrylic acid copolymer was omitted from the inks of their corresponding colors in (7) were used in an ink set.
Recording was conducted in the same manner as in Examples 11 to 17 except that liquids in which the styrene-maleic acid copolymer or the styrene-acrylic acid copolymer was omitted from the inks of their corresponding colors in (7) were used in an ink set.
TABLE 2______________________________________   pH level adjustedInk set   Yellow  Magenta      Cyan  Black______________________________________     4.2     9.3(         7.6  --(7)            5.6                 8.8         11.3                                     --(8)            9.8                 5.9          2.1                                     --(9)            3.3                 8.1          9.8                                     --(10)            3.3                 5.9          8.3                                   11.2(11)            2.2                 4.9          7.7                                    9.2(12)            5.0                 7.8          9.8                                   12.4______________________________________
TABLE 3______________________________________              Resistance                        Rub-off   Record density              to bleeding                        resistance______________________________________Example 11     A            A         AInk set (6)Example 12       A                            AInk set (7)Example 13       A                            AInk set (8)Example 14             A                      AInk set (9)Example 15       A                            AInk set (10)Example 16             A                      AInk set (11)Example 17             A                      AInk set (12)Comparative            A                       AExample 4Comparative            A                       AExample 5Comparative            A                       AExample 6Comparative            A                       AExample 7______________________________________
First of all, the following respective components were mixed into solutions, and the resultant solutions were then filtered under pressure through a membrane filter (Fluoropore Filter, trade name: product of Sumitomo Electric Industries, Ltd.) having a port size of 0.22 μm, thereby obtaining sets of inks (13) through (18) of yellow, magenta, cyan and black colors.
______________________________________(13)Yellow:   Methyl vinyl ether-maleic                               3 parts      anhydride copolymer (Mw = 2,000)                                     2 partsellow 86                  Ethylene oxide adduct of lauryl                           0.5 part                               alcohol (number of moles added: 10)                    Diethylene glycol                                        30 parts                                       64.5 partsMagenta:  Methyl vinyl ether-maleic                                 3 parts       anhydride copolymer (Mw = 2,000)                      C.I. Acid Red 35                                          3 parts                    Ethylene oxide adduct of lauryl                           0.5 part          alcohol (number of moles added: 10)         Diethylene glycol                                        30 parts        Water                                       63.5 partsCyan:       Methyl vinyl ether-maleic                                 3 parts                    anhydride copolymer (Mw = 2,000)                                      2 partsue 199               Ethylene oxide adduct of lauryl                           0.5 part                alcohol (number of moles added: 10)               Diethylene glycol                                        30 parts              Water                                 64.5 partsBlack:     Styrene-acrylic acid-acrylic                              2 parts                  ester copolymer (Mw = 10,000)                                          0.5 part                                         2 parts                                        30 parts                  Water                             65.5 parts(14)Yellow:   Styrene-maleic acid copolymer                             1 part      (MW = 90,000)                                           0.5 part                    C.I. Direct Yellow 86                                     2 parts                 Ethylene oxide adduct of nonyl-                           5 parts                phenol (number of moles added: 18)             Diethylene glycol                                        30 parts            Water                                   60.5 partsMagenta:  Styrene-maleic acid copolymer                            1 part       (Mw = 90,000)        Aqueous ammonia                  0.5 part                                          3 parts                           5 partslene oxide adduct of nonyl-                    phenol (number of moles added: 18)        Diethylene glycol                                        30 parts        Water                                       60.5 partsCyan:      Styrene-maleic acid copolymer                            1 part       (Mw = 90,000)              Aqueous ammonia                                           0.5 part                                      2 partsue 199                   Ethylene oxide adduct of nonyl-                           5 parts                            phenol (number of moles added: 18)                                        30 parts                                                    61.5 partsBlack:    Polyacrylic acid                     2 parts      (Mw = 10,000)       C.I. Food Black 2                 2 parts       Diethylene glycol                30 parts       Water                                        66 parts(15)Yellow:   Styrene-maleic acid copolymer                           13 parts         (Mw = 3,000)        Sodium hydroxide                 0.2 part        C.I. Direct Yellow 86                                     2 parts                    Ethylene oxide-propylene oxide                            3 parts                      copolymer (number of moles       added: 7)                     Diethylene glycol                                        30 parts                  Water                             51.8 partsMagenta:  Styrene-maleic acid copolymer                          13 parts                    (Mw = 3,000)                        Sodium hydrbxide                                        0.2 part                                          3 parts                            3 parts oxide-propylene oxide         copolymer (number of moles       added: 7)                    Diethylene glycol                                        30 parts               Water                               50.8 partsCyan:       Styrene-acrylic acid copolymer                          13 parts       (Mw = 5,000)         Sodium hydroxide                                         0.5 part                                      2 parts 199                    Ethylene oxide-propylene oxide                            3 parts                            copolymer (number of moles         added: 7)                                        30 parts                    Water                                                    51.5 partsBlack:     Methyl vinyl ether-monoethyl                             2 parts                    maleate copolymer         (Mw = 10,000)                                         2 parts                                        30 parts                                                    66 parts(16)Yellow:   Pectinic acid                           2 parts                       C.I. Direct Yellow 86                                     2 parts                      Ethylene oxide adduct of                                  1 part             acetylene glycol                    (number of moles added: 10)                                        30 parts                                                    65 partsMagenta:  Methyl vinyl ether-maleic                                2 parts                             anhydride copolymer (Mw = 5,000)                    C.I. Acid Red 35                                          3 parts                        Ethylene oxide adduct of                                  1 part                    acetylene glycol                   (number of moles added: 10)                                         30 partsl                                                     64 partsCyan:       Polyacrylic acid                    2 parts                        (Mw = 2,000)                                       2 partslue 199                                   1 part xide adduct of                                 acetylene glycol                     (number of moles added: 10)                                         30 partsl                                                     65 partsBlack:     Isobutylene-maleic anhydride                              2 parts            copolymer (Mw = 20,000)                     Sodium hydroxide                                          0.5 part                                          2 parts2                                         30 parts                                                     65.5 parts(17)Yellow:   Styrene-acrylic acid copolymer                            2 parts             (Mw = 10,000)            Sodium hydroxide                                           0.3 part                                      2 partsYellow 86                                  15 partsol monolaurate                     Diethylene glycol                                         30 parts                                                     50.7 partsMagenta:  Styrene-acrylic acid copolymer                           2 parts                (Mw = 10,000)               Sodium hydroxide                                           0.3 part                                           2 parts                    Decaglycerol monolaurate                                  15 parts                                         30 parts                                                     50.7 partsCyan:       Styrene-acrylic acid copolymer                            2 parts         (Mw = 10,000)        Sodium hydroxide                  0.3 part           C.I. Direct Blue 199                                       2 parts          Decaglycerol monolaurate                                  15 parts         Diethylene glycol                                         30 parts        Water                                        50.7 partsBlack:    Polyitaconic acid                    2 parts        (Mw = 50,000)                                          2 parts2                                         30 parts                                                     66 parts(18)Yellow:   Styrene-acrylic acid copolymer                             2 parts                                 (Mw = 10,000)                                           0.3 part                                      2 partsYellow 86                    Sodium salt of lauryl sulfate                             0.2 part                                         30 partsl                    Water                                                   65.5 partsMagenta:  Styrene-acrylic acid copolymer                           2 parts                    (Mw = 10,000)                                         0.3 part                    C.I. Acid Red 35                                         2 parts                            0.2 part um salt of lauryl sulfate                                       30 partscol                                                   65.5 partsCyan:       Styrene-acrylic acid copolymer                           2 parts                    (Mw = 10,000)                                         0.3 part                                     2 parts Blue 199                            0.2 part m salt of lauryl sulfate                                       30 partscol                    Water                                                   65.5 partsBlack:    Polyitaconic acid                  2 parts                                (Mw = 50,000)                                        2 partsk 2                                       30 partsol                    Water                                                   66______________________________________                         parts
Recording was conducted in the same manner as in Examples 18 to 23 except that inks in which the methyl vinyl ether-maleic anhydride copolymer or the styrene-acrylic acid-acrylic ester copolymer was omitted from the inks of their corresponding colors in (13) were used in an ink set.
Recording was conducted in the same manner as in Examples 18 to 23 except that inks in which the methyl vinyl ether-maleic anhydride copolymer was omitted from the inks of their corresponding colors in (13) were used in an ink set.
Recording was conducted in the same manner as in Examples 18 to 23 except that inks in which the styrene-acrylic acid-acrylic ester copolymer was omitted from the inks of their corresponding colors in (13) were used in an ink set.
Recording was conducted in the same manner as in Examples 11 to 17 except that inks in which the ethylene oxide adduct of lauryl alcohol was omitted from the inks of their corresponding colors in (13) were used in an ink set.
Recording was conducted in the same manner as in Examples 18 to 23 except that inks in which the methyl vinyl ether-maleic anhydride copolymer or the styrene-acrylic acid-acrylic ester copolymer was omitted from the inks of their corresponding colors in (13) and with 0.5 part of ethylene oxide adduct of lauryl alcohol added to the black ink were used in an ink set.
Quality of black-colored characters
TABLE 4______________________________________   pH level adjustedInk set   Yellow  Magenta      Cyan  Black______________________________________(13)        4.1   4.2           4.5    8.8(14)           9.3                 9.4          9.1                                    3.8(15)          12.8                13.0         12.5                                    2.2(16)           5.7                 3.2          2.1                                    8.3(17)          10.5                10.8         10.3                                    6.2(18)           9.8                10.2          9.9                                    5.6______________________________________
TABLE 5______________________________________                Resistance      Resistance                to bleeding                          Quality      to bleeding                between   of black-                                 Rub-offRecord     between   color and colored                                 resis-density    color inks                black ink character                                 tance______________________________________Ex. 18 A       A         A       A      AInk set(13)Ex. 19 A       A         A       A      AInk set(14)Ex. 20 A       A         A       A      AInk set(15)Ex. 21 A       A         A       A      AInk set(16)Ex. 22 A       A         A       A      AInk set(17)Ex. 23 A       A         A       A      AInk set(18)Comp.  A       A         C       A      AEx. 8Comp.  A       A         C       A      AEx. 9Comp.  A       A         C       A      AEx. 10Comp.  A       C         A       A      AEx. 11Comp.  A       A         A       C      AEx. 12______________________________________
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