JP4549670B2 - Manufacturing method of water-based ink - Google Patents
Manufacturing method of water-based ink Download PDFInfo
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- JP4549670B2 JP4549670B2 JP2003435741A JP2003435741A JP4549670B2 JP 4549670 B2 JP4549670 B2 JP 4549670B2 JP 2003435741 A JP2003435741 A JP 2003435741A JP 2003435741 A JP2003435741 A JP 2003435741A JP 4549670 B2 JP4549670 B2 JP 4549670B2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 38
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000006185 dispersion Substances 0.000 claims description 99
- 239000000049 pigment Substances 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 26
- 229920003176 water-insoluble polymer Polymers 0.000 claims description 15
- 239000002612 dispersion medium Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 5
- 239000000976 ink Substances 0.000 description 43
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 33
- 229920000642 polymer Polymers 0.000 description 21
- 239000002245 particle Substances 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000002904 solvent Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
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- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 3
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- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
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- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000004606 Fillers/Extenders Substances 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
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- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical compound N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 229940121375 antifungal agent Drugs 0.000 description 2
- 239000003429 antifungal agent Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
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- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
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- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000012860 organic pigment Substances 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- RBNPOMFGQQGHHO-UHFFFAOYSA-N -2,3-Dihydroxypropanoic acid Natural products OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 description 1
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- RBNPOMFGQQGHHO-UWTATZPHSA-N D-glyceric acid Chemical compound OC[C@@H](O)C(O)=O RBNPOMFGQQGHHO-UWTATZPHSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
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- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 description 1
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- Inks, Pencil-Leads, Or Crayons (AREA)
Description
本発明は、水系インクの製造法に関する。更に詳しくは、インクジェット記録用水系インク等に好適に使用しうる水系インクの製造法に関する。 The present invention relates to a method for producing a water-based ink. More specifically, the present invention relates to a method for producing a water-based ink that can be suitably used for a water-based ink for inkjet recording.
インクジェット記録方式は、カラー化が容易であり、記録部材として普通紙を使用することができるので、近年広く用いられている。 The ink jet recording system has been widely used in recent years because it can be easily colored and can use plain paper as a recording member.
インクジェットに使用されるインクには、ノズルにインクが目詰まりするのを防止するために、水溶性染料及び多価アルコールが用いられている。しかし、このインクには、耐水性や耐光性に劣り、特に熱ジェット方式のインクとして使用した場合には、ヒーター面の熱により染料が酸化され、インクがヒーター面に焦げつきやすく、吐出性が低下するという欠点がある。 Water-soluble dyes and polyhydric alcohols are used for inks used in ink jets in order to prevent ink from clogging the nozzles. However, this ink is inferior in water resistance and light resistance, especially when used as a heat jet ink, the dye is oxidized by the heat of the heater surface, the ink tends to scorch on the heater surface, and the discharge property is reduced. There is a drawback of doing.
この欠点を解消するために、顔料インクが提案されている。顔料インクが目詰まりを起こさず安定した吐出特性を有するものとするためには、分散液中で顔料が沈降しないように、その粒径を十分小さいものにして分散させる必要がある。 In order to eliminate this drawback, a pigment ink has been proposed. In order for the pigment ink to have stable ejection characteristics without causing clogging, it is necessary to disperse the pigment ink with a sufficiently small particle size so that the pigment does not settle in the dispersion.
一般に、顔料の分散は、分散液の製造法を利用して行なわれており、撹拌機によるミキシングは、通常、10Pa程度の低せん断応力で行なわれている。しかし、このような低せん断応力では、分散不良を生じたり、インク特性が悪くなるという欠点がある。 In general, the pigment is dispersed using a manufacturing method of the dispersion, and the mixing by the stirrer is usually performed at a low shear stress of about 10 Pa. However, such a low shear stress has a drawback in that poor dispersion occurs and ink characteristics deteriorate.
また、分散させる際には、ビーズミル、サンドミル、ボールミル等の分散機によるメディアを用いた分散方法も提案されている。しかし、この分散方法は、メディアとベッセルやメディア同士の衝突によって発生する無機不純物量が多く、吐出速度が低下する等の欠点があるため、機能面から好ましくない。 In addition, a dispersion method using media by a disperser such as a bead mill, a sand mill, or a ball mill has been proposed. However, this dispersion method is not preferable in terms of function because it has a disadvantage that the amount of inorganic impurities generated by collision between the medium and the vessel or the medium is large and the discharge speed is reduced.
前記欠点を解消するために、高圧ホモジナイザーを用いた顔料インクの製造法、例えば、分散剤及び顔料を少なくとも含む混合物を複数のオリフィスを有するチャンバーを通過させ、処理液同士を衝突させて微粒子化する顔料インクの製造法(例えば、特許文献1参照)が提案されている。この製造法により、顔料の分散は大きく改善される。しかし、この方法における処理条件では、処理圧力が低く、パス回数も少ないため、経時的にインクの粘度が変化し、安定に印字できなくなる場合があり、この方法で得られた分散体よりも更に分散安定性の良好な分散体が望まれている。 In order to eliminate the above disadvantages, a method for producing a pigment ink using a high-pressure homogenizer, for example, a mixture containing at least a dispersant and a pigment is passed through a chamber having a plurality of orifices, and the treatment liquids collide with each other to make fine particles. A method for producing a pigment ink has been proposed (see, for example, Patent Document 1). This production method greatly improves the dispersion of the pigment. However, under the processing conditions in this method, since the processing pressure is low and the number of passes is small, the viscosity of the ink may change over time and stable printing may not be possible, and even more than the dispersion obtained by this method. A dispersion having good dispersion stability is desired.
また、分散媒と顔料と水不溶性ポリマーを混合し、1.0×105 Pa 以上のせん断応力で分散する顔料インクの製造法が提案されている(例えば、特許文献2参照)。この製造法により、顔料の分散は大きく改善される。しかし、この方法では、高い処理圧力で顔料インクを分散されているが、パス回数が少なく、経時的にインクの粘度が変化し、安定に印字できなくなる場合があり、この方法で得られた分散体よりも更に分散安定性の良好な分散体が望まれている。 Further, a method for producing a pigment ink in which a dispersion medium, a pigment, and a water-insoluble polymer are mixed and dispersed with a shear stress of 1.0 × 10 5 Pa or more has been proposed (for example, see Patent Document 2). This production method greatly improves the dispersion of the pigment. However, with this method, the pigment ink is dispersed at a high processing pressure. However, the number of passes is small, and the viscosity of the ink changes over time, so that stable printing may not be possible. A dispersion having better dispersion stability than the body is desired.
また、分散剤及び顔料を少なくとも含む混合物を単一のせん断管路をもつ液−壁衝突式高圧ホモジナイザーで分散する顔料インクの製造法が提案されている(例えば、特許文献3参照)。この製造法により、顔料の分散は大きく改善される。しかし、この方法では、パス回数は多いが、処理圧力が低いため、経時的にインクの粘度が変化し、安定に印字できなくなる場合があり、この方法で得られた分散体よりも、更に分散安定性の良好な分散体が望まれている。 In addition, a method for producing a pigment ink has been proposed in which a mixture containing at least a dispersant and a pigment is dispersed by a liquid-wall collision type high-pressure homogenizer having a single shear line (see, for example, Patent Document 3). This production method greatly improves the dispersion of the pigment. However, with this method, the number of passes is large, but because the processing pressure is low, the viscosity of the ink may change over time, and stable printing may not be possible. The dispersion is further dispersed than the dispersion obtained by this method. A dispersion having good stability is desired.
また、分散剤及び顔料を少なくとも含む混合物を複数のオリフィスを有するチャンバーを通過させ、処理液同士を衝突させて微粒子化する顔料インクの製造法が提案されている(例えば、特許文献4参照)。この製造法により、顔料の分散は大きく改善される。しかし、この方法では、種々の処理圧力及び種々のパス回数での分散処理条件が記載されているが、処理圧力とパス回数の両方を満足する様な条件ではなく、経時的にインクの粘度が変化し、安定に印字できなくなる場合があり、この方法で得られた分散体よりも、更に分散安定性の良好な分散体が望まれている。 In addition, a method for producing a pigment ink is proposed in which a mixture containing at least a dispersant and a pigment is passed through a chamber having a plurality of orifices, and the treatment liquids collide with each other to form fine particles (see, for example, Patent Document 4). This production method greatly improves the dispersion of the pigment. However, in this method, the dispersion processing conditions at various processing pressures and various pass times are described, but this is not a condition that satisfies both the processing pressure and the pass times. The dispersion may change and may not be able to be printed stably, and a dispersion having better dispersion stability than the dispersion obtained by this method is desired.
本発明は、分散安定性に優れ、ヘッドの目詰まりがなく、優れた印字特性(光沢度)を有する水系インクを提供することを課題とする。 An object of the present invention is to provide a water-based ink having excellent dispersion stability, no clogging of the head, and excellent printing characteristics (glossiness).
本発明は、分散媒と、顔料と、水不溶性ポリマーを混合した混合液を高圧ホモジナイザーにより1.2×108 Pa以上の処理圧力でかつ9パス以上の分散処理を行う分散工程を有する水系インクの製造法に関する。 The present invention relates to a water-based ink having a dispersion step in which a mixed solution of a dispersion medium, a pigment, and a water-insoluble polymer is subjected to a dispersion treatment of 9 × or more at a treatment pressure of 1.2 × 10 8 Pa or more by a high-pressure homogenizer. Relates to the manufacturing method.
本発明の製造方法によって得られる水系インクは、分散安定性に優れ、更にヘッドの目詰まりがなく、優れた印字特性(光沢度)を有するという効果を奏する。 The water-based ink obtained by the production method of the present invention is excellent in dispersion stability, has no clogging of the head, and has excellent printing characteristics (glossiness).
顔料は、無機顔料及び有機顔料のいずれであってもよい。また、必要により、この顔料と体質顔料とを併用することもできる。 The pigment may be either an inorganic pigment or an organic pigment. Moreover, this pigment and extender can also be used together as needed.
無機顔料としては、カーボンブラック、金属酸化物、金属硫化物、金属塩化物等が挙げられる。これらの中では、特に黒色系インクでは、カーボンブラックが好ましい。カーボンブラックとしては、ファーネスブラック、サーマルブラック、アセチレンブラック、チャンネルブラック等が挙げられる。 Examples of the inorganic pigment include carbon black, metal oxide, metal sulfide, and metal chloride. Among these, carbon black is particularly preferable for black ink. Examples of carbon black include furnace black, thermal black, acetylene black, and channel black.
有機顔料としては、アゾ顔料、ジアゾ顔料、フタロシアニン顔料、キナクリドン顔料、イソインドリノン顔料、ジオキサジン顔料、ペリレン顔料、ペリノン顔料、チオインジゴ顔料、アンソラキノン顔料、キノフタノン顔料等が挙げられる。
体質顔料としては、シリカ、炭酸カルシウム、タルク等が挙げられる。
Examples of organic pigments include azo pigments, diazo pigments, phthalocyanine pigments, quinacridone pigments, isoindolinone pigments, dioxazine pigments, perylene pigments, perinone pigments, thioindigo pigments, anthoraquinone pigments, and quinophthalone pigments.
Examples of extender pigments include silica, calcium carbonate, and talc.
分散媒は、水を必須とし、水単独であってもよく、あるいは水と有機溶媒とを併用してもよい。
有機溶媒の中では、アルコール系溶媒、ケトン系溶媒、エーテル系溶媒、芳香族炭化水素系溶媒、脂肪族炭化水素系溶媒及びハロゲン化脂肪族炭化水素系溶媒が好ましい。
The dispersion medium requires water and may be water alone, or water and an organic solvent may be used in combination.
Among organic solvents, alcohol solvents, ketone solvents, ether solvents, aromatic hydrocarbon solvents, aliphatic hydrocarbon solvents, and halogenated aliphatic hydrocarbon solvents are preferable.
アルコール系溶媒としては、例えば、メタノール、エタノール、イソプロパノール、n−ブタノール、第3級ブタノール、イソブタノール、ジアセトンアルコール等が挙げられる。ケトン系溶媒としては、例えば、アセトン、メチルエチルケトン、ジエチルケトン、メチルイソブチルケトン等が挙げられる。エーテル系溶媒としては、例えば、ジブチルエーテル、テトラヒドロフラン、ジオキサン等が挙げられる。芳香族炭化水素系溶媒としては、例えば、ベンゼン、トルエン等が挙げられる。脂肪族炭化水素系溶媒としては、例えば、ヘプタン、ヘキサン、シクロヘキサン等が挙げられ。ハロゲン化脂肪族炭化水素系溶媒としては、例えば、塩化メチレン、1,1,1 −トリクロロエタン、クロロホルム、四塩化炭素、1,2 −ジクロロエタン等が挙げられる。これらの有機溶媒の中では、イソプロパノール、アセトン及びメチルエチルケトンが好ましい。 Examples of the alcohol solvent include methanol, ethanol, isopropanol, n-butanol, tertiary butanol, isobutanol, diacetone alcohol and the like. Examples of the ketone solvent include acetone, methyl ethyl ketone, diethyl ketone, and methyl isobutyl ketone. Examples of the ether solvent include dibutyl ether, tetrahydrofuran, dioxane and the like. Examples of the aromatic hydrocarbon solvent include benzene and toluene. Examples of the aliphatic hydrocarbon solvent include heptane, hexane, cyclohexane and the like. Examples of the halogenated aliphatic hydrocarbon solvent include methylene chloride, 1,1,1-trichloroethane, chloroform, carbon tetrachloride, 1,2-dichloroethane, and the like. Of these organic solvents, isopropanol, acetone and methyl ethyl ketone are preferred.
水不溶性ポリマーとしては、水不溶性の、ビニル系ポリマー、ポリエステル系ポリマー、ポリウレタン系ポリマー等が挙げられる。これらの水不溶性ポリマーの中では、水不溶性ビニル系ポリマーが好ましい。水不溶性ビニル系ポリマーとしては、スチレン、(メタ)アクリル酸、(メタ)アクリル酸エステル及び(メタ)アクリル酸アミドからなる群より選ばれた1種以上のモノマーの重合体が挙げられる。 Examples of water-insoluble polymers include water-insoluble vinyl polymers, polyester polymers, polyurethane polymers, and the like. Among these water-insoluble polymers, water-insoluble vinyl polymers are preferable. Examples of the water-insoluble vinyl polymer include a polymer of one or more monomers selected from the group consisting of styrene, (meth) acrylic acid, (meth) acrylic acid ester, and (meth) acrylic acid amide.
水不溶性ポリマーの重量平均分子量は、吐出性、プリンタヘッドの焦げ付きの防止、印刷後のインクの耐久性及び溶液又は分散液の安定性の観点から、3000〜200000、好ましくは10000〜100000であることが望ましい。 The weight average molecular weight of the water-insoluble polymer is 3000 to 200,000, preferably 10,000 to 100,000, from the viewpoints of ejection properties, prevention of scorching of the printer head, durability of the ink after printing, and stability of the solution or dispersion. Is desirable.
なお、水不溶性ポリマーは、塩生成基を有し、さらに中和剤で中和されていることが分散安定性の観点から好ましい。 The water-insoluble polymer preferably has a salt-forming group and is further neutralized with a neutralizing agent from the viewpoint of dispersion stability.
中和剤として、塩生成基の種類に応じて酸又は塩基を使用することができる。酸としては、塩酸、硫酸等の無機酸、及び酢酸、プロピオン酸、乳酸、コハク酸、グリコール酸、グルコン酸、グリセリン酸、ポリエチレングリコール酸等の有機酸が挙げられる。塩基としては、トリメチルアミン、トリエチルアミン等の3級アミン類、アンモニア、水酸化ナトリウム、水酸化カリウム等が挙げられる。 As the neutralizing agent, an acid or a base can be used depending on the type of the salt-forming group. Examples of the acid include inorganic acids such as hydrochloric acid and sulfuric acid, and organic acids such as acetic acid, propionic acid, lactic acid, succinic acid, glycolic acid, gluconic acid, glyceric acid, and polyethylene glycol acid. Examples of the base include tertiary amines such as trimethylamine and triethylamine, ammonia, sodium hydroxide, potassium hydroxide and the like.
水不溶性ポリマーの中和度は、特に制限されないが、通常、顔料含有ポリマー粒子の水分散体の液性が中性、例えば、pH4.5〜10となるように調整することが好ましい。 The degree of neutralization of the water-insoluble polymer is not particularly limited, but it is usually preferable to adjust the aqueous dispersion of pigment-containing polymer particles to be neutral, for example, pH 4.5-10.
水不溶性ポリマーの量は、印字濃度及び吐出安定性の観点から、顔料100重量部に対して、5〜400重量部、好ましくは10〜150重量部であることが望ましい。 The amount of the water-insoluble polymer is 5 to 400 parts by weight, preferably 10 to 150 parts by weight, with respect to 100 parts by weight of the pigment, from the viewpoint of printing density and ejection stability.
また、分散媒の量は、混合物の粘度の観点から、顔料と水不溶性ポリマーとの合計量100重量部に対して、100〜2000重量部、好ましくは150〜1000重量部であることが望ましい。 Further, the amount of the dispersion medium is 100 to 2000 parts by weight, preferably 150 to 1000 parts by weight with respect to 100 parts by weight of the total amount of the pigment and the water-insoluble polymer, from the viewpoint of the viscosity of the mixture.
本発明においては、まず、分散媒と、顔料と、水不溶性ポリマーとを混合する。これらの成分の混合の程度には特に限定がなく、これらの成分が単に混ざり合っていてもよく、あるいは均一な組成となるように混合されていてもよい。 In the present invention, first, a dispersion medium, a pigment, and a water-insoluble polymer are mixed. The degree of mixing of these components is not particularly limited, and these components may be simply mixed or may be mixed so as to have a uniform composition.
混合の際には、プロペラ式攪拌装置等の通常の混合撹拌装置を用いることができる。混合撹拌装置の中では、ディスパー等の高速撹拌混合装置が好ましい。 In mixing, a normal mixing and stirring device such as a propeller type stirring device can be used. Among the mixing and stirring devices, a high-speed stirring and mixing device such as a disper is preferable.
次に、分散媒と、顔料と、水不溶性ポリマーとの混合物は分散工程に供される。この分散工程では、顔料及び水不溶性ポリマーを分散媒中に分散させる。分散工程では、高圧ホモジナナイザーを使用する。高圧ホモジナイザーとして、高圧ホモゲナイザー〔(株)イズミフードマシナリ製、商品名〕、ミニラボ8.3H型〔ラニー(Rannie)社製、商品名〕に代表されるホモバルブ式の高圧ホモジナイザー、マイクロフルイダイザー〔マイクロフルイディクス(Microfluidics)社製、商品名〕、ナノマイザー〔ナノマイザー(株)製、商品名〕、アルティマイザー〔スギノマシン(株)製、商品名〕、ジーナスPY〔白水化学(株)製、商品名〕、DeBEE2000〔日本ビーイーイー(株)製、商品名〕等のチャンバー式の高圧ホモジナイザー等が挙げられる。これらの中では、作業性及び高せん断応力が容易に得られる観点から、チャンバー式の高圧ホモジナイザーがより好ましい。 Next, the mixture of the dispersion medium, the pigment, and the water-insoluble polymer is subjected to a dispersion step. In this dispersion step, the pigment and the water-insoluble polymer are dispersed in the dispersion medium. In the dispersion step, a high pressure homogenizer is used. As a high-pressure homogenizer, a high-pressure homogenizer represented by a high-pressure homogenizer [manufactured by Izumi Food Machinery Co., Ltd., trade name], Minilab 8.3H type (manufactured by Rannie, trade name), a microfluidizer [Micro Product name], Nanomizer [product name made by Nanomizer Co., Ltd.], Optimizer [Product name made by Sugino Machine Co., Ltd.], Genus PY [Product name made by Hakusui Chemical Co., Ltd., trade name] ], A chamber-type high-pressure homogenizer such as DeBEE2000 (trade name, manufactured by Nippon BEE Co., Ltd.) and the like. Among these, a chamber-type high-pressure homogenizer is more preferable from the viewpoint of easy workability and high shear stress.
チャンバー式高圧ホモジナイザーに用いられる分散チャンバーとして、液−液衝突型チャンバーと液−壁衝突型チャンバーとが知られている。 Liquid-liquid collision type chambers and liquid-wall collision type chambers are known as dispersion chambers used in chamber-type high-pressure homogenizers.
液−液衝突型チャンバーの一例を図1に示す。図1に示されているように、液−液衝突型チャンバーは、複数の液体の流入管路1、流入管路と同じ数のせん断管路2及び単一の流出管路3が順次連結され、複数のせん断管路の流出管路に近い方の端が1カ所で接続されており、該接続箇所での液体流同士の衝突で分散させるものである。
An example of a liquid-liquid collision type chamber is shown in FIG. As shown in FIG. 1, in the liquid-liquid collision type chamber, a plurality of
次に、液−壁衝突型チャンバーの一例を図2に示す。図2に示されている液−壁衝突形チャンバーは、各々単一の、液体の流入管路1、せん断管路2及び流出管路が順次連結され、せん断管路と流出管路のなす角度が通常45〜135度であり、せん断管路3の液体流を流出管路の内壁に衝突させるものである。液−壁衝突型チャンバーは、チャンバーの構造が単純なことから、チャンバー内での処理液の目詰まりが少なく、チャンバーの寿命が延びるという利点を有する。また、液−壁衝突型チャンバーの他の例を図3に示す。図3に示されている液−壁衝突型チャンバーは、単一の流入管路1、複数のせん断管路2及び単一の流出管路が順次連結されているものであり、大量の液体を処理する場合に好適である。
Next, an example of a liquid-wall collision type chamber is shown in FIG. In the liquid-wall collision type chamber shown in FIG. 2, a single
分散処理圧力及びパス回数は、分散体の分散安定性の観点から分散処理圧力は、120×106 Pa以上でかつパス回数は9パス以上である。なお、分散処理圧力は、150×106 Pa以上がより好ましい。また、上限は分散体の耐久性観点から250×106 Pa以下が好ましく、220×106 Pa以下がより好ましい。一方、パス回数の上限は分散体の耐久性や生産性の観点から50パス以下であり、好ましくは40パス以下、より好ましくはくは20パス以下である。 From the viewpoint of dispersion stability of the dispersion, the dispersion treatment pressure and the number of passes are 120 × 10 6 Pa or more and the number of passes is 9 or more. The dispersion treatment pressure is more preferably 150 × 10 6 Pa or more. Further, the upper limit is preferably 250 × 10 6 Pa or less, more preferably 220 × 10 6 Pa or less, from the viewpoint of durability of the dispersion. On the other hand, the upper limit of the number of passes is 50 passes or less from the viewpoint of the durability and productivity of the dispersion, preferably 40 passes or less, more preferably 20 passes or less.
分散処理における分散液のパス方法としては、例えば、図4に示されるように、単一の分散槽Aと高圧ホモジナイザーを用いて、分散液を循環させて処理する方法(パス回数は〔高圧ホモジナイザーを通過した分散液体積〕÷〔分散処理した分散液体積〕で算出する)、図5に示されるように、高圧ホモジナイザーと複数の分散槽A及びBを用いて、分散槽Aの分散液を高圧ホモジナイザー処理した後、別の分散槽Bへ入れ、一旦、分散槽Aの分散液の全量を処理した後、同様の処理を分散槽Bから分散槽A、次いで分散槽Aから分散槽Bへと分散液を移動させる処理繰り返して行う方法(以下、キャッチボール方式という)等が挙げられる。これらの方法の中では、キャッチボール方式が、効率的に処理をすることができる観点から好ましい。 For example, as shown in FIG. 4, the dispersion liquid passing method in the dispersion treatment is a method in which the dispersion liquid is circulated using a single dispersion tank A and a high-pressure homogenizer (the number of passes is [high-pressure homogenizer]. The volume of the dispersion liquid that has passed through the liquid is divided by the volume of the dispersion liquid that has been subjected to the dispersion treatment), and the dispersion liquid in the dispersion tank A is obtained using a high-pressure homogenizer and a plurality of dispersion tanks A and B, as shown in FIG. After the high-pressure homogenizer treatment, it is put into another dispersion tank B and once the entire amount of the dispersion liquid in the dispersion tank A is treated, the same treatment is performed from the dispersion tank B to the dispersion tank A, and then from the dispersion tank A to the dispersion tank B. And a method of repeatedly performing the process of moving the dispersion (hereinafter referred to as a catch ball method). Among these methods, the catch ball method is preferable from the viewpoint of efficient processing.
分散処理中の分散液の温度は、分散液の増粘を抑制し、安定した分散液を得る観点から、好ましくは5℃以上、より好ましくは10℃以上であり、また凝集を抑制し、分散安定性の良好な分散体を得る観点から、好ましくは50℃以下、より好ましくは30℃以下である。これらの観点から、分散処理中の分散液の温度は、5〜50℃が好ましく、10〜30℃がより好ましい。 The temperature of the dispersion during the dispersion treatment is preferably 5 ° C. or more, more preferably 10 ° C. or more from the viewpoint of suppressing the thickening of the dispersion and obtaining a stable dispersion, and also suppressing aggregation and dispersion. From the viewpoint of obtaining a dispersion having good stability, it is preferably 50 ° C. or lower, more preferably 30 ° C. or lower. From these viewpoints, the temperature of the dispersion during the dispersion treatment is preferably 5 to 50 ° C, and more preferably 10 to 30 ° C.
なお、分散工程において高圧ホモジナイザーを用いる場合、流路径の異なる複数の高圧ホモジナイザーを用いて、まず流路径の大きい高圧ホモジナイザーで1パス以上分散処理した後、流路径の小さい高圧ホモジナイザーで処理することもできる。このような方法を用いることにより、流路径の小さい高圧ホモジナイザーの流路の閉塞を防止することができる。 When a high-pressure homogenizer is used in the dispersion step, a plurality of high-pressure homogenizers having different flow path diameters may be used to first disperse one or more passes with a high-pressure homogenizer with a large flow path diameter and then with a high-pressure homogenizer with a small flow path diameter. it can. By using such a method, blockage of the flow path of the high-pressure homogenizer having a small flow path diameter can be prevented.
以上のようにして、分散媒と、顔料と、水不溶性ポリマーを混合した混合液を高圧ホモジナイザーにより120×106 Pa以上の処理圧力でかつ9パス以上の分散処理で分散させることにより、顔料及びポリマーが微細化され、所望の平均粒子径を有する顔料含有ポリマー粒子の分散体得ることができる。 As described above, the dispersion liquid, the pigment, and the mixed liquid of the water-insoluble polymer are dispersed by a high-pressure homogenizer at a treatment pressure of 120 × 10 6 Pa or more and a dispersion treatment of 9 or more passes, whereby the pigment and The polymer is refined and a dispersion of pigment-containing polymer particles having a desired average particle size can be obtained.
なお、顔料含有ポリマー粒子の平均粒子径は、分散安定性及び印字特性の観点から、0.05〜1μmが好ましく、0.05〜0.2μmがより好ましい。平均粒子径は、レーザー粒子解析システム〔大塚電子(株)製、ELS−8000〕によって測定したときの値である。 The average particle size of the pigment-containing polymer particles is preferably 0.05 to 1 μm, more preferably 0.05 to 0.2 μm, from the viewpoint of dispersion stability and printing characteristics. The average particle diameter is a value measured by a laser particle analysis system [ELS-8000, manufactured by Otsuka Electronics Co., Ltd.].
顔料含有ポリマー粒子の水分散体に有機溶媒が含まれている場合には、減圧蒸留等により、有機溶媒を除去して水系とすることができる。 When the organic dispersion is contained in the aqueous dispersion of the pigment-containing polymer particles, the organic solvent can be removed to obtain an aqueous system by vacuum distillation or the like.
次に、顔料含有ポリマー粒子の水分散体に、必要に応じて湿潤剤、分散剤、消泡剤、キレート剤、防黴剤等の添加剤を適量で添加することにより、水系インクを得ることができる。 Next, an aqueous ink is obtained by adding an appropriate amount of additives such as a wetting agent, a dispersing agent, an antifoaming agent, a chelating agent, and an antifungal agent to the aqueous dispersion of the pigment-containing polymer particles as necessary. Can do.
また、必要に応じて、湿潤剤、分散剤、消泡剤、キレート剤、防黴剤等の添加剤を添加することができる。 If necessary, additives such as a wetting agent, a dispersing agent, an antifoaming agent, a chelating agent, and an antifungal agent can be added.
製造例1
反応容器内に、メチルエチルケトン20重量部及び重合連鎖移動剤(2- メルカプトエタノール)0.03 重量部を入れ、モノマーとして、スチレンマクロマー〔東亜合成(株)製、商品名:AS-6S、数平均分子量:6000 、重合性官能基:メタクロイルオキシ基〕10重量部、ポリエチレングリコールモノメタクリレート〔エチレンオキシド9モル付加、新中村化学(株)製、商品名:NK エステルM-90G 〕10重量部、ポリプロピレングリコールモノメタクリレート〔アルドリッチジャパン(株)製、数平均分子量:375〕10重量部、メタクリル酸12重量部及びスチレンモノマー58重量部のそれぞれの10重量%ずつを入れて混合し、窒素ガス置換を十分に行い、混合溶液を得た。
Production Example 1
In a reaction vessel, 20 parts by weight of methyl ethyl ketone and 0.03 part by weight of a polymerization chain transfer agent (2-mercaptoethanol) were added, and as a monomer, styrene macromer [manufactured by Toagosei Co., Ltd., trade name: AS-6S, number average molecular weight: 6000, polymerizable functional group: methacryloyloxy group] 10 parts by weight, polyethylene glycol monomethacrylate [addition of 9 moles of ethylene oxide, manufactured by Shin-Nakamura Chemical Co., Ltd., trade name: NK ester M-90G], 10 parts by weight, polypropylene glycol mono 10 parts by weight of each of methacrylate (Aldrich Japan Co., Ltd., number average molecular weight: 375) 10 parts by weight, 12 parts by weight of methacrylic acid and 58 parts by weight of styrene monomer were mixed and thoroughly replaced with nitrogen gas. A mixed solution was obtained.
一方、滴下ロートに、前記各モノマーの残りの90重量%の量を仕込み、重合連鎖移動剤(2- メルカプトエタノール)0.27 重量部、メチルエチルケトン60重量部及び2,2'- アゾビス(2,4- ジメチルバレロニトリル)1.2重量部を入れて混合し、十分に窒素ガス置換を行い、混合溶液を得た。 On the other hand, the remaining 90% by weight of each monomer was charged into a dropping funnel and 0.27 parts by weight of a polymerization chain transfer agent (2-mercaptoethanol), 60 parts by weight of methyl ethyl ketone and 2,2′-azobis (2,4- Dimethylvaleronitrile) 1.2 parts by weight was added and mixed, and nitrogen gas substitution was sufficiently performed to obtain a mixed solution.
窒素雰囲気下、反応容器内の混合溶液を攪拌しながら65℃まで昇温し、滴下ロート中の混合溶液を3時間かけて徐々に滴下した。滴下終了から65℃で2時間経過後、2,2'- アゾビス(2,4- ジメチルバレロニトリル)0.3重量部をメチルエチルケトン5重量部に溶解した溶液を加え、更に65℃で2時間、70℃で2時間熟成させた後、メチルエチルケトン135 重量部を加えて濃度を調整し、ポリマー溶液(以下、ポリマーAという)を得た。 Under a nitrogen atmosphere, the mixed solution in the reaction vessel was heated to 65 ° C. while stirring, and the mixed solution in the dropping funnel was gradually added dropwise over 3 hours. After 2 hours at 65 ° C from the end of the dropwise addition, a solution of 0.3 parts by weight of 2,2'-azobis (2,4-dimethylvaleronitrile) in 5 parts by weight of methyl ethyl ketone was added, and further at 65 ° C for 2 hours, 70 ° C. Then, 135 parts by weight of methyl ethyl ketone was added to adjust the concentration to obtain a polymer solution (hereinafter referred to as polymer A).
得られたポリマー溶液の一部を、減圧下、105 ℃で2時間乾燥させ、溶媒を除去することによって単離した。得られた塩生成基を有する水不溶性ポリマーの重量平均分子量を測定したところ、74000 であった。 A portion of the resulting polymer solution was isolated by drying at 105 ° C. under reduced pressure for 2 hours and removing the solvent. The weight average molecular weight of the obtained water-insoluble polymer having a salt-forming group was measured and found to be 74000.
〔シアン色材〕
実施例1
ポリマーA4. 8重量部に、5規定の水酸化ナトリウム水溶液0. 48重量部、メチルエチルケトン1 .5重量部、イオン交換水7. 6重量部、銅フタロシアニン顔料〔大日本インキ化学工業(株)製、商品名:TGR−SD〕2. 5重量部を添加し、ディスパー槽内で3時間混合した。
[Cyan color material]
Example 1
4.8 parts by weight of Polymer A, 0.48 parts by weight of 5N aqueous sodium hydroxide solution, 1.5 parts by weight of methyl ethyl ketone, 7.6 parts by weight of ion-exchanged water, copper phthalocyanine pigment [manufactured by Dainippon Ink & Chemicals, Inc. , Trade name: TGR-SD] 2.5 parts by weight were added and mixed in a disper tank for 3 hours.
得られた混合液をチャンバー式の高圧ホモジナイザー〔マイクロフルイディクス社製、商品名:マイクロフルイダイザーM−210C、Z型チャンバー(液−壁衝突型チャンバー)〕を用い、以下の条件で分散体を得た。
・処理圧力:180×106 Pa
・パス回数:10パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
The obtained mixed liquid was subjected to dispersion under the following conditions using a chamber-type high-pressure homogenizer [manufactured by Microfluidics, trade name: Microfluidizer M-210C, Z-type chamber (liquid-wall collision type chamber)]. Obtained.
・ Processing pressure: 180 × 10 6 Pa
・ Number of passes: 10 passes (catch ball method)
-Chamber orifice diameter: 87 μm
実施例2
パス回数を20パスとした以外は、実施例1と同じ様に処理した。
・処理圧力:180×106 Pa
・パス回数:20パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
Example 2
Processing was performed in the same manner as in Example 1 except that the number of passes was 20 passes.
・ Processing pressure: 180 × 10 6 Pa
・ Number of passes: 20 passes (catch ball method)
-Chamber orifice diameter: 87 μm
実施例3
パス回数を30パスとした以外は、実施例1と同じ様に処理した。
・処理圧力:180×106 Pa
・パス回数:30パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
Example 3
Processing was performed in the same manner as in Example 1 except that the number of passes was 30.
・ Processing pressure: 180 × 10 6 Pa
-Number of passes: 30 passes (catch ball method)
-Chamber orifice diameter: 87 μm
比較例1
パス回数を3パスで処理した以外は、実施例1と同様にして処理した。
Comparative Example 1
Processing was performed in the same manner as in Example 1 except that the number of passes was processed in 3 passes.
実施例1〜3及び比較例1それぞれ得られた分散体に、イオン交換水35重量部を加え、撹拌した後、減圧下で60℃でメチルエチルケトンを除去し、更に一部の水を除去することにより、固形分濃度が25重量%の顔料含有ポリマー粒子の水分散体を得た。 To each of the dispersions obtained in Examples 1 to 3 and Comparative Example 1, 35 parts by weight of ion exchange water was added and stirred, and then methyl ethyl ketone was removed at 60 ° C. under reduced pressure, and a part of the water was further removed. Thus, an aqueous dispersion of pigment-containing polymer particles having a solid content concentration of 25% by weight was obtained.
それぞれ得られた顔料含有ポリマー粒子の分散体30重量部、グリセリン10重量部、プロピレングリコールモノブチルエーテル7重量部、サーフィノール465〔エアプロダクツジャパン(株)製、商品名〕0. 3重量部及びイオン交換水52. 7重量部を混合し、得られた混合液を0. 5μmのフィルター〔アセチルセルロース膜、外径:2. 5cm、富士写真フィルム(株)製〕を取り付けた容量25mLの針なしシリンジ〔テルモ(株)製〕で濾過し、粗大粒子を除去し、水系インクを得た。
得られた水系インクについて、分散安定性を調べた。その結果を表1に示す。
30 parts by weight of the pigment-containing polymer particle dispersion obtained, 10 parts by weight of glycerin, 7 parts by weight of propylene glycol monobutyl ether, Surfynol 465 (trade name, manufactured by Air Products Japan Ltd.), 0.3 parts by weight and ions 52.7 parts by weight of exchange water was mixed, and the resulting mixture was mixed with a 0.5 μm filter (acetylcellulose membrane, outer diameter: 2.5 cm, manufactured by Fuji Photo Film Co., Ltd.) with a capacity of 25 mL without a needle. Filtration was performed with a syringe [manufactured by Terumo Corporation] to remove coarse particles to obtain a water-based ink.
The dispersion stability of the obtained water-based ink was examined. The results are shown in Table 1.
〔マゼンタ色材〕
実施例4
ポリマーA1. 5重量部に、5規定の水酸化ナトリウム水溶液0. 17重量部及びイオン交換水1. 0重量部を添加し、ディスパー翼で30分間混合した後、容量10Lの加圧式ニーダー〔(株)モリヤマ製〕に仕込んだ。
[Magenta color material]
Example 4
To 1.5 parts by weight of Polymer A, 0.17 part by weight of 5N sodium hydroxide aqueous solution and 1.0 part by weight of ion-exchanged water were added and mixed for 30 minutes with a disperser blade. Made by Moriyama Co., Ltd.].
次に、キナクリドン顔料〔大日本インキ化学工業(株)、商品名:ファストゲンスーパーマゼンタRG〕3. 0重量部をこれに加えた。その際の固形分濃度は、67重量%であった。 Next, 3.0 parts by weight of quinacridone pigment [Dainippon Ink Chemical Co., Ltd., trade name: Fastgen Super Magenta RG] was added thereto. The solid content concentration at that time was 67% by weight.
このニーダーに蓋をし、密閉状態にして、ジャケットに1℃の冷却水を流し、25℃で2時間混練して混練物を得た。混練物1kgあたりの積算動力値は、0. 8kWhであった。 The kneader was covered and sealed, and 1 ° C. cooling water was passed through the jacket and kneaded at 25 ° C. for 2 hours to obtain a kneaded product. The integrated power value per kg of the kneaded material was 0.8 kWh.
得られた混練物5. 6重量部に、イオン交換水2. 2重量部を加えながら、3本ロールミルで混練した後、イオン交換水7. 2重量部を加えて希釈した。 The resulting kneaded product was kneaded with a three-roll mill while adding 2.2 parts by weight of ion-exchanged water to 5.6 parts by weight, and then diluted by adding 7.2 parts by weight of ion-exchanged water.
得られた混練物の希釈液をチャンバー式の高圧ホモジナイザー(マイクロフルイディクス社製、商品名:マイクロフルイダイザーM−210C、Z型チャンバー)を用い、以下の条件で分散体を得た。
・処理圧力:200×106 Pa
・パス回数:10パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
A dispersion was obtained by using a chamber-type high-pressure homogenizer (trade name: Microfluidizer M-210C, Z-type chamber) manufactured by a chamber type high-pressure homogenizer.
・ Processing pressure: 200 × 10 6 Pa
・ Number of passes: 10 passes (catch ball method)
-Chamber orifice diameter: 87 μm
実施例5
実施例4において、パス回数を20パスとした以外は、実施例4と同じ様に処理した。
・処理圧力:200×106 Pa
・パス回数:20パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
Example 5
In Example 4, the same process as in Example 4 was performed except that the number of passes was 20 passes.
・ Processing pressure: 200 × 10 6 Pa
・ Number of passes: 20 passes (catch ball method)
-Chamber orifice diameter: 87 μm
比較例2
実施例4において、パス回数を5パスとした以外は、実施例4と同じ様に処理した。
・処理圧力:200×106 Pa
・パス回数:5パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
Comparative Example 2
In Example 4, the process was performed in the same manner as in Example 4 except that the number of passes was 5 passes.
・ Processing pressure: 200 × 10 6 Pa
-Number of passes: 5 passes (catch ball method)
-Chamber orifice diameter: 87 μm
実施例4、5及び比較例2により、それぞれ得られた水分散体に、イオン交換水15重量部加え、撹拌した後、減圧下で60℃でメチルエチルケトンを除去し、更に一部の水を除去することにより、固形分濃度が20重量%の顔料含有ポリマー粒子の水分散体を得た。 After adding 15 parts by weight of ion-exchanged water to each of the aqueous dispersions obtained in Examples 4 and 5 and Comparative Example 2 and stirring, methyl ethyl ketone was removed at 60 ° C. under reduced pressure, and a part of the water was removed. As a result, an aqueous dispersion of pigment-containing polymer particles having a solid content concentration of 20% by weight was obtained.
それぞれ得られた顔料含有ポリマー粒子の分散体30重量部、グリセリン10重量部、プロピレングリコールモノブチルエーテル7重量部、サーフィノール465〔エアプロダクツジャパン(株)製、商品名〕0. 3重量部及びイオン交換水52. 7重量部を混合し、得られた混合液を0. 5μmのフィルター〔アセチルセルロース膜、外径:2. 5cm、富士写真フィルム(株)製〕を取り付けた容量25mLの針なしシリンジ〔テルモ(株)製〕で濾過し、粗大粒子を除去し、水系インクを得た。
得られた水系インクについて、分散安定性を調べた。その結果を表1に示す。
30 parts by weight of the pigment-containing polymer particle dispersion obtained, 10 parts by weight of glycerin, 7 parts by weight of propylene glycol monobutyl ether, Surfynol 465 (trade name, manufactured by Air Products Japan Ltd.), 0.3 parts by weight and ions 52.7 parts by weight of exchange water was mixed, and the resulting mixture was mixed with a 0.5 μm filter (acetylcellulose membrane, outer diameter: 2.5 cm, manufactured by Fuji Photo Film Co., Ltd.) with a capacity of 25 mL without a needle. Filtration was performed with a syringe [manufactured by Terumo Corporation] to remove coarse particles to obtain a water-based ink.
The dispersion stability of the obtained water-based ink was examined. The results are shown in Table 1.
(イエロー色材)
実施例6
ポリマーA160重量部に、5規定の水酸化ナトリウム水溶液0. 48重量部、メチルエチルケトン11重量部、イオン交換水407重量部及びピグメントイエロー顔料〔大日本精化(株)、商品名:ファーストエロー031〕144重量部を添加し、ディスパー槽内で1.5時間混合した。
(Yellow color material)
Example 6
Polymer A (160 parts by weight), 5N sodium hydroxide aqueous solution (0.48 parts by weight), methyl ethyl ketone (11 parts by weight), ion-exchanged water (407 parts by weight) and pigment yellow pigment (Dainippon Seika Co., Ltd., trade name: First Yellow 031) 144 parts by weight was added and mixed for 1.5 hours in a disper tank.
得られた混合液をチャンバー式の高圧ホモジナイザー(マイクロフルイディクス社製、商品名:マイクロフルイダイザーM−210C、Z型チャンバー)で、予めオリフィス径の大きい(φ550μm)Z型チャンバーで処理圧力:50×106 Pa、パス回数:2パス(キャッチボール方式)で処理された予備高圧分散体を、さらに以下の条件による本分散で分散体を得た。
・処理圧力:150×106 Pa
・パス回数:10パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
The obtained mixed solution was treated with a chamber type high-pressure homogenizer (trade name: Microfluidizer M-210C, Z-type chamber) manufactured by Microfluidics, Inc. in a Z-type chamber with a large orifice diameter (φ550 μm) in advance. × 10 6 Pa, number of passes: A preliminary high-pressure dispersion treated by 2 passes (catch ball method) was further obtained by this dispersion under the following conditions.
・ Processing pressure: 150 × 10 6 Pa
・ Number of passes: 10 passes (catch ball method)
-Chamber orifice diameter: 87 μm
実施例7
パス回数を20パスとした以外は、実施例6と同じ様に処理した。
・処理圧力:150×106 Pa
・パス回数:20パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
Example 7
Processing was performed in the same manner as in Example 6 except that the number of passes was 20 passes.
・ Processing pressure: 150 × 10 6 Pa
・ Number of passes: 20 passes (catch ball method)
-Chamber orifice diameter: 87 μm
比較例3
パス回数を7パスとした以外は、実施例6と同じ様に処理した。
・処理圧力:150×106 Pa
・パス回数:7パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
Comparative Example 3
Processing was performed in the same manner as in Example 6 except that the number of passes was 7 passes.
・ Processing pressure: 150 × 10 6 Pa
-Number of passes: 7 passes (catch ball method)
-Chamber orifice diameter: 87 μm
比較例4
パス回数を10パス、分散圧力を100×106 Paとした以外は、実施例6と同じ様に処理した。
・処理圧力:100×106 Pa
・パス回数:10パス(キャッチボール方式)
・チャンバーオリフィス径:87μm
Comparative Example 4
The treatment was performed in the same manner as in Example 6 except that the number of passes was 10 and the dispersion pressure was 100 × 10 6 Pa.
・ Processing pressure: 100 × 10 6 Pa
・ Number of passes: 10 passes (catch ball method)
-Chamber orifice diameter: 87 μm
実施例6〜7及び比較例3〜4で得られた各分散体に、イオン交換水240重量部を加え、撹拌した後、減圧下で60℃でメチルエチルケトンを除去し、更に一部の水を除去することにより、固形分濃度が20重量%の顔料含有ポリマー粒子の分散体を得た。 To each of the dispersions obtained in Examples 6 to 7 and Comparative Examples 3 to 4, 240 parts by weight of ion-exchanged water was added and stirred, and then methyl ethyl ketone was removed at 60 ° C. under reduced pressure. By removing, a dispersion of pigment-containing polymer particles having a solid content concentration of 20% by weight was obtained.
それぞれ得られた顔料含有ポリマー粒子の分散体30重量部、グリセリン10重量部、プロピレングリコールモノブチルエーテル7重量部、サーフィノール465〔エアプロダクツジャパン(株)製、商品名〕0. 3重量部及びイオン交換水52. 7重量部を混合し、得られた混合液を0. 5μmのフィルター〔アセチルセルロース膜、外径:2. 5cm、富士写真フィルム(株)製〕を取り付けた容量25mLの針なしシリンジ〔テルモ(株)製〕で濾過し、粗大粒子を除去し、水系インクを得た。 30 parts by weight of the pigment-containing polymer particle dispersion obtained, 10 parts by weight of glycerin, 7 parts by weight of propylene glycol monobutyl ether, Surfynol 465 (trade name, manufactured by Air Products Japan Ltd.), 0.3 parts by weight and ions 52.7 parts by weight of exchange water was mixed, and the resulting mixture was mixed with a 0.5 μm filter (acetylcellulose membrane, outer diameter: 2.5 cm, manufactured by Fuji Photo Film Co., Ltd.) with a capacity of 25 mL without a needle. Filtration was performed with a syringe [manufactured by Terumo Corporation] to remove coarse particles to obtain a water-based ink.
次に、各実施例及び各比較例で得られた水系インクを、温度70℃で恒温槽に保存し、保存から1日経過後及び30日経過後における各粘度をE型粘度計(ローター:8°34′×R24、20℃)で測定した。水系インクの[粘度保持率]を以下の式に基づいて求め、以下の評価基準にしたがって評価した。その結果を表1に示す。 Next, the water-based inks obtained in each Example and each Comparative Example were stored in a thermostatic bath at a temperature of 70 ° C., and the viscosities after 1 day and 30 days from storage were measured for E-type viscometer (rotor: 8 ° 34 ′ × R24, 20 ° C.). [Viscosity retention] of the water-based ink was determined based on the following formula and evaluated according to the following evaluation criteria. The results are shown in Table 1.
〔粘度保持率〕
=〔(保存30日経過後の粘度)÷(保存1日経過後の粘度)〕×100
[Viscosity retention]
= [(Viscosity after 30 days storage) ÷ (viscosity after 1 day storage)] × 100
〔評価基準〕
○:粘度保持率が90%以上、110%以下
×:粘度保持率が110%を超えるか又は90%未満
〔Evaluation criteria〕
○: Viscosity retention is 90% or more and 110% or less ×: Viscosity retention exceeds 110% or less than 90%
また、実施例4、実施例5及び比較例2で得られた水系インクを用いて、インクジェットプリンター[セイコーエプソン(株)製、型番:EM900C]で、市販のMC光沢紙にベタ印字し、25℃で1時間放置後、光沢度を光沢度計[日本電飾(株)製、商品名:HANDYGLOSSMETER、品番:PG−1]で測定し、以下の基準に基づいて評価した。その結果を表1に示す。 Further, using the water-based ink obtained in Example 4, Example 5 and Comparative Example 2, solid printing was performed on commercially available MC glossy paper with an ink jet printer [Seiko Epson Corporation, model number: EM900C], 25 The glossiness was measured with a gloss meter [manufactured by Nippon Denshoku Co., Ltd., trade name: HANDYGLOSSSMETER, product number: PG-1] after being allowed to stand at 0 ° C. for 1 hour, and evaluated based on the following criteria. The results are shown in Table 1.
〔評価基準〕
○:28以上
△:25以上28未満
×:25未満
〔Evaluation criteria〕
○: 28 or more Δ: 25 or more and less than 28 ×: Less than 25
表1に示された結果から、実施例4及び5で得られたインクジェット記録用水系インクは、いずれも、専用紙を使用した場合に高い光沢の印字が得られ、更には分散安定性にも優れたものであることがわかる。 From the results shown in Table 1, the inkjet recording water-based inks obtained in Examples 4 and 5 both have high gloss prints when using dedicated paper, and also have good dispersion stability. It turns out that it is excellent.
本発明の製造法で得られた水系インクは、例えば、インクジェット記録用水系インク等に好適に使用しうるものである。 The water-based ink obtained by the production method of the present invention can be suitably used for, for example, a water-based ink for inkjet recording.
1 流入管路
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3 流出管路
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JP2002309122A (en) * | 2001-04-16 | 2002-10-23 | Toyo Ink Mfg Co Ltd | Method for manufacturing aqueous pigment dispersion |
JP2003253146A (en) * | 2003-05-08 | 2003-09-10 | Sanyo Shikiso Kk | Pigment for ink jet and pigment dispersion for ink jet obtained using the same |
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JPH05188614A (en) * | 1992-01-13 | 1993-07-30 | Konica Corp | Production of electrophotographic sensitive body |
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