JP6176486B2 - Aqueous pigment dispersion for preparing water-based ink for ink-jet recording and water-based ink for ink-jet recording - Google Patents
Aqueous pigment dispersion for preparing water-based ink for ink-jet recording and water-based ink for ink-jet recording Download PDFInfo
- Publication number
- JP6176486B2 JP6176486B2 JP2013241879A JP2013241879A JP6176486B2 JP 6176486 B2 JP6176486 B2 JP 6176486B2 JP 2013241879 A JP2013241879 A JP 2013241879A JP 2013241879 A JP2013241879 A JP 2013241879A JP 6176486 B2 JP6176486 B2 JP 6176486B2
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- Prior art keywords
- ink
- water
- dispersion
- polyurethane resin
- resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000006185 dispersion Substances 0.000 title claims description 127
- 239000000049 pigment Substances 0.000 title claims description 95
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- 238000002360 preparation method Methods 0.000 claims description 4
- 125000003827 glycol group Chemical group 0.000 claims description 3
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- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
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Landscapes
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Ink Jet (AREA)
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
Description
本発明は、インクジェット記録用水性インク調製のための水性顔料分散液及びインクジェット記録水性インクに関する。 The present invention relates to an aqueous pigment dispersion for preparing an aqueous inkjet recording ink and an aqueous inkjet recording ink.
インクジェット印刷分野では、印字物の堅牢性（耐候性・耐水性）などの項目が近年重要視されている。こうした背景から、色材として顔料が用いられるようになった。一方、顔料インクは耐擦性や光沢性には劣るといった欠点があった。その対策の一つとして、水溶性ウレタン樹脂を添加する方法がある。樹脂を添加することで、印刷メディアと顔料の定着で耐擦性や、印刷面を平滑にすることで光沢を付与することができる。一方、樹脂を添加することで、インクジェット吐出性においては充分な性能を発揮できなくなることであった。特に、吐出停止後、再び吐出した際の吐出速度は重要な特性であるにも関わらず、充分な速度が得られないでいた。 In the ink jet printing field, items such as fastness (weather resistance and water resistance) of printed matter have recently been regarded as important. From this background, pigments have come to be used as coloring materials. On the other hand, the pigment ink has a drawback of being inferior in abrasion resistance and glossiness. One countermeasure is to add a water-soluble urethane resin. By adding a resin, it is possible to impart rubbing resistance by fixing the printing medium and the pigment, and gloss by smoothing the printing surface. On the other hand, the addition of a resin makes it impossible to exhibit sufficient performance in terms of inkjet discharge properties. In particular, the discharge speed when discharging again after stopping the discharge is an important characteristic, but a sufficient speed cannot be obtained.
これらの課題を解決すべく、少なくともカーボンブラックとアミド結合、ウレタン結合を有する高分子と水とならなるインクジェット記録液が提案されている（特許文献１）。しかし、カーボンブラックを主としたインクジェット記録液であり、他のカラー記録液に応用することは難しく、再吐出性が不十分であった。 In order to solve these problems, an inkjet recording liquid comprising at least carbon black and an amide bond, a polymer having a urethane bond and water has been proposed (Patent Document 1). However, it is an ink jet recording liquid mainly composed of carbon black, and it is difficult to apply to other color recording liquids, and re-ejection properties are insufficient.
また、印字濃度、耐摩擦性、耐マーカー性、耐水性、耐光性に優れるインクジェット記録液が提案されているものの、ウレタン樹脂の構成が異なるため、同様に再吐出性が十分ではなかった（特許文献２）。 In addition, although an ink jet recording liquid excellent in print density, friction resistance, marker resistance, water resistance, and light resistance has been proposed, the structure of the urethane resin is different, so that the re-discharge property is not sufficient (patent) Reference 2).
また、（メタ）アクリル酸エステル樹脂とある特定粒子径のポリウレタン樹脂を特徴とする水性顔料分散体を提案されているが、同様にウレタン樹脂の構成がことなっているため、再吐出性が十分ではなかった（特許文献３）。 An aqueous pigment dispersion featuring a (meth) acrylic ester resin and a polyurethane resin with a specific particle size has been proposed, but the urethane resin composition is also different, so re-ejection properties are sufficient. It was not (Patent Document 3).
また、ポリエーテル系ポリウレタン樹脂として、ポリ（オキシテトラメチレン）構造を有することを特徴としたインクジェット記録用水性インクが提案されているが、同様に樹脂の構成成分が異なっている（特許文献４）。 Further, water-based inks for inkjet recording characterized by having a poly (oxytetramethylene) structure have been proposed as polyether-based polyurethane resins, but the constituent components of the resins are also different (Patent Document 4). .
さらに、ポリウレタン系樹脂を含み、ポリウレタンウレア部分の比率を特定し、顔料の分散粒径Ｄ５０が４０〜１００ｎｍであることを特徴とした顔料分散水性記録的が提案されているが、再吐出性に関しては不十分であった（特許文献５）。 Furthermore, a pigment-dispersed aqueous recording method has been proposed that includes a polyurethane-based resin, specifies the ratio of the polyurethane urea portion, and has a pigment dispersed particle diameter D50 of 40 to 100 nm. Was insufficient (Patent Document 5).
そこで、吐出停止後、再び吐出した際の吐出速度の速度低下率が低く、耐擦性や光沢性にも優れ、かつ、分散安定性に優れたインクジェット記録用水性インクが求められている。 Accordingly, there is a need for a water-based ink for ink jet recording that has a low rate of reduction in discharge speed when discharged again after stopping discharge, is excellent in abrasion resistance and glossiness, and is excellent in dispersion stability.
本発明は、モノカラー印字およびフルカラー印字においても、吐出停止後、再び吐出した際の吐出速度の速度低下率が低く、着弾ズレが無く、連続吐出時の吐出速度が速い上に吐出速度が安定しているインクジェット記録用水性インク、ひいてはそれを簡便に調整し得る水性顔料分散液を提供することを目的とする。 In the present invention, even in mono-color printing and full-color printing, the rate of decrease in the ejection speed when ejection is stopped after ejection is low, there is no landing deviation, the ejection speed during continuous ejection is high, and the ejection speed is stable It is an object of the present invention to provide a water-based ink for inkjet recording, and thus an aqueous pigment dispersion that can be easily adjusted.
本発明者らは、前記実状に鑑みて鋭意検討した結果、スチレン−アクリル樹脂で分散した水性顔料分散液とポリプロピレングリコールから構成されるポリウレタン樹脂粒子分散体からなるインクジェット記録用水性インク調整のための水性顔料分散体を用いることで、吐出停止後、再び吐出した際の吐出速度の速度低下率が低く、着弾ズレが無く、連続吐出時の吐出速度が速い上に吐出速度が安定しているインクジェット記録用水性インクを提供できることを見出し、本発明を完成するに至った。 As a result of intensive studies in view of the above-mentioned circumstances, the present inventors have prepared an aqueous ink for inkjet recording comprising a polyurethane resin particle dispersion composed of an aqueous pigment dispersion dispersed with styrene-acrylic resin and polypropylene glycol. By using the aqueous pigment dispersion, after the discharge is stopped, the rate of decrease in the discharge speed when discharging again is low, there is no landing deviation, the discharge speed during continuous discharge is high, and the discharge speed is stable The present inventors have found that a water-based ink for recording can be provided and have completed the present invention.
即ち本発明は、顔料と皮膜形成樹脂とが水性媒体に分散したインクジェット記録用水性インク調整のためお水性顔料分散体において、顔料１００部あたり、スチレン−アクリル樹脂１０〜７０部で分散した水性顔料分散体と、ポリプロピレングリコールから構成されるポリウレタン樹脂粒子分散体からなるインクジェット記録用水性インク調整のための水性顔料分散体。 That is, the present invention relates to an aqueous pigment dispersed in 10 to 70 parts of styrene-acrylic resin per 100 parts of pigment in an aqueous pigment dispersion for preparing an aqueous ink for inkjet recording in which a pigment and a film-forming resin are dispersed in an aqueous medium. An aqueous pigment dispersion for adjusting an aqueous ink for inkjet recording, comprising a dispersion and a polyurethane resin particle dispersion composed of polypropylene glycol.
前記ポリウレタン樹脂のポリスチレン換算重量平均分子量（Ｍｗ）が、８０００〜１７０００である前記記載のインクジェット記録用水性インク調整のための水性顔料分散体。 The aqueous pigment dispersion for adjusting the aqueous ink for inkjet recording according to the above, wherein the polyurethane resin has a polystyrene-equivalent weight average molecular weight (Mw) of 8000 to 17000.
前記ポリウレタン樹脂の酸価が５２±１０ｍｇＫＯＨ／ｇである請求項１記載のインクジェット記録用水性インク調整のための水性顔料分散体。 2. The aqueous pigment dispersion for preparing an aqueous ink for ink jet recording according to claim 1, wherein the acid value of the polyurethane resin is 52 ± 10 mg KOH / g.
前記ポリウレタン樹脂を構成するポリプロピレングリコールのＭｗが１０００〜２０００である前記記載のインクジェット記録用水性インク調整のための水性顔料分散体。 The aqueous pigment dispersion for adjusting the aqueous ink for ink-jet recording described above, wherein Mw of polypropylene glycol constituting the polyurethane resin is 1000 to 2000.
前記のいずれかに記載のインクジェット記録用水性顔料分散体と、質量換算で液媒体全体を１００％とした際に多価アルコール４０％未満と水６０％以上とからなる液媒体から調製されたインクジェット記録用水性インクを提供する。 An inkjet prepared from the aqueous pigment dispersion for inkjet recording according to any one of the above and a liquid medium comprising less than 40% polyhydric alcohol and 60% or more water when the entire liquid medium is 100% in terms of mass A water-based ink for recording is provided.
本発明のインクジェット記録用水性顔料分散液は、吐出停止後、再び吐出した際の吐出速度の速度低下率が低く、着弾ズレが無く、連続吐出時の吐出速度が速い上に吐出速度が安定している、という格別顕著な技術的効果を奏する。 The aqueous pigment dispersion for ink-jet recording of the present invention has a low rate of decrease in discharge speed when discharged again after stopping discharge, no landing deviation, high discharge speed during continuous discharge, and stable discharge speed. It has a particularly remarkable technical effect.
以下、本発明の詳細について説明する。
本発明で提供されるインクジェット記録用水性インク調整のための水性顔料分散体は、顔料１００部あたり、スチレン−アクリル樹脂１０〜７０部で分散した水性顔料分散体と、ポリプロピレングリコールから構成されるウレタン樹脂粒子を用いることを特徴とするインクジェット記録用水性インク調整のための水性顔料分散体および該水性顔料分散体から調整されたインクジェット記録用水性インクである。
Details of the present invention will be described below.
The aqueous pigment dispersion for preparing an aqueous ink for inkjet recording provided in the present invention is a urethane composed of an aqueous pigment dispersion dispersed with 10 to 70 parts of styrene-acrylic resin per 100 parts of pigment and polypropylene glycol. A water-based pigment dispersion for preparing a water-based ink for ink-jet recording, characterized by using resin particles, and a water-based ink for ink-jet recording prepared from the water-based pigment dispersion.
本発明の特徴は、インクジェット記録用水性インク調整のための水性顔料分散体において、従来、経時安定性を付与するために、ポリ（オキシテトラメチレン）グリコール（ＰＴＭＧ）やポリエチレングリコール（ＰＥＧ）を構成成分とした、高分子量のポリウレタン樹脂分散体が使用されおり、発一性が極めて低かったが、顔料と皮膜形成樹脂からなる顔料分散体に、ポリオール成分としてポリプロピレングリコールを構成成分とする、低分子量のポリウレタン樹脂分散体を混合することで、経時安定性の付与に加え、発一性が高く、さらに着弾ズレが無く、吐出速度の速い分散体を得られることがわかった。 A feature of the present invention is that, in an aqueous pigment dispersion for preparing an aqueous ink for ink jet recording, conventionally, poly (oxytetramethylene) glycol (PTMG) or polyethylene glycol (PEG) is used to provide stability over time. A high molecular weight polyurethane resin dispersion used as a component was used, and the low-molecular weight was extremely low in uni-formity. However, the pigment dispersion consisting of a pigment and a film-forming resin was composed of polypropylene glycol as a polyol component. It was found that by mixing this polyurethane resin dispersion, it was possible to obtain a dispersion having a high discharge property and a high ejection speed in addition to imparting stability over time.
構成成分をポリプロピレングリコールとしたことや、低分子量としたことで、インクジェット記録用水性インク調整のための水性顔料分散体およびそれを用いたインクジェット記録用水性インクの顔料とウレタン樹脂の吸着作用を維持しつつ、系の親水性を高めることができた結果、インクジェットプリンターの吐出口において、ウレタン樹脂の皮膜を形成が抑制され、貯蔵安定性・光択と、発一性・着弾ズレの少なさ・吐出速度の両立ができた。 By using polypropylene glycol as the constituent component and having a low molecular weight, the water-based pigment dispersion for adjusting the water-based ink for ink-jet recording and the water-based ink for ink-jet recording using the same and the adsorption action of the urethane resin are maintained. However, as a result of improving the hydrophilicity of the system, the formation of a urethane resin film is suppressed at the discharge port of the ink jet printer, storage stability, photoselection, lightness, and less impact deviation. The discharge speed was compatible.
本発明のインクジェット記録用水性インクを調製する際、顔料としては、公知慣用の無機顔料や有機顔料がいずれも使用できる。 When preparing the water-based ink for ink-jet recording of the present invention, any of publicly known and commonly used inorganic pigments and organic pigments can be used.
無機顔料としては、例えば、二酸化チタン、酸化亜鉛、酸化鉄、酸化クロム、鉄黒、コバルトブルー、アルミナ白、酸化鉄黄、ビリジアン、硫化亜鉛、リトボン、カドミウムイエロー、朱、カドミウムレッド、黄鉛、モリブデートオレンジ、ジンククロメート、ストロンチウムクロメート、ホワイトカーボン、クレー、タルク、群青、沈降性硫酸バリウム、バライト粉、炭酸カルシウム、鉛白、紺青、マンガンバイオレット、カーボンブラック、アルミニウム粉、パール系顔料等が挙げられる。 Examples of inorganic pigments include titanium dioxide, zinc oxide, iron oxide, chromium oxide, iron black, cobalt blue, alumina white, iron oxide yellow, viridian, zinc sulfide, lithobon, cadmium yellow, vermilion, cadmium red, yellow lead, Examples include molybdate orange, zinc chromate, strontium chromate, white carbon, clay, talc, ultramarine, precipitated barium sulfate, barite powder, calcium carbonate, lead white, bitumen, manganese violet, carbon black, aluminum powder, pearl pigment, etc. It is done.
有機顔料としては、例えば、キナクリドン系顔料、フタロシアニン系顔料、スレン系顔料、ペリレン系顔料、フタロン系顔料、ジオキサジン系顔料、イソインドリノン系顔料、メチン・アゾメチン系顔料、ジケトピロロピロール系顔料、アゾレーキ顔料系顔料、不溶性アゾ系顔料、縮合アゾ系顔料等が挙げられる。 Examples of organic pigments include quinacridone pigments, phthalocyanine pigments, selenium pigments, perylene pigments, phthalone pigments, dioxazine pigments, isoindolinone pigments, methine / azomethine pigments, diketopyrrolopyrrole pigments, Examples include azo lake pigments, insoluble azo pigments, and condensed azo pigments.
本発明においてポリウレタン樹脂とは、ウレタン結合以外に尿素結合をも含有する樹脂（ポリウレタンポリ尿素樹脂という。） を包含する広義のウレタン樹脂を意味する。本発明に用いられるポリウレタン樹脂は、ポリプロピレングリコールから構成されるポリウレタン樹脂であり、酸価５２±１０ｍｇＫＯＨ／ｇであり、より好ましくは酸価５５±５ｍｇＫＯＨ／ｇである。 In the present invention, the polyurethane resin means a urethane resin in a broad sense including a resin containing a urea bond in addition to the urethane bond (referred to as a polyurethane polyurea resin). The polyurethane resin used in the present invention is a polyurethane resin composed of polypropylene glycol, and has an acid value of 52 ± 10 mg KOH / g, more preferably an acid value of 55 ± 5 mg KOH / g.
ポリエーテル系ポリウレタン樹脂は、ポリエーテル部分が加水分解を受けないので、ポリエステル系ポリウレタン樹脂に比べて、湿熱履歴後の着色画像の被記録媒体上での密着性やその光沢が低下し難いという優れた特徴を持っている。中でもポリプロピレングリコールから構成されるウレタン樹脂は、その他のポリエーテル系ポリウレタン樹脂比べて、ポリオール成分の疎水骨格と親水骨格のバランスが、顔料との相互作用による分散安定化と、インクの親水性向上による発一性良化の双方に効果的であるという特徴が顕著である。 The polyether polyurethane resin is superior in that the polyether portion is not hydrolyzed, so that the adhesion of the colored image after the wet heat history on the recording medium and its gloss are less likely to be lower than the polyester polyurethane resin. Have the characteristics. Above all, urethane resin composed of polypropylene glycol has a balance between the hydrophobic skeleton and the hydrophilic skeleton of the polyol component due to dispersion stabilization by the interaction with the pigment and improved hydrophilicity of the ink, compared to other polyether polyurethane resins. The feature that it is effective for both improvement of the uniformity is remarkable.
また酸価とは、酸基含有ポリエーテル系ポリウレタン樹脂の不揮発分１ｇを中和するのに必要な水酸化カリウムのミリグラム数を意味する。酸価の単位は、ｍｇＫＯＨ／ｇである。この酸価は、ポリエーテル系ポリウレタン樹脂中の中和されていない（遊離の）酸基に基づくものである。酸基としては、例えば、カルボキシル基、スルホン酸基、燐酸基等が挙げられる。 The acid value means the number of milligrams of potassium hydroxide required to neutralize 1 g of the nonvolatile content of the acid group-containing polyether polyurethane resin. The unit of the acid value is mgKOH / g. This acid value is based on unneutralized (free) acid groups in the polyether-based polyurethane resin. Examples of the acid group include a carboxyl group, a sulfonic acid group, and a phosphoric acid group.
本発明に用いられるポリウレタン樹脂中のポリプロピレングリコール構造の含有量は、特に制限されるものではないが、着色画像の優れた光沢と水性媒体中への優れた初期分散性と分散安定性を兼備することができる点で、４０〜７０重量％とすることが好ましい。ポリプロピレングリコール構造以外の構造は、例えば２〜３官能のアルコール、２価以下の酸性基を持つ２〜３官能のアルコール、ジイソシアネート化合物等で構成することができる。 The content of the polypropylene glycol structure in the polyurethane resin used in the present invention is not particularly limited, but has both excellent gloss of colored images and excellent initial dispersibility and dispersion stability in an aqueous medium. It is preferable to set it as 40 to 70 weight% at the point which can be performed. The structure other than the polypropylene glycol structure can be composed of, for example, a bifunctional or trifunctional alcohol, a bifunctional or trifunctional alcohol having a divalent or less acidic group, a diisocyanate compound, and the like.
本発明に用いられるポリウレタン樹脂は、前記した要件を満たしたものであればどの様な製造方法で得られたものでも良いが、それは、例えば、ポリプロピレングリコールと、有機ジイソシアネート化合物と、酸基とそれ以外の活性水素原子を２つ含有する活性水素化合物とを必須成分として、必要に応じて前記以外の活性水素化合物を用いて反応させることで得ることが出来る。勿論、末端イソシアネート基のプレポリマーを製造し、これを鎖伸長させる方法で製造することも出来る。 The polyurethane resin used in the present invention may be obtained by any production method as long as it satisfies the above-described requirements. For example, it may be polypropylene glycol, an organic diisocyanate compound, an acid group, and the like. An active hydrogen compound containing two other active hydrogen atoms as an essential component can be obtained by reacting with an active hydrogen compound other than those described above as necessary. Of course, it can also be produced by producing a prepolymer of a terminal isocyanate group and subjecting it to chain extension.
ポリプロピレングリコールとは、当業界においてＰＰＧと略記され、後記一般式（１）で表されるポリプロピレン構造を分子内に含有するジオール化合物である。後記一般式（１）中の繰り返し単位数ｎ については、種々の繰り返し単位数ｎ のものの混合物であることから、ｎ は平均値として表される。 Polypropylene glycol is a diol compound that is abbreviated as PPG in the industry and contains a polypropylene structure represented by the following general formula (1) in the molecule. The number of repeating units n in the general formula (1) described later is a mixture of various repeating units of n 1, and therefore n is expressed as an average value.
−(-CH2CH(CH3)-O-)n− n=34 一般式（１） -(-CH2CH (CH3) -O-) n- n = 34 General formula (1)
有機ジイソシアネート化合物としては、特に限定はなく、例えばヘキサメチレンジイソシート、２，２，４−トリメチルヘキサメチレンジイソシアネート等の脂肪族ジイソシアネー卜化合物、イソホロンジイソシアネー卜、水添キシリレンジイソシアネート、４，４−シクロヘキシルメタンジイソシアネート等の脂環族ジイソシアネー卜化合物、キシリレンジイソシアネート、テトラメチルキシレンジイソシアネー卜等の芳香脂肪族ジイソシアネー卜化合物、トルイレンジイソシアネー卜、フェニルメタンジイソシアネート等の芳香族ジイソシアネー卜化合物が挙げられる。 The organic diisocyanate compound is not particularly limited. For example, an aliphatic diisocyanate compound such as hexamethylene diisosheet, 2,2,4-trimethylhexamethylene diisocyanate, isophorone diisocyanate compound, hydrogenated xylylene diisocyanate, 4, Cycloaliphatic diisocyanate compounds such as 4-cyclohexylmethane diisocyanate, aromatic diisocyanate compounds such as xylylene diisocyanate and tetramethylxylene diisocyanate, aromatic diisocyanate compounds such as toluylene diisocyanate and phenylmethane diisocyanate Is mentioned.
有機ジイソシアネート化合物としては、着色画像の耐光変色が起こり難い点では、一般に脂肪族または脂環族ジイソシアネート化合物が好ましく、着色画像の光沢がより高い点では、芳香族または脂環族ジイソシアネート化合物が好ましい。 As the organic diisocyanate compound, an aliphatic or alicyclic diisocyanate compound is generally preferable from the viewpoint that the light fast discoloration of the colored image does not occur, and an aromatic or alicyclic diisocyanate compound is preferable from the viewpoint of higher gloss of the colored image.
このような活性水素化合物としては、例えば、酸基としてカルボキシル基及び／ 又はスルホン酸基を含有しそれ以外の活性水素原子を２つ含有する活性水素化合物が特に制限なく使用できるが、例えば、２，２−ジメチロール乳酸、２，２−ジメチロールプロピオン酸、２，２−ジメチロールブタン酸、２，２−ジメチロール吉草酸、３，４−ジアミノブタンスルホン酸、３，６−ジアミノ−２−トルエンスルホン酸等が挙げられる。酸基とそれ以外の活性水素原子を２つ含有する活性水素化合物の使用量は、ポリウレタン樹脂の酸価が前記範囲となる様な量である。 As such an active hydrogen compound, for example, an active hydrogen compound containing a carboxyl group and / or a sulfonic acid group as an acid group and containing two other active hydrogen atoms can be used without particular limitation. , 2-dimethylollactic acid, 2,2-dimethylolpropionic acid, 2,2-dimethylolbutanoic acid, 2,2-dimethylolvaleric acid, 3,4-diaminobutanesulfonic acid, 3,6-diamino-2-toluene A sulfonic acid etc. are mentioned. The amount of the active hydrogen compound containing an acid group and two other active hydrogen atoms is such that the acid value of the polyurethane resin falls within the above range.
本発明に用いられるポリウレタン樹脂は、前記した様にポリプロピレングリコールと、有機ジイソシアネート化合物と、酸基とそれ以外の活性水素原子を２つ含有する活性水素化合物のみに基づく化学構造の樹脂であっても良いが、着色画像に対応する皮膜の硬度の調整等のために、その他の活性水素化合物に基づく化学構造を含有していても良い。 The polyurethane resin used in the present invention may be a resin having a chemical structure based only on an active hydrogen compound containing polypropylene glycol, an organic diisocyanate compound, and an acid group and two other active hydrogen atoms as described above. Although it is good, it may contain a chemical structure based on other active hydrogen compounds in order to adjust the hardness of the film corresponding to the colored image.
酸基を導入するため以外に必要に応じて用いる活性水素化合物としては、例えば、エチレングリコール、ジエチレングリコール、プロピレングリコール、ジプロピレングリコール、１，２−プロパンジオール、１，３−プロパンジオール、１，４−ブタンジオール等の低分子ジオールが挙げられる。 Examples of the active hydrogen compound used as needed other than for introducing an acid group include, for example, ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4 -Low molecular diols such as butanediol.
この際の活性水素化合物としては、分岐構造を有する低分子ジオールを併用することが好ましい。分岐構造を有する低分子ジオールと有機ジイソシアネートとの重付加反応構造をポリウレタン樹脂に導入すると、側鎖の立体障害により結晶性が乱されるため水性媒体中での分散粒子の初期分散性や分散安定性が向上する。このような分岐構造を有する低分子ジオールとしては、例えば、ネオペンチルグリコールやブチルエチルプロパンジオール等の脂肪族ジオールが挙げられる。 In this case, as the active hydrogen compound, it is preferable to use a low molecular diol having a branched structure in combination. When a polyaddition reaction structure of a low molecular diol having a branched structure and an organic diisocyanate is introduced into a polyurethane resin, the crystallinity is disturbed by steric hindrance of the side chain, so that the initial dispersibility and dispersion stability of dispersed particles in an aqueous medium Improves. Examples of the low molecular diol having such a branched structure include aliphatic diols such as neopentyl glycol and butyl ethyl propane diol.
本発明に用いるポリウレタン樹脂は、直鎖状（ リニアー） であることが着色画像の皮膜物性の観点からは好ましいが、直鎖状ポリウレタン樹脂であることの特徴を損なわない範囲において、必要に応じて、前記した原料に加えて、３ 官能以上の活性水素化合物や３官能以上の有機ポリイソシアネート化合物を適宜併用して、３ 次元網目構造を有するポリウレタン樹脂を、直鎖状のポリウレタン樹脂に極少量含有させても良い。 The polyurethane resin used in the present invention is preferably linear (linear) from the viewpoint of the physical properties of the colored image, but as long as the characteristics of being a linear polyurethane resin are not impaired, as necessary. In addition to the raw materials described above, a tri- or higher-functional active hydrogen compound or a tri- or higher-functional organic polyisocyanate compound is used in combination, and a polyurethane resin having a three-dimensional network structure is contained in a very small amount in a linear polyurethane resin. You may let them.
本発明に用いられるポリウレタン樹脂は、酸価５２±１０ｍｇＫＯＨ／ｇにあることが、塩基性物質を添加した際の、水性媒体への顔料の初期分散性や水性媒体中の分散安定性が良好で、また調製されたインクジェット記録用水性インクの印字安定性が良く、着色画像の耐水性も良好な上、耐摩擦性、耐棒積み性等の画像保存性も良好となるので好ましい。 The polyurethane resin used in the present invention has an acid value of 52 ± 10 mg KOH / g, and when the basic substance is added, the initial dispersibility of the pigment in the aqueous medium and the dispersion stability in the aqueous medium are good. Further, the prepared water-based ink for ink jet recording has good printing stability, the water resistance of the colored image is good, and the image preservability such as the friction resistance and the sticking resistance is also good.
塩基性物質としては、例えば、アンモニア、エチルアミン、トリメチルアミン、トリエチルアミン、トリイソプロピルアミン、トリブチルアミン、トリエタノールアミン、Ｎ−メチルジエタノールアミン、Ｎ−フェニルジエタノールアミン、モノエタノールアミン、ジメチルエタノールアミン、ジエチルエタノールアミン、モルホリン、Ｎ−メチルモルホリン、２−アミノ−２−エチル−１−プロパノール等の有機アミン類、リチウム、カリウム、ナトリウム等のアルカリ金属、水酸化ナトリウム、水酸化カリウムの無機アルカリ類等が挙げられる。塩基性物質の使用量は、ポリウレタン樹脂の物性に応じて適宜設定されるが、塩基性物質の使用量は特に制限されるものではないが、通常、ポリウレタン樹脂の酸価の７０〜１３０％を中和するのに必要な量の塩基性物質が用いられる。 Examples of basic substances include ammonia, ethylamine, trimethylamine, triethylamine, triisopropylamine, tributylamine, triethanolamine, N-methyldiethanolamine, N-phenyldiethanolamine, monoethanolamine, dimethylethanolamine, diethylethanolamine, morpholine. , N-methylmorpholine, organic amines such as 2-amino-2-ethyl-1-propanol, alkali metals such as lithium, potassium and sodium, and inorganic alkalis such as sodium hydroxide and potassium hydroxide. The amount of the basic substance used is appropriately set according to the physical properties of the polyurethane resin, but the amount of the basic substance used is not particularly limited, but usually 70 to 130% of the acid value of the polyurethane resin. The amount of basic material necessary to neutralize is used.
本発明に用いられるポリウレタン樹脂は、通常重量平均分子量で、８０００〜１７０００、好ましくは９０００〜１６５００、さらに好ましくは１２０００〜１５４００である。ポリウレタン樹脂の分子量は、ゲルパーミエーションクロマトグラフィーにより測定され、ポリスチレン換算の値として表される。以下、特に断りのない限り、本発明においてポリウレタン樹脂の分子量は重量平均を基準とする。 The polyurethane resin used in the present invention usually has a weight average molecular weight of 8000 to 17000, preferably 9000 to 16500, and more preferably 12000 to 15400. The molecular weight of the polyurethane resin is measured by gel permeation chromatography and expressed as a value in terms of polystyrene. Hereinafter, unless otherwise specified, in the present invention, the molecular weight of the polyurethane resin is based on the weight average.
ポリウレタン樹脂の分子量が２０００未満であると、被記録媒体への顔料の定着性が乏しくなるとともに水性媒体中での顔料の分散安定性が低下し好ましくない。一方、ポリウレタン樹脂の分子量が１０００００を超えると、塩基性物質を添加しても水性媒体中へのポリウレタン樹脂の溶解性が低下すると共に、調製されるインクジェット記録用水性インクの粘度が高くなるので好ましくない。 If the molecular weight of the polyurethane resin is less than 2,000, the fixing property of the pigment to the recording medium becomes poor and the dispersion stability of the pigment in the aqueous medium is lowered, which is not preferable. On the other hand, when the molecular weight of the polyurethane resin exceeds 100,000, the solubility of the polyurethane resin in the aqueous medium is lowered even when a basic substance is added, and the viscosity of the prepared aqueous ink for inkjet recording is preferably increased. Absent.
本発明のインクジェット記録用水性インクを調製するに当たっては、質量換算で顔料１１００部に対してポリウレタン樹脂の不揮発分を通常５〜８０部、好ましくは１０〜４０部となる様にする。インク中の顔料に対するポリウレタン樹脂の量が少ないと着色画像の耐擦性が低下する傾向にあるし、一方、多いとインク粘度や流動性の面から使用しにくくなるので好ましくない。 In preparing the water-based ink for ink-jet recording of the present invention, the non-volatile content of the polyurethane resin is usually 5 to 80 parts, preferably 10 to 40 parts with respect to 1100 parts of pigment in terms of mass. If the amount of the polyurethane resin relative to the pigment in the ink is small, the abrasion resistance of the colored image tends to be lowered. On the other hand, if the amount is large, it is difficult to use from the viewpoint of ink viscosity and fluidity.
本発明のインクジェット記録用水性インクは、例えば顔料濃度がより高いポリウレタン樹脂を含む水性顔料分散体を調製し、それを希釈する等して調製することが出来る。
このポリウレタン樹脂を含む水性顔料分散体は、例えば後記する様な１）〜４）の方法で製造することが出来る。
１）ポリウレタン樹脂の水性分散体に、顔料を機械的に強制分散する水性顔料分散体の製造方法。
２）顔料の存在下の液媒体中で分散剤を用いて、ポリウレタン樹脂の各原料成分を反応させポリウレタン樹脂とした後、かつ任意の工程で水を含ませ、必要に応じて会合や脱溶剤を行う水性顔料分散体の製造方法。
３）顔料とポリウレタン樹脂と有機溶剤の混合物を、水と塩基性物質を用いて徐徐に油相から水相に転相させてから脱溶剤して、顔料がポリウレタン樹脂で被覆されたマイクロカプセル型複合粒子とする、同複合粒子を含む水性顔料分散体の製造方法。
４）顔料とポリウレタン樹脂と塩基性物質と有機溶剤と水との均一混合物から脱溶剤を行い、酸を加えて酸析し析出物を洗浄後、この析出物を塩基性物質と共に水性媒体に分散させる、顔料がポリウレタン樹脂で被覆されたマイクロカプセル型複合粒子とする、同複合粒子を含む水性顔料分散体の製造方法。
The aqueous inkjet recording ink of the present invention can be prepared, for example, by preparing an aqueous pigment dispersion containing a polyurethane resin having a higher pigment concentration and diluting it.
The aqueous pigment dispersion containing this polyurethane resin can be produced, for example, by the methods 1) to 4) as described later.
1) A method for producing an aqueous pigment dispersion in which a pigment is mechanically forcedly dispersed in an aqueous dispersion of a polyurethane resin.
2) After each polyurethane resin raw material component is reacted with a dispersant in a liquid medium in the presence of a pigment to obtain a polyurethane resin, water is added at an optional step, and associating or solvent-removing as necessary. A method for producing an aqueous pigment dispersion.
3) A microcapsule type in which a pigment, polyurethane resin, and organic solvent mixture is gradually phase-inverted from an oil phase to an aqueous phase using water and a basic substance, and then the solvent is removed. A method for producing an aqueous pigment dispersion containing composite particles, which is composite particles.
4) Solvent removal from a uniform mixture of pigment, polyurethane resin, basic substance, organic solvent and water, acid addition, acid precipitation, washing the precipitate, and dispersing the precipitate together with the basic substance in an aqueous medium A method for producing an aqueous pigment dispersion containing the composite particles, wherein the microcapsule composite particles are coated with a polyurethane resin.
本発明において、水性媒体とは水のみ又は水と有機溶剤との混合物であって水の含有割合が質量換算で６０％以上であるものを言う。水性媒体としては、有機溶剤を全く含まないか又は極力含有しないものを用いることが、火災防止や環境安全の面から好ましい。これは後記する水性顔料分散体の場合も、本発明のインクジェット記録用水性インクの場合でも同様である。 In the present invention, the aqueous medium means water alone or a mixture of water and an organic solvent and the water content is 60% or more in terms of mass. As the aqueous medium, it is preferable from the viewpoint of fire prevention and environmental safety to use one containing no organic solvent or containing as much as possible. The same applies to the case of the aqueous pigment dispersion described later and the case of the aqueous ink for inkjet recording of the present invention.
水性顔料分散体の製造方法では、前記いずれの製造方法をとるにせよ、顔料、ポリウレタン樹脂、塩基性物質および水からなる混合物を分散する工程を必須として含ませることが好ましい。この混合物には水溶性有機溶剤を含めるのが好ましい。より具体的には、少なくとも顔料、ポリウレタン樹脂、塩基性物質、水溶性有機溶剤および水からなる混合物を分散する工程（分散工程）を含ませることが好ましい。 In any of the above production methods, the method for producing an aqueous pigment dispersion preferably includes a step of dispersing a mixture comprising a pigment, a polyurethane resin, a basic substance and water as an essential step. This mixture preferably contains a water-soluble organic solvent. More specifically, it is preferable to include a step (dispersion step) of dispersing a mixture of at least a pigment, a polyurethane resin, a basic substance, a water-soluble organic solvent, and water.
また、分散工程において水溶性有機溶剤を併用することができ、それにより分散工程における液粘度を低下させることができる場合がある。水溶性有機溶剤の例としては、アセトン、メチルエチルケトン、メチルブチルケトン、メチルイソブチルケトン、等のケトン類；メタノール、エタノール、２−プロパノール、２−メチル−１−プロパノール、１−ブタノール、２−メトキシエタノール、等のアルコール類； テトラヒドロフラン、１ ，４−ジオキサン、１，２−ジメトキシエタン、等のエーテル類；ジメチルホルムアミド、Ｎ−メチルピロリドン、等のアミド類が挙げられ、とりわけ炭素原子数が３〜６のケトンおよび炭素原子数が１〜５のアルコールからなる群から選ばれる化合物を用いるのが好ましい。これらの水溶性有機溶剤はポリウレタン樹脂溶液として用いられても良く、別途独立に分散混合物中に加えられても良い。 In addition, a water-soluble organic solvent can be used in combination in the dispersion step, which can reduce the liquid viscosity in the dispersion step. Examples of water-soluble organic solvents include ketones such as acetone, methyl ethyl ketone, methyl butyl ketone, and methyl isobutyl ketone; methanol, ethanol, 2-propanol, 2-methyl-1-propanol, 1-butanol, 2-methoxyethanol Alcohols such as tetrahydrofuran, 1,4-dioxane, 1,2-dimethoxyethane, and the like; amides such as dimethylformamide, N-methylpyrrolidone, and the like. It is preferable to use a compound selected from the group consisting of a ketone and an alcohol having 1 to 5 carbon atoms. These water-soluble organic solvents may be used as a polyurethane resin solution, or may be separately added to the dispersion mixture.
本発明のインクジェット記録用水性インクは、少なくとも顔料、酸基含有ポリエーテル系ポリウレタン樹脂、塩基性物質および水からなる混合物を分散装置により分散する工程を含むプロセスによって製造することができる。 The water-based ink for inkjet recording of the present invention can be produced by a process including a step of dispersing a mixture of at least a pigment, an acid group-containing polyether polyurethane resin, a basic substance and water with a dispersing device.
製造プロセスに組み込み得るその他の工程の例としては、予備分散工程、溶解工程、希釈工程、蒸留工程、遠心分離工程、酸析工程、濾過工程、再分散工程、ｐ H調整工程、充填工程等が挙げられる。 Examples of other steps that can be incorporated into the manufacturing process include pre-dispersion step, dissolution step, dilution step, distillation step, centrifugation step, acid precipitation step, filtration step, redispersion step, pH adjustment step, filling step, etc. Can be mentioned.
予備分散工程の例には、溶液状態または溶融状態の樹脂と顔料を混合、分散し、スラリー状、ペースト状もしくはマスターバッチまたはチップと呼ばれる固体状態にする工程等がある。溶解工程の例には、固体状の酸基含有ポリエーテル系ポリウレタン樹脂を有機溶剤、好ましくは水溶性有機溶剤中、または塩基性物質を含む水性媒体中に溶解させる工程、もしくは酸基含有ポリエーテル系ポリウレタン樹脂の水溶性有機溶剤溶液を塩基性物質を含む水性媒体中に溶解させる工程等がある。 Examples of the pre-dispersing step include a step of mixing and dispersing a resin in a solution state or a molten state and a pigment to form a solid state called a slurry, paste, masterbatch or chip. Examples of the dissolving step include a step of dissolving a solid acid group-containing polyether polyurethane resin in an organic solvent, preferably a water-soluble organic solvent, or an aqueous medium containing a basic substance, or an acid group-containing polyether. For example, a step of dissolving a water-soluble organic solvent solution of a polyurethane resin in an aqueous medium containing a basic substance.
蒸留工程の例には、分散工程において有機溶剤を使用した場合にこれを除去する工程、所望の固形分濃度にするため余剰の水を除去する工程がある。遠心分離工程の例には、インクジェット記録用水性インクとしての使用適性に悪影響を及ぼす分散体中の粗大粒子を除去する工程等がある。 Examples of the distillation step include a step of removing an organic solvent when used in the dispersion step and a step of removing excess water to obtain a desired solid content concentration. Examples of the centrifugation step include a step of removing coarse particles in the dispersion that adversely affect the suitability for use as a water-based ink for inkjet recording.
酸析工程の例には、分散工程で得られた水性顔料分散体に塩酸、硫酸、酢酸等の酸を加えて酸性化し、塩基と塩を形成することによって溶解状態にある酸基含有ポリエーテル系ポリウレタン樹脂を顔料表面に析出させる工程がある。この工程により顔料と酸基含有ポリエーテル系ポリウレタン樹脂との相互作用を高めることができる。その結果、顔料が酸基含有ポリエーテル系ポリウレタン樹脂の濃密な層によって被覆される。これにより、顔料が酸基含有ポリエーテル系ポリウレタン樹脂によって被覆された、いわゆるマイクロカプセル化顔料が水性媒体中に分散している形態を取らせることができ、水性顔料分散体として、分散到達レベルや分散安定性等の物性面や耐溶剤性等の使用適性の面で、より優れた特性を発揮させることができる。 Examples of acid precipitation processes include acid group-containing polyethers that are dissolved by adding acid such as hydrochloric acid, sulfuric acid, and acetic acid to the aqueous pigment dispersion obtained in the dispersion process to form a salt with a base. There is a step of depositing a polyurethane resin on the pigment surface. By this step, the interaction between the pigment and the acid group-containing polyether polyurethane resin can be enhanced. As a result, the pigment is covered with a dense layer of the acid group-containing polyether polyurethane resin. As a result, a so-called microencapsulated pigment in which the pigment is coated with an acid group-containing polyether-based polyurethane resin can be dispersed in an aqueous medium. More excellent characteristics can be exhibited in terms of physical properties such as dispersion stability and suitability for use such as solvent resistance.
濾過工程の例には、遠心分離工程と同様に分散粒子中の粗大粒子をカートリッジフィルターやメンブレンフィルターにより除去する工程、前述した酸析工程後にフィルタープレス、ヌッチェ式濾過装置、加圧濾過装置等により濾過する工程等がある。 Examples of the filtration step include a step of removing coarse particles in the dispersed particles with a cartridge filter or a membrane filter as in the centrifugal separation step, a filter press, a Nutsche filtration device, a pressure filtration device, etc. after the acid precipitation step described above. There is a process of filtering.
再分散工程の例には、酸析工程、濾過工程によって得られた固形分に塩基性物質および必要により水や添加物を加えて再び分散体とする工程がある。それにより酸基含有ポリエーテル系ポリウレタン樹脂中のイオン化した酸基の対イオンを分散工程で用いたものから変更することができる。 Examples of the redispersion step include a step of adding a basic substance and, if necessary, water and additives to the solid content obtained by the acid precipitation step and the filtration step to form a dispersion again. Thereby, the counter ion of the ionized acid group in the acid group-containing polyether polyurethane resin can be changed from that used in the dispersion step.
分散工程において用いることのできる分散装置として、既に公知の種々の方式による装置が使用でき、特に限定されるものではないが、例えば、スチール、ステンレス、ジルコニア、アルミナ、窒化ケイ素、ガラス等でできた直径０．1〜１０ｍｍ程度の球状分散媒体の運動エネルギーを利用する方式、機械的攪拌によるせん断力を利用する方式、高速で供給された被分散物流束の圧力変化、流路変化あるいは衝突に伴って発生する力を利用する方式、等の分散方式を採ることができる。 As a dispersion apparatus that can be used in the dispersion step, apparatuses by various known methods can be used, and are not particularly limited. For example, the dispersion apparatus can be made of steel, stainless steel, zirconia, alumina, silicon nitride, glass, or the like. A method that uses the kinetic energy of a spherical dispersion medium with a diameter of about 0.1 to 10 mm, a method that uses shearing force by mechanical stirring, a change in pressure of a dispersed flow bundle supplied at high speed, a flow path change, or a collision It is possible to adopt a dispersion method such as a method using the force generated by
本発明のインクジェット記録用水性インクは、少なくとも顔料、酸基含有ポリエーテル系リウレタン樹脂および塩基性物質を含有する水性顔料分散体に、例えば、水溶性有機溶剤、水等を更に混合して調製される。本発明のインクジェット記録用水性インクは、顔料１００部に対して不揮発分にして５〜８０部のポリエーテル系ポリウレタン樹脂を含有する様に調製することが好ましい。本発明のインクジェット記録用水性インクの調製に当たっては、必要に応じて界面活性剤、水溶性樹脂、防腐剤、粘度調整剤、ｐ H調整剤、キレート化剤等を添加することもできる。 The water-based ink for inkjet recording of the present invention is prepared by further mixing, for example, a water-soluble organic solvent, water and the like with an aqueous pigment dispersion containing at least a pigment, an acid group-containing polyether-based urethane resin and a basic substance. The The water-based ink for ink-jet recording of the present invention is preferably prepared so as to contain 5 to 80 parts of a polyether-based polyurethane resin in a nonvolatile content with respect to 100 parts of the pigment. In preparing the water-based ink for inkjet recording of the present invention, a surfactant, a water-soluble resin, a preservative, a viscosity adjuster, a pH adjuster, a chelating agent, and the like can be added as necessary.
インクジェット記録用水性インクの調製に用いることのできる水溶性有機溶剤としては、例えば、前記したものの他に、１−プロパノール、２−ブトキシエタノール、２−（２−メトキシエトキシ）エタノール、２−（２−ブトキシエトキシ）エタノール、２−［２−（２−メトキシエトキシ）エトキシ］エタノール、２−［２−（ ２−ブトキシエトキシ）エトキシ］エタノール等のアルコール類；１，２−エタンジオール、１，２−プロパンジオール、１，２−プロパンジオール、１，２−ブタンジオール、２，３−ブタンジオール、２，２ ´ −オキシビスエタノール、２，２ ´ ―エチレンジオキシビス（ エタノール） 、チオエタノール、グリセリン、１，２，６−ヘキサントリオール等の多価アルコール類；ジメチルアセトアミド、１，３−ジメチル−２−イミダゾリジノン等のアミド類； メチルn− ブチルケトン等のケトン類；１，２−ジエトキシエタン、２，２ ´−オキシビス（２−メトキシエタン） 、２，２ ´−オキシビス（２−エトキシエタン） 、２， ２ ´ エチレンジオキシビス（２−メトキシエタン） 、２，２ ´ ―エチレンオキシビス（ ２ − メトキシエタン）等のエーテル類が挙げられる。記録液中の水溶性有機溶剤の含有割合は、５０重量％以下が好ましく、５〜４０重量％の範囲が特に好ましい。 Examples of the water-soluble organic solvent that can be used for the preparation of the water-based ink for inkjet recording include, in addition to those described above, 1-propanol, 2-butoxyethanol, 2- (2-methoxyethoxy) ethanol, 2- (2 Alcohols such as 2-butoxyethoxy) ethanol, 2- [2- (2-methoxyethoxy) ethoxy] ethanol, 2- [2- (2-butoxyethoxy) ethoxy] ethanol; 1,2-ethanediol, 1,2 -Propanediol, 1,2-propanediol, 1,2-butanediol, 2,3-butanediol, 2,2'-oxybisethanol, 2,2'-ethylenedioxybis (ethanol), thioethanol, Polyhydric alcohols such as glycerin and 1,2,6-hexanetriol; dimethylacetamide, Amides such as 1,3-dimethyl-2-imidazolidinone; Ketones such as methyl n-butyl ketone; 1,2-diethoxyethane, 2,2′-oxybis (2-methoxyethane), 2,2′- Examples thereof include ethers such as oxybis (2-ethoxyethane), 2,2 ′ ethylenedioxybis (2-methoxyethane), and 2,2′-ethyleneoxybis (2-methoxyethane). The content of the water-soluble organic solvent in the recording liquid is preferably 50% by weight or less, and particularly preferably in the range of 5 to 40% by weight.
本発明のインクジェット記録用水性インクを調製する際には、アニオン性、カチオン性、両性イオン性、非イオン性のいずれの界面活性剤を用いることが出来る。 In preparing the water-based ink for inkjet recording of the present invention, any of anionic, cationic, zwitterionic and nonionic surfactants can be used.
アニオン性界面活性剤としては、例えば、脂肪酸塩類、アルキル硫酸エステル塩類、ベンゼンスルホン酸塩類、ナフタレンスルホン酸塩類、スルホコハク酸エステル塩類、ポリオキシエチレン硫酸エステル塩類、リン酸エステル類が挙げられる。 Examples of the anionic surfactant include fatty acid salts, alkyl sulfate esters, benzene sulfonates, naphthalene sulfonates, sulfosuccinate esters, polyoxyethylene sulfate esters, and phosphate esters.
カチオン性界面活性剤としては、例えば、アルキルアミン塩類、第４級アンモニウム塩類が挙げられる。両性イオン性界面活性剤としては、例えば、アルキルベタイン類等が挙げられる。 Examples of the cationic surfactant include alkylamine salts and quaternary ammonium salts. Examples of zwitterionic surfactants include alkylbetaines.
非イオン性活性剤としては、例えば、ポリオキシエチレンアルキルエーテル類、ポリオキシエチレンフェニルエーテル類、オキシラン重合体類、ソルビタン脂肪酸エステル類、ソルビトール脂肪酸エステル類、グリセリン脂肪酸エステル類が挙げられる。これらの非イオン性活性剤の中でもＨＬＢが１４以上のものが特に好ましい。 Examples of nonionic activators include polyoxyethylene alkyl ethers, polyoxyethylene phenyl ethers, oxirane polymers, sorbitan fatty acid esters, sorbitol fatty acid esters, and glycerin fatty acid esters. Among these nonionic active agents, those having an HLB of 14 or more are particularly preferred.
本発明のインクジェット記録用水性インク及びその前駆体である水性顔料分散体における、顔料粒子とポリウレタン樹脂粒子或いは顔料がポリウレタン樹脂で被覆されたマイクロカプセル型複合粒子からなる分散粒子は、着色画像特性や吐出安定性の面から、１００ｎｍ以上２００ｎｍ未満であることが好ましい。 In the water-based ink for inkjet recording of the present invention and the aqueous pigment dispersion which is a precursor thereof, dispersed particles composed of pigment particles and polyurethane resin particles or microcapsule composite particles in which a pigment is coated with a polyurethane resin, From the viewpoint of ejection stability, it is preferably 100 nm or more and less than 200 nm.
本発明のインクジェット記録用水性インクの調製には水溶性樹脂を用いることが出来る。この水溶性樹脂としては、例えば、にかわ、ゼラチン、カゼイン、アルブミン、アラビアゴム、フィッシュグリュー、アルギン酸、メチルセルロース、カルボキシメチルセルロース、ヒドロキシエチルセルロース、ポリ酸化エチレン、ポリビニルアルコール、ポリアクリルアミド、ポリアクリル酸、ポリビニルエーテル、ポリビニルピロリドン、スチレン− マレイン酸共重合体、スチレン−（メタ）アクリル酸共重合体、（メタ）アクリル酸エステル−（メタ）アクリル酸共重合体等が挙げられる。 A water-soluble resin can be used for the preparation of the water-based ink for inkjet recording of the present invention. Examples of the water-soluble resin include glue, gelatin, casein, albumin, gum arabic, fish mulled, alginic acid, methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyethylene oxide, polyvinyl alcohol, polyacrylamide, polyacrylic acid, polyvinyl ether, Examples include polyvinylpyrrolidone, styrene-maleic acid copolymer, styrene- (meth) acrylic acid copolymer, (meth) acrylic acid ester- (meth) acrylic acid copolymer, and the like.
スチレン−（メタ）アクリル酸共重合体、（メタ）アクリル酸エステル−（メタ）アクリル酸共重合体の様なスチレン−アクリル樹脂は、本発明で用いる前記した様なポリウレタン樹脂との相溶性に優れており、本発明における特定ポリウレタン樹脂との併用により、初期顔料分散性を損ねることなく、被記録媒体上における着色画像の濃度や耐光性をより高めることが出来る。この際、前記した様な共重合体は、質量換算でポリウレタン樹脂の不揮発分１００部当たり、不揮発分０．５〜１００部とすることが好ましい。 Styrene-acrylic resins such as styrene- (meth) acrylic acid copolymer and (meth) acrylic acid ester- (meth) acrylic acid copolymer are compatible with the above-described polyurethane resin used in the present invention. It is excellent, and the combined use with the specific polyurethane resin in the present invention can increase the density and light resistance of the colored image on the recording medium without impairing the initial pigment dispersibility. Under the present circumstances, it is preferable that the above-mentioned copolymer shall be 0.5-100 parts of non volatile matters per 100 parts of non volatile matters of a polyurethane resin in mass conversion.
本発明のインクジェット記録用水性インクは、前記した様な水性顔料分散体に質量換算で顔料が３〜１０％となる様に添加剤や液媒体を添加して希釈し、必要に応じて遠心分離や濾過する等することで調製することが出来る。 The aqueous ink for inkjet recording of the present invention is diluted by adding an additive or a liquid medium so that the pigment is 3 to 10% in terms of mass in the aqueous pigment dispersion as described above, and is centrifuged if necessary. Or by filtering.
本発明のインクジェット記録用水性インクは、各種の被記録媒体への印字記録等に用いることが出来る。この際の被記録媒体としては、例えば、普通紙、写真用紙、マット紙、合成樹脂フイルム・シート等が挙げられる。本発明のインクジェット記録用水性インクで印字記録を行うことで、特に優れた光沢が得られるのは、写真用紙である。 The water-based ink for inkjet recording of the present invention can be used for printing and recording on various recording media. Examples of the recording medium at this time include plain paper, photographic paper, matte paper, synthetic resin film and sheet. Photographic paper is particularly excellent in gloss when printed and recorded with the aqueous inkjet recording ink of the present invention.
以下、実施例にて本発明を詳細に説明するが、これらの実施例は本発明を具体的に説明するものであり、実施の態様がこれにより限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, these Examples demonstrate this invention concretely and an aspect is not limited by this.
＜製造例１＞（ポリウレタンＡ樹脂分散体の作成）
温度計、攪拌機、窒素導入管、冷却管を備えた４つ口フラスコに、重量平均分子量２０００のポリプロピレングリコール（ＰＰＧ）を４８０ｇ 、イソホロンジイソシアネート（ I P D I） を２６３ｇ 、ジブチル錫ジラウレート（ＤＢＴＤＬ） を０．００７ｇ仕込み、窒素ガス雰囲気下１００ ℃ で１時間反応させた。その後６５℃ 以下に冷却しジメチロールプロピオン酸（ＤＭＰＡ）１１５ｇ 、ネオペンチルグリコール（ＮＰＧ）１４ｇおよびメチルエチルケトン（ＭＥＫ）２９１ｇを添加し、７５ ℃で２．５時間反応させ、ＧＰＣによるポリスチレン換算重量平均分子量が８７００になったことを確認したのち、M E K １４０ｇ、メタノールを加えて反応を停止し、酸価５２ 、直鎖状の酸基含有ポリエーテル系ポリウレタン樹脂を得た。
さらに、４８％水酸化カリウム９５ｇを加え１時間攪拌した。その後、イオン交換水４１０７ｇを加え、４０℃にて減圧蒸留を行なった。メチルエチルケトンを完全に留去し、ウレタン樹脂分散体を得た。
<Production Example 1> (Preparation of polyurethane A resin dispersion)
In a four-necked flask equipped with a thermometer, a stirrer, a nitrogen introducing tube, and a cooling tube, 480 g of polypropylene glycol (PPG) having a weight average molecular weight of 2000, 263 g of isophorone diisocyanate (IPDI), and 0.02 of dibutyltin dilaurate (DBTDL). 007 g was charged and reacted at 100 ° C. for 1 hour in a nitrogen gas atmosphere. Thereafter, the mixture was cooled to 65 ° C. or lower, 115 g of dimethylolpropionic acid (DMPA), 14 g of neopentyl glycol (NPG) and 291 g of methyl ethyl ketone (MEK) were added, and the mixture was reacted at 75 ° C. for 2.5 hours. Then, 140 g of MEK and methanol were added to stop the reaction, and an acid value of 52 and a linear acid group-containing polyether polyurethane resin were obtained.
Further, 95 g of 48% potassium hydroxide was added and stirred for 1 hour. Then, 4107 g of ion-exchanged water was added and vacuum distillation was performed at 40 ° C. Methyl ethyl ketone was completely distilled off to obtain a urethane resin dispersion.
＜製造例２＞（ポリウレタンＢ樹脂分散体の合成）
製造例１のＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で４時間とし、反応停止時の重量平均分子量が１２０００とした意外は、同様の方法で、ポリウレタンＢ樹脂分散体の合成行なった。
<Production Example 2> (Synthesis of polyurethane B resin dispersion)
The polyurethane B resin dispersion was synthesized by the same method except that the reaction time after addition of DMPA, NPG and MEK in Production Example 1 was 4 hours at 75 ° C. and the weight average molecular weight at the time of stopping the reaction was 12000. It was.
＜製造例３＞（ポリウレタンＣ樹脂分散体の合成）
製造例１のＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で６時間とし、反応停止時の重量平均分子量が１５４００とした意外は、同様の方法で、ポリウレタンＣ樹脂分散体の合成行なった。
<Production Example 3> (Synthesis of polyurethane C resin dispersion)
The polyurethane C resin dispersion was synthesized in the same manner except that the reaction time after addition of DMPA, NPG, and MEK in Production Example 1 was 6 hours at 75 ° C. and the weight average molecular weight at the time of stopping the reaction was 15400. It was.
＜製造例４＞（ポリウレタンＤ樹脂分散体の合成）
製造例１のＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で７時間とし、反応停止時の重量平均分子量が１６５００とした意外は、同様の方法で、ポリウレタンＤ樹脂分散体の合成行なった
＜製造例５＞（ポリウレタンＥ樹脂分散体の合成）
製造例１の重量平均分子量２０００のＰＰＧ４８０ｇの代わりに、重量平均分子量１０００のＰＰＧ ４８０ｇを用い、ＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で６時間とし、反応停止時の重量平均分子量が１５０００とした意外は、同様の方法で、ポリウレタンＥ樹脂分散体の合成行なった
＜製造例６＞（ポリウレタンＦ樹脂分散体の合成）
製造例１の重量平均分子量２０００のＰＰＧ４８０ｇの代わりに、重量平均分子量２０００のＰＴＭＧ ４８０ｇを用い、ＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で６時間とし、反応停止時の重量平均分子量が１５０００とした意外は、同様の方法で、ポリウレタンＦ樹脂分散体の合成行なった
＜製造例７＞（ポリウレタンＧ樹脂分散体の合成）
製造例１の重量平均分子量２０００のＰＰＧ４８０ｇの代わりに、重量平均分子量２０００のＰＥＧ ４８０ｇを用い、ＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で６時間とし、反応停止時の重量平均分子量が１５２００とした意外は、同様の方法で、ポリウレタンＧ樹脂分散体の合成行なった
＜製造例８＞（ポリウレタンＨ樹脂分散体の合成）
製造例１のＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で１．５時間とし、反応停止時の重量平均分子量が７８００とした意外は、同様の方法で、ポリウレタンＨ樹脂分散体の合成行なった。
＜製造例９＞（ポリウレタンＩ樹脂分散体の合成）
製造例１のＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で８時間とし、反応停止時の重量平均分子量が１７４００とした意外は、同様の方法で、ポリウレタンＩ樹脂分散体の合成行なった。
＜製造例１０＞（ポリウレタンＪ樹脂分散体の合成）
製造例１の重量平均分子量２０００のＰＰＧ４８０ｇの代わりに、重量平均分子量７００のＰＰＧ ４８０ｇを用い、ＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で６時間とし、反応停止時の重量平均分子量が１５３００とした意外は、同様の方法で、ポリウレタンＪ樹脂分散体の合成行なった
＜製造例１１＞（ポリウレタンＫ樹脂分散体の合成）
製造例１の重量平均分子量２０００のＰＰＧ４８０ｇの代わりに、重量平均分子量３２００のＰＰＧ ４８０ｇを用い、ＤＭＰＡ、ＮＰＧ、ＭＥＫを添加後の反応時間を７５℃で６時間とし、反応停止時の重量平均分子量が１５２００とした意外は、同様の方法で、ポリウレタンＫ樹脂分散体の合成行なった
<Production Example 4> (Synthesis of polyurethane D resin dispersion)
The polyurethane D resin dispersion was synthesized in the same manner except that the reaction time after addition of DMPA, NPG and MEK in Production Example 1 was 7 hours at 75 ° C. and the weight average molecular weight at the time of the reaction stop was 16500. <Production Example 5> (Synthesis of polyurethane E resin dispersion)
Instead of 480 g of PPG having a weight average molecular weight of 2000 in Production Example 1, 480 g of PPG having a weight average molecular weight of 1000 was used, the reaction time after addition of DMPA, NPG, and MEK was 6 hours at 75 ° C., and the weight average molecular weight at the time when the reaction was stopped The polyurethane E resin dispersion was synthesized in the same manner except that 15,000 was 15,000 <Production Example 6> (Synthesis of polyurethane F resin dispersion)
Instead of 480 g of PPG having a weight average molecular weight of 2000 in Production Example 1, 480 g of PTMG having a weight average molecular weight of 2000 was used, the reaction time after addition of DMPA, NPG, and MEK was 6 hours at 75 ° C., and the weight average molecular weight when the reaction was stopped The polyurethane F resin dispersion was synthesized in the same manner except that 1 was 15000 <Production Example 7> (Synthesis of polyurethane G resin dispersion)
Instead of 480 g of PPG having a weight average molecular weight of 2000 in Production Example 1, 480 g of PEG having a weight average molecular weight of 2000 was used, the reaction time after addition of DMPA, NPG, and MEK was 6 hours at 75 ° C., and the weight average molecular weight when the reaction was stopped The polyurethane G resin dispersion was synthesized in the same manner except that the value of 15200 was 15200 <Production Example 8> (Synthesis of polyurethane H resin dispersion)
The reaction time after adding DMPA, NPG, and MEK in Production Example 1 was 1.5 hours at 75 ° C., and the weight average molecular weight at the time of stopping the reaction was 7800. Synthesis was performed.
<Production Example 9> (Synthesis of polyurethane I resin dispersion)
The polyurethane I resin dispersion was synthesized by the same method except that the reaction time after addition of DMPA, NPG and MEK in Production Example 1 was 8 hours at 75 ° C. and the weight average molecular weight at the time of the reaction stop was 17400. It was.
<Production Example 10> (Synthesis of polyurethane J resin dispersion)
Instead of 480 g of PPG having a weight average molecular weight of 2000 in Production Example 1, 480 g of PPG having a weight average molecular weight of 700 was used, the reaction time after addition of DMPA, NPG, and MEK was 6 hours at 75 ° C., and the weight average molecular weight when the reaction was stopped The polyurethane J resin dispersion was synthesized in the same manner except that the product was 15300 <Production Example 11> (Synthesis of polyurethane K resin dispersion)
Instead of 480 g of PPG having a weight average molecular weight of 2000 in Production Example 1, 480 g of PPG having a weight average molecular weight of 3200 was used, and the reaction time after addition of DMPA, NPG, and MEK was 6 hours at 75 ° C., and the weight average molecular weight when the reaction was stopped The polyurethane K resin dispersion was synthesized by the same method except that the value of 15200 was 15200.
＜顔料分散体の作成＞
冷却用ジャケットを備えた混合槽に、任意の顔料（例：BASF製 マゼンタ顔料Ｃｒｏｍｏｐｈｔａｌ Ｊｅｔ Ｍａｇｅｎｎｔａ ２ＢＣ）４５０部と、ＷＨＬ−７０１（ＤＩＣ（株）製、スチレン−アクリル系樹脂４３．４％を含むＩＰＡとＭＥＫの比率８：２の溶液）２５９部、２５％水酸化ナトリウム水溶液７７．５部、イソプロピルアルコール７８部 イオン交換水１０１０部を仕込み、スリーワンモーターで１時間攪拌し混合した。得られた混合液を直径０．３ｍｍのジルコニアビーズを充填した分散装置（ＳＣミル ＳＣ１００／３２型、三井鉱山（株）製）に通し、循環方式（分散装置より出た分散液を混合槽に戻す方式）により分散した。分散工程中は、冷却用ジャケットに冷水を通して分散液温度を３０℃以下に保つよう制御し、分散装置のローター周速を１１．２５ｍ／秒に固定して４．５時間分散した。分散終了後、混合槽より分散原液を抜き採り、次いで水１４００部で混合槽および分散装置流路を洗浄し、分散原液と合わせてミル分散液を得た。
ガラス製蒸留装置にミル分散液を入れ、イソプロピルアルコールおよびメチルエチルケトンの全量と水の一部を留去した。室温まで放冷後、攪拌しながら２％塩酸を滴下してｐＨ４．５に調整した後、固形分をヌッチェ式濾過装置で濾過、水洗した。水洗後、分散液に含有されるＣａ Ｍｇ Ｓｉは５０ＰＰＭ以下に減少していることを確認した。ケーキを容器に採り、２５％水酸化ナトリウム水溶液部を加えた後、ディスパー（ＴＫホモディスパー２０型、特殊機化工業（株）製）にて再分散した。さらに水を加えて不揮発分２３重量％に調整後、６０００Ｇで３０分間の遠心分離処理を行って、水性の顔料分散原液を得た。
<Creation of pigment dispersion>
A mixing tank equipped with a cooling jacket contains 450 parts of an arbitrary pigment (eg, magenta pigment Cromoth Jet Magnenta 2BC manufactured by BASF) and WHL-701 (manufactured by DIC Corporation, 43.4% styrene-acrylic resin). (IPA / MEK ratio 8: 2 solution) 259 parts, 257.5% aqueous sodium hydroxide solution 77.5 parts, isopropyl alcohol 78 parts Ion-exchanged water 1010 parts were stirred and mixed with a three-one motor for 1 hour. The obtained mixed liquid is passed through a dispersion apparatus (SC mill SC100 / 32 type, manufactured by Mitsui Mining Co., Ltd.) filled with zirconia beads having a diameter of 0.3 mm, and the circulation system (dispersion liquid discharged from the dispersion apparatus is placed in the mixing tank. It was dispersed by the return method). During the dispersion step, the dispersion temperature was controlled to be kept at 30 ° C. or lower by passing cold water through the cooling jacket, and the rotor peripheral speed of the dispersion apparatus was fixed at 11.25 m / second for dispersion for 4.5 hours. After the dispersion, the dispersion stock solution was extracted from the mixing tank, and then the mixing tank and the dispersion device flow path were washed with 1400 parts of water, and the mill dispersion liquid was obtained together with the dispersion stock solution.
The mill dispersion was put into a glass distillation apparatus, and all of isopropyl alcohol and methyl ethyl ketone and a part of water were distilled off. After cooling to room temperature, 2% hydrochloric acid was added dropwise with stirring to adjust the pH to 4.5, and the solid content was filtered with a Nutsche filter and washed with water. After washing with water, it was confirmed that Ca Mg Si contained in the dispersion was reduced to 50 PPM or less. The cake was taken in a container, a 25% aqueous sodium hydroxide solution was added, and then redispersed with a disper (TK homodisper 20 type, manufactured by Tokushu Kika Kogyo Co., Ltd.). Further, water was added to adjust the non-volatile content to 23% by weight, followed by centrifugation at 6000 G for 30 minutes to obtain an aqueous pigment dispersion stock solution.
［実施例１］（インク１の製造方法）
上記顔料分散体の作成した顔料分散体とウレタン樹脂分散体Ａを、顔料濃度１．５〜５％、ウレタン樹脂濃度０．１５〜５．０％となるようにインクを作製した。その他成分は下記の通りである。
１，２−ヘキサンジオール ５％
グリセリン １０％
サーフィノール４６５（エアプロダクツ・アンド・ケミカル社製） １％
イオン交換水 その他
[Example 1] (Method for producing ink 1)
An ink was prepared using the pigment dispersion prepared from the pigment dispersion and the urethane resin dispersion A so that the pigment concentration was 1.5 to 5% and the urethane resin concentration was 0.15 to 5.0%. Other components are as follows.
1,2-hexanediol 5%
Glycerin 10%
Surfinol 465 (Air Products and Chemicals) 1%
Ion exchange water Other
［実施例２］（インク２の製造方法）
実施例１の樹脂分散体Ａを樹脂分散体Ｂに変更した以外は、同様にしてインクを作成した。
[Example 2] (Method for producing ink 2)
An ink was prepared in the same manner except that the resin dispersion A of Example 1 was changed to the resin dispersion B.
［実施例３］（インク３の製造方法）
実施例１の樹脂分散体Ａを樹脂分散体Ｃに変更した以外は、同様にしてインクを作成した。
[Example 3] (Method for producing ink 3)
An ink was prepared in the same manner except that the resin dispersion A in Example 1 was changed to the resin dispersion C.
［実施例４］（インク４の製造方法）
実施例１の樹脂分散体Ａを樹脂分散体Ｄに変更した以外は、同様にしてインクを作成した。
Example 4 (Method for Producing Ink 4)
An ink was prepared in the same manner except that the resin dispersion A in Example 1 was changed to the resin dispersion D.
［実施例５］（インク５の製造方法）
実施例１の樹脂分散体Ａを樹脂分散体Ｅに変更した以外は、同様にしてインクを作成した。
[Example 5] (Method for producing ink 5)
An ink was prepared in the same manner except that the resin dispersion A in Example 1 was changed to the resin dispersion E.
［比較例１］（インク６の製造方法）
製造例１の樹脂分散体Ａを樹脂分散体Ｆに変更した以外は、同様にしてインクを作成した。
[Comparative Example 1] (Method for producing ink 6)
An ink was prepared in the same manner except that the resin dispersion A in Production Example 1 was changed to the resin dispersion F.
［比較例２］（インク７の製造方法）
製造例１の樹脂分散体Ａを樹脂分散体Gに変更した以外は、同様にしてインクを作成した。
[Comparative Example 2] (Method for producing ink 7)
An ink was prepared in the same manner except that the resin dispersion A in Production Example 1 was changed to the resin dispersion G.
［比較例３］（インク８の製造方法）
製造例１の樹脂分散体Ａを樹脂分散体Hに変更した以外は、同様にしてインクを作成した。
[Comparative Example 3] (Method for Producing Ink 8)
An ink was prepared in the same manner except that the resin dispersion A in Production Example 1 was changed to the resin dispersion H.
［比較例４］（インク９の製造方法）
製造例１の樹脂分散体Ａを樹脂分散体Iに変更した以外は、同様にしてインクを作成した。
[Comparative Example 4] (Method for producing ink 9)
An ink was prepared in the same manner except that the resin dispersion A in Production Example 1 was changed to the resin dispersion I.
［比較例５］（インク１０の製造方法）
製造例１の樹脂分散体Ａを樹脂分散体Jに変更した以外は、同様にしてインクを作成した。
[Comparative Example 5] (Method for producing ink 10)
An ink was prepared in the same manner except that the resin dispersion A in Production Example 1 was changed to the resin dispersion J.
［比較例６］（インク１１の製造方法）
製造例１の樹脂分散体Ａを樹脂分散体Kに変更した以外は、同様にしてインクを作成した。
比較例１〜比較例６
[Comparative Example 6] (Production Method of Ink 11)
An ink was prepared in the same manner except that the resin dispersion A in Production Example 1 was changed to the resin dispersion K.
Comparative Examples 1 to 6
＜評価方法＞
作製したインクを任意の吐出回数を設定できるインクジェット試験機（例：Ｍｉｃｒｏ ｊｅｔ社製 Ｌａｂｏ Ｊｅｔ−５００）を用いて以下の要領で吐出試験を行なう。液滴速度の測定は、高速度カメラ（キーエンス社製 ＶＷ−９００）を用いて行った。
評価内容は下記の通りである。
１．連続吐出を行なう。
２．高速度カメラなどで液滴のスピードを測定する。
３．吐出を停止する。30秒。
４．5滴吐出させる。このとき、下部の紙は一定速度でスライドさせる。
５．1滴目の吐出速度を測定する。（吐出再開時の液滴の吐出速度を測定する。）
６．5滴分印刷された紙を観察し、着弾ずれなどの有無を確かめる。（着弾ズレの有無を測定する。）
<Evaluation method>
A discharge test is performed in the following manner using an ink jet tester (for example, Labo Jet-500 manufactured by Micro Jet) that can set an arbitrary number of discharges for the prepared ink. The measurement of the droplet velocity was performed using a high-speed camera (VW-900 manufactured by Keyence Corporation).
The evaluation contents are as follows.
1. Perform continuous discharge.
2. Measure the droplet speed with a high-speed camera.
3. Stop dispensing. 30 seconds.
4.5 Discharge 5 drops. At this time, the lower paper is slid at a constant speed.
5. Measure the discharge speed of the first drop. (Measures the discharge speed of the liquid droplet when the discharge is resumed.)
6. Observe the paper printed for 5 drops and check for any landing misalignment. (Measure the presence or absence of landing deviation.)
＜発一性試験＞
発一性は下記の式で求める。
発一性=吐出再開時の速度/連続吐出時の速度
発一性評価のスコアは下記の通りである。
０：吐出再開時に吐出しない。
１：発一性０．２以下。
２：発一性０．２〜０．４
３：発一性０．４〜０．６
４：発一性０．６〜０．８
５：発一性０．８以上
<Uniformity test>
Uniformity is obtained by the following formula.
Uniformity = Velocity at resumption of discharge / Score of evaluation of velocity uniformity at the time of continuous discharge is as follows.
0: Does not discharge when restarting discharge.
1: Less than 0.2.
2: Uniformity 0.2-0.4
3: Uniformity 0.4 to 0.6
4: Uniformity 0.6-0.8
5: Uniformity 0.8 or more
＜着弾ズレテスト＞
上記評価方法の４の一定速度でスライドさせた紙に並んでいる五つの液滴が均等かつ直線上に並んでいるか確認を行なう。
<Landing deviation test>
It is confirmed whether the five droplets arranged on the paper slid at a constant speed of 4 in the evaluation method are arranged evenly and on a straight line.
＜吐出速度＞
上記評価方法の連続吐出時の吐出速度を比較する。
<Discharge rate>
The discharge speed at the time of continuous discharge in the above evaluation method is compared.
評価結果を表１及び表２にまとめた。 The evaluation results are summarized in Tables 1 and 2.
表１および表２の結果から明らかなように、構成成分であるポリオールを分子量１０００〜２０００程度のＰＰＧ、重合反応停止後の分子量を８７００〜１６５００程度とした場合のみ、良好な発一性を得られる。 As is apparent from the results of Tables 1 and 2, only when the polyol as a constituent component is PPG having a molecular weight of about 1000 to 2000 and the molecular weight after the termination of the polymerization reaction is about 8700 to 16500, good unidirectionality is obtained. It is done.
Claims (4)
顔料１００部あたり、スチレン−アクリル樹脂１０〜７０部で分散した水性顔料分散体と、少なくともポリプロピレングリコール、ジイソシアネート化合物、及び２価以下の酸性基を持つ２〜３官能のアルコールから構成されるポリウレタン樹脂粒子分散体と、からなり、
前記ポリウレタン樹脂の酸価が５２±１０ｍｇＫＯＨ／ｇであり、
前記ポリウレタン樹脂のポリスチレン換算重量平均分子量（Ｍｗ）が、８０００〜１７０００であり、
前記ポリウレタン樹脂を構成するポリプロピレングリコールの重量平均分子量（Ｍｗ）が１０００〜２０００であり、
前記ポリウレタン樹脂中のポリプロピレングリコール構造の含有量が４０重量％〜７０重量％であることを特徴とするインクジェット記録用水性インク調整のための水性顔料分散体。 An aqueous pigment dispersion for preparing an inkjet recording water-based ink in which a pigment and a film-forming resin are dispersed in an aqueous medium,
A polyurethane resin composed of an aqueous pigment dispersion dispersed with 10 to 70 parts of styrene-acrylic resin per 100 parts of pigment, and at least a polypropylene glycol , a diisocyanate compound, and a difunctional or trifunctional alcohol having a divalent or less acidic group. and particle dispersion, consists of,
The acid value of the polyurethane resin is 52 ± 10 mg KOH / g,
The polyurethane resin has a polystyrene equivalent weight average molecular weight (Mw) of 8000 to 17000,
The weight average molecular weight (Mw) of polypropylene glycol constituting the polyurethane resin is 1000 to 2000,
A water-based pigment dispersion for preparing a water-based ink for ink-jet recording, wherein the content of the polypropylene glycol structure in the polyurethane resin is 40% by weight to 70% by weight .
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