JPH11228857A - Pigment composition and water borne pigment dispersion using the same - Google Patents
Pigment composition and water borne pigment dispersion using the sameInfo
- Publication number
- JPH11228857A JPH11228857A JP10259064A JP25906498A JPH11228857A JP H11228857 A JPH11228857 A JP H11228857A JP 10259064 A JP10259064 A JP 10259064A JP 25906498 A JP25906498 A JP 25906498A JP H11228857 A JPH11228857 A JP H11228857A
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- pigment
- water
- weight
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- pigment composition
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- 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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- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、水性塗料、水性イ
ンキ、捺染、自動車塗料、カラーフィルター、ジェット
インキ等の水系顔料分散体を製造する際に使用する顔料
組成物および水系顔料分散体に関する。The present invention relates to a pigment composition and a water-based pigment dispersion used for producing a water-based pigment dispersion such as a water-based paint, a water-based ink, textile printing, an automobile paint, a color filter, and a jet ink.
【０００２】[0002]
【従来の技術】従来、水系顔料分散体用の顔料を製造す
る方法としては、無機塩および助剤の存在下においてボ
ールミルまたはニーダー中において粗製顔料を長時間摩
砕し、続いてさらに無機塩および助剤を除去することに
よって顔料化する。さらにこれを用いて水系分散体を製
造する方法としてはサンドミルなどの分散機を使用して
顔料の乾燥凝集状態を解しインキビヒクル中に分散する
ことを必要とした。したがって、この方法では顔料化に
おいて無機塩および助剤の回収やそれに対する廃水処理
に大きなエネルギーを必要とし、また水系顔料分散体を
製造するためにも大きな分散エネルギーが必要とする欠
点がある。2. Description of the Related Art Conventionally, as a method for producing a pigment for an aqueous pigment dispersion, a crude pigment is milled for a long time in a ball mill or a kneader in the presence of an inorganic salt and an auxiliary agent, followed by further grinding the inorganic salt and It is pigmented by removing the auxiliaries. Further, as a method for producing an aqueous dispersion using this, it was necessary to disperse the pigment in the ink vehicle by using a disperser such as a sand mill to disperse the dried and aggregated state of the pigment. Therefore, this method has a disadvantage that a large amount of energy is required for the recovery of the inorganic salt and the auxiliary agent and the treatment of the wastewater therefor in the pigmentation, and a large amount of dispersion energy is required for producing the aqueous pigment dispersion.
【０００３】これらの問題を解決すべく、特開昭55-754
53号公報には、粗銅フタロシアニンと界面活性剤を乾式
粉砕して得られた顔料組成物を水/ 溶剤中で処理するこ
とにより容易に分散する顔料の製造方法について公開さ
れている。しかしながら、この製造方法では、溶剤処理
において排出される廃溶剤の回収作業が必要であり、ま
た分散性は不十分であった。また、特開平9-217019号公
報には、第一工程で粗製顔料を乾式粉砕し、第二工程で
樹脂および有機溶剤を機械的に分散させ、第三工程で分
散物に酸を加えて樹脂を析出させ、さらに、第四工程で
アルカリを加えて再中和することにより顔料組成物製造
する方法が提案されている。この方法は室温で水中に攪
拌することにより容易に分散する顔料組成物を製造でき
るが、製造工程が長く樹脂を処理するエネルギーが大き
い欠点がある。In order to solve these problems, Japanese Patent Application Laid-Open No. 55-754
No. 53 discloses a method for producing a pigment which can be easily dispersed by treating a pigment composition obtained by dry-milling crude copper phthalocyanine and a surfactant in water / solvent. However, in this production method, it is necessary to collect the waste solvent discharged in the solvent treatment, and the dispersibility is insufficient. Further, JP-A-9-217019 discloses that, in a first step, a crude pigment is dry-pulverized, a resin and an organic solvent are mechanically dispersed in a second step, and an acid is added to the dispersion in a third step. Has been proposed to produce a pigment composition by precipitating and then re-neutralizing by adding an alkali in a fourth step. This method can produce a pigment composition which can be easily dispersed by stirring in water at room temperature, but has a disadvantage that the production process is long and the energy for treating the resin is large.
【０００４】特開平9-188845号公報には、粗銅フタロシ
アニンを樹脂および有機液体とともに乾式粉砕し、得ら
れた顔料組成物をインキ溶剤中に混練りしてインキ濃縮
物を製造する方法が提案されている。この方法は製造工
程が簡便であるが顔料組成物を分散しインキ濃縮物を作
るための混練りをする工程に大きなエネルギーが必要で
ある。Japanese Patent Application Laid-Open No. Hei 9-188845 proposes a method for producing an ink concentrate by dry-pulverizing crude copper phthalocyanine together with a resin and an organic liquid, and kneading the obtained pigment composition in an ink solvent. ing. This method has a simple manufacturing process, but requires a large amount of energy in the kneading process for dispersing the pigment composition to form an ink concentrate.
【０００５】[0005]
【発明が解決しようとする課題】本発明者らは、驚くべ
きことに、大量の水や溶剤を使用せず、単一工程で製造
でき、水系で容易に分散する顔料組成物を見出した。こ
の顔料組成物をアルカリを含む水中に投入、攪拌するこ
とにより容易に水系顔料分散体となる。この水系顔料分
散体は優れた分散性、着色力、光沢および流動特性を有
する水性インキとなる。SUMMARY OF THE INVENTION The present inventors have surprisingly found a pigment composition which can be produced in a single step without using a large amount of water or a solvent and which can be easily dispersed in an aqueous system. An aqueous pigment dispersion can be easily obtained by charging and stirring the pigment composition in water containing alkali. This aqueous pigment dispersion becomes an aqueous ink having excellent dispersibility, tinting strength, gloss and flow characteristics.
【０００６】[0006]
【課題を解決するための手段】本発明は、顔料を、該顔
料に対して１〜20重量％の界面活性剤および該顔料に対
して２〜50重量％の水溶性樹脂の存在下に乾式粉砕して
なる粉体状の顔料組成物に関する。SUMMARY OF THE INVENTION The present invention relates to a method for preparing a pigment in a dry form in the presence of 1 to 20% by weight of a surfactant based on the pigment and 2 to 50% by weight of a water-soluble resin based on the pigment. The present invention relates to a powdery pigment composition obtained by pulverization.
【０００７】更に本発明は、顔料が粗製顔料である上記
顔料組成物に関する。更に本発明は顔料が縮合多環系顔
料である上記顔料組成物に関する。更に本発明は、界面
活性剤がエチレンオキシドが付加した芳香族系化合物で
ある上記顔料組成物に関する。[0007] The present invention further relates to the above pigment composition, wherein the pigment is a crude pigment. Furthermore, the present invention relates to the above pigment composition, wherein the pigment is a condensed polycyclic pigment. Furthermore, the present invention relates to the above pigment composition, wherein the surfactant is an aromatic compound to which ethylene oxide is added.
【０００８】更に本発明は、水溶性樹脂が酸性基を有し
アルカリの存在下に水に溶解する樹脂である上記顔料組
成物に関する。更に本発明は、水溶性樹脂が固体樹脂で
ある上記顔料組成物関する。Further, the present invention relates to the above pigment composition, wherein the water-soluble resin is a resin having an acidic group and soluble in water in the presence of an alkali. Furthermore, the present invention relates to the above pigment composition, wherein the water-soluble resin is a solid resin.
【０００９】更に本発明は、顔料を界面活性剤および水
溶性樹脂の存在下に乾式粉砕する粉体状の顔料組成物の
製造方法であって、上記乾式粉砕時および／または乾式
粉砕後に加熱処理することを特徴とする粉体状の顔料組
成物の製造方法に関する。Further, the present invention relates to a method for producing a powdery pigment composition in which a pigment is dry-pulverized in the presence of a surfactant and a water-soluble resin, wherein a heat treatment is carried out during the dry pulverization and / or after the dry pulverization. And a method for producing a powdery pigment composition.
【００１０】更に本発明は、顔料に水溶性樹脂のみを添
加して乾式粉砕し、次いで界面活性剤を添加して乾式粉
砕する請求項７記載の粉体状の顔料組成物の製造方法に
関する。更に本発明は、乾式粉砕時の加熱温度が30〜15
0 ℃である上記製造方法に関する。更に本発明は、乾式
粉砕後の加熱処理温度が50〜150 ℃である上記製造方法
に関する。Further, the present invention relates to a method for producing a powdery pigment composition according to claim 7, wherein the pigment is dry-ground by adding only a water-soluble resin to the pigment and then dry-ground by adding a surfactant. Further, the present invention, the heating temperature during dry pulverization is 30 to 15
The present invention relates to the above production method at 0 ° C. Further, the present invention relates to the above-mentioned production method, wherein the heat treatment temperature after dry pulverization is 50 to 150 ° C.
【００１１】更に本発明は、乾式粉砕がアトライター、
ボールミルおよび振動ミルからなる群から選ばれる一種
の粉砕装置を使用する上記製造方法に関する。更に本発
明は、上記顔料組成物を水中に分散してなる水系顔料分
散体に関する。[0011] The present invention further provides an attritor,
The present invention relates to the above production method using a kind of pulverizing device selected from the group consisting of a ball mill and a vibration mill. Furthermore, the present invention relates to an aqueous pigment dispersion obtained by dispersing the above pigment composition in water.
【００１２】[0012]
【発明の実施の形態】本発明の顔料は特に限定されない
が、例えば、フタロシアニン系粗顔料、キナクリドン系
粗顔料、ジオキサジン系粗顔料等の縮合多環系の粗製顔
料が好ましい。粗製顔料は、一般に発色不良のため通常
の色材としての適正を欠くものであり、粒子径としては
１０〜６０μｍである。又、本発明においては平均粒径
が０．３〜０．５μｍ程度の市販の顔料を粉砕原料とし
て使用することもでき、この場合には粉砕して得られる
顔料の平均粒径を０．０１〜０．０３μｍ程度となる。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The pigment of the present invention is not particularly limited. For example, a crude condensed polycyclic pigment such as a crude phthalocyanine pigment, a crude quinacridone pigment or a crude dioxazine pigment is preferred. A crude pigment generally lacks appropriateness as a normal coloring material due to poor color development, and has a particle size of 10 to 60 μm. In the present invention, a commercially available pigment having an average particle size of about 0.3 to 0.5 μm can be used as a raw material for pulverization. In this case, the average particle diameter of the pigment obtained by pulverization is 0.01 to 0.01 μm. About 0.03 μm.
【００１３】本発明の乾式粉砕は、ビーズ等の粉砕メデ
ィアを内蔵した粉砕装置を使用して、顔料を粉体の形態
を維持したまま粉砕するものである。粉砕は、粉砕メデ
ィア同士の衝突による粉砕力や破壊力を利用し、粉砕助
剤としての水溶性無機塩を添加しないで行われる。乾式
粉砕中、粉体としての形態を維持できる範囲で水や水溶
性溶剤を添加しても良い。粉砕装置としては、乾式のア
トライター、ボールミル、振動ミルなどの公知の方法を
用いることができる。生産効率の点からアトライターが
好ましい。In the dry pulverization of the present invention, a pigment is pulverized using a pulverizer incorporating a pulverizing medium such as beads while maintaining the form of the powder. The pulverization is performed without using a water-soluble inorganic salt as a pulverization aid, using a pulverizing force or a destructive force due to collision between pulverizing media. During dry pulverization, water or a water-soluble solvent may be added as long as the form as a powder can be maintained. As the pulverizer, a known method such as a dry attritor, a ball mill, and a vibration mill can be used. Attritors are preferred in terms of production efficiency.
【００１４】本発明の界面活性剤は、水系顔料分散体の
分散安定化に通常使用されている界面活性剤が使用でき
る。好ましい界面活性剤としては、エチレンオキシド等
のアルキレンオキシドが４〜40モル付加した親水性部
と、置換もしくは無置換のベンゼン、ナフタレン、アン
トラセン、ビフェニル等の芳香族環が疎水性部として作
用するものが好ましい。これらの界面活性剤として、例
えば、ポリオキシエチレンアルキルフェニルエーテル、
ポリオキシエチレンスルホン酸アルキルフェニルエーテ
ル、ポリオキシエチレンナフチルオキシエーテル、ポリ
オキシエチレンスルホン酸ナフチルオキシエーテルなど
が例示できる。As the surfactant of the present invention, a surfactant generally used for stabilizing the dispersion of an aqueous pigment dispersion can be used. Preferred surfactants include those in which 4 to 40 moles of an alkylene oxide such as ethylene oxide is added, and those in which an aromatic ring such as a substituted or unsubstituted benzene, naphthalene, anthracene, or biphenyl acts as a hydrophobic part. preferable. As these surfactants, for example, polyoxyethylene alkyl phenyl ether,
Examples include polyoxyethylene sulfonic acid alkyl phenyl ether, polyoxyethylene naphthyl oxy ether, and polyoxyethylene sulfonic acid naphthyl oxy ether.
【００１５】界面活性剤の使用量は、粗製顔料に対して
１〜20重量％、好ましくは、２〜１２重量％である。界
面活性剤の使用量が上記上限より多くなると、乾式粉砕
装置内部での顔料組成物が粉体の形態を維持できなくな
り、固着が生じるので好ましくなく、又、上記下限より
少なくなると顔料組成物が水中で解膠、分散せず顔料凝
集体として存在し発色しないので好ましくない。The amount of the surfactant used is 1 to 20% by weight, preferably 2 to 12% by weight, based on the crude pigment. When the amount of the surfactant is more than the above upper limit, the pigment composition inside the dry pulverizer cannot maintain the form of the powder, it is not preferable because sticking occurs, and when the amount is less than the above lower limit, the pigment composition becomes It is not preferable because it does not peptize or disperse in water, and is present as a pigment aggregate and does not develop color.
【００１６】本発明の水溶性樹脂は、乾式粉砕時または
乾式粉砕後の加熱処理において溶融したり、軟化して粉
砕物が固着しないような固体の状態のもので、好ましく
はカルボキシル基やスルホン基などの酸性基を有するも
のである。具体的には、カルボキシル基を有する水溶性
樹脂としては、アクリル樹脂、アクリル−スチレン共重
合体、アクリル−α−メチルスチレン共重合体、マレイ
ン酸樹脂、マレイン酸−スチレン共重合体があり、アク
リル酸、メタクリル酸、マレイン酸、イタコン酸、部分
エステル化マレイン酸等のアルカリ成分の存在下に水溶
性となりえるモノマー成分を含むものである。また、ス
ルホン基を有する水溶性樹脂としては、アクリル-3-ス
ルホプロピルエステル、メタクリル-3-スルホプロピル
エステル、スチレンスルホン酸などをモノマーの一部と
して使用した樹脂がある。以上は使用できる樹脂の一例
であり、共重合により酸性基を導入できる樹脂であれば
使用できる。また、これらの他に、樹脂を変性すること
により、カルボキシル基やスルホン基を導入した水溶性
樹脂も使用できる。粉砕工程において配合される水溶性
樹脂はペレット状形態であると操作上好ましい。The water-soluble resin of the present invention is in a solid state such that it does not melt or soften in the heat treatment during dry pulverization or heat treatment after dry pulverization so that the pulverized material does not adhere. And the like having an acidic group such as Specifically, examples of the water-soluble resin having a carboxyl group include an acrylic resin, an acrylic-styrene copolymer, an acrylic-α-methylstyrene copolymer, a maleic acid resin, and a maleic acid-styrene copolymer. It contains a monomer component that can become water-soluble in the presence of an alkali component such as an acid, methacrylic acid, maleic acid, itaconic acid, and partially esterified maleic acid. Examples of the water-soluble resin having a sulfone group include resins using acryl-3-sulfopropyl ester, methacryl-3-sulfopropyl ester, styrenesulfonic acid and the like as a part of the monomer. The above is an example of a resin that can be used, and any resin that can introduce an acidic group by copolymerization can be used. In addition, a water-soluble resin into which a carboxyl group or a sulfone group is introduced by modifying the resin can be used. The operation of the water-soluble resin blended in the pulverizing step is preferably in the form of pellets.
【００１７】水溶性樹脂の使用量は、顔料に対して２〜
50重量％、好ましくは５〜２０重量％である。水溶性樹
脂の使用量が上記上限より多くなると、分散体に使用す
る樹脂が本発明の顔料組成物で使用した樹脂に制約され
るので好ましくなく、又、上記下限より少なくなると粉
砕時の凝集防止効果が発揮されず、顔料組成物が水中で
解膠しないため発色不良となり好ましくない。使用する
界面活性剤と水溶性樹脂は夫々の機能を発揮して水中へ
の分散に対し加算効果を与えているのみではなく、夫々
が互いに相溶して相乗効果を与えることによって水中に
容易に分散する分散体が得られるのである。The amount of the water-soluble resin used is 2 to
It is 50% by weight, preferably 5 to 20% by weight. When the amount of the water-soluble resin is more than the upper limit, the resin used in the dispersion is restricted by the resin used in the pigment composition of the present invention, which is not preferable. The effect is not exhibited, and the pigment composition is not deflocculated in water. The surfactant and the water-soluble resin used not only exert their respective functions to give an additive effect to the dispersion in water, but also easily dissolve in water by being compatible with each other to give a synergistic effect. A dispersion that disperses is obtained.
【００１８】本発明の乾式粉砕は、粉砕温度を30〜150
℃で行うことが好ましい。粉砕温度は使用する装置によ
り設定する。しかし、粉砕温度が使用する樹脂の軟化点
より高くなると乾式粉砕装置内部での固着が生じるの
で、使用する樹脂の軟化点よりなるべく低く設定する必
要がある。粉砕時間は粉砕装置の種類によって異なる
が、10分〜６時間で行うことが好ましい。粗製顔料を使
用する場合には、粉砕時間が短いと粗製顔料が粉砕され
ないため分散した顔料粒子は不均一になる。また、生産
効率からあまり長くする必要がない。In the dry pulverization of the present invention, the pulverization temperature is from 30 to 150.
It is preferably carried out at a temperature of ° C. The pulverization temperature is set according to the equipment used. However, if the pulverization temperature is higher than the softening point of the resin used, sticking occurs inside the dry pulverizer, so it is necessary to set the pulverization temperature as low as possible. Although the pulverization time varies depending on the type of the pulverizer, it is preferable to perform the pulverization in 10 minutes to 6 hours. When a crude pigment is used, if the pulverization time is short, the coarse pigment is not pulverized, so that the dispersed pigment particles become non-uniform. Further, it is not necessary to make the length too long in terms of production efficiency.
【００１９】本発明の顔料組成物の製造方法は、乾式粉
砕中か乾式粉砕後、加熱処理を行う。勿論、乾式粉砕中
と後の両方で加熱処理をすることができる。In the method for producing a pigment composition of the present invention, a heat treatment is performed during or after dry pulverization. Of course, heat treatment can be performed both during and after the dry pulverization.
【００２０】本発明で乾式粉砕工程で得られた顔料組成
物を加熱処理することにより分散粒子の大きさや形状、
結晶構造などをコントロールすることが可能である。つ
まり、顔料分散粒子の大きさや形状を整えられ、色相や
着色力を変えることができる。又、縮合多環系顔料の一
部は結晶型をいくつか有し、その構造により色相や着色
力が異なる。例えば、銅フタロシアニン顔料は結晶構造
をいくつか有し、α型結晶構造では色相が赤味になりβ
型結晶構造では色相が黄味になる。これらの結晶構造は
お互い平衡関係にあり、熱などのエネルギーにより転移
するので、加熱処理により顔料の結晶構造を変化させる
ことができる。The pigment composition obtained in the dry pulverization step of the present invention is subjected to a heat treatment so that the size and shape of the dispersed particles are reduced.
It is possible to control the crystal structure and the like. That is, the size and shape of the pigment-dispersed particles can be adjusted, and the hue and coloring power can be changed. Some of the condensed polycyclic pigments have several crystal forms, and the hue and tinting power vary depending on the structure. For example, a copper phthalocyanine pigment has several crystal structures, and in an α-type crystal structure, the hue becomes reddish and β
The hue becomes yellowish in the type crystal structure. Since these crystal structures are in equilibrium with each other and are transferred by energy such as heat, the crystal structure of the pigment can be changed by heat treatment.
【００２１】乾式粉砕後の加熱処理装置は、箱形乾燥
機、バンド乾燥機など加熱処理できる装置であれば種類
は問わない。乾式粉砕後の加熱処理温度および加熱処理
時間は、目的の顔料組成物により設定する必要があるた
め、希望とする顔料粒子の大きさや形状、結晶構造に応
じて任意に設定すればよい。加熱処理温度が低いと処理
時間が長くなり、温度が高いと大きなエネルギーが必要
である。したがって、加熱処理温度が50〜150 ℃が好ま
しい。The type of the heat treatment device after the dry pulverization is not particularly limited as long as it can be subjected to heat treatment such as a box dryer or a band dryer. Since the heat treatment temperature and the heat treatment time after the dry pulverization need to be set according to the target pigment composition, they may be set arbitrarily according to the desired size, shape, and crystal structure of the pigment particles. When the heat treatment temperature is low, the treatment time becomes long, and when the temperature is high, large energy is required. Therefore, the heat treatment temperature is preferably 50 to 150 ° C.
【００２２】本発明の顔料組成物は、顔料の表面を界面
活性剤と樹脂が被覆した、流動性のある粉体状の組成物
である。粉体の粒径は５〜１００μｍの範囲にある。
又、この粉体を水中に分散した時の顔料粒子径は、乾式
粉砕工程や加熱処理工程の条件により調整でき、０．０
１〜０．３μｍであり、ソルベントソルトミリング法に
より得られた顔料粒子とほぼ同じレベルにもなる。The pigment composition of the present invention is a flowable powdery composition in which the surface of a pigment is coated with a surfactant and a resin. The particle size of the powder is in the range from 5 to 100 μm.
The pigment particle size when this powder is dispersed in water can be adjusted by the conditions of the dry pulverization step and the heat treatment step.
1 to 0.3 μm, which is almost the same level as the pigment particles obtained by the solvent salt milling method.
【００２３】本発明の顔料組成物は、アルカリ金属、ア
ミン、アンモニア等のアルカリ存在下で水中に容易に解
膠し分散し、水性顔料分散体となる。この際、水中に水
系顔料分散体用ビヒクルを存在させていてもよい。又、
本発明の顔料組成物を、一旦、アルカリを含む水中に分
散させて濃縮分散体とし、次いで、この濃縮分散体をバ
インダー樹脂を含む最終製品のビヒクルに分散させても
よい。アルカリの使用量は使用した樹脂に含まれる酸性
基に対し１．０〜１．４当量である。The pigment composition of the present invention is easily peptized and dispersed in water in the presence of an alkali such as an alkali metal, an amine or ammonia to form an aqueous pigment dispersion. At this time, a vehicle for an aqueous pigment dispersion may be present in water. or,
The pigment composition of the present invention may be once dispersed in water containing alkali to form a concentrated dispersion, and then the concentrated dispersion may be dispersed in a vehicle of a final product containing a binder resin. The amount of the alkali used is 1.0 to 1.4 equivalents to the acidic group contained in the resin used.
【００２４】本発明の製造方法で得られる顔料組成物を
用いた水系顔料分散体としては、例えば、水性塗料、捺
染剤、水性インキ、インキジェット用インキ、カラーフ
ィルター用の分散液等が挙げられるが、これらの用途に
限定されるものではない。The aqueous pigment dispersion using the pigment composition obtained by the production method of the present invention includes, for example, aqueous paints, printing agents, aqueous inks, inks for ink jet, and dispersions for color filters. However, it is not limited to these uses.
【００２５】[0025]
【実施例】以下、実施例、比較例により本発明を具体的
に説明する。なお、実施例１〜６および比較例１〜２で
標準インキとして使用しているのは、比較例３で作成し
た粗製顔料をソルベントソルトミリングにより顔料化し
たものである。なお、実施例および比較例で得られた銅
フタロシアニン顔料濃縮分散体のα化度、平均分散粒子
径、分散安定性の評価は、下記の方法で行った。The present invention will be specifically described below with reference to examples and comparative examples. In addition, what is used as a standard ink in Examples 1 to 6 and Comparative Examples 1 and 2 is obtained by converting the crude pigment prepared in Comparative Example 3 into a pigment by solvent salt milling. The degree of α-formation, average dispersed particle diameter, and dispersion stability of the copper phthalocyanine pigment concentrated dispersions obtained in Examples and Comparative Examples were evaluated by the following methods.
【００２６】1)α結晶化度 RINT1000 X-ray Diffactometer(理学社製)を用いて結晶
型の測定を行い、ピークの積分強度からα型結晶の百分
率を算出した。 2)平均分散粒子径 実施例１〜6および比較例1〜2の平均粒子径は、電子顕
微鏡により測定した。実施例7〜24の平均粒子径は、レ
ーザー回折方式の粒度分布計(日機装社製「マイクロト
ラックUPA」)を用いて測定した。 3)分散安定性 50mlの蓋付きスクリュー管に濃縮分散体を30ml加え、50
℃で1週間後の沈降性を評価した。(◎:沈降物なし、○:
沈降物が高さ0.5mm未満、△:沈降物が高さ5mm未満、沈
降物が高さ5mm以上) 4)着色力、色相 着色力および色相は、実施例および比較例で作製したイ
ンキの顔料分率を同じにして塗工し、SZ Opitical Sens
or(日本電色工業社製)で測色し、80 Color Measuring S
ystem(日本電子工業社製)で解析した。1) α Crystallinity The crystal form was measured using a RINT1000 X-ray Diffactometer (manufactured by Rigaku Corporation), and the percentage of α-form crystals was calculated from the integrated intensity of the peak. 2) Average dispersed particle diameter The average particle diameter of Examples 1 to 6 and Comparative Examples 1 and 2 was measured by an electron microscope. The average particle diameters of Examples 7 to 24 were measured using a laser diffraction type particle size distribution meter (“Microtrack UPA” manufactured by Nikkiso Co., Ltd.). 3) Dispersion stability 30 ml of the concentrated dispersion was added to a 50 ml screw tube with a lid, and 50
The sedimentation after 1 week at ℃ was evaluated. (◎: No sediment, ○:
(Sediment is less than 0.5 mm in height, 物: Sediment is less than 5 mm in height, sediment is 5 mm or more in height) 4) Coloring power, hue The coloring power and hue are the pigments of the inks prepared in Examples and Comparative Examples. Coating with the same fraction, SZ Opitical Sens
or (manufactured by Nippon Denshoku Industries Co., Ltd.) and measure 80 Color Measuring S
The analysis was performed using ystem (manufactured by Nippon Denshi Kogyo).
【００２７】[0027]
【実施例１】乾式アトライターに粗製銅フタロシアニン
70重量部とアクリル系樹脂( ジョンソンポリマー社製の
「ジョンクリルJ-679 」)30 重量部を加え120 ℃で30分
間粉砕した。次に、ノニオン界面活性剤( 日本乳化剤社
製の「Newcol B13」)8重量部を加え120 ℃で15分間粉砕
した。得られた顔料組成物のα型結晶の含有率は10%以
下であった。次に、得られた顔料組成物10重量部とイオ
ン交換水10重量部と樹脂を溶解するために25% 水酸化ナ
トリウム溶液１．６部を加え室温で緩やかに攪拌するこ
とにより濃縮分散体を得た。次に、得られた濃縮分散体
に水性塗料用ビヒクル( 大日本塗料社製「ハイライト70
0 」)400重量部加え最終インキに調整した後、同一顔料
分を含む標準インキと比較したところ、本実施例のイン
キは着色力、光沢、色相などの点において標準インキよ
り優れており着色力は140%程度の品位を有していた。こ
のインキ中に分散した顔料の平均粒径は50〜100nm であ
った。Example 1 Crude copper phthalocyanine was added to a dry attritor.
70 parts by weight and 30 parts by weight of an acrylic resin ("Johncryl J-679" manufactured by Johnson Polymer) were added and pulverized at 120 ° C for 30 minutes. Next, 8 parts by weight of a nonionic surfactant (“Newcol B13” manufactured by Nippon Emulsifier Co., Ltd.) was added, and the mixture was ground at 120 ° C. for 15 minutes. The content of α-type crystals in the obtained pigment composition was 10% or less. Next, 10 parts by weight of the obtained pigment composition, 10 parts by weight of ion-exchanged water, and 1.6 parts of a 25% sodium hydroxide solution to dissolve the resin were added, and the mixture was stirred gently at room temperature to form a concentrated dispersion. Obtained. Next, a vehicle for water-based paint ("Highlight 70" manufactured by Dainippon Paint Co., Ltd.) was added to the obtained concentrated dispersion.
0 ") 400 parts by weight, adjusted to the final ink, and compared with the standard ink containing the same pigment, the ink of this example was superior to the standard ink in terms of tinting strength, gloss, hue, etc. Had a grade of about 140%. The average particle size of the pigment dispersed in this ink was 50 to 100 nm.
【００２８】[0028]
【比較例１】乾式アトライターに粗製銅フタロシアニン
70重量部とアクリル系樹脂( ジョンソンポリマー社製の
「ジョンクリルJ-679 」)30 重量部を加え120 ℃で30分
間粉砕した。次に、得られた顔料組成物10重量部とイオ
ン交換水10重量部と樹脂を溶解するために25% 水酸化ナ
トリウム溶液１．６部を加え室温で緩やかに攪拌するこ
とにより濃縮分散体を得た。このとき得られたインキ濃
縮物は沈降が生じ、得られた濃縮分散体に水性塗料用ビ
ヒクル( 「ハイライト700 」)400重量部加え最終インキ
に調整した後、同一顔料分を含む標準インキと比較した
ところ、かなり劣るものであった。Comparative Example 1 Crude copper phthalocyanine was added to a dry attritor.
70 parts by weight and 30 parts by weight of an acrylic resin ("Johncryl J-679" manufactured by Johnson Polymer) were added and pulverized at 120 ° C for 30 minutes. Next, 10 parts by weight of the obtained pigment composition, 10 parts by weight of ion-exchanged water, and 1.6 parts of a 25% sodium hydroxide solution to dissolve the resin were added, and the mixture was stirred gently at room temperature to form a concentrated dispersion. Obtained. At this time, the obtained ink concentrate sedimented, and 400 parts by weight of a water-based paint vehicle ("Highlight 700") was added to the obtained concentrated dispersion to prepare a final ink, which was then mixed with a standard ink containing the same pigment content. In comparison, it was quite inferior.
【００２９】[0029]
【比較例２】乾式アトライターに粗製銅フタロシアニン
70重量部とノニオン界面活性剤( 日本乳化剤社製の「Ne
wcol B13」)10 重量部を加え120 ℃で30間粉砕した。次
に、得られた顔料組成物10重量部とイオン交換水10重量
部を加え室温で緩やかに攪拌することにより濃縮分散体
を得た。このとき、得られた濃縮分散体に水性塗料用ビ
ヒクル( 「ハイライト700 」)400重量部加え最終インキ
に調整した後、同一顔料分を含む標準インキと比較した
ところ、不鮮明であり着色力は70% 程度であった。Comparative Example 2 Crude copper phthalocyanine was added to a dry attritor.
70 parts by weight of a nonionic surfactant ("Ne
wcol B13 ") 10 parts by weight and pulverized at 120 ° C for 30 minutes. Next, 10 parts by weight of the obtained pigment composition and 10 parts by weight of ion-exchanged water were added, followed by gentle stirring at room temperature to obtain a concentrated dispersion. At this time, 400 parts by weight of a water-based paint vehicle ("Highlight 700") was added to the obtained concentrated dispersion, and the resulting dispersion was adjusted to a final ink.Compared with a standard ink containing the same pigment, the result was unclear and the coloring power was poor. It was about 70%.
【００３０】[0030]
【比較例３】銅フタロシアニン顔料(「FG7330」東洋イ
ンキ製造社製)70重量部、アクリル系樹脂(ジョンソンポ
リマー社製の「ジョンクリルJ-679」)30重量部、ノニオ
ン界面活性剤(日本乳化剤社製の「Newcol B13」)8部、2
5%水酸化ナトリウム水溶液1.6重量部をマヨネーズビン
に取り、ペイントコンディショナーを用いて2時間分散
させて、濃縮分散体を作製した。その後、水性塗料用ビ
ヒクル(「ハイライト700」)400重量部加え最終インキに
調整した。Comparative Example 3 70 parts by weight of a copper phthalocyanine pigment (“FG7330” manufactured by Toyo Ink Mfg. Co., Ltd.), 30 parts by weight of an acrylic resin (“Johncryl J-679” manufactured by Johnson Polymers), a nonionic surfactant (Nippon Emulsifier) (Newcol B13) 8 parts, 2
1.6 parts by weight of a 5% aqueous sodium hydroxide solution was placed in a mayonnaise bottle, and dispersed using a paint conditioner for 2 hours to prepare a concentrated dispersion. Thereafter, 400 parts by weight of a vehicle for a water-based paint ("Highlight 700") was added to prepare a final ink.
【００３１】[0031]
【実施例２】乾式アトライターに粗製銅フタロシアニン
70重量部とアクリル系樹脂( ジョンソンポリマー社製の
「ジョンクリルJ-68」)30 重量部を加え50℃で30分間粉
砕した。次に、ノニオン界面活性剤( 日本乳化剤社製の
「Newcol B13」)8重量部を加え50℃で15分間粉砕した。
得られた顔料組成物のα型結晶の含有率は55% 程度であ
った。次に、実施例１と同じ方法で濃縮分散体にし、水
性塗料用ビヒクル( 「ハイライト700 」)を400重量部加
え最終インキに調整した後、同一顔料分を含む標準イン
キと比較したところ、本実施例のインキの着色力は140%
程度で色相は赤味の品位を有していた。このインキ中に
分散された顔料の平均粒径は20〜50nmであった。Example 2 Crude copper phthalocyanine was added to a dry attritor.
70 parts by weight and 30 parts by weight of an acrylic resin (“Johncryl J-68” manufactured by Johnson Polymer) were added and pulverized at 50 ° C. for 30 minutes. Next, 8 parts by weight of a nonionic surfactant (“Newcol B13” manufactured by Nippon Emulsifier Co., Ltd.) was added, and the mixture was pulverized at 50 ° C. for 15 minutes.
The content of α-type crystals in the obtained pigment composition was about 55%. Next, a concentrated dispersion was prepared in the same manner as in Example 1, and 400 parts by weight of a vehicle for aqueous paint ("Highlight 700") was added to adjust the final ink. The coloring power of the ink of this example is 140%
The hue was of a reddish grade. The average particle size of the pigment dispersed in the ink was 20 to 50 nm.
【００３２】[0032]
【実施例３】乾式アトライターに粗製銅フタロシアニン
70重量部とアクリル系樹脂( ジョンソンポリマー社製の
「ジョンクリルJ-679 」)10 重量部を加え50℃で30分間
粉砕した。次に、ノニオン界面活性剤( 日本乳化剤社製
の「Newcol B13」)3.5重量部を加え50℃で15分間粉砕し
た。次に、顔料組成物を120 ℃で２４時間加熱処理を行
った。得られた顔料組成物のα型結晶の含有率は1%以下
であった。次に、実施例１と同じ方法で濃縮分散体に
し、水性塗料用ビヒクル( 「ハイライト700 」)を400重
量部加え最終インキに調整した後、同一顔料分を含む標
準インキと比較したところ、本実施例のインキの着色力
は同程度で色相はやや赤味の品位を有していた。このイ
ンキ中に分散された顔料の平均粒径は100 〜200nm で針
状の形態であった。Example 3 Crude copper phthalocyanine was added to a dry attritor.
70 parts by weight and 10 parts by weight of an acrylic resin ("Johncryl J-679" manufactured by Johnson Polymer) were added and pulverized at 50 ° C for 30 minutes. Next, 3.5 parts by weight of a nonionic surfactant (“Newcol B13” manufactured by Nippon Emulsifier Co., Ltd.) was added, and the mixture was pulverized at 50 ° C. for 15 minutes. Next, the pigment composition was subjected to a heat treatment at 120 ° C. for 24 hours. The content of α-type crystals in the obtained pigment composition was 1% or less. Next, a concentrated dispersion was prepared in the same manner as in Example 1, and 400 parts by weight of a vehicle for aqueous paint ("Highlight 700") was added to adjust the final ink. The coloring power of the ink of this example was almost the same, and the hue had a grade of slightly reddish. The pigment dispersed in this ink had an average particle size of 100 to 200 nm and was in the form of needles.
【００３３】[0033]
【実施例４】乾式アトライターに粗製銅フタロシアニン
70重量部とアクリル系樹脂( ジョンソンポリマー社製の
「ジョンクリルJ-679 」)10 重量部を加え120 ℃で30分
間粉砕した。次に、アニオン界面活性剤( 日本乳化剤社
製の「Newcol B4SN 」)8重量部を加え50℃で120 分間粉
砕した。得られた顔料組成物のα型結晶の含有率は20%
程度であった。次に、実施例１と同じ方法で濃縮分散体
にし、水性塗料用ビヒクル( 「ハイライト700 」)を400
重量部加え最終インキに調整した後、同一顔料分を含む
標準インキと比較したところ、本実施例のインキの着色
力、色相、光沢は標準品と同等の品位を有していた。Example 4 Crude copper phthalocyanine was added to a dry attritor.
70 parts by weight and 10 parts by weight of an acrylic resin ("Johncryl J-679" manufactured by Johnson Polymer) were added and pulverized at 120 ° C for 30 minutes. Next, 8 parts by weight of an anionic surfactant ("Newcol B4SN" manufactured by Nippon Emulsifier Co., Ltd.) was added, and pulverized at 50 ° C for 120 minutes. The content of α-type crystals in the obtained pigment composition is 20%
It was about. Next, a concentrated dispersion was prepared in the same manner as in Example 1, and a vehicle for water-based paint (“Highlight 700”) was added to 400%.
After adjusting to the final ink by adding parts by weight, when compared with a standard ink containing the same pigment, the coloring power, hue, and gloss of the ink of this example were equivalent to the standard product.
【００３４】[0034]
【実施例５】乾式アトライターに粗製銅フタロシアニン
70重量部とアクリル系樹脂( ジョンソンポリマー社製の
「ジョンクリルJ-679 」)10 重量部を加え120 ℃で30分
間粉砕した。次に、ノニオン界面活性剤( 日本乳化剤社
製の「Newcol B4SN 」)8重量部を加え120 ℃で15分間粉
砕した。得られた顔料組成物のα型結晶の含有率は30%
程度であった。次に、実施例１と同じ方法で濃縮分散体
にし、水性塗料用ビヒクル( 「ハイライト700 」)を400
重量部加え最終インキに調整した後、同一顔料分を含む
標準インキと比較したところ、本実施例のインキの着色
力、色相、光沢は標準品と同等の品位を有していた。Example 5 Crude copper phthalocyanine was added to a dry attritor.
70 parts by weight and 10 parts by weight of an acrylic resin ("Johncryl J-679" manufactured by Johnson Polymer) were added and pulverized at 120 ° C for 30 minutes. Next, 8 parts by weight of a nonionic surfactant ("Newcol B4SN" manufactured by Nippon Emulsifier Co., Ltd.) was added and the mixture was ground at 120 ° C for 15 minutes. The content of α-type crystals in the obtained pigment composition is 30%
It was about. Next, a concentrated dispersion was prepared in the same manner as in Example 1, and a vehicle for water-based paint (“Highlight 700”) was added to 400%.
After adjusting to the final ink by adding parts by weight, when compared with a standard ink containing the same pigment, the coloring power, hue, and gloss of the ink of this example were equivalent to the standard product.
【００３５】[0035]
【実施例６】乾式アトライターに粗製銅フタロシアニン
70重量部とアクリル系樹脂( ジョンソンポリマー社製の
「ジョンクリルHPD-671 」)10 重量部を加え120 ℃で30
分間粉砕した。次に、ノニオン界面活性剤( 日本乳化剤
社製の「Newcol B13」)8重量部を加え120 ℃で15分間粉
砕した。得られた顔料組成物のα型結晶の含有率は30%
程度であった。次に、実施例１と同じ方法で濃縮分散体
にし、水性塗料用ビヒクル( 「ハイライト700 」)を400
重量部加え最終インキに調整した後、同一顔料分を含む
標準インキと比較したところ、本実施例のインキの着色
力、色相、光沢は標準品と同等の品位を有していた。Example 6 Crude copper phthalocyanine was added to a dry attritor.
Add 70 parts by weight and 10 parts by weight of acrylic resin ("Johncryl HPD-671" manufactured by Johnson Polymer) and add 30 parts at 120 ° C.
Milled for minutes. Next, 8 parts by weight of a nonionic surfactant (“Newcol B13” manufactured by Nippon Emulsifier Co., Ltd.) was added, and the mixture was ground at 120 ° C. for 15 minutes. The content of α-type crystals in the obtained pigment composition is 30%
It was about. Next, a concentrated dispersion was prepared in the same manner as in Example 1, and a vehicle for water-based paint (“Highlight 700”) was added to 400%.
After adjusting to the final ink by adding parts by weight, when compared with a standard ink containing the same pigment, the coloring power, hue, and gloss of the ink of this example were equivalent to the standard product.
【００３６】実施例1〜6および比較例1〜3で作製した水
性塗料のα化度、平均粒子径および測色の結果をまとめ
て表1に示す。Table 1 summarizes the results of the degree of pregelatinization, the average particle size, and the colorimetry of the aqueous paints prepared in Examples 1 to 6 and Comparative Examples 1 to 3.
【００３７】[0037]
【表１】 [Table 1]
【００３８】[0038]
【実施例７】乾式アトライターに粗製銅フタロシアニン
70重量部とアクリル系樹脂(ジョンソンポリマー社製の
「ジョンクリルJ-679」)10重量部を加え120℃で30分間
粉砕した。次に、ノニオン界面活性剤(日本乳化剤社製
の「Newcol B13」)8重量部を加え120℃で15分間粉砕し
た。得られた顔料組成物のα型結晶の含有率は10%以下
であった。次に、得られた顔料組成物10重量部とイオン
交換水10重量部と樹脂を溶解するために25%水酸化ナト
リウム溶液1.6重量部を加え室温で緩やかに攪拌するこ
とにより濃縮分散体を得た。次に、下記インキジェット
用バインダー成分を攪拌混合した後、3.00μmのフィル
ターにて、濾過し、インキジェットインキを作製した。Example 7 Crude copper phthalocyanine was added to a dry attritor.
70 parts by weight and 10 parts by weight of an acrylic resin (“Johncryl J-679” manufactured by Johnson Polymer Co.) were added and pulverized at 120 ° C. for 30 minutes. Next, 8 parts by weight of a nonionic surfactant (“Newcol B13” manufactured by Nippon Emulsifier Co., Ltd.) was added, and the mixture was ground at 120 ° C. for 15 minutes. The content of α-type crystals in the obtained pigment composition was 10% or less. Next, 10 parts by weight of the obtained pigment composition, 10 parts by weight of ion-exchanged water and 1.6 parts by weight of a 25% sodium hydroxide solution to dissolve the resin were added, and a concentrated dispersion was obtained by gentle stirring at room temperature. Was. Next, the following ink jet binder component was stirred and mixed, and then filtered through a 3.00 μm filter to prepare an ink jet ink.
【００３９】 上記濃縮分散液 5重量部 1,3-プロパンジオール 10重量部 グリセリン 5重量部 アクリル樹脂エマルジョン 0.2重量部 防黴剤 0.05重量部 イオン交換水 79.75重量部The above concentrated dispersion 5 parts by weight 1,3-propanediol 10 parts by weight Glycerin 5 parts by weight Acrylic resin emulsion 0.2 parts by weight Fungicide 0.05 parts by weight Deionized water 79.75 parts by weight
【００４０】[0040]
【比較例４】銅フタロシアニン顔料(「FG7351」東洋イ
ンキ製造社製)70重量部、アクリル系樹脂(ジョンソンポ
リマー社製の「ジョンクリルJ-679」)30重量部、ノニオ
ン界面活性剤(日本乳化剤社製の「Newcol B13」)8重量
部、25%水酸化ナトリウム水溶液1.6重量部をマヨネーズ
ビンに取り、ペイントコンディショナーを用いて2時間
分散させて、濃縮分散体を作製した。その後、実施例7
で使用したインキジェット用バインダー成分を攪拌混合
した後、3.00μmのフィルターにて、濾過し、インキジ
ェットインキを作製した。Comparative Example 4 70 parts by weight of copper phthalocyanine pigment (“FG7351” manufactured by Toyo Ink Mfg. Co., Ltd.), 30 parts by weight of acrylic resin (“Johncryl J-679” manufactured by Johnson Polymer Co., Ltd.), nonionic surfactant (Nippon Emulsifier) 8 parts by weight of “Newcol B13” (manufactured by Sharp Corporation) and 1.6 parts by weight of a 25% aqueous sodium hydroxide solution were placed in a mayonnaise bottle, and dispersed using a paint conditioner for 2 hours to prepare a concentrated dispersion. Then, Example 7
After stirring and mixing the ink jet binder components used in the above, the mixture was filtered through a 3.00 μm filter to prepare an ink jet ink.
【００４１】[0041]
【実施例８〜１４】実施例7と同様の方法で、表2に示す
処理を行い、インキジェットインキを作製した。また、
加熱処理は120℃で12時間行った。濃縮分散体のα化
度、平均分散粒子径および分散性は表2に示すとおりで
あった。Examples 8 to 14 In the same manner as in Example 7, the treatments shown in Table 2 were performed to produce ink jet inks. Also,
The heat treatment was performed at 120 ° C. for 12 hours. The degree of pregelatinization, average dispersed particle diameter and dispersibility of the concentrated dispersion were as shown in Table 2.
【００４２】[0042]
【表２】 [Table 2]
【００４３】P1 粗製銅フタロシアニン(川崎化成社製) P2 粗製ジメチルキナクリドン(フランカラー社製) P3 粗製カルバゾールジオキサジンバイオレット(住友
化学工業社製) P4 銅フタロシアニン顔料（FG7330：東洋インキ製造社
製) P5 銅フタロシアニン顔料（FG7351：東洋インキ製造社
製) R1 J679(ジョンソンポリマー社製)(スチレン-アクリル
共重合体、酸価=200、Tg=85℃、Mw=7,000) R2 SMA1440(川原油化社製)(スチレン-部分エステル化
マレイン酸共重合体、酸価=185、Tg=44℃、Mw=6,700) R3 SMA2625(川原油化社製)(スチレン-部分エステル化
マレイン酸共重合体、酸価=220、Tg=110℃、Mw=7,500) R4 HPD671(ジョンソンポリマー社製)(スチレン-アクリ
ル共重合体、酸価=214、Tg=128、Mw=17,250) R5 J68(ジョンソンポリマー社製)(スチレン-アクリル
共重合体、酸価=195、Tg=70℃、Mw=10,000) S1 Newcol B13(日本乳化社製)(ナフタレン-エチレンオ
キシド型ノニオン活性剤) S2 Newcol B4SN(日本乳化社製)(ナフタレン-エチレン
オキシド型アニオン活性剤) S3 Newcol 723(日本乳化社製)(スチリルベンジル-エチ
レンオキシド型ノニオン活性剤) S4 Newcol 560(日本乳化社製)(アルキルフェニル-エチ
レンオキシド型ノニオン活性剤) インキジェットインキを用いて、市販のピエゾ方式プリ
ンターを用いて、コピー紙に記録した。着色力、色相の
比較を表3に示した。P1 Crude copper phthalocyanine (Kawasaki Kasei) P2 Crude dimethylquinacridone (Francolor) P3 Crude carbazole dioxazine violet (Sumitomo Chemical) P4 Copper phthalocyanine pigment (FG7330: Toyo Ink) P5 Copper phthalocyanine pigment (FG7351: manufactured by Toyo Ink Mfg. Co., Ltd.) R1 J679 (manufactured by Johnson Polymer Co., Ltd.) (styrene-acryl copolymer, acid value = 200, Tg = 85 ° C., Mw = 7,000) ) (Styrene-partially esterified maleic acid copolymer, acid value = 185, Tg = 44 ° C., Mw = 6,700) R3 SMA2625 (manufactured by Kawahara Yuka Co., Ltd.) (styrene-partially esterified maleic acid copolymer, acid value = 220, Tg = 110 ° C, Mw = 7,500) R4 HPD671 (manufactured by Johnson Polymer) (styrene-acryl copolymer, acid value = 214, Tg = 128, Mw = 17,250) R5 J68 (manufactured by Johnson Polymer) ( (Styrene-acryl copolymer, acid value = 195, Tg = 70 ° C, Mw = 10,000) S1 Newcol B13 (Manufactured by Nippon Emulsion Co., Ltd.) S4 Newcol 560 (manufactured by Nippon Emulsion Co., Ltd.) (alkylphenyl-ethylene oxide type nonionic activator) Using an ink jet ink, recording was performed on copy paper using a commercially available piezo printer. Table 3 shows a comparison of tinting strength and hue.
【００４４】[0044]
【表３】 [Table 3]
【００４５】[0045]
【実施例１５】乾式アトライターに粗製銅フタロシアニ
ン70重量部とアクリル系樹脂(ジョンソンポリマー社製
の「ジョンクリルJ-679」)10重量部を加え120℃で30分
間粉砕した。次に、ノニオン界面活性剤(日本乳化剤社
製の「Newcol B13」)8重量部を加え120℃で15分間粉砕
した。得られた顔料組成物のα型結晶の含有率は10%以
下であった。次に、得られた顔料組成物10重量部とイオ
ン交換水10重量部と樹脂を溶解するために25%水酸化ナ
トリウム溶液1.6重量部とエチレングリコール1重量部を
加え室温で緩やかに攪拌することにより濃縮分散体を得
た。次に、濃縮分散体と活性剤、添加剤、水溶性樹脂か
らなるコンパウンドと添加剤、防腐剤等を含むエマルジ
ョンワニスを混合攪拌し、水性グラビアインキを作製し
た。色相および着色力の評価は、作製した水性グラビア
インキ2重量部にアクアコンテG65白(東洋インキ製造社
製)20重量部を混合し、アート紙に塗工して測色した。EXAMPLE 15 70 parts by weight of crude copper phthalocyanine and 10 parts by weight of an acrylic resin ("Johncryl J-679" manufactured by Johnson Polymer) were added to a dry attritor and ground at 120 ° C. for 30 minutes. Next, 8 parts by weight of a nonionic surfactant (“Newcol B13” manufactured by Nippon Emulsifier Co., Ltd.) was added, and the mixture was ground at 120 ° C. for 15 minutes. The content of α-type crystals in the obtained pigment composition was 10% or less. Next, 10 parts by weight of the obtained pigment composition, 10 parts by weight of ion-exchanged water, and 1.6 parts by weight of a 25% sodium hydroxide solution and 1 part by weight of ethylene glycol to dissolve the resin are added and slowly stirred at room temperature. To obtain a concentrated dispersion. Next, an aqueous gravure ink was prepared by mixing and stirring the concentrated dispersion and a compound comprising an activator, an additive, and a water-soluble resin, and an emulsion varnish containing an additive, a preservative, and the like. For evaluation of hue and tinting strength, 20 parts by weight of Aquaconte G65 white (manufactured by Toyo Ink Mfg. Co., Ltd.) was mixed with 2 parts by weight of the prepared aqueous gravure ink, and the mixture was applied to art paper and measured for color.
【００４６】[0046]
【比較例５】銅フタロシアニン顔料(「FG7330」東洋イ
ンキ製造社製)70重量部、アクリル系樹脂(ジョンソンポ
リマー社製の「ジョンクリルJ-679」)30重量部、ノニオ
ン界面活性剤(日本乳化剤社製の「Newcol B13」)8重量
部、25%水酸化ナトリウム水溶液1.6重量部とエチレング
リコール1重量部をマヨネーズビンに取り、ペイントコ
ンディショナーを用いて2時間分散させて、濃縮分散体
を作製した。次に、濃縮分散体と活性剤、添加剤、水溶
性樹脂からなるコンパウンドと添加剤、防腐剤等を含む
エマルジョンワニスを混合攪拌し、水性グラビアインキ
を作製した。色相および着色力の評価は、作製した水性
グラビアインキ2重量部にアクアコンテG65白(東洋イン
キ製造社製)20重量部を混合し、アート紙に塗工して測
色した。Comparative Example 5 70 parts by weight of a copper phthalocyanine pigment (“FG7330” manufactured by Toyo Ink Mfg. Co., Ltd.), 30 parts by weight of an acrylic resin (“Johncryl J-679” manufactured by Johnson Polymer Co., Ltd.), a nonionic surfactant (Nippon Emulsifier) (Newcol B13) 8 parts by weight, 1.6 parts by weight of a 25% aqueous sodium hydroxide solution and 1 part by weight of ethylene glycol were placed in a mayonnaise bottle and dispersed for 2 hours using a paint conditioner to prepare a concentrated dispersion. . Next, an aqueous gravure ink was prepared by mixing and stirring the concentrated dispersion and a compound comprising an activator, an additive, and a water-soluble resin, and an emulsion varnish containing an additive, a preservative, and the like. For evaluation of hue and tinting strength, 20 parts by weight of Aquaconte G65 white (manufactured by Toyo Ink Mfg. Co., Ltd.) was mixed with 2 parts by weight of the prepared aqueous gravure ink, and the mixture was applied to art paper and measured for color.
【００４７】[0047]
【実施例１６〜１９】実施例15と同様の方法で、表4に
示す処理を行い、水性グラビアインキを作製した。ま
た、着色力および色相の結果を表4に示す。Examples 16 to 19 In the same manner as in Example 15, the treatments shown in Table 4 were performed to produce aqueous gravure inks. Table 4 shows the results of tinting strength and hue.
【００４８】[0048]
【表４】 [Table 4]
【００４９】[0049]
【発明の効果】本発明によれば、現在一般的に使用され
ているソルベントソルトミリング法の顔料と比較して同
等もしくはそれ以上の品質であるばかりか、より低コス
トの顔料組成物を提供することが可能である。また、本
発明によれば、顔料組成物により水系顔料分散体を安価
に提供することができる。According to the present invention, it is possible to provide a pigment composition which is not only of the same quality or better than the pigments of the solvent salt milling method which is generally used at present but also of lower cost. It is possible. Further, according to the present invention, an aqueous pigment dispersion can be provided at a low cost by using the pigment composition.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｂ０２Ｃ 17/00 Ｂ０２Ｃ 17/00 Ｄ Ｃ０９Ｃ 3/10 Ｃ０９Ｃ 3/10 Ｃ０９Ｄ 17/00 Ｃ０９Ｄ 17/00 // Ｃ０９Ｂ 67/04 Ｃ０９Ｂ 67/04 67/12 67/12 ──────────────────────────────────────────────────続 き Continuation of front page (51) Int.Cl. 6 Identification code FI B02C 17/00 B02C 17/00 D C09C 3/10 C09C 3/10 C09D 17/00 C09D 17/00 // C09B 67/04 C09B 67/04 67/12 67/12
Claims (12)
の界面活性剤および該顔料に対して２〜５０重量％の水
溶性樹脂の存在下に乾式粉砕してなる粉体状の顔料組成
物。1. A pigment is used in an amount of 1 to 20% by weight based on the weight of the pigment.
A powdery pigment composition obtained by dry grinding in the presence of a surfactant and a water-soluble resin in an amount of 2 to 50% by weight based on the pigment.
料組成物。2. The pigment composition according to claim 1, wherein the pigment is a crude pigment.
載の顔料組成物。3. The pigment composition according to claim 1, wherein the pigment is a condensed polycyclic pigment.
た芳香族系化合物である請求項１記載の顔料組成物。4. The pigment composition according to claim 1, wherein the surfactant is an aromatic compound to which ethylene oxide has been added.
在下に水に溶解する樹脂である請求項１記載の顔料組成
物。5. The pigment composition according to claim 1, wherein the water-soluble resin has an acidic group and is soluble in water in the presence of an alkali.
載の顔料組成物。6. The pigment composition according to claim 1, wherein the water-soluble resin is a solid resin.
在下に乾式粉砕する粉体状の顔料組成物の製造方法であ
って、上記乾式粉砕時および／または乾式粉砕後に加熱
処理することを特徴とする粉体状の顔料組成物の製造方
法。7. A method for producing a powdery pigment composition in which a pigment is dry-pulverized in the presence of a surfactant and a water-soluble resin, wherein a heat treatment is performed during the dry pulverization and / or after the dry pulverization. A method for producing a powdery pigment composition characterized by the following.
砕し、次いで界面活性剤を添加して乾式粉砕する請求項
７記載の粉体状の顔料組成物の製造方法。8. The method for producing a powdery pigment composition according to claim 7, wherein only the water-soluble resin is added to the pigment, followed by dry pulverization, and then a surfactant is added to carry out dry pulverization.
る請求項７記載の製造方法法。9. The method according to claim 7, wherein the heating temperature during the dry pulverization is 30 to 150 ° C.
℃である請求項７記載の製造方法。10. The heat treatment temperature after dry pulverization is 50 to 150.
The method according to claim 7, wherein the temperature is ° C.
および振動ミルからなる群から選ばれる一種の粉砕装置
を使用する請求項７記載の製造方法。11. The production method according to claim 7, wherein the dry pulverization uses a kind of pulverizer selected from the group consisting of an attritor, a ball mill and a vibration mill.
組成物を水中に分散してなる水系顔料分散体。12. An aqueous pigment dispersion obtained by dispersing the pigment composition according to claim 1 in water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25906498A JP3882358B2 (en) | 1997-12-08 | 1998-09-14 | Pigment composition and aqueous pigment dispersion using the same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33670197 | 1997-12-08 | ||
| JP9-336701 | 1997-12-08 | ||
| JP25906498A JP3882358B2 (en) | 1997-12-08 | 1998-09-14 | Pigment composition and aqueous pigment dispersion using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11228857A true JPH11228857A (en) | 1999-08-24 |
| JP3882358B2 JP3882358B2 (en) | 2007-02-14 |
Family
ID=26543943
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25906498A Expired - Lifetime JP3882358B2 (en) | 1997-12-08 | 1998-09-14 | Pigment composition and aqueous pigment dispersion using the same |
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| Country | Link |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006506489A (en) * | 2002-11-18 | 2006-02-23 | ビーエーエスエフ アクチェンゲゼルシャフト | Solid pigment preparations containing water-soluble anionic carboxylate-containing surfactant additives |
| JP2010265452A (en) * | 2009-04-17 | 2010-11-25 | Canon Inc | Pigment and manufacturing method thereof, pigment dispersion, yellow toner |
| US8946320B2 (en) | 2004-03-22 | 2015-02-03 | Hewlett-Packard Development Company, L.P. | Ink system containing polymer binders |
-
1998
- 1998-09-14 JP JP25906498A patent/JP3882358B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006506489A (en) * | 2002-11-18 | 2006-02-23 | ビーエーエスエフ アクチェンゲゼルシャフト | Solid pigment preparations containing water-soluble anionic carboxylate-containing surfactant additives |
| US8946320B2 (en) | 2004-03-22 | 2015-02-03 | Hewlett-Packard Development Company, L.P. | Ink system containing polymer binders |
| JP2010265452A (en) * | 2009-04-17 | 2010-11-25 | Canon Inc | Pigment and manufacturing method thereof, pigment dispersion, yellow toner |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3882358B2 (en) | 2007-02-14 |
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