JP2008163059A - Method for producing aqueous dispersion of pigment-containing polymer particle and water-based pigment ink composition - Google Patents

Method for producing aqueous dispersion of pigment-containing polymer particle and water-based pigment ink composition Download PDF

Info

Publication number
JP2008163059A
JP2008163059A JP2006350545A JP2006350545A JP2008163059A JP 2008163059 A JP2008163059 A JP 2008163059A JP 2006350545 A JP2006350545 A JP 2006350545A JP 2006350545 A JP2006350545 A JP 2006350545A JP 2008163059 A JP2008163059 A JP 2008163059A
Authority
JP
Japan
Prior art keywords
pigment
containing polymer
aqueous dispersion
resin solution
water
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.)
Granted
Application number
JP2006350545A
Other languages
Japanese (ja)
Other versions
JP4632314B2 (en
Inventor
Ryuichi Aoki
隆一 青木
Hiroji Sasaki
博治 佐々木
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dai Nippon Toryo KK
Original Assignee
Dai Nippon Toryo KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Dai Nippon Toryo KK filed Critical Dai Nippon Toryo KK
Priority to JP2006350545A priority Critical patent/JP4632314B2/en
Publication of JP2008163059A publication Critical patent/JP2008163059A/en
Application granted granted Critical
Publication of JP4632314B2 publication Critical patent/JP4632314B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Ink Jet (AREA)
  • Ink Jet Recording Methods And Recording Media Thereof (AREA)
  • Polymerisation Methods In General (AREA)
  • Graft Or Block Polymers (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing an aqueous dispersion of a pigment-containing polymer particle suitable for the preparation of a water-based pigment ink composition for inkjet recording use containing an encapsulated pigment and to provide a water-based pigment ink composition containing the aqueous dispersion of a pigment-containing polymer particle obtained by the production method. <P>SOLUTION: The method for producing an aqueous dispersion of a pigment-containing polymer particle comprises (1) a step for preparing a resin solution by dissolving a vinyl resin in an ethylenic unsaturated monomer, (2) a step for preparing a pigment-dispersed resin solution by adding a pigment to the resin solution and homogenizing the mixture, (3) a step for preparing a mini-emulsion by adding the pigment-dispersed resin solution to an aqueous solution of an emulsifier and homogenizing the mixture to disperse the pigment-dispersed resin solution in water, and (4) a step for adding a radical initiator to the mini-emulsion and polymerizing the monomer. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明は顔料含有ポリマー粒子水分散体の製造方法及び水系顔料インク組成物に関し、より詳しくは、インクジェット記録用水系顔料インク組成物の調製に用いるのに適した顔料含有ポリマー粒子水分散体の製造方法及び該製造方法で得られる顔料含有ポリマー粒子水分散体を含有する水系顔料インク組成物に関する。   TECHNICAL FIELD The present invention relates to a method for producing an aqueous dispersion of pigment-containing polymer particles and an aqueous pigment ink composition, and more specifically, production of an aqueous dispersion of pigment-containing polymer particles suitable for use in the preparation of an aqueous pigment ink composition for inkjet recording. The present invention relates to a method and an aqueous pigment ink composition containing an aqueous dispersion of pigment-containing polymer particles obtained by the production method.

インクジェット記録方式は記録部材として普通紙を使用することができ、また、カラー化が容易であるので、近年広く用いられている。   Inkjet recording methods have been widely used in recent years because plain paper can be used as a recording member and colorization is easy.

インクジェットに使用されるインクとして、インクがノズルに目詰まりするのを防止するために、水溶性染料及び多価アルコールを用いたものがある。しかし、この種のインクは耐水性や耐光性に劣り、特に熱ジェット方式のインクとして使用した場合には、ヒーター面の熱により染料が酸化され、インクがヒーター面に焦げつきやすく、吐出性が低下するという欠点がある。   As an ink used for inkjet, there is an ink using a water-soluble dye and a polyhydric alcohol in order to prevent the ink from clogging the nozzle. However, this type of ink is inferior in water resistance and light resistance, especially when used as a heat jet ink, the dye is oxidized by the heat of the heater surface, the ink tends to scorch on the heater surface, and the discharge property is reduced. There is a drawback of doing.

このような欠点を解消するために、顔料インクが提案されている。顔料インクには、界面活性剤や水溶性ポリマーにより顔料を水中へ分散させた顔料分散型インクと、水不溶性ポリマーの粒子中に顔料を含有させ、それを水中に分散させた顔料内包型インクとが提案されている。   In order to eliminate such drawbacks, pigment inks have been proposed. The pigment ink includes a pigment-dispersed ink in which a pigment is dispersed in water with a surfactant or a water-soluble polymer, and a pigment-encapsulated ink in which a pigment is contained in water-insoluble polymer particles and dispersed in water. Has been proposed.

顔料分散型インクを用いた場合には、前記欠点がかなり改善されるものの、耐水性及び耐光性が不十分であるという欠点がある。これに対して、顔料内包型インクは、耐水性及び耐光性に優れている。   In the case of using a pigment-dispersed ink, the above-mentioned drawbacks are considerably improved, but there is a disadvantage that water resistance and light resistance are insufficient. On the other hand, the pigment-containing ink is excellent in water resistance and light resistance.

本発明の目的は、顔料内包型のインクジェット記録用水系顔料インク組成物の調製に用いるのに適した顔料含有ポリマー粒子水分散体の製造方法及び該製造方法で得られる顔料含有ポリマー粒子水分散体を含有する水系顔料インク組成物を提供することである。   An object of the present invention is to provide a method for producing a pigment-containing polymer particle aqueous dispersion suitable for use in preparing a pigment-encapsulated water-based pigment ink composition for inkjet recording, and a pigment-containing polymer particle aqueous dispersion obtained by the production method. An aqueous pigment ink composition containing

本発明の顔料含有ポリマー粒子水分散体の製造方法は、
(1)エチレン性不飽和モノマー中にビニル系樹脂を溶解させて樹脂溶液を調製する工程、
(2)該樹脂溶液に顔料を添加し、ホモジナイズ処理により顔料分散樹脂溶液を調製する工程、
(3)該顔料分散樹脂溶液を乳化剤水溶液中に添加し、ホモジナイズ処理により顔料分散樹脂溶液を水中に分散させてミニエマルションを調製する工程、及び
(4)該ミニエマルションにラジカル開始剤を添加し、重合させる工程
からなることを特徴とする。
The method for producing the pigment-containing polymer particle aqueous dispersion of the present invention comprises:
(1) A step of preparing a resin solution by dissolving a vinyl resin in an ethylenically unsaturated monomer,
(2) A step of adding a pigment to the resin solution and preparing a pigment-dispersed resin solution by homogenization treatment;
(3) adding the pigment-dispersed resin solution into an aqueous emulsifier solution and dispersing the pigment-dispersed resin solution in water by homogenization to prepare a miniemulsion; and (4) adding a radical initiator to the miniemulsion. , Characterized by comprising a step of polymerizing.

本発明の製造方法で得られる顔料含有ポリマー粒子水分散体は、耐水性及び耐光性に優れた顔料内包型のインクジェット記録用水系顔料インク組成物の調製に用いるのに特に適している。   The pigment-containing polymer particle aqueous dispersion obtained by the production method of the present invention is particularly suitable for use in the preparation of a pigment-encapsulated water-based pigment ink composition for inkjet recording excellent in water resistance and light resistance.

本発明の顔料含有ポリマー粒子水分散体の製造方法の第一工程は、エチレン性不飽和モノマー中にビニル系樹脂を溶解させて樹脂溶液を調製する工程である。エチレン性不飽和モノマー中にビニル系樹脂を添加し、攪拌することにより容易に樹脂溶液を得ることができる。   The first step of the method for producing a pigment-containing polymer particle aqueous dispersion of the present invention is a step of preparing a resin solution by dissolving a vinyl resin in an ethylenically unsaturated monomer. A resin solution can be easily obtained by adding a vinyl resin to an ethylenically unsaturated monomer and stirring the mixture.

本発明の製造方法で用いるエチレン性不飽和モノマーとして、例えば、(メタ)アクリル酸メチル、(メタ)アクリル酸エチル、(メタ)アクリル酸n−プロピル、(メタ)アクリル酸イソプロピル、(メタ)アクリル酸(n−、i−、t−)ブチル、(メタ)アクリル酸へキシル、(メタ)アクリル酸2−エチルへキシル、(メタ)アクリル酸n−オクチル、(メタ)アクリル酸デシル、(メタ)アクリル酸ラウリル、(メタ)アクリル酸ステアリル、(メタ)アクリル酸シクロヘキシル等のアクリル酸又はメタクリル酸のアルキルエステル又はシクロアルキルエステル;(メタ)アクリル酸メトキシエチル、(メタ)アクリル酸エトキシエチル、(メタ)アクリル酸エトキシブチル等のアクリル酸又はメタクリル酸のアルコキシアルキル;アクリル酸、メタクリル酸、クロトン酸、イタコン酸、マレイン酸、フマル酸等のカルボキシル基含有不飽和モノマー;2−ヒドロキシエチル(メタ)アクリレート、2−又は3−ヒドロキシプロピル(メタ)アクリレート等のアクリル樹脂又はメタクリル酸の炭素数2〜8のヒドロキシアルキルエステル;N,N−ジメチルアミノエチル(メタ)アクリレート、N,N−ジエチルアミノエチル(メタ)アクリレート等の含窒素アルキル(メタ)アクリレート;アクリルアミド、メタクリルアミド、N−ブトキシメチル(メタ)アクリルアミド、N,N−ジメチルアミノプロピル(メタ)アクリルアミド、N,N−ジメチルアミノエチル(メタ)アクリルアミド等の重合性アミド類;グリシジル(メタ)アクリレート、アリルグリシジルエーテル等のエポキシ基含有不飽和モノマー;酢酸ビニル、スチレン、α−クロロスチレン、アクリロニトリル等を挙げることができる。   Examples of the ethylenically unsaturated monomer used in the production method of the present invention include, for example, methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, isopropyl (meth) acrylate, and (meth) acrylic. Acid (n-, i-, t-) butyl, hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, n-octyl (meth) acrylate, decyl (meth) acrylate, (meth ) Acrylic acid or methacrylic acid alkyl ester or cycloalkyl ester such as lauryl acrylate, stearyl (meth) acrylate, cyclohexyl (meth) acrylate; methoxyethyl (meth) acrylate, ethoxyethyl (meth) acrylate, ( Alkoxyalkyl of acrylic acid or methacrylic acid such as methacrylic acid ethoxybutyl Carboxyl group-containing unsaturated monomers such as acrylic acid, methacrylic acid, crotonic acid, itaconic acid, maleic acid, fumaric acid; acrylic resins such as 2-hydroxyethyl (meth) acrylate, 2- or 3-hydroxypropyl (meth) acrylate Or a C2-C8 hydroxyalkyl ester of methacrylic acid; nitrogen-containing alkyl (meth) acrylates such as N, N-dimethylaminoethyl (meth) acrylate and N, N-diethylaminoethyl (meth) acrylate; acrylamide, methacrylamide , N-butoxymethyl (meth) acrylamide, N, N-dimethylaminopropyl (meth) acrylamide, polymerizable amides such as N, N-dimethylaminoethyl (meth) acrylamide; glycidyl (meth) acrylate, allyl glycidyl ester Epoxy group-containing unsaturated monomers such as ether, vinyl acetate, styrene, alpha-chlorostyrene, and acrylonitrile.

本発明の製造方法で用いるビニル系樹脂として、塩化ビニル系樹脂、酢酸ビニル系樹脂等を挙げることができ、例えば、塩化ビニルの単独重合体のほか、主成分の塩化ビニルと他の共重合可能なコモノマーとの共重合体等、塩化ビニルを主な構成単位とする樹脂を挙げることができる。共重合可能なコモノマーとしては、エチレン、プロピレン、アクリロニトリル、酢酸ビニル、マレイン酸またはそのエステル、アクリル酸またはそのエステル、メタクリル酸またはそのエステル等を挙げることができる。   Examples of vinyl resins used in the production method of the present invention include vinyl chloride resins and vinyl acetate resins. For example, in addition to vinyl chloride homopolymers, the main component vinyl chloride can be copolymerized with other resins. Examples thereof include resins having vinyl chloride as a main structural unit, such as copolymers with various comonomers. Examples of the copolymerizable comonomer include ethylene, propylene, acrylonitrile, vinyl acetate, maleic acid or its ester, acrylic acid or its ester, methacrylic acid or its ester, and the like.

本発明の顔料含有ポリマー粒子水分散体の製造方法の第二工程は、上記のようにして得た樹脂溶液に顔料を添加し、ホモジナイズ処理により顔料分散樹脂溶液を調製する工程である。ホモジナイズ処理は、例えば、超音波、ビーズミル、剪断混合装置等で実施することができる。このホモジナイズ処理により、顔料を樹脂溶液中に均一に分散させることができる。   The second step of the method for producing a pigment-containing polymer particle aqueous dispersion of the present invention is a step of adding a pigment to the resin solution obtained as described above and preparing a pigment-dispersed resin solution by homogenization treatment. The homogenization treatment can be performed with, for example, an ultrasonic wave, a bead mill, a shear mixing device, or the like. By this homogenization treatment, the pigment can be uniformly dispersed in the resin solution.

本発明の製造方法で用いる顔料は、無機顔料及び有機顔料のいずれであってもよい。また、必要により、これらの顔料と体質顔料とを併用することもできる。無機顔料として、カーボンブラック、金属酸化物、金属硫化物、金属塩化物等を挙げることができる。これらの中では、特に黒色系インクでは、カーボンブラックが好ましい。カーボンブラックとして、ファーネスブラック、サーマルブラック、アセチレンブラック、チャンネルブラック等を挙げることができる。   The pigment used in the production method of the present invention may be either an inorganic pigment or an organic pigment. If necessary, these pigments and extender pigments can be used in combination. Examples of the inorganic pigment include carbon black, metal oxide, metal sulfide, and metal chloride. Among these, carbon black is particularly preferable for black ink. Examples of carbon black include furnace black, thermal black, acetylene black, and channel black.

有機顔料として、アゾ顔料、ジアゾ顔料、フタロシアニン顔料、キナクリドン顔料、イソインドリノン顔料、ジオキサジン顔料、ペリレン顔料、ペリノン顔料、チオインジゴ顔料、アンソラキノン顔料、キノフタノン顔料等を挙げることができる。また、体質顔料として、シリカ、炭酸カルシウム、タルク等を挙げることができる。   Examples of organic pigments include azo pigments, diazo pigments, phthalocyanine pigments, quinacridone pigments, isoindolinone pigments, dioxazine pigments, perylene pigments, perinone pigments, thioindigo pigments, anthoraquinone pigments, and quinophthalone pigments. Examples of extender pigments include silica, calcium carbonate, and talc.

本発明の顔料含有ポリマー粒子水分散体の製造方法の第三工程は、上記のようにして得た顔料分散樹脂溶液を乳化剤水溶液中に添加し、ホモジナイズ処理により顔料分散樹脂溶液を水中に分散させてミニエマルションを調製する工程である。このホモジナイズ処理は第二工程におけるホモジナイズ処理と同様に実施することができ、このホモジナイズ処理により、上記のようにして得た顔料分散樹脂溶液が水中に微分散されてミニエマルションとなる。   In the third step of the method for producing the pigment-containing polymer particle aqueous dispersion of the present invention, the pigment-dispersed resin solution obtained as described above is added to an aqueous emulsifier solution, and the pigment-dispersed resin solution is dispersed in water by homogenization treatment. This is a step of preparing a miniemulsion. This homogenization treatment can be carried out in the same manner as the homogenization treatment in the second step. By this homogenization treatment, the pigment-dispersed resin solution obtained as described above is finely dispersed in water to form a miniemulsion.

本発明の製造方法では種々の乳化剤を用いることができる。例えば、ステアリルアミン塩酸塩、ラウリルトリメチルアンモニウムクロライド、トリメチルオクタデシルアンモニウムクロライド等のカチオン乳化剤、オレイン酸カリウム、ラウリル酸ナトリウム、ドデシルベンゼンスルホン酸ナトリウム、アルカンスルホン酸ナトリウム、アルキルナフタレンスルホン酸ナトリウム、ジアルキルスルホコハク酸ナトリウム、ポリオキシエチレンアルキルエーテル硫酸ナトリウム、ポリオキシエチレンアルキルアリルエーテル硫酸ナトリウム、ポリオキシエチレンアルキル燐酸エステル、ポリオキシエチレンアルキルアリル燐酸エステル等のアニオン系乳化剤、ポリオキシエチレンアルキルエーテル、ポリオキシエチレンアルキルアリルエーテル、ポリオキシエチレンプロピルブロックポリマー、ポリエチレングリコール脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステル等のノニオン系乳化剤、ラウリルペタイン、ラウリルジメチルアミンオキサイド等の両イオン性乳化剤等を用いることができる。しかし、本発明の製造方法ではアニオンノニオンタイプの乳化剤、特に反応性乳化剤を用いることが好ましい。   Various emulsifiers can be used in the production method of the present invention. For example, cationic emulsifiers such as stearylamine hydrochloride, lauryltrimethylammonium chloride, trimethyloctadecylammonium chloride, potassium oleate, sodium laurate, sodium dodecylbenzenesulfonate, sodium alkanesulfonate, sodium alkylnaphthalenesulfonate, sodium dialkylsulfosuccinate Anionic emulsifiers such as sodium polyoxyethylene alkyl ether sulfate, sodium polyoxyethylene alkyl allyl ether sulfate, polyoxyethylene alkyl phosphate ester, polyoxyethylene alkyl allyl phosphate ester, polyoxyethylene alkyl ether, polyoxyethylene alkyl allyl ether , Polyoxyethylenepropyl block polymer, polyethylene Glycol fatty acid ester, nonionic emulsifiers such as polyoxyethylene sorbitan fatty acid esters, lauryl betaine, may be used both ionic emulsifiers such as lauryl dimethyl amine oxide. However, it is preferable to use an anionic nonionic emulsifier, particularly a reactive emulsifier, in the production method of the present invention.

本発明の顔料含有ポリマー粒子水分散体の製造方法の第四工程は、上記のようにして得たミニエマルションにラジカル開始剤を添加し、重合させる工程である。この重合工程を好ましくは30〜95℃の範囲内の温度で実施することができる。この重合により顔料の周りに樹脂が付着した顔料含有ポリマー粒子が形成され、この顔料含有ポリマー粒子は水中に分散している。即ち、顔料含有ポリマー粒子水分散体が得られる。   The fourth step of the method for producing the pigment-containing polymer particle aqueous dispersion of the present invention is a step of adding a radical initiator to the miniemulsion obtained as described above and polymerizing it. This polymerization step can be carried out preferably at a temperature in the range of 30-95 ° C. By this polymerization, pigment-containing polymer particles having a resin attached around the pigment are formed, and the pigment-containing polymer particles are dispersed in water. That is, a pigment-containing polymer particle aqueous dispersion is obtained.

本発明の製造方法で用いるラジカル開始剤として、例えば、2,2’−アゾビスイソブチロニトリル、2,2’− アゾビス−(2−メチルプロパンニトリル) 、2,2’−アゾビス−(2,4−ジメチルペンタンニトリル)、2,2’−アゾビス−(2−メチルブタンニトリル)、1,1’−アゾビス−(シクロヘキサンカルボニトリル)、2,2’−アゾビス−(2,4−ジメチル−4−メトキシバレロニトリル)、2,2’−アゾビス−(2,4−ジメチルバレロニトリル)、2,2’−アゾビス−(2−アミジノプロパン)ヒドロクロリド等のアゾ(アゾビスニトリル)タイプの開始剤、過酸化ベンゾイル、クメンヒドロペルオキシド、過酸化水素、過酸化アセチル、過酸化ラウロイル、過硫酸塩(例えば過硫酸アンモニウム)、過酸エステル(例えばt−ブチルペルオクテート、α−クミルペルオキシピバレート及びt−ブチルペルオクテート)等の過酸化物タイプの開始剤を挙げることができる。   Examples of the radical initiator used in the production method of the present invention include 2,2′-azobisisobutyronitrile, 2,2′-azobis- (2-methylpropanenitrile), 2,2′-azobis- (2 , 4-dimethylpentanenitrile), 2,2′-azobis- (2-methylbutanenitrile), 1,1′-azobis- (cyclohexanecarbonitrile), 2,2′-azobis- (2,4-dimethyl-) Initiation of azo (azobisnitrile) types such as 4-methoxyvaleronitrile), 2,2′-azobis- (2,4-dimethylvaleronitrile), 2,2′-azobis- (2-amidinopropane) hydrochloride Agents, benzoyl peroxide, cumene hydroperoxide, hydrogen peroxide, acetyl peroxide, lauroyl peroxide, persulfates (eg ammonium persulfate) It can be mentioned esters (for example, t- butyl peroxide octoate, alpha-cumyl peroxypivalate and t- butyl per octoate) peroxide type initiators such as.

上記のようにして得た顔料含有ポリマー粒子水分散体に、必要に応じて湿潤剤、分散剤、消泡剤、キレート剤、防黴剤等の添加剤を適量で添加することにより、水系顔料インク組成物を得ることができる。かくして得られた水系顔料インク組成物は、分散安定性、耐水性、耐光性及び印字特性に優れたものである。   By adding an appropriate amount of additives such as a wetting agent, a dispersing agent, an antifoaming agent, a chelating agent, and an antifungal agent to the pigment-containing polymer particle aqueous dispersion obtained as described above, an aqueous pigment is obtained. An ink composition can be obtained. The water-based pigment ink composition thus obtained is excellent in dispersion stability, water resistance, light resistance and printing characteristics.

実施例1
メタクリル酸メチル60g、アクリル酸ブチル20g及びメタクリル酸ラウリル20gからなるエチレン性不飽和モノマー100gに塩化ビニル/酢酸ビニル共重合体20gを添加し、攪拌して均一に溶解させて樹脂溶液を得た。
Example 1
20 g of vinyl chloride / vinyl acetate copolymer was added to 100 g of ethylenically unsaturated monomer consisting of 60 g of methyl methacrylate, 20 g of butyl acrylate and 20 g of lauryl methacrylate, and stirred to dissolve uniformly to obtain a resin solution.

上記の樹脂溶液に顔料としてフタロシアニンブルー(Ciba S.C.社製、PTB8700)30gを添加し、ビーズミルに30分間かけ、分散させて顔料分散樹脂溶液を調製した。分散後の顔料の平均粒子径は、 日機装株式会社製マイクロトラックMT3300EXで測定して、180ナノメートルであった。   30 g of phthalocyanine blue (manufactured by Ciba S.C., PTB8700) was added as a pigment to the resin solution, and the mixture was dispersed in a bead mill for 30 minutes to prepare a pigment-dispersed resin solution. The average particle size of the pigment after dispersion was 180 nanometers as measured with Nikkiso Microtrack MT3300EX.

上記の顔料分散樹脂溶液を乳化剤水溶液中に添加し、超音波ホモジナイザー(日機装株式会社製、US−600TCVP)にかけて顔料分散樹脂溶液が水中に分散したO/W型ミニエマルションを得た。この乳化剤水溶液として反応性乳化剤SE1025A(アデカ社製)の2%水溶液を300g使用した 。   The above pigment dispersion resin solution was added to an emulsifier aqueous solution, and an ultrasonic homogenizer (manufactured by Nikkiso Co., Ltd., US-600TCVP) was used to obtain an O / W type miniemulsion in which the pigment dispersion resin solution was dispersed in water. As this emulsifier aqueous solution, 300 g of a 2% aqueous solution of reactive emulsifier SE1025A (manufactured by Adeka) was used.

攪拌機、温度センサー及びコンデンサーを備えた反応器をウォーターバス中にセットし、この反応器に上記のミニエマルションを移し、撹拌しながら70℃まで昇温させた。70℃に到達した時点で、過硫酸アンモニウム0.8gを溶解した水溶液を注入して重合をスタートさせた。その後5時間、70℃に保ち、更に80℃に昇温させて3時間保って重合を完結させた。   A reactor equipped with a stirrer, a temperature sensor and a condenser was set in a water bath, and the above-mentioned mini-emulsion was transferred to this reactor, and the temperature was raised to 70 ° C. while stirring. When the temperature reached 70 ° C., an aqueous solution in which 0.8 g of ammonium persulfate was dissolved was injected to start polymerization. Thereafter, the temperature was maintained at 70 ° C. for 5 hours, further heated to 80 ° C. and maintained for 3 hours to complete the polymerization.

このようにして得られた顔料含有ポリマー粒子(顔料−ポリマー複合粒子)水分散体は、固形分濃度32.5%で、固形分の平均粒子径230ナノメートルであった。また、この顔料含有ポリマー粒子水分散体に分散剤、消泡剤を適量添加した水系顔料インク組成物は、分散安定性、耐水性、耐光性及び印字特性に優れたものであった。   The pigment-containing polymer particles (pigment-polymer composite particles) aqueous dispersion thus obtained had a solid content concentration of 32.5% and an average particle size of solids of 230 nanometers. Further, the water-based pigment ink composition in which appropriate amounts of a dispersant and an antifoaming agent were added to the pigment-containing polymer particle aqueous dispersion was excellent in dispersion stability, water resistance, light resistance and printing characteristics.

Claims (6)

(1)エチレン性不飽和モノマー中にビニル系樹脂を溶解させて樹脂溶液を調製する工程、
(2)該樹脂溶液に顔料を添加し、ホモジナイズ処理により顔料分散樹脂溶液を調製する工程、
(3)該顔料分散樹脂溶液を乳化剤水溶液中に添加し、ホモジナイズ処理により顔料分散樹脂溶液を水中に分散させてミニエマルションを調製する工程、及び
(4)該ミニエマルションにラジカル開始剤を添加し、重合させる工程
からなることを特徴とする顔料含有ポリマー粒子水分散体の製造方法。
(1) A step of preparing a resin solution by dissolving a vinyl resin in an ethylenically unsaturated monomer,
(2) A step of adding a pigment to the resin solution and preparing a pigment-dispersed resin solution by homogenization treatment;
(3) adding the pigment-dispersed resin solution into an aqueous emulsifier solution and dispersing the pigment-dispersed resin solution in water by homogenization to prepare a miniemulsion; and (4) adding a radical initiator to the miniemulsion. A method for producing an aqueous dispersion of pigment-containing polymer particles, characterized by comprising a step of polymerizing.
ビニル系樹脂が塩化ビニル系樹脂であることを特徴とする請求項1記載の顔料含有ポリマー粒子水分散体の製造方法。   The method for producing an aqueous dispersion of pigment-containing polymer particles according to claim 1, wherein the vinyl resin is a vinyl chloride resin. ホモジナイズ処理を超音波、ビーズミル又は剪断混合装置で実施することを特徴とする請求項1又は2記載の顔料含有ポリマー粒子水分散体の製造方法。   The method for producing an aqueous dispersion of pigment-containing polymer particles according to claim 1 or 2, wherein the homogenization treatment is performed with an ultrasonic wave, a bead mill or a shear mixing device. 乳化剤としてアニオンノニオンタイプの乳化剤を用いることを特徴とする請求項1、2又は3記載の顔料含有ポリマー粒子水分散体の製造方法。   The method for producing an aqueous dispersion of pigment-containing polymer particles according to claim 1, 2, or 3, wherein an anionic nonionic emulsifier is used as the emulsifier. 重合を30〜95℃の範囲の温度で実施することを特徴とする請求項1、2、3又は4記載の顔料含有ポリマー粒子水分散体の製造方法。   The method for producing an aqueous dispersion of pigment-containing polymer particles according to claim 1, 2, 3 or 4, wherein the polymerization is carried out at a temperature in the range of 30 to 95 ° C. 請求項1、2、3、4又は5記載の製造方法で得られる顔料含有ポリマー粒子水分散体を含有することを特徴とする水系顔料インク組成物。   An aqueous pigment ink composition comprising an aqueous dispersion of pigment-containing polymer particles obtained by the production method according to claim 1, 2, 3, 4 or 5.
JP2006350545A 2006-12-26 2006-12-26 Method for producing pigment-containing polymer particle aqueous dispersion and water-based pigment ink composition Active JP4632314B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2006350545A JP4632314B2 (en) 2006-12-26 2006-12-26 Method for producing pigment-containing polymer particle aqueous dispersion and water-based pigment ink composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2006350545A JP4632314B2 (en) 2006-12-26 2006-12-26 Method for producing pigment-containing polymer particle aqueous dispersion and water-based pigment ink composition

Publications (2)

Publication Number Publication Date
JP2008163059A true JP2008163059A (en) 2008-07-17
JP4632314B2 JP4632314B2 (en) 2011-02-16

Family

ID=39692974

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2006350545A Active JP4632314B2 (en) 2006-12-26 2006-12-26 Method for producing pigment-containing polymer particle aqueous dispersion and water-based pigment ink composition

Country Status (1)

Country Link
JP (1) JP4632314B2 (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010083968A (en) * 2008-09-30 2010-04-15 Dainippon Toryo Co Ltd Preparation of sublimable dye-containing polymer particle aqueous dispersion, and water-based sublimable dye ink composition
US10538681B2 (en) 2017-04-10 2020-01-21 Seiko Epson Corporation Aqueous ink for ink jet recording
US10787585B2 (en) 2017-08-07 2020-09-29 Seiko Epson Corporation Aqueous ink for ink jet recording
WO2022202045A1 (en) * 2021-03-26 2022-09-29 株式会社ミマキエンジニアリング Aqueous ink composition
WO2023068378A1 (en) * 2021-10-20 2023-04-27 株式会社Adeka Pigment-in-water dispersing agent, method for dispersing pigment in water, and aqueous coating material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003089757A (en) * 2001-06-29 2003-03-28 Canon Inc Colored resin fine particle and method for producing the same, aqueous dispersion of colored resin particle, ink, ink cartridge, recording unit, ink jet recording device, and ink jet recording method
JP2004264629A (en) * 2003-03-03 2004-09-24 Canon Inc Resin for toner and toner using same
JP2007156297A (en) * 2005-12-08 2007-06-21 Canon Inc Toner

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003089757A (en) * 2001-06-29 2003-03-28 Canon Inc Colored resin fine particle and method for producing the same, aqueous dispersion of colored resin particle, ink, ink cartridge, recording unit, ink jet recording device, and ink jet recording method
JP2004264629A (en) * 2003-03-03 2004-09-24 Canon Inc Resin for toner and toner using same
JP2007156297A (en) * 2005-12-08 2007-06-21 Canon Inc Toner

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010083968A (en) * 2008-09-30 2010-04-15 Dainippon Toryo Co Ltd Preparation of sublimable dye-containing polymer particle aqueous dispersion, and water-based sublimable dye ink composition
US10538681B2 (en) 2017-04-10 2020-01-21 Seiko Epson Corporation Aqueous ink for ink jet recording
US10787585B2 (en) 2017-08-07 2020-09-29 Seiko Epson Corporation Aqueous ink for ink jet recording
WO2022202045A1 (en) * 2021-03-26 2022-09-29 株式会社ミマキエンジニアリング Aqueous ink composition
WO2023068378A1 (en) * 2021-10-20 2023-04-27 株式会社Adeka Pigment-in-water dispersing agent, method for dispersing pigment in water, and aqueous coating material

Also Published As

Publication number Publication date
JP4632314B2 (en) 2011-02-16

Similar Documents

Publication Publication Date Title
AU2012220750B2 (en) Polymer encapsulated titanium dioxide particles
JP4632314B2 (en) Method for producing pigment-containing polymer particle aqueous dispersion and water-based pigment ink composition
US7354476B2 (en) Inkjet ink composition
US20060167137A1 (en) Inkjet ink binder and inkjet ink composition
US20120065323A1 (en) Temporary coatings
JP2013163794A (en) Ink composition and image forming method
WO2014104319A1 (en) Acrylic resin emulsion for water-based inkjet inks, and water-based inkjet ink composition produced using same
CN104311727A (en) Acrylic resin for transfer ink
JP2011111492A (en) Coating composition for sealer
EP3374454B1 (en) Aqueous latex-based coating compositions
US7381753B2 (en) Inkjet ink composition
JP2011046783A (en) Aqueous emulsion resin composition and coating obtained by blending the same
JP2010001334A (en) Method for producing aqueous polyolefin dispersion
JP4534178B2 (en) Emulsion polymerization method and emulsion obtained thereby
JP5334101B2 (en) Process for producing sublimable dye-containing polymer particle aqueous dispersion and water-based sublimable dye ink composition
JP5547460B2 (en) Resin composition for sealer
JP2008050489A (en) Adhesive for print laminate
WO2013133418A1 (en) Resin emulsion for water-based inkjet ink, composition for water-based inkjet ink using same, and ink-coated material
JP5293919B2 (en) Seed particles, vinyl polymer, and production method thereof
JPH11322812A (en) Production of emulsion resin
JP2006346599A (en) Method of forming aqueous resin cured coating film
JP2007246800A (en) Multi-step polymerization polymer emulsion and method for producing the same
JP2020172613A (en) Aqueous resin composition for coating material
JP2001163903A (en) Method for preparing aqueous emulsion
AU2023213622A1 (en) Hydrophobic polymer compositions and a method to prepare hydrophobic polymer compositions

Legal Events

Date Code Title Description
A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20100805

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20100811

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20101004

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20101110

A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20101111

R150 Certificate of patent or registration of utility model

Ref document number: 4632314

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150

Free format text: JAPANESE INTERMEDIATE CODE: R150

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20131126

Year of fee payment: 3