JP2016196117A - Treatment liquid for material to be recorded, material to be recorded, and method for producing them - Google Patents
Treatment liquid for material to be recorded, material to be recorded, and method for producing them Download PDFInfo
- Publication number
- JP2016196117A JP2016196117A JP2015076476A JP2015076476A JP2016196117A JP 2016196117 A JP2016196117 A JP 2016196117A JP 2015076476 A JP2015076476 A JP 2015076476A JP 2015076476 A JP2015076476 A JP 2015076476A JP 2016196117 A JP2016196117 A JP 2016196117A
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- Prior art keywords
- recording material
- cationic polymer
- treatment liquid
- ink
- polymer
- 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
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Abstract
Description
本発明は、インクジェット印刷に適した被記録材において、被記録材の表面に設けられるインク受容層を形成するために用いられる被記録材用処理液、当該処理液で処理された被記録材及びそれらの製造方法に関する。 The present invention relates to a recording material suitable for ink jet printing, a recording material treatment liquid used for forming an ink receiving layer provided on the surface of the recording material, a recording material treated with the treatment liquid, and The present invention relates to a manufacturing method thereof.
インクジェット印刷に用いられるインクは、水、染料等の着色剤、浸透剤、その他添加剤等を含んでいる。インクジェット印刷では、プリンタのノズルから極めて微細な液粒としてインクが排出され、当該液粒が被記録材に付着、浸透及び定着することによって画像が形成される。インクジェット印刷の画質の向上、具体的には高精細化やニジミの低減を図るために、被記録材には様々な工夫が施されている。 The ink used for inkjet printing contains water, a coloring agent such as a dye, a penetrating agent, and other additives. In ink jet printing, ink is discharged as extremely fine liquid particles from a nozzle of a printer, and an image is formed by the liquid particles adhering, penetrating, and fixing to a recording material. In order to improve the image quality of ink jet printing, specifically, to achieve high definition and reduce blurring, various measures have been applied to the recording material.
インクジェット印刷用の被記録材において、インクのニジミ等を防止するために、被記録材の表面にインクを速やかに吸収するインク受容層を形成することが公知である。特許文献１には、記録画像の耐水性、ドット周辺の鮮明度及びドット濃度を改善させるために、カチオン性ポリマー及びアニオン性ポリマーを含有してなる被記録材用処理液、ないし、当該処理液を塗工してなる被記録材が開示されている。カチオン性ポリマーとしては特定の構造を有するポリアミンが特に好ましく、アニオン性ポリマーとしてはスチレン−アクリル酸共重合体が好ましいことが記載されている。 In a recording material for ink jet printing, it is known to form an ink receiving layer that quickly absorbs ink on the surface of the recording material in order to prevent ink blurring. Patent Document 1 discloses a recording material treatment liquid containing a cationic polymer and an anionic polymer in order to improve the water resistance of recorded images, the vividness of dots and the dot density, or the treatment liquid. There is disclosed a recording material obtained by coating the film. It is described that a polyamine having a specific structure is particularly preferable as the cationic polymer, and a styrene-acrylic acid copolymer is preferable as the anionic polymer.
またインク受容層を形成する材料として、多孔質合成シリカ等の高いインク吸収性を有する無機顔料を組み合わせることも公知である。特許文献２は、無機顔料を多く含有するインク受容層形成材料は、その材料自体の隠ぺい力が高いために、原紙（基材）の風合いや色合いを損なってしまうという問題に着目し、インクジェット特性に優れ、かつ、原紙の風合いや色合いを維持したインクジェット記録用紙を提供する。特許文献２は、スチレン−アクリル共重合体であるアニオン性ポリマーとポリアミンであるカチオン性ポリマーとを作用させ、凝集体を形成させた後に、この凝集をほどくことによって得られたエマルジョンタイプのカチオン性樹脂だけを紙の表面に塗工することを開示している。 It is also known to combine an inorganic pigment having high ink absorbability such as porous synthetic silica as a material for forming the ink receiving layer. Patent Document 2 pays attention to the problem that an ink receiving layer forming material containing a large amount of inorganic pigment has a high hiding power of the material itself, so that the texture and color of the base paper (base material) are impaired. An ink jet recording paper that is excellent in quality and maintains the texture and color of the base paper is provided. In Patent Document 2, an anionic polymer that is a styrene-acrylic copolymer and a cationic polymer that is a polyamine are allowed to act to form an aggregate, and then an emulsion type cationic property obtained by unwinding the aggregate. It discloses that only the resin is applied to the paper surface.
特許文献３は、プリンタ内で供給される中間記録体に関する。特許文献３の発明は、インクを受容するインク受容性粒子であって、少なくとも前記インクの液体成分をトラップするトラップ構造を有し、かつ、吸液性樹脂を含んで構成したインク受容性粒子に関する。当該インク受容性粒子は、微粒子が集合した複合体粒子の形態を有する。 Patent Document 3 relates to an intermediate recording medium supplied in a printer. The invention of Patent Document 3 relates to ink receiving particles that receive ink, have a trap structure that traps at least a liquid component of the ink, and include a liquid-absorbing resin. . The ink receptive particles have a form of composite particles in which fine particles are aggregated.
被記録材として、紙類の他にも、樹脂フィルム、キャンバス、不織布等の様々な材質からなる基材が用いられる。しかしながら、紙類に用いられるインク受容層形成用処理液を樹脂フィルム等の基材に塗工すると、表面にべたつきが生じる、塗膜（インク受容層）の耐剥離性や耐水性が不足する等の課題があり、また、印刷後のインク定着性やインク耐水性が不足するなど十分なインクジェット印刷性能が得られないことがあった。すなわち、紙類に用いるインク受容層形成用処理液を樹脂フィルム等にそのまま転用することはできなかった。 As the recording material, in addition to papers, substrates made of various materials such as resin films, canvases and nonwoven fabrics are used. However, when the ink-receiving layer forming treatment liquid used for paper is applied to a substrate such as a resin film, the surface becomes sticky, and the coating film (ink-receiving layer) has insufficient peel resistance and water resistance. In addition, sufficient ink jet printing performance may not be obtained due to insufficient ink fixing properties and ink water resistance after printing. That is, the ink-receiving layer forming treatment liquid used for papers could not be diverted directly to a resin film or the like.
本発明は上記の状況に鑑み、樹脂フィルム等の基材に適用した時にも塗膜（インク受容層）の耐剥離性及び耐水性に優れ、べたつきが無く、かつ、インクジェット印刷性能にも優れたインク受容層を形成することができる被記録材用処理液、及び、当該被記録材用処理液を用いて作成された被記録材を提供することを目的とする。 In view of the above situation, the present invention is excellent in peeling resistance and water resistance of a coating film (ink receiving layer) when applied to a substrate such as a resin film, is not sticky, and is excellent in ink jet printing performance. It is an object of the present invention to provide a recording material treatment liquid capable of forming an ink receiving layer and a recording material prepared using the recording material treatment liquid.
発明者らは上記課題に対して、水溶性のアニオン性ポリマーと水溶性のカチオン性ポリマーとを混合しながら分散させて得られる、アニオン性ポリマーとカチオン性ポリマーとが一体となった非水溶性の有機複合粒子に着目した。さらに、カチオン性ポリマーとして、架橋性を有するカチオン性ポリマーを少なくとも含むことによって、べたつきがなく、耐剥離性及び耐水性に優れた塗膜を形成可能な被記録材用処理液を得られることを見出し、さらに、当該被記録材用処理液を塗工して得たインク受容層は、インクジェット印刷性能も優れたものとなることを見出し、本発明を完成した。 In order to solve the above problems, the inventors have obtained a water-insoluble anionic polymer and a cationic polymer, which are obtained by dispersing a water-soluble anionic polymer and a water-soluble cationic polymer while mixing them. We focused on organic composite particles. Furthermore, by containing at least a cationic polymer having a crosslinking property as a cationic polymer, it is possible to obtain a treatment liquid for a recording material that can form a coating film having no stickiness and excellent in peel resistance and water resistance. Further, the present inventors have found that the ink receiving layer obtained by applying the recording material treatment liquid has excellent ink jet printing performance and completed the present invention.
すなわち本発明は、架橋性を有するカチオン性ポリマーを少なくとも含むカチオン性ポリマーと、アニオン性ポリマーとを含有してなる有機複合粒子が分散された、被記録材用処理液に関する。また、架橋性を有するカチオン性ポリマーと、架橋性を有さないカチオン性ポリマーと、アニオン性ポリマーとを含有してなる有機複合粒子であることが好ましい。当該有機複合粒子の平均粒径は、０．１〜１０μｍであることが好ましい。 That is, the present invention relates to a processing liquid for recording material in which organic composite particles containing a cationic polymer containing at least a cationic polymer having crosslinkability and an anionic polymer are dispersed. Moreover, it is preferable that it is an organic composite particle containing the cationic polymer which has crosslinkability, the cationic polymer which does not have crosslinkability, and an anionic polymer. The average particle diameter of the organic composite particles is preferably 0.1 to 10 μm.
また、前記架橋性を有するカチオン性ポリマーは、ポリアミドアミン−エピハロヒドリン樹脂であることが好ましく、アニオン性ポリマーは、スチレン−（メタ）アクリル酸共重合体であることが好ましい。 The cationic polymer having crosslinkability is preferably a polyamidoamine-epihalohydrin resin, and the anionic polymer is preferably a styrene- (meth) acrylic acid copolymer.
また、全カチオン性ポリマーに対する、架橋性を有するカチオン性ポリマーの割合は、１％〜１００％（質量比）であることが好ましい。なお全カチオン性ポリマーとは前記架橋性を有するカチオン性ポリマーと、架橋性を有さないカチオン性ポリマーの合計を表す。
また、全ポリマーに対する、全カチオン性ポリマーの割合が、１０％〜９０％（質量比）であることが好ましい。なお全ポリマーとは全カチオン性ポリマーとアニオン性ポリマーの合計を表す。
Moreover, it is preferable that the ratio of the cationic polymer which has crosslinkability with respect to all the cationic polymers is 1%-100% (mass ratio). The total cationic polymer represents the total of the cationic polymer having crosslinkability and the cationic polymer having no crosslinkability.
Moreover, it is preferable that the ratio of all the cationic polymers with respect to all the polymers is 10%-90% (mass ratio). The total polymer represents the total of all cationic polymers and anionic polymers.
また本発明は、前記のいずれかに記載の被記録材用処理液に含まれる、有機複合粒子に関する。 The present invention also relates to organic composite particles contained in any of the recording material processing liquids described above.
また本発明は、前記のいずれかに記載の被記録材用処理液を基材に塗工してなる、被記録材に関する。前記基材は、紙、樹脂フィルム又は布帛であることが好ましい。 The present invention also relates to a recording material obtained by coating a substrate with the recording material treatment liquid described in any one of the above. The substrate is preferably paper, a resin film, or a fabric.
さらに本発明は、前記の被記録材に、インクジェット印刷を行うインクジェット記録方法に関する。 Furthermore, the present invention relates to an ink jet recording method for performing ink jet printing on the recording material.
本発明によれば、樹脂フィルム等の基材に対して適用した場合でも塗膜のべたつきが無く、かつ、塗膜の密着性（耐剥離性、耐水性）に優れたインク受容層を形成することが可能な被記録材用処理液を得ることができる。また当該形成されたインク受容層はインクジェット印刷性能にも優れる。本発明によれば、インクジェット印刷性能及び画像の耐久性に優れた被記録材を得ることができる。 According to the present invention, even when applied to a substrate such as a resin film, an ink receiving layer having no stickiness of the coating film and excellent in adhesion (peeling resistance, water resistance) of the coating film is formed. It is possible to obtain a processing liquid for a recording material that can be recorded. The formed ink receiving layer is also excellent in ink jet printing performance. According to the present invention, a recording material excellent in ink jet printing performance and image durability can be obtained.
本発明の被記録材用処理液は、水系溶媒中に非水溶性の有機複合粒子が分散された水系分散液である。有機複合粒子とは、複数種類の有機成分がポリマーコンプレックス、イオンコンプレックス、化学結合等の任意の態様で互いに一体となって粒子を形成しているものを意味している。有機複合粒子は、有機成分のみからなるものに限定されず、有機成分と無機成分とを含んでもよい。分散液の溶媒は、主に水を含むものであれば限定されず、分散剤、酸、塩、有機溶媒等の任意の物質を含んでいてもよい。 The recording material treatment liquid of the present invention is an aqueous dispersion in which water-insoluble organic composite particles are dispersed in an aqueous solvent. The organic composite particles mean particles in which a plurality of types of organic components are integrated with each other in any manner such as a polymer complex, an ion complex, and a chemical bond. The organic composite particles are not limited to those composed only of organic components, and may include organic components and inorganic components. The solvent of the dispersion is not limited as long as it mainly contains water, and may contain any substance such as a dispersant, an acid, a salt, and an organic solvent.
有機複合粒子は、少なくとも架橋性を有するカチオン性ポリマーとアニオン性ポリマーとを含むが、架橋性を有するカチオン性ポリマーと、架橋性を有さないカチオン性ポリマーと、アニオン性ポリマーとを含むことが好ましい。
架橋性を有するカチオン性ポリマーは、架橋性の官能基を有するカチオン性のポリマーで水溶性を有するものが用いられる。このようなポリマーとしては、特開２００９−１０８４３３号公報に記載のポリアミドポリアミン−エピハロヒドリン樹脂や、メラミンホルムアルデヒド樹脂、尿素ホルムアルデヒド樹脂、ジシアンジアミド−ホルムアルデヒド樹脂等が挙げられる。中でもポリアミドポリアミン−エピハロヒドリン樹脂、具体的には、ポリアミドポリアミン−エピクロロヒドリン樹脂であることが好ましい。
The organic composite particles include at least a cationic polymer having crosslinkability and an anionic polymer, but may include a cationic polymer having crosslinkability, a cationic polymer having no crosslinkability, and an anionic polymer. preferable.
As the cationic polymer having crosslinkability, a cationic polymer having a crosslinkable functional group and having water solubility is used. Examples of such a polymer include polyamide polyamine-epihalohydrin resin, melamine formaldehyde resin, urea formaldehyde resin, dicyandiamide-formaldehyde resin described in JP-A-2009-108433. Of these, polyamide polyamine-epihalohydrin resin, specifically, polyamide polyamine-epichlorohydrin resin is preferable.
ポリアミドポリアミン−エピハロヒドリン樹脂としては、例えば、ポリ（Ｎ−アルキルジアリルアミン）酸付加塩とエピハロヒドリンを反応させ、ついで無機酸を反応させ、ついでエポキシ基をハロヒドリン基に転化させて得られるものが挙げられ、一般に湿潤紙力向上剤として使用されるカチオン性ポリマーを好適に用いることができる。具体的には、星光ＰＭＣ社製湿潤紙力剤「ＷＳシリーズ」、荒川化学工業社製湿潤紙力増強剤「アラフィックスシリーズ」等が挙げられる。これらの架橋性カチオン性ポリマーは湿潤紙力向上剤として公知であったが、インク受容層を形成するための処理剤において、これらの架橋性カチオン性ポリマーをアニオン性ポリマーと併用することによって優れたインク受容層形成用処理剤となることは、本発明において初めて見出された。より好ましくは、架橋性カチオン性ポリマーを非架橋性カチオン性ポリマー及びアニオン性ポリマーと併用することである。 Examples of the polyamide polyamine-epihalohydrin resin include those obtained by reacting a poly (N-alkyldiallylamine) acid addition salt with an epihalohydrin, then reacting with an inorganic acid, and then converting an epoxy group to a halohydrin group, Cationic polymers that are generally used as wet paper strength improvers can be suitably used. Specific examples include wet paper strength agent “WS series” manufactured by Seiko PMC, and wet paper strength enhancer “Arafix series” manufactured by Arakawa Chemical Industries. These crosslinkable cationic polymers were known as wet paper strength improvers, but they were excellent by using these crosslinkable cationic polymers in combination with anionic polymers in the treatment agent for forming the ink receiving layer. It has been found for the first time in the present invention that it becomes a treatment agent for forming an ink receiving layer. More preferably, the crosslinkable cationic polymer is used in combination with a non-crosslinkable cationic polymer and an anionic polymer.
架橋性を有さないカチオン性ポリマーとしては、架橋性の官能基を有さない、水溶性のカチオン性ポリマーが用いられる。このようなポリマーとしては、架橋性の無いポリアミン樹脂が挙げられる。例えば、ポリアミンとして、グアニジン系縮合ポリアミン、ジシアンジアミドホルマリン縮合物、アクリルアミド−ジアリルアミン塩共重合物、第２級アミノ基、第３級アミノ基や第４級アンモニウム基を有するアクリル重合体、ポリビニルアミン、ポリビニルアミジン、５員環アミジン類、ジシアンジアミド−ホルマリン共重合体に代表されるジシアン系カチオン樹脂、ジシアンジアミド−ポリエチレンアミン共重合物に代表されるポリアミン系カチオン樹脂、ポリエチレンポリアミンやポリプロピレンポリアミンなどのポリアルキレンポリアミン類又はその誘導体、ジアリルジメチルアンモニウム−ＳＯ２共重合物、ジアリルアミン塩−ＳＯ２共重合物、ジアリルジメチルアンモニウムクロライド重合物、アリルアミン塩の重合物、ビニルベンジルトリアリルアンモニウム塩の単独重合体又は共重合体、ジアルキルアミノエチル（メタ）アクリレート４級塩共重合物等が挙げられる。なかでも、ジシアンジアミド・ポリアルキレンポリアミン縮合物、アルキルアミン・エピクロロヒドリン縮合物、ポリエチレンイミン−エピクロロヒドリン縮合物等が挙げられる。 As the cationic polymer having no crosslinkability, a water-soluble cationic polymer having no crosslinkable functional group is used. Examples of such a polymer include polyamine resins having no crosslinkability. For example, polyamines include guanidine-based condensed polyamine, dicyandiamide formalin condensate, acrylamide-diallylamine salt copolymer, secondary amino group, acrylic polymer having tertiary amino group or quaternary ammonium group, polyvinylamine, polyvinyl Amidine, 5-membered ring amidines, dicyan cation resin represented by dicyandiamide-formalin copolymer, polyamine cation resin represented by dicyandiamide-polyethyleneamine copolymer, polyalkylene polyamines such as polyethylene polyamine and polypropylene polyamine or derivatives thereof, diallyl dimethyl ammonium -SO 2 copolymer, diallylamine salt -SO 2 copolymer, diallyl dimethyl ammonium chloride polymer, polymer of allylamine salt, bi- Homopolymers or copolymers of Le benzyl triallyl ammonium salts, dialkyl aminoethyl (meth) acrylate 4 Kyushiotomo polymer and the like. Among them, dicyandiamide / polyalkylenepolyamine condensate, alkylamine / epichlorohydrin condensate, polyethyleneimine-epichlorohydrin condensate and the like can be mentioned.
ポリアミンとして、具体的には例えば、ＰＡＰ−１、ＰＡＰ−２、ＰＡＬ−１、ＫＺ−１２５Ｋ、ユニセンスＣＰ−１０１（以上センカ社製）、モーリンフィックスコンク＃３００Ｂ（以上モーリン化学工業社製）等が挙げられる。 Specific examples of polyamines include PAP-1, PAP-2, PAL-1, KZ-125K, Unisense CP-101 (above made by Senka), Morinfix concrete # 300B (above made by Morin Chemical Industries), etc. Is mentioned.
本発明の特徴は、有機複合粒子を形成するカチオン性ポリマーとして、架橋性のカチオン性ポリマーを用いることである。特に好ましくは架橋性のカチオン性ポリマーと非架橋性のカチオン性ポリマーとを組み合わせて用いることであり、全カチオン性ポリマー対する、架橋性を有するカチオン性ポリマーの割合は、１％〜１００％（質量比）とすることが好ましい。更に好ましくは１０％〜５０％（質量比）である。この範囲であれば、フィルム等の基材に塗工した際、基材の表面上で架橋が生じて密着性と耐久性に優れ、かつ、べたつきの無い塗膜が得られるものと考えられている。 The feature of the present invention is that a crosslinkable cationic polymer is used as the cationic polymer forming the organic composite particles. Particularly preferably, a crosslinking cationic polymer and a non-crosslinking cationic polymer are used in combination, and the ratio of the cationic polymer having crosslinking property to the total cationic polymer is 1% to 100% (mass). Ratio). More preferably, it is 10% to 50% (mass ratio). If it is within this range, it is considered that when coated on a substrate such as a film, a cross-linking occurs on the surface of the substrate, resulting in excellent adhesion and durability and a non-sticky coating film. Yes.
アニオン性ポリマーとは、負の電荷を有するポリマーであり、例えば、カルボキシル基、スルホン基、リン酸基等のアニオン性基を有する不飽和結合含有モノマーの重合体又は共重合体である。本発明においては、水溶性のアニオン性ポリマーが用いられ、スチレン−（メタ）アクリル酸共重合体、ポリ（メタ）アクリル酸、スチレン−無水マレイン酸共重合体、（メタ）アクリル酸アルキルエステル−（メタ）アクリル酸共重合体、（メタ）アクリル酸アルキルエステル−スチレンスルホン酸共重合体、（メタ）アクリル酸アルキルエステル−クロトン酸共重合体、（メタ）アクリル酸アルキルエステル−イタコン酸共重合体、（メタ）アクリル酸アルキルエステル−フマル酸共重合体、それらの塩等が挙げられ、特に、スチレン−（メタ）アクリル酸共重合体であることが好ましい。アニオン性ポリマーは、１種でも２種以上を混合して用いてもよい。 An anionic polymer is a polymer having a negative charge, for example, a polymer or copolymer of an unsaturated bond-containing monomer having an anionic group such as a carboxyl group, a sulfone group, and a phosphate group. In the present invention, a water-soluble anionic polymer is used, and styrene- (meth) acrylic acid copolymer, poly (meth) acrylic acid, styrene-maleic anhydride copolymer, (meth) acrylic acid alkyl ester- (Meth) acrylic acid copolymer, (meth) acrylic acid alkyl ester-styrene sulfonic acid copolymer, (meth) acrylic acid alkyl ester-crotonic acid copolymer, (meth) acrylic acid alkyl ester-itaconic acid copolymer Examples thereof include a copolymer, a (meth) acrylic acid alkyl ester-fumaric acid copolymer, and salts thereof, and a styrene- (meth) acrylic acid copolymer is particularly preferable. Anionic polymers may be used alone or in combination of two or more.
アニオン性ポリマーとして具体的には、ＢＡＳＦ社製Ｊｏｎｃｒｙｌ６９０、Ｊｏｎｃｒｙｌ６７８等のＪｏｎｃｒｙｌシリーズ、荒川化学工業社製「ポリマロン３８５」、「ポリマロン１３３３」、「ＷＲ−３００Ｄ」、モンサント社製「スクリプセット５２０」、星光ＰＭＣ社製「ＳＳ２５６０」等が挙げられる。 Specific examples of the anionic polymer include Joncryl 690 and Joncryl 678 manufactured by BASF, “Polymaron 385”, “Polymallon 1333”, “WR-300D”, “SCRIPSET 520” manufactured by Monsanto, Examples include “SS2560” manufactured by Seiko PMC.
また、全ポリマー（架橋性カチオン性ポリマーと非架橋性カチオン性ポリマーとアニオン性ポリマーの合計）に対する、全カチオン性ポリマー（架橋性カチオン性ポリマーと非架橋性カチオン性ポリマーの合計）の割合が、１０％〜９０％（質量比）好ましくは５０％〜８０％（質量比）とすることができる。カチオン性ポリマーの割合を５０％〜８０％（質量比）の範囲とすれば、十分なインク吸液性および耐水性が得られるため好ましい。 Further, the ratio of the total cationic polymer (the total of the crosslinkable cationic polymer and the non-crosslinkable cationic polymer) to the total polymer (the total of the crosslinkable cationic polymer, the non-crosslinkable cationic polymer, and the anionic polymer) is 10% to 90% (mass ratio), preferably 50% to 80% (mass ratio). If the ratio of the cationic polymer is in the range of 50% to 80% (mass ratio), it is preferable because sufficient ink absorbability and water resistance can be obtained.
本発明の被記録材用処理液は、任意の割合で水と混合可能であり、濃度は特に制限されるものではないが、例えば処理液全体に対する、アニオン性ポリマーとカチオン性ポリマー成分の合計（有機複合粒子の含有量）を１％〜５０％（質量比）とすることができる。この範囲であれば、分散安定性および塗布性の点で好ましい。 The processing liquid for recording material of the present invention can be mixed with water at an arbitrary ratio, and the concentration is not particularly limited. For example, the total of the anionic polymer and the cationic polymer component with respect to the entire processing liquid ( The content of the organic composite particles) can be 1% to 50% (mass ratio). If it is this range, it is preferable at the point of dispersion stability and applicability | paintability.
また、本発明の処理液には、上記のポリマー成分以外に任意の成分を含むことができる。例えば、分散剤を、処理液全体に対して０．１％〜１０％（質量比）含むことができる。分散剤は公知の分散剤、例えば、高分子分散剤、界面活性剤あるいはカップリング剤などを使用することができる。高分子分散剤の好ましい例としては天然高分子が挙げられ、その具体例としては、にかわ、ゼラチン、カゼイン、若しくはアルブミンなどのたんぱく質類、アラビアゴム、若しくはトラガントゴムなどの天然ゴム類、サポニンなどのグルコシド類、アルギン酸及びアルギン酸プロピレングリコールエステル、アルギン酸トリエタノールアミン、若しくはアルギン酸アンモニウムなどのアルギン酸誘導体、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、若しくはエチルヒドロキシセルロースなどのセルロース誘導体などが挙げられる。これらは、単独で又は二種以上を組み合わせて使用することができる。 In addition, the treatment liquid of the present invention may contain any component other than the above polymer components. For example, the dispersant can be contained in an amount of 0.1% to 10% (mass ratio) with respect to the entire processing liquid. As the dispersant, a known dispersant such as a polymer dispersant, a surfactant, or a coupling agent can be used. Preferred examples of the polymer dispersant include natural polymers. Specific examples thereof include proteins such as glue, gelatin, casein or albumin, natural gums such as gum arabic or gum tragacanth, and glucosides such as saponin. Alginic acid and alginic acid propylene glycol ester, alginic acid triethanolamine, alginic acid derivatives such as ammonium alginate, and cellulose derivatives such as methylcellulose, carboxymethylcellulose, hydroxyethylcellulose, and ethylhydroxycellulose. These can be used alone or in combination of two or more.
さらに、高分子分散剤の他の好ましい例として合成高分子が挙げられる。その具体的な例として、ポリアミン系樹脂、ポリカルボン酸系樹脂、ポリエステル系樹脂、ポリウレタン系樹脂、ポリビニルアルコール類、ポリビニルピロリドン類、ポリアクリル酸系樹脂、アクリル酸−アクリルニトリル共重合体、アクリル酸カリウム−アクリルニトリル共重合体、酢酸ビニル−アクリル酸エステル共重合体、若しくはアクリル酸−アクリル酸エステル共重合体等のアクリル酸系樹脂、スチレン−アクリル酸共重合体、スチレン−メタクリル酸共重合体、スチレン−メタクリル酸−アクリル酸エステル共重合体、スチレン−α−メチルスチレン−アクリル酸共重合体、若しくはスチレン−α−メチルスチレン−アクリル酸−アクリル酸エステル共重合体等のスチレン−アクリル酸系樹脂、スチレン−マレイン酸共重合体、スチレン−無水マレイン酸共重合体、ビニルナフタレン−アクリル酸共重合体、ビニルナフタレン−マレイン酸共重合体、及び酢酸ビニル−エチレン共重合体、酢酸ビニル−脂肪酸ビニルエチレン共重合体、酢酸ビニル−マレイン酸エステル共重合体、酢酸ビニル−クロトン酸共重合体、酢酸ビニル−アクリル酸共重合体等の酢酸ビニル系共重合体及びそれらの塩が挙げられる。 Furthermore, another preferred example of the polymer dispersant is a synthetic polymer. Specific examples include polyamine resins, polycarboxylic acid resins, polyester resins, polyurethane resins, polyvinyl alcohols, polyvinyl pyrrolidones, polyacrylic acid resins, acrylic acid-acrylonitrile copolymers, acrylic acid. Acrylic resins such as potassium-acrylonitrile copolymer, vinyl acetate-acrylic ester copolymer, or acrylic acid-acrylic ester copolymer, styrene-acrylic acid copolymer, styrene-methacrylic acid copolymer Styrene-acrylic acid type copolymer such as styrene-methacrylic acid-acrylic acid ester copolymer, styrene-α-methylstyrene-acrylic acid copolymer, or styrene-α-methylstyrene-acrylic acid-acrylic acid ester copolymer Resin, styrene-maleic acid copolymer, Tylene-maleic anhydride copolymer, vinylnaphthalene-acrylic acid copolymer, vinylnaphthalene-maleic acid copolymer, vinyl acetate-ethylene copolymer, vinyl acetate-fatty acid vinylethylene copolymer, vinyl acetate-malein Examples thereof include vinyl acetate copolymers such as acid ester copolymers, vinyl acetate-crotonic acid copolymers, vinyl acetate-acrylic acid copolymers, and salts thereof.
また、界面活性剤の好ましい例としては、例えばポリオキシエチレンアルキルエーテル、ポリオキシアルキレンアルキルエーテル、ポリオキシエチレン誘導体、オキシエチレン−オキシプロピレンブロック共重合体、ソルビタン脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステル、ポリオキシエチレンソルビトール脂肪酸エステル、グリセリン脂肪酸エステル、ポリオキシエチレン脂肪酸エステル、ポリオキシエチレンアルキルアミン、アルキルアルカノードアミド、ノニルフェノール、アルキルノニルフェノール、ポリオキシアルキレングリコール、アルキルアミンオキサイド、アセチレンジオール、ポリオキシエチレンノニルフェニルエーテル、ポリオキシエチレンアルキルフェニルエーテル変性シリコーンなどのシリコーン系界面活性剤、炭化水素系界面活性剤の疎水基にある水素原子の少なくとも１つがフッ素原子で置換されたフッ素系界面活性剤等のノニオン系界面活性剤が挙げられる。 Further, preferable examples of the surfactant include, for example, polyoxyethylene alkyl ether, polyoxyalkylene alkyl ether, polyoxyethylene derivative, oxyethylene-oxypropylene block copolymer, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, Polyoxyethylene sorbitol fatty acid ester, glycerin fatty acid ester, polyoxyethylene fatty acid ester, polyoxyethylene alkylamine, alkyl alkanodeamide, nonylphenol, alkylnonylphenol, polyoxyalkylene glycol, alkylamine oxide, acetylenic diol, polyoxyethylene nonylphenyl Silicone such as ether and polyoxyethylene alkylphenyl ether modified silicone System surfactant, a nonionic surfactant such as a fluorine-containing surfactant at least one substituted with a fluorine atom of the hydrogen atoms in the hydrophobic group of a hydrocarbon-based surfactants.
あるいは、例えば塩化ラウリルトリメチルアンモニウム、臭化セチルトリメチルアンモニウム、塩化ステアリルトリメチルアンモニウム、または、アルキルジメチルベンジルアンモニウム塩類、塩化ステアリルジメチルベンジルアンモニウム、塩化ベンザルコニウム、塩化ラウリルジメチルベンジルアンモニウム塩等のカチオン系界面活性剤が挙げられる。 Alternatively, cationic surface activity such as lauryltrimethylammonium chloride, cetyltrimethylammonium bromide, stearyltrimethylammonium chloride, or alkyldimethylbenzylammonium salts, stearyldimethylbenzylammonium chloride, benzalkonium chloride, lauryldimethylbenzylammonium chloride, etc. Agents.
あるいは、脂肪酸塩、アルキル硫酸エステル塩、アルキルエーテル硫酸エステル塩、アルキルベンゼンスルホン酸塩、アルキルナフタレンスルホン酸塩、アルキルスルホコハク酸塩、アルキルジフェニルエーテルジスルホン酸塩、アルキルリン酸塩、ポリオキシエチルアルキル硫酸エステル塩、ポリオキシエチルアルキルアリル硫酸エステル塩、α−オレフィンスルホン酸塩、メチルタウリン酸塩、エーテルカルボン酸塩、ナフタレンスルホン酸ホルマリン縮合物、ポリオキシエチレンアルキルリン酸エステル等のアニオン系界面活性剤が挙げられる。 Alternatively, fatty acid salt, alkyl sulfate ester salt, alkyl ether sulfate ester salt, alkyl benzene sulfonate, alkyl naphthalene sulfonate, alkyl sulfosuccinate, alkyl diphenyl ether disulfonate, alkyl phosphate, polyoxyethyl alkyl sulfate salt Anionic surfactants such as polyoxyethyl alkyl allyl sulfate, α-olefin sulfonate, methyl taurate, ether carboxylate, naphthalene sulfonate formalin condensate, polyoxyethylene alkyl phosphate, etc. It is done.
あるいは、アラニン系、イミダゾリウムベタイン系、アミドプロピルベタイン系、アミノジプロピオン酸塩等の両性界面活性剤が挙げられる。さらに、シラン系カップリング剤、アルミニウム系カップリング剤、チタン系カップリング剤、ジルコニウム系カップリング剤等のカップリング剤が挙げられる。 Alternatively, amphoteric surfactants such as alanine, imidazolium betaine, amidopropyl betaine, aminodipropionate and the like can be mentioned. Furthermore, coupling agents, such as a silane coupling agent, an aluminum coupling agent, a titanium coupling agent, and a zirconium coupling agent, are mentioned.
さらに処理液には本発明の効果を妨げない限りにおいて、各種の添加剤、例えば、バインダー、粘度調整剤、安定化剤、顔料分散剤、流動性変性剤、消泡剤、抑泡剤、離型剤、発泡剤、浸透剤、架橋剤、耐水化剤、保湿剤、防腐剤、酸化防止剤、蛍光増白剤、紫外線吸収剤、着色染料、顔料などの任意の成分を含むことができる。 Furthermore, various additives such as a binder, a viscosity modifier, a stabilizer, a pigment dispersant, a fluidity modifier, an antifoaming agent, an antifoaming agent, a release agent are used in the treatment liquid as long as the effects of the present invention are not impaired. Optional components such as a mold agent, a foaming agent, a penetrating agent, a crosslinking agent, a water-resistant agent, a moisturizing agent, an antiseptic, an antioxidant, a fluorescent brightening agent, an ultraviolet absorber, a coloring dye, and a pigment can be included.
バインダーとしては一般にインクジェット受容層に用いられる公知のものが使用でき、例えば水溶性ポリマーとしてはポリビニルアルコール、ポリビニルピロリドン、ポリエチレングリコール、ポリウレタン、ポリエチレンオキサイド、ポリエステル、澱粉、ポリアクリル酸エステルやそれらの誘導体等が挙げられる。 As the binder, known ones generally used in an ink jet receiving layer can be used. Examples of water-soluble polymers include polyvinyl alcohol, polyvinyl pyrrolidone, polyethylene glycol, polyurethane, polyethylene oxide, polyester, starch, polyacrylic acid ester, and derivatives thereof. Is mentioned.
粘度調整剤としては公知のものが使用でき、例えば、デキストリン、キサンタンガム、カルボキシメチルセルロースなどの多糖類およびその誘導体等が挙げられる。 As the viscosity modifier, known ones can be used, and examples thereof include polysaccharides such as dextrin, xanthan gum, carboxymethylcellulose, and derivatives thereof.
架橋剤としては本発明の処理液の含有成分を架橋しうるものであれば特に制限はないが、例えばホルムアルデヒド、グリオキザール、グルタルアルデヒド、サクシンアルデヒド等のアルデヒド類、ジメチロール尿素等のＮ−メチロール類、ビニルスルホン基やアクリルアミド基等を有する活性エチレン類、エチレンイミン類、エポキシ類、カルボジイミド類等が挙げられる。 The crosslinking agent is not particularly limited as long as it can crosslink the components contained in the treatment liquid of the present invention. For example, aldehydes such as formaldehyde, glyoxal, glutaraldehyde, and succinaldehyde, N-methylols such as dimethylolurea, Examples thereof include active ethylenes having a vinyl sulfone group and an acrylamide group, ethyleneimines, epoxies, carbodiimides and the like.
顔料としては公知のものが使用でき、シリカ、クレー、雲母、タルク、酸化チタン、酸化亜鉛、炭酸カルシウム、硫酸バリウム、酸化アルミニウム等の無機顔料や、アクリル、ポリスチレン等の有機顔料が挙げられる。 Known pigments can be used, and examples thereof include inorganic pigments such as silica, clay, mica, talc, titanium oxide, zinc oxide, calcium carbonate, barium sulfate, and aluminum oxide, and organic pigments such as acrylic and polystyrene.
本発明の処理液の溶媒は水であるが、粘度や塗工性等の改善の目的で本発明の効果を妨げないかぎりにおいて、各種水溶性溶媒を含むことができる。 The solvent of the treatment liquid of the present invention is water, but various water-soluble solvents can be included as long as the effects of the present invention are not hindered for the purpose of improving viscosity, coating properties, and the like.
水溶性溶媒としてはメタノール、エタノール、１−プロパノール、イソプロピルアルコール、エチレングリコール、アセトン、テトラヒドロフラン、酢酸エチル等が挙げられる。 Examples of the water-soluble solvent include methanol, ethanol, 1-propanol, isopropyl alcohol, ethylene glycol, acetone, tetrahydrofuran, and ethyl acetate.
本発明の処理液に含有される有機複合粒子の粒径は、０．１〜１０μｍであることが好ましく、０．５〜５μｍであれば十分なインク吸液性および塗工時の平滑性が得られるためより好ましい。なお、本明細書での粒径は、粒子の平均メディアン径であり、例えば、日機装社製の商品名：「マイクロトラックＭＴ３０００ＩＩ」を用いて水分散性微粒子の平均粒子径（メディアン径：ｄ５０）を測定することができる。 The particle diameter of the organic composite particles contained in the treatment liquid of the present invention is preferably 0.1 to 10 μm, and if it is 0.5 to 5 μm, sufficient ink absorbability and smoothness at the time of coating are obtained. Since it is obtained, it is more preferable. The particle diameter in this specification is the average median diameter of the particles. For example, the average particle diameter of the water-dispersible fine particles (median diameter: d50) using a trade name “MICROTRACK MT3000II” manufactured by Nikkiso Co., Ltd. Can be measured.
本発明の処理液は公知の製造方法に準じて作成することができる。例えば、前記の架橋性カチオン性ポリマー、（非架橋性カチオン性ポリマー）及びアニオン性ポリマー及び水、必要に応じて添加剤等を配合し、混合、撹拌することによって、有機複合粒子が分散された処理液を得ることができる。混合、撹拌の方法は特に制限されず、従来公知の手法を用いればよいが、例えば、ホモジナイザー、ビーズミル、ボールミル、ジェットミル、ディスパー等を用いることができる。 The treatment liquid of the present invention can be prepared according to a known production method. For example, the above-mentioned crosslinkable cationic polymer, (non-crosslinkable cationic polymer), an anionic polymer and water, and additives as necessary are mixed, mixed, and stirred to disperse the organic composite particles. A treatment liquid can be obtained. The method of mixing and stirring is not particularly limited, and a conventionally known method may be used. For example, a homogenizer, a bead mill, a ball mill, a jet mill, a disper, or the like can be used.
前記の製造方法によって得られた被記録材用処理液を、基材の表面に塗工する。基材としては、木質紙、非木質紙、合成紙等の紙類の他、樹脂フィルム（ＰＥＴフィルム、ポリエステルフィルム、ポリプロピレンフィルム、塩ビフィルム、ポリカーボネートフィルム、ポリ（メタ）アクリレートフィルム、酢酸セルロースフィルム等）、天然繊維及び／又は合成繊維からなる織布及び／又は不織布等の布帛、ターポリン、ガラス、金属、皮革等を用いることができる。特に、本発明の処理液は樹脂フィルムに対して好適に用いられる。 The recording material treatment liquid obtained by the above production method is applied to the surface of the substrate. As base materials, in addition to paper such as wood paper, non-wood paper, and synthetic paper, resin films (PET film, polyester film, polypropylene film, polyvinyl chloride film, polycarbonate film, poly (meth) acrylate film, cellulose acetate film, etc. ), Fabrics such as woven fabrics and / or nonwoven fabrics made of natural fibers and / or synthetic fibers, tarpaulins, glass, metals, leathers, and the like. In particular, the treatment liquid of the present invention is suitably used for a resin film.
基材の表面には、インク受容層の下地として、アンカー層（バインダー層）が設けられていてもよい。アンカー層は特に制限されないが、例えば、オキサゾリン基含有ポリマー（例えば、エポクロスＫ−２０１０Ｅ、エポクロスＫ−２０２０Ｅ、エポクロスＫ−２０３０Ｅ、エポクロスＷＳ−３００、エポクロスＷＳ−５００、エポクロスＷＳ−７００等のエポクロスシリーズ、日本触媒社製）、ポリビニルアルコール、ポリエステル系樹脂、ポリウレタン系樹脂、アクリル系樹脂、スチレン−アクリル系樹脂、エチレン−酢酸ビニル系樹脂等のうち接着性を有するものを用いることができる。なお、本発明の処理液によって形成される塗膜の基材への密着性が特に優れるときには、アンカー層が不要となる場合もある。 An anchor layer (binder layer) may be provided on the surface of the substrate as a base for the ink receiving layer. The anchor layer is not particularly limited. For example, an oxazoline group-containing polymer (for example, Epocross such as Epocross K-2010E, Epocross K-2020E, Epocross K-2030E, Epocross WS-300, Epocross WS-500, Epocross WS-700, etc.) Series, manufactured by Nippon Shokubai Co., Ltd.), polyvinyl alcohol, polyester resin, polyurethane resin, acrylic resin, styrene-acrylic resin, ethylene-vinyl acetate resin, and the like can be used. In addition, when the adhesiveness to the base material of the coating film formed with the process liquid of this invention is especially excellent, an anchor layer may become unnecessary.
水系分散液である本発明の処理液は、必要に応じて所定の濃度に調整され、また、必要に応じて他の処理剤と混合されて、基材上に塗工される。塗工方法は公知の方法を用いることができ、特に制限されないが、例えば、メーヤーバー、バーコーター、ナイフコーター、ロールコーター、ブレードコーター、グラビアコーター、スプレーコーター、ブラシコーター、サイズプレス等を用いることができる。また、この処理液をインクとして、凸版式印刷、フレキソ印刷、オフセット印刷、グラビア印刷、スクリーン印刷などの公知の印刷法により基材に塗工することも可能である。なお、基材上にアンカー層が形成されている場合は当然、アンカー層の上に処理液が塗工されるが、本明細書においてはこれらの場合も「基材上に処理液を塗工する」という。 The treatment liquid of the present invention, which is an aqueous dispersion, is adjusted to a predetermined concentration as necessary, and is mixed with other treatment agents as needed and coated on a substrate. A known method can be used as the coating method, and is not particularly limited. For example, a Mayer bar, bar coater, knife coater, roll coater, blade coater, gravure coater, spray coater, brush coater, size press or the like may be used. it can. Moreover, it is also possible to apply this treatment liquid as an ink on a substrate by a known printing method such as letterpress printing, flexographic printing, offset printing, gravure printing, and screen printing. Of course, when the anchor layer is formed on the base material, the treatment liquid is applied on the anchor layer. However, in this specification, the treatment liquid is applied to the base material. It is said.
基材への本発明の処理液の塗工量は基材によって異なるため特に限定されないが、一般的に１〜５００ｇ／ｍ２とすることができる。所定量の処理液を塗工した後乾燥、定着処理が行われ、本発明の処理液を基材に塗工してなる被記録材が得られる。処理液中の有機複合粒子の濃度は１％〜５０％（質量比）であるため、基材表面に塗工される有機複合粒子の量は０．１〜５０ｇ／ｍ２程度となり、基材が樹脂フィルムの場合は１０〜４０ｇ／ｍ２程度が好ましい。１０ｇ／ｍ２以下になるとインク吸収性が不十分でインクが乾燥しない恐れがあり、４０ｇ／ｍ２以上では塗工量を増やしても性能は変わらず、経済面で不利となる。 Although the coating amount of the treatment liquid of the present invention on the substrate is not particularly limited because it varies depending on the substrate, it can generally be 1 to 500 g / m 2 . After applying a predetermined amount of the processing liquid, drying and fixing processes are performed, and a recording material obtained by coating the base material with the processing liquid of the present invention is obtained. Since the concentration of the organic composite particles in the treatment liquid is 1% to 50% (mass ratio), the amount of the organic composite particles applied to the substrate surface is about 0.1 to 50 g / m 2 , Is preferably about 10 to 40 g / m 2 . If it is 10 g / m 2 or less, the ink absorbability is insufficient and the ink may not be dried. If it is 40 g / m 2 or more, the performance does not change even if the coating amount is increased, which is disadvantageous in terms of economy.
乾燥方法としては特に限定されないが、熱風乾燥法、赤外乾燥法、ドラム乾燥法などが挙げられる。また公知のキャストコート法を用いて乾燥を行い、光沢面を形成することも可能である。 The drying method is not particularly limited, and examples thereof include a hot air drying method, an infrared drying method, and a drum drying method. It is also possible to form a glossy surface by drying using a known cast coating method.
また光沢度や平滑性の向上を目的にカレンダー処理を行うことができる。カレンダー処理としてはグロスカレンダー、スーパーカレンダー、ソフトカレンダーなどが挙げられる。 In addition, calendar processing can be performed for the purpose of improving glossiness and smoothness. Examples of calendar processing include gross calendar, super calendar, and soft calendar.
前記被記録材は、各種印刷、例えばインクジェット印刷、オフセット印刷、レーザー印刷、昇華転写等に使用できるが、特にインクジェット印刷に好適である。また基材が樹脂フィルムである本発明の被記録材は、インク受容層の密着性と透明性に優れるため、意匠性の高い梱包用フィルム、ラベル、シール、電飾用乳白ＰＥＴフィルム等として好適に用いられる。 The recording material can be used for various types of printing such as inkjet printing, offset printing, laser printing, sublimation transfer, and the like, and is particularly suitable for inkjet printing. In addition, the recording material of the present invention in which the base material is a resin film is excellent in adhesion and transparency of the ink receiving layer, and is therefore suitable as a packaging film, label, seal, and white milk PET film for electric decoration with high design properties. Used for.
本発明に係る被記録材は、基材の片面もしくは両面に塗工層が形成される。その際、同一面の塗工層を必要に応じて２層以上の多層構造にすることも可能である。なお、両面塗工や多層構造にする場合、各々の塗液が同一または同一塗工量である必要はなく、所望の品質レベルに応じて適宜調整して配合すればよい。多層構造の例としては、本発明の被記録材用処理液を基材に下塗りし、当該塗布層上に感熱層を設けたものや、逆に基材に感熱層塗液を下塗りし、当該塗布層上に本発明の被記録材用処理液の塗布層を設けたものが挙げられる。 In the recording material according to the present invention, a coating layer is formed on one side or both sides of a base material. In that case, it is also possible to make the coating layer of the same surface into the multilayered structure of two or more layers as needed. In addition, when it makes double-sided coating or a multilayer structure, each coating liquid does not need to be the same or the same coating amount, and should just adjust and mix | blend suitably according to a desired quality level. As an example of a multilayer structure, the recording material treatment liquid of the present invention is primed on a substrate, and a thermal layer is provided on the coating layer, or conversely, a thermal layer coating liquid is primed on the substrate, What provided the coating layer of the processing liquid for recording materials of this invention on the coating layer is mentioned.
また、本発明の被記録材の裏面に、カール防止、印刷適性付与、給排紙適性付与、帯電防止性付与等のための塗工層を設けることができる。さらに、裏面には、粘着、感熱、熱転写、インクジェット、磁性、難燃、耐熱、耐水、耐油、防滑等の性質を付与するための後加工を施すこともできる。 In addition, a coating layer for preventing curling, imparting printability, imparting paper supply / dischargeability, imparting antistatic property and the like can be provided on the back surface of the recording material of the present invention. Furthermore, the back surface can be subjected to post-processing for imparting properties such as adhesion, heat sensitivity, thermal transfer, ink jet, magnetism, flame retardancy, heat resistance, water resistance, oil resistance, and slip resistance.
以下に実施例および比較例を挙げて本発明をより具体的に説明するが、勿論本発明はこれらの実施例に限定されるものではない。また、実施例および比較例中の％および部数はそれぞれ質量％、質量部を示す。また、基材上への被記録材用処理液の塗布量は、処理液の質量を示す。 Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples. However, the present invention is not limited to these examples. Moreover,% and part in an Example and a comparative example show the mass% and the mass part, respectively. Moreover, the coating amount of the recording material treatment liquid on the substrate indicates the mass of the treatment liquid.
［実施例１］
濃度３０％のスチレン−（メタ）アクリル酸共重合体（アニオン性ポリマー、商品名：「Ｊｏｎｃｒｙｌ６９０」、ＢＡＳＦ社製）４８．７質量部、水６２．７質量部及びポリアクリル酸系分散剤１質量部に、濃度５０％のジシアンジアミド・ポリアルキレンポリアミン縮合物（非架橋性カチオン性ポリマー、商品名：「ＰＡＰ−１」、センカ社製）２９．２質量部と濃度２５％のポリアミドポリアミン−エピクロロヒドリン樹脂（架橋性カチオン性ポリマー、商品名：「ＷＳ４０２０」、星光ＰＭＣ社製）５８．４質量部を混合し、毎分３００回転で撹拌を行った。この時のＪｏｎｃｒｙｌ６９０とカチオン性ポリマーの比率は１：２（固形分）である。得られた水溶液をホモジナイザー（商品名：「ＴＷＩＮ ＰＡＮＤＡ ６００型」、Ｎｉｒｏ Ｓｏａｖｉ社製）を用いて圧力４００ｂａｒにて２回分散操作を行って、平均粒子径３μｍの本発明の有機複合粒子を含む被記録材用処理液を得た。
[Example 1]
30% styrene- (meth) acrylic acid copolymer (anionic polymer, trade name: “Joncry 690”, manufactured by BASF) 48.7 parts by mass, water 62.7 parts by mass and polyacrylic acid dispersant 1 Containing 50% concentration of dicyandiamide-polyalkylenepolyamine condensate (non-crosslinkable cationic polymer, trade name: “PAP-1”, manufactured by Senka) 29.2 parts by mass and 25% concentration of polyamide polyamine-epi 58.4 parts by mass of a chlorohydrin resin (crosslinkable cationic polymer, trade name: “WS4020”, manufactured by Seiko PMC Co., Ltd.) was mixed and stirred at 300 rpm. The ratio of Joncryl 690 to the cationic polymer at this time is 1: 2 (solid content). The obtained aqueous solution is dispersed twice using a homogenizer (trade name: “TWIN PANDA 600 type”, manufactured by Niro Soavi) at a pressure of 400 bar, and contains the organic composite particles of the present invention having an average particle diameter of 3 μm. A processing liquid for recording material was obtained.
被記録材の基材として、厚さ１００μｍのＰＥＴフィルム（商品名：「ルミラーＴ６０」、東レ社製）にアンカーコートとしてオキサゾリン基含有エマルジョン（商品名：「エポクロスＫ−２０２０Ｅ」、日本触媒社製）を塗工量が２ｇ／ｍ２となるようにバーコーターで塗工・乾燥し、基材シートを得た。 As a base material of the recording material, an oxazoline group-containing emulsion (trade name: “Epocross K-2020E”, manufactured by Nippon Shokubai Co., Ltd.) as an anchor coat on a 100 μm thick PET film (trade name: “Lumirror T60”, manufactured by Toray Industries, Inc.) ) Was coated and dried with a bar coater such that the coating amount was 2 g / m 2 to obtain a substrate sheet.
前記の基材シートに実施例１の被記録材用処理液をバーコーターにより１００ｇ／ｍ２塗工・乾燥し、実施例１の被記録材を得た。 The recording material for recording material of Example 1 was applied to the substrate sheet at 100 g / m 2 using a bar coater and dried to obtain the recording material of Example 1.
［実施例２］
実施例１においてアニオン性ポリマーとカチオン性ポリマーとの比率を１：３となるように配合量を変更した以外は、実施例１と同様にして本発明の有機複合粒子を含む被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例２の被記録材を得た。
[Example 2]
The processing for a recording material containing the organic composite particles of the present invention was carried out in the same manner as in Example 1 except that the blending amount was changed so that the ratio of the anionic polymer to the cationic polymer was 1: 3 in Example 1. A liquid was obtained.
A substrate sheet was prepared in the same manner as in Example 1, and the recording material for recording material was coated and dried to obtain the recording material of Example 2.
［実施例３］
実施例１においてアニオン性ポリマーとカチオン性ポリマーとの比率を１：６となるように配合量を変更した以外は、実施例１と同様にして本発明の有機複合粒子を含む被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例３の被記録材を得た。
[Example 3]
The processing for a recording material containing the organic composite particles of the present invention was carried out in the same manner as in Example 1 except that the blending amount was changed so that the ratio of the anionic polymer to the cationic polymer was 1: 6 in Example 1. A liquid was obtained.
A base sheet was prepared in the same manner as in Example 1, and a recording material treatment liquid was applied and dried to obtain a recording material of Example 3.
［実施例４］
実施例１においてアニオン性ポリマーとカチオン性ポリマーとの比率を２：１となるように配合量を変更した以外は、実施例１と同様にして本発明の有機複合粒子を含む被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例４の被記録材を得た。
[Example 4]
Treatment for recording material containing organic composite particles of the present invention in the same manner as in Example 1 except that the blending amount was changed so that the ratio of the anionic polymer to the cationic polymer was 2: 1 in Example 1. A liquid was obtained.
A base sheet was prepared in the same manner as in Example 1, and a recording material treatment liquid was applied and dried to obtain a recording material of Example 4.
［実施例５］
実施例１において、ホモジナイザー処理の条件を圧力２００ｂａｒにて１回分散処理に変更して、有機複合粒子の平均粒子径が１５μｍである被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例５の被記録材を得た。
[Example 5]
In Example 1, the condition of the homogenizer treatment was changed to a single dispersion treatment at a pressure of 200 bar to obtain a recording material treatment liquid in which the average particle diameter of the organic composite particles was 15 μm.
A base sheet was prepared in the same manner as in Example 1, and a recording material treatment liquid was applied and dried to obtain a recording material of Example 5.
［実施例６］
実施例１においてホモジナイザーの代わりにビーズミル（商品名：「ラボスター」、アシザワ・ファインテック社製）を用いて撹拌速度３００ｒｐｍで２時間分散操作を行った以外は実施例１と同様にして、平均粒子径０．５μｍの本発明の有機複合粒子を含む被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例６の被記録材を得た。
[Example 6]
The average particle size was the same as in Example 1 except that a dispersion operation was performed for 2 hours at a stirring speed of 300 rpm using a bead mill (trade name: “Labstar”, manufactured by Ashizawa Finetech) instead of the homogenizer in Example 1. A treatment liquid for recording material containing the organic composite particles of the present invention having a diameter of 0.5 μm was obtained.
A base sheet was prepared in the same manner as in Example 1, and the recording material treatment liquid was applied and dried to obtain a recording material of Example 6.
［実施例７］
実施例１において、非架橋性カチオン性ポリマーを、ポリアミンとしてジシアンジアミド・ポリアルキレンポリアミン縮合物からジメチルアミン・エピクロロヒドリン縮合物（商品名：「フィックスオイルＲ−７３７」、明成化学工業社製）に変更した以外は実施例１と同様にして平均粒子径３μｍの本発明の有機複合粒子を含む被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例７の被記録材を得た。
[Example 7]
In Example 1, a non-crosslinkable cationic polymer was converted from a dicyandiamide / polyalkylene polyamine condensate as a polyamine to a dimethylamine / epichlorohydrin condensate (trade name: “Fix Oil R-737”, manufactured by Meisei Chemical Co., Ltd.). A treatment liquid for recording material containing the organic composite particles of the present invention having an average particle diameter of 3 μm was obtained in the same manner as in Example 1 except that the above was changed.
A base sheet was prepared in the same manner as in Example 1, and a recording material treatment liquid was applied and dried to obtain a recording material of Example 7.
［実施例８］
実施例１において、アニオン性ポリマーについて、Ｊｏｎｃｒｙｌ６９０をＪｏｎｃｒｙｌ６７８（ＢＡＳＦ社製）に変更した以外は、実施例１と同様にして本発明の有機複合粒子を含む被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例８の被記録材を得た。
[Example 8]
In Example 1, a treatment liquid for recording material containing the organic composite particles of the present invention was obtained in the same manner as in Example 1 except that Joncryl 690 was changed to Joncryl 678 (manufactured by BASF) for the anionic polymer.
A base sheet was prepared in the same manner as in Example 1, and a recording material treatment liquid was applied and dried to obtain a recording material of Example 8.
［実施例９］
実施例１において、架橋性カチオン性ポリマーについて、ＷＳ４０２０をアラフィックス２５５（荒川化学工業社製）に変更した以外は、実施例１と同様にして本発明の有機複合粒子を含む被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例９の被記録材を得た。
[Example 9]
In Example 1, the processing for a recording material containing the organic composite particles of the present invention was performed in the same manner as in Example 1 except that WS4020 was changed to Araffix 255 (manufactured by Arakawa Chemical Industries) with respect to the crosslinkable cationic polymer. A liquid was obtained.
A base sheet was prepared in the same manner as in Example 1, and a recording material treatment liquid was applied and dried to obtain a recording material of Example 9.
［実施例１０］
実施例１において、ジシアンジアミド・ポリアルキレンポリアミン縮合物（非架橋性カチオン性ポリマー）を加えず、ポリアミドポリアミン−エピクロロヒドリン樹脂（架橋性カチオン性ポリマー、商品名：「ＷＳ４０２０」、星光ＰＭＣ社製）を１１６．８質量部とした以外は、実施例１と同様にして本発明の有機複合粒子を含む被記録材用処理液を得た。
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して実施例１０の被記録材を得た。
[Example 10]
In Example 1, a dicyandiamide-polyalkylene polyamine condensate (non-crosslinkable cationic polymer) was not added, and a polyamide polyamine-epichlorohydrin resin (crosslinkable cationic polymer, trade name: “WS4020”, manufactured by Seiko PMC Co., Ltd.) ) Was changed to 116.8 parts by mass in the same manner as in Example 1 to obtain a recording material treatment liquid containing the organic composite particles of the present invention.
A base sheet was prepared in the same manner as in Example 1, and the recording material treatment liquid was applied and dried to obtain the recording material of Example 10.
［実施例１１］
実施例１において、被記録材用処理液の塗工量を１５０ｇ／ｍ２に変更した以外は実施例１と同様にして被記録材を作成した。
[Example 11]
In Example 1, a recording material was prepared in the same manner as in Example 1 except that the coating amount of the recording material treatment liquid was changed to 150 g / m 2 .
［実施例１２］
実施例１において、被記録材用処理液の塗工量を５０ｇ／ｍ２に変更した以外は実施例１と同様にして被記録材を作成した。
[Example 12]
In Example 1, a recording material was prepared in the same manner as in Example 1 except that the coating amount of the recording material treatment liquid was changed to 50 g / m 2 .
［比較例１］
ポリアミン樹脂（商品名：「ＰＡＰ−２」）２０質量部、スチレン−アクリル酸共重合体（商品名：「ジョンクリル６１Ｊ」、ＢＡＳＦ社製）６７質量部、水１５０質量部、スチレン−無水マレイン酸エチレンオキサイド付加物５質量部、ポリビニルピロリドン５質量部を混合し、ビーズミル（商品名：「ラボスター」、アシザワ・ファインテック社製）を用いて撹拌速度３００ｒｐｍで２時間分散操作を行い、被記録材用処理液を得た。
[Comparative Example 1]
20 parts by weight of a polyamine resin (trade name: “PAP-2”), 67 parts by weight of a styrene-acrylic acid copolymer (trade name: “Johncrill 61J”, manufactured by BASF), 150 parts by weight of water, styrene-anhydrous maleic acid 5 parts by mass of an acid ethylene oxide adduct and 5 parts by mass of polyvinylpyrrolidone are mixed, and dispersed using a bead mill (trade name: “Labstar”, manufactured by Ashizawa Finetech Co., Ltd.) at a stirring speed of 300 rpm for 2 hours. A processing solution for the material was obtained.
実施例１と同様に基材シートを作成し、被記録材用処理液を塗工・乾燥して比較例１の被記録材を得た。 A substrate sheet was prepared in the same manner as in Example 1, and the recording material for recording material was coated and dried to obtain a recording material of Comparative Example 1.
［比較例２］
スチレン−アクリル酸共重合体であるアニオン性ポリマーとポリアミンであるカチオン性ポリマーとを作用させ、凝集体を形成させた後に、この凝集をほどくことによって得られた被記録材用処理液である、御国色素社製（商品名：「ＣＷ−６」）を用いた以外は比較例１と同様にして被記録材を作成した。
[Comparative Example 2]
A processing liquid for a recording material obtained by allowing an anionic polymer that is a styrene-acrylic acid copolymer and a cationic polymer that is a polyamine to act to form an aggregate and then unwinding the aggregate. A recording material was prepared in the same manner as in Comparative Example 1 except that Gokoku Dye Co., Ltd. (trade name: “CW-6”) was used.
［比較例３］
被記録材用処理液として御国色素社製（商品名：「ＣＷ−７２」）を用いた以外は比較例２と同様にして被記録材を作成した。
[Comparative Example 3]
A recording material was prepared in the same manner as in Comparative Example 2, except that Mikuni Dye Co., Ltd. (trade name: “CW-72”) was used as the processing material for the recording material.
＜測定・評価方法＞
［平均粒子径の測定方法］
上記の実施例及び比較例では、日機装社製の商品名：「マイクロトラックＭＴ３０００ＩＩ」を用いて水分散性微粒子の平均粒子径（メディアン径：ｄ５０）を測定した。
<Measurement and evaluation method>
[Measurement method of average particle size]
In the above Examples and Comparative Examples, the average particle diameter (median diameter: d50) of the water-dispersible fine particles was measured using a trade name “Microtrack MT3000II” manufactured by Nikkiso Co., Ltd.
上記の実施例、比較例で得られた被記録材について、被記録材のインク受容層の耐剥離性及び耐水性、及び、被記録材の表面のべたつきを下記の通りに評価した。 For the recording materials obtained in the above Examples and Comparative Examples, the peel resistance and water resistance of the ink receiving layer of the recording material and the stickiness of the surface of the recording material were evaluated as follows.
［耐剥離性］
被記録材に粘着テープを貼り付け、３０分後に剥離試験を行い、下記の基準で塗工層の耐剥離性を目視判定した。剥離試験は被記録材にセロファンテープ（登録商標 セロテープ（Ｒ）、ニチバン社製）を貼り付け、常温にて１８０度剥離で約５ｍｍ／ｓの速さでテープを剥がして行った。
○：まったく塗工層の剥離がなく、実用性に極めて優れる
△：若干塗工層の剥離があるが、実用上問題ないレベルである
×：塗工層の剥離がひどく、実用上問題となるレベルである
[Peeling resistance]
Adhesive tape was affixed to the recording material, a peel test was performed 30 minutes later, and the peel resistance of the coating layer was visually determined according to the following criteria. The peeling test was performed by attaching a cellophane tape (registered trademark Cello Tape (R), manufactured by Nichiban Co., Ltd.) to the recording material and peeling the tape at a speed of about 5 mm / s at 180 ° peeling at room temperature.
○: There is no peeling of the coating layer and it is extremely excellent in practicality. Δ: There is a slight peeling of the coating layer, but there is no practical problem. ×: The peeling of the coating layer is severe, causing a practical problem. Is level
［耐水性］
被記録材を水道水に６０分浸漬後、被記録材表面の塗工層の溶出、剥離を下記の基準で目視判定した。
○：まったく塗工層の溶出、剥離がなく、実用性に極めて優れる
△：若干塗工層の溶出、剥離があるが、実用上問題ないレベルである
×：塗工層の溶出、剥離がひどく、実用上問題となるレベルである
[water resistant]
After immersing the recording material in tap water for 60 minutes, elution and peeling of the coating layer on the surface of the recording material were visually determined according to the following criteria.
○: No elution or peeling of the coating layer at all, and extremely excellent practicality. Δ: Slight elution and peeling of the coating layer, but at a practically no problem level. X: Elution and peeling of the coating layer are severe. This is a practically problematic level
［べたつき］
被記録材の塗工層の表面を触り、べたつきを評価した。
○：まったく粘りを感じない
△：指先に若干粘りを感じる
×：指先に強く粘りを感じる
[Stickiness]
The surface of the coating layer of the recording material was touched to evaluate stickiness.
○: No stickiness at all △: Some stickiness at the fingertips ×: Strong stickiness at the fingertips
上記試験の結果を表１にまとめる。 The results of the above tests are summarized in Table 1.
表１に示されるとおり、実施例１〜１２の被記録材はいずれも、塗膜の耐剥離性、耐水性及び被記録材表面のべたつきについて極めて優れる、もしくは問題ないレベルであった。
一方、架橋性カチオン性ポリマーを含有しない比較例１は、塗膜の耐水性が不足し、表面のべたつきが生じた。比較例２及び比較例３の被記録材は、耐剥離性及び耐水性が十分ではなかった。
As shown in Table 1, all of the recording materials of Examples 1 to 12 were extremely excellent or no problem with respect to the peeling resistance of the coating film, water resistance, and stickiness of the surface of the recording material.
On the other hand, Comparative Example 1 containing no crosslinkable cationic polymer was insufficient in water resistance of the coating film, resulting in surface stickiness. The recording materials of Comparative Example 2 and Comparative Example 3 did not have sufficient peel resistance and water resistance.
上記の実施例及び比較例の被記録材について、インクジェット印刷適性（発色性、ニジミ、インク乾燥性、インク定着性、インク耐水性）を下記の通りに評価した。 The recording materials of the examples and comparative examples described above were evaluated for ink jet printing suitability (color development, bleeding, ink drying, ink fixability, and ink water resistance) as follows.
［発色性］
被記録材にインクジェットプリンター（商品名：「ＰＭ−７６０Ｃ」及び「ＰＸ−１００４」、エプソン社製）にてスーパーファイン用紙モードで印刷し、黒・シアン・マゼンタ・イエローのベタ印刷部の色濃度を日本電色社製の商品名「Ｓｐｅｃｔｒｏ Ｃｏｌｏｒ Ｍｅｔｅｒ ＳＥ ２０００」にて測定し、下記の基準で発色性を判定した。
○：色濃度の合計が５以上で、非常に発色性に優れている
△：色濃度の合計が４以上５未満で、実用上問題ない発色レベルである
×：色濃度が４未満で、発色性が悪く色再現性に劣る
[Color development]
Printed in super fine paper mode on an ink jet printer (trade names: “PM-760C” and “PX-1004”, manufactured by Epson Corporation) on the recording material, and the color density of the black / cyan / magenta / yellow solid printing part Was measured with a trade name “Spectro Color Meter SE 2000” manufactured by Nippon Denshoku Co., Ltd.
○: The total color density is 5 or more, and the color development is very good. Δ: The total color density is 4 or more and less than 5, and it is a practical color level. ×: The color density is less than 4 and the color is developed. Poor color reproducibility
［ニジミ］
被記録材にインクジェットプリンター（商品名：「ＰＭ−７６０Ｃ」及び「ＰＸ−１００４」、エプソン社製）にてスーパーファイン用紙モードで印刷し、下記の基準でニジミを目視判定した。
○：まったくニジミがなく、実用性に極めて優れる
△：若干ニジミがあるが、実用上問題ないレベルである
×：ニジミがひどく、実用上問題となるレベルである
[Nijimi]
Printing was performed on the recording material in a super fine paper mode using an inkjet printer (trade names: “PM-760C” and “PX-1004”, manufactured by Epson Corporation), and blurring was visually determined according to the following criteria.
○: There is no blurring at all, and it is extremely excellent in practical use. Δ: There is a slight blurring, but it is a level that is not a problem in practical use.
［インク乾燥性］
被記録材にインクジェットプリンター（商品名：「ＰＭ−７６０Ｃ」及び「ＰＸ−１００４」、エプソン社製）にてスーパーファイン用紙モードで印刷し、一定時間後にベタ印刷部に紙をあててインクが転写するか否かを観察し、下記の基準でインク乾燥性を目視判定した。
○：１０分以内でインクの転写がなくなったもの
△：３０分以内でインクの転写がなくなったもの
×：３０分以上経過してもインクが転写したもの
[Ink drying]
Print on the recording material in the super fine paper mode with an inkjet printer (trade names: “PM-760C” and “PX-1004”, manufactured by Epson Corporation), and transfer the ink by applying paper to the solid printing section after a certain period of time. The ink drying property was visually determined according to the following criteria.
○: No ink transfer within 10 minutes Δ: No ink transfer within 30 minutes ×: Ink transferred even after 30 minutes
［インク定着性］
被記録材にインクジェットプリンター（商品名：「ＰＭ−７６０Ｃ」及び「ＰＸ−１００４」、エプソン社製）にてスーパーファイン用紙モードで印刷し、ベタ印刷部に粘着テープを貼り付け、３０分後に剥離試験を行い、下記の基準でインク定着性を目視判定した。剥離試験は被記録材にセロファンテープ（登録商標 セロテープ（Ｒ）、ニチバン社製）を貼り付け、常温にて１８０度剥離で約５ｍｍ／ｓの速さでテープを剥がして行なった。
○：まったくインク剥離がなく、実用性に極めて優れる
△：若干インク剥離があるが、実用上問題ないレベルである
×：インク剥離がひどく、実用上問題となるレベルである
[Ink fixability]
Print on the recording material in the super fine paper mode with an inkjet printer (trade names: “PM-760C” and “PX-1004”, manufactured by Epson Corporation), attach the adhesive tape to the solid print section, and peel off after 30 minutes. A test was performed, and the ink fixability was visually determined according to the following criteria. The peel test was performed by attaching cellophane tape (registered trademark Cello Tape (R), manufactured by Nichiban Co., Ltd.) to the recording material, and peeling the tape at a speed of about 5 mm / s at 180 ° peeling at room temperature.
○: There is no ink peeling at all, and it is extremely excellent in practical use. Δ: There is some ink peeling, but it is a level that is not a problem for practical use.
［インク耐水性］
被記録材にインクジェットプリンター（商品名：「ＰＭ−７６０Ｃ」及び「ＰＸ−１００４」、エプソン社製）にてスーパーファイン用紙モードで印刷し、該印刷した試料を水道水に６０分浸漬後のインクの溶出、ニジミを下記の基準で目視判定した。
○：まったくインク溶出、ニジミがなく、実用性に極めて優れる
△：若干インク溶出、ニジミがあるが、実用上問題ないレベルである
×：インク溶出、ニジミがひどく、実用上問題となるレベルである
[Ink water resistance]
Ink after printing in super fine paper mode on an ink jet printer (trade names: “PM-760C” and “PX-1004”, manufactured by Epson Corporation) on the recording material, and immersing the printed sample in tap water for 60 minutes The elution and bleeding were visually determined according to the following criteria.
○: There is no ink elution or blurring, and it is extremely excellent in practical use. Δ: Slight ink elution and blurring are present, but there is no practical problem. ×: Ink elution and blurring are severe and practically problematic.
上記試験の結果を表２にまとめる。 The results of the above tests are summarized in Table 2.
表２に示されるとおり、実施例１〜１２の被記録材はいずれも、発色性、ニジミ、インク乾燥性、インク定着性、インク耐水性に極めて優れるか、問題のないレベルであった。
一方、架橋性カチオン性ポリマーを含まない比較例１はすべての評価項目が不十分であった。また、比較例２及び比較例３は、インク乾燥性、インク定着性、インク耐水性の点で不十分であった。
As shown in Table 2, all of the recording materials of Examples 1 to 12 were excellent in color developing property, bleeding, ink drying property, ink fixing property, and ink water resistance, or at a level with no problem.
On the other hand, in Comparative Example 1 which does not contain a crosslinkable cationic polymer, all evaluation items were insufficient. Further, Comparative Example 2 and Comparative Example 3 were insufficient in terms of ink drying property, ink fixing property, and ink water resistance.
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| CN116622265A (en) * | 2022-02-18 | 2023-08-22 | 精工爱普生株式会社 | Treatment liquid composition, inkjet ink composition, and set of treatment liquid compositions and treatment method |
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