JP2021050301A - インク及び印刷物の製造方法 - Google Patents
インク及び印刷物の製造方法 Download PDFInfo
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- JP2021050301A JP2021050301A JP2019175519A JP2019175519A JP2021050301A JP 2021050301 A JP2021050301 A JP 2021050301A JP 2019175519 A JP2019175519 A JP 2019175519A JP 2019175519 A JP2019175519 A JP 2019175519A JP 2021050301 A JP2021050301 A JP 2021050301A
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- 229920005792 styrene-acrylic resin Polymers 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- JOUDBUYBGJYFFP-FOCLMDBBSA-N thioindigo Chemical compound S\1C2=CC=CC=C2C(=O)C/1=C1/C(=O)C2=CC=CC=C2S1 JOUDBUYBGJYFFP-FOCLMDBBSA-N 0.000 description 1
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- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Images
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Abstract
Description
(i)顔料を顔料分散剤と共に、後述する分散方法で水等の水性媒体中に分散させる方法
(ii)顔料の表面に分散性付与基(親水性官能基および/またはその塩)を直接またはアルキル基、アルキルエーテル基またはアリール基等を介して間接的に結合させた自己分散型顔料を水等の水性媒体に分散および/または溶解させる方法が挙げられる。
前記顔料分散剤は、前記色材(D)として顔料を使用する場合に、好適に使用することができる。
(1)ポリマー(E)の酸価を予め、JIS試験方法K 0070−1992に基づく酸価測定方法により測定する。具体的には、テトラヒドロフランにポリマー(E)0.5gを溶解させ、フェノールフタレインを指示薬として、0.1M水酸化カリウムアルコール溶液で滴定し酸価を求める。
(2)水50mlに対して、ポリマー(E)を1g添加後、得られた酸価を100%中和するだけの0.1mol/L水酸化カリウム水溶液を加え、100%中和とする。
(3)100%中和させた液を、25℃の温度下で、2時間超音波洗浄器(株式会社エスエヌディ超音波洗浄器US−102、38kHz自励発振)中で超音波を照射させた後24時間室温で放置する。
ゲル・パーミエーション・クロマトグラフィー(GPC)法により、下記の条件で測定した。
測定装置:高速GPC装置(東ソー株式会社製「HLC−8220GPC」)
カラム:東ソー株式会社製の下記のカラムを直列に接続して使用した。
「TSKgel G4000」(7.8mmI.D.×30cm)×1本
「TSKgel G3000」(7.8mmI.D.×30cm)×1本
「TSKgel G2000」(7.8mmI.D.×30cm)×1本
検出器:RI(示差屈折計)
カラム温度:40℃
溶離液:テトラヒドロフラン
流速:1.0mL/分
注入量:100μL(試料濃度0.4質量%のテトラヒドロフラン溶液)
標準試料:下記の標準ポリスチレンを用いて検量線を作成した。
(標準ポリスチレン)
東ソー株式会社製「TSKgel 標準ポリスチレン A−500」
東ソー株式会社製「TSKgel 標準ポリスチレン A−1000」
東ソー株式会社製「TSKgel 標準ポリスチレン A−2500」
東ソー株式会社製「TSKgel 標準ポリスチレン A−5000」
東ソー株式会社製「TSKgel 標準ポリスチレン F−1」
東ソー株式会社製「TSKgel 標準ポリスチレン F−2」
東ソー株式会社製「TSKgel 標準ポリスチレン F−4」
東ソー株式会社製「TSKgel 標準ポリスチレン F−10」
東ソー株式会社製「TSKgel 標準ポリスチレン F−20」
東ソー株式会社製「TSKgel 標準ポリスチレン F−40」
東ソー株式会社製「TSKgel 標準ポリスチレン F−80」
東ソー株式会社製「TSKgel 標準ポリスチレン F−128」
東ソー株式会社製「TSKgel 標準ポリスチレン F−288」
東ソー株式会社製「TSKgel 標準ポリスチレン F−550」
芳香環または複素環を有するモノマーのポリマーブロックとは、具体的には、スチレン系モノマー等の芳香族環を有するモノマーや、ビニルピリジン系モノマー等の複素環を有するモノマーを単独重合または共重合して得たホモポリマーまたはコポリマーのポリマーブロックである。
前記ポリマーブロックA3におけるアニオン性基は、例えば、カルボキシル基、スルホン酸基または燐酸基等があげられる。なかでも、カルボキシル基がその調製やモノマー品種の豊富さ入手し易さから好ましい。また2つのカルボキシル基が分子内または分子間において脱水縮合した酸無水基となっていてもよい。
第一のモノマーと重合を開始させる重合開始剤とを、それぞれチューブリアクターP1及びP2(図1中7及び8)から、複数の液体を混合可能な流路を備えるT字型マイクロミキサーM1(図1中1)に導入し、T字型マイクロミキサーM1内で、第一のモノマーをリビングアニオン重合し第一の重合体を形成する(工程1)。
なお、このとき反応調整剤の種類や使用量により、前記一般式(3)におけるnの数をコントロールすることが可能である。
次に、反応調整剤を使用して成長末端の反応性を調整した後、前記アニオン性基に再生可能な保護基を有する(メタ)アクリレートを含むモノマーを前記第二のモノマーとして反応させポリマーブロックを得る。
前記ポリマーブロック(A2)とポリマーブロック(A3)のモル比A2:A3を、ポリマーブロック(A2)を構成する芳香環または複素環を有するモル数と、(A3)を構成するアニオン性基のモル数のモル比で表した場合は100:7.5〜100:400が好ましい。
本発明のインクは、前記色材(D)が顔料である場合、顔料を高濃度で含有する水性顔料分散体を製造し、前記水性顔料分散体と、前記溶媒(C)と、前記ポリウレタン(A)、ポリウレタン(B)、必要に応じてその他のバインダー樹脂や界面活性剤や添加剤とを混合することによって製造することができる。
(1)分散樹脂及び水を含有する混合物に、顔料を添加した後、攪拌分散装置を用いて顔料を前記混合物中に分散させることにより水性顔料分散体を調製する方法。
(2)顔料及び分散樹脂を2本ロールやミキサー等の混練機を用いて混練し、得られた混練物を、水、および必要に応じて水と混和する有機溶剤を添加し、攪拌分散装置を用いて水性顔料分散体を調製する方法。
(3)メチルエチルケトン、テトラヒドロフラン等のような水と相溶性を有する有機溶剤中に分散樹脂を溶解して得られた溶液に顔料を添加した後、攪拌分散装置を用いて顔料を有機溶液中に分散させ、次いで水等の水性媒体を用いて転相乳化させた後、前記有機溶剤を留去し水性顔料分散体を調製する方法。
BuLiのヘキサン溶液と、スチレンを予めテトラヒドロフランに溶解したスチレン溶液とを図1に示すチューブリアクターP1及びP2から、T字型マイクロミキサーM1に導入し、リビングアニオン重合させることによって重合体を得た。
(BuLi/スチレン/α−メチルスチレン/tert−ブチルメタクリレート)=1.0/12.0/1.3/8.1であった。
ゲル・パーミエーション・クロマトグラフィー(GPC)法により、下記の条件で測定した。
カラム:東ソー株式会社製の下記のカラムを直列に接続して使用した。
「TSKgel G4000」(7.8mmI.D.×30cm)×1本
「TSKgel G3000」(7.8mmI.D.×30cm)×1本
「TSKgel G2000」(7.8mmI.D.×30cm)×1本
検出器:RI(示差屈折計)
カラム温度:40℃
溶離液:テトラヒドロフラン(THF)
流速:1.0mL/分
注入量:100μL(試料濃度0.4質量%のTHF溶液)
標準試料:下記の標準ポリスチレンを用いて検量線を作成した。
東ソー株式会社製「TSKgel 標準ポリスチレン A−500」
東ソー株式会社製「TSKgel 標準ポリスチレン A−1000」
東ソー株式会社製「TSKgel 標準ポリスチレン A−2500」
東ソー株式会社製「TSKgel 標準ポリスチレン A−5000」
東ソー株式会社製「TSKgel 標準ポリスチレン F−1」
東ソー株式会社製「TSKgel 標準ポリスチレン F−2」
東ソー株式会社製「TSKgel 標準ポリスチレン F−4」
東ソー株式会社製「TSKgel 標準ポリスチレン F−10」
東ソー株式会社製「TSKgel 標準ポリスチレン F−20」
東ソー株式会社製「TSKgel 標準ポリスチレン F−40」
東ソー株式会社製「TSKgel 標準ポリスチレン F−80」
東ソー株式会社製「TSKgel 標準ポリスチレン F−128」
東ソー株式会社製「TSKgel 標準ポリスチレン F−288」
東ソー株式会社製「TSKgel 標準ポリスチレン F−550」
JIS試験方法K 0070−1992に準拠して測定した。THFに試料0.5gを溶解させ、フェノールフタレインを指示薬として、0.1M水酸化カリウムアルコール溶液で滴定することにより求めた。
顔料としてFastogen Blue SBG−SD(DIC株式会社製、C.I.PigmentBlue 15)を150質量部、前記分散樹脂(P−1)を30質量部、トリエチレングリコールを105質量部、34質量%水酸化カリウム水溶液12.8質量部を、1.0Lのインテンシブミキサー(日本アイリッヒ株式会社)に仕込み、ローター周速2.94m/s、パン周速1m/sで、60分間混練した。
温度計、窒素ガス導入管、攪拌器を備えた窒素置換された容器中で、1,6−ヘキサンジオールとメチルカーボネートとを反応して得られるポリカーボネートポリオール(数平均分子量2000)500質量部、2,2―ジメチロールプロピオン酸37.7質量部及びメチルエチルケトン 420質量部を加え、均一に混合した。次いで、イソホロンジイソシアネート140.8質量部を加えた後、ジブチル錫ジラウレート0.1質量部を加え、80℃で7時間反応させることによって、重量平均分子量が40000のポリウレタン(酸価35mgKOH/g)の有機溶剤溶液を得た。その後、50℃まで冷却し、トリエチルアミン29.8質量部及び水2069質量部を加え、減圧下、40℃〜60℃の温度下でメチルエチルケトンを除去し、水を加えて濃度調節を行うことによって、前記ポリウレタンが水性媒体中に分散された不揮発分23質量%のウレタン樹脂組成物PUD−A1を得た。
温度計、窒素ガス導入管、攪拌器を備えた窒素置換された容器中で、1,6−ヘキサンジオールとメチルカーボネートとを反応して得られるポリカーボネートポリオール(数平均分子量2000)500質量部、2,2―ジメチロールプロピオン酸36.5質量部及びメチルエチルケトン436質量部を加え、ジシクロヘキシルメタンジイソシアネートを183.5質量部使用し、80℃で3時間反応させることによって、分子末端にイソシアネート基を有するウレタンプレポリマーのメチルエチルケトン溶液を得た。上記で得られたウレタンプレポリマーのメチルエチルケトン溶液にトリエチルアミン41.3質量部を加え、前記ウレタンプレポリマー中のカルボキシル基を中和した後、水1504質量部を加えた。次いで、ヒドラジン5.2質量部を加えて反応させた。反応終了後、減圧下、40℃〜60℃の温度下でメチルエチルケトンを除去し、水を加えて濃度調節を行うことによって、前記ウレタン樹脂が水性媒体中に分散された不揮発分23質量%の重量平均分子量が150000で酸価23mgKOH/gのポリウレタンを含有するウレタン樹脂組成物PUD−A2を得た。
温度計、窒素ガス導入管、攪拌器を備えた窒素置換された容器中で、ポリオキシテトラメチレングリコール(数平均分子量1000)500質量部、2,2―ジメチロールプロピオン酸28.2質量部及びメチルエチルケトン436質量部を加え、イソホロンジイソシアネートを133.8質量部使用し、80℃で3時間反応させることによって、分子末端にイソシアネート基を有するウレタンプレポリマーのメチルエチルケトン溶液を得た。上記で得られたウレタンプレポリマーのメチルエチルケトン溶液に25%アンモニア水溶液14.3質量部を加え、前記ウレタンプレポリマー中のカルボキシル基を中和した後、水1504質量部を加えた。次いで、ヒドラジン1.1質量部を加えて反応させた。反応終了後、減圧下、40℃〜60℃の温度下でメチルエチルケトンを除去し、水を加えて濃度調節を行うことによって、前記ウレタン樹脂が水性媒体中に分散された不揮発分23質量%の重量平均分子量が39000で酸価7mgKOH/gのポリウレタンを含有するウレタン樹脂組成物PUD−B1を得た。
温度計、窒素ガス導入管、攪拌器を備えた窒素置換された容器中で、ポリオキシテトラメチレングリコール(数平均分子量2000)500質量部、2,2―ジメチロールプロピオン酸122.7質量部及びメチルエチルケトン420質量部を加え、均一に混合した。次いで、イソホロンジイソシアネート280.0質量部を加えた後、ジブチル錫ジラウレート0.1質量部を加え、80℃で7時間反応させることによって、重量平均分子量が38000のポリウレタン(酸価55mgKOH/g)の有機溶剤溶液を得た。その後、50℃まで冷却し、40質量%水酸化カリウム水溶液122.9質量部及び水2069質量部を加え、減圧下、40℃〜60℃の温度下でメチルエチルケトンを除去し、水を加えて濃度調節を行うことによって、前記ポリウレタンが水性媒体中に分散された不揮発分23質量%のウレタン樹脂組成物PUD−B2を得た。
前記水性顔料分散体(1)29.3質量部、ポリウレタン(A)としてウレタン樹脂組成物PUD−A1(不揮発分23質量%)18.3 質量部、ポリウレタン(B)としてウレタン樹脂組成物PUD−B1(不揮発分23質量%)12.2質量部、サーフィノール440(EVONIK製、アセチレン系界面活性剤)1質量部、グリセリンを25.0質量部、プロピレングリコールを5.0質量部、防腐剤としてACTICIDE B−20(ソー・ジャパン(株)製)0.05質量部、イオン交換水9.15質量部を混合することによって水性インクを得た。前記水性インクの25℃での粘度は10mPa・s、表面張力は33mN/mであった。
測定装置:TVE−25形粘度計(社製、TVE−25 L)
校正用標準液:JS20
測定温度:25℃
回転速度:10〜100rpm
注入量:1200μL
インクの静的表面張力は、ウィルへルミ法を適用した自動表面張力計を用い、下記条件にて測定した。
測定装置:自動表面張力計(協和界面科学(株)社製、CBVP−Z型)
測定温度:25℃
測定子:白金プレート
水性インクの配合を下記表1及び2に変更したこと以外は、実施例1と同様の方法で水性インクを調整し、印刷物を得た。
前記循環ろ過特性は、孔径12μmのSUS製のメッシュフィルター(真鍋工業株式会社製)を備えた循環経路を有する循環装置内で、実施例及び比較例で得られた水性インク200gを循環させることによって評価した。前記循環開始直後の水性インクの流速は50g/minに調整した。
B:循環開始から120時間以上168時間未満
C:循環開始から72時間以上120時間未満
D:循環開始から24時間以上72時間未満
E:循環開始から24時間未満
前記方法で得られた印刷物の洗濯堅牢性を、JIS L 0844:2005のA−2法に準拠して、試験を行った後、JIS L 0801:2004の変退色用グレースケールを用いた視感法の判定基準にしたがって、1級〜5級で等級を判定した。なお、等級は、1級が最も退色が大きく、5級に近づくほど退色が少ないことを指す。
・△:3級以上4級未満
・×:3級未満
製造直後の水性インクの粘度V0を、上記した方法で測定した。次に、前記水性インク20mLをガラス容器に密閉し、60℃の環境下に4週間静置した後、上記と同様の方法で粘度V1を測定した。前記測定結果と、式[(V1−V0)/V0]×100に基づいて粘度の変化率を算出し、下記基準に基づいて評価した。
・△:粘度の変化率が±5%以上±10%未満
・×:粘度の変化率が±10%以上
水性インク1mLをSUS基板上に塗布し、40℃のホットプレート上で5分間加熱することによって印刷物を得た。前記印刷物を20mLの純水に浸漬し、1分経過後、前記印刷物の印刷面を目視で観察し、下記基準で評価した。
△:薄い着色膜が残る
×:濃い着色膜が残る
2:T字型マイクロミキサーM2
3:T字型マイクロミキサーM3
4:チューブリアクターR1
5:チューブリアクターR2
6:チューブリアクターR3
7:プレクーリングの為のチューブリアクターP1
8:プレクーリングの為のチューブリアクターP2
9:プレクーリングの為のチューブリアクターP3
10:プレクーリングの為のチューブリアクターP4
Claims (9)
- インク循環型インクジェットヘッドを備えた印刷装置に使用するインクであって、前記インクが、カーボネート構造を有するポリウレタン(A)とエーテル構造を有するポリウレタン(B)と溶媒(C)とを含有することを特徴とするインク。
- 前記ポリウレタン(A)と前記ポリウレタン(B)との質量割合[前記ポリウレタン(A)/前記ポリウレタン(B)]が1.5〜9の範囲である請求項1に記載のインク。
- 前記ポリウレタン(A)の重量平均分子量が10000〜200000の範囲であり、かつ、前記ポリウレタン(B)の重量平均分子量が10000〜50000の範囲である請求項1または2に記載のインク。
- 前記ポリウレタン(A)が、ウレア結合を有さない重量平均分子量10000〜50000のポリウレタン、または、ウレア結合を有する重量平均分子量70000〜170000のポリウレタンである請求項1〜3のいずれか1項に記載のインク。
- 前記インク循環型インクジェットヘッドがその循環経路内に孔径5μm〜20μmの範囲のフィルターを備えたものである請求項1〜4のいずれか1項に記載のインク。
- 前記インクの全量に対する、前記ポリウレタン(A)及び前記ポリウレタン(B)の合計質量の割合が5質量%〜15質量%の範囲である請求項1〜5のいずれか1項に記載のインク。
- 布帛への印刷に使用する請求項1〜6のいずれか1項に記載のインク。
- インク循環型インクジェットヘッドを備えた印刷装置を用い、請求項7に記載のインクを布帛に印刷することによって印刷物を得る印刷工程を備え、前記印刷工程において、前記インク循環型インクジェットヘッドのインク吐出口と前記布帛との最短距離が2mm以上であり、前記インク循環型インクジェットヘッドから吐出されるインク液滴1個のサイズが10〜50plの範囲であることを特徴とする印刷物の製造方法。
- インク循環型インクジェットヘッドが、インク吐出ノズルと、インクの流入経路とインクの流出経路とを有し、前記流出経路から流出されたインクが、前記流入経路を経てインクジェットヘッドに供給される構造を有するものである請求項8に記載の印刷物の製造方法。
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