JP2008214385A - 着色塗料粒子分散物の製造方法 - Google Patents
着色塗料粒子分散物の製造方法 Download PDFInfo
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- JP2008214385A JP2008214385A JP2007049725A JP2007049725A JP2008214385A JP 2008214385 A JP2008214385 A JP 2008214385A JP 2007049725 A JP2007049725 A JP 2007049725A JP 2007049725 A JP2007049725 A JP 2007049725A JP 2008214385 A JP2008214385 A JP 2008214385A
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- XDSGMUJLZDSCPA-UHFFFAOYSA-N diazanium;phenoxybenzene;sulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=O.C=1C=CC=CC=1OC1=CC=CC=C1 XDSGMUJLZDSCPA-UHFFFAOYSA-N 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
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- 230000004069 differentiation Effects 0.000 description 1
- 125000005442 diisocyanate group Chemical group 0.000 description 1
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [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])* 0.000 description 1
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- 239000011733 molybdenum Substances 0.000 description 1
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- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- CRVVHBFLWWQMPT-UHFFFAOYSA-N naphthalene-1-sulfonic acid;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 CRVVHBFLWWQMPT-UHFFFAOYSA-N 0.000 description 1
- 150000002791 naphthoquinones Chemical class 0.000 description 1
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229940096992 potassium oleate Drugs 0.000 description 1
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 description 1
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- 235000010413 sodium alginate Nutrition 0.000 description 1
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Landscapes
- Paints Or Removers (AREA)
Abstract
水性多彩模様塗料に適用可能な着色塗料粒子分散物を工業的に安定に生産するのに適する製造方法を提供する。
【解決手段】
水性樹脂組成物(A)と水性着色塗料組成物(B)とを接触させることにより着色塗料粒子が水性媒体中に分散されてなる着色塗料粒子分散物(I)を製造する製造方法であって、該水性樹脂組成物(A)が、水性樹脂(a1)、金属化合物(a2)及び水を含み、水性樹脂(a1)の酸価が2〜20mgKOH/gの範囲内にあることを特徴とする着色塗料粒子分散物(I)の製造方法。
【選択図】なし
Description
即ち本発明は、
1. 水性樹脂組成物(A)と水性着色塗料組成物(B)とを接触させることにより着色塗料粒子が水性媒体中に分散されてなる着色塗料粒子分散物(I)を製造する製造方法であって、該水性樹脂組成物(A)が、水性樹脂(a1)、金属化合物(a2)及び水を含み、水性樹脂(a1)の酸価が2〜20mgKOH/gの範囲内にあることを特徴とする着色塗料粒子分散物(I)の製造方法、
2. 水性樹脂(a1)が、塩化カルシウムによる凝集率が3.0%以下にある1項に記載の製造方法、
3. 水性樹脂(a1)が、マロン式機械安定性試験機による凝集率が3.0%以下にある1項または2項に記載の製造方法、
4. 水性樹脂組成物(A)と水性着色塗料組成物(B)が、それぞれ、互いに反応し得る官能基(x)及び(y)を含有する1項ないし3項のいずれか1項に記載の製造方法、
5. 金属化合物(a2)が、その成分の一部として金属水酸化物及び/又は有機酸金属塩を含む1項ないし4項のいずれか1項に記載の製造方法、
6.水性樹脂組成物(A)が、ポリオキシアルキレン単位を有する化合物を含むことを特徴とする1項ないし5項のいずれか1項に記載の製造方法、
7. 水性樹脂組成物(A)が、体質顔料をさらに含む1項ないし6項のいずれか1項に記載の製造方法、
8. 水性樹脂組成物(A)が、固形分が20〜70%の範囲内にある1項ないし7項のいずれか1項に記載の製造方法、
9. 水性着色塗料組成物(B)が、水性樹脂(b1)、着色剤(b2)及び水溶性多糖類(b3)を含む1項ないし8項のいずれか1項に記載の製造方法、
10.水性着色塗料組成物(B)が、ポリオキシアルキレン単位を有する化合物を含むことを特徴とする1項ないし9項のいずれか1項に記載の製造方法、
11. 1種の水性樹脂組成物(A)に対して、色調が互いに異なる2種以上の水性着色塗料組成物(B)を順次接触させることを特徴とする1項ないし10項のいずれか1項に記載の製造方法、
12. 水性樹脂組成物(A)中の金属化合物(a2)の量が、水性着色塗料組成物(B)中の水溶性多糖類(b3)のカルボキシル基に由来する基1molに対して0.2〜3molの範囲内にある9項ないし11項のいずれか1項に記載の製造方法、
13. 1項ないし12項のいずれか1項に記載の製造方法により得られる着色塗料粒子分散物(I)を用いることを特徴とする水性多彩模様塗料の製造方法、
14. 1項ないし12項のいずれか1項に記載の製造方法により得られる着色塗料粒子分散物(I)に、塗膜形成成分(II)をさらに加えてなる水性多彩模様塗料の製造方法、
15. 着色塗料粒子分散物(I)と塗膜形成成分(II)が、それぞれ、互いに反応し得る官能基(m)及び(n)を含有する14項に記載の水性多彩模様塗料の製造方法、
に関する。
本発明の製造方法において使用される水性樹脂(a1)は、酸価が2〜20mgKOH/gの範囲内にあることを特徴とする。水性樹脂(a1)の酸価が2mgKOH/g未満では、着色塗料粒子分散物(I)の製造安定性が悪くなり、一方20mgKOH/gを超えると、水性樹脂組成物(A)と接触した際における水性着色塗料組成物(B)の粒状化がしにくくなり好ましくない。本発明において上記水性樹脂(a1)の好ましい酸価としては、2〜20mgKOH/g、特に2〜16mgKOH/gの範囲内を挙げることができる。
本発明の製造方法において、水性着色塗料組成物(B)を粒状化せしめる際に用いられる金属イオンの供給源となる金属化合物(a2)における金属種としては、着色塗料粒子の強度などの観点から、多価金属、特に二価金属が好適であり、二価金属としては、例えば、マグネシウム、カルシウム、ストロンチウム、バリウム等の周期表2族元素;クロム、モリブデン等の周期表6族元素;マンガン等の周期表7族元素;鉄、ルテニウム等の周期表8族元素;コバルト、ロジウム等の周期表9族元素;ニッケル、パラジウム等の周期表10族元素;銅等の周期表11族元素;亜鉛、カドミウム等の周期表12族元素などを挙げることができ、中でも、周期表2属元素、特にカルシウムが好適である。
本発明の製造方法において、水性樹脂組成物(A)の貯蔵安定性を良好なものとさせ、且つ着色塗料粒子分散物(I)の製造安定性、貯蔵安定性を良好なものとさせるために水性樹脂組成物(A)が、ポリオキシアルキレン単位を有する化合物を含有することが望ましい。
本発明の製造方法において、水性着色塗料組成物(B)は、粒状化されることによって着色塗料粒子となりうる組成物であり、着色剤を含む水性塗料組成物であって、従来公知のものを制限なく使用することができ、固形分が20〜60%、特に25〜50%のものを使用することが適している。
本発明の製造方法においては金属化合物(a2)由来の金属イオンを含有する上記水性樹脂組成物(A)と、水性着色塗料組成物(B)とを接触させることにより着色塗料粒子が形成され、該粒子が分散されてなる着色塗料粒子分散物(I)を製造することができる。この接触は、例えば、注射器の先端から水性着色塗料組成物(B)を水性樹脂組成物(A)中に滴下する方法;水性着色塗料組成物(B)を遠心力を利用して飛散させ、水性樹脂組成物(A)中に滴下する方法;スプレーノズルの先端から水性着色塗料組成物(B)を霧化させ、水性樹脂組成物(A)中に滴下する方法;水性着色塗料組成物(B)を水性樹脂組成物(A)中に加え、分散機で攪拌混合する方法などの方法により行うことができる。
以上に述べた本発明の製造方法によれば、製造途中の各段階における中間原料の貯蔵安定性が良好でありながら着色塗料粒子を安定に製造でき、しかも最終的に得られる着色塗料粒子分散物(I)中における着色塗料粒子の貯蔵安定性が良好となり得る。
製造例1
容量2リットルの4つ口フラスコに、脱イオン水285部及び「ニューコール707SF」(注1)1部加え、窒素置換後、85℃に保った。その中に下記の組成の成分をエマルション化してなるプレエマルションの3%分と、過硫酸アンモニウム3部を脱イオン水120部に溶解させた開始剤水溶液123部のうちの41部とそれぞれ添加し、添加20分後から、残りのプレエマルションと過硫酸アンモニウム水溶液とを4時間かけてフラスコに滴下した。
脱イオン水 368部
スチレン 150部
メチルメタクリレート 375部
n−ブチルアクリレート 240部
2−エチルヘキシルアクリレート 155部
ダイアセトンアクリルアミド 20部
2−ヒドロキシエチルアクリレート 40部
アクリル酸 20部
「ニューコール707SF」(注1) 66部
滴下後、これをさらに2時間85℃に保持した後、40〜60℃に降温した。次いで、アンモニア水でpHを調整し、固形分が55%のエマルション(a1)を得た。エマルション(a1)の固形分酸価は15mgKOH/g、平均粒子径は180nm、pHは8.3であり、塩化カルシウムによる凝集率は0.1%、マロン式機械安定性試験機による凝集率は0.2%であった。
(注1) 「ニューコール707SF」:商品名、日本乳化剤社製、ポリオキシエチレン鎖を有するアニオン性界面活性剤、不揮発分30%。
上記製造例1におけるプレエマルションの代わりに下記組成の成分をエマルション化してなるプレエマルションを用いる以外は製造例1と同様にして、固形分が55%のエマルション(a2)を得た。エマルション(a2)の固形分酸価は1mgKOH/g、平均粒子径は245nm、pHは8.2であり、塩化カルシウムによる凝集率は18%、マロン式機械安定性試験機による凝集率は10%であった。
脱イオン水 368部
スチレン 150部
メチルメタクリレート 430部
n−ブチルアクリレート 259部
2−エチルヘキシルアクリレート 150部
2−ヒドロキシエチルアクリレート 10部
アクリル酸 1部
「ニューコール707SF」(注1) 66部。
製造例3〜8
500ミリリットルのステンレス容器に、下記表1に示す成分を順次攪拌しながら仕込み、その後、均一になるまで攪拌することにより、水性樹脂組成物(A−1)〜(A−6)を得た。
(注3)「TEXANOL」:商品名、イーストマンケミカル社製、2,2,4−トリメチル−1,3−ペンタンジオールモノイソブチレート、造膜助剤、
(注4)「SNデフォーマー380」:商品名、サンノプコ社製、消泡剤、
(注5)「アデカノールUH−438」:商品名、アデカ社製、増粘剤。
製造例9
1リットルのステンレス容器に下記の成分を仕込み、攪拌機にて30分間攪拌混合することにより、白顔料ペースト(b1)を得た。
水 225部
「スラオフ72N」(注6) 15部
「DISPER BYK−190」(注7) 30部
「SNデフォーマー380」(注4) 15部
「TITANIX JR−605」(注8) 500部
(注6)「スラオフ72N」:商品名、武田薬品工業(株)製、防腐剤、
(注7)「DISPER BYK−190」:商品名、BYKケミー社製、スチレンマレイン酸共重合体のポリオキシエチレン変性物、顔料分散剤、
(注8)「TITANIX JR−605」:商品名、テイカ社製、チタン白。
製造例10
1リットルのステンレス容器に下記の成分を仕込み、攪拌機にて60分間攪拌混合することにより、赤錆顔料ペースト(b2)を得た。
水 400部
「スラオフ72N」(注6) 15部
「DISPER BYK−190」(注7) 48部
「SNデフォーマー380」(注4) 15部
酸化鉄 240部。
製造例11
容器に下記の成分を順次配合し、均一となるように攪拌混合して、着色塗料粒子用水性着色塗料組成物(B−1)を得た。
55%エマルション(a1) 175部
白顔料ペースト(b1) 50部
10%アジピン酸ジヒドラジド水溶液 2部
「TEXANOL」(注3) 11部
「SNデフォーマー380」(注4) 1部
「アデカノールUH−438」(注5) 1部
2%アルギン酸ナトリウム水溶液 105部。
上記製造例11における白顔料ペースト(b1)の代わりに赤錆顔料ペースト(b2)を用いる以外は製造例11と同様にして、着色塗料粒子用水性着色塗料組成物(B−2)を得た。
実施例1
1リットルステンレス容器に、上記製造例3で得られた水性樹脂組成物(A−1)を280部仕込み、50mmの径を有する攪拌羽根を用いて回転数1500rpmで攪拌しながら、上記製造例11で得られた水性着色塗料組成物(B−1)345部を徐々に容器内に滴下し、着色塗料粒子を生成させ、ついで容器内液を同回転速度でさらに15分攪拌し、着色塗料粒子分散物(C−1)を得た。
上記実施例1において、水性樹脂組成物と滴下する水性着色塗料組成物の配合を表2の通りとする以外は上記実施例1と同様にして着色塗料粒子分散物(C−2)〜(C−3)を製造した。
実施例4
1リットルステンレス容器に、上記製造例3で得られた水性樹脂組成物(A−1)を280部仕込み、50mmの径を有する攪拌羽根を用いて回転数1500rpmで攪拌しながら、上記製造例11で得られた水性着色塗料組成物(B−1)245部を徐々に容器内に滴下し、白色塗料粒子を生成させた後、製造例12で得られた水性着色塗料組成物(B−2)100部を徐々に容器内に滴下し、赤錆色塗料粒子を生成させた後、容器内液を同回転速度でさらに15分攪拌し、白色塗料粒子と赤錆色塗料粒子が分散されてなる着色塗料粒子分散物(C−4)を得た。
上記実施例4において、水性樹脂組成物と滴下する水性着色塗料組成物を表2の通りとする以外は上記実施例4と同様にして着色塗料粒子分散物(C−5)〜(C−10)を製造した。
攪拌中の容器の中を目視にて観察し、次の基準で評価した。
○:着色塗料粒子が崩壊することなく容易に製造でき、容器壁面に凝集物の付着がない、
○△:着色塗料粒子が崩壊することなく容易に製造でき、容器壁面に凝集物の付着が若干あるが実用レベル、
△:着色塗料粒子の崩壊が一部認められる、または容器壁面に凝集物の付着が認められる、
×:容器内液全体が凝集し、攪拌できない。
実施例10〜18および比較例2
1リットルのステンレス容器に、下記表3に示す成分を順次攪拌しながら仕込み、その後、均一になるまで攪拌することにより、水性多彩模様塗料(D−1)〜(D−10)を得た。得られた塗料の塗膜性能評価も併せて表3に示す。
2リットルのステレンス容器に下記の成分を仕込み、攪拌機にて30分間攪拌混合することにより、水性クリヤー塗料(c1)を得た。
55%エマルション(a1) 750部
「TEXANOL」(注3) 50部
水 279部
「タルク SS」(注2) 250部
「SNデフォーマー380」(注4) 10部
「アデカノールUH−438」(注5) 6部。
スレート板(150×70×3mm)上に、「EPシーラー透明」(関西ペイント社製、水系アクリルエマルション系シーラー)を塗布量が100g/m2になるようにローラー塗装し乾燥させた後、「ビニデラックス300」(関西ペイント社製、JIS K5663 1種適合アクリルエマルション系塗料)を塗布量が100g/m2になるようにローラー塗装し、気温20℃、相対湿度60%の条件下で1日間乾燥させたものを被塗板とし、この上に各多彩模様塗料を塗布量が300g/m2になるようにスプレーで塗装した。その後、気温23℃、相対湿度60%の条件下で7日間乾燥して、各試験板を得、各試験塗板を下記性能試験に供した。
(*2)肉持ち感
各試験塗板の塗膜を目視で観察し、次の基準で評価した。
○:肉持ち感が十分にある、
○△:肉持ち感がややある、
△: 肉持ち感がやや乏しい、
×:肉持ち感が乏しい。
(*3)耐水性
各試験塗板を23℃の上水に2日間浸漬し、引き上げた後、目視にて観察し、次の基準で評価した。
○:良好、
○△:艶引けが若干認められる、
△:艶引け、白化、フクレが認められる、
×:著しいフクレが認められる、又は塗膜が軟化する。
Claims (15)
- 水性樹脂組成物(A)と水性着色塗料組成物(B)とを接触させることにより着色塗料粒子が水性媒体中に分散されてなる着色塗料粒子分散物(I)を製造する製造方法であって、該水性樹脂組成物(A)が、水性樹脂(a1)、金属化合物(a2)及び水を含み、水性樹脂(a1)の酸価が2〜20mgKOH/gの範囲内にあることを特徴とする着色塗料粒子分散物(I)の製造方法。
- 水性樹脂(a1)が、塩化カルシウムによる凝集率が3.0%以下にある請求項1に記載の製造方法。
- 水性樹脂(a1)が、マロン式機械安定性試験機による凝集率が3.0%以下にある請求項1または2に記載の製造方法。
- 水性樹脂組成物(A)と水性着色塗料組成物(B)が、それぞれ、互いに反応し得る官能基(x)及び(y)を含有する請求項1ないし3のいずれか1項に記載の製造方法。
- 金属化合物(a2)が、その成分の一部として金属水酸化物及び/又は有機酸金属塩を含む請求項1ないし4のいずれか1項に記載の製造方法。
- 水性樹脂組成物(A)が、ポリオキシアルキレン単位を有する化合物を含むことを特徴とする請求項1ないし5のいずれか1項に記載の製造方法。
- 水性樹脂組成物(A)が、体質顔料をさらに含む請求項1ないし6のいずれか1項に記載の製造方法。
- 水性樹脂組成物(A)が、固形分が20〜70%の範囲内にある請求項1ないし7のいずれか1項に記載の製造方法。
- 水性着色塗料組成物(B)が、水性樹脂(b1)、着色剤(b2)及び水溶性多糖類(b3)を含む請求項1ないし8のいずれか1項に記載の製造方法。
- 水性着色塗料組成物(B)が、ポリオキシアルキレン単位を有する化合物を含むことを特徴とする請求項1ないし9のいずれか1項に記載の製造方法。
- 1種の水性樹脂組成物(A)に対して、色調が互いに異なる2種以上の水性着色塗料組成物(B)を順次接触させることを特徴とする請求項1ないし10のいずれか1項に記載の製造方法。
- 水性樹脂組成物(A)中の金属化合物(a2)の量が、水性着色塗料組成物(B)中の水溶性多糖類(b3)のカルボキシル基に由来する基1molに対して0.2〜3molの範囲内にある請求項9ないし11のいずれか1項に記載の製造方法。
- 請求項1ないし12のいずれか1項に記載の製造方法により得られる着色塗料粒子分散物(I)を用いることを特徴とする水性多彩模様塗料の製造方法。
- 請求項1ないし12のいずれか1項に記載の製造方法により得られる着色塗料粒子分散物(I)に、塗膜形成成分(II)をさらに加えてなる水性多彩模様塗料の製造方法。
- 着色塗料粒子分散物(I)と塗膜形成成分(II)が、それぞれ、互いに反応し得る官能基(m)及び(n)を含有する請求項14に記載の水性多彩模様塗料の製造方法。
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US11505658B2 (en) | 2017-03-03 | 2022-11-22 | Harland Medical Systems, Inc. | Coating composition comprised of a hydrophilic crosslinker, a hydrophobic crosslinker and optionally a hydrogel and methods of making and using the same |
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