JP2008063373A - 床用水性塗料および床塗工方法 - Google Patents
床用水性塗料および床塗工方法 Download PDFInfo
- Publication number
- JP2008063373A JP2008063373A JP2006240119A JP2006240119A JP2008063373A JP 2008063373 A JP2008063373 A JP 2008063373A JP 2006240119 A JP2006240119 A JP 2006240119A JP 2006240119 A JP2006240119 A JP 2006240119A JP 2008063373 A JP2008063373 A JP 2008063373A
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- Prior art keywords
- acrylic resin
- floor
- water
- paint
- group
- 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.)
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Abstract
【解決手段】ポリイソシアネート(A)と、少なくとも60モル%が2級水酸基となるモル比で1級水酸基と2級水酸基を有し、水酸基価が50〜120mgKOH/gで、かつ1級水酸基に基づく水酸基価が20〜40mgKOH/gのアクリル系樹脂(B)と、重量平均分子量350,000以上で、水酸基価0〜15mgKOH/gのアクリル系樹脂(C)が水性媒体中に分散してなる床用水性塗料、および、この床用水性塗料を、旧塗膜やプライマーを有していてもよい床材の上に塗工し、乾燥させた後、その上にさらに前記床用水性塗料を塗工し、乾燥させることを特徴とする床塗工方法。
【選択図】なし
Description
はじめに、本発明で使用するポリイソシアネート(A)について説明する。本発明に使用するポリイソシアネート(A)としては、各種のポリイソシアネートを用いることができる。かかるポリイソシアネート(A)の代表的なものとしては、1,4−テトラメチレンジイソシアネート、エチル(2,6−ジイソシアナート)ヘキサノエート、1,6−ヘキサメチレンジイソシアネート、1,12−ドデカメチレンジイソシアネート、2,2,4−または2,4,4−トリメチルヘキサメチレンジイソシアネート等の脂肪族ジイソシアネート;1,3,6−ヘキサメチレントリイソシアネート、1,8−ジイソシアナート−4−イソシアナートメチルオクタン、2−イソシアナートエチル(2,6−ジイソシアナート)ヘキサノエート等の脂肪族トリイソシアネート;1,3−または1,4−ビス(イソシアナートメチルシクロヘキサン)、1,3−または1,4−ジイソシアナートシクロヘキサン、3,5,5−トリメチル(3−イソシアナートメチル)シクロヘキシルイソシアネート、ジシクロヘキシルメタン−4,4’−ジイソシアネート、2,5−または2,6−ジイソシアナートメチルノルボルナン等の脂環式ジイソシアネート;2,5−または2,6−ジイソシアナートメチル−2−イソシネートプロピルノルボルナン等の脂環式トリイソシアネート;m−キシリレンジイソシアネート、α,α,α′α′−テトラメチル−m−キシリレンジイソシアネート等のアラルキレンジイソシアネート;
本発明で使用するアクリル系樹脂(B)は、水酸基価が50〜120mgKOH/gであることが必要である。水酸基価が50より低いと十分な耐水性が得られず、120より高いと親水性基である水酸基が耐水性を低下させる。塗膜の初期硬度、耐水性に優れる床用水性塗料が得られることから、水酸基価の範囲は60〜100mgKOH/gであることが好ましく、65〜90mgKOH/gであることがより好ましい。
下記のFoxの式で計算した絶対温度(K)表示のガラス転移温度(TgK)を摂氏温度(℃)に換算した数値を、本発明におけるガラス転移温度(Tg)とする。
100/TgK=W1/Tg1+W2/Tg2+W3/Tg3+W4/Tg4・・・
・式中、W1、W2、W3、W4・・・は各種成分の質量分率(質量%)を示す。
・式中、Tg1、Tg2、Tg3、Tg4・・・は各モノマー成分のホモポリマーの絶対温度(K)表示のガラス転移温度を示す。ここで、上記各モノマー成分のホモポリマーの絶対温度(K)表示のガラス転移温度(Tg1、Tg2、Tg3、Tg4・・・)は、Polymer Handbook(Second Edition、J,Brandrup・E,H,Immergut編)に記載の値を使用した。
=W/ΣNi=Σ(Mi×Ni)/ΣNi=ΣHi/Σ(Hi/Mi)
重量平均分子量(Mw)
=Σ(Wi×Mi)/W=Σ(Hi×Mi)/ΣHi
式中、W :高分子の総重量
Wi:i番目の高分子の重量
Mi:i番目の溶出時間における分子量
Ni:分子量Miの個数
Hi:i番目の溶出時間における高さ
である。
測定装置
装置 :東ソー(株)製 HLC−8120GPC
使用カラム:東ソー(株)製 TSKgel G2000HXL(カラム1)
東ソー(株)製 TSKgel G3000HXL(カラム2)
東ソー(株)製 TSKgel G4000HXL(カラム3)
東ソー(株)製 TSKgel G5000HXL(カラム4)
東ソー(株)製 TSKgel GMHXL(カラム5)
東ソー(株)製 ガードカラムHXL−H(カラム6)
カラム接続:
重量分子量10万〜100万の場合:(カラム6)に(カラム5)を4本接続したものを使用する。
重量分子量10万以下の場合:(カラム6)、(カラム4)、(カラム3)、(カラム2)、(カラム1)を順に接続したものを使用する。
検出器:RI(示差屈折計)
データ処理:東ソー(株)製マルチステーション−8020
標準ポリスチレンの調製:分子量の異なる5種または6種の標準ポリスチレンを、各々10mg秤量し、テトラヒドロフラン(以下、THFと略称する。)100mlで溶解する。溶解は20℃で実施し、24時間静置後使用。
試料の調製:試料(固形分)80mgを秤量し、THF20mlで溶解する。
カラム温度:40℃
溶媒:THF
流量:1ml/分
試料注入量:100μl
有機溶剤としては、アクリル系樹脂(B2)の溶液ラジカル重合法に使用できる有機溶剤として列記したものをそのまま使用することができるが、特にエステル類、ケトン類、エーテル類が好ましい。水性媒体に含まれる有機溶剤は単独又は2種類以上であっても良く、その使用割合は水性媒体中30重量%以下であることが好ましく、15重量%以下であることがより好ましく、5重量%以下であることが更に好ましいが、使用しないことが最も好ましい。なお、有機溶剤を使用する場合の使用割合は少なくとも1重量%以上であることが好ましい。
本発明で使用するアクリル系樹脂(C)は、重量平均分子量が350,000以上であることが必要である。重量平均分子量が350,000未満であると、旧塗膜付着性、初期の塗膜硬度、耐水性を低下させる。なかでも、旧塗膜付着性、初期の塗膜硬度、耐水性に優れる床用水性塗料が得られることから、数平均分子量が80,000以上で、重量平均分子量が350,000以上であることが好ましく、数平均分子量が90,000で、重量平均分子量が400,000以上であることがより好ましく、数平均分子量が100,000で、重量平均分子量が500,000以上であることが最も好ましい。
攪拌機、温度計、冷却管および窒素導入管を装備した4つ口のフラスコに、数平均分子量560のメトキシポリエチレングリコール32部、および、ポリイソシアネート(p−1)〔大日本インキ化学工業(株)製バーノックDN−980S:ヘキサメチレンジイソシアネート(以下、HDIと略称する。)系イソシアヌレート型ポリイソシアネート、イソシアネート基含有率(以下、NCO基含有率と略称する。)21%、不揮発分100%〕100部を仕込み、30分間かけて90℃に昇温した後、90℃にて6時間反応させて、不揮発分100%、NCO基含有率14%のメトキシポリエチレングリコールで変性されたポリイソシアネートを得た。以下、これをポリイソシアネート(A−1)と略称する。
参考例1と同様の4つ口のフラスコに、ジエチレングリコールジエチルエーテル(以下、EDEと略称する。)429部を仕込み、窒素気流下に110℃に昇温した後、ポリオキシエチレン基の数平均分子量が400のメトキシポリエチレングリコールのメタアクリレート(以下、MPEGMAと略称する。)400部、シクロヘキシルメタクリレート(以下、CHMAと略称する。)200部、メチルメタクリレート(以下、MMAと略称する。)400部、t−ブチルパーオキシ−2−エチルヘキサノエート(以下、TBPEHと略称する。)45部およびt−ブチルパーオキシベンゾエート5部からなる混合液を5時間かけて滴下した。滴下終了後、110℃にて9時間反応させて、不揮発分70%、重量平均分子量18,000のアクリル系重合体の溶液を得た。以下、これをアクリル系重合体溶液(q−1)と略称する。
参考例1と同様の4つ口のフラスコに、「ニューコール707SF」〔日本乳化剤(株)製アニオン性乳化剤〕16部、「ノイゲンTDS−200D」〔第一工業製薬(株)製ノニオン性乳化剤〕6.5部および脱イオン水220部を仕込み、窒素気流下に80℃に昇温した後、過硫酸アンモニウム0.8部を脱イオン水16部に溶解させた水溶液を添加した。さらに、ブチルアクリレート(以下、BAと略称する。)54部、MMA102部、アクリル酸(以下、AAと略称する。)4部、2−ヒドロキシエチルメタクリレート(以下、2−HEMAと略称する。)12部および2−ヒドロキシプロピルメタクリレート(以下2−HPMAと略称する。)28部からなる混合液を、3時間かけて滴下した。滴下終了後、2時間反応せしめた後、25℃まで冷却し、28%アンモニア水1.5部で中和し、脱イオン水を加えて不揮発分を45%に調整して、固形分水酸基価80mgKOH/g、ガラス転移温度(Tg)30℃のアクリル系樹脂の水分散液を得た。以下、これをアクリル系樹脂水分散液(B−1)と略称する。
下記第1表に記載した比率でアクリル系単量体を反応させた以外は参考例3と同様にして、アクリル系樹脂水分散液(B−2)〜(B−5)を得た。
下記第2表に記載した比率でアクリル系単量体を反応させた以外は参考例3と同様にして、アクリル系樹脂水分散液(RB−1)〜(RB−3)を得た。
下記第3表に記載した比率でアクリル系単量体を反応させた以外は参考例3と同様にして、アクリル系樹脂水分散液(C−1)〜(C−3)を得た。
3−MPTMS:3−メタクリロキシプロピルトリメトキシシラン
EDMA:エチレングリコールジメタクリレート
下記第4表に記載した比率でアクリル系単量体を反応させた以外は参考例3と同様にして、アクリル系樹脂水分散液(RC−1)〜(RC−3)を得た。
3−MPTMS:3−メタクリロキシプロピルトリメトキシシラン
EDMA:エチレングリコールジメタクリレート
LM:ラウリルメルカプタン
脱イオン水85.4部、「Disperbyk−190」(BYKケミ−社製分散剤)23.7部、ジメチルエタノールアミンの25%水溶液1.5部、「Ti−Pure R−960」(DuPont社製酸化チタン)270.6部および「BYK−011」(BYKケミ−社製消泡剤)の10%水溶液5.4部からなる混合物を、ディスパーで1時間分散させた。次いで、アクリル系樹脂水分散液(B−1)290部、アクリル系樹脂水分散液(C−1)290部、「BYK−346」(BYKケミ−社製レベリング剤)8.3部、「プライマルRM−8W」(ローム&ハース社製増粘剤)の10%水溶液4.8部、ジメチルエタノールアミンの25%水溶液1.1部、「BYK−028」(BYKケミ−社製消泡剤)の10%水溶液16部およびジエチレングリコールジブチルエーテル3.3部を加えて攪拌し、不揮発分55%の床用水性塗料主剤成分(D−1)を得た。
アクリル系樹脂水分散液(B−1)とアクリル系樹脂水分散液(C−1)の代わりに、アクリル系樹脂水分散液(B−2)〜(B−5)とアクリル系樹脂水分散液(C−2)〜(C−3)を、第5表(1)〜(3)に示す組み合わせで用いた以外は参考例17と同様にして、床用水性塗料主剤成分(D−2)〜(D−7)を得た。
アクリル系樹脂水分散液(B−1)とアクリル系樹脂水分散液(C−1)の代わりに、アクリル系樹脂水分散液(RB−1)〜(RB−3)とアクリル系樹脂水分散液(RC−1)〜(RC−3)を、第6表(1)〜(2)に示す組み合わせで用いた以外は参考例17と同様にして、比較用床用水性塗料主剤成分(RD−1)〜(RD−5)を得た。
ポリイソシアネート溶液(A−2)中のイソシアネート基(NCO)とアクリル系樹脂水分散液(B−1)およびアクリル系樹脂水分散液(C−1)中の水酸基(OH)のモル比(NCO/OH)が1.2となるように、ポリイソシアネート溶液(A−2)6.7部と床用水性塗料主剤成分(D−1)100部を混合し、さらに不揮発分が50%となるように水で希釈を行い、白色水性塗料(E−1)を得た。
(s−1):溶剤系エポキシ樹脂塗料アーキフロアEH(エスケー化研社製)
(s−2):溶剤系ウレタン樹脂塗料アーキフロアUT(エスケー化研社製)
(s−3):溶剤系アクリル樹脂塗料アーキフロアAS(エスケー化研社製)
(s−4):水系エポキシ樹脂塗料水性アトムエポクリーン(アトミクス社製)
(s−5):水系ウレタン樹脂塗料アクアクリーンU(アトミクス社製)
(s−6):水系アクリル樹脂塗量フロアトップ#1000(アトミクス社製)
評価基準
◎ :ブリスタなし
○ :わずかにブリスタあり。ブリスタの面積2%未満。
○―△:わずかにブリスタあり。ブリスタの面積2%以上〜5%未満。
△ :全面にブリスタあり。ブリスタの面積5%以上〜15%未満。
△−×:全面にブリスタあり。ブリスタの面積15%以上〜30%未満。
× :全面にブリスタあり。ブリスタの面積30%以上。
ポリイソシアネート(A−2)と床用水性塗料主剤成分(D−1)の代わりに、ポリイソシアネート(A−1)〜(A−2)と床用水性塗料主剤成分(D−1)〜(D−7)を第5表(1)〜(2)に示す組み合わせで用いた以外は実施例1と同様にして、白色床用水性塗料(E−2)〜(E−9)を調製し、実施例1と同様の評価を行った。試験結果を第5表(1)〜(2)に示す。
ポリイソシアネート(A−2)と床用水性塗料主剤成分(D−1)の代わりに、ポリイソシアネート(A−1)〜(A−2)と床用水性塗料主剤成分(RD−1)〜(RD−5)を第6表(1)〜(2)に示す組み合わせで用いた以外は実施例1と同様にして、白色床用水性塗料(RE−1)〜(RE−5)を調製し、実施例1と同様の評価を行った。試験結果を第6表に示す。
Claims (14)
- ポリイソシアネート(A)と、少なくとも60モル%が2級水酸基となるモル比で1級水酸基と2級水酸基を有し、水酸基価が50〜120mgKOH/gで、かつ1級水酸基に基づく水酸基価が20〜40mgKOH/gのアクリル系樹脂(B)と、重量平均分子量が350,000以上で、水酸基価が0〜15mgKOH/gのアクリル系樹脂(C)が水性媒体中に分散してなることを特徴とする床用水性塗料。
- アクリル系樹脂(B)が、60〜80モル%が2級水酸基となるモル比で1級水酸基と2級水酸基を有し、水酸基価が60〜100mgKOH/gで、かつ1級水酸基に基づく水酸基価が25〜35mgKOH/gのアクリル系樹脂であり、アクリル系樹脂(C)が水酸基価0〜12mgKOH/gのアクリル系樹脂である請求項1に記載の床用水性塗料。
- アクリル系樹脂(B)のガラス転移温度(Tgb)が15〜70℃であり、アクリル系樹脂(C)のガラス転移温度(Tgc)が30〜75℃である請求項1に記載の床用水性塗料。
- アクリル系樹脂(B)とアクリル系樹脂(C)の重量比(B/C)が0.3〜3の範囲である請求項2に記載の床用水性塗料。
- ポリイソシアネート(A)中のイソシアネート基(NCO)と、アクリル系樹脂(B)中の水酸基およびアクリル系樹脂(C)中の水酸基の合計(OH)のモル比(NCO/OH)が0.5〜2.5である請求項1に記載の床用水性塗料。
- アクリル系樹脂(B)が数平均分子量5,000〜500,000、重量平均分子量10,000〜1,000,000のアクリル系樹脂であり、アクリル系樹脂(C)が数平均分子量80,000以上、重量平均分子量350,000以上のアクリル系樹脂である請求項1〜5のいずれか1項に記載の床用水性塗料。
- アクリル系樹脂(B)のガラス転移温度(Tgb)が25〜60℃であり、アクリル系樹脂(C)のガラス転移温度(Tgc)が40〜65℃である請求項6に記載の床用水性塗料。
- アクリル系樹脂(B)とアクリル系樹脂(C)の重量比(B/C)が0.4〜2.2の範囲である請求項6に記載の床用水性塗料。
- ポリイソシアネート(A)中のイソシアネート基(NCO)と、アクリル系樹脂(B)中の水酸基およびアクリル系樹脂(C)の有する水酸基の合計(OH)のモル比(NCO/OH)が0.7〜1.5である請求項6に記載の床用水性塗料。
- 請求項1〜9のいずれか1項に記載の床用水性塗料を、旧塗膜が存在する床材の上に塗工し、乾燥させることを特徴とする床塗工方法。
- 請求項1〜9のいずれか1項に記載の床用水性塗料を、旧塗膜が存在する床材の上に塗工し、乾燥させた後、その上にさらに前記床用水性塗料を塗工し、乾燥させることを特徴とする床塗工方法。
- 旧塗膜が存在する床材が、旧塗膜が存在する無機質床材である請求項10または11に記載の床塗工方法。
- 請求項1〜9のいずれか1項に記載の床用水性塗料を、プライマーが塗工されていてもよい床材の上に塗工し、乾燥させた後、その上にさらに前記床用水性塗料を塗工し、乾燥させることを特徴とする床塗工方法。
- プライマーが塗工されていてもよい床材が、プライマーが塗工されていてもよい無機質床材である請求項13に記載の床塗工方法。
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