JP2017155368A - 繊維加工用樹脂組成物、それを用いた布帛 - Google Patents
繊維加工用樹脂組成物、それを用いた布帛 Download PDFInfo
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- JP2017155368A JP2017155368A JP2016040659A JP2016040659A JP2017155368A JP 2017155368 A JP2017155368 A JP 2017155368A JP 2016040659 A JP2016040659 A JP 2016040659A JP 2016040659 A JP2016040659 A JP 2016040659A JP 2017155368 A JP2017155368 A JP 2017155368A
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- JP
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- Prior art keywords
- titanium oxide
- mass
- photocatalyst
- copper
- polymerizable monomer
- 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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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 152
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 103
- 239000000178 monomer Substances 0.000 claims abstract description 94
- 239000011941 photocatalyst Substances 0.000 claims abstract description 76
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- 239000010949 copper Substances 0.000 description 29
- 229910052802 copper Inorganic materials 0.000 description 28
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 4
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- 125000005250 alkyl acrylate group Chemical group 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 4
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- 229910000431 copper oxide Inorganic materials 0.000 description 3
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
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Abstract
Description
アクリル樹脂(A)は、特定の重合性単量体組成を有する。具体的には、アクリル樹脂(A)の原料となる重合性単量体全量中の2個のカルボキシル基を有する重合性単量体(a1)の比率が0.5質量%以上かつ1個のカルボキシル基を有する重合性単量体(a2)の比率が2.8質量%以下である。すなわち、アクリル樹脂(A)は、2個のカルボキシル基を有する重合性単量体(a1)を必須原料として共重合して得られるものである。
1/Tg=W1/Tg1+W2/Tg2+・・・+Wi/Tgi+・・・+Wn/Tgn
上記FOX式において、Tgは、n種類の重合性単量体からなる重合体のガラス転移温度であり、Tg(1、2、i、n)は、各重合性単量体のホモポリマーのガラス転移温度であり、W(1、2、i、n)は、各重合性単量体の質量分率であり、W1+W2+・・・+Wi+・・・+Wn=1である。
光触媒(B)は、結晶性ルチル型酸化チタンを含む酸化チタンと2価銅化合物とを含有する光触媒であって、前記結晶性ルチル型酸化チタンが、Cu−Kα線による回折角度2θに対する回折線強度をプロットしたX線回折パターンにおいて、ルチル型酸化チタンに対応する最も強い回折ピークの半値全幅が0.65度以下の酸化チタンであり、前記酸化チタン中における前記結晶性ルチル型酸化チタンの含有量が50モル%以上、アナターゼ型酸化チタンの含有量が50モル%未満である光触媒である。
なお、本発明において、「明所」とは、可視光の存在する箇所のことをいい、「暗所」とは、光の存在しない箇所のことをいう。
光触媒(B)に用いる酸化チタンは、結晶性ルチル型酸化チタンを含むものである。
本発明において、結晶性ルチル型酸化チタンとは、Cu−Kα線による回折角度2θに対する回折線強度をプロットしたX線回折パターンにおいて、ルチル型酸化チタンに対応する最も強い回折ピークの半値全幅が0.65度以下の酸化チタンのことを意味する。
光触媒(B)は、2価銅化合物を含む。この2価銅化合物単独では、明所及び暗所における抗ウイルス性、明所における有機化合物分解性、可視光応答性を有しないが、前述した結晶性ルチル型酸化チタンと組み合わせることにより、明所及び暗所における抗ウイルス性、明所における有機化合物分解性、及び可視光応答性が十分に発現する。また、この2価銅化合物は、1価銅化合物と比べて酸化等による変色が少ないため、この2価銅化合物を用いた光触媒は、変色が抑制される。
Cu2(OH)3X (1)
一般式(1)において、Xは陰イオンであり、好ましくはCl、Br、I等のハロゲン、CH3COO等のカルボン酸の共役塩基、NO3、(SO4)1/2等の無機酸の共役塩基、又はOHである。
ここで、この酸化チタン100質量部に対する2価銅化合物の銅換算含有量は、2価銅化合物の原料と酸化チタンの原料との仕込み量から算出することができる。また、この銅換算含有量は、後述するICP(誘導結合プラズマ)発光分光分析により光触媒を測定することで特定することもできる。
水性媒体(C)としては、水、水と混和する有機溶剤、及び、これらの混合物が挙げられる。水と混和する有機溶剤としては、例えば、メタノール、エタノール、n−プロパノール及びイソプロパノール等のアルコール;アセトン、メチルエチルケトン等のケトン;エチレングリコール、ジエチレングリコール、プロピレングリコール等のポリアルキレングリコール;ポリアルキレングリコールのアルキルエーテル;N−メチル−2−ピロリドン等のラクタム等が挙げられる。なお、これらの有機溶剤は、1種で用いることも2種以上併用することもできる。本発明では、水のみを用いても良く、また水及び水と混和する有機溶剤との混合物を用いても良く、水と混和する有機溶剤のみを用いても良い。安全性や環境に対する負荷の点から、水のみ、または、水及び水と混和する有機溶剤との混合物が好ましく、水のみを使用することが特に好ましい。
(合成例1:アクリル樹脂(A−1)の合成)
アクリル酸エチル(エチルアクリレート)53.6質量部、アクリル酸n−ブチル(n−ブチルアクリレート)29.6質量部、アクリロニトリル15.7質量部、イタコン酸1.1質量部、水36.5質量部、及び非イオン性乳化剤(第一工業製薬株式会社製「ノイゲンEA−207D」)41.2質量部を混合した後、ホモジナイザー(特殊機化工業株式会社製「TKホモディスパー」)を用いて乳化して単量体乳化物を調製した。
表1に示した原料を用いた点以外は合成例1と同様に行い、アクリル樹脂(A−2)〜(A−11)の水性樹脂エマルジョンを得た。
まず、使用する酸化チタン原料(昭和電工セラミックス株式会社製)について、次のとおり性状を測定した。
酸化チタン原料のBET比表面積は、株式会社マウンテック製の全自動BET比表面積測定装置「Macsorb,HM model−1208」を用いて測定した。
酸化チタン原料中におけるルチル型酸化チタンの含有量(ルチル化率)及び結晶性(半値全幅)は、粉末X線回折法により測定した。
すなわち、乾燥させた酸化チタン原料について、測定装置としてPANalytical社製「X’pertPRO」を用い、銅ターゲットを用い、Cu−Kα1線を用いて、管電圧45kV、管電流40mA、測定範囲2θ=20〜100deg、サンプリング幅0.0167deg、走査速度3.3deg/minの条件でX線回折測定を行った。
ルチル型結晶に対応するピーク高さ(Hr)、ブルッカイト型結晶に対応するピーク高さ(Hb)、及びアナターゼ型結晶に対応するピーク高さ(Ha)を求め、以下の計算式により、酸化チタン中におけるルチル型酸化チタンの含有量(ルチル化率)を求めた。
ルチル化率(モル%)={Hr/(Ha+Hb+Hr)}×100
また、酸化チタン中における、アナターゼ型酸化チタンの含有量(アナターゼ化率)及びブルッカイト型酸化チタンの含有量(ブルッカイト化率)を、それぞれ以下の計算式により求めた。
アナターゼ化率(モル%)={Ha/(Ha+Hb+Hr)}×100
ブルッカイト化率(モル%)={Hb/(Ha+Hb+Hr)}×100
上記X線回折測定によって得られたX線回折パターンにおいて、ルチル型酸化チタンに対応する最も強い回折ピークを選択し、半値全幅を測定した。
平均一次粒子径(DBET)(nm)は、BET1点法により、酸化チタンの比表面積S(m2/g)を測定し、下式
DBET=6000/(S×ρ)
より算出した。ここでρは酸化チタンの密度(g/cm3)を示す。
使用した酸化チタン原料の測定結果を表2に示す。
蒸留水100mLに6g(100質量部)の酸化チタン原料(昭和電工セラミックス株式会社製)を懸濁させ、0.0805g(銅換算で0.5質量部)のCuCl2・2H2O(関東化学株式会社製)を添加して、10分攪拌した。pHが10になるように、1mol/Lの水酸化ナトリウム(関東化学株式会社製)水溶液を添加し、30分間攪拌混合を行ってスラリーを得た。このスラリーをろ過し、得られた粉体を純水で洗浄し、80℃で乾燥し、ミキサーで解砕し、試料(光触媒)を得た。
製造例1により得られた試料(光触媒)について、酸化チタン中におけるルチル型酸化チタンの含有量(ルチル化率)及び結晶性(半値全幅)を、粉末X線回折法により測定した。
すなわち、乾燥させた光触媒を、乳鉢で擦り潰した粉末を試料とした。この試料について、測定装置としてPANalytical社製「X’pertPRO」を用い、銅ターゲットを用い、Cu−Kα1線を用いて、管電圧45kV、管電流40mA、測定範囲2θ=20〜100deg、サンプリング幅0.0167deg、走査速度3.3deg/minの条件でX線回折測定を行った。
ルチル化率(モル%)={Hr/(Ha+Hb+Hr)}×100
製造例1により得られた試料(光触媒)中に存在する2価銅化合物を、上記の測定装置及び測定条件にて、X線回折測定で同定した。
製造例1で得られた光触媒2質量部、及び水18質量部を混合し、酸化チタン水分散液を得た。
水18.8質量部、合成例1で得られたアクリル樹脂(A−1)の水性樹脂エマルジョン(樹脂分52質量%)38.5質量部(樹脂として20質量部)、調製例1で得られた酸化チタン水分散液20質量部(酸化チタンとして2質量部)、消泡剤(サンノプコ株式会社製「ノプコ8034」)0.2質量部、プロピレングリコール2質量部、非イオン系界面活性剤(第一工業製薬株式会社製「ノイゲン EA−157」)2質量部、ウレタン系増粘剤(株式会社ADEKA製「アデカノールUH−420」)2質量部、アクリル系増粘剤(DIC株式会社製「ボンコートV−E」)16質量部、及び25質量%アンモニア水0.5質量部(合計100質量部)を分散攪拌機(特殊機化工業株式会社製 TKホモディスパー)を用いて均一に混合して繊維加工用樹脂組成物(1)を得た。
表4に示す組成に従った点以外は実施例1と同様に行い、繊維加工用樹脂組成物(2)〜(19)を得た。
表5に示す組成に従った点以外は実施例1と同様に行い、繊維加工用樹脂組成物(R1)〜(R4)を得た。
実施例1〜19、比較例1〜4で得られた各繊維加工用樹脂組成物を、それぞれポリエステル生地(100g/m2)上にオートスクリーン捺染機(辻井染機工業株式会社製)を用いて乾燥前塗布量100g/m2となるようにプリントを実施し、熱風循環式乾燥機にて150℃、2分間乾燥させ、評価用プリント布を得た。
上記で得られた評価用プリント布について、抗ファージウイルス試験(JIS R1756を参照)を実施した。結果を表4、5に示した。
1)光照射条件は、白色蛍光灯の光をN113フィルターによって紫外線をカットし、照度1000ルクスとした。
2)5cm×5cmの評価用プリント布に濃度既知の100μLのQβファージ溶液を垂らした後、5cm×5cmのガラス板で挟んだ。
3)2時間光照射したサンプルを、SCDLP液で回収し、適度に希釈したものを大腸菌と感染させ、寒天培地に塗布し、培養後のコロニー数をカウントすることで評価した。抗ウイルス性はQβファージの不活化度で評価し、不活化度−2〜−5を抗ウイルス性有と評価した。
不活化度が−1が90%、不活化度が−2が99%、不活化度が−3が99.9%不活化していることになり、抗ウイルス性が高いことを示す。検出限界は不活化度−5である。
JIS L 0844:2005のA−4法に準拠して、評価用プリント布を用いて試験を繰り返し30回行った後、抗ウイルス性を評価し、洗濯試験前後の抗ウイルス性を比較評価した。結果を表4、5に示した。
Claims (2)
- アクリル樹脂(A)、光触媒(B)及び水性媒体(C)を含有し、
前記光触媒(B)が、結晶性ルチル型酸化チタンを含む酸化チタンと2価銅化合物とを含有し、
前記結晶性ルチル型酸化チタンが、Cu−Kα線による回折角度2θに対する回折線強度をプロットしたX線回折パターンにおいて、ルチル型酸化チタンに対応する最も強い回折ピークの半値全幅が0.65度以下の酸化チタンであり、
前記酸化チタン中における前記結晶性ルチル型酸化チタンの含有量が50モル%以上、アナターゼ型酸化チタンの含有量が50モル%未満である光触媒であり、
前記アクリル樹脂(A)100質量部に対して、前記光触媒(B)を3〜50質量部含有し、
前記アクリル樹脂(A)の原料となる重合性単量体全量中の2個のカルボキシル基を有する重合性単量体(a1)の比率が0.5質量%以上かつ1個のカルボキシル基を有する重合性単量体(a2)の比率が2.8質量%以下であることを特徴とする繊維加工用樹脂組成物。 - 請求項1記載の繊維加工用樹脂組成物を用いた加工品であることを特徴とする布帛。
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