JP6959606B2 - 化粧シート及び化粧シートの製造方法 - Google Patents
化粧シート及び化粧シートの製造方法 Download PDFInfo
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- JP6959606B2 JP6959606B2 JP2017060153A JP2017060153A JP6959606B2 JP 6959606 B2 JP6959606 B2 JP 6959606B2 JP 2017060153 A JP2017060153 A JP 2017060153A JP 2017060153 A JP2017060153 A JP 2017060153A JP 6959606 B2 JP6959606 B2 JP 6959606B2
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- decorative sheet
- nucleating agent
- polypropylene resin
- crystalline polypropylene
- sheet according
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Description
しかし、従来のオレフィン系樹脂製の化粧シートは、一般的なポリプロピレンシートを使用しているために表面の耐傷性が悪く、従来のポリ塩化ビニル製の化粧シートに比べて耐傷性に劣っているものであった。
ここで、後加工性を向上させた化粧シートとして、特許文献4〜6に記載の化粧シートが提案されている。これらの化粧シートは、ランダム重合タイプのポリプロピレン樹脂に軟質成分を添加した透明樹脂層をもつ化粧シートである。しかしながら、この化粧シートは、後加工性の向上に伴いシートが柔軟になっていることから、耐傷性が悪化するという問題点がある。
課題を解決するために、本発明の一態様である化粧シートは、高結晶性ポリプロピレン樹脂を主成分とする透明樹脂層を少なくとも具備してなる化粧シートであって、
上記透明樹脂層は、高結晶性ポリプロピレン樹脂100質量部に対し、引張り弾性率が25MPa以上500MPa以下の低結晶性ポリプロピレン樹脂が0.1質量部以上20質量部以下で添加されている。
また、本発明の一態様である化粧シートの製造方法は、上記透明樹脂層を、上記高結晶性ポリプロピレン樹脂に、ナノサイズの造核剤を添加して形成する。
また、低結晶性ポリプロピレン樹脂は高結晶性ポリプロピレン樹脂と高い相溶性を示すため、引張り弾性率が上記の範囲である低結晶性ポリプロピレン樹脂を添加することで、透明樹脂層に対して高い透明性を付与しつつ後加工性を向上させることができる。さらに、低結晶性ポリプロピレン樹脂の添加量を上記の範囲とすることによって、耐傷性と後加工性に優れた化粧シートを得ることができる。
また、上記の高結晶性ポリプロピレン樹脂にナノサイズの造核剤を添加して、上記の透明樹脂層を形成することで、高結晶性ポリプロピレン樹脂の結晶化度が向上し、極めて高い透明性を有する化粧シートを得ることができる。また、化粧シートの耐傷性と後加工性とをさらに向上させることができる。
ここで、図面は模式的なものであり、厚さと平面寸法との関係、各層の厚さの比率等は現実のものとは異なる。また、以下に示す実施形態は、本発明の技術的思想を具体化するための構成を例示するものであって、本発明の技術的思想は、構成部品の材質、形状、構造等が下記のものに特定するものでない。本発明の技術的思想は、特許請求の範囲に記載された請求項が規定する技術的範囲内において、種々の変更を加えることができる。
また、基材層6の他方の面(裏面)に、隠蔽層7、プライマー層8がこの順に形成されている。なお、隠蔽層7は、基材層6と絵柄模様層5との間に形成しても良いし、省略しても構わない。
なお、図1においては、本実施形態の化粧シート1を基材Bに貼り付けて化粧板を構成する場合を例示している。
基材層6は、紙、樹脂シート、箔などから構成される。紙としては、薄葉紙、チタン紙、樹脂含浸紙、有機もしくは無機系の不織布、合成紙等が例示出来る。樹脂シートの樹脂としては、ポリエチレン、ポリプロピレン、ポリブチレン、ポリスチレン、ポリカーボネート、ポリエステル、ポリアミド、エチレン−酢酸ビニル共重合体、ポリビニルアルコール、アクリル等の合成樹脂、あるいはこれら合成樹脂の発泡体、エチレン−プロピレン共重合ゴム、エチレン−プロピレン−ジエン共重合ゴム、スチレン−ブタジエン共重合ゴム、スチレン−イソプレン−スチレンブロック共重合ゴム、スチレン−ブタジエン−スチレンブロック共重合ゴム、ポリウレタン等のゴムが例示出来る。箔としては、アルミニウム、鉄、金、銀等の金属箔等が例示出来る。
絵柄模様層5は、既知の印刷手法を用いて設けることが出来る。基材層6が巻取りの状態で用意できる場合には、ロールツーロールの印刷装置で絵柄模様層5の形成のための印刷を行うことができる。印刷手法は特に限定するものではないが、生産性や絵柄の品位を考慮すれば、例えばグラビア印刷法を用いることができる。
絵柄模様は、床材や壁材などの使用箇所に応じた意匠性を考慮して任意の絵柄模様を採用すればよく、木質系の絵柄であれば各種木目が好んで用いられることが多く、木目以外にもコルクを絵柄模様とすることもできる。例えば大理石などの石材の床をイメージしたものであれば大理石の石目などの絵柄模様として用いられることもある。また天然材料の絵柄模様以外にそれらをモチーフとした人工的絵柄模様や幾何学模様などの人工的絵柄模様も用いることができる。
印刷インキには、適宜、通常のインキに含まれている顔料、染料等の着色剤、体質顔料、溶剤、バインダーを添加する。顔料としては、縮合アゾ、不溶性アゾ、キナクリドン、イソインドリン、アンスラキノン、イミダゾロン、コバルト、フタロシアニン、カーボン、酸化チタン、酸化鉄、雲母等のパール顔料等が挙げられる。なお、バインダーは、水性、溶剤系、エマルジョンタイプのいずれでもよく、硬化方法についても1液タイプ、主剤と硬化剤とからなる2液タイプ、もしくは、紫外線や電子線などによって硬化するタイプなど特に限定するものではない。中でも最も一般的な方法は、2液タイプのもので、ウレタン系の主剤と、イソシアネートからなる硬化剤を用いる方法である。この他にも、各種金属の蒸着やスパッタリングで意匠を施すようにしてもよい。
接着剤層4は、基材層6および絵柄模様層5と透明樹脂層3の接着を強固にする目的で設けられる。この接着が強固であることによって、化粧シート1に対し、曲面や直角面に追随する曲げ加工性を付与することができる。接着剤層4は透明であることが好ましい。
接着剤層4は、その接着方法としては任意の材料選定が可能で、熱ラミネート、押出ラミネート、ドライラミネート等による積層方法があり、接着剤はアクリル系、ポリエステル系、ポリウレタン系、エポキシ系などから適宜選択できる。通常はその凝集力から2液硬化タイプのものとして、特にイソシアネートを用いたポリオールとの反応で得られるウレタン系の材料を用いることが望ましい。なお、接着剤層4は、透明樹脂層3と絵柄模様層5との接着強度が十分に得られる場合には、省略してもよい。
透明樹脂層3は、例えば透明樹脂シートとして製造して積層する。
透明樹脂層3は、高結晶性ポリプロピレン樹脂を主成分とする。主成分とは、例えば、透明樹脂層3を構成する樹脂のうちの80〜100質量部、好ましくは90〜100質量部であることを指す。
本実施形態の透明樹脂層3には、高結晶性ポリプロピレン樹脂100質量部に対し、引張り弾性率が25MPa以上500MPa以下の低結晶性ポリプロピレン樹脂が0.1〜20質量部添加されている。引張り弾性率は、より好ましくは50〜120MPaである。
透明樹脂層3の主成分となる高結晶性ポリプロピレン樹脂は、例えば、ペンタッド分率の異なるアイソタクチックポリプロピレンとシンジオタクチックポリプロピレン、ランダムポリプロピレン、ブロックポリプロピレンおよびこれらの混合物から適宜選択して設計することができる。本実施形態においては、当該高結晶性ポリプロピレン樹脂が、ペンタッド分率(mmmm分率)が95%以上、より好ましくは96%以上のプロピレンの単独重合体、すなわちホモポリマーである高結晶性ホモポリプロピレン樹脂とされることが好ましい。
そして、透明樹脂層3の主成分を高結晶性ポリプロピレン樹脂とすることで、化粧シートの表面強度(耐傷性)が高くなる。
透明樹脂層3に添加する低結晶性ポリプロピレン樹脂としては、下記に示す特徴のうちの少なくとも1つを満たすポリプロピレン樹脂であることが好ましい。
・メソペンタッド分率が20〜60%
(より好ましくは、40〜55%)
・230℃におけるMFRが30〜100
(より好ましくは、30〜60)
・質量平均分子量(Mw)が10,000〜500,000
(より好ましくは、50,000〜200,000)
・分子量分布(Mw/Mn)が4未満
・示差走査型熱量計(DSC)を用いて、窒素雰囲気下で、−10℃で5分間保持した後10℃/分で昇温させることによって得られた融解吸熱カーブの最も高温側に観測されるピークのピークトップとして定義される融点が0〜120℃
(より好ましくは、40〜100℃)
透明樹脂層3に、ナノサイズの造核剤が添加されていることが好ましい。特に、ナノサイズの造核剤が、単層膜の外膜を具備するベシクルに内包された、造核剤ベシクルの形で添加されていることが好ましい。
高結晶性ポリプロピレン樹脂に対して造核剤ベシクルを添加することにより、高結晶性ポリプロピレン樹脂の結晶化度を向上させて、極めて高い透明性を有する透明樹脂シートを得ることができる。即ち、ナノサイズの造核剤を添加することで、耐傷性をさらに向上させることが出来る。
造核剤ベシクルは、Bangham法、エクストルージョン法、水和法、界面活性剤透析法、逆相蒸発法、凍結融解法、超臨界逆相蒸発法などによって調製することができる。その中でも特に超臨界逆相蒸発法がより好ましい。
化粧シート1の最表面には、表面の保護や艶の調整としての役割を果たす表面保護層2が設けられている。
表面保護層2の材料としては、ポリウレタン系、アクリルシリコン系、フッ素系、エポキシ系、ビニル系、ポリエステル系、メラミン系、アミノアルキッド系、尿素系などから適宜選択して用いることができる。材料の形態は、水性、エマルジョン、溶剤系など特に限定されるものではない。硬化法についても一液タイプ、二液タイプ、紫外線硬化法など適宜選択して行うことができる。
隠蔽層7は、隠蔽性を保たせることを目的として、例えば、絵柄模様層5と同様に印刷によって形成される。インキに含ませる顔料としては不透明な顔料、酸化チタン、酸化鉄等を使用することが好ましい。また隠蔽性を上げるために金、銀、銅、アルミ等の金属を添加することも可能である。一般的にはフレーク状のアルミを添加することが多い。なお、隠蔽層7は、基材層6が不透明で隠蔽性を有している場合には、省略することができる。
プライマー層8は、基材Bとの密着性を向上させるために形成する。
プライマー層8は、基材Bが木質系基材Bの場合には、例えば、エステル系樹脂、ウレタン系樹脂、アクリル系樹脂、ポリカーボネート系樹脂、塩化ビニル−酢酸ビニル共重合体、ポリビニルブチラール系樹脂、ニトロセルロース系樹脂等を挙げることができ、これらの樹脂は単独ないし混合して接着組成物とし、ロールコート法やグラビア印刷法等の適宜の塗布手段を用いて形成することができる。この場合、プライマー層8を構成する樹脂としては、ウレタン−アクリレート系樹脂が好ましい、すなわち、アクリル系樹脂とウレタン系樹脂との共重合体とイソシアネートとからなる樹脂で形成するのが特に好ましい。
(1)高結晶性ポリプロピレン樹脂を主成分とする透明樹脂層3に、引張り弾性率を本実施形態の範囲とする低結晶性ポリプロピレン樹脂を本実施形態の範囲内で添加する。
低結晶性ポリプロピレン樹脂は、高結晶性ポリプロピレン樹脂と高い相溶性を示すため、透明樹脂層3に対して高い透明性を付与することができる。
さらに、低結晶性ポリプロピレン樹脂の添加量を本実施形態の範囲とすることによって、耐傷性と後加工性に優れた化粧シートを得ることができる。
メソペンタッド分率を20〜60%とすることで、溶融押出時に固化が遅くならず、製膜後の透明樹脂層3がべたつくのを抑制することができる。
(3)低結晶性ポリプロピレン樹脂の230℃におけるMFRが30〜100である。
低結晶性ポリプロピレン樹脂のMFRを該範囲とすることにより、低結晶性ポリプロピレン樹脂の流動性が適度となり、溶融押出機にて問題なく製膜することができる。
低結晶性ポリプロピレン樹脂の質量平均分子量を該範囲とすることにより、低結晶性ポリプロピレン樹脂の粘度が適度となり、溶融押出時に問題なく製膜することができる。
(5)低結晶性ポリプロピレン樹脂の分子量分布(Mw/Mn)が4未満である。
分子量分布を該範囲とすることにより、透明樹脂層3の製膜性の低下が抑制される。
このような低結晶性ポリプロピレン樹脂を使用することで、透明樹脂層3に含まれる添加剤のブリードを抑制することができる。
造核剤にナノ化処理を施すことによって、透明樹脂層3に対する造核剤の分散性を著しく向上させることができる。これによって、透明性と後加工性を維持したまま、耐傷性を向上させることができる。
造核剤にナノ化処理を施すことによって、透明樹脂層3に対する造核剤の分散性を著しく向上させることができる。これによって、透明性と後加工性を維持したまま、耐傷性を向上させることができる。
造核剤をベシクルに内包させることによって、透明樹脂層3に対する造核剤の分散性をさらに向上させることができる。これによって、透明性と後加工性を維持したまま、耐傷性をさらに向上させることができる。
超臨界逆相蒸発法を用いることによって、造核剤をベシクルに確実に内包させることができる。
<実施例1〜22>
各実施例として、透明樹脂層3の主成分である高結晶性ポリプロピレン樹脂100質量部に対して、表1に示すように、低結晶性ポリプロピレン樹脂を添加した透明樹脂層3を有する化粧シート1とした。
各化粧シートの基本的な製造方法については以下のとおりである。
高結晶性ポリプロピレン樹脂としてペンタッド分率が97.8%、MFR(メルトフローレート)が15g/10min(230℃)、分子量分布MWD(Mw/Mn)が2.3の高結晶性ホモポリプロピレン樹脂を使用した。
各実施例において、添加する低結晶性ポリプロピレン樹脂は、表1に記載の通りである。
また、実施例17と実施例21については、ナノ化した造核剤を添加した。ナノ化した造核剤は、後述の通り、超臨界逆相蒸発法によりベシクル化された造核剤ベシクルを使用した。
すなわち、次のようにして、超臨界逆相蒸発法を用いて透明樹脂層3を形成する樹脂組成物の調製を行った。
ここで、外膜がリン脂質のような生体脂質から構成されるベシクルをリポソームと称する。
<比較例1〜7>
低結晶性ポリプロピレン樹脂の有無及びその構成、造核剤の有無を、表2のように設定して、比較例の化粧シートを製造した。その他は実施例と同じようにして製造した。
各実施例の化粧シート、及び各比較例の化粧シートについて、製膜性、結晶性の低下(結晶化度)、透明性、耐傷性、後加工性にて評価を行った。
その結果を、表3,表4に示す。
溶融押出時の透明樹脂シートの状態を目視にて観察した。
評価は下記の2段階にて行った。
○:良好(ネックインやフィルムの破断が確認できなかった)
×:劣る(ネックインやフィルムの破断が認められた)
[結晶性の低下]
結晶性について、IRにて結晶化度を算出したのち、低結晶性ポリプロピレン樹脂を添加していない場合(比較例1)と数値を比較した。
結晶化度は、フーリエ型赤外分光測定において得られた吸光スペクトルから下記の数式1を用いて算出した。ここで、数式1において、I997は波数997cm−1のピーク強度値、I938は波数938cm−1のピーク強度値、I973は波数973cm−1のピーク強度値をあらわす。
○:良好(比較例1の結晶化度と同等以上)
×:劣る(比較例1の結晶化度より劣る)
[透明性]
製造した透明樹脂層3を目視で観察し、下層の絵柄模様の視認性によって評価した。
評価は下記の3段階にて行った。
○:良好(透明である)
△:意匠性は問題ないが、やや白濁している(実用上問題ないレベル)
×:劣る(白濁している)
[耐傷性]
鉛筆硬度試験にて評価した。
試験方法はJIS−K5600に準拠し、評価方法としては、透明樹脂層3の表面に凹みが付かない最高硬度がHB以上の場合「◎」、2B以上の場合「○」、3B以下の場合「×」とした。
V溝曲げ加工適性試験に評価した。
以下に、V溝曲げ加工適性試験の詳しい方法について述べる。
まず、基材Bを構成する中質繊維板(MDF)の一方の面に対して、上記の方法で作製した各化粧シート1をウレタン系の接着剤を用いて貼り付け、基材Bの他方の面に対して、反対側の化粧シート1にキズが付かないようにV型の溝を基材Bと化粧シート1とを貼り合わせている境界まで入れる。次に、化粧シート1の面が山折りとなるように基材Bを当該V型の溝に沿って90度まで曲げ、化粧シート1の表面の折れ曲がった部分に白化や亀裂などが生じていないかを光学顕微鏡を用いて観察し、耐後加工性の優劣の評価を行う。
評価は下記の3段階にて行った。
○:白化・亀裂などが認められなかった
△:軽微な白化・亀裂が認められるが、実用上問題ないレベルである
×:化粧シートとして容認できない白化・亀裂が認められた
また、比較例2の化粧シートでは、溶融押出時にネックインが発生し、製膜不良となっている。更に軟らかすぎて耐傷性が劣化した。
また、比較例3の化粧シートでは、溶融押出時にネックインが発生し、製膜不良となっている。更に軟らかすぎて耐傷性が劣化した。
また、比較例4の化粧シートでは、V溝加工時に白化した。
また、比較例5の化粧シートでは、V溝加工時に白化した。
また、比較例6の化粧シートでは、低結晶性ポリプロピレン樹脂の添加量が少なすぎて、後加工性が良化しなかった、すなわち、白化した。
また、比較例7の化粧シートでは、低結晶性ポリプロピレン樹脂の添加量が多すぎるため、溶融押出時にネックインが発生するとともに、樹脂が軟化しすぎてしまうことによって耐傷性が劣化した。
2 表面保護層
3 透明樹脂層
3a エンボス模様
4 接着剤層
5 絵柄模様層
6 基材層
7 隠蔽層
8 プライマー層
B 基材
Claims (17)
- 高結晶性ポリプロピレン樹脂を主成分とする透明樹脂層を有する化粧シートであって、
上記透明樹脂層は、高結晶性ポリプロピレン樹脂100質量部に対し、引張り弾性率が25MPa以上500MPa以下の低結晶性ポリプロピレン樹脂が0.1質量部以上20質量部以下で添加されており、
上記低結晶性ポリプロピレン樹脂は、メソペンタッド分率が55%以上60%以下であることを特徴とする化粧シート。 - 上記低結晶性ポリプロピレン樹脂は、230℃におけるMFR(melt flow rate)が30以上100以下であることを特徴とする請求項1に記載の化粧シート。
- 上記低結晶性ポリプロピレン樹脂は、質量平均分子量(Mw)が10,000以上500,000以下であることを特徴とする請求項1又は請求項2に記載の化粧シート。
- 上記低結晶性ポリプロピレン樹脂の分子量分布(Mw/Mn)が4未満であることを特徴とする請求項1〜請求項3のいずれか1項に記載の化粧シート。
- 上記低結晶性ポリプロピレン樹脂は、示差走査型熱量計(DSC)を用いて、窒素雰囲気下、−10℃で5分間保持した後、10℃/分で昇温させることによって得られた融解吸熱カーブの最も高温側に観測されるピークのピークトップとして定義される融点が、0℃以上120℃以下であることを特徴とする請求項1〜請求項4のいずれか1項に記載の化粧シート。
- 上記透明樹脂層に、ナノサイズの造核剤が添加されていることを特徴とする請求項1〜請求項5のいずれか1項に記載の化粧シート。
- 上記透明樹脂層を、上記高結晶性ポリプロピレン樹脂に、ナノサイズの造核剤を添加して形成することを特徴とする請求項1〜請求項5のいずれか1項に記載の化粧シート。
- 上記造核剤は、単層膜の外膜を具備するベシクルに造核剤が内包されている造核剤ベシクルであることを特徴とする請求項6又は請求項7に記載の化粧シート。
- 超臨界逆相蒸発法によって、上記造核剤をベシクルに内包させたことを特徴とする請求項8に記載の化粧シート。
- 上記造核剤は、ピメリン酸金属塩、またはベンジリデンソルビトールであることを特徴とする請求項6〜請求項9のいずれか1項に記載の化粧シート。
- 上記造核剤は、非溶融型の造核剤に対して、溶融型の造核剤が混合された造核剤であることを特徴とする請求項6〜請求項9のいずれか1項に記載の化粧シート。
- 上記溶融型の造核剤は、ベンジリデンソルビトールであることを特徴とする請求項11に記載の化粧シート。
- 上記造核剤は、リン脂質が造核剤の表面を単層膜で覆ったナノベシクルであることを特徴とする請求項10〜請求項12のいずれか1項に記載の化粧シート。
- 上記透明樹脂層は、高結晶性ポリプロピレン樹脂100質量部に対し、上記低結晶性ポリプロピレン樹脂が0.1質量部以上5質量部以下で添加されていることを特徴とする請求項1〜請求項13のいずれか1項に記載の化粧シート。
- 請求項1〜請求項14のいずれか1項に記載の化粧シートの製造方法であって、
上記透明樹脂層を、上記高結晶性ポリプロピレン樹脂に、ナノサイズの造核剤を添加して形成することを特徴とする化粧シートの製造方法。 - 上記造核剤は、単層膜の外膜を具備するベシクルに造核剤が内包されている造核剤ベシクルであることを特徴とする請求項15に記載の化粧シートの製造方法。
- 超臨界逆相蒸発法によって、上記造核剤をベシクルに内包させることを特徴とする請求項16に記載の化粧シートの製造方法。
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