JP4700276B2 - ハードコート層を有するポリカーボネート樹脂成形体 - Google Patents
ハードコート層を有するポリカーボネート樹脂成形体 Download PDFInfo
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- JP4700276B2 JP4700276B2 JP2003422468A JP2003422468A JP4700276B2 JP 4700276 B2 JP4700276 B2 JP 4700276B2 JP 2003422468 A JP2003422468 A JP 2003422468A JP 2003422468 A JP2003422468 A JP 2003422468A JP 4700276 B2 JP4700276 B2 JP 4700276B2
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- polycarbonate resin
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- 229920005668 polycarbonate resin Polymers 0.000 title claims description 121
- 239000004431 polycarbonate resin Substances 0.000 title claims description 121
- -1 phosphite compound Chemical class 0.000 claims description 139
- 239000000203 mixture Substances 0.000 claims description 94
- 238000000465 moulding Methods 0.000 claims description 60
- 239000011342 resin composition Substances 0.000 claims description 51
- 125000005375 organosiloxane group Chemical group 0.000 claims description 47
- 229910052751 metal Inorganic materials 0.000 claims description 43
- 239000002184 metal Substances 0.000 claims description 43
- 239000000463 material Substances 0.000 claims description 40
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 39
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 25
- 125000004432 carbon atom Chemical group C* 0.000 claims description 25
- 239000010419 fine particle Substances 0.000 claims description 25
- 229920000642 polymer Polymers 0.000 claims description 22
- 125000000217 alkyl group Chemical group 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 16
- 229920006243 acrylic copolymer Polymers 0.000 claims description 15
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 14
- 238000001746 injection moulding Methods 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 10
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- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical group C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
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- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
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- 125000006273 (C1-C3) alkyl group Chemical group 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 18
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- 239000004417 polycarbonate Substances 0.000 description 18
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 15
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- 229920000515 polycarbonate Polymers 0.000 description 15
- 229920001577 copolymer Polymers 0.000 description 14
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 14
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 12
- 125000003118 aryl group Chemical group 0.000 description 11
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 9
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000002585 base Substances 0.000 description 9
- 229920001971 elastomer Polymers 0.000 description 9
- 239000004611 light stabiliser Substances 0.000 description 9
- 230000007246 mechanism Effects 0.000 description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 8
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- 238000007906 compression Methods 0.000 description 8
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 8
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 8
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- 229920002050 silicone resin Polymers 0.000 description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 7
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 7
- 239000006087 Silane Coupling Agent Substances 0.000 description 7
- 230000002378 acidificating effect Effects 0.000 description 7
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 6
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 6
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
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Images
Description
式(i):0.1≦c≦0.5
式(ii):0.6≦d×c≦3
ここでcはハードコート層中のg/cm3で表される紫外線吸収剤の濃度であり、dは該紫外線吸収剤を含有する層のμmで表される厚みを表す。
第1層は、架橋したアクリル共重合体(アクリル共重合体−I)および紫外線吸収剤からなり、第2層は、架橋したオルガノシロキサン重合体からなり、
該架橋したアクリル共重合体(アクリル共重合体−I)は、50モル%以上の下記式(A−1)
で表される繰り返し単位、および
0〜30モル%の下記式(A−3)
該架橋したオルガノシロキサン重合体は、下記式(b−4)〜(b−6)
で表される繰り返し単位からなり、該繰り返し単位の全量を100モル%としたとき、式(b−4):80〜100モル%、式(b−5):0〜20モル%、および式(b−6):0〜20モル%である架橋したオルガノシロキサン重合体である、ハードコート層である上記構成(1)〜(7)のポリカーボネート樹脂成形体である。かかる構成によれば、耐擦傷性、色相および密着性などの長期の耐久性に優れたハードコート層を有するポリカーボネート樹脂成形体が提供される。
(i)ポリカーボネート樹脂(A成分)を準備する工程、
(ii)La、Pr、Nd、Ce、Y、Ti、Zr、Hf、V、Nb、Ta、Cr、MoおよびWの群から選択される1種以上の金属のホウ化物からなる平均粒径2〜100nmの微粒子(B成分)と、Si、Zr、TiもしくはAlの金属アルコキシドまたは該金属アルコキシドの部分加水分解縮合物、並びに樹脂バインダーの溶液、反応により樹脂バインダーを形成する液状化合物もしくは反応により樹脂バインダーを形成する化合物の溶液とを混合し、該混合物において該金属アルコキシド類を加水分解縮合反応させると共に、溶媒の除去または液状化合物の硬化を行うことにより、B成分とSi、Zr、TiおよびAlの群から選択される少なくとも1種または2種以上の金属酸化物(B’成分)と樹脂分(B”成分)との混合物(B混合成分)を準備する工程、
(iii)ホスファイト化合物(C1成分)およびホスホナイト化合物(C2成分)から選択される少なくとも1種のリン化合物(C成分)を準備する工程、
(iv)A成分、B混合成分およびC成分を押出機に供給し、溶融混練した後ペレット形態の樹脂組成物を得る工程、
(v)該ペレットを射出成形機に供給し、該ペレットを射出成形することにより、その最大投影面積が500cm2以上およびその厚み(D(mm))に対するゲート部から流動末端までの距離(L(mm))の比L/Dが、75以上である射出成形品を成形する工程、
(vi)該射出成形品の少なくとも一面に、下記成分(A)〜(E)からなるアクリル樹脂組成物を成分(A)〜(E)および溶媒からなるコーティング用組成物を塗布することにより積層し、硬化させることにより上記アクリル共重合体−Iおよび紫外線吸収剤からなる第1層を形成する工程であって、ここで、
成分(A)は50モル%以上の上記(A−1)および5〜30モル%の下記式(A−4)、並びに任意に0〜30モル%の上記式(A−3)で示される繰り返し単位からなる共重合体(アクリル共重合体−II)であり、
成分(B)はポリイソシアネート化合物および/またはブロック化されたポリイソシアネート化合物であって、その量はイソシアネート基の含有量が成分(A)のヒドロキシ基1当量に対して0.7〜5当量であり、
成分(C)は硬化触媒であって、その量は成分(A)および成分(B)の合計100重量部に対して0〜0.4重量部であり、
成分(D)は紫外線吸収剤であって、その量は成分(A)および成分(B)の合計100重量部に対して10〜50重量部であり、および、
成分(E)はシランカップリング剤であって、その量は成分(A)および成分(B)の合計100重量部に対して0〜5重量部である工程、並びに
(v)かかる第1層の表面に、下記成分(a)〜(d)を含有するオルガノシロキサン樹脂組成物を積層した後、硬化させることにより上記架橋したオルガノシロキサン重合体からなる第2層を形成する工程であって、ここで、
成分(a)は、コロイダルシリカであり、
成分(b)は、下記式(b−1)〜(b−3)
Q1Si(OQ3)3 (b−1)
Q1Q2Si(OQ3)2 (b−2)
Si(OQ3)4 (b−3)
(式中、Q1、Q2は、炭素数1〜4のアルキル基、ビニル基、またはメタクリロキシ基、アミノ基、グリシドキシ基および3,4−エポキシシクロヘキシル基からなる群より選ばれる1以上の基で置換された炭素数1〜3のアルキル基であり、Q3は炭素数1〜4のアルキル基である。)で表されるアルコキシシランから形成され、式(b−1)〜(b−3)の全量を100モル%としたとき、式(b−1):80〜100モル%、式(b−2):0〜20モル%、および式(b−3):0〜20モル%である、アルコキシシランの加水分解物および/またはそれらの縮合物であって、その量は成分(a)由来のSiと成分(b)由来のSiとのモル比(Sia/Sib)は2/8〜4/6となる量であり、
成分(c)は硬化触媒であって、その量は成分(a)および成分(b)の合計100重量部に対して0.01〜10重量部であり、および、
成分(d)は溶媒であって、その量は硬化反応により得られる樹脂固形分100重量部に対して50〜900重量部である工程
からなることを特徴とするポリカーボネート樹脂成形体の製造方法である。
(A成分:ポリカーボネート樹脂)
本発明でA成分として使用されるポリカーボネート樹脂は、二価フェノールとカーボネート前駆体とを反応させて得られるものである。反応方法の一例として界面重合法、溶融エステル交換法、カーボネートプレポリマーの固相エステル交換法、および環状カーボネート化合物の開環重合法などを挙げることができる。
上記以外の反応形式の詳細についても、成書及び特許公報などで良く知られている。
ηsp/c=[η]+0.45×[η]2c(但し[η]は極限粘度)
[η]=1.23×10−4M0.83
c=0.7
本発明においてB成分として使用されるホウ化物微粒子としては、ホウ化ランタン(LaB6)、ホウ化プラセオジウム(PrB6)、ホウ化ネオジウム(NdB6)、ホウ化セリウム(CeB6)、ホウ化イットリウム(YB6)、ホウ化チタン(TiB2)、ホウ化ジルコニウム(ZrB2)、ホウ化ハフニウム(HfB2)、ホウ化バナジウム(VB2)、ホウ化タンタル(TaB2)、ホウ化クロム(CrB、CrB2)、ホウ化モリブデン(MoB2、Mo2B5、MoB)、ホウ化タングステン(W2B5)などの微粒子がその代表的なものとして挙げられる。特にB成分としてホウ化ランタン(LaB6)が好ましい。
ここで上記A成分、B成分、並びにC成分の組成割合について説明する。B成分の金属ホウ化物微粒子は、ポリカーボネート樹脂100重量部に対して0.0005〜0.03重量部であり、好ましくは0.001〜0.01重量部、より好ましくは0.001〜0.007重量部である。B成分の金属ホウ化物微粒子が上記範囲を超えて少なすぎる場合には熱線を内部に透過し難い性質の改善が十分でない。一方B成分の金属ホウ化物微粒子が上記範囲を超えて多すぎる場合には質感の高い透明性が得られにくい。
次に本発明のハードコート層について説明する。本発明では、ハードコート処理として各種のハードコート剤が使用可能であり、本発明で使用するハードコート剤としては、シリコーン樹脂系ハードコート剤や有機樹脂系ハードコート剤などが例示される。シリコーン樹脂系ハードコート剤は、シロキサン結合をもった硬化樹脂層を形成するものであり、例えば、3官能シロキサン単位に相当する化合物(トリアルコキシシラン化合物など)を主成分とする化合物の部分加水分解縮合物、好ましくは更に4官能シロキサン単位に相当する化合物(テトラアルコキシシラン化合物など)を含む部分加水分解縮合物、並びに更にこれらにコロイダルシリカなどの金属酸化物微粒子を充填した部分加水分解縮合物などが挙げられる。シリコーン樹脂系ハードコート剤は更に2官能性のシロキサン単位および1官能性のシロキサン単位を含んでよい。これらには縮合反応時に発生するアルコール(アルコキシシランの部分加水分解縮合物の場合)などが含まれるが、更に必要に応じて任意の有機溶剤、水、あるいはこれらの混合物に溶解ないしは分散させてもよい。そのための有機溶剤としては、低級脂肪酸アルコール類、多価アルコールとそのエーテル、エステル類などが挙げられる。なお、ハードコート層には平滑な表面状態を得るため各種界面活性剤、例えば、シロキサン系、フッ化アルキル系界面活性剤などを添加してもよい。
式(i):0.1≦c≦0.5
式(ii):0.6≦d×c≦3
式(iii):2≦d≦8
である。ここでcはハードコート層中のg/cm3で表される紫外線吸収剤の濃度であり、dは該紫外線吸収剤を含有する層のμmで表される厚みを表す。ハードコート層が複数の層からなる場合(プライマー層を含む)、いずれか1つの層(特にプライマー層)がかかる式の条件を満足すればよい。
第1層は、架橋したアクリル共重合体(アクリル共重合体−I)および紫外線吸収剤からなり、第2層は、架橋したオルガノシロキサン重合体からなり、
該架橋したアクリル共重合体(アクリル共重合体−I)は、50モル%以上の下記式(A−1)
で表される繰り返し単位、および
0〜30モル%の下記式(A−3)
該架橋したオルガノシロキサン重合体は、下記式(b−4)〜(b−6)
で表される繰り返し単位からなり、該繰り返し単位の全量を100モル%としたとき、式(b−4):80〜100モル%、式(b−5):0〜20モル%、および式(b−6):0〜20モル%である架橋したオルガノシロキサン重合体である、ハードコート層である。
上記式(A−1)で表される繰り返し単位に対応するメタクリレートモノマーは、メチルメタクリレートまたはエチルメタクリレートである。
第2層は、架橋したオルガノシロキサン重合体からなる。該架橋したオルガノシロキサン重合体は、上記式(b−4)〜(b−6)で表される繰り返し単位からなり、該繰り返し単位の全量を100モル%としたとき、式(b−4):80〜100モル%、式(b−5):0〜20モル%、および式(b−6):0〜20モル%である。
本発明の上記第1層を形成するためのアクリル樹脂組成物は、成分(A)〜成分(E)を含有する。以下、各成分について説明する。
成分(A)であるアクリル共重合体−IIは、50モル%以上の上記(A−1)および5〜30モル%の下記式(A−4)、並びに任意に0〜30モル%の上記式(A−3)で示される繰り返し単位からなる共重合体である。
式(A−4)で示される繰り返し単位は以下の構造を有する。
成分(B)は、イソシアネート基の含有量が成分(A)のヒドロキシ基1当量に対して0.7〜5当量である、ポリイソシアネート化合物および/またはブロック化されたポリイソシアネート化合物である。
成分(C)は、成分(A)および成分(B)の合計100重量部に対して0〜0.4重量部の硬化触媒である。硬化触媒としては、主として有機錫化合物および/または4級アンモニウム塩化合物が使用される。
Rx mSn(OCORy)4−m
(式中、Rxは同一または異なっていてもよく炭素数1〜8の炭化水素基、Ryは同一または異なっていてもよく炭素数1〜17の置換または非置換の炭化水素基であり、mは0〜3の整数である。)
で表される有機錫化合物が好ましい。
成分(D)は、成分(A)および成分(B)の合計100重量部に対して10〜50重量部の紫外線吸収剤である。
成分(E)は、成分(A)および成分(B)の合計100重量部に対して0〜5重量部のシランカップリング剤である。
第1層に用いるアクリル樹脂組成物には、必要に応じ光安定剤を含有することができる。光安定剤としては、例えばビス(2,2,6,6−テトラメチル−4−ピペリジル)カーボネート、ビス(2,2,6,6−テトラメチル−4−ピペリジル)サクシネート、ビス(2,2,6,6−テトラメチル−4−ピペリジル)セバケート、4−ベンゾイルオキシ−2,2,6,6−テトラメチルピペリジン、4−オクタノイルオキシ−2,2,6,6−テトラメチルピペリジン、ビス(2,2,6,6−テトラメチル−4−ピペリジル)ジフェニルメタン−p,p′−ジカーバメート、ビス(2,2,6,6−テトラメチル−4−ピペリジル)ベンゼン−1,3−ジスルホネート、ビス(2,2,6,6−テトラメチル−4−ピペリジル)フェニルホスファイト等のヒンダードアミン類、ニッケルビス(オクチルフェニルサルファイド、ニッケルコンプレクス−3,5−ジ−t−ブチル−4−ヒドロキシベンジルリン酸モノエチラート、ニッケルジブチルジチオカーバメート等のニッケル錯体が挙げられる。これらの剤は単独もしくは2種以上を併用してもよい。光安定剤は、成分(A)および成分(B)の合計100重量部に対して好ましくは0.01〜50重量部、より好ましくは0.05〜10重量部用いられる。
かかるコーティング組成物中の溶媒としては、アセトン、メチルエチルケトン、メチルイソブチルケトン、シクロヘキサノン等のケトン類、テトラヒドロフラン、1,4−ジオキサン、1,2−ジメトキシエタン等のエーテル類、酢酸エチル、酢酸エトキシエチル等のエステル類、メタノール、エタノール、1−プロパノール、2−プロパノール、1−ブタノール、2−ブタノール、2−メチル−1−プロパノール、2−メチル−2−プロパノール、2−エトキシエタノール、1−メトキシ−2−プロパノール、2−ブトキシエタノール等のアルコール類、n-ヘキサン、n-ヘプタン、イソオクタン、ベンゼン、トルエン、キシレン、ガソリン、軽油、灯油等の炭化水素類、アセトニトリル、ニトロメタン、水等が挙げられ、これらは単独で使用してもよいし2種以上を混合して使用してもよい。
本発明の第2層を形成するためのオルガノシロキサン樹脂組成物は、成分(a)〜(d)を含有する。以下、各成分について説明する。
本発明で成分(a)として用いられるコロイダルシリカは、直径5〜200nm、好ましくは5〜40nmのシリカ微粒子が水または有機溶媒中にコロイド状に分散されたものである。該コロイダルシリカは、水分散型および有機溶媒分散型のどちらでも使用できるが、水分散型のものを用いるのが好ましい。水分散型のコロイダルシリカの場合、シリカ微粒子の表面に多数の水酸基が存在し、これがアルコキシシラン加水分解縮合物と強固に結合するため、より耐摩耗性に優れたプラスチック積層体が得られるものと考えられる。
成分(b)は、下記式(b−1)〜(b−3)
Q1Si(OQ3)3 (b−1)
Q1Q2Si(OQ3)2 (b−2)
Si(OQ3)4 (b−3)
(式中、Q1、Q2は、炭素数1〜4のアルキル基、ビニル基、またはメタクリロキシ基、アミノ基、グリシドキシ基および3,4−エポキシシクロヘキシル基からなる群より選ばれる1以上の基で置換された炭素数1〜3のアルキル基であり、Q3は炭素数1〜4のアルキル基である。)
で表されるアルコキシシランから形成され、式(b−1)〜(b−3)の全量を100モル%としたとき、式(b−1):80〜100モル%、式(b−2):0〜20モル%、および式(b−3):0〜20モル%である、アルコキシシランの加水分解物および/またはそれらの縮合物である。
Q1、Q2、Q3のアルキル基の具体例として、メチル基、エチル基等が挙げられる。
本発明のオルガノシロキサン樹脂組成物はさらに硬化触媒を含有する。かかる触媒としては、ギ酸、プロピオン酸、酪酸、乳酸、酒石酸、コハク酸等の脂肪族カルボン酸のリチウム塩、ナトリウム塩、カリウム塩等のアルカリ金属塩、ベンジルトリメチルアンモニウム塩、コリン塩、テトラメチルアンモニウム塩、テトラエチルアンモニウム塩等の4級アンモニウム塩が挙げられる。具体的には酢酸ナトリウム、酢酸カリウム、酢酸コリン、酢酸ベンジルトリメチルアンモニウムが好ましく使用される。
本発明のオルガノシロキサン樹脂組成物に用いられる溶媒は成分(a)および成分(b)を安定に溶解することが必要であり、そのためには少なくとも20重量%以上、好ましくは50重量%以上のアルコールを含有することが望ましい。
コロイダルシリカ分散液中で、式(b−1)、(b−2)、(b−3)のアルコキシシランを酸性条件下、加水分解縮合反応させる。
本発明の成形体は、上記A成分〜C成分からなるポリカーボネート樹脂組成物から射出成形により形成された成形品の表面に、上記のハードコート層が形成されたものである。ここで射出成形法としては、通常の射出成形法だけでなく、射出圧縮成形、射出プレス成形、断熱金型成形、急速加熱冷却金型成形、および超高速射出成形など利用することができる。中でも射出プレス成形は下記の理由などから好適である。また成形はコールドランナー方式およびホットランナー方式のいずれも選択することができる。
本発明のポリカーボネート樹脂組成物は、B成分の効果を更に有効に発揮させる目的で、炭素フィラー(D成分)を含むことができる。すなわちかかる炭素フィラーの有する熱線吸収効果との相乗作用により、本発明の樹脂成形体は成形体に覆われた内部に熱線を透過し難い性質において更に有効となる。
(1)樹脂組成物の作成
(1−1)使用原料
原料として下記のものを使用した。
(A成分)
PC:下記製法により得られた分子量24,200のポリカーボネート樹脂パウダー
バッフル付反応容器に、三段六枚羽根の攪拌機および還流冷却管を取り付けた。この反応容器に、ビスフェノールA45.6部、p−tert−ブチルフェノールをビスフェノールAに対して2.78モル%、ジクロロメタン265部及び水200部を入れ、反応容器内の酸素を除去する為に窒素パージを行った。尚、かかる段階で反応容器中の内容物は、容器容量の8割弱であった。次に、上記懸濁液にナトリウムハイドロサルファイト0.09部および水酸化ナトリウム21.8部を供給するための水溶液約80部を供給し、15℃でビスフェノールAを溶解した。撹拌下、この混合物にホスゲン23.35部を30分間で供給した。その後、トリエチルアミン0.016部(ビスフェノールAに対して0.08モル%)を添加して60分間攪拌し、反応を終結させた。その後、反応混合物を静置し、有機相を分液した。得られたポリカーボネート樹脂のジクロロメタン溶液に塩化メチレンを加えて14重量%の濃度の溶液とし、更に多孔板付遠心抽出機(川崎エンジニアリング(株)製KCC遠心抽出機)を用いて0.5%水酸化ナトリウム水溶液を流量1,000ml/min、有機相を流量1,000ml/minの速度で供給し、3,500rpmの条件で処理した後、有機相を塩酸酸性とし、その後水洗を繰り返し、水相の導電率がイオン交換水と殆ど同じになったところで塩化メチレンを蒸発してポリカーボネート樹脂パウダーを得た。
B−1:平均粒径70nmのLaB6微粒子約20重量%、ZrO2約24重量%および樹脂バインダーからなる熱線遮蔽剤(住友金属鉱山(株)製KHDS−06)
(B成分以外の剤)
B−2:三酸化二アンチモン(Sb2 O3 )をドーピングした酸化錫(SnO)微粒子(平均粒径10nm、Sb2 O3 :13重量%、SnO:87重量%)
(C成分)
C1−1:ホスファイト系熱安定剤(チバ・スペシャリティ・ケミカルズ社製:Irgafos168)
C1−2:ホスホナイト系熱安定剤(Sandoz社製:サンドスタブP−EPQ)
EW:脂肪酸フルエステル(理研ビタミン(株)製:リケスターEW−400)
SA:脂肪酸部分エステル(理研ビタミン(株)製:リケマールS−100A)
UVA:紫外線吸収剤(チバ・スペシャリティ・ケミカルズ製:Tinuvin1577)
表1に記載の各成分を表1記載の割合で計量して混合しブレンダーにて混合した後、ベント式二軸押出機を用いて溶融混練しポリカーボネート樹脂組成物のペレットを得た。PCに添加する添加剤はそれぞれ配合量の10〜100倍の濃度を目安に予めPCとの予備混合物として作成した後、ブレンダーによる全体の混合を行った。ベント式二軸押出機は(株)日本製鋼所製:TEX30α(完全かみ合い、同方向回転、2条ネジスクリュー)を使用した。混練ゾーンはベント口手前に1箇所のタイプとした。押出条件は吐出量20kg/h、スクリュー回転数150rpm、ベントの真空度3kPaであり、また押出温度は第1供給口からダイス部分まで270℃とした。尚、上記の樹脂組成物の製造はHEPAフィルターを通した清浄な空気が循環する雰囲気において実施し、また作業時に異物の混入がないよう十分に注意して行った。
上記で製造されたポリカーボネート樹脂組成物のペレットを120℃にて5時間クリーンオーブン中で乾燥した後、成形機としてシリンダー径110mmφ、型締め力12700kNの日本製鋼所製J1300E−C5射出成形機(型圧縮可能なように油圧回路および制御システムを変更した仕様)を使用して成形を行った。更に金型取り付け板の四隅4箇所に平行度矯正機構を設置した。該機構は油圧シリンダーの力により金型の取り付け面に矯正力を付与し金型間の平行度を維持するものである。所定の中間型締め状態において平行度の設定を行い、中間型締めの際の平行度を確保した。更に予め成形時の型締め位置とその金型の傾き量から必要な平行度矯正機構の保持圧力を設定し、それを時間制御することにより中間型締め状態から最終型締め状態までの平行度を確保した。
(3−1)アクリル共重合体(EMA−HEMA(I))の製造
還流冷却器および撹拌装置を備え、窒素置換したフラスコ中にエチルメタクリレート(以下EMAと略称する)102.7部、2−ヒドロキシエチルメタクリレート(以下HEMAと略称する)13部、アゾビスイソブチロニトリル(以下AIBNと略称する)0.18部および1,2−ジメトキシエタン200部を添加混合し、溶解させた。次いで、窒素気流中70℃で6時間攪拌下に反応させた。得られた反応液をn−ヘキサンに添加して再沈精製し、EMA/HEMAの組成比90/10(モル比)のコポリマー(EMA−HEMA(I))98部を得た。該コポリマーの水酸基価は48.7mgKOH/g、重量平均分子量はGPCの測定(カラム;Shodex GPCA−804、溶離液;THF)からポリスチレン換算で90,000であった。
上記EMA−HEMA(I)10部および紫外線吸収剤(チバスペシャルティケミカルス社製チヌビン411L)2.00部をメチルイソブチルケトン50部および2−ブタノール25部からなる混合溶媒に溶解し、さらにこの溶液にEMA−HEMA(I)のヒドロキシ基1当量に対してイソシアネート基が1当量になるようにポリイソシアネート化合物前駆体(デグサジャパン(株)製VESTANATB1358/100)2.96部を添加し、さらにジメチルチンジネオデカノエート0.005部、シランカップリング剤(日本ユニカー(株)製APZ−6633 5%エタノール溶液)1.5部を添加し25℃で30分間攪拌し、第1層用のアクリル樹脂組成物(HC−1)を調製した。
水分散型コロイダルシリカ分散液(触媒化成工業(株)製 カタロイドSN30 固形分濃度30重量%)100部に35%塩酸0.1部を加えて攪拌し、この分散液に氷水浴で冷却下メチルトリメトキシシラン136部、ジメチルジメトキシシラン20.3部を加えた。この混合液を25℃で6時間攪拌して得られた反応液に、硬化触媒およびpH調節剤として45%コリンメタノール溶液1部および酢酸4部を加えイソプロパノール200部で希釈してオルガノシロキサン樹脂組成物(HC−2)を調製した。
上記で製造された車輌用グレージング材の約1/2スケールの成形品を、130℃で1時間クリーンオーブン中でアニール処理を行った。その後上記で調整された第1層用アクリル樹脂組成物(HC−1)を液だまりができないようディップコート法によって両面塗布し、25℃で20分間静置後、130℃で1時間熱風循環オーブン中で熱硬化させ、4.0μmの膜厚の硬化膜を積層させた。次いで該成形品の被膜表面上に上記で調整された第2層用オルガノシロキサン樹脂組成物(HC−2)をディップコート法によって両面塗布し、25℃で20分間静置後、120℃で2時間熱風循環オーブン中で熱硬化させ、4.0μmの膜厚の硬化膜を積層させた。
(5−1)不均一な陰影の有無
ハードコート処理された成形品を2枚の直交する偏光板に挟み込み、その上面部分において観察される陰影の程度を下記の基準に基づき評価した(尚、いずれのサンプルも陰影は10個の成形品において同程度の観察された)。
○:陰影は、そのコントラストが比較的薄く、わずかに観察される
△:陰影は、そのコントラストがある程度強く、明確に観察される
×:陰影は、そのコントラストが強く、極めて明確かつ大面積にわたって観察される
ハードコート処理された板状成形品表面を太陽光の下、肉眼により観察し、クラックの発生の有無を評価した。10サンプル中のクラックのあるサンプル数nを“n/10”として表1に示す。
上記のハードコート処理された10個の成形品からそれぞれほぼ同様の位置から50mm角の試験片を切り出した。かかる試験片をスーパーキセノンテスト(UV照射強度180W/m2、ブラックパネル温度63℃)にて2,000時間の紫外線曝露処理を行い、該処理後の試験片の密着性の評価および外観(色相)の目視観察を行った。
密着性は、上記処理がされた後の角板のほぼ中央部において、ハードコート層にカッターナイフで1mm間隔の100個の碁盤目を作りニチバン製粘着テープ(商品名“セロテープ”)を圧着し、垂直に強く引き剥がして成形品上にすべて残るか否かを評価した。10枚の試験片中、剥がれのあった試験片数nを“n/10”として表1に示す。
外観は、処理前の成形品との色相の際を目視観察し、色相の相違がほとんど認められないものを○、認められるものを×として行った(今回の実施例および比較例ではいずれも色相の相違はほとんど認められなかった)。
上記のハードコート処理された成形品から50mm角の試験片を切り出した。ブラックパネル温度が80℃となるように設定された放射ピークの波長が約1000nmである近赤外線ハロゲンランプを用い、該ブラックパネルとハロゲンランプとの間にかかる試験片を設置したときのブラックパネルの温度(℃)を観察した。試験片はブラックパネルから50mm離れた位置に配置された。ブラックパネルの温度が低いほど熱線遮蔽効果が高いといえ、かかる温度を表1に示す(尚、同じサンプル間での試験片によるバラツキはほとんど認められなかった)。
上記のハードコート処理された成形品から50mm角の試験片を切り出した。その全光線透過率を(株)村上色彩技術研究所製ヘーズメーターHR−100を用いISO13468−1に準拠して測定した。結果を表1に示す。
102 稜線
103 ゲート
104 ノズル部
105 稜線
107 側周面
112 底面側周縁線
113 上面
Claims (9)
- (A)ポリカーボネート樹脂(A成分)100重量部、(B)La、Pr、Nd、Ce、Y、Ti、Zr、Hf、V、Nb、Ta、Cr、MoおよびWの群から選択される1種以上の金属のホウ化物からなる平均粒径2〜100nmの微粒子(B成分)0.0005〜0.03重量部、(C)ホスファイト化合物(C1成分)およびホスホナイト化合物(C2成分)から選択される少なくとも1種のリン化合物(C成分)0.0005〜0.3重量部、および紫外線吸収剤0.05〜3重量部からなるポリカーボネート樹脂組成物から射出成形により形成された成形品の表面にハードコート層を有するポリカーボネート樹脂成形体。
- 該ハードコート層は、下記式(i)および(ii)を満足する量の紫外線吸収剤を含有する層を有する請求項1に記載のポリカーボネート樹脂成形体。
式(i):0.1≦c≦0.5
式(ii):0.6≦d×c≦3
ここでcはハードコート層中のg/cm3で表される紫外線吸収剤の濃度であり、dは該紫外線吸収剤を含有する層のμmで表される厚みを表す。 - 紫外線吸収剤がベンゾフェノン系の紫外線吸収剤である請求項1または2のいずれかに記載のポリカーボネート樹脂成形体。
- 上記成形品は、その最大投影面積が500cm 2 以上である請求項1〜3のいずれか1項に記載のポリカーボネート樹脂成形体。
- 上記成形品は、その厚み(D(mm))に対するゲート部から流動末端までの距離(L(mm))の比L/Dが、75以上である請求項1〜4のいずれか1項に記載のポリカーボネート樹脂成形体。
- 上記ポリカーボネート樹脂組成物は、更に炭素フィラー(D成分)を、該樹脂組成物中0.1〜20ppm(重量割合)含有する請求項1〜5のいずれか1項に記載のポリカーボネート樹脂成形体。
- 上記A成分は粘度平均分子量が20,000〜30,000である請求項1〜6のいずれか1項に記載のポリカーボネート樹脂成形体。
- 上記ハードコート層は、上記射出成形された成形品の表面に第1層が形成され、第1層の表面に第2層が形成された構成のハードコート層であって、
第1層は、架橋したアクリル共重合体(アクリル共重合体−I)および紫外線吸収剤からなり、第2層は、架橋したオルガノシロキサン重合体からなり、
該架橋したアクリル共重合体(アクリル共重合体−I)は、50モル%以上の下記式(A−1)
で表される繰り返し単位、
5〜30モル%の下記式(A−2)
で表される繰り返し単位、および
0〜30モル%の下記式(A−3)
該架橋したオルガノシロキサン重合体は、下記式(b−4)〜(b−6)
で表される繰り返し単位からなり、該繰り返し単位の全量を100モル%としたとき、式(b−4):80〜100モル%、式(b−5):0〜20モル%、および式(b−6):0〜20モル%である架橋したオルガノシロキサン重合体である、ハードコート層である請求項1〜7のいずれか1項に記載のポリカーボネート樹脂成形体。 - 上記成形体は、曲面部を有する車輌用グレージング材である請求項1〜8のいずれか1項に記載のポリカーボネート樹脂成形体。
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JP2002060528A (ja) * | 2000-08-17 | 2002-02-26 | Teijin Chem Ltd | ポリカーボネート樹脂組成物成形体 |
JP2002338719A (ja) * | 2001-05-16 | 2002-11-27 | Teijin Chem Ltd | 表面を保護された透明プラスチック成形体 |
JP2003327717A (ja) * | 2002-05-13 | 2003-11-19 | Sumitomo Metal Mining Co Ltd | 熱線遮蔽樹脂シート材及びその製造用添加液 |
JP2003342403A (ja) * | 2002-05-27 | 2003-12-03 | Teijin Chem Ltd | 表面を保護された透明プラスチック成形体 |
JP2004027109A (ja) * | 2002-06-27 | 2004-01-29 | Teijin Chem Ltd | ハードコート層を有するポリカーボネート樹脂成形体 |
JP2005161919A (ja) * | 2003-12-01 | 2005-06-23 | Teijin Chem Ltd | 車両用合わせ窓 |
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2003
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JPS57162729A (en) * | 1981-03-30 | 1982-10-06 | Mitsubishi Gas Chem Co Inc | Preparation of molded article of polycarbonate resin having improved wear resistance |
JP2000096034A (ja) * | 1998-09-22 | 2000-04-04 | Sumitomo Metal Mining Co Ltd | 日射遮蔽材料、日射遮蔽膜用塗布液、及び、日射遮蔽膜 |
JP2002060527A (ja) * | 2000-08-11 | 2002-02-26 | Teijin Chem Ltd | ポリカーボネート樹脂組成物成形体 |
JP2002060528A (ja) * | 2000-08-17 | 2002-02-26 | Teijin Chem Ltd | ポリカーボネート樹脂組成物成形体 |
JP2002338719A (ja) * | 2001-05-16 | 2002-11-27 | Teijin Chem Ltd | 表面を保護された透明プラスチック成形体 |
JP2003327717A (ja) * | 2002-05-13 | 2003-11-19 | Sumitomo Metal Mining Co Ltd | 熱線遮蔽樹脂シート材及びその製造用添加液 |
JP2003342403A (ja) * | 2002-05-27 | 2003-12-03 | Teijin Chem Ltd | 表面を保護された透明プラスチック成形体 |
JP2004027109A (ja) * | 2002-06-27 | 2004-01-29 | Teijin Chem Ltd | ハードコート層を有するポリカーボネート樹脂成形体 |
JP2005161919A (ja) * | 2003-12-01 | 2005-06-23 | Teijin Chem Ltd | 車両用合わせ窓 |
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