JPWO2017038580A1 - 熱可塑性ポリエステル樹脂組成物、およびこれを用いた光反射体 - Google Patents
熱可塑性ポリエステル樹脂組成物、およびこれを用いた光反射体 Download PDFInfo
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- JPWO2017038580A1 JPWO2017038580A1 JP2016563859A JP2016563859A JPWO2017038580A1 JP WO2017038580 A1 JPWO2017038580 A1 JP WO2017038580A1 JP 2016563859 A JP2016563859 A JP 2016563859A JP 2016563859 A JP2016563859 A JP 2016563859A JP WO2017038580 A1 JPWO2017038580 A1 JP WO2017038580A1
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- DPNUIZVZBWBCPB-UHFFFAOYSA-J titanium(4+);tetraphenoxide Chemical compound [Ti+4].[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1 DPNUIZVZBWBCPB-UHFFFAOYSA-J 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- XWKBMOUUGHARTI-UHFFFAOYSA-N tricalcium;diphosphite Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])[O-].[O-]P([O-])[O-] XWKBMOUUGHARTI-UHFFFAOYSA-N 0.000 description 1
- VMFOHNMEJNFJAE-UHFFFAOYSA-N trimagnesium;diphosphite Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])[O-].[O-]P([O-])[O-] VMFOHNMEJNFJAE-UHFFFAOYSA-N 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- CNUJLMSKURPSHE-UHFFFAOYSA-N trioctadecyl phosphite Chemical compound CCCCCCCCCCCCCCCCCCOP(OCCCCCCCCCCCCCCCCCC)OCCCCCCCCCCCCCCCCCC CNUJLMSKURPSHE-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- MGMXGCZJYUCMGY-UHFFFAOYSA-N tris(4-nonylphenyl) phosphite Chemical compound C1=CC(CCCCCCCCC)=CC=C1OP(OC=1C=CC(CCCCCCCCC)=CC=1)OC1=CC=C(CCCCCCCCC)C=C1 MGMXGCZJYUCMGY-UHFFFAOYSA-N 0.000 description 1
- QQBLOZGVRHAYGT-UHFFFAOYSA-N tris-decyl phosphite Chemical compound CCCCCCCCCCOP(OCCCCCCCCCC)OCCCCCCCCCC QQBLOZGVRHAYGT-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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- B29D11/00—Producing optical elements, e.g. lenses or prisms
- B29D11/0074—Production of other optical elements not provided for in B29D11/00009- B29D11/0073
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
- B29K2067/006—PBT, i.e. polybutylene terephthalate
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Abstract
Description
[1]
100〜50質量部のポリブチレンテレフタレート樹脂(A)と0〜50質量部のポリエチレンテレフタレート樹脂(B)とを含有する樹脂組成物であって、該樹脂組成物が含有する全ポリエステル樹脂100質量部あたり1〜20質量部の平均粒子径0.05〜2μmである表面処理された炭酸カルシウム(C)と0.05〜3質量部の多官能グリシジル基含有スチレン系ポリマー(D)とを含有する、熱可塑性ポリエステル樹脂組成物。
[2]
前記(C)成分の表面処理が、シリカ処理、エポキシシランカップリング剤処理、およびアルキルシランカップリング剤処理から選ばれるいずれか1種または2種以上である、[1]に記載の熱可塑性ポリエステル樹脂組成物。
[3]
前記(C)成分の表面処理が、シリカ処理、シリカ処理とエポキシシランカップリング剤処理の複合処理、シリカ処理とアルキルシランカップリング剤処理の複合処理、のいずれかである、[1]に記載の熱可塑性ポリエステル樹脂組成物。
[4]
全ポリエステル樹脂100質量部あたり0.01〜5質量部のリン化合物(E)を含有する、[1]〜[3]のいずれかに記載の熱可塑性ポリエステル樹脂組成物。
[5]
前記ポリブチレンテレフタレート樹脂(A)が、チタン原子含有量が60ppm以下のポリブチレンテレフタレート樹脂である、[1]〜[4]のいずれかに記載の熱可塑性ポリエステル樹脂組成物。
[6]
前記ポリエチレンテレフタレート樹脂(B)が、酸価が30eq/ton以下のポリエチレンテレフタレート樹脂である、[1]〜[5]のいずれかに記載の熱可塑性ポリエステル樹脂組成物。
[7]
[1]〜[6]のいずれかに記載の熱可塑性ポリエステル樹脂組成物からなる光反射体用部品。
[8]
[7]に記載の光反射体用部品の表面の少なくとも一部に、光反射金属層が直接形成されている光反射体。
[9]
[1]〜[6]のいずれかに記載の熱可塑性ポリエステル樹脂組成物を、内面の少なくとも一部が鏡面である金型内に射出して成形する工程を含む、光反射体用部品の製造方法。
[10]
少なくとも、ポリブチレンテレフタレート樹脂(A)と、ポリエチレンテレフタレート樹脂(B)と、平均粒子径0.05〜2μmである表面処理された炭酸カルシウム(C)と、多官能グリシジル基含有スチレン系ポリマー(D)とを溶融混練する工程を有する熱可塑性ポリエステル樹脂組成物の製造方法であって、(B)の配合比率は(A)100〜50質量部に対して(B)0〜50質量部であり、(C)(D)の配合比率は該樹脂組成物が含有する全ポリエステル樹脂100質量部あたり(C)1〜20質量部かつ(D)0.05〜3質量部である、熱可塑性ポリエステル樹脂組成物の製造方法。
[11]
前記ポリブチレンテレフタレート樹脂(A)としてチタン原子含有量が60ppm以下であるポリブチレンテレフタレート樹脂を用いることを特徴とする[10]に記載の熱可塑性ポリエステル樹脂組成物の製造方法。
[12]
前記ポリエチレンテレフタレート樹脂(B)として酸価が30eq/ton以下であるポリエチレンテレフタレート樹脂を用いることを特徴とする[10]または[11]に記載の熱可塑性ポリエステル樹脂組成物の製造方法。
本発明におけるポリブチレンテレフタレート樹脂(A)は、テレフタル酸あるいはそのエステル形成性誘導体と、1,4−ブタンジオールあるいはそのエステル形成性誘導体とを主成分とし重縮合反応させる等の一般的な重合方法によって得られる重合体である。ブチレンテレフタレート繰返し単位が80モル%以上の重合体であることが好ましく、90モル%以上がより好ましく、95モル%以上がさらに好ましく、100モル%が最も好ましい。特性を損なわない範囲、例えば20質量%程度以下の他の共重合成分を含んでも良い。ポリブチレンテレフタレート樹脂(A)として用いることのできる共重合体の例としては、ポリブチレン(テレフタレート/イソフタレート)、ポリブチレン(テレフタレート/アジペート)、ポリブチレン(テレフタレート/セバケート)、ポリブチレン(テレフタレート/デカンジカルボキシレート)、ポリブチレン(テレフタレート/ナフタレート)、ポリ(ブチレン/エチレン)テレフタレート等が挙げられる。ポリブチレンテレフタレート樹脂(A)は、単独の樹脂からなるものであっても、2種以上の樹脂の混合物であっても良い。
表面処理の前後で、炭酸カルシウム(C)の平均粒子径は実質的には変化しないが、本発明では、表面処理された炭酸カルシウム(C)の平均粒子径は、表面処理後の炭酸カルシウム(C)の平均粒子径を指す。
多官能グリシジル基含有スチレン系ポリマー(D)をこの範囲にすることで、ポリエステルのオリゴマー、モノマー、および遊離有機カルボン酸等のガス化成分を効率的に捕捉することができ、優れた低ガス性を実現できる。
多官能グリシジル基含有スチレン系ポリマー(D)の具体的な成分としては、グリシジル基含有不飽和単量体とビニル芳香族系単量体との共重合体が好ましい。
グリシジル基含有不飽和単量体の共重合量が、1質量%未満ではポリエステル樹脂のオリゴマー、モノマー、および遊離有機カルボン酸等の捕捉効果が小さくなり、低ガス性に悪影響を及ぼす傾向がある。30質量%を超えると樹脂組成物としての安定性が損なわれる場合がある。
ウベローデ型粘度計を使用し、フェノール/テトラクロロエタン(質量比1/1)の混合溶媒を使用し、30℃において測定した。
電子工業用高純度硫酸および電子工業用高純度硝酸でポリブチレンテレフタレートを湿式分解し、高分解能ICP(Inductively Coupled Plasma)−MS(Mass Spectrometer )(サーモクエスト社製)を使用して測定した。
ベンジルアルコール25mlにポリブチレンテレフタレート0.5gを溶解し、水酸化ナトリウムの0.01モル/l ベンジルアルコール溶液を使用して滴定した。指示薬はフェノールフタレイン0.10gをエタノール50mL及び水50mLの混合液に溶解したものを使用した。
ポリブチレンテレフタレートおよびポリエチレンテレフタレートのOH価の定量は共鳴周波数500MHzの1H−NMR測定にて行った。測定装置はBRUKER社製NMR装置AVANCE−500を用い、測定液の調製方法は以下の通りに行った。
試料10mgを重クロロホルム/ヘキサフルオロイソプロパノール=1/1(体積比)0.12mlに溶解後、重クロロホルム0.48mlおよび重ピリジン5μlを加え、よく撹拌した後、その溶液をNMRチューブに充填し1H−NMR測定を行った。
ロック溶媒には重クロロホルムを用い、積算回数は128回とした。
OH価定量は以下の通り実施した。
クロロホルムのピークを7.29ppmとしたとき、8.10ppmのピークがポリブチレンテレフタレートまたはポリエチレンテレフタレート由来のテレフタル酸ピーク(A)である。更にポリブチレンテレフタレート樹脂の場合は3.79ppmに末端の1,4−ブタンジオールピーク(B)が検出される。ポリエチレンテレフタレート樹脂の場合は、4.03ppmに末端のエチレングリコールピーク(C)、括弧内のA〜Cを各ピークの積分値とし、OH価を下記式より求めた。
ポリブチレンテレフタレート樹脂の場合:(B×1000000/2)/(A×220/4)=OH価(eq/ton)
ポリエチレンテレフタレート樹脂の場合:(C×1000000/2)/(A×192/4)=OH価(eq/ton)
検討したフィラーの平均粒子径は、電子顕微鏡像から粒子径を算出する電子顕微鏡法にて求めた。下記には走査型電子顕微鏡(SEM)像より算出する方法を示すが、透過型電子顕微鏡(TEM)像も利用でき、とくに限定されない。
試料の調整方法は以下の通りである。ビーカー(100ml)に無機フィラー3gとメタノール溶媒60gを加え懸濁させ、超音波分散機US−300AT(日本精機製作所製)を使用し、300μAで1分間の一定条件で予備分散した。次に、0.5mlのスポイトを用い試料台に薄く均一に載せ、乾燥し試料を調整した。
調整した試料をSEMにて100〜500個数カウントできる倍率で観察した後、画像解析式粒子径解析ソフトImageJ(オープンソース)を用い、100〜500個の粒子を端から順番にカウントし、平均粒子径を算出した。
射出成形機EC100N(東芝機械社製)を用いて成形した100mm×100mm×2mm厚みの平板成形品をダイヤモンドカッターまたはガラスカッターにて切断して断面を作製し、断面のSEM写真により、凝集物の有無を目視判定した。
◎:凝集物なし、 ○:凝集物があるが、わずかである、 △:凝集物が散見できる、 ×:凝集物が多い
射出成形機EC100N(東芝機械社製)を用い、#6000番のやすりで磨かれた鏡面を片面に有する金型を用いて、100mm×100mm×2mm厚みの平板成形品を射出成形した。成形はシリンダー温度260℃、金型温度60℃、サイクルタイム40秒であり、表面にフィラー浮きが起こりやすい低速の射出速度で実施した。成形品の鏡面を、フィラーの浮きによる不良(白化、表面の荒れ)がないか目視により評価した。
◎:白化、表面の荒れが認められない。
○:白化、表面の荒れが目視の角度によりわずかに認められるが、実用上問題ない程度である。
△:白化、表面の荒れが認められる。
×:白化、表面の荒れが極めて目立つ。
射出成形機EC100N(東芝機械社製)を用いて成形した成形品から30mm×30mm程度の大きさの小片を切り出し、その合計10gを、アルミ箔を被せて底を作製したガラス筒(φ65×80mm)にいれ、ホットプレート(ネオホットプレートHT−1000、アズワン社製)上にセットした。さらに、上記ガラス筒にスライドガラスで蓋をした後ホットプレート設定温度180℃で24時間、熱処理を実施した。この熱処理の結果、スライドガラス内壁には樹脂組成物より昇華した分解物などによる付着物が析出した。これらのスライドガラスのHAZE値(曇り度%)を、ヘイズメーターNDH2000(日本電色工業社製)を用いて測定した。
射出成形機EC100N(東芝機械社製)を用い、金型として、連続成形評価型(外径30mm、内径20mm、厚み3mmのキャビティを有し、流動末端は凹部でガス抜きはない。)を用い、ゲート部反対側の凹部にオリゴマーなどの含有物が蓄積しやすいようにショートショット法で連続成形し、金型汚れを観察した。成形時のシリンダー温度は、260℃で、金型温度60℃、サイクルタイム40秒で成形し、20ショット後の金型汚れにて評価した。金型汚れはデジタルカメラにて撮影し、色の均一化のため、グレースケール処理を実施後、評価した。
◎:汚れが認められない。
○:ほとんど汚れが認められない。
△:ゲート部反対側の凹部付近の中心に汚れがぼんやりと認められる。
×:ゲート部反対側の凹部付近の中心の汚れがはっきりとした輪郭で黒く目立つ。
(A)ポリブチレンテレフタレート樹脂;
(A−1)ポリブチレンテレフタレート樹脂:IV=0.82dl/g、酸価=10eq/ton、OH価=100eq/ton、チタン含有量30ppm、
(A−2)ポリブチレンテレフタレート樹脂:IV=1.04dl/g、酸価=23eq/ton、OH価=43eq/ton、チタン含有量40ppm
(A−3)ポリブチレンテレフタレート樹脂:IV=0.83dl/g、酸価=30eq/ton、OH価=80eq/ton、チタン含有量80ppm
(B)ポリエチレンテレフタレート樹脂;
(B−1)ポリエチレンテレフタレート樹脂:IV=0.62dl/g、酸価=30eq/ton、OH価=60eq/ton
(C−1)軽質炭酸カルシウム(シリカ処理、平均粒子径0.15μm[電子顕微鏡法]):RK−87BR2F(白石工業社製)
(C−2)軽質炭酸カルシウム(シリカ/エポキシシランカップリング剤処理、平均粒子径0.15μm[電子顕微鏡法]):RK−92BR3F(白石工業社製)
(C−3)軽質炭酸カルシウム(シリカ/アルキルシランカップリング剤処理、平均粒子径0.15μm[電子顕微鏡法]):RK−82BR1F(白石工業社製)
(C−4)軽質炭酸カルシウム(酸による中和処理、平均粒子径0.15μm[電子顕微鏡法]):RK−75NC(白石工業社製)
(C−5)軽質炭酸カルシウム(脂肪酸処理、平均粒子径0.15μm[電子顕微鏡法]):Vigot−10(白石工業社製)
(C−6)軽質炭酸カルシウム(表面処理なし、平均粒子径0.15μm[電子顕微鏡法]):Brilliant−1500(白石工業社製)
(C−7)軽質炭酸カルシウム(表面処理なし、平均粒子径0.04μm[電子顕微鏡法]):NPCC−201(長瀬産業社製)
(C−8)重質炭酸カルシウム(表面処理なし、平均粒子径:4.2μm[レーザー回折法、粒度分布50%]、平均粒子径はカタログ値を採用した):KS−1000(林化成社製)
(C−9)軽質炭酸カルシウム(シランカップリング処理、平均粒子径3.0μm[電子顕微鏡法]):SL−101(白石工業社製)
(C−10)焼成カオリン(表面処理なし、平均粒子径0.8μm[電子顕微鏡法]):SATINTONE−5HB(林化成社製)
(D−1)ARUFON UG−4050(東亜合成社製、Mw:8500、エポキシ価0.67meq/g、屈折率1.55)
(D−2)ARUFON UG−4070(東亜合成社製、Mw:9700、エポキシ価1.4meq/g、屈折率1.57)
(E)リン系化合物;
(E−1)アデカスタブPEP−36(ADEKA社製)
(E−2)アデカスタブCDA−6(ADEKA社製)
トリグリセリンフルベヘン酸エステル:ポエムTR−FB(理研ビタミン社製)
安定剤;
酸化防止剤:Irganox1010(BASF社製)
表1、表2に示した配合成分に、さらに離型剤としてポエムTR−FBを0.3質量部、酸化防止剤としてIrganox1010を0.2質量部加えて、シリンダー温度260℃に設定した同方向二軸押出機で溶融混練を行い、得られたストランドを水冷し、ペレット化した。得られた各ペレットを130℃で4時間乾燥し、上述の各評価試験に用いた。結果を表1、表2に記す。
Claims (12)
- 100〜50質量部のポリブチレンテレフタレート樹脂(A)と0〜50質量部のポリエチレンテレフタレート樹脂(B)とを含有する樹脂組成物であって、該樹脂組成物が含有する全ポリエステル樹脂100質量部あたり1〜20質量部の平均粒子径0.05〜2μmである表面処理された炭酸カルシウム(C)と0.05〜3質量部の多官能グリシジル基含有スチレン系ポリマー(D)とを含有する、熱可塑性ポリエステル樹脂組成物。
- 前記(C)成分の表面処理が、シリカ処理、エポキシシランカップリング剤処理、およびアルキルシランカップリング剤処理から選ばれるいずれか1種または2種以上である、請求項1に記載の熱可塑性ポリエステル樹脂組成物。
- 前記(C)成分の表面処理が、シリカ処理、シリカ処理とエポキシシランカップリング剤処理の複合処理、シリカ処理とアルキルシランカップリング剤処理の複合処理、のいずれかである、請求項1に記載の熱可塑性ポリエステル樹脂組成物。
- 全ポリエステル樹脂100質量部あたり0.01〜5質量部のリン化合物(E)を含有する、請求項1〜3のいずれかに記載の熱可塑性ポリエステル樹脂組成物。
- 前記ポリブチレンテレフタレート樹脂(A)が、チタン原子含有量が60ppm以下のポリブチレンテレフタレート樹脂である、請求項1〜4のいずれかに記載の熱可塑性ポリエステル樹脂組成物。
- 前記ポリエチレンテレフタレート樹脂(B)が、酸価が30eq/ton以下のポリエチレンテレフタレート樹脂である、請求項1〜5のいずれかに記載の熱可塑性ポリエステル樹脂組成物。
- 請求項1〜6のいずれかに記載の熱可塑性ポリエステル樹脂組成物からなる光反射体用部品。
- 請求項7に記載の光反射体用部品の表面の少なくとも一部に、光反射金属層が直接形成されている光反射体。
- 請求項1〜6のいずれかに記載の熱可塑性ポリエステル樹脂組成物を、内面の少なくとも一部が鏡面である金型内に射出して成形する工程を含む、光反射体用部品の製造方法。
- 少なくとも、ポリブチレンテレフタレート樹脂(A)と、ポリエチレンテレフタレート樹脂(B)と、平均粒子径0.05〜2μmである表面処理された炭酸カルシウム(C)と、多官能グリシジル基含有スチレン系ポリマー(D)とを溶融混練する工程を有する熱可塑性ポリエステル樹脂組成物の製造方法であって、(B)の配合比率は(A)100〜50質量部に対して(B)0〜50質量部であり、(C)、(D)の配合比率は該樹脂組成物が含有する全ポリエステル樹脂100質量部あたり(C)1〜20質量部かつ(D)0.05〜3質量部である、熱可塑性ポリエステル樹脂組成物の製造方法。
- 前記ポリブチレンテレフタレート樹脂(A)としてチタン原子含有量が60ppm以下であるポリブチレンテレフタレート樹脂を用いることを特徴とする請求項10に記載の熱可塑性ポリエステル樹脂組成物の製造方法。
- 前記ポリエチレンテレフタレート樹脂(B)として酸価が30eq/ton以下であるポリエチレンテレフタレート樹脂を用いることを特徴とする請求項10または11に記載の熱可塑性ポリエステル樹脂組成物の製造方法。
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