JP6673704B2 - 制振材用熱可塑性重合体組成物、成形体の製造方法、および成形体 - Google Patents
制振材用熱可塑性重合体組成物、成形体の製造方法、および成形体 Download PDFInfo
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- JP6673704B2 JP6673704B2 JP2016014590A JP2016014590A JP6673704B2 JP 6673704 B2 JP6673704 B2 JP 6673704B2 JP 2016014590 A JP2016014590 A JP 2016014590A JP 2016014590 A JP2016014590 A JP 2016014590A JP 6673704 B2 JP6673704 B2 JP 6673704B2
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Description
[1]4−メチル−1−ペンテンから導かれる構成単位(A−i)および4−メチル−1−ペンテンを除く炭素原子数2〜20のα−オレフィンから選ばれる少なくとも1種以上のα−オレフィンから導かれる構成単位(A−ii)を含み、任意に非共役ポリエンから導かれる構成単位(A−iii)を含んでもよい4−メチル−1−ペンテン・α−オレフィン共重合体であって、構成単位(A−i)、(A−ii)および(A−iii)の合計を100モル%としたときに、構成単位(A−i)を63〜86モル%、構成単位(A−ii)を14〜37モル%、構成単位(A−iii)を0〜10モル%含む、4−メチル−1−ペンテン・α−オレフィン共重合体(A)と、
エチレンから導かれる構成単位(B−i)、炭素原子数3〜20のα−オレフィンから導かれる構成単位(B−ii)、および非共役ポリエンから導かれる構成単位(B−iii)を含む共重合体[B−I]とポリオレフィン樹脂[B−II]とを含む混合物を動的架橋して得られる熱可塑性エラストマー組成物(B)とを含有し、
前記4−メチル−1−ペンテン・α−オレフィン共重合体(A)と前記熱可塑性エラストマー組成物(B)の質量比(A)/(B)が10/90〜49/51であり、
損失正接tanδの値が最大となる温度が15℃以上40℃以下であることを特徴とする制振材用熱可塑性重合体組成物。
[2]前記4−メチル−1−ペンテン・α−オレフィン共重合体(A)は、前記構成単位(A−i)、(A−ii)および(A−iii)の合計を100モル%としたときに、前記構成単位(A−i)を63〜80モル%、前記構成単位(A−ii)を20〜37モル%、前記構成単位(A−iii)を0〜10モル%含む4−メチル−1−ペンテン・α−オレフィン共重合体である[1]に記載の制振材用熱可塑性重合体組成物。
[3]上記4−メチル−1−ペンテン・α−オレフィン共重合体(A)は、融点が観測されないか、もしくは融点が135℃未満の共重合体であることを特徴とする、[1]または[2]に記載の制振材用熱可塑性重合体組成物。
[4]上記4−メチル−1−ペンテン・α−オレフィン共重合体(A)は、融点が観測されないか、もしくは110℃未満の共重合体であることを特徴とする、[1]〜[3]の何れかに記載の制振材用熱可塑性重合体組成物。
[5]損失正接tanδの値が最大となる温度が0℃以上40℃以下の共重合体であることを特徴とする、[1]〜[4]の何れかに記載の制振材用熱可塑性重合体組成物。
[6][1]〜[5]の何れかに記載の制振材用熱可塑性重合体組成物を成形する工程を含む、成形体の製造方法。
[7]前記成形体は制振部材である、[6]に記載の製造方法。
[8]前記成形体は衝撃吸収材である、[6]に記載の製造方法。
[9]前記成形体は振動吸収材である、[6]に記載の製造方法。
[10]前記成形体は共振吸収材である、[6]に記載の製造方法。
[11][1]〜[5]の何れかに記載の制振材用熱可塑性重合体組成物を含む成形体。
[12]制振部材である、[11]に記載の成形体。
[13]衝撃吸収材である、[11]に記載の成形体。
[14]振動吸収材である、[11]に記載の成形体。
[15]共振吸収材である、[11]に記載の成形体。
本発明の制振材用熱可塑性重合体組成物(以下、単に「本発明の組成物」ともいう。)は、4−メチル−1−ペンテン・α−オレフィン共重合体(A)(以下、単に「共重合体(A)」ともいう。)と、熱可塑性エラストマー組成物(B)(以下、単に「組成物(B)」ともいう。)とを含有する。
なお、上記ΔHSは、以下の式に従って求められる値である。
ΔHS=(押針接触開始直後のショアーA硬度値−押針接触開始から15秒後のショアーA硬度値)
なお、上記ΔHSは、以下の式に従って求められる値である。
共重合体(A)は、4−メチル−1−ペンテンから導かれる構成単位(A−i)(以下、単に「構成単位(A−i)ともいう。」)、および4−メチル−1−ペンテンを除く炭素原子数2〜20のα−オレフィンから選ばれる少なくとも1種以上のα−オレフィンから導かれる構成単位(A−ii)(以下、単に「構成単位(A−ii)ともいう。」)を含み、任意に非共役ポリエンから導かれる構成単位(A−iii)(以下、単に「構成単位(A−iii)ともいう。」)を含んでもよい4−メチル−1−ペンテン・α−オレフィン共重合体である。本発明の効果が奏される限りにおいて、共重合体(A)は、上記以外の構成単位(以下、単に「他の構成単位」ともいう。)を含んでいてもよい。
ΔHS=(押針接触開始直後のショアーA硬度値−押針接触開始から15秒後のショアーA硬度値)
共重合体(A)の製造方法は、特に限定されないが、例えば4−メチル−1−ペンテンと上述した「構成単位(ii)を導くモノマー」とを適当な重合触媒存在下で重合することにより得ることができる。ここで、本発明で用いることのできる重合触媒として、従来公知の触媒、例えばマグネシウム担持型チタン触媒、国際公開第01/53369号、国際公開第01/27124号、特開平3−193796号公報あるいは特開平02−41303号公報中に記載のメタロセン触媒などが好適に用いられ、さらに好ましくは、下記一般式(1)または(2)で表されるメタロセン化合物を含有するオレフィン重合触媒が好適に用いられる。
Mは周期表第4族から選ばれた金属であり、
Yは炭素またはケイ素であり、
Qはハロゲン、炭化水素基、およびアニオン配位子または孤立電子対で配位可能な中性配位子から同一のまたは異なる組合せで選ばれ、
jは1〜4の整数である。
上記一般式(1)または(2)のR1、R2、R3、R4、R5、R6、R7、R8、R9、R10、R11、R12、R13およびR14は、水素、炭化水素基およびケイ素含有炭化水素基から選ばれ、それぞれ同一でも異なっていてもよい。
(a)メタロセン化合物(たとえば、上記一般式(1),(2)または[I]で表されるメタロセン化合物)と、
(b)(b−1)有機アルミニウムオキシ化合物、(b−2)メタロセン化合物(a)と反応してイオン対を形成する化合物、および(b−3)有機アルミニウム化合物から選ばれる少なくとも1種の化合物と、
さらに必要に応じて、
(c)微粒子状担体と
から構成される。製造方法としては、たとえば国際公開第01/27124号に記載の方法を採用することが出来る。
組成物(B)は、エチレンから導かれる構成単位(B−i)、炭素原子数3〜20のα−オレフィンから導かれる構成単位(B−ii)、および非共役ポリエンから導かれる構成単位(B−iii)を含む共重合体(B−I)とポリオレフィン樹脂(B−II)とを含む混合物を動的架橋して得られる熱可塑性エラストマー組成物である。組成物(B)は、本発明の効果が奏される限りにおいて、上記共重合体(B−I)およびポリオレフィン樹脂(B−II)以外の成分を含んでもよい。
共重合体(B−I)は、エチレンから導かれる構成単位(B−i)、炭素原子数3〜20のα−オレフィンから導かれる構成単位(B−ii)、および非共役ポリエンから導かれる構成単位(B−iii)を含むエチレン・α−オレフィン・非共役ポリエン共重合体である。
ポリオレフィン樹脂(B−II)は、α―オレフィンの単独重合体またはα―オレフィンを含む共重合体である。上記α―オレフィンの例には、エチレン、プロピレン、1−ブテン、1−ペンテン、1−ヘキセン、4−メチル−1−ペンテン、1−オクテン、および1−デセンが含まれる。上記共重合体は、最もモル量が多いα−オレフィンの含有量が90モル%以上である共重合体である。
プロピレン系重合体は、プロピレンの単独重合体、プロピレンと他のαーオレフィンとのランダム共重合体、または、プロピレンの単独重合体と非晶性もしくは低結晶性のプロピレン・エチレンランダム共重合体とのブロック共重合体である。上記他のαーオレフィンの例には、エチレン、1−ブテン、1−ペンテンおよび4−メチル−1−ペンテンが含まれる。プロピレン系重合体における上記他のαーオレフィンの量は、10モル%以下であることが好ましい。
プロピレン系重合体は、公知の方法で上記成分を重合させて製造することができる。
上記架橋例の例には、有機過酸化物、イオウ、イオウ化合物、およびフェノール樹脂を含むフェノール系加硫剤が含まれる。
架橋助剤は、架橋点を均一に形成させ、かつ、急激な反応を生じにくくすることができる。
軟化剤は、動的架橋時の材料の流動性を高め、組成物(B)の硬度を所望の程度に調整することができる。
組成物(B)および組成物(B)を製造するための前記混合物は、本発明の効果が奏される限りにおいて、スリップ剤、核剤、充填剤、酸化防止剤、耐候安定剤、着色剤、および発泡剤を含むその他の成分をさらに含有してもよい。
組成物(B)は、共重合体(B−I)とポリオレフィン樹脂(B−II)とを含む混合物を、前記架橋剤の存在下、または前記架橋剤および前記架橋助剤の存在下に、動的架橋させて製造することができる。上記混合物における共重合体(B−I)とポリオレフィン樹脂(B−II)との質量比[(B−I)/(B−II)]は、90/10〜5/95とすることができ、70/30〜10/90とすることが好ましい。
本発明の制振材用熱可塑性重合体組成物には、共重合体(A)の優れた特性を損なわない範囲で、その他の樹脂(C)を添加してもよい。添加量は、組成物を 一般的には50重量%以下、好ましくは40重量%以下である。その他の樹脂(C)の例としては、共重合体(A)以外のオレフィン系重合体、ポリエステル、ポリアミド、変性オレフィン系重合体等が挙げられる。
本発明の樹脂組成物には、その用途に応じて、本発明の効果を阻害しない範囲で他の樹脂用添加剤を任意に添加することができる。かかる樹脂用添加剤としては、例えば、顔料、染料、充填剤、滑剤、可塑剤、離型剤、酸化防止剤、難燃剤、紫外線吸収剤、抗菌剤、界面活性剤、帯電防止剤、耐候安定剤、耐熱安定剤、スリップ防止剤、アンチブロッキング剤、発泡剤、発泡助剤、結晶化助剤、防曇剤、(透明)核剤、老化防止剤、塩酸吸収剤、衝撃改良剤、架橋剤、共架橋剤、架橋助剤、粘着剤、軟化剤、加工助剤などが挙げられる。これらの添加剤は、1種単独でも、適宜2種以上を組み合わせても用いることができる。
本発明の組成物は、たとえば、共重合体(A)と組成物(B)とを公知の方法で機械的に混合する方法で製造することができる。上記混合した後、押出機を用いて混合物を溶融混練してもよい。
本発明の組成物は、公知の成形方法により、本発明の組成物を含む成形体とすることができる。
本発明の熱可塑性重合体組成物の成形体の使用し得る自動車部品としては、例えば、ウェザーストリップ、天井材、バンパーモール、サイドモール、エアスポイラー、エアダクトホース、カップホルダー、サイドブレーキグリップ、シフトノブカバー、シート調整ツマミ、フラッパードアシール、ワイヤーハーネスグロメット、ラックアンドピニオンブーツ、サスペンションカバーブーツ、ガラスガイド、インナーベルトラインシール、ルーフガイド 、トランクリッドシール、モールデッドクォーターウィンドガスケット、コーナーモールディング、グラスエンキャプシュレーション、フードシール、グラスランチャンネル、セカンダリーシール、各種パッキン類、バンパー部品、ボディパネル、サイドシールド、グラスランチャンネル、ウェザーストリップ材、ホース、ステアリングホイール、ブーツ、ワイヤーハーネスカバー、シートアジャスターカバー等を例示できる。
本発明の熱可塑性重合体組成物成形体の使用し得る土木・建材用品としては、例えば、地盤改良用シート、上水板、騒音振動防止壁等の土木資材や建材、土木・建築用各種ガスケットおよびシート、止水材、目地材、建築用窓枠、電気ドリル等の回転機器に使われる振動抑制用グリップ材などを例示できる。
本発明の熱可塑性重合体組成物成形体の使用し得る衛生用品としては、例えば、生理用品、使い捨ておむつ、歯ブラシ用グリップ等の衛生用品などを例示できる。
実施例における物性の測定条件等は、以下のとおりである。
4−メチル−1−ペンテン・α−オレフィン共重合体(A)中の4−メチル−1−ペンテンおよびα−オレフィン含量は、13C−NMRにより以下の装置および条件により測定した。日本電子株式会社製のECP500型核磁気共鳴装置を用い、溶媒としてオルトジクロロベンゼン/重ベンゼン(80/20容量%)混合溶媒,試料濃度55mg/0.6mL、測定温度120℃、観測核は13C(125MHz)、シーケンスはシングルパルスプロトンデカップリング、パルス幅は4.7μ秒(45°パルス)、繰り返し時間は5.5秒、積算回数は1万回以上、27.50ppmをケミカルシフトの基準値として測定した。
共重合体(A)の密度は、ASTM D 1505(水中置換法)に従って、ALFA MIRAGE社電子比重計MD−300Sを用い、水中と空気中で測定された各試料の重量から算出した。
共重合体(A)の極限粘度[η]は,デカリン溶媒を用いて135℃で測定した。
共重合体(A)の分子量は、液体クロマトグラフ:Waters製ALC/GPC 150−C plus型(示唆屈折計検出器一体型)を用い、カラムとして東ソー株式会社製GMH6−HT×2本およびGMH6−HTL×2本を直列接続し、移動相媒体としてo−ジクロロベンゼンを用い、流速1.0ml/分、140℃で測定した。
共重合体(A)の融点(Tm)は,セイコーインスツルメンツ社製DSC220C装置で示差走査熱量計(DSC)により測定した。重合から得られた試料7〜12mgをアルミニウムパン中に密封し、室温から10℃/分で200℃まで加熱した。その試料を、完全融解させるために200℃で5分間保持し、次いで10℃/分で−50℃まで冷却した。−50℃で5分間置いた後、その試料を10℃/分で200℃まで再度加熱した。この再度の(2度目の)加熱での吸熱曲線で高温側のピーク温度を、融点(Tm)として採用した。
共重合体(A)および組成物のショアーA硬度は、厚み2mmに成形したシート状の組成物を打抜き、この打抜いたシート状の組成物を3枚積み重ねて硬度測定用の試験片とし、この試験片について、JIS K6253(2006)「加硫ゴム及び熱可塑性ゴム−硬さの求め方」の6項の「デュロメーター硬さ試験」の試験タイプAの記載に準拠して23℃で測定を行った。加圧板を試験片に接触させた直後および接触時から15秒後の試験片の硬度を測定した。接触させた直後に得られた硬度を「ショアーA硬度(測定直後の値)」、接触時から15秒後に得られた硬度を「ショアーA硬度(測定15秒後の値)」とした。
組成物の応力緩和性は、500μmのシート状の組成物から長さ100mm、幅10mmに打ち抜いたサンプルについて測定した。インストロン社製万能引張試験機3380を用いて、引張速度=200mm/minで試験片を10%伸張させた。10%伸張させた際の応力を計測し、そのまま伸張を120秒間保持させた。その際の応力の変化を計測し、10%伸張直後の応力と60秒後の応力の差から緩和率を算出した。
共重合体(A)組成物の動的粘弾性は、粘弾性測定装置MCR301(AntonPaar社製)を用いて測定した。下記測定条件でシート状の組成物の粘度の温度依存性を測定した。当該測定で得られた、貯蔵弾性率(G’)と損失弾性率(G”)との比(G”/G’:損失正接)をtanδとした。tanδを温度に対してプロットすると、上に凸の曲線すなわちピークが得られ、そのピークの頂点の温度をtanδ―Tgとし、その温度における極大値を測定した。tanδにつき2つ以上のピークが観測された場合には、0℃以上に観測されたtanδ―Tgおよび23℃におけるtanδ―Tg値を記録した。
Frequency:1.6Hz
Temperature:−70〜100℃
Ramp Rate :2.0℃/分
Strain:0.5%
組成物の引張破断点伸び(EL)および引張破断点応力(TS)は、シート状の組成物を打抜いて作製した、JISK 7127に記載されている5号形ダンベル試験片について行った。この試験片を用いて同JISK 7127に規定される方法に従い、測定温度23℃、引張速度30mm/分の条件で引張り試験を行ない、引張破断点伸び(EL)および引張破断点応力(TS)を測定した。
組成物の反発弾性は、厚さ12mm、直径29mmに成形した組成物について、JIS K6255(1996)「加硫ゴム及び熱可塑性ゴムの反発弾性試験方法」の4項の「リュプケ式反発弾性試験」の記載に準拠して、23℃で測定を行って求めた。
組成物の損失係数は、JIS K7391に準拠して、23℃で片持ちはり法試験機((株)小野測器製)により測定した。測定試料として実施例厚さ1mmのプレスシートを10mm×200mm幅に打ち抜き、SUS430製の基材層に張り付けたものを用い、加振は、非接触電磁加振器を用いて定常加振を行い、材料が振動した時の共振周波数から各材料の損失係数を算出した。
〔4−メチル−1−ペンテン・α−オレフィン共重合体(A)〕
充分窒素置換した容量1.5リットルの攪拌翼付SUS製オートクレーブに、23℃で4−メチル−1−ペンテンを750ml装入した。このオートクレーブに、トリイソブチルアルミニウム(TIBAL)の1.0mmol/mlトルエン溶液を0.75ml装入し攪拌機を回した。
熱可塑性エラストマー組成物(B)として、下記の熱可塑性エラストマー組成物を使用した。
組成物B−2:三井化学株式会社製、商品名 ミラストマー5030NHS(エチレン・プロピレン・エチリデンノルボルネン三元共重合体ゴムとポリプロピレンとを含む混合物を動的架橋して得られた熱可塑性エラストマー組成物、ショアーA硬度(直後)=52、MFR(温度230℃、荷重98Nで測定)=4.5g/10分)
10質量部の重合体A−1と90質量部の組成物B−1とを混合して制振材用熱可塑性重合体組成物(組成物1)を得た。100質量部の組成物1に対して、二次抗酸化剤としての耐熱安定剤としてのn−オクタデシル−3−(4’−ヒドロキシ−3’,5’−ジ−t−ブチルフェニル)プロピネートを0.2質量部配合した。その後、株式会社プラスチック工学研究所社製2軸押出機BT−30(スクリュー系30mmφ、L/D=46)を用い、設定温度250℃、樹脂押出量60g/minおよび200rpmの条件で造粒してペレット化し、これをシート成形して成形体1を得た。成形体1の組成および物性を表2に示す。
25質量部の重合体A−1と75質量部の組成物B−1とを混合して制振材用熱可塑性重合体組成物(組成物2)を得た。比較例Aの組成物1に代えて組成物2を用いたほかは同様にして、成形体2を得た。成形体2の組成および物性を表2に示す。
40質量部の重合体A−1と60質量部の組成物B−1とを混合して制振材用熱可塑性重合体組成物(組成物3)を得た。比較例Aの組成物1に代えて組成物3を用いたほかは同様にして、成形体3を得た。成形体3の組成および物性を表2に示す。
10質量部の重合体A−1と90質量部の組成物B−2とを混合して制振材用熱可塑性重合体組成物(組成物4)を得た。比較例Aの組成物1に代えて組成物4を用いたほかは同様にして、成形体4を得た。成形体4の組成および物性を表2に示す。
25質量部の重合体A−1と75質量部の組成物B−2とを混合して制振材用熱可塑性重合体組成物(組成物5)を得た。比較例Aの組成物1に代えて組成物5を用いたほかは同様にして、成形体5を得た。成形体5の組成および物性を表2に示す。
40質量部の重合体A−1と60質量部の組成物B−2とを混合して制振材用熱可塑性重合体組成物(組成物6)を得た。比較例Aの組成物1に代えて組成物6を用いたほかは同様にして、成形体6を得た。成形体6の組成および物性を表2に示す。
比較例Bにおいて、重合体A−1に代えて株式会社クラレ製、商品名 ハイブラー5127(スチレン−イソプレン共重合体系熱可塑性エラストマー)を用いた以外は同様にして、組成物7を得た。比較例Bの組成物2に代えて組成物7を用いたほかは同様にして、成形体7を得た。成形体7の組成および物性を表3に示す。
比較例Bにおいて、重合体A−1に代えて旭化成ケミカルズ株式会社製、S.O.E.S1605(スチレン−ブタジエン共重合体系熱可塑性エラストマー)を用いた以外は同様にして、組成物8を得た。比較例Bの組成物2に代えて組成物8を用いたほかは同様にして、成形体8を得た。成形体8の組成および物性を表3に示す。
比較例Aにおいて、組成物1に代えて、組成物B−1を他の成分と混合せずに用いたほかは同様にして、成形体9を得た。成形体9の組成および物性を表3に示す。
比較例Aにおいて、組成物1に代えて、組成物B−2を他の成分と混合せずに用いたほかは同様にして、成形体10を得た。成形体10の組成および物性を表3に示す。
Claims (15)
- 4−メチル−1−ペンテンから導かれる構成単位(A−i)および4−メチル−1−ペンテンを除く炭素原子数2〜20のα−オレフィンから選ばれる少なくとも1種以上のα−オレフィンから導かれる構成単位(A−ii)を含み、任意に非共役ポリエンから導かれる構成単位(A−iii)を含んでもよい4−メチル−1−ペンテン・α−オレフィン共重合体であって、構成単位(A−i)、(A−ii)および(A−iii)の合計を100モル%としたときに、構成単位(A−i)を63〜86モル%、構成単位(A−ii)を14〜37モル%、構成単位(A−iii)を0〜10モル%含む、4−メチル−1−ペンテン・α−オレフィン共重合体(A)と、
エチレンから導かれる構成単位(B−i)、炭素原子数3〜20のα−オレフィンから導かれる構成単位(B−ii)、および非共役ポリエンから導かれる構成単位(B−iii)を含む共重合体[B−I]とポリオレフィン樹脂[B−II]とを含む混合物を動的架橋して得られる熱可塑性エラストマー組成物(B)とを含有し、
前記4−メチル−1−ペンテン・α−オレフィン共重合体(A)と前記熱可塑性エラストマー組成物(B)の質量比(A)/(B)が10/90〜49/51であり、
損失正接tanδの値が最大となる温度が15℃以上40℃以下であることを特徴とする制振材用熱可塑性重合体組成物。 - 前記4−メチル−1−ペンテン・α−オレフィン共重合体(A)は、前記構成単位(A−i)、(A−ii)および(A−iii)の合計を100モル%としたときに、前記構成単位(A−i)を63〜80モル%、前記構成単位(A−ii)を20〜37モル%、前記構成単位(A−iii)を0〜10モル%含む4−メチル−1−ペンテン・α−オレフィン共重合体である請求項1に記載の制振材用熱可塑性重合体組成物。
- 前記4−メチル−1−ペンテン・α−オレフィン共重合体(A)は、融点が観測されないか、もしくは融点が135℃未満の共重合体であることを特徴とする、請求項1または請求項2に記載の制振材用熱可塑性重合体組成物。
- 前記4−メチル−1−ペンテン・α−オレフィン共重合体(A)は、融点が観測されないか、もしくは110℃未満の共重合体であることを特徴とする、請求項1〜3の何れか1項に記載の制振材用熱可塑性重合体組成物。
- 前記4−メチル−1−ペンテン・α−オレフィン共重合体(A)は、損失正接tanδの値が最大となる温度が0℃以上40℃以下の共重合体であることを特徴とする、請求項1〜4の何れか1項に記載の制振材用熱可塑性重合体組成物。
- 請求項1〜5の何れか1項に記載の制振材用熱可塑性重合体組成物を成形する工程を含む、成形体の製造方法。
- 前記成形体は制振部材である、請求項6に記載の製造方法。
- 前記成形体は衝撃吸収材である、請求項6に記載の製造方法。
- 前記成形体は振動吸収材である、請求項6に記載の製造方法。
- 前記成形体は共振吸収材である、請求項6に記載の製造方法。
- 請求項1〜5の何れか1項に記載の制振材用熱可塑性重合体組成物を含む成形体。
- 制振部材である、請求項11に記載の成形体。
- 衝撃吸収材である、請求項11に記載の成形体。
- 振動吸収材である、請求項11に記載の成形体。
- 共振吸収材である、請求項11に記載の成形体。
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