JP2022536829A - 熱可塑性加硫物組成物 - Google Patents
熱可塑性加硫物組成物 Download PDFInfo
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- AOUVCMGRGUPDDD-UHFFFAOYSA-N [1-(prop-2-enoyloxymethyl)cyclohexyl]methyl prop-2-enoate Chemical class C=CC(=O)OCC1(COC(=O)C=C)CCCCC1 AOUVCMGRGUPDDD-UHFFFAOYSA-N 0.000 description 1
- MUUXBTFQEXVEEI-UHFFFAOYSA-N [2-(dimethyl-$l^{3}-silanyl)phenyl]-dimethylsilicon Chemical compound C[Si](C)C1=CC=CC=C1[Si](C)C MUUXBTFQEXVEEI-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
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- 239000013541 low molecular weight contaminant Substances 0.000 description 1
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- JSOQIZDOEIKRLY-UHFFFAOYSA-N n-propylnitrous amide Chemical compound CCCNN=O JSOQIZDOEIKRLY-UHFFFAOYSA-N 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
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- 238000006384 oligomerization reaction Methods 0.000 description 1
- 150000002895 organic esters Chemical class 0.000 description 1
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- 229910052763 palladium Inorganic materials 0.000 description 1
- 125000005634 peroxydicarbonate group Chemical group 0.000 description 1
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- 238000005191 phase separation Methods 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920002589 poly(vinylethylene) polymer Polymers 0.000 description 1
- 229920005638 polyethylene monopolymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
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- 238000010926 purge Methods 0.000 description 1
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- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
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- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical group [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XHGIFBQQEGRTPB-UHFFFAOYSA-N tris(prop-2-enyl) phosphate Chemical compound C=CCOP(=O)(OCC=C)OCC=C XHGIFBQQEGRTPB-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
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- 239000008096 xylene Substances 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
- PIMBTRGLTHJJRV-UHFFFAOYSA-L zinc;2-methylprop-2-enoate Chemical compound [Zn+2].CC(=C)C([O-])=O.CC(=C)C([O-])=O PIMBTRGLTHJJRV-UHFFFAOYSA-L 0.000 description 1
- XKMZOFXGLBYJLS-UHFFFAOYSA-L zinc;prop-2-enoate Chemical compound [Zn+2].[O-]C(=O)C=C.[O-]C(=O)C=C XKMZOFXGLBYJLS-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/04—Crosslinking with phenolic resin
Abstract
Description
アナンサ ナラヤナ アヤール、クリシュナン;ドウファス、アントニオス、ケー;ゴンシー、マイケル、ジェイ;ジュールダン、エリック、ピー
関連出願の相互参照
本出願は、2019年6月21日に出願された米国特許仮出願第62/864,978号の優先権を主張し、その開示内容は参照によって本明細書に完全に組み込まれる。
技術分野
TPV組成物の配合物化
ゴム相
エチレンベースコポリマー
1. プロピレンベースポリマー
3. 1-ブテンベースポリマー
他の成分
TPV組成物の調製
この式で、Qは、-CH2-、-CH2-O-CH2-から成る群から選ばれた2価の基であり;mは0または1~20の正の整数であり;R’は有機基である。いくつかの実施形態では、Qは2価の基-CH2-O-CH2-であり;mは0または1~10の正の整数であり;R’は20未満の炭素原子を有する有機基である。他の実施形態では、mは0または1~10の正の整数であり、R’は4~12の炭素原子を有する有機基である。
TPV組成物の特性
複素粘度(η*、@ 215℃)を有してもよい。
TPV組成物を作る方法
最終用途
実験結果
2軸押出機(TSE)を使用するサンプル調製
GPC 4D試験方法:複数検出器がハイフンでつながれて記載されたGPC-IRによる、分子量、コモノマー組成および長鎖分枝の測定
小振幅振動せん断(SAOS)からの位相角およびΔδ
Claims (65)
- 熱可塑性加硫物(TPV)組成物であって、
エチレンベースコポリマーであって、400,000g/モル~3,000,000g/モルのMw、10以下のMw/Mnおよび0.7以上のg’visを有するエチレンベースコポリマー;
熱可塑性ポリオレフィン;および
油または可塑剤の1種以上
を含んでおり、前記TPV組成物中の前記油または可塑剤の1種以上の量は、前記エチレンベースコポリマーの100重量部当たり10重量部~200重量部であり、かつ、前記TPV組成物は50μインチ(1.27μm)~120μインチ(3.05μm)である押し出し表面粗さを有する、TPV組成物。 - 前記熱可塑性ポリオレフィンが0.9以上のg’visを有する、請求項1に記載のTPV組成物。
- 前記熱可塑性ポリオレフィンが0.97以上のg’visを有する、請求項1または2に記載のTPV組成物。
- 前記熱可塑性ポリオレフィンが0.9未満のg’visを有する、請求項1~3のいずれか1項に記載のTPV組成物。
- 前記熱可塑性ポリオレフィンが0.7~0.88のg’visを有する、請求項4に記載のTPV組成物。
- 前記エチレンベースコポリマーが、エチレン-プロピレン-ジエンターポリマーである、請求項1~5のいずれか1項に記載のTPV組成物。
- 前記油が、鉱油、合成油、エステル可塑剤またはこれらの組み合わせである、請求項1~6のいずれか1項に記載のTPV組成物。
- 前記鉱油が、芳香族油、ナフテン油、パラフィン油、イソパラフィン油、合成油またはこれらの組み合わせである、請求項7に記載のTPV組成物。
- 前記鉱油が、グループII油であり、前記油の中の芳香族化合物および極性化合物の合計量が、ASTM 2007によって測定された4.5重量%未満であり、かつ、前記油の粘度が40℃で少なくとも80cStである、請求項7に記載のTPV組成物。
- 前記鉱油が、100℃で少なくとも10cStの粘度を有する、請求項7に記載のTPV組成物。
- 相溶化剤、フィラー、造核剤またはこれらの組み合わせをさらに含んでいる、請求項1~10のいずれか1項に記載のTPV組成物。
- 炭酸カルシウム、粘土、シリカ、タルク、二酸化チタン、カーボンブラック、マイカ、木粉、造核剤またはこれらの組み合わせをさらに含んでいる、請求項1~11のいずれか1項に記載のTPV組成物。
- 硬化剤をさらに含んでいる、請求項1~12のいずれか1項に記載のTPV組成物。
- 前記硬化剤がフェノール樹脂、過酸化物、マレイミド、ケイ素ベース硬化剤、シランベース硬化剤、硫黄ベース硬化剤またはこれらの組み合わせを含んでいる、請求項1~13のいずれか1項に記載のTPV組成物。
- 前記硬化剤がフェノール樹脂である、請求項14に記載のTPV組成物。
- 前記エチレンベースコポリマーが、前記エチレンベースコポリマーの全重量当たり70重量%以下のエチレン含有量を有する、請求項1~15のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、前記エチレンベースコポリマーの全重量当たり50重量%~70重量%のエチレン含有量を有する、請求項1~15のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、前記エチレンベースコポリマーの全重量当たり55重量%~65重量%のエチレン含有量を有する、請求項1~15のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、400,000g/モル~1,000,000g/モルのMwを有する、請求項1~18のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、400,000g/モル~700,000g/モルのMwを有する、請求項1~18のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、5-エチリデン-2-ノルボルネン(ENB)、5-ビニル-2-ノルボルネン(VNB)およびこれらの組み合わせから成る群から選ばれたジエンモノマーを含んでいる、請求項1~20のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーのジエン含有量が、前記エチレンベースコポリマーの全重量当たり3重量%~15重量%である、請求項1~21のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーのジエン含有量が、前記エチレンベースコポリマーの全重量当たり4重量%~12重量%である、請求項1~21のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、ジーグラー-ナッタ触媒またはメタロセン触媒を使用して、スラリー重合プロセスによって製造される、請求項1~23のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、ジーグラー-ナッタ触媒またはメタロセン触媒を使用して、溶液または気相重合プロセスによって製造される、請求項1~24のいずれか1項に記載のTPV組成物。
- 前記熱可塑性ポリオレフィンが、
0.1g/10分~50g/10分のメルトマスフローレート(ASTM D1238;230℃;2.16kg);および
100,000g/モル~1,000,000g/モルのMwを有する、
請求項1~25のいずれか1項に記載のTPV組成物。 - 前記熱可塑性ポリオレフィンが、
0.5g/10分~5g/10分のメルトマスフローレート(ASTM D1238;230℃;2.16kg);および
400,000g/モル~800,000g/モルのMwを有する、
請求項1~25のいずれか1項に記載のTPV組成物。 - 前記組成物が、20ショアA~60ショアDの硬度を有する、請求項1~27のいずれか1項に記載のTPV組成物。
- 前記組成物が、40ショアA~80ショアAの硬度を有する、請求項1~27のいずれか1項に記載のTPV組成物。
- 前記組成物が、600kPa~2000kPaのG’値(@90℃、0.6ラジアン/秒および1%ひずみ)を有する、請求項1~29のいずれか1項に記載のTPV組成物。
- 前記組成物が、700kPa~1500kPaのG’値(@90℃、0.6ラジアン/秒および1%ひずみ)を有する、請求項1~29のいずれか1項に記載のTPV組成物。
- 前記組成物が、204℃および1200秒-1のせん断速度で測定された120Pa・秒以下の毛細管粘度を有する、請求項1~31のいずれか1項に記載のTPV組成物。
- 前記熱可塑性ポリオレフィンが0.9以上のg’visを有する、請求項1~32のいずれか1項に記載のTPV組成物。
- 前記TPV組成物の前記エチレンベースコポリマーが、小振幅振動せん断(SAOS)からの30度~80度のΔδまたは3未満の大振幅振動せん断(LAOS)分枝指数を有し、Δδ=δ(0.1ラジアン/秒)-δ(128ラジアン/秒)である、請求項1~33のいずれか1項に記載のTPV組成物。
- 前記TPV組成物が、50μインチ(1.27μm)~150μインチ(3.81μm)である押し出し表面粗さを有する、請求項1~34のいずれか1項に記載のTPV組成物。
- 前記TPV組成物が、58μインチ(1.47μm)~120μインチ(3.05μm)である押し出し表面粗さを有する、請求項1~34のいずれか1項に記載のTPV組成物。
- 前記TPV組成物が16%未満の永久伸びを有する、請求項1~36のいずれか1項に記載のTPV組成物。
- 前記TPV組成物が14%未満の永久伸びを有する、請求項1~36のいずれか1項に記載のTPV組成物。
- 前記TPV組成物が、50μインチ(1.27μm)~150μインチ(3.81μm)である押し出し表面粗さおよび16%未満の永久伸びを有する、請求項1~38のいずれか1項に記載のTPV組成物。
- 前記TPV組成物が、58μインチ(1.47μm)~120μインチ(3.05μm)である押し出し表面粗さおよび14%未満の永久伸びを有する、請求項1~38のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、250MU以上の乾燥ムーニー粘度(ML1+4@125℃)を有する、請求項1~40のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、350MU以上の乾燥ムーニー粘度(ML1+4@125℃)を有する、請求項1~41のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、2.5以下のLCB指数(@125℃)を有する、請求項1~42のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、2.0以下のLCB指数(@125℃)を有する、請求項1~43のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、32°以上のΔδを有し、Δδ(125℃)=δ(0.1ラジアン/秒)-δ(128ラジアン/秒)である、請求項1~44のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、35°以上のΔδを有し、Δδ(125℃)=δ(0.1ラジアン/秒)-δ(128ラジアン/秒)である、請求項1~44のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、前記エチレンベースコポリマー100phr当たり50phr~200phrを有する油を用いて油展されている、請求項1~46のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマーが、前記エチレンベースコポリマー100phr当たり75phr~120phrを有する油を用いて油展されている、請求項1~46のいずれか1項に記載のTPV組成物。
- 前記エチレンベースコポリマー含有量が、前記TPV組成物の全重量当たり10重量%~90重量%である、請求項1~48のいずれか1項に記載のTPV組成物。
- 前記TPV組成物が、Elastocon社応力緩和試験機によって測定された-1~-5(1/分)の応力緩和勾配を有する、請求項1~49のいずれか1項に記載のTPV組成物。
- TPV組成物が0.25~1.0のtan δ値(@ 215℃、5.0ラジアン/秒および100%ひずみ)を有する、請求項1~50のいずれか1項に記載のTPV組成物。
- 前記TPV組成物が、Elastocon社応力緩和試験機によって測定された-2~-4.5(1/分)の応力緩和勾配を有する、請求項1~51のいずれか1項に記載のTPV組成物。
- TPV組成物を作る方法であって、以下の工程を含む方法:
エチレンベースコポリマーを押し出しリアクターに導入する工程;
熱可塑性ポリオレフィンを前記押し出しリアクターに導入する工程;
フィラー、添加物またはフィラーと添加物との組み合わせを前記押し出しリアクターに導入する工程;
第1の量の油または可塑剤の1種以上を硬化剤の前に前記押し出しリアクターに導入する工程;
前記硬化剤を前記押し出しリアクターに導入する工程;
第2の量の油または可塑剤の1種以上を前記硬化剤の後に前記押し出しリアクターに導入する工程であって、前記油または可塑剤の1種以上の全量の3重量%~37重量%が前記硬化剤の前に前記押し出しリアクターに加えられ、かつ、前記油または可塑剤の1種以上の全量の63重量%~97重量%が前記硬化剤の後に前記押し出しリアクターに加えられる工程;および
前記熱可塑性ポリオレフィンの存在下で前記硬化剤とともに前記エチレンベースコポリマーを動的加硫して、前記TPV組成物を形成する工程。 - フィラー、添加物またはフィラーと添加物との組み合わせを導入する工程をさらに含む、請求項53に記載の方法。
- 前記押し出しリアクターが2軸押出機である、請求項53または54に記載の方法。
- 前記第2の量の油または可塑剤の1種以上と前記第1の量の油または可塑剤の1種以上との重量比が2:1~10:1である、請求項53~55に記載の方法。
- 前記第2の量の油または可塑剤の1種以上と前記第1の量の油または可塑剤の1種以上との比が2:1~7:1である、請求項53~55に記載の方法。
- 前記油または可塑剤の1種以上の全量の10重量%~33重量%が前記硬化剤の前に前記押し出しリアクターに加えられ、かつ、前記油または可塑剤の1種以上の全量の67重量%~90重量%が前記硬化剤の後に前記押し出しリアクターに加えられる、請求項53~57のいずれか1項に記載の方法。
- 前記油または可塑剤の1種以上の全量の20重量%~30重量%が前記硬化剤の前に前記押し出しリアクターに加えられ、かつ、前記油または可塑剤の1種以上の全量の70重量%~80重量%が前記硬化剤の後に前記押し出しリアクターに加えられる、請求項53~57のいずれか1項に記載の方法。
- 前記TPV組成物が、請求項1~52のいずれか1項に記載のTPV組成物である、請求項53~59のいずれか1項に記載の方法。
- 物品を形成する方法であって、以下の工程を含む方法:
請求項1~52のいずれか1項に記載のTPV組成物を、押し出す、射出成形する、ブロー成形する、圧縮成形する、熱成形する、または3D印刷する、工程;および
物品を形成する工程。 - 前記物品が、押し出されたテープ、ウェザーシール、ドアパネル、ガスケット、パイプシール、ホース、ベルトまたはトランクである、請求項61に記載の方法。
- 請求項1~52のいずれか1項に記載のTPV組成物を含んでいる、物品。
- 前記物品が、押し出されたテープ、ウェザーシール、ドアパネル、ガスケット、パイプシール、ホース、ベルトまたはトランクである、請求項63に記載の物品。
- 請求項53~64のいずれか1項に記載の方法で作られたTPV組成物を含んでいる、物品。
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