JP5676586B2 - 耐衝撃性プロピレンポリマー組成物の製造方法 - Google Patents
耐衝撃性プロピレンポリマー組成物の製造方法 Download PDFInfo
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- JP5676586B2 JP5676586B2 JP2012515473A JP2012515473A JP5676586B2 JP 5676586 B2 JP5676586 B2 JP 5676586B2 JP 2012515473 A JP2012515473 A JP 2012515473A JP 2012515473 A JP2012515473 A JP 2012515473A JP 5676586 B2 JP5676586 B2 JP 5676586B2
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- 125000000217 alkyl group Chemical group 0.000 description 7
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- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
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- 125000004184 methoxymethyl group Chemical group [H]C([H])([H])OC([H])([H])* 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 3
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
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- 125000001637 1-naphthyl group Chemical group [H]C1=C([H])C([H])=C2C(*)=C([H])C([H])=C([H])C2=C1[H] 0.000 description 2
- RKMGAJGJIURJSJ-UHFFFAOYSA-N 2,2,6,6-tetramethylpiperidine Chemical compound CC1(C)CCCC(C)(C)N1 RKMGAJGJIURJSJ-UHFFFAOYSA-N 0.000 description 2
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- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
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- 229940087101 dibenzylidene sorbitol Drugs 0.000 description 2
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- 238000004817 gas chromatography Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
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- 239000002861 polymer material Substances 0.000 description 2
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- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
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- 230000007704 transition Effects 0.000 description 2
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- HBMODDNTUPGVFW-UHFFFAOYSA-N (1,3-dimethoxy-2-phenylpropan-2-yl)benzene Chemical compound C=1C=CC=CC=1C(COC)(COC)C1=CC=CC=C1 HBMODDNTUPGVFW-UHFFFAOYSA-N 0.000 description 1
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- VFIOZKTXVHLWRA-UHFFFAOYSA-N (2-ethylpiperidin-1-yl)-dimethoxy-(1,1,1-trifluoropropan-2-yl)silane Chemical compound CCC1CCCCN1[Si](OC)(OC)C(C)C(F)(F)F VFIOZKTXVHLWRA-UHFFFAOYSA-N 0.000 description 1
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- WNVMVIYFKFGESM-UHFFFAOYSA-N bis(2-methylpropyl) 2,3-di(propan-2-yl)butanedioate Chemical compound CC(C)COC(=O)C(C(C)C)C(C(C)C)C(=O)OCC(C)C WNVMVIYFKFGESM-UHFFFAOYSA-N 0.000 description 1
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- BTJCEVZMRIJBSM-UHFFFAOYSA-N dimethoxy-methyl-(1,1,1-trifluoropropan-2-yl)silane Chemical compound CO[Si](C)(OC)C(C)C(F)(F)F BTJCEVZMRIJBSM-UHFFFAOYSA-N 0.000 description 1
- 125000005982 diphenylmethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
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- 239000005457 ice water Substances 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
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- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
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- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
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- 125000003538 pentan-3-yl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])C([H])([H])[H] 0.000 description 1
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- 239000000843 powder Substances 0.000 description 1
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- 230000000284 resting effect Effects 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
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- NETBVGNWMHLXRP-UHFFFAOYSA-N tert-butyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C(C)(C)C NETBVGNWMHLXRP-UHFFFAOYSA-N 0.000 description 1
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- ORYGRKHDLWYTKX-UHFFFAOYSA-N trihexylalumane Chemical compound CCCCCC[Al](CCCCCC)CCCCCC ORYGRKHDLWYTKX-UHFFFAOYSA-N 0.000 description 1
- LFXVBWRMVZPLFK-UHFFFAOYSA-N trioctylalumane Chemical compound CCCCCCCC[Al](CCCCCCCC)CCCCCCCC LFXVBWRMVZPLFK-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/04—Monomers containing three or four carbon atoms
- C08F210/06—Propene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F10/04—Monomers containing three or four carbon atoms
- C08F10/06—Propene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/06—Organic solvent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/02—Ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F297/00—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer
- C08F297/06—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type
- C08F297/08—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins
- C08F297/083—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins the monomers being ethylene or propylene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/02—Carriers therefor
- C08F4/022—Magnesium halide as support anhydrous or hydrated or complexed by means of a Lewis base for Ziegler-type catalysts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/06—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen
- C08F4/16—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen of silicon, germanium, tin, lead, titanium, zirconium or hafnium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/04—Monomers containing three or four carbon atoms
- C08F110/06—Propene
Description
高い重合活性が同時に要求される。複数の重合工程があることから、そして2つのポリマーフラクション間で特定の重量バランスを保持しなければならないという事実から、触媒は、時が経過しても受け入れ可能な重合活性レベルを維持する必要があり、特に、気相中での必要な反応性レベルを保持できるものでなければならない。
1,1−ビス(メトキシメチル)−2,3−ジメチルインデン、1,1−ビス(メトキシメチル)−4,5,6,7−テトラヒドロインデン、1,1−ビス(メトキシメチル)−2,3,6,7−テトラフルオロインデン、
1,1−ビス(メトキシメチル)−4,7−ジメチルインデン、1,1−ビス(メトキシメチル)−3,6−ジメチルインデン、1,1−ビス(メトキシメチル)−4−フェニルインデン、1,1−ビス(メトキシメチル)−4−フェニル−2−メチルインデン、1,1−ビス(メトキシメチル)−4−シクロヘキシルインデン、1,1−ビス(メトキシメチル)−7−(3,3,3−トリフルオロプロピル)インデン、1,1−ビス(メトキシメチル)−7−トリメチルシリルインデン、1,1−ビス(メトキシメチル)−7−トリフルオロメチルインデン、1,1−ビス(メトキシメチル)−4,7−ジメチル−4,5,6,7−テトラヒドロインデン、1,1−ビス(メトキシメチル)−7−メチルインデン、1,1−ビス(メトキシメチル)−7−シクロペンチルインデン、1,1−ビス(メトキシメチル)−7−イソプロピルインデン、1,1−ビス(メトキシメチル)−7−シクロヘキシルインデン、1,1−ビス(メトキシメチル)−7−tert−ブチルインデン、1,1−ビス(メトキシメチル)−7−tert−ブチル−2−メチルインデン、1,1−ビス(メトキシメチル)−7−フェニルインデン、1,1−ビス(メトキシメチル)−2−フェニルインデン、1,1−ビス(メトキシメチル)−1H−ベンズ[e]インデン(benz[e]indene)、1,1−ビス(メトキシメチル)−1H−2−メチルベンズ[e]インデン、9,9−ビス(メトキシメチル)フルオレン、9,9−ビス(メトキシメチル)−2,3,6,7−テトラメチルフルオレン、9,9−ビス(メトキシメチル)−2,3,4,5,6,7−ヘキサフルオロフルオレン、9,9−ビス(メトキシメチル)−2,3−ベンゾフルオレン、9,9−ビス(メトキシメチル)−2,3,6,7−ジベンゾフルオレン、9,9−ビス(メトキシメチル)−2,7−ジイソプロピルフルオレン、9,9−ビス(メトキシメチル)−1,8−ジクロロフルオレン、9,9−ビス(メトキシメチル)−2,7−ジシクロペンチルフルオレン、9,9−ビス(メトキシメチル)−1,8−ジフルオロフルオレン、9,9−ビス(メトキシメチル)−1,2,3,4−テトラヒドロフルオレン、9,9−ビス(メトキシメチル)−1,2,3,4,5,6,7,8−オクタヒドロフルオレン、および9,9−ビス(メトキシメチル)−4−tert−ブチルフルオレンなどがある。
反応器グレードのポリマー組成物に対して測定されたキシレン可溶フラクションの固有粘度の値は0.5dl/g〜6.0dl/gの範囲である。
特に、核形成剤を添加すると、重要な物理的−機械的特性〔例えば、曲げ弾性率、加熱撓み温度(HDT)、降伏点引張強さ、および透明性)の大幅な改良がもたらされる。
核形成剤は、本発明の組成物に、総重量を基準として0.05〜2重量%の量にて添加するが好ましく、0.1〜1重量%の量にて添加するのがさらに好ましい。
キシレン可溶性フラクション
2.5gのポリマーと250mlのo−キシレンを、冷却装置と磁気攪拌機を装備したガラスフラスコ中に装入する。温度を30分で溶媒の沸点まで上昇させる。得られた溶液を還流状態に保持し、さらに30分撹拌する。次いで、密閉したフラスコを、氷水浴中に30分保持し、そして恒温水槽中に25℃にて30分保持する。このようにして得られる固体を迅速濾紙により濾過し、濾液を2つの100mlアリコートに分ける。濾液の1つの100mlアリコートを計量済みの容器中に注ぎ、これを窒素気流下にて加熱プレートで加熱して、蒸発により溶媒を除去する。次いで、一定の重量が得られるまで、容器を、オーブン中に減圧にて80℃で保持する。残留物を計量して、キシレン可溶性ポリマーのパーセント値を求める。
IR分光分析法による
成分Bのコモノマー含量を、ポリマーの沈殿した“非晶質”フラクションに対して測定する。沈殿した“非晶質”フラクションは次のようにして得る:上記のように得られる濾液の1つの100mlアリコートに、200mlのアセトンを、激しく撹拌しながら加える。沈殿は、明白な固体−溶液分離によって示されるように完全でなければならない。このようにして得られる固体を金属スクリーンにより濾過し、一定の重量に達するまで、減圧オーブン中にて70℃で乾燥する。
ガスクロマトグラフィーにより測定
溶融流量(MFR)
ISO1133(230℃、2.16kg)に従って測定
固有粘度
テトラヒドロナフタレン中にて135℃で測定
曲げ弾性率
ISO178に従って測定
降伏応力と破断応力
ISO527に従って測定
降伏点伸びと破断点伸び
ISO527に従って測定
アイゾッド衝撃強さ
ISO180/1Aに従って測定
延性/脆性転移温度(D/B)
この方法によれば、二軸耐衝撃性は、コンピュータ制御の自動打撃ハンマーによる衝撃により測定する。
127×127×1.5mmの寸法を有する、D/B測定用のプラークは、以下の方法にしたがって作製される。
主要なプロセスパラメーターは次の通りである:背圧:20バール;射出時間:3秒;最大射出圧力:14Mpa;油圧射出圧力:6〜3Mpa;第1の保持油圧:4±2Mpa;第1の保持時間:3秒;第2の保持油圧:3±2MPa;第2の保持時間:7秒;冷却時間:20秒;金型温度:60℃。
融解温度、融解エンタルピー、および結晶化温度
20℃/分の温度変化にてDSCにより測定。
単色レーザー光線の光回折の原理に基づいた方法により測定。
実施例1〜5
実施例1
固体触媒成分の調製
窒素でパージした500mlの四つ口丸底フラスコに、250mlのTiCl4を0℃にて装入した。撹拌しながら、47μmの平均粒径を有するマイクロ球状MgCl2・2.1C2H5OH(ヨーロッパ特許第728769号の実施例1に記載の方法に従って製造)の10.0gと、ラセミ形の2,3−ジイソプロピルコハク酸ジエチルのある量とを、Mg/コハク酸エステルのモル比が12となるように加えた。温度を100℃に上げ、この温度で60分保持した。その後、撹拌を停止し、液体を吸い上げ、TiCl4による処理を110℃で30分繰り返した。吸い上げ後、フレッシュなTiCl4とある量の9,9−ビス(メトキシメチル)フルオレンとを、Mg/コハク酸エステルのモル比が12となるように加えた。次いで温度を30分で90℃に上げた。85℃での沈殿と吸い上げの後、固体を無水ヘキサン(6×100ml)で60℃にて6回洗浄した。
上記の固体触媒成分を重合反応器中に導入する前に、該触媒成分を、表1に記載の条件下にてトリエチルアルミニウム(TEAL)およびジシクロペンチルジメトキシシラン(DCPMS)と接触させる。
重合
重合は、生成物をある1つの反応器からそのすぐ次の反応器に移すための装置を備えた、一連の2つの反応器中にて連続モードで行われる。第1の反応器は液相ループ型反応器であり、第2の反応器は気相流動床反応器である。プロピレンホモポリマーは、液相ループ型反応器において製造され、エチレンコポリマーは、第1の段階からもたらされるプロピレンホモポリマーの存在下にて気相反応器において製造される。水素が分子量調整剤として使用される。
重合が終了したら、粉末を取り出し、窒素気流下にて乾燥する。
比較例1
同じ触媒を使用して、そして工程(ii)を行わないということ以外は実施例1に関して記載した条件下で重合を行った。
Claims (3)
- 25℃にてキシレンに不溶性のプロピレンポリマーフラクションを50〜90重量%、および25℃にてキシレンに可溶性のエチレンコポリマーフラクションを10〜50重量%含むプロピレンポリマー組成物の製造方法であって、ここで該製造方法が、(a)20〜70μmの範囲の平均粒径を有していて、ハロゲン化マグネシウム;少なくともTi−ハロゲン結合を有するチタン化合物;および、一方がコハク酸エステルから選択されて、供与体の総量を基準として50〜90モル%の量にて存在し、他方が1,3−ジエーテルから選択される、少なくとも2種の電子供与体化合物;を含む固体触媒成分、(b)アルキルアルミニウム、および(c)必要に応じて外部の電子供与体化合物、を含む触媒システムの存在下で行われ、
(i) 触媒成分(a)、(b)、および必要に応じて(c)を、0〜90℃の範囲の温度にて0.1〜120分の範囲の時間にわたって接触させる工程;
(ii) 固体触媒成分(a)の1グラム当たり0.1gから最大で1000gまでのポリマー量が形成されるまで、式CH2=CHR(式中、RはHまたはC1−C10炭化水素である)の1種以上のオレフィンを使用して予備重合させる工程;
(iii) エチレン及び/又はC4−C10α−オレフィンの任意の存在下でプロピレンを重合させて、少なくとも85重量%が25℃にてキシレンに不溶であるプロピレン(コ)ポリマーを得る工程;および
(iv) (iii)からもたらされる生成物の存在下にて気相で行われる後続の工程において、エチレンとα−オレフィンCH2=CHR(式中、Rは1〜10個の炭素原子を有する炭化水素基である)との混合物を重合させて、15〜75重量%の前記α−オレフィンCH2=CHRを含有する該エチレンコポリマーを得る工程;を含む上記製造方法。 - 工程(i)において、触媒成分(a)、(b)、及び必要に応じて(c)を、重量比(b)/(a)が0.1〜10の範囲であるような量にて、そして化合物(c)が存在する場合は、重量比(b)/(c)が10〜200の範囲であるような量にて予備接触容器に供給する、請求項1に記載の製造方法。
- 予備重合度が、固体触媒成分1グラム当たり60〜800gの範囲である、請求項1に記載の製造方法。
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CN107043491A (zh) | 2017-08-15 |
EP2443159B1 (en) | 2018-04-25 |
JP2012530170A (ja) | 2012-11-29 |
US9068028B2 (en) | 2015-06-30 |
CN102803310A (zh) | 2012-11-28 |
EP2443159A1 (en) | 2012-04-25 |
KR101769275B1 (ko) | 2017-08-18 |
ES2672731T3 (es) | 2018-06-15 |
US20120083576A1 (en) | 2012-04-05 |
BRPI1014019B1 (pt) | 2019-10-22 |
RU2012101804A (ru) | 2013-07-27 |
RU2536682C2 (ru) | 2014-12-27 |
WO2010146074A1 (en) | 2010-12-23 |
KR20120042763A (ko) | 2012-05-03 |
BRPI1014019A2 (pt) | 2016-04-12 |
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