JP2009537653A - ポリプロピレン溶液重合方法 - Google Patents
ポリプロピレン溶液重合方法 Download PDFInfo
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- JP2009537653A JP2009537653A JP2009510949A JP2009510949A JP2009537653A JP 2009537653 A JP2009537653 A JP 2009537653A JP 2009510949 A JP2009510949 A JP 2009510949A JP 2009510949 A JP2009510949 A JP 2009510949A JP 2009537653 A JP2009537653 A JP 2009537653A
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- Prior art keywords
- bis
- methyl
- phenyl
- oxoyl
- dibenzo
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 68
- 238000010528 free radical solution polymerization reaction Methods 0.000 title claims abstract description 21
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- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims abstract description 4
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- 238000006243 chemical reaction Methods 0.000 claims description 44
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- 125000004429 atom Chemical group 0.000 claims description 29
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- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical group CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 claims description 4
- LFXVBWRMVZPLFK-UHFFFAOYSA-N trioctylalumane Chemical compound CCCCCCCC[Al](CCCCCCCC)CCCCCCCC LFXVBWRMVZPLFK-UHFFFAOYSA-N 0.000 claims description 4
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- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 4
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- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
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Classifications
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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
- C08F4/00—Polymerisation catalysts
- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
- C08F4/64—Titanium, zirconium, hafnium or compounds thereof
-
- 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
-
- 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
- C08F10/02—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
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
-
- 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
- C08F4/00—Polymerisation catalysts
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Abstract
Description
本出願は米国仮特許出願第60/801,182号(2006年5月17日出願)の優先権を主張する。
A*+はカチオン(特に、プロトン含有カチオン)であり、好ましくは、1又は2のC10-40アルキル基を含有するトリヒドロカルビルアンモニウムカチオンであり、特に、メチルジ(C14-20アルキル)アンモニウムカチオンであり、
R4は独立して、それぞれの存在が、水素、あるいは、水素を除いて30個までの原子を有するハロ基、ヒドロカルビル基、ハロカルビル基、ハロヒドロカルビル基、シリルヒドロカルビル基又はシリル基(モノ(ヒドロカルビル)シリル基、ジ(ヒドロカルビル)シリル基及びトリ(ヒドロカルビル)シリル基を含む)であり、好ましくは、C1-20アルキルであり、
J*’はトリス(ペンタフルオロフェニル)ボラン又はトリス(ペンタフルオロフェニル)アルマンである。
ビス(トリス(ペンタフルオロフェニル)ボラン)イミダゾリド、
ビス(トリス(ペンタフルオロフェニル)ボラン)−2−ウンデシルイミダゾリド、
ビス(トリス(ペンタフルオロフェニル)ボラン)−2−ヘプタデシルイミダゾリド、ビス(トリス(ペンタフルオロフェニル)ボラン)−4,5−ビス(ウンデシル)イミダゾリド、ビス(トリス(ペンタフルオロフェニル)ボラン)−4,5−ビス(ヘプタデシル)イミダゾリド、
ビス(トリス(ペンタフルオロフェニル)ボラン)イミダゾリニド、
ビス(トリス(ペンタフルオロフェニル)ボラン)−2−ウンデシルイミダゾリニド、ビス(トリス(ペンタフルオロフェニル)ボラン)−2−ヘプタデシルイミダゾリニド、ビス(トリス(ペンタフルオロフェニル)ボラン)−4,5−ビス(ウンデシル)イミダゾリニド、ビス(トリス(ペンタフルオロフェニル)ボラン)−4,5−ビス(ヘプタデシル)イミダゾリニド、
ビス(トリス(ペンタフルオロフェニル)ボラン)−5,6−ジメチルベンゾイミダゾリド、
ビス(トリス(ペンタフルオロフェニル)ボラン)−5,6−ビス(ウンデシル)ベンゾイミダゾリド、
ビス(トリス(ペンタフルオロフェニル)アルマン)イミダゾリド、
ビス(トリス(ペンタフルオロフェニル)アルマン)−2−ウンデシルイミダゾリド、ビス(トリス(ペンタフルオロフェニル)アルマン)−2−ヘプタデシルイミダゾリド、ビス(トリス(ペンタフルオロフェニル)アルマン)−4,5−ビス(ウンデシル)イミダゾリド、
ビス(トリス(ペンタフルオロフェニル)アルマン)−4,5−ビス(ヘプタデシル)イミダゾリド、
ビス(トリス(ペンタフルオロフェニル)アルマン)イミダゾリニド、
ビス(トリス(ペンタフルオロフェニル)アルマン)−2−ウンデシルイミダゾリニド、ビス(トリス(ペンタフルオロフェニル)アルマン)−2−ペプタデシルイミダゾリニド、ビス(トリス(ペンタフルオロフェニル)アルマン)−4,5−ビス(ウンデシル)イミダゾリニド、ビス(トリス(ペンタフルオロフェニル)アルマン)−4,5−ビス(ヘプタデシル)イミダゾリニド、
ビス(トリス(ペンタフルオロフェニル)アルマン)−5,6−ジメチルベンゾイミダゾリド及び
ビス(トリス(ペンタフルオロフェニル)アルマン)−5,6−ビス(ウンデシル)ベンゾイミダゾリド
のトリヒドロカルビルアンモニウム塩、特に、それらのメチルジ(C14-20アルキル)アンモニウム塩が含まれる。
本発明に従って使用される好適な金属錯体には、下記式に対応する化合物が含まれる。
R20は独立して、それぞれの存在が、水素を除いて5個〜20個の原子を含有する二価の芳香族基又は不活性に置換された芳香族基である;
T3は、水素を除いて3個〜20個の原子を有する二価の炭化水素基又はシラン基、あるいは、その不活性に置換された誘導体である;及び
RDは独立して、それぞれの存在が、水素を除いて1個〜20個の原子を有する一価の配位子基であるか、又は、2つのRD基は一緒になって、水素を除いて1個〜20個の原子を有する二価の配位子基である。
Ar2は独立して、それぞれの存在が、水素を除いて6個〜20個の原子を有するアリーレン基、アルキル置換アリーレン基、アリール置換アリーレン基、アルコキシ置換アリーレン基もしくはアミノ置換アリーレン基、又は、いずれかの置換基の任意の原子である;
T3は、水素を除いて3個〜20個の原子を有する二価の炭化水素架橋基であり、好ましくは、酸素原子を隔てる少なくとも3個の炭素原子を有する二価の置換又は非置換のC3-6脂肪族基、シクロ脂肪族基又はビス(アルキレン)置換シクロ脂肪族基である;及び
RDは独立して、それぞれの存在が、水素を除いて1個〜20個の原子を有する一価の配位子基であるか、又は、2つのRD基は一緒になって、水素を除いて1個〜40個の原子を有する二価の配位子基である。
Ar4は独立して、それぞれの存在が、C6-20アリール又はその不活性に置換された誘導体であり、特に、3,5−ジ(イソプロピル)フェニル、3,5−ジ(イソブチル)フェニル、ジベンゾ−1H−ピロール−1−イル、ナフチル、アントラセン−5−イル、1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イルである;
T4は独立して、それぞれの存在が、プロピレン−1,3−ジイル基、ビス(アルキレン)シクロヘキサン−1,2−ジイル基、あるいは、それぞれが20個までの炭素を有する1個〜5個のアルキル置換基、アリール置換基又はアラルキル置換基により置換されるそれらの不活性に置換された誘導体である;
R21は独立して、それぞれの存在が、水素、ハロ、水素を除いて50個までの原子を有するヒドロカルビル、トリヒドロカルビルシリル、トリヒドロカルビルシリルヒドロカルビル、アルコキシ又はアミノである;及び
RDは独立して、それぞれの存在が、ハロ、又は、水素を除いて20個までの原子を有するヒドロカルビル基又はトリヒドロカルビルシリル基であるか、あるいは、2つのRD基は一緒になって、水素を除いて40個までの原子を有する二価のヒドロカルビレン基、ヒドロカルバジイル基又はトリヒドロカルビルシリル基である。
Ar4は独立して、それぞれの存在が、3,5−ジ(イソプロピル)フェニル、3,5−ジ(イソブチル)フェニル、ジベンゾ−1H−ピロール−1−イル又はアントラセン−5−イルである;
R21は独立して、それぞれの存在が、水素、ハロ、水素を除いて50個までの原子を有するヒドロカルビル、トリヒドロカルビルシリル、トリヒドロカルビルシリルヒドロカルビル、アルコキシ又はアミノである;
T4はプロパン−1,3−ジイル又はビス(メチレン)シクロヘキサン−1,2−ジイルである;及び
RDは独立して、それぞれの存在が、ハロ、又は、水素を除いて20個までの原子を有するヒドロカルビル基又はトリヒドロカルビルシリル基であるか、あるいは、2つのRD基は一緒になって、水素を除いて40個までの原子を有するヒドロカルビレン基、ヒドロカルバジイル基又はヒドロカルビルシランジイル基である。
A)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジベンジル、
B)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジベンジル、
C)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジベンジル、
D)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジクロリド、及び
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジベンジル。
本明細書において使用される好適なオレフィン混合物には、エチレン、1又はそれ以上のC3-30α−オレフィン及び1又はそれ以上の共役ジエン又は非共役ジエンの混合物が含まれる。好適なα−オレフィンコモノマーには、プロピレン、イソブチレン、1−ブテン、1−ペンテン、1−ヘキセン、1−ヘプテン、1−オクテン、1−ノネン、1−デセン及び1−ドデセン、1−テトラデセン、1−ヘキサデセン、1−オクタデセン、1−エイコセン、3−メチル−1−ブテン、3−メチル−1−ペンテン、4−メチル−1−ペンテン、4,6−ジメチル−1−ヘプテン、並びに、ビニルシクロヘキサンが含まれるが、これらに限定されない。
下記の実施形態が、添付された特許請求の範囲についての具体的な開示のために提供される。
R20は独立して、それぞれの存在が、水素を除いて5個〜20個の原子を含有する二価の芳香族基又は不活性に置換された芳香族基である;
T3は、水素を除いて3個〜20個の原子を有する二価の炭化水素基又はシラン基、あるいは、その不活性に置換された誘導体である;及び
RDは独立して、それぞれの存在が、水素を除いて1個〜20個の原子を有する一価の配位子基であるか、又は、2つのRD基は一緒になって、水素を除いて1個〜20個の原子を有する二価の配位子基である);及び
120℃〜250℃の温度及び100kPa〜300MPaの圧力での活性化共触媒
に対応する、実施形態1に記載の方法。
の1つに対応する、実施形態1〜10のいずれか1つに記載の方法。
A)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジベンジル、
B)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジベンジル、
C)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジベンジル、
D)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジクロリド、及び
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジベンジル
からなる群より選択される、実施形態11に記載の方法。
金属錯体の調製
米国特許出願公開第2004/001013号の合成手順が、下記の金属錯体(A1及びA2)を調製するために実質的に繰り返された。
連続溶液重合が、内部撹拌装置を備えるコンピューター制御のオートクレーブ反応槽において行われる。精製された混合アルカン溶媒(ExxonMobil,Inc.から入手可能なIsopar(商標)E)、エチレン、プロピレン、5−エチリデン−2−ノルボルネン及び水素が、温度制御用ジャケット及び内部熱電対を備える3.8Lの反応槽に連続的に供給される。反応槽への溶媒供給量が質量流量コントローラーによって測定される。可変速度ダイアフラムポンプにより、反応槽への溶媒流速及び圧力が制御される。ポンプが吐出しているとき、側方の流れが、触媒注入ライン及び共触媒注入ライン並びに反応槽撹拌機のためのフラッシュ流れを提供するために取られる。これらの流れは質量流量計によって測定され、制御バルブによって、又は、ニードルバルブの手動調節によって制御される。残留する溶媒がモノマー及び水素と一緒にされ、反応槽に供給される。質量流量コントローラーが、水素を必要に応じて反応槽に送達するために使用される。溶媒/モノマー溶液の温度が、反応槽に入る前に熱交換器の使用によって制御される。この流れは反応槽の底部に入る。
Claims (12)
- プロピレン、場合により、エチレン、並びにさらに場合により、1又はそれ以上のC4-30α−オレフィン及び/又は1又はそれ以上の共役ジエンもしくは非共役ジエンを、高分子量のポリマー又はインターポリマーを調製するための連続溶液重合条件の下で重合するための方法であって、重合を多価アリールオキシエーテルのハフニウム錯体を含む触媒組成物の存在下で行うことを含む方法。
- 前記金属錯体が、下記式、
R20は独立して、それぞれの存在が、水素を除いて5個〜20個の原子を含有する二価の芳香族基又は不活性に置換された芳香族基である;
T3は、水素を除いて3個〜20個の原子を有する二価の炭化水素基又はシラン基、あるいは、その不活性に置換された誘導体である;及び
RDは独立して、それぞれの存在が、水素を除いて1個〜20個の原子を有する一価の配位子基であるか、又は、2つのRD基は一緒になって、水素を除いて1個〜20個の原子を有する二価の配位子基である);及び
120℃〜250℃の温度及び100kPa〜300MPaの圧力での活性化共触媒
に対応する、請求項1に記載の方法。 - プロピレン及びエチレンが、85重量パーセント〜98重量パーセントのプロピレンを含有し、50,000g/mol以上のMwを有するプロピレン/エチレンコポリマーを形成するために重合される、請求項1に記載の方法。
- 130℃〜250℃の温度で操作され、反応槽におけるプロピレン濃度が8パーセント以下であり、反応混合物の固形物含有量が15パーセント以上である連続溶液重合方法である、請求項1に記載の方法。
- 前記重合温度が130℃〜200℃である、請求項4に記載の方法。
- 重合の操作条件下において、未反応のモノマーが反応混合物の再循環の前に反応混合物の残留溶媒から分離されない、請求項1に記載の方法。
- プロピレン転化率が少なくとも75molパーセントである、請求項1に記載の方法。
- プロピレン及びエチレンから本質的になるモノマー混合物が重合される、請求項1に記載の方法。
- 前記共触媒が、20:1〜150:1の、Hfに基づくモル比を提供するための量で存在するアルモキサンである、請求項1に記載の方法。
- 前記アルモキサンがトリ(イソブチル)アルミニウム修飾メタアルモキサン又はトリ(n−オクチル)アルミニウム修飾メタアルモキサンである、請求項9に記載の方法。
- 前記金属錯体が、下記式、
の1つに対応する、請求項1〜10のいずれか一項に記載の方法。 - 前記金属錯体が、下記の錯体、
A)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−1,3−プロパンジイルハフニウム(IV)ジベンジル、
B)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−1,4−ブタンジイルハフニウム(IV)ジベンジル、
C)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシ)−2,4−ペンタンジイルハフニウム(IV)ジベンジル、
D)ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジクロリド、
ビス((2−オキソイル−3−(1,2,3,4,6,7,8,9−オクタヒドロアントラセン−5−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジベンジル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジメチル、
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジクロリド、及び
ビス((2−オキソイル−3−(ジベンゾ−1H−ピロール−1−イル)−5−(メチル)フェニル)−2−フェノキシメチル)−メチレンtrans−1,2−シクロヘキサンジイルハフニウム(IV)ジベンジル
からなる群より選択される、実施形態11に記載の方法。
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