FI114988B - Etensampolymerisationer - Google Patents

Etensampolymerisationer Download PDF

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FI114988B
FI114988B FI953626A FI953626A FI114988B FI 114988 B FI114988 B FI 114988B FI 953626 A FI953626 A FI 953626A FI 953626 A FI953626 A FI 953626A FI 114988 B FI114988 B FI 114988B
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Brian W S Kolthammer
Robert S Cardwell
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Dow Global Technologies Inc
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Claims (22)

1. Förfarande för framställning av en eten/a-ole-finsampolymerkomposition, kännetecknat av att: 5 (A) eten och ätminstone en annan a-olefin bringas att reagera genom att de bringas i kontakt under lösnings-polymerisationsförhällanden i närvaro av en homogenkata-lytkomposition, som inte alls innehäller aluminiumkokata-lyt eller innehäller endast en liten mängd aluminiumkoka-10 talyt, i ätminstone en reaktor för att framställa en lös-ning av en första sampolymer med en smal kompositionsför-delning och en smal molekylviktsfördelning, (B) eten och ätminstone en annan a-olefin bringas att reagera genom att de bringas i kontakt under lösnings- 15 polymerisationsförhällanden och vid en högre polymerisa-tionsreaktionstemperatur än vad som användes i steg (A) i närvaro av en heterogen Ziegler-katalyt i ätminstone en annan reaktor för att erhälla en lösning frän en andra sampolymer med en bred kompositionsfördelning och en bred 20 molekylviktsfördelning, varvid Ziegler-katalyten omfattar: (i) en fast bärarkomponent, som har härletts frän magnesiumhalid eller kisel, och ·· (ii) en övergängsmetallkomponent, som represente- ras av formlerna:
25 TrXVqiOR1),, TrX'4.qR2q, VOX'3 och VO(OR1)3, i vilka Tr är en metal 1 i grupp IVB, VB eller VIB, " ·. q är 0 eller ett tai som är lika med eller mindre * än 4, X' är en halogen och ’ ! 30 R1 är en alkylgrupp, arylgrupp eller cykloalkyl- grupp med 1-20 kolatomer, och h R2 är en alkylgrupp, arylgrupp, aralkylgrupp eller I substituerad aralkylgrupp, och (C) den första sampolymerlösningen förenas med den 35 andra sampolymerlösningen för att framställa en polymer- 114988 lösning med hög temperatur, vilken omfattar eten/a-olefinsampolymerkompositionen, ooh (D) lösningsmedlet avlägsnas frän den i steg (C) erhällna polymerlösningen och eten/a-olefinsampolymer-5 kompositionen tas tili vara.
2. Eten/a-olefinsampolymerkomposition, känneteck-nad av att den har framställts med förfarandet enligt patent kr av 1.
3. Förfarande enligt patentkrav 1, kännetecknat av 10 att a-olefinet i stegen (A) och (B) är i vartdera fallet 1-okten.
4. Eten/l-oktensampolymerkomposition, kännetecknad av att den har framställts med förfarandet enligt patentkrav 3 . 15 5. Förfarande enligt patentkrav 1, kännetecknat av att homogenkatalytkompositionen omfattar ett metallkoordi-nationskomplex, som omfattar en metall frän grupp 4 i grundämnenas periodiska system och en delokaliserad π-bunden del, som är substituerad med en tvingande del, var-20 vid komplexet har en tvingad geometri runt metallatomen sä att vinkein vid metallen mellan den delokaliserade substi-.* tuerade π-bundna delen och ätminstone en äterstäende sub- · stituent är mindre än vinkein i ett liknande komplex, som innehäller en liknande π-bunden del som saknar den tving-25 ande substituenten, och dessutom under förutsättning att hos komplex som omfattar flera än en delokaliserad substituerad π-bunden del är endast en av dem för varje metall-atom i komplexet en cyklisk, delokaliserad substituerad π-, bunden del. ; 30 6. Förfarande enligt patentkrav 5, kännetecknat av i * att homogenkatalytkompositionen vidare omfattar en aktive- ' rande kokat älyt. *; i 7. Förfarande enligt patentkrav 5, kännetecknat av att metallkoordinationskomplexet motsvarar formeln: '! 35 114988 n cp*-ώ där: M är en metall frän grupp 4 i grundämnenas perio-diska system;
5 Cp* är en cyklopentadienyl- eller substituerad cyklopentadienylgrupp, som är bunden vid M med en h5-bindningstyp; Z är en del som omfattar bor eller en atom frän grupp 14 i grundämnenas periodiska system och valbart sva-10 vei eller syre, vilken del har högst 20 icke-väteatomer, och valbart bildar Cp* och Z tillsammans ett förenat ring-system; X är oberoende vid varje enskilt tillfälle en an-jonisk ligandgrupp, som har högst 30 icke-väteatomer; 15 n är 1 eller 2; och Y är en vid Z- eller M-delen bunden anjonisk eller icke-anjonisk ligandgrupp, som omfattar kväve, fosfor, ; syre eller svavel och med högst 20 icke-väteatomer, vai- * · ·* bart bildar Y och Z tillsammans ett förenat ringsystem. 2 0 8. Förfarande enligt patentkrav 5, kännetecknat av * att metallkoordinationskomplexet motsvarar formeln: t R· : X(x,n R* 114988 där: R' vid varje enskilt tillfälle väljs oberoende frän gruppen: väte, alkyl, aryl och silyl och kombinatio-ner av dessa, som har högst 20 icke-väteatomer; 5. vid varje enskilt tillfälle väljs oberoende frän gruppen: hydrid, halo, alkyl, aryl, silyl, aryloxi, al- koxi, amid, siloxi och kombinationer av dessa, som har högst 20 icke-väteatomer; Y är -O-, -S-, -NR1-, -PR1- eller en neutral tvä 10 elektroners avgivarligand, som har valts frän gruppen:OR1, SR1, NR12 eller PR12; M har definierats ovan; och Z är SiR12, CR12, SiR12SiR12, CR12CR12, CR1=CR1, CR12SiR12, BR1; där
15 R1 vid varje enskilt tillfälle oberoende har valts frän gruppen: väte-, alkyl-, aryl-, silyl-, halogenerade alkyl-, halogenerade arylgrupper, som har högst 20 icke-väteatomer, och kombinationer av dessa, eller tvä eller flera R1-grupper frän Y, Z eller bäde Y och Z bildar ett 20 förenat ringsystem; och n är 1 eller 2.
9. Förfarande enligt patentkrav 5, kännetecknat av att metallkoordinationskomplexet är en amidosilan- eller • amidoalkandiylförening, som motsvarar formeln: R1 : /L/V _^(eri) / <4 m v R--^ f —^N-R· Γ R’ ^(x) • : n R’ • 1 . 25 där: » ... M är titan, zirkonium eller hafnium bundet med en h5-bindningsmodell vid cyklopentadienylgruppen; 114988 R vid varje enskilt tillfälle har valts frän grup-pen: väte, alkyl och aryl och kombinationer av dessa, som har högst 7 kolatomer, eller silyl; E är kisel eller kol;
5 X är oberoende vid varje enskilt tillfälle hydrid, halo, alkyl, aryl, aryloxi eller alkoxi, som har högst 10 kol, eller silyl; m är 1 eller 2; och n är 1 eller 2. 10 10. Förfarande enligt patentkrav 5, kännetecknat av att metallkoordinationskomplexet är en jonisk katalyt med en begränsande laddningsseparerad struktur som motsva-rar formeln: Z*-- Y / / .. Cp*·- M + XA \ (X)n-l 15 där: ' S M är en metall frän grupp 4 i grundämnenas perio- : .: diska system; Cp* är en cyklopentadienyl- eller substituerad cyklopentadienylgrupp, som är bunden vid M med en h5- 20 bindningsmodell ; Z är en del som omfattar bor eller en atom frän grupp 14 i grundämnenas periodiska system och valbart sva-vel eller syre, vilken del har högst 20 icke-väteatomer, ; och valbart bildar Cp* och Z tillsammans ett förenat ring- ' t .* 2 5 system; - I X är oberoende vid varje enskilt tillfälle en an- . .: jonisk ligandgrupp, som har högst 30 icke-väteatomer; n är 1 eller 2; och *1 XA* ‘ är -X(B(C6F5)3) . 114588
11. Förfarande enligt patentkrav 1, kännetecknat av att homogenkatalytkompositionens reaktivitetsförhällan-de är under halften av heterogenkatalytens motsvarande.
12. Förfarande för framställning av en eten/a-5 olefinsampolymerkompositiön, kännetecknat av att: (A) eten och ätminstone en annan a-olefin polyme-riseras i ett lösningsförfarande vid lämpliga lösningspo-lymerisationstemperaturer och -tryck i ätminstone en reak-tor, som innehäller en homogenkatalytkomposition, som an-10 tingen inte alls innehäller aluminiumkokatalyt eller innehäller endast en liten mängd aluminiumkokatalyt, för att framställa en första sampolymerlösning, som omfattar en första sampolymer med en smal kompositionsfördelning och en smal molekylviktsfördelning, och 15 (B) sampolymerlösningen (A) förs sekventiellt tili ätminstone en annan reaktor, som innehäller en heterogen Ziegler-katalyt, eten och ätminstone en annan a-olefin under lösningspolymerisationsförhällanden och vid en högre polymerisationstemperatur än vad som användes i steg (A) 20 för att bilda en polymerlösning med hög temperatur, som omfattar eten/a-olefinsampolymerenkompositionen, varvid ·* Ziegler-katalyten omfattar: · (i) en fast bärarkomponent, som har härletts frän magnesiumhalid eller kisel, och : 25 (ii) en övergängsmetallkomponent, som represente- ras av formlerna: » ; TrX' 4-g (OR1) q, TrX'4.gR2q, VOX'3 och VO (OR1) 3, i vilka Tr är en metall i grupp IVB, VB eller VIB, q är 0 eller ett tai som är lika med eller mindre ‘ ! 30 än 4, X' är en halogen och R1 är en alkylgrupp, arylgrupp eller cykloalkyl-grupp med 1-20 kolatomer, och • § R2 är en alkylgrupp, arylgrupp, aralkylgrupp eller 35 substituerad aralkylgrupp, och 114986 (C) lösningsmedlet avlägsnas frän polymerlösningen i steg (B) och eten/a-olefinsampolymerkompositionen tas tili vara.
13. Eten/a-olefinsampolymerkomposition, känneteck-5 nad av att den har framställts med förfarandet enligt pa- tentkrav 12.
14. Förfarande enligt patentkrav 12, kännetecknat av att a-olefinet är 1-okten.
15. Eten/1-oktensampolymerkomposition, känneteck-10 nad av att den har framställts med förfarandet enligt patentkrav 14 .
16. Förfarande enligt patentkrav 12, kännetecknat av att homogenkatalytkompositionen omfattar ett metallko-ordinationskomplex, som omfattar en metall frän grupp 4 i 15 grundämnenas periodiska system och en delokaliserad π-bunden del, som är substituerad med en tvingande del, var-vid komplexet har en tvingad geometri runt metallatomen sä att vinkein vid metallen mellan den delokaliserade substi-tuerade π-bundna delen och ätminstone en äterstäende sub-20 stituent är mindre än vinkein i ett liknande komplex, som innehäller en liknande π-bunden del som saknar den tvingande substituenten, och dessutom under förutsättning att • hos komplex som omfattar flera än en delokaliserad substi- tuerad π-bunden del är endast en av dem för varje metall-25 atom i komplexet en cyklisk, delokaliserad substituerad π-bunden del.
17. Förfarande enligt patentkrav 12, kännetecknat av att homogenkatalytkompositionen vidare omfattar en ak-tiverande kokatalyt. 30 18. Förfarande enligt patentkrav 16, kännetecknat » · av att metallkoordinationskomplexet motsvarar formeln: » . - · t 114988 V 6 6 π cp*- där: M är en metall frän grupp 4 i grundämnenas periodi ska system;
5 Cp* är en cyklopentadienyl- eller substituerad cyklopentadienylgrupp, som är bunden vid M med en h5-bindningstyp; Z är en del som omfattar bor eller en atom frän grupp 14 i grundämnenas periodiska system och valbart sva-10 vei eller syre, vilken del har högst 20 icke-väteatomer, och valbart bildar Cp* och Z tillsammans ett förenat ring-system; X är oberoende vid varje enskilt tillfälle en an-jonisk ligandgrupp, som har högst 30 icke-väteatomer; 15 n är 1 eller 2; och Y är en vid Z- eller M-delen bunden anjonisk eller .· icke-anj onisk ligandgrupp, som omfattar kväve, fosfor, » ·· syre eller svavel och med högst 20 icke-väteatomer, val- : bart bildar Y och Z tillsammans ett förenat ringsystem. 20 19. Förfarande enligt patentkrav 16, kännetecknat av att metallkoordinationskomplexet motsvarar formeln: : : R* : "V R* « 114988 där: R' vid varje enskilt tillfälle väljs oberoende frän gruppen: väte, alkyl, aryl och silyl och kombinatio-ner av dessa, som har högst 20 icke-väteatomer; 5. vid varje enskilt tillfälle väljs oberoende frän gruppen: hydrid, halo, alkyl, aryl, silyl, aryloxi, al- koxi, amid, siloxi och kombinationer av dessa, som har högst 20 icke-väteatomer; Y är -O-, -S-, -NR*-, -PR*- eller en neutral tvä 10 elektroners avgivarligand, som har valts frän gruppen: OR*, SR*, NR*2 eller PR*2; M har definierats ovan; och Z är SiR*2, CR*2, SiR*2SiR*2, CR*2CR*2, CR*=CR*, CR*2SiR*2, BR*; där
15 R* vid varje enskilt tillfälle oberoende har valts frän gruppen: väte-, alkyl-, aryl-, silyl-, halogenerade alkyl-, halogenerade arylgrupper, som har högst 20 icke-väteatomer, och kombinationer av dessa, eller tvä eller flera R*-grupper frän Y, Z eller bäde Y och Z bildar ett 20 förenat ringsystem; och n är 1 eller 2.
20. Förfarande enligt patentkrav 16, kännetecknat , .* av att metallkoordinationskomplexet är en amidosilan- el- · ler amidoalkandiylförening, som motsvarar formeln: R· : S X ^(ERA) • ____— 2 m R* ^(X) / n .: R ’ 25 där: • * M är titan, zirkonium eller hafnium bundet med en h5-bindningsmodell vid cyklopentadienylgruppen; 1 · 1 1 4988 R vid varje enskilt tillfälle har valts frän grup-pen: väte, alkyl och aryl och kombinationer av dessa, som har högst 7 kolatomer, eller silyl; E är kisel eller kol;
5 X är oberoende vid varje enskilt tillfälle hydrid, halo, alkyl, aryl, aryloxi eller alkoxi, som har högst 10 kol, eller silyl; m är 1 eller 2; och n är 1 eller 2.
21. Forfarande enligt patentkrav 16, kännetecknat av att metallkoordinationskomplexet är en jonisk katalyt med en begränsande laddningsseparerad struktur som motsva-rar formeln: z —-y / / .. Cp* ·- M 4 XA \ (X)n-l 15 där: , ·, M är en metal 1 frän grupp 4 i grundämnenas perio- . diska system; .- » Cp* är en cyklopentadienyl- eller substituerad cyklopentadienylgrupp, som är bunden vid M med en h5- ·’ 2 0 bindningsmodell; Z är en del som omfattar bor eller en atom frän • · grupp 14 i grundämnenas periodiska system och valbart sva- vel eller syre, vilken del har högst 20 icke-väteatomer, och valbart bildar Cp* och Z tillsammans ett förenat ring- 25 system; . X är oberoende vid varje enskilt tillfälle en an- jonisk ligandgrupp, som har högst 30 icke-väteatomer; n är 1 eller 2; och XA* · är -X(B(C6F5)3) · 114988
22. Förfarande enligt patentkrav 12, kännetecknat av att homogenkatalytkompositionens reaktivitetsförhallan-de är under halften av heterogenkatalytens motsvarande. » »
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DE69433347D1 (de) 2003-12-24
PT681592E (pt) 2001-01-31
HU225374B1 (en) 2006-10-28
RU95116450A (ru) 1997-06-10
US5844045A (en) 1998-12-01
HU9502022D0 (en) 1995-09-28
NO952995D0 (no) 1995-07-28
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CZ196395A3 (en) 1995-12-13
ATE254635T1 (de) 2003-12-15
TW316268B (sv) 1997-09-21
PL175108B1 (pl) 1998-11-30
CA2153978C (en) 2005-07-12
BR9405715A (pt) 1995-11-28
DE69425556D1 (en) 2000-09-21
KR100301978B1 (ko) 2001-11-14
CZ288678B6 (cs) 2001-08-15
DE69433347T2 (de) 2004-04-15
AU688308B2 (en) 1998-03-12
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RU2113443C1 (ru) 1998-06-20
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