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Ep 0744414 B1 Europaisches Patentamt (19) European Patent Office Office europeenpeen des brevets ^ £P 0 744 414 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) intci.e: C08F 10/00, C08F 4/602, of the grant of the patent: C07F 5/06 14.07.1999 Bulletin 1999/28 (21) Application number: 96107520.7 (22) Date of filing: 10.05.1996 (54) Aluminoxanate compositions Aluminoxanate-Zusammensetzungen Compositions d'aluminoxanate (84) Designated Contracting States: • Wiegand, Karl E. BE DE FR GB IT NL Baton Rouge, LA 70820 (US) (30) Priority: 26.05.1995 US 452170 (74) Representative: Schwabe - Sandmair - Marx Stuntzstrasse 16 (43) Date of publication of application: 81677 Miinchen (DE) 27.11.1996 Bulletin 1996/48 (56) References cited: (73) Proprietor: ALBEMARLE CORPORATION EP-A- 0 360 492 US-A- 5 157 137 Baton Rouge, Louisiana 70801 (US) • DATABASE WPI Derwent Publications Ltd., (72) Inventors: London, GB; AN 72-441 72t XP002012495 • Sangokoya, Samuel A. "Organic aluminium cpds production..." & Baton Rouge, LA 70815 (US) JP-A-470 240 01 1 (SHOWA DENKO) • Howie, Milham S. • DATABASE WPI Derwent Publications Ltd., Baton Rouge, LA 70810 (US) London, GB; AN 72-56272t XP002012496 • Simms, Patrick G. "Organo-aluminium cpds used as Baton Rouge, LA 70817 (US) polymerization catalysts" & JP-A-47 024 011 (SHOWA DENKO) DO ^- ^> ^> Is- Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice the Patent Office of the Notice of shall be filed in o to European opposition to European patent granted. opposition a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. a. 99(1) European Patent Convention). LU Printed by Jouve, 75001 PARIS (FR) 1 EP0 744 414 B1 2 Description 5,157,008. Besides MAO, non-limiting examples of hy- drocarbylaluminoxanes for use in the invention include [0001] The invention relates generally to aluminoxane ethylaluminoxanes (EAO), isobutylaluminoxanes derivatives which are useful components of olefin po- (IBAO), n-propylaluminoxanes, n-octylaluminoxanes, lymerization catalysts and more particularly to alumi- 5 and the like. The hydrocarbylaluminoxanes can also noxanate compositions which are the reaction products contain up to about 20 mole percent (based on alumi- of aluminoxanes, such as methylaluminoxane, and cer- num) of moieties derived from amines, alcohols, ethers, tain salts of polyoxy-compounds such as sodium alumi- esters, phosphoric and carboxylic acids, thiols, alkyl dis- nate and lithium silicate. iloxanes and the like to improve activity, solubility and/ [0002] Aluminoxanes are used in combination with 10 or stability. various types of metallocenes and/or transition metal [0007] The aluminoxanes can be prepared as known compounds to catalyze olefin oligomerization and po- in the art by the partial hydrolysis of trialkylaluminum lymerization. These catalyst components can be sup- compounds. The trialkylaluminum compounds can be ported on inert solid carriers such as metal oxides, for hydrolyzed by adding either free water or water contain- example silica or alumina, for use in heterogeneous and 15 ing solids, which can be either hydrates or porous ma- gas phase polymerizations. It has now been found that terials which have absorbed water. Because it is difficult aluminoxanes can be reacted with certain salts of poly- to control the reaction by adding water per se, even with oxy-compounds to form novel catalyst compositions vigorous agitation of the mixture, the free water is pref- which are useful in making polymeric olefinic products. erably added in the form of a solution or a dispersion in The polymers also have unique properties. 20 an organic solvent. Suitable hydrates include salt hy- [0003] In accordance with this invention there is pro- drates such as, for example, CuS04»5H20, Al2 vided an aluminoxanate composition comprising the re- (S04)3»18H20, FeS04»7H20, AICI3»6H20, Al action product of an aluminoxane and a salt selected (N03)3»9H20, MgS04»7H20, MgCI2»6H20, from the group consisting of alkali metal, alkaline earth ZnS04»7H20, Na2SO4»10H2O, Na3P04»12H20, Li- metal, ammonium, phosphonium and sulfonium salts of 25 Br»2H20, LiCI-1 H20, Lil»2H20, Lil»3H20, KF»2H20, Na- Group 1 3 to 1 6 element containing polyoxy-compounds, Br»2H20 and the like and alkali or alkaline earth metal which product contains from about 0.01 to 5.0 moles of hydroxide hydrates such as, for example, NaOH»H20, salt per mole of aluminum in said aluminoxane. NaOH»2H20, Ba(OH)2»8H20, KOH»2H20, [0004] Also provided is an olefin polymerization cata- CsOH»1H20, LiOH»1H20 and the like. Mixtures of any lyst comprising (a) the solid reaction product of an alu- 30 of the above hydrates can be used. The mole ratios of minoxane and an alkali metal, alkaline earth metal, am- free water or water in the hydrate or in porous materials monium, phosphonium or sulfonium salt of a Group 13 such as alumina or silica to total alkyl aluminum com- to 16 element containing polyoxy-compound, and (b) a pounds in the mixture can vary widely, such as for ex- transition, lanthanide or actinide metal compound. ample from 2:1 to 1:4 with ratios of from 4:3 to 1:3.5 [0005] Also provided is a process for polymerizing an 35 being preferred. olefin comprising contacting an olefin with the catalyst, [0008] Such hydrocarbylaluminoxanes and process- as defined above, under polymerization conditions. es for preparing hydrocarbylaluminoxanes are de- [0006] Hydrocarbylaluminoxanes may exist in the scribed, for example, in U.S. Patent Nos. 4,908,463; form of linear or cyclic polymers with the simplest mon- 4,924,018; 5,003,095; 5,041,583; 5,066,631; omeric compounds being a tetraalkylaluminoxane such 40 5,099,050; 5,157,008; 5,157,137; 5,235,081; as tetramethylaluminoxane, (CH3)2AIOAI(CH3)2, or 5,248,801, and 5,371,260. The methylaluminoxanes tetraethylaluminoxane, (C2H5)2AIOAI(C2H5)2. The com- contain varying amounts, of from 5 to 35 mole percent, pounds preferred for use in olefin polymerization cata- of the aluminum value as unreacted trimethylaluminum. lysts are oligomeric materials, sometimes referred to as Preferably the aluminum content as trimethylaluminum polyalkylaluminoxanes, which usually contain about 4 45 is less than about 23 mole percent of the total aluminum to 20 of the repeating units: value, and more preferably less than about 20 mole per- cent. [0009] The hydrocarbylaluminoxanes are reacted n with certain salts of polyoxy-compounds to form novel so I aluminoxane compositions which are referred to herein {A1-0-) as aluminoxanates. When these aluminoxanates are combined with metallocenes and/or other transition metal compounds, solid granular olefin polymerization where R is C-|-C10 alkyl and especially preferred are catalysts are typically formed which are, in effect, solid polymethylaluminoxanes (MAOs). The methylalumi- 55 catalyst compositions useful as heterogeneous polym- noxanes can contain some higher alkyl groups to im- erization catalysts for slurry, bulk or gas phase process- prove their solubility. Such modified methylaluminox- es. anes are described, for example, in U.S. Patent No. [0010] The salts of polyoxy-compounds for use in 2 3 EP0 744 414 B1 4 forming the compositions of the invention include alkali with 20°C to 100°C being preferred. metal, alkaline earth metal (Groups 1 and 2 elements of [0013] A notable result of methylaluminoxanate for- the new IUPAC notation for the Periodic Table, for ex- mation is that the solid product contains no trimethyla- ample, Li, Na, K, Cs, Mg, Ca, Ba), and ammonium, luminum as indicated by pyridine titration. It should also phosphonium, or sulfonium salts of Group 13 to 16 ele- s be noted that the variability in trimethylaluminum con- ment containing polyoxy-compounds, for example, tent of methylaluminoxane is probably the major source polyoxy-compounds which contain elements such as Al, of inconsistency in previously known supported catalyst B, Ga, C, Si, Ge, P, As, S and Se, which salts can be systems. Therefore, this invention provides a means to either anhydrous or moderately hydrated (1 to 6 weight avoid this inconsistency. percent H20). Non-limiting examples of such salts in- 10 [0014] The aluminoxanates can be used in combina- elude NaAI02, LiAI02, Na2C03, Na3P04, Li2SD3, tion with metallocenes and/or transition metal com- Na2Si03, Li2(C02)2, LiB02, Li2B407, LiN03, K2As04, pounds to provide olefin polymerization catalysts. As LiAI(Si03)2, LiC6H5C02, NaCF3C02, Mg(C2H302)2, used in this application, the term "metallocene" includes NH4AI(S04)2, (NH4)2B407, (PH4)2S04, (NH4)2Se03, metal derivatives which contain at least one cyclopen- and the like. The ammonium, phosphonium and sulfo- 15 tadienyl moiety. Suitable metallocenes are well known nium salt cations can include their organosubstituted in the art include the metallocenes of Groups 3, 4, 5, 6, analogs, for example, tetraalkyl, tetra (mixed) alkyl, lanthanide and actinide metals, for example, the metal- tetraaryl, and tetra (aryl, alkyl) substituted cations such locenes which are described in U.S. Patent Nos. as tetraethylammonium, tetraphenylammonium, 2,864,843; 2,983,7402,983,740; 4,665,0464,665,046; 4,874,8804,874,880; tetrabenzylammonium, dimethyldiphenylammonium as 20 4,892,851; 4,931,4174,931,417; 4,952,7134,952,713; 5,017,7145,017,714; well as the corresponding phosphonium and sulfonium 5,026,798; 5,036,0345,036,034; 5,064,8025,064,802; 5,081,2315,081,231; analogs. Some of these salts are not readily available 5,145,819; 5,162,2785,162,278; 5,245,0195,245,019; 5,268,4955,268,495; but can be derived from the more readily available spe- 5,276,208; 5,304,5235,304,523; 5,324,8005,324,800; 5,329,0315,329,031; cies by ion exchange reactions.
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