US3897364A — Process for the preparation of catalysts for the …

Claim 1

Independent Claim 261 words

PROCESS FOR THE PREPARATION OF CATALYSTS SUITABLE FOR THE PRODUCTION OF POLYMERS OF ETHYLENE AND ALPHA-OLEFINS AND OF COPOLYMERS OF ETHYLENE WITH ALPHA-OLEFINS, CONSISTING ESSENTIALLY OF A ORGANO-METALLIC COMPOUND AND THE PRODUCT OF INTERACTION BETWEEN A HALOGENATED COMPOUND OF A TRANSITION METAL AND A SOLID GRANULAR SUPPORT, CHARACTERIZED IN THAT AT A TEMPERATURE BETWEEN 100 AND 350*C AND FOR A PERIOD OF 10 TO 30 HOURS, A HALIDE TRANSITION METAL IN GROUPS IVB AND VB OF THE PERIODIC SYSTEM IS CAUSED TO REACT WITH A SOLID GRANULAR SUPPORT OBTAINED BY DEPOSITION OF METALLIC ALUMINUM ON AN ALUMINA, SILICA, SILICO-ALUMINA OR MIXTURES THEREOF WIH A SURFACE AEA AT LEAST GREATER THAN 10 SQ.M/G AND A GRANULOMETRIC DISTRIBUTION OF BETWEEN 1/ TO 150 MICRONS, OBTAINED A AFTER ACTIVATION AT A TEMPERATURE OF BETWEEN 350 AND 900*C FOR A PERIOD OF 2 TO 25 HOURS, SUCH DEPOSITION BEING CARRIED OUT IN SUCH A WAY THAT THE END PRODUCT HAS A CONTENT OF HIGHLY DISPERSED ALUMINUM COMPRISED BETWEEN 0.05 AND 5% BY WEIGHT, THE RELATIVE QUANTITIES OF TRANSIION METAL HALIDE AND SOLID SUPPORT USED IN THE REACTION BEING SO REGULATED THAT THE MOLAR RATIO OF TRANSITION METAL HALIDE TO SUPPORTED METALLIC ALUMINUM IS BETWEEN 100 AND 1000, AND IN THAT, AT A TEMPERATURE OF 20* TO 100*C THE PRODUCT OF SUCH REACTION IS BROUGHT INTO CONTACT WITH AN ORGANOMETALLIC COMPOUND CHAOSEN FROM ALUMINUM TRIALKYLS, HALIDES OF DIALKYL ALUMINUM, OR ZINC DIALKYLS, THE RELATIVE QUANTITIES OF ORGANOMETALLIC COMPOUNDS AND OF FIXED TRANSITION METAL BEING SO REGULATED THAT THEIR MOLAR RATIOS ARE COMPRISED BETWEEN 5 TO 100.

Claim 2

Dependent Claim 261 words

PROCESS FOR THE PREPARATION OF CATALYSTS SUITABLE FOR THE PRODUCTION OF POLYMERS OF ETHYLENE AND ALPHA-OLEFINS AND OF COPOLYMERS OF ETHYLENE WITH ALPHA-OLEFINS, CONSISTING ESSENTIALLY OF A ORGANO-METALLIC COMPOUND AND THE PRODUCT OF INTERACTION BETWEEN A HALOGENATED COMPOUND OF A TRANSITION METAL AND A SOLID GRANULAR SUPPORT, CHARACTERIZED IN THAT AT A TEMPERATURE BETWEEN 100 AND 350*C AND FOR A PERIOD OF 10 TO 30 HOURS, A HALIDE TRANSITION METAL IN GROUPS IVB AND VB OF THE PERIODIC SYSTEM IS CAUSED TO REACT WITH A SOLID GRANULAR SUPPORT OBTAINED BY DEPOSITION OF METALLIC ALUMINUM ON AN ALUMINA, SILICA, SILICO-ALUMINA OR MIXTURES THEREOF WIH A SURFACE AEA AT LEAST GREATER THAN 10 SQ.M/G AND A GRANULOMETRIC DISTRIBUTION OF BETWEEN 1/ TO 150 MICRONS, OBTAINED A AFTER ACTIVATION AT A TEMPERATURE OF BETWEEN 350 AND 900*C FOR A PERIOD OF 2 TO 25 HOURS, SUCH DEPOSITION BEING CARRIED OUT IN SUCH A WAY THAT THE END PRODUCT HAS A CONTENT OF HIGHLY DISPERSED ALUMINUM COMPRISED BETWEEN 0.05 AND 5% BY WEIGHT, THE RELATIVE QUANTITIES OF TRANSIION METAL HALIDE AND SOLID SUPPORT USED IN THE REACTION BEING SO REGULATED THAT THE MOLAR RATIO OF TRANSITION METAL HALIDE TO SUPPORTED METALLIC ALUMINUM IS BETWEEN 100 AND 1000, AND IN THAT, AT A TEMPERATURE OF 20* TO 100*C THE PRODUCT OF SUCH REACTION IS BROUGHT INTO CONTACT WITH AN ORGANOMETALLIC COMPOUND CHAOSEN FROM ALUMINUM TRIALKYLS, HALIDES OF DIALKYL ALUMINUM, OR ZINC DIALKYLS, THE RELATIVE QUANTITIES OF ORGANOMETALLIC COMPOUNDS AND OF FIXED TRANSITION METAL BEING SO REGULATED THAT THEIR MOLAR RATIOS ARE COMPRISED BETWEEN 5 TO 100.

Claim 3

Dependent Claim 75 words

Process according to claim 1, characterised in that the deposition of metallic aluminium takes place by preparing a mixture of a powder of metallic aluminium of a granulometry between 0.1 and 10 microns and alumina, silica, silico-aluminate or mixtures thereof, and by maintaining the said mixture at a temperature above the melting point in the mixture being so regulated that the end product has an aluminium content of between 0.05 and 5 percent by weight.

Claim 4

Dependent Claim 48 words

Process according to claim 2, characterised in that the mixtures are prepared from a metallic aluminium powder of a granulometry between 0.5 and 5 microns and in that such mixtures are maintained at a temperature between 700 and 1000*C for a period of between 10 and 15 hours.

Claim 5

Dependent Claim 25 words

Process according to claim 2, characterised in that the mixtures of aluminium powder and particles of alumina silica silico-aluminate or mixtures thereof are prepared mechanically.

Claim 6

Dependent Claim 50 words

Process according to claim 2, characterized in that the mixtures of aluminum powder and particles of alumina, silica, silico-aluminate or mixtures thereof are prepared by suspension of the powders of aluminum and particles of alumina, silica, silico-aluminate or mixtures thereof in a hydrocarbon solvent, after which the solvent is evaporated.

Claim 7

Dependent Claim 128 words

Process according to claim 1, characterized in that the deposition of metallic aluminum is achieved by impregnation in a fluid bed at a temperature between 20* and 100*C, of the aluminas, silicas, silico-aluminates or mixtures thereof with aluminum hydride or a metallorganic compound of aluminum in solution, followed by evaporation of the solvent at the same temperature as impregnation in a period ranging from 1 to 10 hours, and activation of the product obtained at a temperature above that of decomposition of the hydride or of the metallorganic compound of aluminum for a period of 5 to 20 hours, the quantities of hydride or of metallorganic compound of aluminum being so regulated that the end product has an aluminum content of between 0.05 and 5 percent by weight.

Claim 8

Dependent Claim 64 words

Process according to claim 6, characterised in that the deposition of metallic aluminium is achieved by impregnation at a temperature between 20* and 40*C, evaporation of the solvent over a period of 1 to 10 hours and activation at a temperature at least 30*C above that of decomposition of the hydride or of the metallorganic compound for a period of 10 to 15 hours.

Claim 9

Dependent Claim 30 words

Process according to claim 6, characterised in that in impregnation, solvents for the hydrides are aliphatic or aromatic ethers while solvents for the metallorganic compounds are aliphatic or aromatic hydrocarbons.

Claim 10

Dependent Claim 19 words

Process according to claim 1, characterized in that the transition metal halide used is titanium tetrachloride or vanadium oxychloride.

Claim 11

Dependent Claim 50 words

Process according to claim 1, characterised in that the reaction between transition metal halide and the solid granular support is carried out at 225* to 300*C, the relative quantities of reaction being such that the molar ratio of transition metal halide to supported metallic aluminium is between 150 to 400.

Claim 12

Dependent Claim 62 words

Process according to claim 1, characterized in that said compound chosen from aluminum trialkyls, halides of dialkyl aluminum or zinc dialkyls is used in quantities such that the molar ratios, with respect to the fixed transition metals, are comprised between 10 to 50, the temperature at which these ingredients are brought into contact being regulated in the range from 40* to 100*C.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1978-07-28	1979-01-27	1979-07-29	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1982-07-28	1983-01-27	1983-07-29	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1986-07-28	1987-01-27	1987-07-29	$7700.00	Window Closed / Lapsed

Process for the preparation of catalysts for the polymerization of olefins

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