Method of polymerizing butadiene-1, 3-hydrocarbons

Claim 1

A METHOD FOR POLYMERIZING MONOMERIC MATERIAL CONSISTING OF ISOPRENE TO FORM A POLYISOPRENE HIGH IN MOLECULAR WEIGHT, LOW IN GEL AND IN WHICH AT LEAST 90% OF THE ISOPRENE UNITS ARE JOINED CIS-1,4 COMPRISING MIXING SAID MONOMERIC ISOPRENE WITH A REACTION MEDIUM CONSISTING OF AN INERT ALIPHATIC HYDROCARBON BOILING IN THE RANGE OF -10* TO 10*C. AND AN ACTIVE CATALYST PREPARED BY ADDING TO SAID INERT HYDROCARBON, IN THE FOLLOWING ORDER, (1) FROM ABOUT 1 TO ABOUT 20 GRAM MILLIMOLES OF A TRIALKYL ALUMINUM PER LITER OF SAID MEDIUM, (2) A TRIALKYL AMINE IN WHICH EACH ALKYL GROUP CONTAINS FROM 2 TO 12 CARBON ATOMS, (3) A CONDENSATE OF AN ALKYL PHENOL AND ETHYLENE OXIDE HAVING A MOLECULAR WEIGHT BETWEEN 400 AND ABOUT 1500, AND (4) FROM ABOUT 1 TO ABOUT 20 GRAM MILLIMOLES OF TITANIUM TETRACHLORIDE PER LITER OF SAID REACTION MEDIUM, THE SAID INGREDIENTS (1), (2) AND (3) BEING MIXED TOGETHER BEFORE ADDITION OF SAID INGREDIENT (4), THE SAID INGREDIENTS (1) AND (2) BEING ADDED TO SAID ALIPHATIC HYDROCARBON IN A MOLAR RATION AMINE: ALUMINUM BETWEEN ABOUT 0.03:1 AND ABOUT 0.5:1, THE SAID INGREDIENTS (1) AND (3) BEING ADDED TO SAID ALIPHATIC HYDROCARBON IN A MOLAR RATION CONDENSATE: ALUMINUM BETWEEN 0.001:1 AND ABOUT 0.3:1, SAID INGREDIENTS (1) AND (4) BEING ADDED TO SAID ALIPHATIC HYDROCARBON IN A MOLAR RATIO TITANIUM:ALUMINUM BETWEEN ABOUT 0.75:1 AND 1.1:1, AND THE SAID MONOMERIC ISOPRENE CONSTITUTING BETWEEN ABOUT 5 AND 30%/WT. OF THE TOTAL RESULTING MIXTURE, AND CARRYING OUT THE POLYMERIZATION OF SAID MONOMERIC ISOPRENE IN THE SAID RESULTING MIXTURE WHILE REFLUXING SAID ALIPHATIC HYDROCARBON.

Claim 2

A METHOD FOR POLYMERIZING MONOMERIC MATERIAL CONSISTING OF ISOPRENE TO FORM A POLYISOPRENE HIGH IN MOLECULAR WEIGHT, LOW IN GEL AND IN WHICH AT LEAST 90% OF THE ISOPRENE UNITS ARE JOINED CIS-1,4 COMPRISING MIXING SAID MONOMERIC ISOPRENE WITH A REACTION MEDIUM CONSISTING OF AN INERT ALIPHATIC HYDROCARBON BOILING IN THE RANGE OF -10* TO 10*C. AND AN ACTIVE CATALYST PREPARED BY ADDING TO SAID INERT HYDROCARBON, IN THE FOLLOWING ORDER, (1) FROM ABOUT 1 TO ABOUT 20 GRAM MILLIMOLES OF A TRIALKYL ALUMINUM PER LITER OF SAID MEDIUM, (2) A TRIALKYL AMINE IN WHICH EACH ALKYL GROUP CONTAINS FROM 2 TO 12 CARBON ATOMS, (3) A CONDENSATE OF AN ALKYL PHENOL AND ETHYLENE OXIDE HAVING A MOLECULAR WEIGHT BETWEEN 400 AND ABOUT 1500, AND (4) FROM ABOUT 1 TO ABOUT 20 GRAM MILLIMOLES OF TITANIUM TETRACHLORIDE PER LITER OF SAID REACTION MEDIUM, THE SAID INGREDIENTS (1), (2) AND (3) BEING MIXED TOGETHER BEFORE ADDITION OF SAID INGREDIENT (4), THE SAID INGREDIENTS (1) AND (2) BEING ADDED TO SAID ALIPHATIC HYDROCARBON IN A MOLAR RATION AMINE: ALUMINUM BETWEEN ABOUT 0.03:1 AND ABOUT 0.5:1, THE SAID INGREDIENTS (1) AND (3) BEING ADDED TO SAID ALIPHATIC HYDROCARBON IN A MOLAR RATION CONDENSATE: ALUMINUM BETWEEN 0.001:1 AND ABOUT 0.3:1, SAID INGREDIENTS (1) AND (4) BEING ADDED TO SAID ALIPHATIC HYDROCARBON IN A MOLAR RATIO TITANIUM:ALUMINUM BETWEEN ABOUT 0.75:1 AND 1.1:1, AND THE SAID MONOMERIC ISOPRENE CONSTITUTING BETWEEN ABOUT 5 AND 30%/WT. OF THE TOTAL RESULTING MIXTURE, AND CARRYING OUT THE POLYMERIZATION OF SAID MONOMERIC ISOPRENE IN THE SAID RESULTING MIXTURE WHILE REFLUXING SAID ALIPHATIC HYDROCARBON.