Texas Alkyls, Inc

Available from Texas Alkyls Inc., Stauffer Chemical Co., Specialty Chemical Division, Westport, CT 06880. Solutions of various organoaluminum reagents in hydrocarbon solvents may also be purchased directly from Texas Alkyls Inc. 

All polymerizations were carried out in a stainless steel enclosure (8). The purity and analysis of isobutylene, methyl chloride, and aluminum chloride have been described (9). The trialkylaluminums (Texas Alkyls, Inc.) were purified by distillation before use AlEt2Cl was treated with NaCl at 80°C. for 2 hours to remove traces of AlEtCl2. 

Materials. Ethylaluminum dichloride, Texas Alkyls Inc., obtained as a 25% solution in hexane, was diluted with the appropriate amount of benzene (dried over silica gel) to form a 0.2M solution. 

Materials. Alkylaluminum compounds, supplied by Texas Alkyls, Inc., were used without further purification. Analytical data supplied by the manufacturer showed all alkyls to be of greater than 90% purity. The diisobutyl-aluminum hydride was prepared by heating the commercial triisobutyl-aluminum at 130° C. and pumping off the gases evolved. Analysis of the product showed 16.8% aluminum as compared to the theoretical value of 18.97%. 

The alkyrlaluminums were obtained from Texas Alkyls Inc. and purified by vacuum distillation in nitrogen atmosphere. B.P. °C/mm Hg MCaAl 60768.5 EtjAl 977100 Et AlCl 125-126750mm MejAlCl 847200. Prior to distillation the dialkylaluminum chlorides were stirred over dry sodium chloride at 80° C for 2 hrs. to remove alkyl-aluminum dichlorides. The distilled dialkylaluminum chlorides were stored over sodium chloride to prevent the accumulation of the dihalide. 

MeAlClj (Texas Alkyls Inc.) was obtained as a 25% solution in n-hexane, filtered under nitrogen to remove suspended impurities. The hexane was distilled off and the MeAlCl2 was purified by repeated crystallization from n-pentane at —50°. For polymerization reactions <1.0% solution in methyl chloride was used. 

In closing, I would be remiss if I did not acknowledge my former colleagues at Texas Alkyls, Inc. (now Akzo Nobel) with whom I toiled for more than 30 years producing and marketing the metal alkyls that are so crucial to the polyolefins... 

Diethylaluminum chloride, C1A1(C2H5)2. Mol. wt. 120.56. Suppliers ROC/R1C, Texas Alkyls, Inc. 

DUsobutylaluminum hydride, (CH3)2CHCH2AlCH,CH(CHa)j. Mol. wt. 142.21, b.p, 140°/4 mm. Supplier (i lb. unit in pressure cylinder) Texas Alkyls Inc. (Techn, Bull. Pi 640,928, 1964). Being a liquid, the reagent is dissolved more easily than lithium aluminum hydride. Suitable solvents are ether, benzene, toluene, and cyclohexane. Tetrahydrofurane forms a complex with the hydride and is not suitable. Since the reagent is pyrophoric in concentrated form, all operations with this and other organoaluminum compounds must be conducted in an oxygen-free atmosphere. ... 

Texas Alkyls, Inc., 6910 Fannin St., Suite 300A, Houston, Texas 77025 Thallium Ltd., Carrow Road, Norwich, England... 

A nonpyrophoric solution of 25% triethylaluminum in toluene convenient for use in this synthesis is available from Texas Alkyls, Inc., P.O. Box 600, Deer Park, Tex. 77536. 

---