Abstract:
Aluminium trialkyls are prepared by heating an alkylaluminium halide of the general formula AlX2Y, wherein X represents an alkyl radical and Y represents a halogen or vice versa, or a mixture thereof, with a finely divided magnesium or magnesium-aluminium alloy at a temperature up to 180 DEG C. Alloys having the approximate composition Mg3Al2 to Mg2Al, i.e., alloys containing approximately 57 to 65 per cent of magnesium and from 43 to 35 per cent of aluminium are particularly useful. A dialkylaluminium halide used in the above process may be prepared by reacting an alkyl halide with an aluminium-magnesium alloy containing approximately 70 per cent aluminium and 30 per cent magnesium, and a mixture of a monoalkylaluminium dihalide and a dialkylaluminium monohalide used in the above process may be prepared by the reaction of aluminium with an alkyl halide-the aluminium used in this modification of the process may be obtained wholly or in part from the reaction product resulting from a previous reaction of a mixture of alkylaluminium halides with magmesium or magnesium-aluminium alloy referred to above. In the example, triethylaluminium is prepared by reacting diethylaluminium chloride and an alloy of the composition Mg3Al2. Specification 767,400 is referred to.
Abstract:
Alkyl aluminium compounds of general formula AlR3 in which R represents a lower alkyl radical are converted into compounds having higher alkyl radicals than the starting material by a process in which they are sprayed into a stream of ethylene being conveyed at a flow velocity of 1 to 50 m/minute and with a residence time of 1 to 20 minutes through a reaction chamber maintained at a temperature between 120 DEG and 200 DEG C., the reaction chamber having a diameter up to 3 cm. and a length at least 1,000 times the diameter. It is preferred that the starting material should contain at least two carbon atoms. The apparatus comprises a reactor A, a condenser B, a pressure separator C, a regulating valve D, a flow meter E, a circulation compressor F, a pump G for liquid under pressure and a mixing component H. The reactor A consists of a copper tube, suitable dimensions being a diameter of 8 mm. and length 40 metres (capacity 2 litres). This is wound with a 3% inclination on to an iron tube b of diameter about 50 cms. and open top and bottom. The assembly is placed in an oil bath c and a stirrer d disposed inside the iron tube to force the oil downwards in the tube and upwards through the annular gap between the iron tube b and the wall of the bath c. This ensures that the reactor is continuously washed by the oil in the bath. An immersion heater e is provided for heating the oil. The ethylene stream is fed in via the compressor F to the mixing unit H where it entrains the alkyl aluminium starting material in atomized form. It passes through the reactor, unreacted ethylene being separated in the separator C and recirculated, the growth product remaining behind and drawn off as necessary. Details of operation are given in the Specification. Specifications 713,081, 742,642 and 763,824 are referred to.