Determination of Tetraethylgermanium Synthesis Feasibility

Chris Riley

Introduction:
Tetraethylgermanium is used in the fiber optics industry and in the
semiconductor / nuclear industries. It is created by reacting :

Diethylzing + Germanium Tetrachloride

2Zn(C2H5)2 + GeCl4 = Ge(C2H5)4 + 2ZnCl2

Reaction:

Diethylzinc is extremely flammable, and ignites in the presence of air, and

explodes in the presence of water. 100mL of unpurified DEZ is $99.40

Germanium Tetrachloride is unstable, carcinogenic and very reactive. 5 grams of

GeCl4 is $94.20

Equipment Cost: Small scale: ~$200,000 or more. Large scale: ~$1,000,000 or

more, not including the costs of the raw materials.

Safety precautions: Ventilation, fire storage, increased insurance, listing under

EPA and OSHA as potential explosion hazard, advanced protocols for spill or
fire/explosion incident, training. Flame/heat proof vessels capable of
withstanding the use of heavy acids and bases [hastelloy], fume control, gas
storage and dehydration tanks and areas, strong acid storage.

The diethylzinc must be purified and absolutely be without the presence of air,
oxygen, or water. Ethyl iodide is mixed with 25g of Zinc dust and 200g of Copper
under hydrogen gas to get to 500-600 degrees Fahrenheit. The Copper and Zinc
mixture is placed and reacted with the heated ethyl iodide to 100 F.
The resulting compound must be pulverized, and mixed with sand that has been
boiled in Hydrochloric Acid. This is this placed into the vessels of A and B.
CO2 has to be completely dried, and is dried with Calcium Chloride, Sulfuric Acid
and finally by Phosphorous Pentoxide. Zinc ethyl iodide is formed and converted
to ethylzinc. An oil bath is constructed and heated to 190 F, and the reformation
of purified diethylzinc occurs via distillation.
Fractional Distillation occurs 4-5 times to ensure purity and removal of excipients.
At this point , diethylzinc is flown over two small vessels P and Q where small
amounts of Germanium Tetrachloride lie. In order to jumpstart the reaction, a
small amount of Tetraethylgermanium is used to ensure the reaction progresses,

otherwise it is unstable and unpredictable. Zinc Chloride is a by-product and must

be removed from the combination resultant mixture.

Fractional Distillation

Source: Dennis and Hance, Cornell University.

A video of Diethylzincs reactivity - http://www.youtube.com/watch?v=EmkBH-ncG1Y
A picture of precautions taken with diethylzinc [air < 2ppm]

Enclosed box with arm holes and gloves under a vacuum, carefully prepares to
open diethylzinc, afraid of an explosion.

Requirements:
Industrial Chemists, installation of high grade reactors and equipment, explosion
proof storage and reactors, small scale equipment to test the reaction and work
to purify both the reagents and final products. Equipment to test and determine
that the synthesized elements are pure, and the correct products being formed.

Note: This is a beginning outline to the intricate processes of synthesizing

Tetraethylgermanium. There is much more to be explored in depth pursuing this
further.