378 CHEMISTRY AND TECHNOLOGY OF EXPLOSIVES
The residue left after the solvent - alcohol (in the earlier crystallization method)
or xylene (from the washing technique) - has been distilled off, is a semi-solid
substance consisting of α− trinitrotoluene, its isomers, dinitrotoluenes and other
nitro compounds, all of them found as impurities in TNT.
The mixture, known as “TNT oil”, generally melts within a wide temperature
range, for example from room temperature up to 60°C. It may be used as a com-
ponent of ammonium nitrate explosives for the mining industry.
The “exudation process” is a modified purification by crystallization. At present
it is applied to purify grade III TNT and to recover impurities present in TNT
for use as “TNT oil” in the preparation of explosive compositions. The process
may be carried out in two ways.
In one of them TNT, scattered over sloped flat pans (Fig. 79, p. 351), is put
into a chamber heated to 60°C. After several hours the low-melting impurities
segregate as oil which collects in a special vessel placed below the pans.
Another method consists in melting TNT in tilting kettles (converters) heated
by steam or hot water which are then left at rest at room temperature or slightly
higher (e.g. 30°C) for slow crystallization. Under such conditions large crystals
of TNT are formed immersed in an oily mixture of other nitro compounds. The
latter is removed by breaking the solidified substance and inclining the kettle so
as to enable the oil to run out.
The oily product has been used as an ingredient of coal mining explosives as
so-called “liquid TNT”. This material also comprised the liquid mixture of nitro
compounds forming the residue after distillation of alcohol (or any other solvent)
used for crystallization of TNT.
In an earlier Russian method (Belenkii [8]) crude, granulated TNT was washed
with hot water in wooden tanks lined with sheet lead, and equipped with an air
bubbler.
For a batch of 1000 kg of TNT 1000 l. of water were used at a time. The water
was brought to boiling by direct heating with steam (1-2 hr). After boiling for 5 min
heating and air mixing were stopped, and the TNT allowed to settle at the bottom.
After 10-15 min the water was separated by decantation. This operation was repeat-
ed 6-8 times with new portions of fresh water, until the acidity of the TNT fell
to 0.02% (calculated on H 2 SO 4 ). The whole washing process took about 7 hr.
The use of lead-lined tanks for the first two washings, and a wooden tank for the
next ones proved advantageous,
Norell [26] invented a continuous method of crystallization of TNT from nitric
acid. A diagram is given in Fig. 92, according to the A. B. Bofors patent.
The crystallizing vats (1).-(5) are provided with heating jackets (3) and
stirrer (4). The vats communicate through the overflow (7) and pipes (6). The
last crystallizer has an outlet (8) provided with a screw type conveyer to remove
a semi-solid mixture of crystals of TNT plus mother liquor.
The first vat is provided with pre-crystallizer (9) and a stirrer (10). The molten TNT
(II) and solvent (12) (i.e. nitric acid) is introduced to the pie-crystallizer in which TNT