486 CHEMISTRY AND TECHNOLOGY OF EXPLOSIVES
German method.
The German process of hydrolysis (applied at Griesheim) comprises the following
operations :
1300 kg of chlorodinitrobenzene and 7500 1. of water (90°C) are charged into
the reactor. To this mixture, 1500 kg of a 35% solution of NaOH is introduced with
stirring over a period of 4 hr, the temperature being maintained within 95-100°C.
If a test for a complete hydrolysis is satisfactory, the solution is introduced with
stirring to about 780 l. of hydrochloric acid (30%). The mixture is then cooled to
30°C and the separated dinitrophenol is filtered off on a vacuum filter, washed
with cold water, dried and ground.
Dry dinitrophenol prepared by hydrolysis of chlorodinitrobenzene usually melts
at 110-111°C. Its impurities come from the chlorodinitrobenzene, which may
contain unhydrolysed admixtures (such as m- chloronitrobenzene, dichlorodinitro-
benzene isomers, m- dinitrobenzene).
Dinitrophenol from chlorodinitrobenzene, to be used for the preparation of
picric acid, should satisfy the following specifications (Lebedev [39])
melting point (determined as setting point) not below 109°C
inorganic matter (ash) max. 0.2%
iron content in ash trace
lead content in ash none
dinitrophenates and picrates none
acid content (calculated on H 2 SO 4 ) no more than 0.1%
metal chlorides no more than 0.5%
chlorodinitrobenzene no more than 0.5%
dinitrophenol not less than 96%
PICRIC ACID
Picric acid is the most important of the trinitro derivatives of phenol. The com-
mercial product for military purposes is 2,4,6-trinitrophenol of high purity:
AS an explosive it is known under various names: Ekrasit (Austria), Mélinite
(France), Granatfiillung 1888-abbrev. Grf 88 (for shells), Sprengkörper 88 (for
field engineer cartridges) (Germany), Pertite (Italy), Shimoza (Japan), TNF
(Poland), Picrinit (Spain), Lyddit (United Kingdom), Melinit (U.S.S.R.).
PHYSICAL PROPERTIES
Picric acid crystallizes in colourless or yellowish needles or lamellae of the or-
thorhombic-bipyramidal system. The melting point of picric acid is 122.5°C and its