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Патент USA US2410699

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Patented Nov. 5, 1946
Joseph A. Wyler, Allentown, Pa, assignor to
Trojan Powder Company, Allentown, vPa.
No Drawing. Application September 26, 1942,
Serial No. 459,839
3 Claims.
(Cl. 260-248)
This invention relates in general to a process
tion, the following ‘examples, in which all parts
for the recovery of cyclo-trimethylenetrinitra
mine from mixtures comprising cyclo-trimethyl
are by weight, are given.
Example 1
enetrinitramine and nitrotoluenes, and more
particularly to the recovery of cyclo-trimethyl
enetrinitramine from mixtures of cyclo-trimeth
ylenetrinitra-mine and trinitrotoluene.
100 parts of a 50-50 mixture of cyclo-tr'imeth
ylenetrinitramine and trinitrotoluene were dis
solved in 560 parts of acetone at room tempera
The principal object of my invention is to
ture, the mixture ?ltered to remove any insolu
recover both the cyclo-trimethylenetrinitramine
ble foreign matter and the clear solution treated
and the nitrotoluenes in valuable forms from the 10 with water, added in a, thin stream while the
various types of ammunition used in warfare, in
mixture was being stirred vigorously. When
which cyclo-trimethylenetrinitramine is in inti
mate contact with trinitrotoluene, dinitrotoluene,
or mononitrotoluene or with any of these nitro
about 450 parts of water had been added, the
water-addition was discontinued and the'mixture
stirred for half an hour or more additional.
toluenes and conditioning agents as para?in, 15 mixture was ?ltered and the cyclo-trimethylene
graphite, alkali stearates, waxes and the like.
trinitramine which had separated, washed on the
At the present time mixtures of cyclo-trimeth
?lter with aqueous acetone (1-1), followed by
ylenetrinitramine and trinitrotoluene are being
water and dried. The weight of cyclo-trime'thyl
used in anti-aircraft shells, torpedoes, anti-sub
enetrinitramine obtained was 47 parts.
marine bombs and for certain small-sized artil 20
The ?ltrate obtained as just described was
lery pieces. These various compositions are
treated with an excess of water, with stirring.
amenable to my process. Also, mixtures of
This precipitated the trinitrotoluene together
cyclo-trimethylenetrinitramine, trinitrotoluene,
aluminum and ammonium nitrate which are use
with a small amount of cyclo-trimethylenetrini
The mixture was ?ltered and the resi
ful in bombs may advantageously be subjected to 25 due on the ?lter washer with water and dried.
my process.
The weight of this residue, which was fairly pure
I have discovered that if an acetone solution of
trinitrotoluene, was 53 parts.
cyclo-trimethylenetrinitramine and a nitrotolu
Example 2
ene is slowly treated with water, with thorough
agitation of the mixture, that the cyclo-trimeth
mixture of cyclo-trimeth
ylenetrinitramine is the ?rst to separate. If the
ylenetrinitramine and trinitrotoluene were dis
water is added cautiously and the stirring made
solved in 400 parts of acetone at 45° C. and this
very turbulent the cyclo-trimethylenetrinitra
mixture treated with water, at about 45° C., in
mine will separate in a high state of purity and in
essentially the same manner as described above.
an excellent physical condition. The continued 35 In
the present case about 375 parts of water were
addition of the water causes the further precipi
to cause the separation of the'cyclo-tri
tation of the cyclo-trimethylenetrinitramine and
methylenetrinitramine. The yield of the latter
?nally, as more water is added, an oil-like prod
was 49 parts.
uct, instead of a crystalline, separates. Just
Upon dilution and stirring of the ?ltrate with
before this stage is reached it is best to ?lter oil
excess of Water the trinitrotoluene separated
the cyclo-trimethylenetrinitramine crystals in
in a yield of 51 parts of the dried material.
order to prevent their contamination by this oily
Similarly, I may e?ect a separation of cyclo
product which is mainly a nitrotoluene-acetone
trimethylenetrinitramine from admixture with
water phase. In such cases where a. small
dinitrotoluene or mononitrotoluene and it is to
amount of this oily layer does separate the effect
be understood that my process is applicable to
upon the purity of the precipitated cyclo-tri
-,mixtures comprising cyclo-trimethylenetrinitra
methylenetrinitramine is negligible because this
"mine and nitrotoluenes in which the cyclo-tri
oily layer passes through the ?lter. The ?ltrate
methylenetrinitramine content varies from a pre
from the cyclo-trimethylenetrinitramine is treat
dominant proportion to a minor proportion.
ed with a large excess of water in the same man
Consequently, it will be clear to a person skilled
ner as described above and the precipitated nitro
in this art that I may vary considerably the pro
toluene separted by any suitable method, as ?ltra
portion of acetone used to the weight of the mix
tion for the trinitrotoluene and dinitrotoluene
ture of cyclo-trimethylenetrinitramine and nitro
and settling for the mononitrotoluene.
toluene being treated and also the amount of
In order to more clearly point out my inven 55 water used for the precipitations, the essential
and that the maximum amount of Water added is
regulated by observing the beginning of the for
mation of a liquid phase as described above.
Although I prefer to use temperatures of about
25-30°. C. for the precipitation, temperatures as
high as 60° C. are entirely practicable, particu
I claim:
1. The process for the recovery of cycle-tri
methylenetrinitramine from mixtures compris
trinitrotoluene, which comprises treating such a
mixture with an amount of acetone which is
su?icient to dissolve the cyclo-trimethylenetri
nitramine and the trinitrotoluene, ?ltering, add
ing water slowly and in such an amount to the
?ltrate, with stirring, to effect the substantial
precipitation of the cyclo-trimethylene trinitra
10 mine without the precipitation of any appreciable
amount of trinitrotoluene from the solution and
?ltering off the precipitated cyclo-trimethylene
ing essentially 'cyclo-trimethylenetrinitramine
3. The process for the recovery of cyclo-tri~
and a nitrotoluene which comprises treating such
a mixture with an amount of acetone which is
» methylenetrinitramine from a mixture compris
ing about 1 part of cyclo-trimethylenetrinitra
mine to 1 part of trinitrotoluene which comprises
dissolving about 1 part of said mixture in about
sufficient to dissolve the cyclo-trimethylenetri
nitramine and the nitrotoluene, ?ltering, adding
water slowly and in such an amount to the ?l
6 parts of acetone, ?ltering, slowly addingr about
trate, with stirring, to effect the substantial pre
cipiation of the cyclo-trimethylenetrinitramine
methylenetrinitramine from mixtures comprising
essentially cyclo-trimethylenetrinitramine and
operations being that the water is properly added
larly with the trinitrotoluene-cyclo-trimethyl
enetrinitramine mixtures.
20 4.5 parts of Water, with thorough stirring, ?lter
amount of a nitrotoluene from the solution and
ing 01f the precipitated cyclo-trimethylenetrini
tramine, washing the latter with dilute acetone,
?ltering off the precipitated oyclo-trimethylene
then with water and drying.
without the precipitation of any appreciable
2. The process for the recovery of cyclo-tri
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