JNITED STATES PATENT OFFICE.

--------

: FRANZ AIGNER, OF POTSDAM, GERMANY., ASSIGNOR TO THE FIRM OF DYNAMIT-ACTIEN

GESELLSCHAFT woRMALS ALFRED NOBEL UND CO., OF HAMBUKG, GERMANY.
PROCESS OF MANUFACTURING NITRoGLYCERIN.
No. 913,653. Specification of Letters Patent.
Application filed February 28, 1905. Serial No. 247,777.
Patented Feb. 28, 1909.
To all whom it may concern: revived nitrating acid of tie same relative
Be it known ti at I, FRANZ AIGNER, a sub
uly
proportions of acids and water
ject of the Emperor of Austria-Hungary, re
siding at 10 Neue König. traige, iPotsdam, . . (HSO,:HNO, H.O. = 60:30:10),
Kingdom of Prussia, Geinian Empire, jave but composed of 450grams of waste acid
invented new and usefui Improvements in from a previous nitrating operation and 450
Processes of Manufacturing Nitroglycerin, of grams fresh acid. A similar favorable result
Willicii tie following is a specification. .
This invention relates to tie process of was obtained by a furter use of tire already .
once revived nitrating acid containing glyc
manufactuirng nitro-glycerin by causing a erin compounds: I obtained 225 grams pure 6 s
Imixture of nitric acid aid sulfuric acid to act Jaitro-glycerin by nitrating 100 grams glyc
on glycerin, and iias for its object to render egin witi,900 grams
the process more expeditious, considerably vived, of the same nitrating acid, twice re.
relative proportions of .
safer and ci:eaper... .. . .
Tite common process of manufacturing acids and water as quoted .
nitro-glycerin differs froin the usual process (IISO,:HNOHO = 60:30:10) 7
of manufacturing hitro-cellulose among but composed of 450 grams waste acid from
other things essentially in that the waste the third nitrating operation and 450 grams
acids from tie nitration of glycerin cannot be fresh acid.
20 revived but unust be denitrated. The reason
. . . .. . .."
The new technical effect obtained
of the said difference is that the nitrating revived waste nitrating acid containing glyc by using
acids of the nitro-glycerin manufacture are . erin compounds consists in an essential in
used up by the nitrating process in a larger creasing
degree than in tie manufacture of nitrocellu glycerin. ofThe the produced amount of nitro
said effect is shown in an 8. 3.
lose. From these reasons the waste acids of especially distinct
the nitro-glycerin manufacture that have ing acid is used. Idegree obtained if a 170
diluted
grainsnitrat
pure.
been separated from the nitroglycerin by nitro-glycerin by nitrating 100 grams glyc
settling etc. are with reference to tieir com erin with 1200 grams fresh nitrating acid of
position by far inferior to those of the nitro the composition
30 cellulose manufacture. .. .
S5
I have now found that the reviving of the HSO,------------------, 56.7%
waste acids of the nitro-glycerin manufac HNO.------------------ 28.3%
ture (which acids contain glycerin com HO-- - - - - - - - - - - - - - - - - - 15.0%
pounds) gives an unexpected advantage, be
35 cause revived waste acid gives an essentially I obtained however 218 grams pure nitro 9
higher amount of nitro-glycerin than the glycerin, i.e. surplus of 48 grams over the C.
original nitrating acid with tile same relative glycerin with 1200bygrams
quoted amount, nitrating 100 grams
once revived ni
proportions of sulfuric acid, nitric acid and trating acid of the same relative proportions
water in the same manner of operation.
40 reviving of the waste acid containing glyc
The of acids and water as quoted . .
erin compounds is effected by adding a fresh (HSO,:HNO,: H.O-56.7:28.3:15.0)
mixture of highly concentrated sulfuric and but composed of 750 grams waste acid from .
95
nitric acid to the waste acid. . in a suitable
proportion. .. . the first nitration and 450 grams fresh
45 In nitrating 100 grams of glycerin with 900 nitrating acid. A twice revived waste acid
grams of freshly prepared nitrating acid of of the same percentage gave 221 grams pure l 00
nitro-glycerin, i. e. a surplus of 51 grams
the composition when compared with the result of the fresh
50
HSO,---------------...-- 60% nitrating acid. One can obtain the said
HNO-. - - - - - - ------------ 30% . .advantage of an increased yield of pure
- sO------- -------------- 10% nitro-glycerin by using revived nitrating 105
I have for instance obtained 201 grams pure water,even
acid with acids containing 20 per cent.
nitroglycerin. I obtained, however, 228 tures whichapproaching
i.e. to those acid mix
cannot have any nitrating
grams pure nitroglycerin in nitrating 100 action.
55 grams glycerin with 900 grams of a once The difference in the nitrating action 110
 2. 913,653
between a revived nitrating acid and a fresh yield of trinitroglycerin can be obtained than
acid has been quite unknown in the manu inventor hasthealsowaste
by causing acid to stand. The
stated the reason for the
facture of nitro-cellulose. The possibility increasing of the yield of trinitroglycerin by 50
by using revived acids of obtaining essen using a waste acid. In the nitrating process
tially higher amounts of nitroglycerin than
by using fresh acids enables the operator to carried out in the ordinary way, besides
trinitroglycerin
vary the degree of concentration of nitrating glycerin) relatively (i. e. the common nitro
acids in a relatively wide range and espe nitrated nitroglycerins large amounts of lower
cially to use less concentrated nitrating monoglycerin) will be (dinitroglycerin generally
and 55
formed.
0 acids, the use of which was formerly un The common trinitroglycerin now is very
economical in the prior process without re
viving. The concentration of the usual slightly soluble inrelatively
acids andcompletely.
separates there
nitrating acid for manufacturing nitro-glyc mononitroglycerin and dinitroglycerin The
fore quickly and
are, 60
erin differed hitherto only by 5 per cent. It however, very soluble in acids and can there
15 has been considered hitherto by all experts fore not separate, even by very long stand
as nearly unavoidable to use only acids of ing. Mononitroglycerin and dinitroglycerin
the highest concentration in order to pre are converted into trinitroglycerin, if one
vent a reduction of the yield of nitro causes
glycerin to below 200 grams of pure nitro On thisfresh the
nitrating acids to act on them. 65
new process is based.
20 glycerin, the average yield being 205 grams What I claim as my invention, and desire
R" nitro-glycerin from 100 grams glycerin. secure by Letters Patent, is
y the possibility given by the present in to The process of nitrating glycerin to ob
vention of using acids with 10 and even 15
per cent. water one obtains the further ad from successively tain a maximum yield of tri-nitro-glycerin 70
treated portions of glyc
2. vantage of a greater security for the nitrat erin, which consists in nitrating a quantity
ing operation. For instance I obtain an of glycerin with a suitable quantity of a
essentially gentle nitration of glycerin with fresh mixture of concentrated nitric and
out the formation of froth by using a nitrat sulfuric acids, separating the resultant tri 75
ing acid of the composition nitro-glycerin from the partially exhausted
30 (HSO:HNO:HO = 60:30:10) acids, containing less highly nitrated de
according to my method instead of the usual rivatives tity of
of glycerin, adding a suitable quan
fresh concentrated nitric and sulfuric
mixture. acids to restore the acid mixture to sub 80
HSO,------------------- 60% stantially its original percentage content of
35 HNO - - - - - - - - - - - - - - - - - - - - 35% nitric acid, sulfuric acid and water, and
HO--------------------- 5% ! nitrating
said acid
a second portion of glycerin with
mixture, substantially as described.
The greater yield of trinitroglycerin (; b Jn testimony whereof
tained by using the waste acid instead of name to this specificationIinhave the
signed my
presence of
40 fresh acids alone is not caused by nitro two subscribing witnesses.
glycerin suspended in the spent acid. By FRANV, Al(N.E.R.
causing waste acid from nitrating glycerin
stand for a sufficient time, one can only ob Witnesses:
to
tain from it1.1process,
to 1.4%however,
trinitroglycerin. By Wol, DEMAR IIAUPT,
IEN Y IIASPER.
45 the presel a far greater