USRE3381E - Glycerine - Google Patents

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USRE3381E
USRE3381E US RE3381 E USRE3381 E US RE3381E
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US
United States
Prior art keywords
glycerine
nitro
acids
vessel
free
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F Alfred Nobel
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  • ⁇ s nitrine or crystallizing nitro-glycerine prepared by the iadu'iix'ture of glycerine, sulphur-ic acid, and nitric acid, free from hyponitric acid, as -a new article of manufacture, so that the compound thus produced, will not decomposeand so that it may become solidified at a moderate temperature, and vmay batiansported; and used with greater safety than ordinary nitro-glycerine,
  • FIG. 1 represents a funnel-shaped vessel, made oi stone, lead, lor other suitable material.
  • A is-t-he vessel
  • 4D. and E are 'tubes connected with reservoir tanks of sufficient elevation to allow the influence of gravitation and atmospheric pressure to force the liquids contained, to descend in such manner that they will mingle or mix before they reach the water in which the said vessel isplaced.
  • lhere may be perforated disks in the said funnelshened. vessel. placedA so that; v4-.be liquids in have additional opportunity'to mix before they reach the water.
  • the glycerine being thus mixed with rthe acids, nitrine or crystallizing nitro-glycerine will be formed, which, Vwhen in the water separates from the acids.
  • the glycerine should enter-the vessel through the pipe D, and the acids, one part nitric acid, say 48 Baum, specific gravity, free or comparatively free from hyponitric acid, and two parts sulphuric acid, say 66 Baume, specific gravity, through the otherpipe E.
  • Figure 2 represents another mode or :process of manufacturing.
  • A is a tank, or vessel, r'nade of ston'e, lead, or other suitable material, which will not beinj uriously affected by the action of the acids.
  • ⁇ B B is the cover on the tank, or vessel.
  • -G is a'thermometer, intended ⁇ -to be suspended into the liquid D in the tank.
  • F F is a worm,or coil of lead, or of other suitable contrivance that will cause it to be raised and lowered at the will of the manipulator.
  • the vessel A A is filled with the necessary quantity of mixed acids, in the proportions of say, one lpart Amore or-less of nitricacid, free or comparatively free from hyponitric acid, and two parts more or iesspt sulphuricacid.”
  • the glycerine is then allowed to tlow 'intothetank A A through the tube E, in such'quantities as -the temperatme may justify.
  • the temperature will rise and fall in proportion, to the agitation audintroduetion oiltlie glyeerine,l which can be adjusted' by a-faucet attached Vtothe 'pipedr tube E.
  • a change may be Iliade from this-formula, according to the quality of the acids and glycerine respectively.
  • the glyceriue and acids have been thus treated by agitation, to the extent of the formula, they are then disch( rged into a tank, o r vessel containing water,
  • the specific gravity of lthe 'nitrine or 'erystallizing nitro-glycerine. is about 1,60o Baume, or sixtenths heavier than water the acids becoming 'diluted bythe water, are lighter, and the nitro-glycerine bengthe heavier, falls to the bottom vcf the tank;
  • NOBEL accomplishes the manufacture of nitrine.

Description

.:free, 'or nearly anita- THE UNITEDA STATES BLAsTiNG-Ou.- COMPANY, 0F NEW'YORK, N. vASSIGNEES 0E ALFRED NOBEL.
Lettes Patent No. 57,175, dated .August 14, 1866; 'reissue No. 2,538, dated 2, 1867 1 treissue .No..3,381,
dated April 13, 1869. V
.D'lnsron l'.
narnovmnm'r m 'ran Mmn'rucmn or,- mnnm. on cmrsremznw Nrrnoenterarme-n The Scheda-ln referred to in these vLetters Patent and makingvpnrt of the ma V\To lll whom' 'it 'mu/y' concern Beitknown that ALF-mau) NOBEL, of the free city yof Hamburg, Germany, invented a new Explosive Oom pound; and we do herebyA declare the following to -be a full, clear, and exact description of that .part of the said invention which' consists in the. production of `s nitrine or crystallizing nitro-glycerine, prepared by the iadu'iix'ture of glycerine, sulphur-ic acid, and nitric acid, free from hyponitric acid, as -a new article of manufacture, so that the compound thus produced, will not decomposeand so that it may become solidified at a moderate temperature, and vmay batiansported; and used with greater safety than ordinary nitro-glycerine,
The essential physical property which distinguishes the said nitrine or crystallizing nitrog.ycer ine from the nitrglycerine discovered by Sobrero, and described in chemical works, is that the former passes into a solid form when'exposed toa moderate temperature, itsmelting point beingat 55 Fahrenheit, or thereabouts, ac-
cording to its purity, while the ordinary nitro-glycerine, as stated in chemical works,` has been subjected to a cold below the zero .of Fahrenheit, without losing its liquid state, and has in fact, been known for 'twenty years without ever having been obtained in a 4solid form.
The essential difference inv the preparation between the said nitriue or crystallizing nitro-glycerine and the nitro-glycerine previously discovered,'isthat the latter is obtained when fuming nitric acid is used in the operation, whereas, the preparation of the former requires a nitric acid free, or comparatively free from hyponitric acid.
Thecomplet-e distinction between the two compounds is proved by the factthat whenbrystallizednitro-glycerine is made with a nitric acid, but little charged with hyponitric acid, a st nall quantityjof the non-crystallzing nitro-glycerine is obtained,'wh1c h remains liquid, while the c rystallizingv nitro-glycerme passes into a solid state. Another..,distinctionis.thatJ; e crystallizing nitroglycerine is not liable to decomposition, and after being properly washed, does not present any acid reaction, whereas the ordinary nitro-glycerine, as clearly stated in chem-ical works, decomposes of 4itself l and deposes oxalicsalts.
1n order to enable ,others skilled in the arts to use said invention,l we herein describe the process and mechanical parts invented by the said NOBEL, for
umnni'zictnring `'the said nitrine orcrystallizingv nitroing.
In the drawing Figure' 1 represents a funnel-shaped vessel, made oi stone, lead, lor other suitable material.
A is-t-he vessel;
B, perforations through the vessel;
4D. and E are 'tubes connected with reservoir tanks of sufficient elevation to allow the influence of gravitation and atmospheric pressure to force the liquids contained, to descend in such manner that they will mingle or mix before they reach the water in which the said vessel isplaced.
lhere may be perforated disks in the said funnelshened. vessel. placedA so that; v4-.be liquids in have additional opportunity'to mix before they reach the water. Y v
The glycerine being thus mixed with rthe acids, nitrine or crystallizing nitro-glycerine will be formed, which, Vwhen in the water separates from the acids.
The glycerine should enter-the vessel through the pipe D, and the acids, one part nitric acid, say 48 Baum, specific gravity, free or comparatively free from hyponitric acid, and two parts sulphuric acid, say 66 Baume, specific gravity, through the otherpipe E.
Figure 2 represents another mode or :process of manufacturing.
A. A, is a tank, or vessel, r'nade of ston'e, lead, or other suitable material, which will not beinj uriously affected by the action of the acids.
` B B is the cover on the tank, or vessel.
-G is a'thermometer, intended `-to be suspended into the liquid D in the tank. f
E is a pipe entering the tank through the cover B B,
tank.
F F isa worm,or coil of lead, or of other suitable contrivance that will cause it to be raised and lowered at the will of the manipulator. i
The voperation of this apparatus is as follows:
The vessel A Ais filled with the necessary quantity of mixed acids, in the proportions of say, one lpart Amore or-less of nitricacid, free or comparatively free from hyponitric acid, and two parts more or iesspt sulphuricacid."
This mixed wid brought @slew temperatura.:
to conduct glycerine' from arcservoir above, into the material, to conduct cold water from a reservoir above,
` The rod is attached above, to any known mechanicall I I is a faucet, through which the mixed materials, or Y liquids will be drawnfrom the tank A A;
say 325 Fahrenheit, and the dasher H on the rod lGr G is put in motion, up and down, which' produces agitation of the liquids.
The glycerine is then allowed to tlow 'intothetank A A through the tube E, in such'quantities as -the temperatme may justify. v
The temperature will rise and fall in proportion, to the agitation audintroduetion oiltlie glyeerine,l which can be adjusted' by a-faucet attached Vtothe 'pipedr tube E.
Ordinarily' one Apound of glycerine is compounded with eight pounds of mixeda'cids, according to the foregoingproportions of acids.
A change may be Iliade from this-formula, according to the quality of the acids and glycerine respectively. When the glyceriue and acids have been thus treated by agitation, to the extent of the formula, they are then disch( rged into a tank, o r vessel containing water,
one part of the said mixture to-eight parts or more nf pure water. Y
, This aeidula'ted water is well stirred, which. agitation separates thenitri'ne or crystallizing nitro-giycerine from' the acids. l
The specific gravity of lthe 'nitrine or 'erystallizing nitro-glycerine. is about 1,60o Baume, or sixtenths heavier than water the acids becoming 'diluted bythe water, are lighter, and the nitro-glycerine bengthe heavier, falls to the bottom vcf the tank;
Inthis manuel', and by the eontrivances mentioned,
NOBEL accomplishes the manufacture of nitrine. or
' crystallizing nitroglycerine i in any desired lquantity,
more economically than can be accomplished by any f hitherto known mode.`
` -Aitilcuglr'we pi'eieriuuse the ming-coil in lthis process, itmaynbe dispensed with Aif desired, and other modes of agitation adopted.
What we claim as the invention of Ammin NOBEL,
:and d'esire to secure by Letters Patent, is-
'Ilieinodecr process, substantially as hereinbefore' described, of mixing together glyeerine, sulphuric acid, and nitric acid, free or nearly free from hyponitric acid, in the production as a new article of manufacture of nitrine or crystallizing nitroglyceriue.
TAL. P. SHAFFNER,
President, &:c.`
JAMES DEVEAU',
Secre ta-'ry of The Umt'ed States Blas in g- Oil Company.
Vitnesses: i
Oc'mvius KNIGHT, WM. B. Demme.

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