US1833454A - Method for producing explosive - Google Patents

Description

Patented blow. 2%,. 113 331 comma. n. so

snccasumia, nuw 1m wnamrcron, macaw OE WGI'ON, DELAWARE, AND WILLARD DE C. CRATEE, 0F ASSIGNOBS T0 HEBC'ULE POWDER 602i? OF A COB-POBATIOH' OE DELAWARE E01) FOR PRODUCING EXPLOSIVE no Drawing.

This invention relates to a method for the production of an explosive, more particularly adaptable for use in connection with the production of dynamites, gelatins and the like having a low freezing point, or which will not freeze at such low temperatures as ordinarily prevail in temperate climates.

Heretofore an explosive for incorporation into dynamites, gelatins, etc., for the roduction of an explosive having a low reezing point and involving nitroglycerine, nitrodiglycerine, dinitroglycol and the like in admixture with a nitrotoluene, as dinitrotoluone, has been known. However, in the pro? duction oisuch explosiveheretofore, the glycerine, glycol or the like and the toluene have been separately nitrated and the nitrated products admixed for the esired explosive.

While the nitration of glycerine, glycol, or

v the like, does not present a dificult problem,

nitration of toluene is more complicated and is troublesome to a substantial degree. Forexample, in the manufacture of dinitrotoluene, special apparatus is required and the nitrating' acids, after separation from the dinitrotoluene, carry a substantial quantity thereof in solution, which causes considerable dificulty in efiecting denitration of the spent acids.

Now, in accordance with this invention, it found that an explosive of the type desired, that is to say, comprising a mixture of nitrated glycerine, glycol or the like and nitrated toluene, may be produced readily and without diiliculty by effecting the nitration of the glycerine, glycol, or the like, and

the toluene by a combined process, rather than separately as heretofore.

In proceeding in accordance with the method embodying this invention, not only is the necessity for separate apparatus obviated, but the dificultv and trouble incident to the separate manufacture of the nitrated toluene are avoided. At the same time, the nitrated mixture produced is stable after the usual purification treatment, may be made to contain a desirable quantity of nitrated toluene and is usable directly in the manufacture of dynaproduction of the g Application filed Beptember as, 1929. Serial No. 395,194.

mites, gelatins, and the like, having a low freezing point.

As illustrative of the practical adaptation of the method involving this invention, for example, the usual mixture of glycerine and diglycerine is run into a nitrator of usual construction containing a usual nitrating mixture until about 30-40% of the charge has been added, after which, and while continuing the introduction of the glycerinediglycerine mixture into the nitrator, toluene is simultaneousl introduced into the nitrator. The total c arge of toluene is'desirably added by the time (say) 7 0% of the glycerinc-diglycerine mixture has been run or introduced into the nitrator. After the toluene is added, the balance of thecharge of the lycerine-diglycerine mixture is introduced into the nitrator. During the addition of the glycerine and of the toluene the temperature of the nitrating mixture is controlled to obtain maximum yield. The nitrated products are subjected to washing with water and alkaline solution, as is usual for the purification and stabilization of the product.

As a more specific example of the practical adaptation of the method involving this invention, 500 fparts of a nitrating mixture, comprising, or example, H 52.60%; HNO 46.36% HNOSO .95% H 0, 09% are placed in a nitrator of usual construction. The nitrating mixture is cooled to a temperature of (say) about 36 F. and about parts of a glycerine-diglycerine mixture slowly added. After about one-third or (say) 30-40% of the glycerine-diglycerine mixture has been added to the nitrator, 7 parts of toluene are added separately during the addition of a further third or (say) 30-40% of the glycerine-diglycerine mixture, and, finally, the remainin third or (say) 30-40% of the glycerine-dig ycerine mixture is added. When nitration is completed, the nitrated products are separated from the nitrating mixture in the usual manner. Separation from the spent acid will require from about seventeen to twenty-one minutes. The nitrated products, after Washing with Water and alkaline solution in the usual manner, will have a pH value of (say) 7.0 to 7.1. The Water content will be about .38%-.761%. The dry weight of the product from about a hundred parts of the mixture of glycerine-diglycerine and toluene will be about 235 to 240 parts or a yield of about 94: to 97%. The nitrogen cgntent of the finished product will be about 1 It will now be understood that the method in accordance with this invention involves, broadly, the simultaneous nitration of glycerine, glycol or the like and toluene for the production of an explosive involving nitrated glycerine, glycol or the like and nitrated toluene, and that more particularly the invention involves the procedure to effect the nitration comprising the introduction of glycerine, g1 col or the like into a nitrating mixture, and the simultaneous introduction of toluene into the nitratin mixture, the toluene being desirably intro uced into the nitratin mixture after about one-third of the glycerine, glycol or the like has been introduced and the toluene being introduced during the introduction of a second third of the glycerine, glycol or the like.

It will be understood that where, in the claims hereto ap ended, lycerine is s ecified,

it is intended to include i lycerine, g ycerin glycol-sugar mixtures, g ycerin-sugar mixtunes, glycol, or the like, as equivalents for gliIcerme. a

aving now fully described our lnventlon,

what we claim and desire to protect by Letters Patent is:

1. The method of producing an explosive which includes introducing a quantity of glycerine into a nitratin mixture, then introducin a. quantity of g ycerine and 9. mmtity of to uene simultaneously into the nitrating mixture, and finall introducing a further quantity of glycerine unto the nitrating mixture.

2. The method of producing an explosive which includes introducing about 30-40 parts of glycerine into a nitrating mixture, then introducing about 30-40 parts of glycerine into the nitrating mixture while separately introducing about, 7 parts of toluene into the nitrating mixture, and finally introducing about 30-40 parts of glycerine into the nitratin mixture.

n testimony of which invention, we have hereunto respectively set our hands at Wilmin on, Delaware, on this 19th da of Septem r, 1929, and at Kenvil, New ersey, on this 3rd day of Se tember, 1929.

COR ELL H. CORDIE. WILLARD on C. CRATER.