USRE12669E - Anton mikolajczak - Google Patents

Description

have not been employed with real success in practice.

lecture and in its application and are the cause of many the latter. Pure dinitroglycerin does not explode on and more, modifi ed.

without danger,

UNITED sTA rns ENT OFFICE.

- ANTON MIKOLAJCZAK, OF CASTROP, GE RMANY.

DINITROGLYCERIN AND PROCESS OF MAKING Tim SAME- Original No. 798,438, dated August 2:9, 1905. Applicati To all whom it may concern:

Be it known that L'ANTON Mnwmrczxx, a subject of the King of Prussia, residing at Castrop, Westphalia, I ful Improvements in Dinitroglycerin and Processes of Making the Same, of which the following is a specification. 1

According to present practice in the manufacture of dynamite, carbonite, 'and other nitroglycerin explosives the necessary nitroglycerin is prepared in the form of trinitroglycerin of as pure a character as possible, under nitroglycerin the glyceric trinitrate, C H (O.NO being understood. This nitroglycerin, also known as blasting-0i according to the ordinary method of preparation may unintentionally be mixed with a small quantity of less-ni: tra ted compound glyceric others or of dinitroglycerin.

Dinitroglycerin, C H (O.NO OH, first prepared in the pure state by me, formerly could not be isolisted. The valuable properties of this compound either in consequence remained unrealized, and thus the disadvantages, which, 'in addition to its many good qualities, attach to nitroglycerin have had to be tolerated. These disadvantages consist in the highsensibility of the substance against mechanical shocks and heat, in the readiness with which it ireezes', and the like. They lead to difiiculties both in its manuaccidents.

For the purpose of removing the disadvantages of nitroglycerin a number of processes have been invented. Imay mention here that of mixing nitrobenzol, amyl nitrate, ozc. Most of these processes, however, have proved a total failure, while others In the employment of dinitroglycerin,

I have invented a sives which offers referred to.

l. Dinih'oglycerin is a considerably more stable compound than the extremely rinitroglycerin, C H (O'.NO,) lem sensible against mechanical process of manufacturing explogreat advantages over the processes It is therefore much I shocks and heat than ignition at all. By adding a gradually-increasing percentage of dinitroglyccrin to trinitroglycerin the dangerous characteristics of the latter can be more 2. Dinitroglycerin can be prepared altogether since any decomposition acciden- Specification of lteissued Letters Patent.

Germany, have invented certain new and useunstable blasting-oil tally occuring in the course of manufacture, even in Reissued July 2, 1907.

n for reissue filed October 23, 1906. Serial No. 340,223.

' therase of very large quantities, does not cause explosion, as numerous experiments where decomposition has been purposely brought about have proved.

3. Dinitroglycerin for all practical purposes may be considered as uncongealable. its addition to trinitroglycerin lowers the freezing-point of the latter to such an extent that a mixture of, for instance, sixty per cent. dinitroand forty per cent. trinitro-glycerin was found to remain perfectly fluid during severe frost, while nitroglycerin lixiviated from commercial dynaniites, as well as the latter themselves, froze completely under the same experimental conditions.

4. By the selection of suitable quantities of dinitroglycerin and ordinary blasting-oil an oil can be produced superior to ordinary blasting-oil in. explosive power, for nitroglycerin contains more oxygen than is necessary-for combustion of the carbonic acid and of the hydrogen to water, while dinitrog'lycerin contains too little. Thus by mixing these two compound others a product equalizing these two conditions can be obtained, which may be regarded as an ideal blasting-nil and whereby the greatest possible explosive force is obtained.

5. What has been said in paragraphs 1, 3, and 4 in respect to dinitroglycerin and its mixtures with blasting-oil naturally applies also to all explosives prepared from the same for shooting andblasting purposes. In the case of such explosive powders for shooting or military purposes there is the additional advantage that on account of the lower temperature of the generated which are also much more slowly generated, the barrel of the gun is attacked to amuch less degree than in the case-of the well-known nitroglycerin powders.

6. Dinitroglycerin is not onlyreadilysolublein every proportion in nitroglycerin, but by its aid any suitable mixture of di and tri nitroglycerin can-be prepared directly. 7. Dinitroglycerin nizing medium for various substances (such as nitrocellulose, xyloidin, &c.) as is trinitroglycerin. i

The following examples givenz p p a. Sixty-one per cent. vdinitroglycerin, 1.8 per cent.

soluble pyroxylin, thirty per cent. potassium nitrate,

7.2 per cent. wood-mealjtotal, one hundred per cent.

b. 38.4 per cent. dinitroglycerin, 25.6 per cent.'blastv ing-oil, (trinitroglycerin,) 1.7 per cent. soluble pyroxylin, twenty-seven per cent. Osdium nitrate, 7.3 per cent. wood-meal; total, one hundred per cent.

c. 'Seventeen per cent. dinitroglycerin, fifty-eight per cent. blasting-oil, twenty-three per cent. infusorial earth, (kieselguhr,) two per cent.'.chalk; total, one hun- -'dred per cent.

is just as good a solvent and gelatiof explosives may be here d. Fifty per cent. dinitroglycerin, forty-nine per cent.

soluble pyroxylin, one per cent. diphenylamin; total,

one hundred per cent. V e. Twenty per cent. dinitroglycerin, eighty per cent. soluble pyroxylin; total, one hundred per cent.

f. Forty per cent. dinitroglycerin, ten per cent. blasting-oil, forty-nine per cent. soluble pyroxylin, one per cent. 'diphenylamin; total, one hundred per cent.

g: Twelve per cent. dinitroglycerin, eight per cent. trinitroglycerin, seventy-nine per cent. nitro-starch, one per cent. diphenylamin; total, one hundred per cent.

h. 7.5 per cent. dinitroglycerin, 42.5 per cent. trinitroglycerin, forty-nine per cent. soluble pyroxylin, one per cent. diphenylamin; total, one hundred per cent.

i. Forty-five per cent. dinitroglycerin, thirty per ,cent. trinitroglycerin, two per cent. chalk, twentythree per cent. ini'usorial earth, (kieselguhr;) total, one hundred per cent.

k. Forty-one per cent. dinitroglycerin, thirty-four per cent. trinitroglycerin, one per cent. chalk, twentyiour per cent. infusorial earth, (kieselguhr;) total, one hundred per cent.

l. Fourteen per cent. dinitroglycerin, seventy-eight per cent. trinitroglycerin,eight per cent. soluble pyroxylin; total, one hundred per cent.

m. 12.5 per cent. dinitroglycerin, 62.5 per cent. trinitroglycerin, one per cent'. chalk, twenty-four per cent. infusorial earth, (kieselguhr;) total; one hundred per cent.

As an example of my method of manufacturing dinitroglycerin 1 may cite the following: To ten parts by weight, of glycerin of 1.262 specificgravity thirtythree parts, by weight, of nitric acid of 1.50 specific gravity are added, preferably by allowing the nitric.

acid to slowly flow into the glycerin while being stirred, (the temperature being kept down.) The mixture, chiefly mono-nitroglycerin, is now allowed to cool for some time (it may be several hours) until the mononitroglycerin is converted into dinitroglycerin. The entire mass is then diluted with about ten parts, by weight, of cold water and the nitric acid neutralized by a suitable agent until the lye'for example, in case of using carbonate of lime for neutralization -hss a specific gravity of 1,58. The dinitroglycerin rises therein and can be readily separated, purified, and dried. Any dinitroglycerin which may remain in the lye can be readily removed by means of a solvent, such as other, and obtained from the. latter by distillation. If desired, the mixture of oil and lye deprived of acid can be treated in the same manner without prior separation, no technical difficulties being presented.

- Dinitroglycerin is obtained as a colorless oil when the glycerin and the nitric acid are colorless-that is to say,

free from impurities. It is soluble in water to a large extent, and by reason of this property can very well be obtained quite purefor instance, by fractional evaporation of the water. The well-known solvents for nitroglycerin also readily absorb dinitroglycerin. The percentage of nitrogen according to calculation is 15.38. An actual analysis (nitrometer and organic analysis) showed the average to be 15.38 per cent.

If mixtures of dinitroglycerin with trinitroglycerin are employed for manufacturing explosives or gunpowder, the dinitrin and trinitrin' can first be prepared separately and then mixed. If, however, from nitric acid and sulphuric acid a suitable mixture of certain nitrifying eificiency or nitration value is made, said mixture may be used for preparing and obtaining direct a mixture of both the trinitroglycerin and the dinitroglycerin'i. a, a mixture containing the desired percentage of dinitroglycerin.

On the percentage of diand trinitroglycerin in the product, in addition to the concentration and proportion of the two acids, the temperature and the duration of nitrification exert an influence, as well known in the. case of nitrifications generally.

With this method of working, therefore, the separated oil consists of diand trinitroglycerin. A considerable part of the nitrated glycerin remains dissolved in the 0 waste acid and can by the addition of further acid mixture, concentrated sulphuric acid, or other dehydrating agent be separated from it in the form of an oil consisting partly or wholly of trinitroglycerin.

What I claim as my invention and desire to secure by Letters Patent, is:- I

1. The process of manufacturing dinitroglycerin which consists in reacting on glycerin with nitric acid, maintaining a. lowtemperature until dinitroglycerin is formed and neutralizing the excess of acid, as set forth.-

2. The process of manufacturing dinitroglycerin which consists in reacting on glycerin with nitric acid, maintaining a low temperature until dinitroglycerin is formed and neutralizing the excess of acid by means of an alkaline carbonate.

3. The'process of manufacturing dinitroglycerin which consists in reacting on glycerin with nitric acid, maintaining a low temperature until dinitroglycerin is formed and neutralizing the excess of acid by means of an alkaline earth carbonate.

4. The compound dinitroglycerin, an oily liquid having the formula C,H 0H(0NO=)2, and being further characterlzed by solidifying at a lower temperature and possessing a. greater solubility in water than trinitroglycerin.

5. The process of manufacturing dinitroglycerin, which consists in producing an acid solution of dinitroglycerin. by reacting on glycerin with nitric acid and separating the dinitroglycerin in the mixture by neutralizing the excess of acid.

6. The process of manufacturing dinitroglycerin, which consists in producing an acid solution of dinitroglycerin by reacting on glycerin with nitric acid, and then separating the dinitroglycerin from the solution.

7. in the process of manufacturing dinitroglycerin, the steps which consist in reacting "on glycerin with nitric acid and allowing the mixture to stand until the mono nitroglycerin formed has been converted into dinitroglycerin.

8. The process oi. manufacturing dinitroglycerin, which consists in reacting'on glycerin with nitric acid, allowing the mixture to stand until the mono-nitroglycerin formed has been converted into dinitroglycerin and then separating the dinitroglycerin'from the solution thus produced.

9. The process if manufacturing dinitroglycerin which consists in reacting on glycerin with nitric acid, allowing the mixture to stand, until the mononitroglycerinformed has been converted into dinitroglycerin, diluting the mix-