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US1560426A - Harold a - Google Patents

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US1560426A
US1560426A US1560426DA US1560426A US 1560426 A US1560426 A US 1560426A US 1560426D A US1560426D A US 1560426DA US 1560426 A US1560426 A US 1560426A
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explosive
product
compound
producing
nitrate
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C203/00Esters of nitric or nitrous acid
    • C07C203/02Esters of nitric acid
    • C07C203/04Esters of nitric acid having nitrate groups bound to acyclic carbon atoms
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C201/00Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
    • C07C201/06Preparation of nitro compounds
    • C07C201/12Preparation of nitro compounds by reactions not involving the formation of nitro groups
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00Systems containing only non-condensed rings
    • C07C2601/12Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/16Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated

Definitions

  • My invention relates particularly to a process for producing a new explosive of advantageous character and the product thereof.
  • the object of my invention is to provide a new and useful explosive compound suitable for use in detonators and so-called booster charges.
  • My process furnishes a simple and economical means of producing explosives of the nitro-nitrate class where the nitric ester side chain is attached to. the benzene nucleus through oxygen.
  • glycols such as propylene and trimethylene glycol can be treated in the same manner yielding the corresponding trinitrophenoxyalkyl nitrates, such substances constituting valuable explosive compounds.
  • dinitrochlorbenzene condensed with a polyhydric alcohol such as ylcerol gives dinitrophenoxy-glycerol, w iich on nit-ration gives trinitrophenoxy-glycerol dinitrate.
  • Trinitrophenoxy-ethyl. nitrate as produced by my process, is particularly well adapted for use in blasting caps or in socalled booster charges, or in any of the numerous explosive devices for which such explosives as trinitrotoluene, picric acid and tetryl have proved adapted.
  • a compressed charge consisting of 3 grains of trinitrophenoXy-ethyl nitrate in the base of the shell, and a primer of t grains of a 90-10 mixture of fulminate and chlorate with a superimposed inner capsule exhibits an explosive force entirely comparable with that given by tetryl loaded and fired under the same conditions.
  • a process or producing an explosive compound which comprises condensing a polyhydric alcohol, having not more than 3 'hydroxyl groups, with a. nitro-chlor aromatic compound and nitrating the product of condensation.
  • a process of producing anexplosive compound which comprises condensing ethylene glycolwith dinitrochlorbenzene and nitrating the product of condensation.
  • a process of producing an explosive compound which comprises'nitrating the product obtainable iby the condensation of a glycol with dinitrochlorbenzene.
  • An explosive comprising an organic compound of the aromatic series, having a plurality of nitro groups attached to the ring and a side chain comprising a mono nitrate of an aliphatic alcohol attached to the ring through oxygen.
  • An explosive comprising a nitro-eryloxy-alkyl nitrate.
  • An explosive comprising a'polynitrophenyloxy-alkyl nitrate.
  • An explosive comprising the compound obtainable by nitrating the product resulting from the condensation of a glycol containing less than five carbon atoms with a nitro-chlor aromatic compound of the-benzene series.
  • An explosive comprising a nitrated dinitrophenoxy-ethanol.
  • An explosive comprising trinitrophenoxy-ethyl nitrate.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

Patented Nov. 3, 1925.
UNITED STATES PATENT orrlce.
HAROLD A. LEWIS, OF WOODBURY, NEW JERSEY, ASSIGNOR TO E. I. DU PONT DE NEMOURS &, COMPANY, OF WILMINGTON, DELAWARE, A CORPORATION OF DELA- WARE.
EXPLOSIVE COMPOUND AND PROCESS OF PRODUCING SAME.
N 0 Drawing.
To all whom it may concern:
Be it known that I, HAROLD A. LEWIS, a citizen of the United States, and a resident of \Voodbury. in the county of Gloucester and State of New Jersey, have invented certain new and useful Explosive Compounds and Processes of Producing Same, of which the following is a specification.
My invention relates particularly to a process for producing a new explosive of advantageous character and the product thereof. The object of my invention is to provide a new and useful explosive compound suitable for use in detonators and so-called booster charges. My process furnishes a simple and economical means of producing explosives of the nitro-nitrate class where the nitric ester side chain is attached to. the benzene nucleus through oxygen.
I have discovered that the condensation product of a nitro-chlor aromatic compound with a polyhydric alcohol nitrates readily in the presence of sulphuric and nitric acid, forming an aromatic compound having a plurality of nitro groups attached to- .the ring and a side chain comprised of a nitric ester of an aliphatic alcohol attached tothe ring through oxygen. For example, if I condense dinitrochlorbenzene with a dihvdric alcohol such as ethylene glycol, I obtain dinitrophenoxy-ethanol which on nitration yields trinitrophenoxy-ethyl nitrate. Other glycols such as propylene and trimethylene glycol can be treated in the same manner yielding the corresponding trinitrophenoxyalkyl nitrates, such substances constituting valuable explosive compounds. Likewise dinitrochlorbenzene condensed with a polyhydric alcohol such as ylcerol gives dinitrophenoxy-glycerol, w iich on nit-ration gives trinitrophenoxy-glycerol dinitrate. Although the exact details of the various steps of my process may be varied, I
have found the following to yielda very satisfactory explosive compound, starting with dinitrochlorbenzene and ethylene glycol 100 parts by weight of 2, 4-dinitrochlorbenzene are dissolved in 322 parts by weight of ethylene glycol. To this is added an ethylene glycol solution of NaOH made by dissolving parts of NaOH in 12 parts of water and adding 322-parts of glycol. The
Application filed January 26, 1925. Serial No. 4,961.
mixture is heated at 90 to 100 C. for hour, during which time sodium chloride crystallizes out. The hot mixture'is then drowned in about 600 parts of water and the dinitrophenoxy-ethanol separated. 100 parts by weightof this product, after drying, are then dissolved in 1000 parts by weight of 95% sulphuric acid and the solution slowly added to 300 parts of nitric acid (1.47 sp. gr.) which is constantly agitated and kept at 35 C. The temperature is then raised and kept at to for one hour, after which the mixture is drowned in water and the crystalline product separated and washed by any one of the well known methods; The crude product obtained by me in following the process, as described above, gave a product melting at 10l102 C. \Vhen recrystallized fro-m benzene it melted at l05106 C. The nitrate nitrogen as determined by nitromet/en was 4.23% as compared with the theoretical value of 4.40% for trinitrophenoxyethyl nitrate. The product flashed when heated on a steel spatula and detonated when primed with fulminate of mercury.
Trinitrophenoxy-ethyl. nitrate, as produced by my process, is particularly well adapted for use in blasting caps or in socalled booster charges, or in any of the numerous explosive devices for which such explosives as trinitrotoluene, picric acid and tetryl have proved adapted. For example, in a blasting cap shell, I have found that a compressed charge consisting of 3 grains of trinitrophenoXy-ethyl nitrate in the base of the shell, and a primer of t grains of a 90-10 mixture of fulminate and chlorate with a superimposed inner capsule exhibits an explosive force entirely comparable with that given by tetryl loaded and fired under the same conditions.
While I have described my process in detail only as a plied to the condensation and nitration of dmitrochlorbenzcne and ethylene glycol, it is understood that other nitrochloro aromatic compounds, such, for ex ample, as dinitrochlo-rotolueaie, may be used, as well as various polyhydric alcohols other than those specifically mentioned above. My process is also not confined to the particular method of condensation or nitration given in the specific example.
I claim: 7
1. A process or producing an explosive compound which comprises condensing a polyhydric alcohol, having not more than 3 'hydroxyl groups, with a. nitro-chlor aromatic compound and nitrating the product of condensation.
2. A process of producing an explosive compound which com rises condensing a glycol with a nitro-c lor aromatic compound and nitrating sation. 7
3. A process of producing anexplosive compound which comprises condensing ethylene glycolwith dinitrochlorbenzene and nitrating the product of condensation.
4. A process of producing an explosive compound which comprises'nitrating the product obtainable iby the condensation of a glycol with dinitrochlorbenzene.
5. A process 'of producing an explosive compound which-comprises nitrating :the product obtainable by condensing ethylene glycol with 2, 4-dinitrochlorbenzene.
6. A process of producing an explosive the product of condencompound which comprises nitrating dinitrophenoxy-ethanol. Y
'7. An explosive comprising an organic compound of the aromatic series, having a plurality of nitro groups attached to the ring and a side chain comprising a mono nitrate of an aliphatic alcohol attached to the ring through oxygen.
8. An explosive comprising a nitro-eryloxy-alkyl nitrate.
9. An explosive comprising a'polynitrophenyloxy-alkyl nitrate.
10. An explosive comprising the compound obtainable by nitrating the product resulting from the condensation of a glycol containing less than five carbon atoms with a nitro-chlor aromatic compound of the-benzene series. v
11. An explosive comprising a nitrated dinitrophenoxy-ethanol.
12. An explosive comprising trinitrophenoxy-ethyl nitrate.
In testimony whereof I aflix my signature.
. HAROLD A.-LEWIS.
US1560426D Harold a Expired - Lifetime US1560426A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3037057A (en) * 1959-01-23 1962-05-29 Union Carbide Corp Production of aromatic aminoalcohols

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3037057A (en) * 1959-01-23 1962-05-29 Union Carbide Corp Production of aromatic aminoalcohols

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