U.S. patent number 3,631,802 [Application Number 04/862,544] was granted by the patent office on 1972-01-04 for detonator comprising n-nitro-n-methylglucamine pentanitrate.
This patent grant is currently assigned to Atlas Chemical INdustries, Inc.. Invention is credited to Joseph W. Lawrence.
United States Patent |
3,631,802 |
Lawrence |
January 4, 1972 |
**Please see images for:
( Certificate of Correction ) ** |
DETONATOR COMPRISING N-NITRO-N-METHYLGLUCAMINE PENTANITRATE
Abstract
A method is disclosed for preparing new N-nitro-N-lower alkyl
glucamine pentanitrates. These new compounds possess explosive
characteristics similar to pentaerythritol tetranitrate (PETN) and
may be similarly employed in explosive devices such as primers,
boosters and explosive initiators.
Inventors: |
Lawrence; Joseph W. (Lexington,
OH) |
Assignee: |
Atlas Chemical INdustries, Inc.
(Wilmington, DE)
|
Family
ID: |
27101429 |
Appl.
No.: |
04/862,544 |
Filed: |
June 11, 1969 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
|
|
675860 |
Oct 17, 1967 |
3491140 |
Jan 20, 1970 |
|
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Current U.S.
Class: |
102/202.11;
102/202.14; 102/202.9; 149/92 |
Current CPC
Class: |
C06C
7/00 (20130101); C06B 25/00 (20130101); F42B
3/124 (20130101); C06B 25/34 (20130101) |
Current International
Class: |
C06C
7/00 (20060101); F42B 3/00 (20060101); C06B
25/34 (20060101); C06B 25/00 (20060101); F42B
3/12 (20060101); F42c 011/00 () |
Field of
Search: |
;102/28M,7.2A |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
Primary Examiner: Sebastian; Leland A.
Parent Case Text
This is a division of application Ser. No. 675,860, filed Oct. 17,
1967, now U.S. Pat. No. 3,491,140.
Claims
What is claimed is:
1. A detonator comprising
a. a shell;
b. a base charge of N-nitro-N-lower alkyl glucamine pentanitrate
within said shell;
c. two lead wires passing through said shell in insulated
relationship thereto; and
d. electrically-actuated means for initiating said base charge,
said means being electrically connected to said lead wires.
2. A detonator according to claim 1 wherein said means for
initiating said base charge is a bridgewire in contact with an
ignition composition.
3. A detonator according to claim 2 wherein said means for
initiating said base charge is an electric match.
4. A detonator according to to claim 3 wherein said ignition
composition is selected from the group comprising cuprous
acetylide, diazodinitrophenol, lead mononitroresorcinate, and
mixtures of lead mononitroresorcinate and potassium chlorate.
5. A detonator according to claim 1 wherein said lower alkyl group
contains from 1 to 6 carbon atoms.
6. A detonator according to claim 5 wherein said lower alkyl group
is methyl.
7. A detonator according to claim 1 wherein said means for
initiating said base charge includes a priming charge.
8. A detonator according to claim 7 wherein said priming charge is
selected from the group consisting of mannitol hexanitrate,
diazodinitophenol, mercury fulminate, lead azide, or mixtures
thereof with oxidizing agents.
Description
This invention relates to N-nitro-N-lower alkyl glucamine
pentanitrates and more particularly to a method of preparing
compounds of the formula: ##SPC1##
Wherein R is either straight or branched chain lower alkyl of 1 to
about 6 carbon atoms and exemplified by methyl, ethyl, N-propyl,
n-butyl, and other similarly related radicals. The present
invention also relates to improved ignition devices such as
detonators, squibs, primers, boosters and the like containing as a
component, the present N-nitro-N-lower alkyl glucamine
pentanitrates.
Base charges for use in explosive initiators typically include
pentaerythritol tetranitrate (PETN), which may be classified as
secondary high explosive as contrasted to primary high explosives
such as mercury fulminate and lead azide.
It has now been found that a new series of compounds which possess
similar sensitivity and explosive characteristics to PETN may be
prepared by the method of the present invention. The compounds of
the present invention may thus be employed in explosive devices
such as primers, boosters and explosive initiators.
The compounds of the present invention may be readily prepared by
first nitrating with, for example, nitric acid, a N-lower alkyl
glucamine compound of the formula: ##SPC2##
To form N-nitrato-N-lower alkyl glucamine pentanitrate of the
formula: ##SPC3##
Wherein R is lower alkyl as previously defined.
The nitration step may be performed by using nitric acid
vacuum-distilled from mixed nitric-sulfuric acids to avoid adding
water to the nitrating system. A dehydrating agent such as acetic
anhydride or sulfuric acid may also be included as a compound of
the nitrating step to further limit the influence of water in the
nitrating system.
The nitrating step is generally carried out at a temperature above
0.degree. C. and more specifically at a temperature of about
30.degree. C. Variations in the reaction conditions are possible
but higher temperatures tend to be difficult to maintain.
The N-nitrato-N-lower alkyl glucamine pentanitrate prepared in the
nitrating step may be isolated and dehydrated to form
N-nitro-N-lower alkyl glucamine pentanitrate. Desirably, the
dehydrating step is performed with a combination of materials such
as concentrated nitric acid, zinc chloride, and acetic
anhydride.
The dehydrating step is generally performed at a temperature above
25.degree. C. and generally at a temperature of about 50.degree. C.
Higher temperatures tend to reduce yields and increase the
difficulty of controlling the dehydration reaction.
A series of initiators containing the new composition of the
present invention may be prepared as illustrated in the
accompanying drawing in which like numerals represent the same
elements throughout the several views.
In the FIGS.
FIG. 1 is an enlarged half-sectional view taken as a side elevation
and illustrating an electric explosion initiator containing the
composition of the present invention as a base charge;
FIG. 2 is an enlarged half-sectional view taken as a side elevation
and illustrating a second type electric explosion initiator also
containing the composition of the present invention as a base
charge;
FIG. 3 is an enlarged half-sectional view taken as a side elevation
and illustrating a third type initiator containing the composition
of the present invention as a base charge; and
FIG. 4 is an enlarged half-sectional view taken as a side elevation
and illustrating a fuse cap containing the composition of the
present invention.
FIG. 1 illustrates electric explosion initiator 8 having shell 10
in which may be positioned base charge 12 formed of the explosive
N-nitro-N-lower alkyl glucamine pentanitrate prepared by the method
of the present invention. Superimposed on base charge 12 is priming
charge 14. The priming charge which is normally fired by electric
match assembly 16 may include any suitable material such as
mannitol hexanitrate, diazodinitrophenol, mercury fulminate, lead
azide, or mixtures thereof with oxidizing agents such as potassium
chlorate.
Electric match assembly 16 includes electric conductive plates 18
and 20 generally formed of a metallic material such as copper or
aluminum and applied upon opposite sides of insulating material
base 22 formed of an electric nonconductive material such as, for
example, cardboard. Bridge wire 24, which may be embedded in match
composition 26, is electrically secured to the lower ends of
electric conductive plates 18 and 20. Match composition 26 may
include, for example, an ignition composition such as cuprous
acetylide, diazodinitrophenol, lead mononitroresorcinate, mixtures
of lead mononitroresorcqnate and potassium chlorate, and related
materials and mixtures thereof which may be applied in any
convenient fashion, as desired. The ignition composition may be
applied, for example, in the plastic state with lacquer about the
bridge wire and allowed to harden. A deflagrating composition such
as mixtures of ammonium picrate and potassium dichromate or carbon
and potassium chlorate may also be included as part of match
composition 26. One or more coating layers of, for example lacquer
may also be included, if desired, when the match composition is
formed as a match head.
Opposite match composition 26 are lead wires 28 and 30 which are
connected, as illustrated, to the upper ends of electric conductive
plates 18 and 20 by a suitable solder material 31. Lead wires 28
and 30 may be coated with a suitable insulating material such as
polyvinyl chloride, if desired.
Sealing plug 32 is illustrated at one end of shell 10 for
supporting lead wires 28 and 30. The sealing plug may be formed of
any suitable material such as rubber, neoprene, or other material
which is sufficiently elastic for insertion into shell 10 during
assembly.
FIG. 2 illustrates a second type electric explosion initiator 33
having shell 34 containing base charge 12 formed of N-nitro-N-lower
alkyl glucamine pentanitrate. Bridge wire 36, embedded in match
composition 26 is electrically connected to lead wires 28 and 30
within sealing plug 32.
FIG. 3 illustrates a third type initiator 39 having shell 40, cap
portion 42 inserted into shell 40, base charge 12 formed of
N-nitro-N-lower alkyl glucamine pentanitrate positioned within
shell 40 and in igniting position to match composition 26. Bridge
wire 44 of high electrical-resistance wire is embedded in match
composition 26 and is electrically connected to electrodes 48 and
50 secured in plug 52.
FIG. 4 illustrates fuse cap 54 having flash charge 56 superimposed
on primer charge 14 and base charge 12.
Other variations of initiators in addition to those illustrated as
well as explosive primers and boosters are also possible devices
for using the composition of the present invention.
In order to further illustrate the present invention, the following
examples are given:
EXAMPLE 1
3.9 grams of N-methyl glucamine was added to 21 ml. of concentrated
nitric acid at a temperature maintained between 0.degree. C. and
about 5.degree. C. Thereafter, 13.5 ml. of acetic anhydride was
added and the nitration mixture was heated to 30.degree. C. for 20
minutes and drowned in 100 grams of crushed ice. A granular product
was formed. The solid product was washed with water and dried under
vacuum. 8.5 grams of white granules melting at 115.degree. C.
resulted having an actual percent by weight nitrate nitrogen
content of 17.25. The produce was identified to be
N-nitrato-N-methyl glucamine pentanitrate (C.sub.7 H.sub.13
O.sub.18 N.sub.7) which has a calculated percent by weight nitrate
nitrogen content of 17.39. A dehydration mixture was prepared
consisting of 0.6 gram of concentrated nitric acid, 0.5 gram of
zinc chloride and 25 grams of acetic anhydride. At a temperature of
about 25.degree. C., 4 grams of the prepared N-nitrato-N-methyl
glucamine pentanitrate was added to the dehydration mixture. This
mixture was next heated to a temperature of about 50.degree. C. for
5 minutes. The mixture was then cooled and poured into 60 ml. of
ice water wherein a granular powder formed immediately. The cold
suspension was stirred for 1 hour and the solids were removed by
filtration. After washing with water and drying under vacuum, 3.3
grams of white powder were recovered. The recovered powder was
found to melt at 102.degree. C. and was found to have an actual
percent by weight nitrate nitrogen content of 15.04. The product
was identified to be N-nitro-N-methyl glucamine pentanitrate, which
has a calculated percent by weight nitrate nitrogen content of
15.06.
EXAMPLE 2
Two compound detonators similar to that of FIG. 4 were prepared in
2-inch gilding metal tubes 54 of 0.22 inch inside diameter,
employing as base charge 12 in each, 0.30 gram of N-nitro-N-methyl
glucamine pentanitrate pressed with 150 pounds on a 0.216-inch
diameter pin; as primer charge 14, 0.13 gram of mannitol
hexanitrate; and, as flash charge 56, 0.06 gram of a 75/25 mixture
of diazodinitrophenol and mannitol hexanitrate pressed with 25
pounds on a 0.216-inch diameter pin. The height of the total charge
was about 42/64 of an inch. The loaded detonators were fused in
standard fashion, and each primed into a 1-1/4".times.8" stick of a
high ammonium nitrate-nitroglycerine dynamite, and shot. Complete
detonation was effected. Ten detonators prepared over this formula
were test-fired in the standard lead plate test, resulting in 10
"A" plates. N-nitro-N-methyl glucamine pentanitrate thus functioned
satisfactorily as the base charge in a compound detonator.
It is understood that the foregoing detailed description is given
merely by way of illustration and that many variations may be made
therein without departing from this invention.
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