US3265545A - Method of desensitizing lead azide and tetryl - Google Patents
Method of desensitizing lead azide and tetryl Download PDFInfo
- Publication number
- US3265545A US3265545A US394087A US39408764A US3265545A US 3265545 A US3265545 A US 3265545A US 394087 A US394087 A US 394087A US 39408764 A US39408764 A US 39408764A US 3265545 A US3265545 A US 3265545A
- Authority
- US
- United States
- Prior art keywords
- tetryl
- lead azide
- explosive
- weight
- pvp
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- AGUIVNYEYSCPNI-UHFFFAOYSA-N N-methyl-N-picrylnitramine Chemical group [O-][N+](=O)N(C)C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O AGUIVNYEYSCPNI-UHFFFAOYSA-N 0.000 title claims description 24
- 150000001540 azides Chemical class 0.000 title description 17
- 238000000034 method Methods 0.000 title description 10
- 239000002360 explosive Substances 0.000 claims description 29
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 claims description 7
- SVTDYSXXLJYUTM-UHFFFAOYSA-N disperse red 9 Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2NC SVTDYSXXLJYUTM-UHFFFAOYSA-N 0.000 claims description 4
- ISEQAARZRCDNJH-UHFFFAOYSA-N lead(ii) azide Chemical compound [N-]=[N+]=N[Pb]N=[N+]=[N-] ISEQAARZRCDNJH-UHFFFAOYSA-N 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 17
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 17
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 17
- 239000000975 dye Substances 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 13
- 239000003921 oil Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000011369 resultant mixture Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000001993 wax Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000005474 detonation Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229940090898 Desensitizer Drugs 0.000 description 1
- SNIOPGDIGTZGOP-UHFFFAOYSA-N Nitroglycerin Chemical compound [O-][N+](=O)OCC(O[N+]([O-])=O)CO[N+]([O-])=O SNIOPGDIGTZGOP-UHFFFAOYSA-N 0.000 description 1
- 239000000006 Nitroglycerin Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 239000003975 dentin desensitizing agent Substances 0.000 description 1
- 238000000586 desensitisation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229960003711 glyceryl trinitrate Drugs 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/005—Desensitisers, phlegmatisers
Definitions
- This invention relates generally to new explosives and more particularly concerns improved methods of treating certain explosives to render them less sensitive to detonation by accidental mechanical shock.
- Desenitization of solid and liquid explosives is not new.
- Those liquid explosives, for example, which were considered to be dangerously sensitive to mechanical shock, e.g., nitroglycerin, are ordinarily diluted with a nonexplosive material which is compatible with the liquid explosive.
- This method of desenitization was subject to one disadvantage which detracted considerably from the usefulness of the desensitized explosive. That is, a rather large amount of desensitizing agent was required to produce an explosive of sufficiently low sensitivity for safe handling and storage. Accordingly, explosives desensitized by this method were characterized by marked reduction in the explosive power. Persons using these liquid explosives were faced with a dilemma which usually could be solved only by the unsatisfactory compromise of employing a minimum amount of desensitizer so that the explosive provided only marginal safety in its handling and use.
- Desensitization of solid explosives by parafiin waxes or mineral oils suffer generally from a non-uniformity of coating of each grain or crystal and causing the crystal to segregate by exudation of the oil or wax. Further, the use of waxes and oils requires specialized equipment and is adversely alfected by unfavorable environmental conditions resulting in poor shelf life and less than 100% reliability.
- the present invention overcomes these and other difficulties by providing new explosives comprising tetryl or lead azide which are rendered more insensitive to shock by treatment with suit-able organic dyes, the resultant product being capable of withstanding impact tests and yet having a good shelf life without undergoing deleterious changes in properties.
- Another object of the invention is to provide methods of making these explosives.
- Still another object of the invention is to provide a generally insensitive lead azide or tetryl explosive and methods of making therefor, both of which are substantially free of the aforementioned disadvantages.
- PbN lead azide
- tetryl 2,4,6-trinitrophenylmethyl nitramine
- water soluble organic dyes such as 1-methylamino-anthraquinone, rosaniline, Calco Oil Blue NS and Calcophen Red Y, a non-subliming azotype dye.
- the selected dye must be chemically non-reactive with the explosive and soluble in common solvents such as acetone, ethyl alcohol or methyl alcohol.
- the final product should have no negative charges thereon and thereby minimizing any danger of accidental electrostatic detonation.
- Example 1 Ten parts by weight of powdered dye, in this instance 1-methylaminoanthraquinone, is dissolved in about 200 parts by weight acetone in a metallic round-bottom vessel. About 1,000-2,000 parts by weight of alcohol-wet lead azide explosive are mixed with about 1-2 parts by weight polyvinyl pyrrolidone (PVP which is soluble in alcohol or water such that about 0.1% by weight of PVP is incorporated into the explosive. The PVP is used to improve the affinity of the explosive for the dye such that the latter will complex with the PVP to render the final coating water insoluble. The PVP-treated lead azide may now be slowly added to the acetone-dye solution with gentle stirring. The resultant mixture is then heated to 5060 C. with stirring until dry.
- PVP polyvinyl pyrrolidone
- the coated lead azide will then be placed in a tray and heated again to about 60 C. until complete dryness is assured and then stored in approved containers.
- the final desensitized product will consist of about 9999.7% by weight lead azide having about 0.34% by weight of dye coating complexed thereon.
- the product is stable at C. and is capable of withstanding a ten-inch drop test and a friction sensitivity test without exploding whereas the prior art dextrinated lead azide exploded when subjected to the drop test aforementioned at three inches and was considerably more frictionally sensitive.
- the drop test comprises permitting -a two kilogram steel cylinder to freely fall into a metal cylinder approximately one and a half inches inside diameter and about four-inches long onto a specified quantity of explosive contained therein.
- the friction test involves a swinging pendulum which is caused to abrade a specified quantity of explosive.
- tetryl is dissolved in about 300 parts by weight acetone in a metallic round-bottom vessel.
- About 1,500-2,500 parts by weight tetryl is islurried with a sufficient quantity of water and then treated with PVP such that about 0.l- 0.2% by weight PVP remained on the explosive when calculated in the dry state.
- the PVP-treated tetryl is now slowly added to the acetone-rosaniline solution with gentle stirring.
- the resultant mixture is then heated to about 60 C. with stirring until dry.
- the coated tetryl will then be placed in a tray and heated again to about 60 C. until complete dryness is assured and then stored in approved containers.
- the final desensitized product will consist of about 99-99.7% by weight tetryl having about 0.3%1% by weight of rosaniline coating complexed thereon.
- the product is stable at 120 C. and is capable of Withstanding a 14-inch drop test whereas the untreated tetryl successfully withstood only a 6-inch drop test. Further, my desensitized tetryl is frictionally non-sensitive when compared to the untreated tetryl.
- Example III Ten parts by weigh-t of powdered dye, in this instance Calco Oil Blue NS, is dissolved in about 200 parts by 3 weight acetone in a metallic round'bot'tom vessel. About LOGO-2,000 parts by weight of alcohol-wet lead azide explosive are mixed with about 12 parts by weight polyvinyl pyrrolidone (PVP). The preparation procedure then proceeds as indicated in Example -I.
- the Calco Oil Blue NS has the formula The final desensitized tetryl product withstood the drop and friction tests aforedescribed substantially identical with the l-methylamino-anthraquinone coated lead azide.
- a desensitized explosive consisting essentially of about 99-99] weight percent of a member selected from the group consisting of lead azide and tetryl and about 0.34% of a dye selected from the group consisting of 1-methylamino-anthraquinone, rosaniline, Calco Oil Blue NS, and Calcophen Red Y.
- a method of desensitizing lead azide comprising the steps of dissolving about one part by weight of an organic dye selected from the group consisting of l-methylaminoanthraquinone, rosaniline, Calcophen Red Y, and
- a method of desensitizing tetryl comprising the steps dissolving about one part by weight of a dye selected from the group consisting of l-methylamino-anthraquinone, rosaniline, Calco Oil Blue NS and Calcophen Red Y in about 200-300 parts by weight acetone to form a solution,
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
United States Patent 3,265,545 METHOD OF DESENSITIZING LEAD AZIDE AND TETRYL Eugene J. Murray, East Orange, N.J., assignor to the United States of America as represented by the Secreta'ry of the Army No Drawing. Filed Sept. 2, 1964, Ser. No. 394,087 5 Claims. (Cl. 14935) The invention described herein may be manufactured and used by or for the Government for governmental purposes without the payment to me of any royalty thereon.
This invention relates generally to new explosives and more particularly concerns improved methods of treating certain explosives to render them less sensitive to detonation by accidental mechanical shock.
Desenitization of solid and liquid explosives is not new. Those liquid explosives, for example, which were considered to be dangerously sensitive to mechanical shock, e.g., nitroglycerin, are ordinarily diluted with a nonexplosive material which is compatible with the liquid explosive. This method of desenitization was subject to one disadvantage which detracted considerably from the usefulness of the desensitized explosive. That is, a rather large amount of desensitizing agent was required to produce an explosive of sufficiently low sensitivity for safe handling and storage. Accordingly, explosives desensitized by this method were characterized by marked reduction in the explosive power. Persons using these liquid explosives were faced with a dilemma which usually could be solved only by the unsatisfactory compromise of employing a minimum amount of desensitizer so that the explosive provided only marginal safety in its handling and use.
Desensitization of solid explosives by parafiin waxes or mineral oils, for example, suffer generally from a non-uniformity of coating of each grain or crystal and causing the crystal to segregate by exudation of the oil or wax. Further, the use of waxes and oils requires specialized equipment and is adversely alfected by unfavorable environmental conditions resulting in poor shelf life and less than 100% reliability.
The present invention overcomes these and other difficulties by providing new explosives comprising tetryl or lead azide which are rendered more insensitive to shock by treatment with suit-able organic dyes, the resultant product being capable of withstanding impact tests and yet having a good shelf life without undergoing deleterious changes in properties.
It is therefore a broad object of this invention to provide an easily manipulatable lead azide or tetryl explosive which can be safely loaded and transported.
Another object of the invention is to provide methods of making these explosives.
Still another object of the invention is to provide a generally insensitive lead azide or tetryl explosive and methods of making therefor, both of which are substantially free of the aforementioned disadvantages.
Other and further objects of the invention will be apparent to those skilled in the art upon study of this disclosure.
, In accordance with my invention, PbN (lead azide) and tetryl (2,4,6-trinitrophenylmethyl nitramine) are rendered less hazardous in their handling and manufacture by suitable treatment with water soluble organic dyes such as 1-methylamino-anthraquinone, rosaniline, Calco Oil Blue NS and Calcophen Red Y, a non-subliming azotype dye.
ice
The selected dye must be chemically non-reactive with the explosive and soluble in common solvents such as acetone, ethyl alcohol or methyl alcohol. The final product should have no negative charges thereon and thereby minimizing any danger of accidental electrostatic detonation.
Example 1 Ten parts by weight of powdered dye, in this instance 1-methylaminoanthraquinone, is dissolved in about 200 parts by weight acetone in a metallic round-bottom vessel. About 1,000-2,000 parts by weight of alcohol-wet lead azide explosive are mixed with about 1-2 parts by weight polyvinyl pyrrolidone (PVP which is soluble in alcohol or water such that about 0.1% by weight of PVP is incorporated into the explosive. The PVP is used to improve the affinity of the explosive for the dye such that the latter will complex with the PVP to render the final coating water insoluble. The PVP-treated lead azide may now be slowly added to the acetone-dye solution with gentle stirring. The resultant mixture is then heated to 5060 C. with stirring until dry. The coated lead azide will then be placed in a tray and heated again to about 60 C. until complete dryness is assured and then stored in approved containers. The final desensitized product will consist of about 9999.7% by weight lead azide having about 0.34% by weight of dye coating complexed thereon.
The product is stable at C. and is capable of withstanding a ten-inch drop test and a friction sensitivity test without exploding whereas the prior art dextrinated lead azide exploded when subjected to the drop test aforementioned at three inches and was considerably more frictionally sensitive. The drop test comprises permitting -a two kilogram steel cylinder to freely fall into a metal cylinder approximately one and a half inches inside diameter and about four-inches long onto a specified quantity of explosive contained therein. The friction test involves a swinging pendulum which is caused to abrade a specified quantity of explosive.
Example II About ten parts by weight rosaniline,
[ 3 s a zl OOH [C6H4NH2] 2,
is dissolved in about 300 parts by weight acetone in a metallic round-bottom vessel. About 1,500-2,500 parts by weight tetryl is islurried with a sufficient quantity of water and then treated with PVP such that about 0.l- 0.2% by weight PVP remained on the explosive when calculated in the dry state. The PVP-treated tetryl is now slowly added to the acetone-rosaniline solution with gentle stirring. The resultant mixture is then heated to about 60 C. with stirring until dry. The coated tetryl will then be placed in a tray and heated again to about 60 C. until complete dryness is assured and then stored in approved containers. The final desensitized product will consist of about 99-99.7% by weight tetryl having about 0.3%1% by weight of rosaniline coating complexed thereon.
The product is stable at 120 C. and is capable of Withstanding a 14-inch drop test whereas the untreated tetryl successfully withstood only a 6-inch drop test. Further, my desensitized tetryl is frictionally non-sensitive when compared to the untreated tetryl.
Example III Ten parts by weigh-t of powdered dye, in this instance Calco Oil Blue NS, is dissolved in about 200 parts by 3 weight acetone in a metallic round'bot'tom vessel. About LOGO-2,000 parts by weight of alcohol-wet lead azide explosive are mixed with about 12 parts by weight polyvinyl pyrrolidone (PVP). The preparation procedure then proceeds as indicated in Example -I. The Calco Oil Blue NS has the formula The final desensitized tetryl product withstood the drop and friction tests aforedescribed substantially identical with the l-methylamino-anthraquinone coated lead azide.
The invention is not to be construed as limited in any manner by the foregoing illustrative examples but is susceptible of many modifications and alterations without departing from the spirit or scope thereof. Accordingly, the invention is to be defined only by the scope of the appended claims.
I claim:
1. A desensitized explosive consisting essentially of about 99-99] weight percent of a member selected from the group consisting of lead azide and tetryl and about 0.34% of a dye selected from the group consisting of 1-methylamino-anthraquinone, rosaniline, Calco Oil Blue NS, and Calcophen Red Y.
2. An explosive according to claim 1 wherein said member comprises lead azide.
3. An explosive according to claim 1 wherein said member comprises tetryl.
4. A method of desensitizing lead azide comprising the steps of dissolving about one part by weight of an organic dye selected from the group consisting of l-methylaminoanthraquinone, rosaniline, Calcophen Red Y, and
Calco Oil Blue NS in about 200300 parts by weight of acetone to form a solution,
mixing a suificient quantity of PVP with alcohol-wet lead azide such that about 0.l0.2% PVP is incorponated into said lead azide when calculated on a dry ibasis,
slowly adding the PVP-treated lead az-ide to said solution to form a mixture,
drying said mixture until the resultant desensitized explosive contains about 0.3-l% of said dye.
5. A method of desensitizing tetryl comprising the steps dissolving about one part by weight of a dye selected from the group consisting of l-methylamino-anthraquinone, rosaniline, Calco Oil Blue NS and Calcophen Red Y in about 200-300 parts by weight acetone to form a solution,
slurrying said tetryl by mixing with water,
mixing a sufiicient quantity of PVP into said slurrying tetryl such that the resultant mixture contains about 0.10.'2% PVP when said tetryl is calculated on a a dry basis,
slowly adding the PVP-treated tetryl to said solution to form a mixture, and
drying said mixture until the resultant desensitized tetryl contains about 0.3-l% of said dye.
No references cited.'
BENJAMIN R. PADGETT, Acting Primary Examiner.
S. J. LECI-lERT, Assistant Examiner.
Claims (1)
1. A DESENSITIZED EXPLOSIVE CONSISTING ESSENTIALLY OF ABOUT 99-99.7 WEIGHT PERCENT OF A MEMBER SELECTED FROM THE GROUP CONSISTING OF LEAD AZIDE AN TETRYL AND ABOUT 0.3-1% OF A DYE SELECTED FROM THE GROUP CONSISTING OF 1-METHYLAMINO-ANTHRAQUINONE, ROSANILINE, CALCO OIL BLUE NS, AND CALCOPHEN RED Y.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US394087A US3265545A (en) | 1964-09-02 | 1964-09-02 | Method of desensitizing lead azide and tetryl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US394087A US3265545A (en) | 1964-09-02 | 1964-09-02 | Method of desensitizing lead azide and tetryl |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3265545A true US3265545A (en) | 1966-08-09 |
Family
ID=23557500
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US394087A Expired - Lifetime US3265545A (en) | 1964-09-02 | 1964-09-02 | Method of desensitizing lead azide and tetryl |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US3265545A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3496041A (en) * | 1967-09-28 | 1970-02-17 | Hans Joachim Riedl | Fusible explosive composition comprising trinitrophenylmethylnitramine and trinitrophenylethylnitramine |
| US4336085A (en) * | 1975-09-04 | 1982-06-22 | Walker Franklin E | Explosive composition with group VIII metal nitroso halide getter |
-
1964
- 1964-09-02 US US394087A patent/US3265545A/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| None * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3496041A (en) * | 1967-09-28 | 1970-02-17 | Hans Joachim Riedl | Fusible explosive composition comprising trinitrophenylmethylnitramine and trinitrophenylethylnitramine |
| US4336085A (en) * | 1975-09-04 | 1982-06-22 | Walker Franklin E | Explosive composition with group VIII metal nitroso halide getter |
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