US2653863A - Process of producing initiating composition containing lead azide - Google Patents
Process of producing initiating composition containing lead azide Download PDFInfo
- Publication number
- US2653863A US2653863A US251627A US25162751A US2653863A US 2653863 A US2653863 A US 2653863A US 251627 A US251627 A US 251627A US 25162751 A US25162751 A US 25162751A US 2653863 A US2653863 A US 2653863A
- Authority
- US
- United States
- Prior art keywords
- salt
- lead
- azide
- acid
- normal
- 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
- 239000000203 mixture Substances 0.000 title claims description 18
- 150000001540 azides Chemical class 0.000 title claims description 17
- 230000000977 initiatory effect Effects 0.000 title claims description 14
- 238000000034 method Methods 0.000 title claims description 10
- 150000003839 salts Chemical class 0.000 claims description 37
- 239000002253 acid Substances 0.000 claims description 20
- LQCKFXAPVKCRRU-UHFFFAOYSA-N 2,4-dinitrobenzene-1,3-diol Chemical compound OC1=CC=C([N+]([O-])=O)C(O)=C1[N+]([O-])=O LQCKFXAPVKCRRU-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 229920001353 Dextrin Polymers 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 9
- JUINSXZKUKVTMD-UHFFFAOYSA-N hydrogen azide Chemical compound N=[N+]=[N-] JUINSXZKUKVTMD-UHFFFAOYSA-N 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000004375 Dextrin Substances 0.000 claims description 2
- 235000019425 dextrin Nutrition 0.000 claims description 2
- ISEQAARZRCDNJH-UHFFFAOYSA-N lead(ii) azide Chemical compound [N-]=[N+]=N[Pb]N=[N+]=[N-] ISEQAARZRCDNJH-UHFFFAOYSA-N 0.000 claims description 2
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- FYGDTMLNYKFZSV-MRCIVHHJSA-N dextrin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)OC1O[C@@H]1[C@@H](CO)OC(O[C@@H]2[C@H](O[C@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-MRCIVHHJSA-N 0.000 description 10
- 238000001556 precipitation Methods 0.000 description 10
- WETZJIOEDGMBMA-UHFFFAOYSA-L lead styphnate Chemical compound [Pb+2].[O-]C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C([O-])=C1[N+]([O-])=O WETZJIOEDGMBMA-UHFFFAOYSA-L 0.000 description 9
- 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 description 8
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 6
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 239000002360 explosive Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005474 detonation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- UFBJCMHMOXMLKC-UHFFFAOYSA-N 2,4-dinitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O UFBJCMHMOXMLKC-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- TZRXHJWUDPFEEY-UHFFFAOYSA-N Pentaerythritol Tetranitrate Chemical compound [O-][N+](=O)OCC(CO[N+]([O-])=O)(CO[N+]([O-])=O)CO[N+]([O-])=O TZRXHJWUDPFEEY-UHFFFAOYSA-N 0.000 description 1
- 239000000026 Pentaerythritol tetranitrate Substances 0.000 description 1
- -1 azide salt Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008241 heterogeneous mixture Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229960004321 pentaerithrityl tetranitrate Drugs 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B41/00—Compositions containing a nitrated metallo-organic compound
- C06B41/02—Compositions containing a nitrated metallo-organic compound the compound containing lead
- C06B41/08—Compositions containing a nitrated metallo-organic compound the compound containing lead with a metal azide or a metal fulminate
Definitions
- azide is commonly employed in detonators as the primary initiating explosive whose detonation induces the detonation of the less sensitive secondary explosive charge in the detonator, for example, tetryl or pentaerythritol tetranitrate.
- Lead azide the precipitation of which from lead nitrate and sodium azide solutions is frequently conducted in presence of dextrine in order to diminish the liability to spontaneous explosions, is however, insufficiently sensitive to ignition by flame to ignite from the spit of a safety fuse or from an electric fusehead, and it is also lacking in the capacity for cohering when compressed into the detonator tube.
- lead styphnate which has excellent capacity for ignition and is capable when ignited of causing the detonation of the lead az'ide and also enables the composition when compressed to cohere. It is also usual to include minor proportions of tetryl and of aluminium powder in the composition, since the tetryl still further increases the binding properties of the composition and the aluminium serves as a press lubricant and aids inspection. Lead styphnate, however, is extremely sensitive to ignition by electrostatic charges and this constitutes a certain hazard in its own manufacture and that of the initiating composition containing it.
- compositions for blasting detonators characterised by the fact that combinations of lead styphnate and lead azide are produced by graduall running together solutions of readily soluble salts ofstyphnic acid and hydrazoic acid with solutions of soluble lead salts, but the products obtained are heterogeneous mixtures and tend to cake on dry ing giving products of poor running properties,
- a coprecipitated initiating composition of homogeneous appearinitiating properties comprising acompound can be obtained by precipitation by mixing a solution of a water soluble normal lead salt of a monobasic acid and an aqueous solution containing a salt of hydrazoic acid and both a normal 2:4 dinitroresorcinate and an acid 2:4 dinitroresorcinate of a cation having a soluble azide.
- An initiating composition according to the invention consists of aggregates comprising a major proportion of lead azide and a minor proportion of a normal lead salt of 2:4 dinitroresorcinol.
- Sodium azide and the sodium normal and acid salts of 2:4 dinitroresorcinol are preferred but the corresponding magnesium salts of 2:4 dinitroresorcinol may be used.
- the amount of the acid salt of 2:4 dinitroresorcinol should be at least ⁇ -0- of the amount of the normal salt of 2:4 dinitroresorcinol, and the amount of the water soluble lead salt of the monobasic acid with which the precipitation is carried out should be chemically equivalent to the amounts of azide and of both the aforesaid salts of 2:4 dinitroresorcinol calculated on the assumption that both of the latter are capable of reacting with the water soluble lead salt of the monobasic acid to form normal lead 2:4 dinitroresorcinate.
- the soluble normal lead salt of monobasic acid it is preferred to use lead nitrate; but lead acetate may alternatively be used.
- The'precipitation is also preferably carried out in the presence of a small proportion of dextrine (preferably 0.01-0.025% calculated on the total weight of the water)
- The'precipitation is also preferably carried out in the presence of a small proportion of Rochelle salt (sodium potassium tartrate tetrahydrate) in addition to the dextrine.
- the amount of Rochelle salt may advantageously be from 015-075 of the weight of the soluble salt of hydrazoic acid used and it is preferably employed in the solution con- .2 taining the salt of hydrazoic acid and the salts of 2:4 dinitroresorcinol.
- the flowing properties are good, and the minimum weight of the material required for complete initiation of tetryl in a detonator is 0.11 g. compared with 0.18-0.20 g. for an initiating explosive consisting of a mixture of 64.8% lead azide, 27.8% lead styphnate, 2.8% aluminium powder and 4.6% tetryl.
- the ignitibility of the material in a detonator is determined by leaving a known gap between the composition and a safety fuse crimpedinto a detonator and finding the proportion of ignitions from the fuse over the gap. In this test the coprecipitate gives similar results to those of the aforesaid composition containing lead styphnate.
- the coprecipitate In respect of electrostatic sensitivity, the coprecipitate is found to require a critical electrostatic energy discharge of 200,000-470,000 ergs, according to the capacity of the condenser delivering this energy, to efiect ignition.
- a similar test conducted on lead styphnate which is electrostatically the most sensitive ingredient of the aforesaid composition containing it requires 34:0 ergs.
- Example II The preparation of the co-precipitate is conducted as in Example I except that the 125 cc. of solution containing the sodium azide and the normal and acid sodium salts of 2:4 dinitroresorcinol contains 0.012 g. Rochelle salt, while the 800 cc. dextrine solution is of 0.015% concentration.
- the reaction proceeds in a similar manner to that of Example I, and'the product has good running properties.
- a minimum charge of 0.09 g. is required for initiation of tetryl in a detonator.
- the ignitibility is again similar to that of the aforesaid lead azide, lead styphnate, aluminium, tetryl composition, and for electrostatic discharge the critical energy value ranges from 1'?4,000-865,000 ergs compared with about 250 ergs for a sample of lead styphnate tested at the same time.
- Example III Two aqueous solutions each of 500 cc. volume, one containing 31.2 g. sodium azide, 12 g. 2:4 dinitroresorcinol, 4.46 g. sodium hydroxide, and 0.07 g. Rochelle salt, and the other containing 100 g. lead nitrate are added simultaneously at a constant rate over 23 minutes to 3.2 litres of a 0.018% (by weight) dextrine solution, while maintaining the temperature at 70 C. Changes similar to those described in Example I occur during the reaction, and the co-precipitated product is obtained in 94% 0f the theoretical yield (based on the usage of sodium azide, lead nitrate and dinitroresorcinol) and consists of almost circular or oval particles.
- the material has good flow properties and as a primary initiator for a base charge of tetryl, 0.12 g. of it is required.
- the cohesive properties of the co-precipitate when pressed in a detonator are far superior to those of the aforesaid composition con taining lead styphnate, while the ignitibility is similar.
- the electrostatic energy discharges necessary to ignite the material are of the order of a million ergs.
- a method for the production of an initiating composition comprising a major proportion of lead azide and a minor proportion of a normal lead salt of dinitroresorcinol which comprises forming a precipitate by mixing an aqueous solution of a water-soluble normal lead salt of a monobasic acid with an aqueous solution containing a salt of hydrazoic acid as well as a normal and an acid salt of 2:4 dinitroresorcinol of which the cation has a soluble azide, the said acid salt of 2:4 dinitroresorcinol being present in amount at least 6 of that of the normal salt of 2:4 dinitroresorcinol and, the said mixing being carried out in the presence of dextrin in amount of from about 0.01% to 0.025% by weight of water present,
- a method as claimed in claim 1 wherein the 5 cation of the salts of 2:4 dinitroresorcinol having a soluble azide is sodium.
- a method as claimed in claim 1 wherein the precipitate is formed at a temperature between precipitation is carried out in the presence of Rochelle salt present in an amount of 0.15 to 0.75% of the weight of the soluble salt of hydrazoic acid used.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Air Bags (AREA)
- Dental Preparations (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB29725/50A GB697475A (en) | 1950-12-05 | 1950-12-05 | Improved initiating compositions for use in blasting and military detonators and their production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2653863A true US2653863A (en) | 1953-09-29 |
Family
ID=10296126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US251627A Expired - Lifetime US2653863A (en) | 1950-12-05 | 1951-10-16 | Process of producing initiating composition containing lead azide |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US2653863A (is") |
| BE (1) | BE519148A (is") |
| CH (1) | CH314646A (is") |
| FR (1) | FR1075495A (is") |
| GB (1) | GB697475A (is") |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2772633A (en) * | 1953-02-25 | 1956-12-04 | Olin Mathieson | Electric blasting cap |
| CN116082105A (zh) * | 2023-04-07 | 2023-05-09 | 中国万宝工程有限公司 | 叠氮化铜叠氮化铅碳纤维复合起爆药及其制备方法 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1552836A (en) * | 1921-10-12 | 1925-09-08 | Friederich Walter | Priming composition and process for producing the same |
| GB616456A (en) * | 1946-09-04 | 1949-01-21 | Leon Rubenstein | Improvements in or relating to the production of normal lead dinitroresorcinate |
-
1950
- 1950-12-05 GB GB29725/50A patent/GB697475A/en not_active Expired
-
1951
- 1951-10-16 US US251627A patent/US2653863A/en not_active Expired - Lifetime
-
1953
- 1953-02-25 CH CH314646D patent/CH314646A/de unknown
- 1953-03-05 FR FR1075495D patent/FR1075495A/fr not_active Expired
- 1953-04-11 BE BE519148D patent/BE519148A/xx unknown
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1552836A (en) * | 1921-10-12 | 1925-09-08 | Friederich Walter | Priming composition and process for producing the same |
| GB616456A (en) * | 1946-09-04 | 1949-01-21 | Leon Rubenstein | Improvements in or relating to the production of normal lead dinitroresorcinate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2772633A (en) * | 1953-02-25 | 1956-12-04 | Olin Mathieson | Electric blasting cap |
| CN116082105A (zh) * | 2023-04-07 | 2023-05-09 | 中国万宝工程有限公司 | 叠氮化铜叠氮化铅碳纤维复合起爆药及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| FR1075495A (fr) | 1954-10-18 |
| GB697475A (en) | 1953-09-23 |
| BE519148A (is") | 1953-10-12 |
| CH314646A (de) | 1956-06-30 |
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