US2493551A - Production of normal lead dinitroresorcinate - Google Patents
Production of normal lead dinitroresorcinate Download PDFInfo
- Publication number
- US2493551A US2493551A US759705A US75970547A US2493551A US 2493551 A US2493551 A US 2493551A US 759705 A US759705 A US 759705A US 75970547 A US75970547 A US 75970547A US 2493551 A US2493551 A US 2493551A
- Authority
- US
- United States
- Prior art keywords
- normal
- lead
- magnesium salt
- dinitroresorcinol
- dinitroresorcinate
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 159000000003 magnesium salts Chemical class 0.000 claims description 23
- 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 17
- 238000000034 method Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- PNZVFASWDSMJER-UHFFFAOYSA-N acetic acid;lead Chemical compound [Pb].CC(O)=O PNZVFASWDSMJER-UHFFFAOYSA-N 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 229940046892 lead acetate Drugs 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 7
- 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 6
- 150000001540 azides Chemical class 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 244000215068 Acacia senegal Species 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229920000084 Gum arabic Polymers 0.000 description 1
- 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 1
- 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 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000009527 percussion Methods 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
Definitions
- priming compositions for propellent powders and other explosives consisting of normal lead 2:4 dinitroresorcinate prepared by the action of a lead salt such as lead nitrate on sodium dinitroresorcinate.
- a lead salt such as lead nitrate on sodium dinitroresorcinate.
- a solution of soluble normal lead salt to an aqueous solution of a normal salt of 2:4 dinitroresorcinol normal lead 2:4 dinitroresorcinate has no free flowing properties, and hitherto it has been necessary to corn it with gum arabic before it .can be used for certain purposes, such as the production of delay fuses, or as an ignition agent in detonators.
- the process for the production of normal lead 2:4 dinitroresorcinate comprises mixing together at a temperature not lower than 60 C. an aqueous solution of normal lead acetate with an aqueous solution containing a magnesium salt of 2:4 dinltroresorcinol having about to A the quantity of magnesium present in the normal magnesium salt, the said lead acetate and magnesium salt being admixed in stoichiometrical equivalent weights.
- the precipitate thus formed may then be washed with water and dried.
- magnesium salt of 2:4 dinitroresorcinol having about /2 to the quantity of magnesium present in th normal magnesium salt is meant a product such as is obtained by interaction of 2:4 dinitroresorcinol and for example magnesium oxide in /2 to the proportion necessary to give the normal magnesium salt of 2 :4 dinitroresorcinol.
- the pH of the solution containing the magnesuim salt of 2:4 dinitroresorcinol having about /2 to the quantity of magnesium present in the normal magnesium salt is about 3.8 to 5.4 when measured at ordinary temperature.
- This solution may obviously be formed either by addition of 2:4 dinitroresorcinol to a hot solution of the normal magnesium salt thereof, or by adding to a hot suspension of 2 4 dinitroresorcinol in water from about /2 to of the amount of magnesium oxide or carbonate required to form the normal magnesium salt.
- the normal lead acetate solution may be gradually added to the aforesaid solution containing the said magnesium salt of 2:4 dinitroresorcinol, or both solutions may be run together into water.
- the precipitation temperature is preferably about 70 C.
- the resulting free-running normal lead 2:4 dinitroresorcinate may be used as a substitute for lead styphnate as an igniting agent in detonators and the like, for instanc in place of lead styphnate in compositions containing lead styphnate and lead azide together. Mixtures of the said normal lead 2:4 dinitroresorcinate and lead azide show less tendency to segregation than the azide with lead styphnate. It may also be used as a fast burning delay fuse composition in military and commercial detonators. Since it does not require'to be corned it can be loaded very easily by apparatus employing charging plates.
- Example 10 gm. of 2:4 dinitroresorcinol are mixed into 150 c. c. of water at 80 C. with 1.0 gm. magnesium oxide /2 equivalent), until substantially complete solution is attained.
- a curdy orange-yellow precipitate is formed at first, but soon this changes to a dark red dense granular precipitate. After cooling, filtering and washing with water, the material is dried at 40 C.
- the slightly lumpy product breaks down on gentle pressure to a dark red free-running powder.
- the product is found to be less sensitive to percussion and friction but somewhat more sensitive to flame than lead styphnate. It mixes well with lead azide, being superior to lead styphnate in this respect, and the resulting mixtures in proportions around 70% lead azide: 30% normal lead 2:4 dinitroresorcinate ignite satisfactorily in detonators for safety fuse or electric fuseheads, and initiate satisfactorily a base charge of tetryl.
- a process for the production of normal lead 2:4 dinitroresorcinate which comprises mixing together at a temperature not lower than 60 C. an aqueous solution of normal lead acetate with an aqueous solution containing a magnesium salt of 2:4 dinitroresorcinol having about V to the quantity of magnesium present in the normal magnesium salt, the said lead acetate and mag- 3 nesium salt being admixed in stoichiometrical equivalent weights.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB26542/46A GB616456A (en) | 1946-09-04 | 1946-09-04 | Improvements in or relating to the production of normal lead dinitroresorcinate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2493551A true US2493551A (en) | 1950-01-03 |
Family
ID=10245263
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US759705A Expired - Lifetime US2493551A (en) | 1946-09-04 | 1947-07-08 | Production of normal lead dinitroresorcinate |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US2493551A (en(2012)) |
| BE (1) | BE475824A (en(2012)) |
| DE (1) | DE817919C (en(2012)) |
| FR (1) | FR952626A (en(2012)) |
| GB (1) | GB616456A (en(2012)) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3301882A (en) * | 1963-01-07 | 1967-01-31 | Taylor George William Charles | Manufacture of normal lead 2:4-dinitroresorcinate |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB697475A (en) * | 1950-12-05 | 1953-09-23 | Ici Ltd | Improved initiating compositions for use in blasting and military detonators and their production |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1999728A (en) * | 1927-11-08 | 1935-04-30 | Remington Arms Co Inc | Manufacture of lead styphnate |
| US2116514A (en) * | 1935-09-26 | 1938-05-10 | George C Hale | Priming compositions |
-
0
- BE BE475824D patent/BE475824A/xx unknown
-
1946
- 1946-09-04 GB GB26542/46A patent/GB616456A/en not_active Expired
-
1947
- 1947-07-08 US US759705A patent/US2493551A/en not_active Expired - Lifetime
- 1947-09-01 FR FR952626D patent/FR952626A/fr not_active Expired
-
1949
- 1949-03-31 DE DEP2402D patent/DE817919C/de not_active Expired
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1999728A (en) * | 1927-11-08 | 1935-04-30 | Remington Arms Co Inc | Manufacture of lead styphnate |
| US2116514A (en) * | 1935-09-26 | 1938-05-10 | George C Hale | Priming compositions |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3301882A (en) * | 1963-01-07 | 1967-01-31 | Taylor George William Charles | Manufacture of normal lead 2:4-dinitroresorcinate |
Also Published As
| Publication number | Publication date |
|---|---|
| GB616456A (en) | 1949-01-21 |
| BE475824A (en(2012)) | |
| FR952626A (fr) | 1949-11-21 |
| DE817919C (de) | 1951-10-22 |
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