CA1080732A - Process for producing lead styphnate - Google Patents
Process for producing lead styphnateInfo
- Publication number
- CA1080732A CA1080732A CA260,355A CA260355A CA1080732A CA 1080732 A CA1080732 A CA 1080732A CA 260355 A CA260355 A CA 260355A CA 1080732 A CA1080732 A CA 1080732A
- Authority
- CA
- Canada
- Prior art keywords
- styphnate
- lead
- lead styphnate
- aqueous solution
- crystals
- 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
Links
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
-
- 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
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
Abstract
Abstract of the Disclosure A process for producing lead styphnate, which process comprises adding of an aqueous solution of lead nitrate with stirring to an aqueous solution of magnesium styphnate, the temperature being maintained above 40°C, and the process being carried out in the presence of a suspension of fine lead styphnate crystals. The lead styphnate may be used as an initiating explosive in priming compositions, particularly for sports ammunition cart-ridges.
Description
The invention relates to a process of producing lead styphnate, also known as lead 2,4,6 trinitroresorcinate, which may be used as initiating explosive in priming compositions for sports ammunition cartridges.
In order to be of practical value a priming composition must be able to fulfill a number of requirements. Particularly, although it must be capable of being exploded by a small pulse of energy from mechanical impact to ignite a charge of propellant, a priming composition must also be reason-ably safe and not easily exploded during manufacture and handling and filling into a cartridge case.
A priming composition for sports ammunition cartridges containing lead styphnate can be considered safe enough if an amount of 0.360 g of lead styphnate including 0.060 g of water is not ignited by a 5 g charge of black powder.
Known in the art is a process for producing lead styphnate accord-ing to which an aqueous solution of lead nitrate is added with stirring over a period of time, depending on the quantity of said solution, to an a~ueous soluti~n of magnesium styphnate. The temperature of tbis double decomposi-tion reaction is main~ained above 40C. The precipitated lead styphnate is washed by decantation with distilled water.
It is an object of the present invention to provide a process for the manufacture of lead styphnate in form of fine crystals of less than ~ ~t in si~e, which may be used as nuclei of crystallisation.
It is a further object of the invention to pro~ide a process for the manufacture of lead styphnate which in an amount of 0.360 g in a wet state, is not ignited by a charge of 5 g of black powder.
It is another object of the invention to provide lead styphnate in particles less than 50~4in si~e containing 20 % by weight of water, which may be used in making a priming composition, which easily ignites a charge of propellant, but is reasonably safe during manufacture, handling and fill-ing into cartridge cases.
~P~
According to the present invention there is provided a process for producing fine lead styphnate, which process comprises precipitating lead styphnate by adding an aqueous solution of lead nitrate with stirring to an aqueous solution of magnesium styphnate and further stirring the precipitated lead styphnate until lt becomes crystalline~ the temperature being maintained below 40C. during addition and stirring.
Thus, in one aspect, an aqueous solution of lead nitrate is quickly and instantaneously added with stirring to an aqueous solution of magnesium styphnate. The temperature of both solutions is maintained below 40C. The precipitated lead styphnate is stirred until it becomes crystalline. The crystalline lead styphnate, being in a wet state, is in the form of very fine and even crystals less than 4~ in size and may be used as the nuclei of cry-stallisation during manufac~ure of lead styphnate otherwise in accordance with methods known in the art.
According to another aspect of the invention, fine lead styphnate crystals are added with stirring to an aqueous solution of magnesium styph-nate. Then to the solution and dispersed fine lead styphnate crystals, an aqueous solution of lead nitrate is added with stirring over a period of time, the temperature being maintained above 40C. The precipitated lead styphna~e washed by decantation with distilled water is in the form of small even part-icles ]ess than 50 microns in si~e. An amount of 0.360 g of this lead styph-nate containing 0.060 g of water is not ignited by a 5 g charge of black powder.
The fine crystals of lead styphnate are added to the aqueous solu-tion of magnesium styphnate in any desired quantity, advantageously up to 8 percent by weight of dry mass based on the magnesium styphnate.
The formation of fine crystals of lead styphna~e, being the nuclei of crystallisation, is conveniently carried out in a liquid medium by a double decomposition reaction.
According to an important feature of the invention, lead styphnate is formed in a liquid mediwm in the presence of a suspension of fine crystals of lead styphnate, being the nuclei of crystallisation, whereby lead styph-nate as primary explosive is produced in a form of even crystalline particles having the size as desired.
Another feature of the invention is to provide lead styphnate in particles less than 50 microns in size which while wet in a 0.360 g amount is not ignited by a 5 g charge of black powder and which is suitable as a priming composition for sports ammunition cartridges, said composition in turn, although easily igniting a charge of propellent, is reasonably safe during manufacture, handling and filling into cartridge cases.
Three examples of processas for producing fine lead styphnate cry-stals, lead styphnate particles as primar~ explosive together with applica-tions of the lead styphnate particles in making priming compositions and sports ammunition cartridges will be described below.
Example 1 20 mls of an aqueous solution containing 8 g of lead nitrate is added quickly and instantaneously with rapid stirring to 90 ml of an aqueous solution containing 6.3 g of magnesium styphnate. The temperature of the both solutions is 30C. The resulting slurry is stirred until the precip-itated amorphous lead styphnate becomes crystalline. The size of the fine crystals is between 1.5 and 3 microns. 20 ml of the slurry containing fine crystals of lead styphnate is added with stirring to 900 ml of an aqueous solution oontaining 63 g of magnesium styphnate. Then to that suspension of fine lead styphnate crystals in the aqueous solution of magnesium styphnate, 200 ml of an aqueous solution containing 80 g of lead nitrate is added with stirring over a period of 3 minutes. The temperature of the magnesium sty-phnate solution and dispersed fine lead styphnate crystals in it is maintain-ed at 50C during the addition of the lead nitrate solution~ The precipitat-ed lead styphnate washed twice by decantation with distilled water and fil-tered contains 20 % of water by weight and has particles of 20 to 45 microns - ::
8~73~ ~ -in size. An amount of 0.360 g of this wet lead styphna~e is not ignited by a charge of 5 g of black powder. Then a priming composition is made using the wet lead styphnate, tetracene, barium nitrate, lead dioxide, ground glass and a water solution of arabic gum. Said priming composition is filled into cartridge cases and dried. Then propellant and bullets are added. The re-sulting sports ammunition cartridges, when tested in three sets and ten shots in each set~ hav0 a scatter diameter of 12 n~.
Exan~le 2 The procedure of Example l was followed~ except that 20 n~ of an aqueous solution containing 4 g of lead nitrate and 90 ~1 of an aqueous solu-tion containing 3.2 g of magnesium styphnate are used for obtaining the fine lead styphnate crystals.
The resulting fine lead styphnate crystals are 0.6 to 2.0 microns in size and the resulting lead styphnate particles are between 15 and ~0 microns in size.
Example 3 The procedure of Example 2 is followed, except that the temperature of the solution during precipitation of fine lead styphnate crystals is 20C.
The resulting fine lead styphnate crystals are 0O3 to 1.0 microns in si~e and the resulting particles of lead styphnate are between 15 and 30 microns in size.
In order to be of practical value a priming composition must be able to fulfill a number of requirements. Particularly, although it must be capable of being exploded by a small pulse of energy from mechanical impact to ignite a charge of propellant, a priming composition must also be reason-ably safe and not easily exploded during manufacture and handling and filling into a cartridge case.
A priming composition for sports ammunition cartridges containing lead styphnate can be considered safe enough if an amount of 0.360 g of lead styphnate including 0.060 g of water is not ignited by a 5 g charge of black powder.
Known in the art is a process for producing lead styphnate accord-ing to which an aqueous solution of lead nitrate is added with stirring over a period of time, depending on the quantity of said solution, to an a~ueous soluti~n of magnesium styphnate. The temperature of tbis double decomposi-tion reaction is main~ained above 40C. The precipitated lead styphnate is washed by decantation with distilled water.
It is an object of the present invention to provide a process for the manufacture of lead styphnate in form of fine crystals of less than ~ ~t in si~e, which may be used as nuclei of crystallisation.
It is a further object of the invention to pro~ide a process for the manufacture of lead styphnate which in an amount of 0.360 g in a wet state, is not ignited by a charge of 5 g of black powder.
It is another object of the invention to provide lead styphnate in particles less than 50~4in si~e containing 20 % by weight of water, which may be used in making a priming composition, which easily ignites a charge of propellant, but is reasonably safe during manufacture, handling and fill-ing into cartridge cases.
~P~
According to the present invention there is provided a process for producing fine lead styphnate, which process comprises precipitating lead styphnate by adding an aqueous solution of lead nitrate with stirring to an aqueous solution of magnesium styphnate and further stirring the precipitated lead styphnate until lt becomes crystalline~ the temperature being maintained below 40C. during addition and stirring.
Thus, in one aspect, an aqueous solution of lead nitrate is quickly and instantaneously added with stirring to an aqueous solution of magnesium styphnate. The temperature of both solutions is maintained below 40C. The precipitated lead styphnate is stirred until it becomes crystalline. The crystalline lead styphnate, being in a wet state, is in the form of very fine and even crystals less than 4~ in size and may be used as the nuclei of cry-stallisation during manufac~ure of lead styphnate otherwise in accordance with methods known in the art.
According to another aspect of the invention, fine lead styphnate crystals are added with stirring to an aqueous solution of magnesium styph-nate. Then to the solution and dispersed fine lead styphnate crystals, an aqueous solution of lead nitrate is added with stirring over a period of time, the temperature being maintained above 40C. The precipitated lead styphna~e washed by decantation with distilled water is in the form of small even part-icles ]ess than 50 microns in si~e. An amount of 0.360 g of this lead styph-nate containing 0.060 g of water is not ignited by a 5 g charge of black powder.
The fine crystals of lead styphnate are added to the aqueous solu-tion of magnesium styphnate in any desired quantity, advantageously up to 8 percent by weight of dry mass based on the magnesium styphnate.
The formation of fine crystals of lead styphna~e, being the nuclei of crystallisation, is conveniently carried out in a liquid medium by a double decomposition reaction.
According to an important feature of the invention, lead styphnate is formed in a liquid mediwm in the presence of a suspension of fine crystals of lead styphnate, being the nuclei of crystallisation, whereby lead styph-nate as primary explosive is produced in a form of even crystalline particles having the size as desired.
Another feature of the invention is to provide lead styphnate in particles less than 50 microns in size which while wet in a 0.360 g amount is not ignited by a 5 g charge of black powder and which is suitable as a priming composition for sports ammunition cartridges, said composition in turn, although easily igniting a charge of propellent, is reasonably safe during manufacture, handling and filling into cartridge cases.
Three examples of processas for producing fine lead styphnate cry-stals, lead styphnate particles as primar~ explosive together with applica-tions of the lead styphnate particles in making priming compositions and sports ammunition cartridges will be described below.
Example 1 20 mls of an aqueous solution containing 8 g of lead nitrate is added quickly and instantaneously with rapid stirring to 90 ml of an aqueous solution containing 6.3 g of magnesium styphnate. The temperature of the both solutions is 30C. The resulting slurry is stirred until the precip-itated amorphous lead styphnate becomes crystalline. The size of the fine crystals is between 1.5 and 3 microns. 20 ml of the slurry containing fine crystals of lead styphnate is added with stirring to 900 ml of an aqueous solution oontaining 63 g of magnesium styphnate. Then to that suspension of fine lead styphnate crystals in the aqueous solution of magnesium styphnate, 200 ml of an aqueous solution containing 80 g of lead nitrate is added with stirring over a period of 3 minutes. The temperature of the magnesium sty-phnate solution and dispersed fine lead styphnate crystals in it is maintain-ed at 50C during the addition of the lead nitrate solution~ The precipitat-ed lead styphnate washed twice by decantation with distilled water and fil-tered contains 20 % of water by weight and has particles of 20 to 45 microns - ::
8~73~ ~ -in size. An amount of 0.360 g of this wet lead styphna~e is not ignited by a charge of 5 g of black powder. Then a priming composition is made using the wet lead styphnate, tetracene, barium nitrate, lead dioxide, ground glass and a water solution of arabic gum. Said priming composition is filled into cartridge cases and dried. Then propellant and bullets are added. The re-sulting sports ammunition cartridges, when tested in three sets and ten shots in each set~ hav0 a scatter diameter of 12 n~.
Exan~le 2 The procedure of Example l was followed~ except that 20 n~ of an aqueous solution containing 4 g of lead nitrate and 90 ~1 of an aqueous solu-tion containing 3.2 g of magnesium styphnate are used for obtaining the fine lead styphnate crystals.
The resulting fine lead styphnate crystals are 0.6 to 2.0 microns in size and the resulting lead styphnate particles are between 15 and ~0 microns in size.
Example 3 The procedure of Example 2 is followed, except that the temperature of the solution during precipitation of fine lead styphnate crystals is 20C.
The resulting fine lead styphnate crystals are 0O3 to 1.0 microns in si~e and the resulting particles of lead styphnate are between 15 and 30 microns in size.
Claims (6)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for producing fine lead styphnate, which process comprises precipitating lead styphnate by adding an aqueous solution of lead nitrate with stirring to an aqueous solution of magnesium styphnate and further stirring the precipitated lead styphnate until it becomes crystalline, the temperature being maintained below 40°C. during addition and stirring.
2. A process for producing lead styphnate, which comprises adding an aqueous solution of lead nitrate with stirring to an aqueous solution of magnesium styphnate at a temperature above 40°C, there being provided a suspension of fine lead styphnate seed crystals in the solution of lead nitrate.
3. A process according to claim 2, wherein the fine lead styphnate crystals are those obtained by the process of claim 1.
4. A process according to claim 2, wherein the fine lead styphnate crystals are added in a quantity up to 8 percent by weight of dry mass based on the magnesium styphnate.
5. A process according to claim 2, 3 or 4, wherein the lead styphnate crystals are less than 4 microns in size.
6. A process according to claim 2, 3 or 4, wherein the lead styphnate is normal or basic one.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL18309175A PL116447B1 (en) | 1975-09-02 | 1975-09-02 | Method of manufacture of microcrystalline lead trinitroresorcinate |
| PL18874176A PL110860B1 (en) | 1976-04-12 | 1976-04-12 | Method of manufacture of priming composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1080732A true CA1080732A (en) | 1980-07-01 |
Family
ID=26652877
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA260,355A Expired CA1080732A (en) | 1975-09-02 | 1976-09-01 | Process for producing lead styphnate |
Country Status (3)
| Country | Link |
|---|---|
| AU (1) | AU1718876A (en) |
| BE (1) | BE845713A (en) |
| CA (1) | CA1080732A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030598A (en) * | 2010-11-04 | 2011-04-27 | 云南燃一有限责任公司 | DPLG (dinitro-diazophenol) burster and preparation method thereof |
| RU2754562C1 (en) * | 2020-10-08 | 2021-09-03 | Акционерное общество "Новосибирский механический завод "Искра" | Method for obtaining finely-crystalline lead trinitroresorcinate |
| RU2756556C1 (en) * | 2020-10-08 | 2021-10-01 | Акционерное общество "Новосибирский механический завод "Искра" | Lead trinitroresorcinate modified with carbon nanotubes and method for production thereof |
-
1976
- 1976-08-26 AU AU17188/76A patent/AU1718876A/en not_active Expired
- 1976-08-31 BE BE170243A patent/BE845713A/en unknown
- 1976-09-01 CA CA260,355A patent/CA1080732A/en not_active Expired
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030598A (en) * | 2010-11-04 | 2011-04-27 | 云南燃一有限责任公司 | DPLG (dinitro-diazophenol) burster and preparation method thereof |
| RU2754562C1 (en) * | 2020-10-08 | 2021-09-03 | Акционерное общество "Новосибирский механический завод "Искра" | Method for obtaining finely-crystalline lead trinitroresorcinate |
| RU2756556C1 (en) * | 2020-10-08 | 2021-10-01 | Акционерное общество "Новосибирский механический завод "Искра" | Lead trinitroresorcinate modified with carbon nanotubes and method for production thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| AU1718876A (en) | 1978-03-02 |
| BE845713A (en) | 1976-12-16 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MKEX | Expiry |