US3704185A - Progressive burning smokeless powder coated with an organic ester - Google Patents
Progressive burning smokeless powder coated with an organic ester Download PDFInfo
- Publication number
- US3704185A US3704185A US437632A US3704185DA US3704185A US 3704185 A US3704185 A US 3704185A US 437632 A US437632 A US 437632A US 3704185D A US3704185D A US 3704185DA US 3704185 A US3704185 A US 3704185A
- Authority
- US
- United States
- Prior art keywords
- powder
- ester
- coated
- grain
- nitrocellulose
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/20—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component
- C06B45/28—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component the component base containing nitrocellulose and nitroglycerine
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
Definitions
- Smokeless powder is the name given to a propellant consisting mainly of nitrocellulose.
- a propellant consisting mainly of nitrocellulose.
- the particles, or grains as they are commonly called, of the smokeless powder with what is referred to as a deterrent material, explosive or non-explosive, which will retard the initial burning rate of the powder grains.
- the quantity of coating material which penetrates the powder grains decreases toward the interior thereof, so that as the powder burns, the successively exposed surfaces contain gradually less and less of the deterrent material, thus causing the combustion of the grains to proceed with increasing speed.
- a common deterrent is dinitrotoluene.
- dinitrotoluene as the deterrent material, powder grains coated with dinitrotolucne are subjected to heat with or without the presence of moisture or water.
- the powder grains are coated by treatment with a solution of dinitrotoluene in benzene, the benzene evaporated, and penetration of the dinitrotoluene into the grain of powder obtained by immersing the coated powder grains in a hot water bath for several hours or several days.
- the powder grains and deterrent material are covered with water, and after mixing, heat is applied for varying periods.
- the powder grains are surface treated by an alkyl phthalate, either in solution or in aqueous emulsion.
- This invention provides deterrent-coated smokeless powder having, inter alia, outstanding ballistic stability.
- the smokeless powder of this invention is progressiveburning powder base grain surface-coated with a waterinsoluble organic ester, said ester melting below about 35 C., and boiling above about 200 C. and having a solubility for the nitrocellulose in said smokeless powder between about that of ethylene dimethacrylate and ethylene dipropionate.
- the smokeless powder of this invention is prepared by agitating the smokeless powder grains with one or more of the aforementioned esters at a temperature of about from 20 to C., the ester component usually being present in amounts of about 2 to 10% based on the weight of base grain.
- the ester is introduced in the form of an emulsion in a non-solvent therefor, preferably water.
- the smokeless powder compositions of the present invention are designed to be used at chamber pressures above 10,000 p.s.i. and comprise both single and double base propellants and sporting as well as military powder.
- the manufacture of the base grain, i.e., the grain on which the deterrents of the present invention are coated, is standard in the industry and descriptions can be found, for example, in Military Explosives Technical Manual 9-1910, 1957.
- the nitrocellulose used in the base grain used for the present invention is conventional military-grade nitrocellulose having an overall nitrogen content between about 12.8 and 13.4%. A single lot of nitrocellulose having the aforementioned nitrogen content can be used or, alternately, a blend having an overall nitrogen content within the desired range can be used. In addition to nitrocellulose, other energetic ingredients such as nitroglycerin, nitroguanidine, diethylene glycol dinitrate, triethylene glycol dinitrate and others can be present.
- the agitation of the base grain with the ester can be carried out in several ways.
- an aqueous emulsion of the ester deterrent is agitated with water-wet base grain.
- a conventional sweetie barrel such as that used in the powder industry for applying dinitrotoluene coatings is a suitable apparatus for carrying out the agitation.
- the base grain also can be slurried with water and the ester in an agitated tank fitted with a heating jacket or heating coils.
- ester either per se or as a solution or dispersion in a nonsolvent for the base grain, can be sprayed on the base grain while it is tumbled or otherwise agitated to spread the ester evenly.
- a continuous process can be used with, for example, the base grain being placed in one end of a rotating tubular agitator and progressing down the agitator. During its progression down the agitator the base grain enters a zone where it is sprayed with the ester, then a zone where it is heated to within the aforementioned temperature range, and finally to a discharge zone where it falls from the agitator into containers.
- Other operations such as glazing with graphite, also can be carried out in the tubular agitator after the ester coating has been formed, before discharge of the glazed powder.
- emulsification is effected by vigorously agitating the ester with from about 0.5 to 6, and preferably 0.8 to 1.5 times its weight of water, and about from 0.2 to 5%, and preferably 0.6 to 2% of an anionic emulsifier alone or mixed with up to an equal quantity of a non-ionic emulsifier, both based on the total weight of ester.
- Emulsifiers of these classes are described in Detergents and EmulsifiersUp to Date, 1963, John W. McCutcheon Inc.
- emulsifiers include alkaryl sodium sulfonates such as Nacconol NRSF, Sulframin L, Sulframin NAB, Santomerse SX, Santomerse E, Santomerse 85 (dodecylbenzene sodium sulfonate), Ultrawet 3ODS, 68KN, 60L, 35KK, SK and Oronite S; alkyl sulfates such as Duponol C (sodium lauryl sulfate), sodium oleyl sulfate, sodium stearyl sulfate, Teepol, Duponol ME, Alcoterge, sodium cetyl sulfate, Conco Sulfate WA (sodium lauryl sulfate), Dehydag Wax E, Nopco 1477; alkyl aryl polyether sulfates such as Triton 770, X-301 and 202; amide sulfonates such as
- phosphate esters such as Tergitol P-28 (sodium di(2-ethylhexyl)phosphate), Victamuls 20, 24C, 27, 89; esters of polyphosphoric acids such as Na R (P O where R is a C radical such as capryl or Z-ethylhexyl (Victawets 35B and 58B), ester and ether-linked sulfonates such as Igepon AC-78 (coconut oil acid ester of sodium isethionate), dialkyl sodium sulfosuccinates (Aerosol OT-di-2-ethylhexyl sodium sulfosuccinate).
- non-ionic emulsifiers which can be used in conjunction with the anionic detergents in proportions up to 50% or more by weight of the total emulsifier include polyethenoxy ethers of alkyl phenols such as Igepals RC-76'0, DM-710, DM730 and RC-520 (alkylphenoxypoly(ethylenoxy)ethanols) and Tritons N128, N101 and N-100 (nonylphenyl polyethoxy ethanols); polyethenoxy ethers of fatty alcohols such as Tergitols 3A3, 3A6 and 3A9 (polyoxyethylated tridecyl alcohol); polyethenoxy esters such as Teox 120 (polyethenoxy tallate); polyethenoxy mercaptans such as Penetrant 100; polyethenoxy glycols such as the Tweens (polyoxyethylene sorbitan monolaurate, monopalmitate, monostea
- the quantity of ester coated on the surface of the base grain depends on the ballistic qualities desired in the powder. In general, the quantity of ester will range between about 2% and about 10% of the weight of the base grain with the preferred quantity being from about 2.5 to about 6%.
- the quantity of ester of the present invention needed for obtaining desired ballistic properties is generally considerably less than the quantity of dinitrotoluene needed to obtain similar ballistic properties in conventional powder.
- the temperature of coating can be varied between about C. and about 120 C. and the time of coating can be varied between about 5 minutes and about six hours depending on the ester used, the type of powder coated, the procedure employed, and the results desired.
- the preferred temperature lies between about 70 C. and 100 C. for about A to 1 hour.
- the base grain can be water-dried after coating if preferred.
- a water-dry treatment reduces the chamber pressure of the coated powder to a level slightly below that generated by the powder not water-dried.
- water-dry treatments merely involve heating the coated base grain in water at about from 50 to 60 C. for about 12 to 48 hours.
- the organic esters used in this invention have a melting point below about 35 C., a boiling point above about 200 C. at atmospheric pressure and a solvency for the nitrocellulose in the product between about that of ethylene dimethacrylate and ethylene dipropionate, inclusive, Esters, such as dibutyl phthalate, in which the nitrocellulose is considerably more soluble, lead to ballistic instability. Esters which are substantially poorer solvents are not well enough absorbed to give required muzzle velocities at or below the maximum allowable pressure.
- Solvency can often be measured visually. However, since the smokeless powder is often a blend containing some relatively insoluble factions, a convenient method for measuring solubility is as follows: A sample of the nitrocellulose is leached thoroughly with ten times its weight of 65/35 ether/ethanol, filtered, the solvent evaporated and the recovered nitrocellulose dried at 45 C. Solutions of this nitrocellulose are prepared 1% concentration by weight) in ethylene dimethacrylate, ethylene dipropionate and the ester under test. The viscosity of each is then measured in an Ostwald-Fenske viscometer. Since the solvent power of the ester is related to the viscosity of the solutions, the viscosity of the ester under test measured as described above should fall between about that of the ethylene dimethacrylate solution and that of the ethylene dipropionate solution.
- esters which can be used in accordance with this invention are esters of aromatic, aliphatic, and cycloaliphatic polyols or polybasic acids with monobasic acids or monohydric alcohols, respectively, particularly the aliphatic monofunctional derivatives.
- the esters can be saturated, that is, free of ethylenic unsaturation as in the case of ethylene dipropionate.
- esters bearing vinyl (CH C unsaturation, and preferably two or three such substituents are particularly preferred.
- esters examples include the alkylene acrylates such as ethylene dimethacrylate, triethylene diacrylate and triethylene dimethacrylate as well as the allyl phthalates such as diallyl phthalate and diallyl isophthalate.
- alkylene acrylates such as ethylene dimethacrylate, triethylene diacrylate and triethylene dimethacrylate as well as the allyl phthalates such as diallyl phthalate and diallyl isophthalate.
- 'Ethylene dimethacrylate is a particularly preferred ester because of the optimum stability of products made therewith.
- the esters should be substantially water insoluble, i.e., soluble to an extent less than 10% in water at 25 C.
- the powder of the present invention shows several advantages over conventionally-coated powder. It has a higher gravimetric density, thus allowing more powder to be placed in a shell of fixed size.
- the chemical stability as indicated by conventional tests such as the Taliani test and the methyl violet paper (MVP) test is considerably greater.
- the velocity-pressure relationship is higher, thus a lower weight of charge can be used to attain the same velocity.
- the velocity-pressure relationship is more stable to hot storage.
- the flame temperature is lower, thus giving a longer barrel life.
- EDM-ethylenedimethacrylate MVPmethyl violet paper stability test (MIL-STD-286 Method 404.1.1, June 28, 1956)
- TalianiTaliani stability test (MIL-STD-286, Method 406.1 (T) June 28, 1956) tExplosionHours to explosion when heated at 134.5 C.
- EXAMPLE 1 The nitrocellulose used in this example is leached thoroughly with ten times its weight of 65/35 ether/alcohol and filtered. The solvent is evaporated and the nitrocellulose dried at 45 C. Solutions of this dried nitrocellulose (1% by weight) are made in ethylene dipropionate and ethylene dimethacrylate. The viscosities are measured in an Ostwald-Fenske viscometer. The solution in ethylene dipropionate has a viscosity of 69.5 centistokes and the solution in ethylene dimethacrylate has a viscosity of 167.1 centistokes.
- a mixture of 100 parts of nitrocellulose containing 13.2% nitrogen, 1 part of potassium sulfate and 0.7 part of diphenylamine is converted into a perforated singlebase extruded, base grain through a 0.046 OD. x 0.015 die and cut to & inch lengths by conventional means.
- the powder of this example gained only 5400 p.s.i. in chamber pressure while the DNT-coated powder gained 8200 p.s.i. in pressure at the same weight of charge.
- the following table shows ballistic test results on the powder of this example in comparison with the aforementioned DNT coated control powder and an IMR 4475 commercial powder used for 30/06, .308 and 7.62 mm. rifles.
- the tests are made in the same 7.62 mm. barrel using drilled cases, the charges are shot within l-2 hour period and corrected to original barrel assessment.
- the components are: shellFrankford Arsenal with No. 36M primer; bulletFrankford Arsenal M-80 ball, 147 grain.
- a shotgun powder base grain is made having the following characteristics:
- Composition 100 parts nitrocellulose (13.2% nitrogen);
- NorE.-Final powder dimensions 0.057 by 0.009 by 0.0008.
- Example 1 The general procedure of Example 1 was repeated using the powders and coating materials noted below.
- the table below records the chemical stability of the products so components (grains) 4 5 0 Obtained.
- the base grain is an IMR 4350 granulation for the .30/06 rifle. Final grain dimensions 0.050 x 0.008 x 0.084 inch.
- Example 9 the water-wet base grain of Example 1 (15% total volatile) (100 parts dry basis) is charged to a sweetie barrel.
- An emulsion is prepared by vigorously agitating 4 parts of ethylenedimethacrylate with 4 parts of water and 0.04 part of Gafac RE610. This emulsion is added to the rotating sweeties barrel slowly over about 5 minutes; agitation is continued at room temperature for a total of 25 minutes. Steam is then introduced into the barrel while continuing agitation to raise the temperature to 8590 C. over a period of 25 minutes. Agitation is continued at 8590 C. for 30 minutes. The contents of the sweetie barrel are discharged while hot and the powder is air dried at 55 C. overnight. The dry powder is glazed and screened. The moisture content of the powder is adjusted to 1.10i0.l%.
- Example 10 the procedure above is repeated except EXAMPLES 16 AND 17
- the following table shows the exceptional ballistic stability of commercial single-base propellant base grains similar to those in Example 1 coated in accordance with this invention as compared to a DNT coated standard powder after long periods of storage at 150 F. in 7.62 mm. cartridges:
- Example 16 41.8 4.0% EDM Before heat aging 2, 740 44, 900 2, 701 44, 600 2, 715 44, 500 After heat aging. 2, 736 46, 200 2, 707 46, 100 2, 703 45, 900 Change 4 +1, 300 +6 +1, 500 +12 +1, 400
- Example 17 42.0 4.5% EDM Before heat aging. 2, 725 42, 800 2, 681 41, 000 2, 687 40, 600 After heat aging 2, 716 43, 400 2, 718 44, 800 2, 731 47, 100 Change 0 600 +37 +3, 800 +44 +6, 500 Control Before heat aging. 2, 758 50, 700 2, 740 49, 800 2, 741 49, 500 After heat aging 2, 791 58, 100 2, 762 58, 600 2, 829 71, 900 Change +33 +7, 400 +22 +8, 800 +88 +22, 400
- the properties of the products are:
- Example 0 Example 10 Control Ballistics:
- the deterrent rating is calculated by determining the ballistics of powder coated with 4% of the deterrent after several days storage at ambient conditions and after days storage at 150 F. Each powder is fired at a constant velocity against a standard. The difference between the pressure of the ester-coated powders under ambient conditions from the standard is algebraically added to the increase in pressure of the ester-coated powder on heat aging. The more negative the result the better the powder.
- Progressive burning smokeless powder made from base grain coated with about from 2 to 10% based on the weight of said base grain of at least one of the group consisting of ethylene dipropionate, ethylene dimethacrylate, triethylene diacrylate, diallyl phthalate and triethylene dimethacrylate.
- a powder of claim 2 wherein said ester is ethylene dimethacrylate.
- a powder of claim 2 wherein said ester is ethylene dipropionate.
- a powder of claim 2 wherein said ester is diallyl phthalate.
- a process which comprises agitating smokeless powder base grains with organic ester at a temperature of about from 20 to 120 C., said ester having a melting point below 35 C. and a boiling point above 200 C., the nitrocellulose in said base grain having a solubility in said ester between about that in ethylene dimethacrylate and that in ethylene dipropionate, inclusive.
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Medicinal Preparation (AREA)
- Paints Or Removers (AREA)
Abstract
Description
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US43763265A | 1965-03-01 | 1965-03-01 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3704185A true US3704185A (en) | 1972-11-28 |
Family
ID=23737244
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US437632A Expired - Lifetime US3704185A (en) | 1965-03-01 | 1965-03-01 | Progressive burning smokeless powder coated with an organic ester |
Country Status (3)
Country | Link |
---|---|
US (1) | US3704185A (en) |
FR (1) | FR1605059A (en) |
GB (1) | GB1282861A (en) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3897733A (en) * | 1973-03-19 | 1975-08-05 | Us Army | High bulk density extruded propellant for small arms cartridges |
US4092187A (en) * | 1976-08-18 | 1978-05-30 | The United States Of America As Represented By The Secretary Of The Army | Process for coating crystalline high explosives |
US4106960A (en) * | 1976-02-03 | 1978-08-15 | Dynamit Nobel Aktiengesellschaft | Temperature-compensating propellant charge |
US4300961A (en) * | 1980-04-28 | 1981-11-17 | Hercules Incorporated | Process for deterrent coating of triple base propellant compositions |
US4654093A (en) * | 1983-07-13 | 1987-03-31 | Aktiebolaget Bofors | Method of producing progressively burning artillery propellant powder and agent adapted thereto |
US20150321969A1 (en) * | 2013-01-29 | 2015-11-12 | Nitrochemie Wimmis Ag | Powder for accelerating projectiles for mortar systems |
RU2627406C1 (en) * | 2016-06-15 | 2017-08-08 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") | Spherical powder |
RU2762228C2 (en) * | 2020-05-27 | 2021-12-16 | Федеральное казенное предприятие "Казанский государственный казенный пороховой завод" | PYROXYLIN POWDER FOR EQUIPMENT OF HUNTING AND SPORTS CARTRIDGES OF CALIBER 7.62x51 |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2623796B1 (en) * | 1987-11-30 | 1991-08-30 | Poudres & Explosifs Ste Nale | PROCESS FOR THE PRODUCTION OF NITROCELLULOSE-CONTAINING TWO-COMPOSITION PROPULSIVE POWDER ELEMENTS AND POWDER ELEMENTS THUS OBTAINED |
CN102826942B (en) * | 2012-09-18 | 2013-07-31 | 湖南省浏阳金生花炮有限公司 | Smokeless firework propellant |
RU2561083C1 (en) * | 2014-02-04 | 2015-08-20 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") | Powder phlegmatising agent |
RU2584284C2 (en) * | 2014-08-14 | 2016-05-20 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") | Charge for 7,62(53 mm sporting rifle cartridge |
RU2633920C1 (en) * | 2016-06-22 | 2017-10-19 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") | BALL POWDER FOR 5,6 mm SPORTS HUNTING CARTRIDGE OF RING IGNITION |
-
1965
- 1965-03-01 US US437632A patent/US3704185A/en not_active Expired - Lifetime
-
1966
- 1966-03-01 FR FR1605059D patent/FR1605059A/fr not_active Expired
- 1966-03-01 GB GB9033/66A patent/GB1282861A/en not_active Expired
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3897733A (en) * | 1973-03-19 | 1975-08-05 | Us Army | High bulk density extruded propellant for small arms cartridges |
US4106960A (en) * | 1976-02-03 | 1978-08-15 | Dynamit Nobel Aktiengesellschaft | Temperature-compensating propellant charge |
US4092187A (en) * | 1976-08-18 | 1978-05-30 | The United States Of America As Represented By The Secretary Of The Army | Process for coating crystalline high explosives |
US4300961A (en) * | 1980-04-28 | 1981-11-17 | Hercules Incorporated | Process for deterrent coating of triple base propellant compositions |
US4654093A (en) * | 1983-07-13 | 1987-03-31 | Aktiebolaget Bofors | Method of producing progressively burning artillery propellant powder and agent adapted thereto |
US20150321969A1 (en) * | 2013-01-29 | 2015-11-12 | Nitrochemie Wimmis Ag | Powder for accelerating projectiles for mortar systems |
RU2627406C1 (en) * | 2016-06-15 | 2017-08-08 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") | Spherical powder |
RU2762228C2 (en) * | 2020-05-27 | 2021-12-16 | Федеральное казенное предприятие "Казанский государственный казенный пороховой завод" | PYROXYLIN POWDER FOR EQUIPMENT OF HUNTING AND SPORTS CARTRIDGES OF CALIBER 7.62x51 |
Also Published As
Publication number | Publication date |
---|---|
FR1605059A (en) | 1973-01-12 |
GB1282861A (en) | 1972-07-26 |
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Legal Events
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Owner name: ETI EXPLOSIVES TECHNOLOGIES INTERNATIONAL INC., RO Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:E.I. DU PONT DE NEMOURS AND COMPANY;REEL/FRAME:004834/0446 Effective date: 19880118 Owner name: ETI EXPLOSIVES TECHNOLOGIES INTE,STATELESS Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:E.I. DU PONT DE NEMOURS AND COMPANY;REEL/FRAME:004834/0446 Effective date: 19880118 |
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Owner name: TORONTO DOMINION BANK,STATELESS Free format text: SECURITY INTEREST;ASSIGNOR:ETI EXPLOSIVES TECHNOLOGIES INTERNATIONAL INC.;REEL/FRAME:004829/0868 Effective date: 19871231 Owner name: TORONTO DOMINION BANK Free format text: SECURITY INTEREST;ASSIGNOR:ETI EXPLOSIVES TECHNOLOGIES INTERNATIONAL INC.;REEL/FRAME:004829/0868 Effective date: 19871231 |