EP0021896B1 - Nouveau procédé de fabrication de poudres propulsives à base de nitrocellulose sans déshydratation préalable - Google Patents
Nouveau procédé de fabrication de poudres propulsives à base de nitrocellulose sans déshydratation préalable Download PDFInfo
- Publication number
- EP0021896B1 EP0021896B1 EP19800400768 EP80400768A EP0021896B1 EP 0021896 B1 EP0021896 B1 EP 0021896B1 EP 19800400768 EP19800400768 EP 19800400768 EP 80400768 A EP80400768 A EP 80400768A EP 0021896 B1 EP0021896 B1 EP 0021896B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- nitrocellulose
- solvent
- powder
- weight
- grains
- 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
- 239000000020 Nitrocellulose Substances 0.000 title claims description 47
- 229920001220 nitrocellulos Polymers 0.000 title claims description 47
- 239000003380 propellant Substances 0.000 title claims description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 230000018044 dehydration Effects 0.000 title description 3
- 238000006297 dehydration reaction Methods 0.000 title description 3
- 239000000843 powder Substances 0.000 claims description 43
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 36
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 36
- 239000002904 solvent Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000003381 stabilizer Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- 238000003490 calendering Methods 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- RUKISNQKOIKZGT-UHFFFAOYSA-N 2-nitrodiphenylamine Chemical compound [O-][N+](=O)C1=CC=CC=C1NC1=CC=CC=C1 RUKISNQKOIKZGT-UHFFFAOYSA-N 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 5
- 238000009987 spinning Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000013557 residual solvent Substances 0.000 description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 1
- DYSXLQBUUOPLBB-UHFFFAOYSA-N 2,3-dinitrotoluene Chemical compound CC1=CC=CC([N+]([O-])=O)=C1[N+]([O-])=O DYSXLQBUUOPLBB-UHFFFAOYSA-N 0.000 description 1
- 241000723346 Cinnamomum camphora Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 229960000846 camphor Drugs 0.000 description 1
- 229930008380 camphor Natural products 0.000 description 1
- PZIMIYVOZBTARW-UHFFFAOYSA-N centralite Chemical compound C=1C=CC=CC=1N(CC)C(=O)N(CC)C1=CC=CC=C1 PZIMIYVOZBTARW-UHFFFAOYSA-N 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
- 229940035422 diphenylamine Drugs 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000004381 surface treatment 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
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0066—Shaping the mixture by granulation, e.g. flaking
Definitions
- the present invention relates to the manufacture of propellant powders in grains based on nitrocellulose.
- the propellant powders in grains based on nitrocellulose are generally obtained by gelatinization of the fibrous nitrocellulose and cutting into grain of the nitrocellulose thus gelatinized.
- the gelatinization of the nitrocellulose is carried out by kneading the nitrocellulose fibers in the presence of suitable solvents and by extrusion of the paste thus formed.
- the extruded dough is cut into grains and the solvents are removed, often by soaking in water and air drying the powder grains which are then subjected to various surface treatments intended to fix agents on the powder grain surface.
- combustion moderators sino-called “smoothing” operation
- graphite in order to prevent the accumulation of static electricity on the powder grain (so-called “graphitizing” operation).
- nitrocellulose is a very sensitive and therefore dangerous body
- this product is kept wet with water so as to avoid any risk of ignition during its conservation or transport. It should therefore be dehydrated before using it for the production of a propellant powder.
- the dehydration of nitrocellulose is generally carried out by replacing the water with alcohol by means of a dehydrating press.
- the object of the present invention is to provide a simple and inexpensive process for manufacturing fine propellant powders based on non-dehydrated nitrocellulose.
- the starting point is aqueous nitrocellulose which is mixed in a kneader with a solvent.
- the choice of solvent is essential for the production and only the solvents chosen from the group consisting of methyl ethyl ketone, ethyl acetate or their mixtures in all proportions make it possible to achieve the result targeted by the invention: namely, thanks to a calendering operation, perfect elimination of the water contained in the nitrocellulose as well as good gelatinization of the latter.
- solvents usually used in the manufacture of powders such as acetone, methyl isobutyl ketone, ethyl alcohol or ethyl ether do not make it possible to achieve the result targeted by the invention.
- the content of the solvents used is generally between 50 ° / o and 100% by weight relative to the weight of dry nitrocellulose and according to a preferred embodiment of the invention between 60 ° / o and 80%.
- a stabilizer such as, for example, diphenylamine or 2-nitro-diphenylamine and preferably a plasticizer such as, for example, dinitro toluene or centralite, is preferably added.
- the duration of the mixing is generally close to two and a half hours.
- the dough thus obtained is then passed through a cold calender. During calendering the water contained in the dough is expelled and ensures by the same occasion me a cooling of the calender rollers; simultaneously, the passage between the rollers of the calender causes gelatinization of the nitrocellulose.
- the strip leaving the calendering machine is then wrung in air at room temperature and cut into flakes using a conventional cutter for strip powders.
- the powder grains thus obtained are soaked in hot water to remove the solvents and dried. They are then optionally smoothed so as to incorporate on their surface a combustion moderator such as camphor for example and finally they are graphitized.
- a combustion moderator such as camphor for example
- This example relates to the manufacture of propellant powder grains from wet nitrocellulose and ethyl acetate as a solvent.
- the powder grains thus obtained are soaked in hot water at 80 ° C for 8 hours and then air dried. Finally, the grains are graphitized in a bezel using 2% by weight of graphite relative to the weight of the powder.
- a propellant powder is thus obtained having a potential of 964 cal / g, an apparent density of 480 g / dm 3 , a weight content of residual solvent of 0.5 ° / o and a residual humidity of 1.20% by weight . In addition, there are 5000 grains per gram for this powder.
- This powder was fired into a 12.65 caliber shotgun.
- the cartridges contained 32 g of lead n. 6 and a felt pad.
- the firing results were as follows:
- the powder according to the invention gives entirely satisfactory ballistic performance. Furthermore, the Applicant has observed that this powder lights up very well, this is understandable in view of the high number of grains per gram of powder.
- This example relates to the manufacture of propellant powder grains from wet nitrocellulose and ethyl acetate as a solvent.
- a propellant powder is thus obtained having a potential of 972 cal / g, an apparent density of 524 g / dm ', a weight content of residual solvent of 1.0 ° / o and a residual humidity of 1.28% by weight .
- This powder was fired in a 12.65 caliber shotgun.
- the cartridges contained 32 g of lead n. 6 and a felt pad.
- the firing results were as follows:
- This example relates to the manufacture of propellant powder grains from nitrocellulose wet and a mixture of ethyl acetate, methyl ethyl ketone as solvent.
- a propellant powder is obtained having a potential of 967 cal / g, an apparent density of 500 g / dm 3 , a weight content of residual solvent of 0.60% and a residual humidity of 1.32% by weight.
- This example relates to the manufacture of propellant powder grains from wet nitrocellulose and a mixture of ethyl acetate, methyl ethyl ketone as solvent.
- the duration of the mixing is 2 hours.
- the dough is passed through a calendering machine, the rollers of which are spaced 0.08 mm apart.
- the strip coming out of the calendering machine is cut into flakes of 1 mm sides after half an hour of spinning.
- the powder grains are then soaked, dried and graphitized as described in Example 1.
- This example relates to the manufacture of propellant powder grains from wet nitrocellulose and methyl ethyl ketone as solvent.
- the duration of the mixing is two hours.
- the dough is passed through a calendering machine, the rollers of which are spaced 0.08 mm apart.
- the strip coming out of the calendering machine is cut into flakes with sides of 1 mm after half an hour of spinning at room temperature.
- the powder grains are then soaked, dried and graphitized as described in Example 1.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Medicinal Preparation (AREA)
- Paints Or Removers (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR7914539 | 1979-06-07 | ||
| FR7914539A FR2458523A1 (fr) | 1979-06-07 | 1979-06-07 | Nouveau procede de fabrication de poudres propulsives a base de nitrocellulose sans deshydratation prealable |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0021896A2 EP0021896A2 (fr) | 1981-01-07 |
| EP0021896A3 EP0021896A3 (en) | 1981-05-27 |
| EP0021896B1 true EP0021896B1 (fr) | 1982-12-01 |
Family
ID=9226307
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP19800400768 Expired EP0021896B1 (fr) | 1979-06-07 | 1980-05-30 | Nouveau procédé de fabrication de poudres propulsives à base de nitrocellulose sans déshydratation préalable |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP0021896B1 (show.php) |
| DE (1) | DE3061203D1 (show.php) |
| ES (1) | ES492073A0 (show.php) |
| FR (1) | FR2458523A1 (show.php) |
| IN (1) | IN159891B (show.php) |
| YU (1) | YU41928B (show.php) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2220934C2 (ru) * | 2002-03-19 | 2004-01-10 | Федеральное государственное унитарное предприятие "Научно-исследовательский институт полимерных материалов" | Способ изготовления зарядов для ракетных двигателей твердого топлива |
| RU2333189C1 (ru) * | 2007-01-09 | 2008-09-10 | Федеральное государственное унитарное предприятие "Научно-исследовательский институт полимерных материалов" | Способ изготовления заряда баллиститного твердого ракетного топлива |
| RU2434832C1 (ru) * | 2010-05-26 | 2011-11-27 | Федеральное государственное унитарное предприятие "Научно-исследовательский институт полимерных материалов" | Способ изготовления заряда баллиститного твердого ракетного топлива |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE560358A (show.php) * | ||||
| FR1145114A (fr) * | 1953-09-18 | 1957-10-22 | France Etat | Procédé pour la fabrication de poudres à la nitrocellulose |
| US3325571A (en) * | 1966-01-25 | 1967-06-13 | Hercules Inc | Process for the manufacture of smokeless powder |
-
1979
- 1979-06-07 FR FR7914539A patent/FR2458523A1/fr active Granted
-
1980
- 1980-05-14 IN IN352/DEL/80A patent/IN159891B/en unknown
- 1980-05-30 EP EP19800400768 patent/EP0021896B1/fr not_active Expired
- 1980-05-30 DE DE8080400768T patent/DE3061203D1/de not_active Expired
- 1980-06-02 ES ES492073A patent/ES492073A0/es active Granted
- 1980-06-04 YU YU148380A patent/YU41928B/xx unknown
Also Published As
| Publication number | Publication date |
|---|---|
| EP0021896A2 (fr) | 1981-01-07 |
| FR2458523A1 (fr) | 1981-01-02 |
| YU41928B (en) | 1988-02-29 |
| EP0021896A3 (en) | 1981-05-27 |
| ES8200319A1 (es) | 1981-11-01 |
| ES492073A0 (es) | 1981-11-01 |
| YU148380A (en) | 1983-02-28 |
| FR2458523B1 (show.php) | 1982-10-01 |
| DE3061203D1 (en) | 1983-01-05 |
| IN159891B (show.php) | 1987-06-13 |
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