US3714306A - Method of treating spherical powder grains - Google Patents
Method of treating spherical powder grains Download PDFInfo
- Publication number
- US3714306A US3714306A US00762641A US3714306DA US3714306A US 3714306 A US3714306 A US 3714306A US 00762641 A US00762641 A US 00762641A US 3714306D A US3714306D A US 3714306DA US 3714306 A US3714306 A US 3714306A
- Authority
- US
- United States
- Prior art keywords
- powder
- weight
- parts
- powder grains
- suspension
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000000725 suspension Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000008187 granular material Substances 0.000 claims abstract description 17
- 239000000084 colloidal system Substances 0.000 claims abstract description 16
- 230000001681 protective effect Effects 0.000 claims abstract description 13
- 108091005804 Peptidases Proteins 0.000 claims abstract description 8
- 102000035195 Peptidases Human genes 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 102000004190 Enzymes Human genes 0.000 claims description 22
- 108090000790 Enzymes Proteins 0.000 claims description 22
- 239000004922 lacquer Substances 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 229940024999 proteolytic enzymes for treatment of wounds and ulcers Drugs 0.000 abstract description 3
- 229940088598 enzyme Drugs 0.000 description 20
- 239000003380 propellant Substances 0.000 description 13
- 210000003491 skin Anatomy 0.000 description 11
- ALOUNLDAKADEEB-UHFFFAOYSA-N dimethyl sebacate Chemical compound COC(=O)CCCCCCCCC(=O)OC ALOUNLDAKADEEB-UHFFFAOYSA-N 0.000 description 6
- 239000003112 inhibitor Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 239000000020 Nitrocellulose Substances 0.000 description 4
- SNIOPGDIGTZGOP-UHFFFAOYSA-N Nitroglycerin Chemical compound [O-][N+](=O)OCC(O[N+]([O-])=O)CO[N+]([O-])=O SNIOPGDIGTZGOP-UHFFFAOYSA-N 0.000 description 4
- 239000000006 Nitroglycerin Substances 0.000 description 4
- 239000002360 explosive Substances 0.000 description 4
- 239000003925 fat Substances 0.000 description 4
- 229960003711 glyceryl trinitrate Drugs 0.000 description 4
- 229920001220 nitrocellulos Polymers 0.000 description 4
- 235000018102 proteins Nutrition 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229940014772 dimethyl sebacate Drugs 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 description 2
- 239000004367 Lipase Substances 0.000 description 2
- 102000004882 Lipase Human genes 0.000 description 2
- 108090001060 Lipase Proteins 0.000 description 2
- 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 2
- 239000000654 additive Substances 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229920002301 cellulose acetate Polymers 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 235000019421 lipase Nutrition 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- UZGLIIJVICEWHF-UHFFFAOYSA-N octogen Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)CN([N+]([O-])=O)C1 UZGLIIJVICEWHF-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 239000004449 solid propellant Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- AGUIVNYEYSCPNI-UHFFFAOYSA-N N-methyl-N-picrylnitramine Chemical compound [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
- 108010019160 Pancreatin Proteins 0.000 description 1
- 108090000526 Papain Proteins 0.000 description 1
- 239000000026 Pentaerythritol tetranitrate Substances 0.000 description 1
- 102000057297 Pepsin A Human genes 0.000 description 1
- 108090000284 Pepsin A Proteins 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 102000004142 Trypsin Human genes 0.000 description 1
- 108090000631 Trypsin Proteins 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 241001148470 aerobic bacillus Species 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000021120 animal protein Nutrition 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000002639 bone cement Substances 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 210000002808 connective tissue Anatomy 0.000 description 1
- LYAGTVMJGHTIDH-UHFFFAOYSA-N diethylene glycol dinitrate Chemical compound [O-][N+](=O)OCCOCCO[N+]([O-])=O LYAGTVMJGHTIDH-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012354 overpressurization Methods 0.000 description 1
- 229940055695 pancreatin Drugs 0.000 description 1
- 229940055729 papain Drugs 0.000 description 1
- 235000019834 papain Nutrition 0.000 description 1
- 229960004321 pentaerithrityl tetranitrate Drugs 0.000 description 1
- 229940111202 pepsin Drugs 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
- AGCQZYRSTIRJFM-UHFFFAOYSA-N triethylene glycol dinitrate Chemical compound [O-][N+](=O)OCCOCCOCCO[N+]([O-])=O AGCQZYRSTIRJFM-UHFFFAOYSA-N 0.000 description 1
- 239000012588 trypsin Substances 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
- C06B21/0091—Elimination of undesirable or temporary components of an intermediate or finished product, e.g. making porous or low density products, purifying, stabilising, drying; Deactivating; Reclaiming
Definitions
- Propellant powder grains made by the globular powder process have been used extensively for casting solid rocket propellants.
- the use of propellants in the form of a rod, a rod with internal star, hollow rod, multiple port rod, and the like is well known in the art for the purpose of controlling thrust throughout the combustion period.
- powder grains produced by the globular powder process have a skin present on their outer surface. It is theorized that this skin is caused by the retention by strong adsorption at the surface of protective colloids of animal origin which are used in the process. This skin adversely affects the propellant-inhibitor bond strength, as well as the tensile strength, of propellants cast from such powder grains.
- a more specific object of this invention is to provide a method for treating globular powder which results in an increase in the propellant-inhibitor bond strength and tensile strength of a propellant cast from such powder.
- Yet another object of this invention is to provide a method for removing the skin from globular powder grains caused by the adsorption of animal origin colloids.
- the invention contemplates treating globular powder grains with an enzyme which will hydrolyze either protein or fats. Since this skin is of animal origin and may contain a wide variety of fats and proteins, this invention further contemplates a mixture of enzymes including proteolytic enzymes which are substances which have the ability to attack proteins and effect hydrolysis to amino acids and lipases which are enzymes that effect the hydrolysis of fat.
- the powder grains to be treated are prepared in accordance with the conventional globular powder process.
- a lacquer is prepared consisting of a suitable powder base, such as nitrocellulose, dissolved in a solvent.
- suitable powder base such as nitrocellulose
- solvents suitable for use with nitrocellulose include methyl ethyl ketone, ethyl formate, isopropyl acetate, diethyl ketone, ethyl acetate and mixtures thereof.
- the lacquer prepared in accordance with the above.- identified procedure may be presized if desired and then admixed with a non-solvent suspending material.
- a non-solvent suspending material may be any liquid that is substantially immiscible with the lacquer, an aqueous medium is generally preferred.
- the non-solvent material also contains a protective colloid and/or other additives which are described more fully below.
- the protective colloids are preferably of animal origin such as the type derived from animal protein, animal bone glue, or the like. Chemically each of these protective colloids is a collagen which by definition is an albuminoid comprising the major portion of the white fiber in the connectivetissues of the animal body, particularly in the skin, bones and tendons. This colloid may be present in the non-solvent material in a proportion equivalent to between about 0.1 and about 0.5 percent by weight.
- Liquid high energy compounds such as triethylene glycol dinitrate, diethylene glycol dinitrate, and nitroglycerin may be added with the lacquer to the suspending material in a proportion up to about 50 percent by weight of the powder base in order to increase the burning rate of the solid powder grains ultimately produced and to serve as a plasticizer when the powder is used as a component of solid propellants.
- a crystalline high explosive composition in finely divided form may be added to the lacquer or solvent material prior to or during mixing. Any crystalline high explosive composition which is substantially insoluble in the water immisciblesolvent used in preparing the lacquer of nitrocellulose can be used in thepreparation of the novel rocket cast granules of this invention.
- Suitable explosive compositions include HMX (cyclotetramethylenetetranitramine), RDX (cyclotrimethylenetrinitramine), PETN (pentaerythritol tetranitrate), 2,4,6-trinitrophenylmethylnitramine, and mixtures thereof.
- Any suitable mixing vessel provided with a mechanical agitator or other mixing device may beemployed.
- the mixture is kept under agitationsufficient to maintain the state of suspension until the suspended presized bodies of lacquer become rounded under the force of interfacial tension.
- Mixing of the lacquer and suspending material, and the formation of the globules may be carried out ata temperature between about 10C and about C, or any temperature above the freezing point of the mixture and below the boiling point of the volatile solvent. Pressures above atmospheric pressure may be employed during mixing to inhibit evaporation of the solvent at higher temperatures.
- Agitation of the lacquer in the suspending material for a period of at least about one-half hour, and as long as 1 hours or more, is generally necessary to form globules of the desired size and shape and, if utilized, to effect substantially complete dispersion of the particles of highly explosive composition or other solid additives in the lacquer globules.
- an additional amount of solvent for the nitrocellulose may be slowly added for agitation with the suspension. This addition of solvent causes a breakdown in the lacquer globules and additional lacquer globules are formed having a diameter substantially less than the original globules.
- the solvent may then be evaporated from the lacquer globules by increasing the temperature of the suspension up to the distillation temperature by bubbling air or other inert gas through the suspension. If the specific gravity and porosity of the individual powder grains are not critical, the evaporation may be continued until complete solidification of the lacquer globules is obtained whereupon the resulting solids are then separated from the non-solvent material for further processing in accordance with this invention. If the specific gravity and porosity of the powder grains is critical, additional processing may be performed prior to the final evaporation and complete solidification of the globules.
- powder grains produced by the globular powder process are further treated with an enzyme or mixture of enzymes which will hydrolize proteins and/or fats which are in the skin of the powder particles due to the protective colloid.
- an enzyme or mixture of enzymes which will hydrolize proteins and/or fats which are in the skin of the powder particles due to the protective colloid.
- any proteolytic enzymes, any of the lipases, or combinations of the two types may be used.
- the enzymes which are particularly effective are pepsin, papain, those enzymes produced by aerobic bacteria, trypsin, and pancreatin.
- Serizyme which is a trademark for a standardized bacterial proteolytic enzyme preparation of the Wallerstein Co. may be used.
- the powder grains to be treated may be loaded into a vessel equipped with an agitator along with suitable quantity of water.
- the agitation is started and run at a sufficient speed to keep the powder grains in suspension in the water.
- the proportion of water in relation to the powder grains may vary widely with the only requirement being that there must be enough water present to suspend the powder grains.
- one part by weight powder grains to three parts by weight water is used.
- l00 parts by weight of powder grains produced by the globular powder process were loaded into a vessel equipped with an agitator along with 300 parts by weight of water.
- Swift Colloid No. l was used as the protective colloid.
- the agitation was started and continued at a sufficient speed to keep the powder grains in suspension.
- the enzyme Serizyme in the proportion of nine parts by weight enzyme to parts by weight powder grains, was added to the vessel and the temperature raised to 40C. The agitation was continued for 4 hours, after which the powder was separated from the treatment material in a centrifuge, washed with clear water to remove the residual material, and dried.
- Test specimens were prepared by mixing the treated powder grains with a solution of 60 parts by weight nitroglycerin and 40 parts by weight dimethyl sebacate in a ratio of approximately 69 parts by weight of powder to 31 parts by weight of the solution. The resulting slurry was cast into a cylindrical mold, cured at F for 48 hours, and then machined to produce a dumbbell-shaped specimen. The average of standard tensile tests performed on the specimens was a tensile strength of 620 p.s.i.
- powder grains produced by the same globular powder process and treated with the enzyme Serizyme in the manner described above were mixed with a solution of 60 parts by weight nitroglycerin and 40 parts by weight dimethyl sebacate. The mixture was approximately 69 parts by weight powder to 31 parts by weight solution.
- the mixture was cast into a mold having a cellulose acetate inhibitor and cured to bond the propellant thereto. After curing, the propellant with the cellulose acetate inhibitor was mounted in a testing machine and the propellant peeled from the inhibitor. The average of the tests performed was 35.7 pounds per inch.
- specimens prepared from powder grains produced by the globular powder process, but untreated with an enzyme were tested to provide a comparison.
- the results of the tests performed upon such specimens were 17 pounds per inch, less than half that exhibited by the specimens prepared with grains treated in accordance with this invention.
- a method of treating powder granules that have a skin present on their outer surface due to a protective colloid of animal origin being present during the formation thereof comprising suspending said powder granules in a mixture of an aqueous solution and a proteolytic enzyme, agitating said suspension until substantially all of said skin is removed, and
- suspension comprises one part by weight powder grains to 3 parts by weight water and 9 parts by weight enzyme to 100 parts by weight powder grains.
- a method of treating globular powder granules that have been produced by suspending droplets of lacquer of a smokeless powder base and a solvent in a non-solvent medium and a protective colloid of animal origin and then solidified into granules of a globular shape, having a skin on their outer surface, said method comprising suspending said solidified globular powder granules in a mixture of an aqueous solution and a proteolytic enzyme, agitating said suspension until substantially all of said skin is removed, and thereafter separating said powder granules from the remainder of the materials.
- suspension comprises one part by weight powder grains to 3 parts by weight water and 9 parts by weight enzyme to I parts by weight powder grains.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Cosmetics (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US76264168A | 1968-09-25 | 1968-09-25 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3714306A true US3714306A (en) | 1973-01-30 |
Family
ID=25065676
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US00762641A Expired - Lifetime US3714306A (en) | 1968-09-25 | 1968-09-25 | Method of treating spherical powder grains |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US3714306A (https=) |
| BE (1) | BE739375A (https=) |
| DE (1) | DE1946824A1 (https=) |
| FR (1) | FR2018832A1 (https=) |
| GB (1) | GB1233295A (https=) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2496757C1 (ru) * | 2012-04-10 | 2013-10-27 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") | Способ получения сферического пороха для стрелкового оружия |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2027114A (en) * | 1932-03-12 | 1936-01-07 | Western Cartridge Co | Manufacture of smokeless powders |
| US3400026A (en) * | 1967-01-16 | 1968-09-03 | Du Pont | Thickened aqueous inorganic oxidizer salt explosive composition containing dissolvedproteinaceous material |
-
1968
- 1968-09-25 US US00762641A patent/US3714306A/en not_active Expired - Lifetime
-
1969
- 1969-06-13 GB GB1233295D patent/GB1233295A/en not_active Expired
- 1969-09-16 DE DE19691946824 patent/DE1946824A1/de not_active Withdrawn
- 1969-09-23 FR FR6932399A patent/FR2018832A1/fr not_active Withdrawn
- 1969-09-25 BE BE739375D patent/BE739375A/xx unknown
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2027114A (en) * | 1932-03-12 | 1936-01-07 | Western Cartridge Co | Manufacture of smokeless powders |
| US3400026A (en) * | 1967-01-16 | 1968-09-03 | Du Pont | Thickened aqueous inorganic oxidizer salt explosive composition containing dissolvedproteinaceous material |
Also Published As
| Publication number | Publication date |
|---|---|
| GB1233295A (https=) | 1971-05-26 |
| FR2018832A1 (https=) | 1970-06-26 |
| DE1946824A1 (de) | 1970-08-20 |
| BE739375A (https=) | 1970-03-25 |
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