US3903219A - Process for mixing, pulverizing and grinding black powder - Google Patents

Process for mixing, pulverizing and grinding black powder Download PDF

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Publication number
US3903219A
US3903219A US425938A US42593873A US3903219A US 3903219 A US3903219 A US 3903219A US 425938 A US425938 A US 425938A US 42593873 A US42593873 A US 42593873A US 3903219 A US3903219 A US 3903219A
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United States
Prior art keywords
mill
particles
mixture
carbon
potassium nitrate
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US425938A
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English (en)
Inventor
Nicholas N Stephanoff
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Fluid Energy Processing and Equipment Co
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Fluid Energy Processing and Equipment Co
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Priority to US425938A priority Critical patent/US3903219A/en
Priority to ZA740624A priority patent/ZA74624B/xx
Priority to US05/529,373 priority patent/US3937405A/en
Priority to DE19742459624 priority patent/DE2459624A1/de
Priority to NO744553A priority patent/NO141471C/no
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/50—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle
    • B01F25/51—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle in which the mixture is circulated through a set of tubes, e.g. with gradual introduction of a component into the circulating flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/06—Jet mills
    • 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
    • C06B21/0008—Compounding the ingredient

Definitions

  • ABSTRACT A process and apparatus utilizing said process, whereby potassium nitrate, carbon and sulfur, plus any other desired additive, are inserted into a jet mill where the particles are mixed, pulverized and ground in a vortex of gaseous fluid while the vortex is moved through a curvilinear path, the smaller, lighter particles being centrifugally separated from the larger, heavier particles and then exhausted from the mill, the mill being constructed to decelerate the particles during initial mixture and to thereafter accelerate them through the curvilinear path, and then introducing the particles exhausted from the first mill into a second similar jet mill where an additional coating material is introduced and where the entire mixture is permitted to tumble and roll slowly to effect improved smoothing and coating.
  • Black powder consists essentially of an oxidizing agent such as potassium nitrate (KNO;,), charcoal and sulfur, with the optional addition of specific additives for specific purposes, as, for example, wood flour which is used to slow the burning for use in fuses or the like.
  • KNO potassium nitrate
  • charcoal and sulfur with the optional addition of specific additives for specific purposes, as, for example, wood flour which is used to slow the burning for use in fuses or the like.
  • the three essential raw materials are first pulverized separately, then mixed and ground together, this mixing and grinding constituting what is called incorporation.
  • this meal powder is compacted, then disintegrated, then sieved and finally polished, the polishing consisting of rounding and smoothing the particles by abrasion (called glazing) and then finishing which constitutes further smoothing by abrasion during which time a coating of finely pulverized carbonaceous material such as graphite is applied to the particles.
  • Jet or fluid energy mills utilize the particles themselves as the abrading and grinding means. This is accomplished by passing a stream of high velocity gaseous fluid through a curvilinear path. The particles are passed into the whirling stream of gas where they are engaged in a vortex action in which they collide and pulverize each other. At the same time they are whirled through the curvilinear path together with the gaseous stream. During this whirling action. the smaller. lighter particles are centrifugally separated from the larger. heavier particles and centrifugally exhausted from the mill While the heavier particles are returned for further pulverization with fresh material.
  • the aforesaid proposed method attempted to utilize the inherent cooling effect of the jet mills to speed up the process by pre-mixing the three essential components prior to insertion into the mill and then continuously passing a stream of the premixed composition through the mill, thereby avoiding the necessity of slow grinding andthe use of small batches. It was supposed that the incorporation step could take place in the completely dry state because the meal black powder prepared in this manner had no significant dusting and, therefore, it was not necessary to use moisture to bind the dust and increase compressibility, nor was it believed that water was necessary for safety. It was proposed to optionally add water to the cyclone dust collector which received the meal black powder after incorporation, but even this was not considered really necessary, nor was there any conception of the amount of water to be added or in what manner.
  • Another object of the present invention is to provide a process of the aforesaid type which is relatively simple and easy to use.
  • FIG. I is a generally schematic view of a jet mill system embodying the present invention, said system being utilized for the pulverization and incorporation steps used in the production of black powder.
  • FIG. 2 is a generally schematic view of a jet mill system embodying the present invention. said system being utilized for the polishing step.
  • the water is introduced into the mill in the form of a fine spray mist with the particles of water or other coolant preferably in a size range of about 0.01 to microns.
  • the amount of water entering the mill should be automatically metered in accordance with varying temperatures and pressures in the mill to retain 8595 percent RH.
  • This metering can be effected by any standard control means which may include a valve device, the opening of which is varied in accordance with a thermostat device set in a proper area of the mill.
  • Such heat-eontrolled valves are not, per se, part of the present invention, but any standard type may be used.
  • the water is dispersed into the fine mist by any desired means such as by a continuous stream of highpressure air causing fine atomization of the water.
  • This water mist or spray is directed into an incoming stream of potassium nitrate which is fed into the mill separately from the carbon and sulfur feed.
  • the water in addition to being dispersed into a fine mist, is preferably heated to a temperature higher than ambient, most preferably to a temperature between about 70 to 100C. This is done to permit more potassium nitrate to dissolve in the water mist, because potassium nitrate is sparingly soluble in cold water but easily soluble in hot water. in this respect, 100 grams of water will dissolve 246 grams of KNO at 100C. whereas at C. it will dissolve only 20 grams.
  • the collision of the water particles in the mist with the potassium nitrate particles dissolves at least a portion of the potassium nitrate and disperses the remainder so that there is created a spray of potassium nitrate, both dissolved and dispersed, which is directed toward the fed stream of carbon and sulfur mixture.
  • the spray is slowed down by an expanded portion in the downstack part of the mill, so that, upon impact, the mixing of the three components and the adsorption of the potassium nitrate on the carbon and sulfur is effected over a period of time sufficient to complete the mixture and adsorption.
  • the more potassium nitrate in solution the better, because the solution is not only more easily adsorbed onto the carbon but is also more easily absorbed thereinto to effect an impregnation of the carbon.
  • the carbon is preferably introduced in a chilled state, lower than ambient temperature, and, most preferably, lower than 0C.
  • the carbon may be pre-cooled to very low temperatures in liquid air or nitrogen.
  • carbon is much more absorptive when cold than when warm; for example, a piece of charcoal which will absorb 18 times its volume of oxygen at 0C, will absorb 230 times its own volume at lC. (the temperature of liquid air); and
  • the cold carbon and sulfur mixture will dissipate the heat resulting from the use of warm water in the spray directed against the dispersed potassium nitrate and from the heat generated by the grinding action. Though cooling is effected by the gas expansion itself, this further cooling action has been found most desirable.
  • the spray has been described as water so as to perform the double function of moisture additive and potassium nitrate dispersant and solvent, it is possible to add the water by other means and to use any other desired fluid in the spray.
  • the fluid may be a coolant material where it is not desired to obtain any great degree of solution of the potassium nitrate.
  • the mixture is then pulverized, mixed and ground in the usual manner in the jet mill and the meal is passed therefrom into a cyclone collector or the like. From there it passes to a hopper where any additional moisture which may be required is added. The mixture then. drops onto a conveyor where it is compacted. It is then disintegrated and sieved in the usual manner.
  • the product is now ready for polishing.
  • the polishing is effected in another jet mill, but not the same type as used for the incorporation.
  • This polishing mill is somewhat similar to the first one but is somewhat reversed in that it has an expanded portion in the upstack part of the mill, that is, in the part of the mill downstream from the part in which admixture of the components takes place. This is to permit the particles of the mixture to slow down and tumble over each other at the same time that they continue to travel around the mill. This permits smoother glazing and more satisfactory coating of the particles, which are the aspects of this polishing operation.
  • the components used in the polishing step are (a) the product of the incorporation, compacting, disintegration and sieving described above, and (b) graphite or the like.
  • the polishing operation as described above, comprises rounding and smoothing the particles by abrasion with each other (glazing) and further smoothing and simultaneous coating with graphite or the like (finishing")v Both operations are carried out simultaneously in the jet mill used for this purpose.
  • the powder from the first mill and the graphite are introduced into the mill by adjacent feed means and then passed through a first portion of the mill where low-pressure, low velocity air streams entrain them and cause glazing, after which they pass through the expanded portion of the upstack where finishing takes place.
  • the finished particles are then centrifugally exhausted from the mill to a cyclone collector, from where they pass to a hopper as a finished product.
  • FIG. 1 a jet or fluid energy mill, generally designated 10, comprising an inlet section 12, an upstack 14, a classification section 16, an exhaust duct 18 and a downstack 20.
  • the exhaust duct 18 is connected to an exhaust outlet on the inner periphery of the mill between the classification section 16 and the downstack 20.
  • the inlet section 12, upstack l4 and classifier section 16 all preferably combine to constitute a tractrix or antifriction, constant acceleration curveture, such as disclosed in US. Pat. No. 3,648,936, dated Mar. 14, 1972, to permit most efficient operation and to obviate undue wear of the mill.
  • the downstack 20 is made of expanded shape for the purpose of decreasing the velocity of the particles to permit more efficient mixing thereof and a greater time for adsorption and absorption of the potassium nitrate into the carbon and, to a lesser extent, the sulfur particles.
  • the mill operates in the general manner of such mills, having tangential inlet nozzles 22 leading from a manifold 24 into the inlet section 12.
  • the nozzle tips are preferably provided with nonfriction plastic liners such as nylon or the like, to decrease the possibility of generation of static electricity.
  • the manifold 24 is connected to a source of high pressure gaseous fluid, such as air, through a valve 26.
  • Raw feed particles entering through inlets hereinafter described, are entrained in the vortex and pulverize and grind each other at the same time that these particles are carried by the air through the upstack 14 and into the classification section 16.
  • the lighter particles are centrifugally separated from the heavier particles, the lighter particles passing along the radially inner wall of the mill and the heavier particles along the radially outer wall.
  • This classification is completed in the classification section 16 and, during their descent toward the downstack 20, the lighter particles pass through the exhaust outlet to the duct 18 from where they pass to a cyclone dust collector 28.
  • the heavier particles return through the downstack 20 to the inlet section 12, being admixed during this travel with fresh raw feed.
  • the raw feed comprises as indicated previously, three essential components, namely potassium nitrate, carbon (charcoal) and sulfur,
  • the carbon and sulfur may be fed into the mill separately or in pre-mixed admixture. the latter being preferred,
  • a mixture of carbon and sulfur is fed into the mill through a hopper 30, the particles of the mixture being propelled into the mill by a stream of gaseous fluid, such as air, under pressure, such gaseous fluid being shown as supplied by a conduit 32.
  • the conduit 32 is connected by a valve 34 to two separate, alternatively utilized conduits, indicated at 36 and 38 respectively.
  • the conduit 36 leads into the manifold 24 and utilizes the same high pressure air (usually at room temperature) as is passed through the inlets 22.
  • the conduit 38 is connected to a source (not shown) of chilled fluid which may be a cold gas, or which may be liquid air, nitrogen or the like.
  • the potassium nitrate is inserted separately into the mill, and whereas the carbon-sulfur mixture is inserted through hopper 30 situated below the downstack, the potassium nitrate is inserted through a hopper 40 situated above the downstack.
  • the potassium nitrate is propelled into the mill by high pressure gaseous fluid supplied by a conduit 42.
  • the conduit 42 is connected through a valve 44 to the manifold 24.
  • Both the inlets from hoppers 30 and 40 are preferably provided with Venturi passages in order to increase the velocity of their respective fluids.
  • the inlet from hopper 40 is directed at a downward angle so that the fed potassium nitrate moves angularly into the downstack.
  • an inlet duct 46 connected to a source of warm water (not shown), the water being preferably at a temperature of between about to C.
  • the inlet end 48 of the duct 46 is offset so that the water issuing therefrom is propelled into impact with a stream of high pressure air or the like issuing from a duct 50 connected to a source of high pressure air or the like, which may be the manifold 24 or any other desired source.
  • the high pressure air upon impact with the water, atomizes the water and projects a fine spray or mist angularly down toward impact with the potassium nitrate particles issuing from the hopper 40.
  • this warm water spray not only wets the potassium nitrate particles but dissolves a substantial portion thereof while dispersing the remainder in the spray.
  • the heated spray of potassium nitrate is slowed during passage through the expanded downstack and mixes intimately with the carbon-sulfur mixture, the warm spray being readily adsorbed and absorbed on the carbon particles which are particularly activated as they are simultaneously pulverized.
  • the carbon-sulfur mixture is fed into the mill by high pressure air or the like directed from the manifold 24 through conduits 36 and 32.
  • the carbon-sulfur mixture is fed by either chilled or liquid gas directed from a source thereof through conduits 38 and 32.
  • chilled fluid is also effective in cooling the heated temperature caused by the introduction of the heated potassium nitrate spray.
  • the gaseous fluid passes from the collector 28 through a duct 51 into filter 52 from where clean gas is exhausted through a duct 54 while residual powder passes through conduit 56 to a receiver 58.
  • the receiver 58 also receives the separated solids from collector 28.
  • the solid mixture passes to a rotary valve 60 through which the mixture is dropped onto a conveyor 62. While on the conveyor 62, the mixture is compacted by a compactor 64.
  • An additives, such as wood flour or the like, may be introduced into the mill either in admixture with the carbon and sulfur or through a separate feed inlet.
  • the incorporated" product produced by the system of FIG. 1 is now introduced into the system shown in FIG. 2 for polishing.
  • the polishing system comprises a jet or fluid energy" mill, generally designated 100, which is, in many respects, similar to the mill in that it has an inlet section 102 provided with tangential gaseous fluid inlets 104, an upstack 106, a
  • a hopper 114 having a high pressure fluid conduit 116 for propelling the material into the mill, is provided below the exhaust duct 112, this hopper being used for insertion of the incorporated mixture into the mill 100.
  • a second similar hopper 118 having a high pressure fluid conduit 120 is provided below the hopper 114, this hopper 118 being used for the introduction into the mill of finely divided graphite.
  • the upstack 106 of the mill 100 although still preferably provided with the tractrix" configuration, has an expanded portion while the downstack 110 is relatively narrow.
  • the particles are not only moving relatively slowly due to the low pressure air, but are further slowed down by the expanded upstack 106. As a result, the particles tumble and roll over each other, as indicated by the arrows in FIG. 2. This not only prevents excessive grinding while permitting rounding and smoothing, but increases the coating action of the graphite on the incorporated" particles.
  • the product which passes from exhaust duct 112 into a cyclone collector 122 is then freed from gaseous fluid, which flows upwardly through duct 124, and passes down into receiver 126 from where it passes through rotary valve 128 into a container 130 for the finished product.
  • mills and all other components of the system should be electrically grounded in order to avoid electrostatic sparking and the conse quent danger of explosion during the processing.
  • a method of making black powder which comprises pulverizing, grinding and blending a mixture of fed materials comprising potassium nitrate, carbon and sulfur by means of entraining said mixture in a centrifugally circulating stream of high pressure, high velocity gaseous fluid in a first curvilinear mill, said stream comprising a vortex wherein the particles of said mixture impact each other to pulverize and grind each other while simultaneously intermixing, said circulating stream causing the lighter particles to centrifugally separate from the heavier particles, said lighter particles being centrifugally exhausted from said mill while said heavier particles continue to circulate in said mill for further interaction with freshly fed materials, at least a portion of said particles being decelerated adjacent the area into which they are fed into the mill to provide enhanced intermixture thereof, the separated particles which are exhausted from the mill being thereafter compressed, disintegrated and sieved to form an incorporated mixture, said incorporated mixture being then fed into a second curvilinear mill having a centrifugally circulating stream of low pressure, low velocity gaseous fluid

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Paper (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
US425938A 1973-12-18 1973-12-18 Process for mixing, pulverizing and grinding black powder Expired - Lifetime US3903219A (en)

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US425938A US3903219A (en) 1973-12-18 1973-12-18 Process for mixing, pulverizing and grinding black powder
ZA740624A ZA74624B (en) 1973-12-18 1974-01-30 Process and apparatus for mixing,pulverizing and grinding black powder
US05/529,373 US3937405A (en) 1973-12-18 1974-12-04 Apparatus for mixing pulverizing and grinding black powder
DE19742459624 DE2459624A1 (de) 1973-12-18 1974-12-17 Verfahren und vorrichtung zum herstellen von schwarzpulver
NO744553A NO141471C (no) 1973-12-18 1974-12-17 Fremgangsmaate for fremstilling av svartkrutt

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US425938A US3903219A (en) 1973-12-18 1973-12-18 Process for mixing, pulverizing and grinding black powder

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4362584A (en) * 1980-09-03 1982-12-07 Pyrodex Corporation Method for binary propellant
EP0152280A2 (en) * 1984-02-08 1985-08-21 Dyno Industrier A.S. A method for coating high energy explosive crystals
US5541009A (en) * 1993-03-08 1996-07-30 Buck Werke Gmbh & Co. Process for preparing water-based pyrotechnic active compositions containing metal powder, coated metal powders and use thereof
US5633476A (en) * 1992-10-13 1997-05-27 Cioffe; Anthony Method of making a propellant and explosive composition
US5670098A (en) * 1996-08-20 1997-09-23 Thiokol Corporation Black powder processing on twin-screw extruder
US6451486B1 (en) 2000-05-01 2002-09-17 The Gillette Company Battery cathode including a mixture of manganese dioxide with carbon particles of expanded and non-expanded graphite
US20050158627A1 (en) * 2001-07-11 2005-07-21 The Gillette Company, A Delaware Corporation Battery
CN104030864A (zh) * 2014-06-26 2014-09-10 浏阳市工业园浏河机械厂 一种制造军工硝或黑火药的工艺及系统
CN105363314A (zh) * 2015-12-14 2016-03-02 浏阳市闩山木业有限公司 一种家具生产空气污染处理系统

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102010004738B4 (de) * 2010-01-14 2012-12-06 Wano Schwarzpulver Gmbh Schwarzpulver und Verfahren zu seiner Herstellung
CN104058903A (zh) * 2013-03-21 2014-09-24 蔡效铸 一种黑火药的制成方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3660546A (en) * 1970-02-04 1972-05-02 Norsk Spraengstofindustri As Process for the preparation of black powder

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3660546A (en) * 1970-02-04 1972-05-02 Norsk Spraengstofindustri As Process for the preparation of black powder

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4362584A (en) * 1980-09-03 1982-12-07 Pyrodex Corporation Method for binary propellant
EP0152280A2 (en) * 1984-02-08 1985-08-21 Dyno Industrier A.S. A method for coating high energy explosive crystals
EP0152280A3 (en) * 1984-02-08 1985-09-18 Dyno Industrier A.S. A method for coating high energy explosive crystals
US5633476A (en) * 1992-10-13 1997-05-27 Cioffe; Anthony Method of making a propellant and explosive composition
US5541009A (en) * 1993-03-08 1996-07-30 Buck Werke Gmbh & Co. Process for preparing water-based pyrotechnic active compositions containing metal powder, coated metal powders and use thereof
US5670098A (en) * 1996-08-20 1997-09-23 Thiokol Corporation Black powder processing on twin-screw extruder
US6451486B1 (en) 2000-05-01 2002-09-17 The Gillette Company Battery cathode including a mixture of manganese dioxide with carbon particles of expanded and non-expanded graphite
US20050158627A1 (en) * 2001-07-11 2005-07-21 The Gillette Company, A Delaware Corporation Battery
US6921610B2 (en) 2001-07-11 2005-07-26 The Gillette Company Battery
US7132198B2 (en) 2001-07-11 2006-11-07 The Gillette Company Battery
CN104030864A (zh) * 2014-06-26 2014-09-10 浏阳市工业园浏河机械厂 一种制造军工硝或黑火药的工艺及系统
CN105363314A (zh) * 2015-12-14 2016-03-02 浏阳市闩山木业有限公司 一种家具生产空气污染处理系统

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NO141471B (no) 1979-12-10
NO744553L (no) 1975-07-14
DE2459624A1 (de) 1975-10-30
ZA74624B (en) 1974-12-24
NO141471C (no) 1980-03-19

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