SE192003C1

SE192003C1 -

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Publication number: SE192003C1
Authority: SE
Publication date: 1964-01-01

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Uppfinnare: R L Cook och E A Andrew, Jr Prioritet begard frcin den 4 oktober 1954 (USA) Denna uppfinning hfinfor sig allmant till framstallningen av drivmedelskrut och den avser nfirmare besta.mt framstallningen av sfariska och nastan sffiriska korn av rokfritt krut. Inventors: R L Cook and E A Andrew, Jr Priority Required April 4, 1954 (USA) This invention relates generally to the production of propellant gunpowder and relates more closely to the production of spherical and almost spherical grains of smokeless gunpowder.

Uppfinningen avser ett forfarande for framstfillning av globulara krutkorn med i huvudsak likformig sammansattning hestaende i losning av ett rokfritt krutmaterial i ett lasningsmedel for detta till bildning av en massa, utpressning av massan genom en oppning till en strom av en suspenderingsvatska, vilken fir i huvudsak joke blandbar med losningsmedlet, och avskarning av lika stora kroppar fran den utpressade massan nar den lamnar oppningen, varigenom massakropparna suspenderas i vatskan. Det for uppfinningen kilnnetecknande är, att bade suspenderingsvatskan och massan bringas att stromma i reglerad mangd, sa att forhallandet mellan suspenderingsvatska och massa Mlles i huvudsak konstant under forfarandet, och att suspenderingsvatskan med de dari suspenderade massakropparna ledes till en med omrorare forsedd destillationsapparat och att de suspenderade massakropparna darefter avrundas och hardas pa i och for sig kfint satt i destillationsapparaten. The invention relates to a process for producing globular powder grains having a substantially uniform composition in solution of a smokeless powder material in a welding agent therefor to form a mass, squeezing the mass through an opening into a stream of a suspension liquid, which is essentially a joke. miscible with the release agent, and cutting off bodies of equal size from the extruded pulp as it leaves the opening, thereby suspending the pulp bodies in the liquid. It is characteristic of the invention that both the suspension liquid and the pulp are caused to flow in a controlled amount, so that the ratio between suspension liquid and pulp is substantially constant during the process, and that the suspension liquid with the pulp bodies suspended therein is led to a stirred distillation apparatus and the suspended pulp bodies are then rounded and hardened in and of themselves neatly placed in the distillation apparatus.

I den amerikanska patentskriften 2 027 114 beskrives ett forfarande for framstallning av rokfritt knit, dar droppar air lOsning, besta.ende av rokfritt krutmaterial och losningsmedel, bringas att hardna medan de aro suspenderade i ett icke-losningsmedelsmedium. Ett sâdant forfarande for framstallning air drivmedelskrut har beteclmats forfarande for framstallning air globulart krut. Tekniken for reglering av forfarandet for framstallning av globulart krut sa att det bildas korn med olika fysikaliska och kemiska egenskaper be-shrives vidare i de amerikanska patentskrif- Dupl. kl. 78 c: 8; 78 c: 9; 78 c: terna 2 160 626, 2 213 255 och 2 375 175. Dessa patentskrifter beskriva variationer i den grundlaggande tekniken for framstfillning av globulart krut, varigenom arten, likformigheten och de ballistiska egenskaperna hos det bildade krutet regleras. U.S. Pat. No. 2,027,114 discloses a process for preparing a smokeless knit in which droplets of air solution, consisting of smokeless gunpowder and solvent, are allowed to harden while suspended in a non-solvent medium. One such process for the production of propellant air has the same process for the production of globular gunpowder. The technique for regulating the process for the production of globular powder said that the formation of grains with different physical and chemical properties is further described in the American patent specification- Dupl. at 78 c: 8; 78 c: 9; 78 c. 2,160,626, 2,213,255 and 2,375,175. These patents describe variations in the basic technique for producing globular gunpowder, thereby regulating the nature, uniformity and ballistic properties of the gunpowder formed.

I patentet 2 027 114 beskrives bland annat en utfOringsform av forfarandet for framstfillning air globulart krut, enligt vilken del raffia krutmaterialet loses i losningsmedel for bildning av losningen hell och hallet i franyaro av suspensionsvatskan, men i praktiken utmarktes denna utforingsform av mind-re kemisk likformighet hos kornen an de utforingsformer, dar materialet lOstes av lOsningsmedlet i narvaro air suspensionsvatskan. A andra sidan är genomforandet air forfarandet fOr framstallning av globulfirt krut forbmidet med manga betingelser, dar den forstnamnda utforingsformen erbjuder fordelar Over den sistnananda utforingsformen. I fall, cla man onskar i de ffirdiga kornen infOrliva ett material, vilket antingen icke uppvisar Omsesidig loslighet med losningen av rOkfritt krutmaterial, eller vilket an losligt i suspenderingslosningen, är det exempelvis miijligt att genom mekaniska medel bOrdela detta material i god likformighet i hela losningen av rokfritt krutmaterial, vilken beredes separat och skild frail suspenderingsmediet, men det fir praktiskt taget omOjligt att uppnâ nagonting som narmar sig likformig fordelning air ett sadant material, nar losningen av krutmaterial beredes i nfirvaro av suspenderingsmediet. Kalciumkarbonat an ett exempel pa ett sadant material, vilket, da det fir olOsligt i losningen av krutmaterial, kan dispergeras i denna losning (i franvaro av suspenderingsliisningen) med sadan likformighet, att varje bildat globulärt krutkorn teoretiskt bör inne- hâllanara samma procenthalt kal- 2— — eiumkarbonat. Det har emellertid iakttagits, att i en given charge ha vissa korn innehallit den onskade mangden kalciumkarbonat, medan andra korn innehallit mindre och andra inget kalciumkarbonat ails. Det formodas att denna olikformighet hos produkten har berott pa det fOrhallandet, att vid det vanliga forfarandet sattes krutmateriallosning i mangd till icke-losningsmedelsmediet och nedlnytes till slutlig partikelstorlek. Nedbrytningsprocessen stracker sig over en avsevard tidrymd — ett korn kan uppna sin slutliga storlek omedelbart, medan ett storre uppdelas ett antal ganger, innan det uppnar sin slutliga storlek — sa att det foreligger en avsevard lucka melIan den slutliga formningen av de forsta och sista kornen. Denna lucka inverkar pa den likformighet, med vilken tillsatsen kvarhalles av de individuella kornen i 15sningen. Nar tillsatsen icke är lOslig i krutmateriallosningen, beror forlusten darav fran losningen pa den grad av knadfling, som utfores pa en given kropp av krutmateriallosning vid dess reduktion till slutlig storlek. Ju forr en sadan kropp av krutmateriallOsning uppnar sin slutliga storlek, desto forr upphOr dess uppdelning (med atfoljande exponering av nya ytor) och desto mindre av tillsatsen gar forlorad. Nar a andra sidan tillsatsen fir i huvudsak loslig i suspenderingslosningen, gar den fOrlorad fran kornen av krutmateriallosning genom lakning. Lakningen är delvis en funktion av den totals. ytan (i relation till total volym). I sin slutliga storlek ha salunda kropparna av krutmateriallOsning en stor specifik yta i jamforelse med sin volym, och de f6rsta kornen som uppna. sin slutliga storlek utsattas for maximal lakning. I de tidiga stadierna av operationen ar en jamforelsevis star volym suspensionslosning tillganglig for att inverka pa de fá sma kropparna, som omedelbart reduceras till slutlig storlek, medan den stoma massan av krutmateriallosning ãr nastan ogenomtranglig for lakningsverkan vid detta tillfalle. De sma kropparna, vilka bildas senare, utsattas aven for lakning, men under tiden ha tva saker intraffat, vilka minska effekten darav. FOr det forsta är den tid, under vilken senare bildade kroppar utsattas f8r lakning, kortare an den lid, under vilken tidigare bildade kroppar utsattas for lakning. For det andra okas koncentrationen av material, som lakas, i suspenderingslosningen alit eftersom operationen fortgar, och den drivkraft, som bestfimmer lakningskraften, reduceras foljaktligen successivt alit eftersom operationen fortgar. Patent 2,027,114 discloses, inter alia, an embodiment of the process for producing air globular gunpowder, according to which part of the raffia powder material is dissolved in solvent to form the solution poured and the hall in the form of the suspension liquid, but in practice this embodiment is distinguished by less chemical uniformity. in the case of the granules of the embodiments where the material is dissolved by the solvent in the narvaro air suspension liquid. On the other hand, the implementation of the process for the production of globular gunpowder powder is provided with many conditions, where the former embodiment offers advantages over the latter embodiment. In cases where it is desired in the finished grains to incorporate a material which either does not show reciprocal solubility with the solution of smokeless gunpowder material, or which is soluble in the suspension solution, it is possible, for example, by mechanical means to distribute this material in good uniformity throughout the solution. of smokeless gunpowder material, which is prepared separately and separately from the suspending medium, but it is practically impossible to achieve anything which approaches a uniform distribution of such a material when the solution of gunpowder material is prepared in the presence of the suspending medium. Calcium carbonate is an example of such a material, which, since it is insoluble in the solution of gunpowder material, can be dispersed in this solution (in the absence of the suspension solution) with such uniformity that each globular powdered granule formed should theoretically contain the same percentage of calcium. - - eium carbonate. It has been observed, however, that in a given batch some grains contained the desired amount of calcium carbonate, while other grains contained less and others no calcium carbonate ails. It is presumed that this non-uniformity of the product has been due to the fact that in the usual process powder solution solution was added in quantity to the non-solvent medium and reduced to final particle size. The decomposition process extends over a considerable period of time - a grain can reach its final size immediately, while a larger one is divided a number of times, before it reaches its final size - so that there is a considerable gap between the final formation of the first and last grains. This gap affects the uniformity with which the additive is retained by the individual grains in the seed. When the additive is not soluble in the powder material solution, the loss thereof from the solution depends on the degree of kneading carried out on a given body of powder material solution when it is reduced to final size. The sooner such a body of powder material solution reaches its final size, the sooner its division ceases (with consequent exposure to new surfaces) and the less of the additive is lost. On the other hand, when the additive is substantially soluble in the suspension solution, it is lost from the grains of powder material solution by leaching. The leaching is partly a function of the total. surface (in relation to total volume). In their final size, the salunda bodies of powder material solution have a large specific surface area in comparison with their volume, and the first grains to reach. its final size is exposed to maximum leaching. In the early stages of the operation, a comparatively large volume of suspension solution is available to affect the few small bodies, which are immediately reduced to final size, while the solid mass of powder material solution is almost impermeable to the leaching effect in this case. The small bodies, which are formed later, are also exposed to leaching, but in the meantime two things have occurred, which reduce the effect thereof. First, the time during which later formed bodies are subjected to leaching is shorter than the time during which previously formed bodies are subjected to leaching. Second, the concentration of material being leached in the suspension solution alit as the operation proceeds, and the driving force which optimizes the leaching force is consequently gradually reduced alit as the operation proceeds.

En tillsats, sasom kalciumkarbonat, vilken fir bade oloslig i krutmateriallosningen och vasentligt loslig i suspenderingsvatskan, utsattes salunda for tva typer av forIust, men de utbalansera icke varandra pa grund av det foreliggande tidsintervallet, vilket bidrager till skillnaden. radian de forst och de sist bildade kropparna av krutmateriallosning. An additive such as calcium carbonate, which is both insoluble in the powder material solution and substantially soluble in the suspension liquid, is thus subjected to two types of loss, but they do not balance each other due to the present time interval, which contributes to the difference. radian the first and last formed bodies of powder material release.

DetdarfOr ett andamal med denna upp- finning att astadkomma ett forfarande for framstallning av globulart krut, vid vilket krutmateriallosningen beredes i franvaro av suspenderingsvatskan, men dar den ovan beskrivna olikformigheten bland kornen i samma charge reduceras eller i huvudsak elimineras. It is an object of this invention to provide a process for the production of globular powder, in which the powder material solution is prepared in the absence of the suspension liquid, but in which the above-described uniformity among the grains in the same batch is reduced or substantially eliminated.

Enligt denna uppfinning loses det rokfria krutmaterialet i losningsmedel i franvaro av suspenderingsmediet och alla tillsatser, vilka Onskas i de fardiga globulara kornen, inblandas mekaniskt i den erhallna krutmateriallosningen for att sakerstalla den onskade likformigheten hos fordelningen dad — alltsammans fore den tidpunkt, da. krutmateriallosningen bringas i beroring med suspenderingsmediet. Exempel pa sadana tillsatser aro kalciumkarbonat, kimrok, tenn, nitroguanidin och vilket annat material som heist, inbegripet vatten, vars narvaro I krutmateriallosningen astadkommer eller framkallar onskvarda egenskaper (fysikaliska eller kemiska) i de bildade kornen. Sedan tillsatsen eller tillsatserna fordelats likformigt i hela krutmateriallosningen, sonderdelas denna I forkalibrerade kroppar med slutlig volym nastan omedelbart. Dessa kroppar suspenderas omedelhart i en relativt liten volym suspenderingsmedium, och den bildade suspensionen avlagsnas omedelbart fran det stalle, dar den beretts. Nar mera krutmateriallosning sonderdelas, tillsattas alikvota delar suspenderingslosning, sa att massfOrhallandet mellan krutmateriallosning och suspenderingsvatska ar konstant och koncentrationsandringseffekter minskas. En serie av sma. tillskott av krutmateriallosning och suspenderingsvatska sammanforas och omvandlas fran sina ursprungliga till sina slutliga (volym- och suspensions-)-tillstand, innan de bildade tillskotten av suspensionen sammanfOras i ett lampligt karl, i vilket formnings- och hardningsfaserna fOrfarandet for framstallning av globulart krut genomforas. According to this invention, the smokeless powder material is dissolved in solvent in the absence of the suspending medium and all additives desired in the finished globular grains are mechanically mixed into the obtained powder material solution to ensure the desired uniformity of the distribution dad - all for the time being. the powder material solution is brought into contact with the suspending medium. Examples of such additives are calcium carbonate, carbon black, tin, nitroguanidine and any other material which is raised, including water, the presence of which in the powder material solution creates or produces undesirable properties (physical or chemical) in the formed grains. After the additive or additives are uniformly distributed throughout the powder material solution, it is subdivided into pre-calibrated bodies with final volume almost immediately. These bodies are immediately hard-suspended in a relatively small volume of suspension medium, and the resulting suspension is immediately removed from the stable where it was prepared. When more powder material solution is probed, aliquot parts of suspension solution are added, so that the mass ratio between powder material solution and suspension liquid is constant and concentration change effects are reduced. A series of small. additions of gunpowder material solution and suspension liquid are combined and converted from their original to their final (volume and suspension) state, before the formed additions of the suspension are combined in a suitable vessel in which the forming and curing phases of the globular powder production process are carried out.

Uppdelningen och den ursprungliga suspensionen av losningskropparna kan genomforas och gen:omfores lampligen vid en sadan temperatur, att de forkalibrerade lOsningskropparna bringas att »stelna», vilket betyder att de ej aro tillrackligt flytande for att ge efter for ytspanningskrafter 1 den gemensamma ytan och icke tillrackligt klibbiga fOr att vidhafta vid tillfallig beroring eller att forenas till en kontinuerlig fas. Harigenom blir det m6jligt att driva suspensionen genom rorledningar Over avsevarda avstand eller att forvara den tillffilligt med ej mer omroring an vad som erfordras, for att halla suspensionen i rorelse, vilket Or langt mindre an den grad av omroring, som tidigare ansetts nodvandig for att undvika sammansmaltning av — — de uppdelade losningskropparna. I sjalva. verket kan omroringen avbrytas och losmngskropparna tillatas avsatta sig pa varandra under nagra minuter utan olagliga resultat nar de pa detta satt bringas att »stelna». The partition and the initial suspension of the release bodies can be carried out and resuspended at such a temperature that the precalibrated solution bodies are caused to "solidify", which means that they are not sufficiently liquid to give way to surface tension forces in the common surface and are insufficient. sticky to adhere to accidental contact or to unite into a continuous phase. This makes it possible to drive the suspension through pipelines over considerable distances or to store it temporarily with no more agitation than is required, in order to keep the suspension in motion, which is far less than the degree of agitation previously considered necessary to avoid fusion of - - the divided discharges. In itself. the agitation can be stopped and the release bodies are allowed to settle on each other for a few minutes without illegal results when they are thereby caused to "solidify".

Tillsatsen av en liten mangd vatten till losningen av krutmaterial och den likformiga fOrdelningen darav i hela lOsningen innan denna bringas i beroring med suspenderingsmedlet medfor flera fordelar, forutsatt att mangden vatten inorn varje sadan forkalibrerad kropp av losning regleras kvantitativt och vattenhalten i de individuella forkalibrerade losningskropparna kan bringas att fOrbli likformig. Kvantitativ reglering av vattenmangden i en forkalibrerad kropp av 15sning är emellertid omojlig, nar lOsningskroppen underkastas omroring av sadan haftighet, att den medfOr notning i ett snspenderingsmedium bestaende huvudsakligen av vatten, emedan sa haftig °mewing ej endast har bendgenhet att emulgera mera vatten in i losningen, utan varje ny losningsyta, som blottas under denna nOtning, mojliggOr bortgang av nagot vatten frail det inre av losningskroppen. Nar vatten utgor tillsatsen Ar det dad& viktigt ej endast att sAdan kraftig °mewing, som emulgerar vatten in i ltisningen, undvikes, utan aven att varje forkalibrerad 18sningskropp reduceras till sin slutliga storlek med endast en avskiljning i narvaro av suspenderingsvatskan (i motsats till ett forfarande for uppdelning, I vilket en given kropp av losningen skulle kunna uppdelas i tva delar, de bildade halvorna uppdelas i tva. delar, de darvid bildade fjardedelarna uppdelas i tva delar etc.). Anvandningen av vatten som tillsats till losningen under kvantitativ reglering mojliggor framstallning av globuldra korn, som aro porosa invandigt (med sammanhangande ytskikt), och porositetsgraden regleras genom vattenmangden inom varje forkalibrerad losningskropp, och genom reglering av vattenmangden thorn varje kalibrerad kropp kan man darfor framstalla globulara krutkorn med storre eller mindre gravimetrisk Whet. The addition of a small amount of water to the solution of gunpowder material and the uniform distribution thereof throughout the solution before it is brought into contact with the suspending agent has several advantages, provided that the amount of water within each such precalibrated body of solution is quantitatively regulated and the water content of the individual precalibrated solution brought to remain uniform. However, quantitative control of the amount of water in a pre-calibrated body of solution is impossible when the solution body is subjected to agitation of such vigor that it involves use in a suspension medium consisting mainly of water, since such vigorous motion does not only tend to emulsify more water into the solution. , without each new discharge surface, which is exposed during this use, it is possible to remove some water from the interior of the discharge body. When water is the additive, it is important not only that such a strong mixture, which emulsifies water into the ice, is avoided, but also that each precalibrated solution body is reduced to its final size with only one separation in the presence of the suspension liquid (as opposed to a procedure for division, in which a given body of the solution could be divided into two parts, the formed halves divided into two parts, the thereby formed quarter parts divided into two parts, etc.). The use of water as an additive to the solution under quantitative control makes it possible to produce globular grains, which are porous internally (with coherent surface layers), and the degree of porosity is regulated by the amount of water within each precalibrated solution body, and by regulating the amount of water in each calibrated body. powder grains with larger or smaller gravimetric Whet.

Oberoende av mu tillsatser inf8rlivas i losningen Ar forfarandet enligt uppfinningen fordelaktigt, i den man det omfattar fOrkalibrering och suspendering av losningskroppar en relativt liten volym suspenderingsvatska och omedelbart avlagsnande av den bildade suspensionen Iran bildningsstallet. Foljaktligen ar uppfinningen icke begransad till losningar, i vilka tillsatser inforlivas. Regardless of the additives incorporated in the solution, the process according to the invention is advantageous, in that it comprises precalibration and suspension of solution bodies a relatively small volume of suspension liquid and immediate removal of the formed suspension from the formation. Accordingly, the invention is not limited to solutions in which additives are incorporated.

PA den bifogade ritningen visar fig. 1 ett arbetsschema, som belyser relationen mellan de olika stegen i forfarandet och schematiskt visar den anvanda apparaten. Fig. 2 Ar en sidoprojektion (varav en del Ar bortbruten for att visa relationen mellan elementen.), delvis i sektion, av en apparat for uppdelning av en strOm av losning i fOrkalibrerade kroppar. In the accompanying drawing, Fig. 1 shows a working diagram which illustrates the relationship between the various steps in the process and schematically shows the apparatus used. Fig. 2 is a side projection (part of which is broken away to show the relationship between the elements.), Partly in section, of an apparatus for dividing a stream of discharge into precalibrated bodies.

PA fig. 1 pa ritningen Ar en lOsningsbehaIlare 1 genom en pump 2 och en r5rledning 3 forbunden med en kornbildningsapparat 4 av den typ, som beskrives narmare i det foljande. Ett forrad av suspenderingsvatska hallos i en behallare 5, vilken genom en. pump 6 och en strOmningsmatare 7 Ar fOrbunden med kornbildningsapparaten 4. Den senare Ar forsedd med ett tangentiellt utlopp 8, vilket genom en rOrledning 9 Ar fOrbundet med en destillationsapparat 10 av det slag, som vanligen anvandes i forfarandet fOr framstallning av globulart krut. In Fig. 1 of the drawing, a solution container 1 is connected by a pump 2 and a pipeline 3 to a grain-forming apparatus 4 of the type described in more detail below. A supply of suspension water is poured into a container 5, which through a. pump 6 and a flow feeder 7 are connected to the granulating apparatus 4. The latter is provided with a tangential outlet 8, which through a pipeline 9 is connected to a distillation apparatus 10 of the kind commonly used in the process for producing globular gunpowder.

En fOrbiledning 11 stracker sig fran pumpens 6 trycksida till behallaren 5. Forbiledningen Ar forsedd med en ventil 12. Ledningen mellan pumpen 6 och strtimningsmataren 7 Ar forsedd med en ventil 13, och de namnda ventilerna 12 och 13 kunna regleras automatiskt av stromningsmataren 7 f Or att sakerstalla en konstant strOm av suspenderingsvatska, som avlamnas till kornbildningsapparaten 4 och for att mojliggora reglering av denna f Or uppratthallande av ett fixerat forhallande mellan suspenderingsvatska och krutmateriallosning, som avlamnas till kornbildningsapparaten 4. Behallaren 1 Ar fOretradesvis ett slutet kArl, som halles under konstant tryck genom inftirande av indifferent gas, vilken infores volym few volym, i avsikt att ersatta losningen som avlagsnas darifran och for att medverka till pumpens matning. Atgarder kunna vidtagas for att kontinuerligt infora losning i behallaren 1. I den pa fig. 1 visade formen Ar behallaren 1 dimensionerad for att i en charge rymma den mangd losning, vilken an-Andes vid en destillation av en sats 1 destillationsapparaten 10, men det skall framhallas att produktionen fran ett flertal sadana behallare kan samtidigt tillforas samma destillationsanordning, eller °dish kan produktionen Iran en enda behallare uppdelas pit ett flertal destillationsanordningar. A bypass 11 extends from the pressure side of the pump 6 to the container 5. The bypass is provided with a valve 12. The line between the pump 6 and the flow feeder 7 is provided with a valve 13, and the said valves 12 and 13 can be regulated automatically by the flow feeder 7 f Or to ensure a constant flow of suspension liquid, which is unloaded to the granulating apparatus 4 and to enable regulation of this for maintaining a fixed ratio between suspension liquid and powder material solution, which is unloaded to the granulating apparatus 4. The container 1 is preferably kept as a closed grain. pressure by introducing inert gas, which is introduced volume few volume, in order to replace the solution deposited therefrom and to assist in the supply of the pump. Procedures can be taken to continuously introduce discharge into the container 1. In the form shown in Fig. 1, the container 1 is dimensioned to accommodate in a batch the amount of discharge which is used in a distillation of a batch 1 of the distillation apparatus 10, but it it should be emphasized that the production from a plurality of such containers can be fed to the same distillation apparatus at the same time, or ° dish the production Iran a single container can be divided into a plurality of distillation devices.

Kornbildningsapparaten 4, som visas i detalj pa fig. 2, bestar av ett slutet karl, som Ar dimensionerat for att rymma omkring 2 1, dvs. omkring 1/2 % av hela chargen for destillationsapparaten 10. I mitten av karlets hot-ten Ar anordnad en oppningsplatta 15 med ett flertal oppningar 16. Oppningsplattans undersida Ar innesluten genom ett holje 17, vilket i sin tur Ar forbundet med ledningen 3, vilken leder till losningspumpen 2. Over plat-tan 15 Ar anordnad en rotor med fyra radiellt utskjutande skovlar 18. Skovlarna 18 lopa pa plattans 15 oversida och rotorn drives av en lamplig motor pa karlets utsida medelst en axel 20. Intill och under huset 17 Ar kornbildningsapparaten 4 forsedd med en inIoppsOppning 21, vilken i sin tur Ar forbunden med rOrledningen, som leder till stromningsmataren eller stromningsregulatorn 7. Vid den 4— — owe anden av apparaten 4 fir en tangentiell utloppsoppning 8 anordnad. The grain forming apparatus 4, shown in detail in Fig. 2, consists of a closed vessel, which is dimensioned to accommodate about 2 l, i.e. about 1/2% of the entire charge of the distillation apparatus 10. In the middle of the vessel's hot Ar an arrangement plate 15 is arranged with a plurality of openings 16. The underside of the opening plate Ar is enclosed by a housing 17, which in turn Ar is connected to the line 3, which leads to the discharge pump 2. Above the plate 15 is arranged a rotor with four radially projecting vanes 18. The vanes 18 run on the upper side of the plate 15 and the rotor is driven by a lamp motor on the outside of the vessel by means of a shaft 20. Next to and below the housing 17 is the grain forming apparatus 4 is provided with an inlet opening 21, which in turn is connected to the pipe leading to the flow feeder or flow regulator 7. At the end of the apparatus 4 a tangential outlet opening 8 is provided.

Vid driften av systemet pampas krutmateriallosning genom oppningarna 16 i reglerad mangd samtidigt som suspenderingsvatska inf8res genom oppningen 21 i reglerad mangd och under samtidig rotation av skovlarna 18 med f8rutbestaind hastighet. Stork-ken av oppningarna 16 heron p storleken av de Onskade kornen. For bildning av kern, varav starre delen ligger mellan granserna 0,064 och 0,086 cm i diameter, kunna i5ppningarna exempelvis vara 0,76 ± 0,013 cm i diameter, och f8r bildning av kern, varav sten.- re delen ligger mellan gransema 0,041 och 0,064 cm i diameter, kunna oppningarna ha en diameter av 0,051 ± 0,013 cm. Vid en Oppning av given storlek samordnas skovlarnas 18 rotationshastighet med losningens strOmning genom oppningarna sá att man erhaller kroppar med onskat forhallande mellan diameter och langd, vilket är i huvudsak 1:1. Man inser att olika platter 15, alla med Oppningar med olika diameter, kunna anordnas for alternativ anvandning i kornbildningsapparaten. Det shall framhallas att nar en. platta med stOrre oppningar anvandes, reduceras skovlarnas 18 rotationshastighet, sa att man uppratthaller den lampliga betingelsen, att de forkalibrerade kropparna, som avskilj as vid Oppningarnas 16 mynningar, aro ungefar lika breda som langa. During operation of the system, powder material discharge is pumped through the openings 16 in a controlled amount at the same time as suspension liquid is introduced through the opening 21 in a regulated amount and during simultaneous rotation of the vanes 18 at a predetermined speed. The stork of the openings 16 heron on the size of the desired grains. For the formation of nuclei, of which the larger part is between the boundaries 0.064 and 0.086 cm in diameter, the openings may, for example, be 0.76 ± 0.013 cm in diameter, and for the formation of nuclei, of which the stone part is between the boundaries 0.041 and 0.064 cm in diameter, the openings can have a diameter of 0.051 ± 0.013 cm. At an aperture of a given size, the rotational speed of the vanes 18 is coordinated with the flow of the unloading through the apertures so as to obtain bodies with a desired ratio between diameter and length, which is essentially 1: 1. It will be appreciated that different plates 15, all with apertures of different diameters, may be provided for alternative use in the grain forming apparatus. It should be emphasized that when one. plate with larger apertures is used, the rotational speed of the vanes 18 is reduced, so that the suitable condition is maintained that the precalibrated bodies, which are separated at the mouths of the apertures 16, are approximately as wide as long.

Nfir losningen avgfir genom oppningarna 16 och skares till forkalibrerade kroppar av skovlarna 18, suspenderas de forkalibrerade kropparna omedelbart i suspenderingsvatskan, vilken samtidigt avlamnas till kornbildningsapparaten 4. Skovlarnas 18 rotation astadkommer tillracklig omroring for att halla de forkalibrerade kropparna i suspension, och nfir ytterligare vatska och losning infores i apparaten 4, avledes suspensionen genom det tangentiella utloppet 8 och rorledningen 9 till destillationsapparaten 10, vilken är forsedd med en vanlig omrorare och drives sa att den bibehaller suspensionen av fOrkalibrerade kroppar av krutmateriallosning, som utmatas dit fran apparaten 4. Nar hela chargen har avlamnats till destillationsapparaten 10, astadkommes formningen och det efterfolj an-de hardnandet, som inga. i forfarandet f8r framstfillning av gIobulart krut, i destillationsapparaten. After the discharge is discharged through the openings 16 and cut into pre-calibrated bodies by the vanes 18, the pre-calibrated bodies are immediately suspended in the suspension liquid, which is simultaneously discharged to the granulating apparatus 4. The rotation of the vanes 18 provides sufficient agitation to keep the pre-calibrated bodies in suspension, and solution is introduced into the apparatus 4, the suspension is diverted through the tangential outlet 8 and the pipeline 9 to the distillation apparatus 10, which is equipped with a standard stirrer and operated so that it maintains the suspension of precalibrated bodies of powder material discharge discharged therefrom from the apparatus 4. After being discharged to the distillation apparatus 10, the molding and subsequent hardening are accomplished as none. in the process for the production of gIobular powder, in the distillation apparatus.

Som ett typiskt exempel ph den losning som kan anvandas, kan 61 kg etylacetat mekaniskt blandas med 0,06 kg kalciumkarbonat och 0,23 kg difenyIamin. Blandningen upphettas till 50°C och inforlivas langsamt med 36 kg vattenvat nitrocellulosa (25 kg torr nitrocellulosa). Dessa blandningsoperationer genomfores i vilken som helst lamplig mekanisk blandare, som ar forsedd med anordningar for utvandig upphettning, och fortsattas tills en homogen losning bildas. Under blandnings- operationen hoj es blandningens temperatur lampligen frail 50°C till omkring 60°C. Den bildade losningen har, vid en temperatur av 60°C, en viskositet av ungeffir 9 sekunder, bestamd genom foljande meted: en stang av rostfritt sta.' med 0,8 cm diameter och med en vikt av 60 g, som har en plan ande ocli ett marke runt omkretsen 4 cm fran den plana anden, anbringas pa en kropp av krutmateriallosningen med den plana anden ned5.t, och den tid, som erfordras for att stangen skall sjunka ned till det 4 cm Mgt belagna market, betraktas som losningens viskositet. As a typical example of the solution that can be used, 61 kg of ethyl acetate can be mechanically mixed with 0.06 kg of calcium carbonate and 0.23 kg of diphenylamine. The mixture is heated to 50 ° C and incorporated slowly with 36 kg of aqueous nitrocellulose (25 kg of dry nitrocellulose). These mixing operations are carried out in any suitable mechanical mixer equipped with external heating devices and are continued until a homogeneous solution is formed. During the mixing operation, the temperature of the mixture is suitably raised from 50 ° C to about 60 ° C. The solution formed has, at a temperature of 60 ° C, a viscosity of about 9 seconds, determined by the following method: a stainless steel rod. ' 0.8 cm in diameter and weighing 60 g, having a flat spirit and a mark around the circumference 4 cm from the flat spirit, is applied to a body of the powder material solution with the flat spirit down 5.t, and the time required for the rod to sink to the 4 cm Mgt covered market, is considered as the viscosity of the solution.

Den anvanda nitrocellulosan kan vara av samma slag som den, vilken tidigare anvants vid genomforandet av forfarandet for framstallning av globulart krut, exempelvis en nitrocellulosa med en nitrering av 13,2 % N (eller en blandning med i genomsnitt ungeffir detta varde) och en. egentlig viskositet jamforbar med viskositeten hos den nitrocellulosa, vilken fares i marknaden, sasom 6-10 sekunder. Uppfinningen är icke ph nagot satt begransad till nagon sarskild nitreringsgrad eller flagon sarskild grad av viskositet hos nitrocellulosan, och vissa variationer i proceduren och proportionerna av de olika materialen maste n8dvandigt goras, nar nitrocellulosans kvalitet andras. Nar en andring av nitrocellulosans viskositet uppstar i praktiken eller en andring av losningens vattenhalt uppstar, kan installning pa. den ratta arbetsviskositeten latt astadkommas genom lamplig variation av antingen nitrocellulosahalten eller losningsmedelshalten i krutmateriallosningen. The nitrocellulose used may be of the same kind as that previously used in carrying out the process for producing globular gunpowder, for example a nitrocellulose having a nitration of 13.2% N (or a mixture having an average of about this value) and a. actual viscosity comparable to the viscosity of the nitrocellulose which is marketed, such as 6-10 seconds. The invention is not limited in any way to any particular degree of nitriding or to any particular degree of viscosity of the nitrocellulose, and certain variations in the procedure and proportions of the various materials must be made when the quality of the nitrocellulose is different. When a change in the viscosity of the nitrocellulose occurs in practice or a change in the water content of the solution occurs, installation on. the steering working viscosity is easily achieved by suitable variation of either the nitrocellulose content or the solvent content in the powder material solution.

Suspenderingsvatskan, som skall anvandas i samband med den ovan beskrivna krutmateriallosningen, kan beredas genom losning av 6,3 kg gummi arabicum i 23 kg varmt vatten. Deima losning filtreras i 320 kg vatten vid 60°C och blandas noggrant. 12,3 kg natriumsulfat loses darefter i losningen, men man Mir tillse, att natriumsulfatet icke bildar en kaka pa blandningskarlets botten. Darefter tillsattes 6,8 kg etylacetat till losningen och temperaturen hos denna halles vid 60°C. The suspension liquid to be used in connection with the powder material solution described above can be prepared by dissolving 6.3 kg of gum arabic in 23 kg of hot water. This solution is filtered into 320 kg of water at 60 ° C and mixed thoroughly. 12.3 kg of sodium sulphate are then dissolved in the solution, but care must be taken that the sodium sulphate does not form a cake on the bottom of the mixing vessel. Then 6.8 kg of ethyl acetate were added to the solution and the temperature of this was kept at 60 ° C.

For att rekapitulera genomforandet av forfarandet anbringas de ovannamnda 97,5 kg krutmateriall8sning i behallaren 1 ocli de oyannamnda 366 kg suspenderingsvatska anbringas i behallaren 5. Med skovlarnas 18 rotationshastighet installd pa. det onskade vardet (exempelvis 1000 vary per minut for en fyra skovlars kniv, som samverkar med Oppningar med 0,102 cm diameter, belagna 3,5 cm fran appningsplattans mitt), pumpas suspenderingsvatskan in i apparaten 4 (med en hastighet eller i en mangd av 2,95 kg per minut). Krutmateriallosningen pumpas samtidigt fran behallaren 1 till apparaten 4 (i en mangd av 1,2 kg per minut), dar tradarna ay krutmateriallosning, som utpressas genom oppningarna 16 avskaras till cylindrar (med en langd av 0,102 cm och en diameter av — • — 0,102 cm) och omedelbart suspenderas i suspenderingsltisningen i apparaten 4. Vid fort- gaende drift utmatas suspensionen av avskur- na tradar av kratmateriallosning i suspenderingsmediet av apparaten 4 genom utloppet 8 och ledningen 9 till destillationsapparaten 10. To recapitulate the execution of the process, the above-mentioned 97.5 kg of powder material solution is placed in the container 1 and the above-mentioned 366 kg of suspension liquid are placed in the container 5. With the rotational speed of the vanes 18 set to. the desired value (for example 1000 vary per minute for a four-shovel knife, which cooperates with openings with 0.102 cm diameter, coated 3.5 cm from the center of the opening plate), the suspension liquid is pumped into the apparatus 4 (at a speed or in an amount of 2 , 95 kg per minute). The powder material solution is simultaneously pumped from the container 1 to the apparatus 4 (in an amount of 1.2 kg per minute), where the trades of powder material solution, which are extruded through the openings 16, are cut into cylinders (with a length of 0.102 cm and a diameter of - • - 0.102 cm) and immediately suspended in the slurry defrosting in the apparatus 4. During further operation, the suspension of cut trades of scrub material solution in the slurry medium is discharged from the apparatus 4 through the outlet 8 and the line 9 to the distillation apparatus 10.

Nar suspensionen utmatas fran apparaten 4, bestar den av 0,45 kg forkalibrerade kroppar per kg suspenderingsvatska. Under denna pe- riod Mlles temperaturen hos de olika komponenterna vid eller under 60°C, och innehal- let i destillationsapparaten 10 Mlles under mit ornroring. Nar hela chargen uppnatt destillationsapparaten 10, kommer dess nivà dari att befinna sig vid nivan for den ovre omrorareskoveln, som visas pa ritningen. Temperaturen hos innehallet i destillationsapparaten hojes darefter till 70°C pa en tid av en timme, under vilken tid tiltracklig omraring utfores fOr att halla de farkalibrerade kropparna i suspension. Mr destillationsapparatens innehall uppnar en temperatur av 70°C, ha de ftirkalibrerade kropparna (vilka ursprungligen hade formen av cylindrar) erhallit sfarisk form. Om man, sasom utlares I det amerikanska patentet 2 160 626, onskar framstalla korn med hog tathet °eh ett salt har inforlivats i suspenderingsmediet for uppnaende av detta resultat, Mlles temperaturen i destillationsapparaten vid omkring 70°C i omkring tva timmar i avsikt att avlagsna vattnet, vilket emulgeras i de suspenderade kropparna av krutmateriallosning. Den fas av processen, 1 vilken kropparna bringas att hardna, kan darefter genomforas. Denna omfattar avlagsnande av losningsmedlet fran de suspenderade fOrkalibrerade kropparna och kan iistadkommas antingen genom ytterligare okning av temperaturen hos innehallet i destillationsapparaten till omkring 100°C ph en tid av fyra timmar eller genom reducering av trycket pa innehallet i destillationsapparaten till omkring 0,53 kg/cm2 absolut tryck, medan temperaturen dari Mlles vid 70°C under en tid av sex. timmar. Sedan de suspenderade globulara kropparna bringats att hfirdna, utvinnas de frail destillationsapparaten 10 och avvattnas pa vanligt salt. Produkten, som erMlles genom den ovan beskrivna serien av operationer med den ovan beskrivna losningen av krutmaterial och suspenderingsvatskan bestod av 22,7 kg val awundade korn, av vilkas diametrar Over 80 % voro mom storleksomradet 0,086-0,104 cm, och hade en specifik vikt av 0,95. When the suspension is discharged from the apparatus 4, it consists of 0.45 kg of pre-calibrated bodies per kg of suspension liquid. During this period, the temperature of the various components is measured at or below 60 ° C, and the contents of the distillation apparatus are measured during my stirring. When the whole charge has reached the distillation apparatus 10, its level therein will be at the level of the upper agitator paddle, as shown in the drawing. The temperature of the contents of the distillation apparatus is then raised to 70 ° C over a period of one hour, during which time sufficient agitation is carried out to keep the vessel-calibrated bodies in suspension. The contents of the distillation apparatus reach a temperature of 70 ° C, the pre-calibrated bodies (which were originally in the form of cylinders) having a spherical shape. If, as stated in U.S. Pat. No. 2,160,626, it is desired to produce high density grains or a salt has been incorporated into the suspending medium to achieve this result, the temperature in the distillation apparatus at about 70 ° C for about two hours is intended to be removed. the water, which is emulsified in the suspended bodies by powder material release. The phase of the process in which the bodies are hardened can then be carried out. This involves removing the solvent from the suspended precalibrated bodies and can be achieved either by further raising the temperature of the contents of the distillation apparatus to about 100 ° C for a period of four hours or by reducing the pressure of the contents of the distillation apparatus to about 0.53 kg / cm2 absolute pressure, while the temperature dari Mlles at 70 ° C for a period of six. hours. After the suspended globular bodies have been allowed to dry, they are recovered from the distillation apparatus 10 and dewatered on ordinary salt. The product obtained by the above-described series of operations with the above-described solution of gunpowder material and the suspension liquid consisted of 22.7 kg of selected undiluted grains, whose diameters over 80% were in the range of 0.086-0.104 cm, and had a specific gravity of 0.95.

Medan vid det vanliga tillvagagangssattet for genomforande av forfarandet for framstallning av globulart krut (dar krutmateriallosningen beredes i franvaro av suspenderingsvatskan) under inforandet av krutmateriallasningen 1 vatskan forhallandet mellan krutmateriallosning och suspenderingsvatska successivt akar fran noll till ett slutligt varde av exempelvis 1:2, vilket slutliga varde upp nas Horst vid slutet av inforandet, Mlles .enligt fOreliggande uppfinning farhallandet lan krutmaterialltisning och suspenderingsvatska i huvudsak konstant under kalibrerings- och de ursprungliga suspenderingsoperationerna samt chargeringen av destillationsapparaten 10. Sedan all krutmateriallosning uppdelats och suspensionen av denim anbringats i destillationsapparaten 10, kan naturligtvis ytterligare suspenderingsmedium inforas i destillationsapparaten, men med hansyn till det forhallandet, att det ytterligare suspenderingsmediet sattes till en redan existerande suspension av losningskroppar, exponeras alla de suspenderade losningskropparna samtidigt, och de exponeras fOljaktligen under samma tidrymd for den &kande mangden suspenderingsvatska (i motsats till vad som an fallet om krutmateriallosningen sattes till suspenderingsmediet). While in the usual procedure for carrying out the process for producing globular gunpowder (where the powder material solution is prepared in the absence of the suspension liquid) during the introduction of the powder material solution into the liquid, the ratio between powder material solution and suspension liquid successively ranges from, for example, Horst was present at the end of the introduction. According to the present invention, the propulsion of gunpowder thawing and slurry liquids is substantially constant during the calibration and initial slurry operations and the charging of the distillation apparatus 10. After all the powdered material solution has been split and the denim apparatus suspended, additional suspension medium is introduced into the distillation apparatus, but in view of the fact that the additional suspension medium was added to an already existing suspension of discharge bodies, expone all the suspended discharges are discharged simultaneously, and they are consequently exposed for the same amount of time to the increasing amount of suspension liquid (as opposed to the case where the powder material discharge was added to the suspension medium).

Av ovanstaende beskrivning framgar, att uppfinningen uppnar de avsedda andamalen och astadkommer ej endast ett forfarande, enligt vilket tillsatser inforlivade i krutrimteriallosning med sakerhet i den onskade proportionen Overfares till de slutliga avrundade globulara kropparna, utan att en sadan globular kropp forlorat mera sadan tillsats an en annan, men. genom att uppdelningen och den ursprungliga suspenderingen utfores vid en temperatur, vid vilken krutmateriallosningen dr »stelnad», kan den bildade suspensionen transporteras genom rorledningar ldnga stycken eller hfillas i forvaring, forutsatt att temperaturen ej tillates overstiga den, vid vilken de suspenderade krutmaterialkropparna bli klibbiga. Pastan forfarandet for framstallning av globulart krut avgjort an ett diskontinuerligt forfarande vad behalf ar kropparnas avrundning och deras bringande att hardna, kati foljaktligen kornbildningsoperationen vara kontinuerlig under matning av ett flertal destillationsapparater, i vilka avrundningen och hardnandet astadkommes. From the above description it appears that the invention achieves the intended purposes and not only provides a process according to which additives incorporated in powder material solution with certainty in the desired proportion are transferred to the final rounded globular bodies, without such a globular body losing more such additive to a another, but. by carrying out the division and the initial suspension at a temperature at which the powder material solution is "solidified", the resulting suspension can be transported by pipelines into long pieces or filled into storage, provided that the temperature is not allowed to exceed that at which the suspended powder material bodies become tacky. The paste process for the production of globular powder is decidedly a discontinuous process in terms of rounding the bodies and causing them to harden, and consequently the granulation operation is continuous while feeding a plurality of distillation apparatus in which the rounding and hardening are effected.

I ovanstaende beskrivning har uppfinningen allmant beskrivits i anslutning till ett speciellt exempel, men det skall framhallas, att uppfinningen icke àr begransad till de speciella material, proportioner, temperaturer eller andra betingelser, som angivits ovan i avsikt att belysa uppfinningen. Tvartom inser en fackman, aft det finnes manga variabler i forfarandet for framstallning av globulart krut, och att dessa variabler aro lika tillampbara ph foreliggande forbattring av detta fOrfarande. Medan den foreliggande forbattringen är sarskilt tillampbar pa utf8ringsformer av forfarandet far framstallning av globulart krut, i vilka krutmateriallosningen beredes i franvaro av suspenderingsmediet, aro vissa kannetecken for uppfinningen, exempelvis de uppdelade kropparnas bringande att stelna, tillampbara pa utfOringsformer av forfarandet fOr framstallning av globulart krut, vid 6— — vilka ltisningen beredes 1 narvaro av nagot suspenderingsmedium. Det skall darfor framhallas, att den ovanstilende beskrivningen endast är belysande och att modifikationer och variationer kunna goras utan att man gar utanfor ramen fOr uppfinningen. In the above description, the invention has been generally described in connection with a particular example, but it should be emphasized that the invention is not limited to the particular materials, proportions, temperatures or other conditions set forth above for the purpose of illustrating the invention. On the contrary, one skilled in the art will recognize that there are many variables in the process for producing globular gunpowder, and that these variables are equally applicable to the present improvement of this process. While the present improvement is particularly applicable to embodiments of the process for producing globular gunpowder, in which the powder material solution is prepared in the absence of the suspending medium, certain features of the invention, such as the splitting of the divided bodies, are applicable to embodiments of the process. , at 6— - which ltisningen is prepared in the presence of some suspending medium. It should therefore be emphasized that the above description is merely illustrative and that modifications and variations may be made without departing from the scope of the invention.

Claims

Patent claim:

A process for producing globular powder granules having a substantially uniform composition comprising dissolving a smokeless powder material in a solvent therefor to form a pulp, squeezing the pulp through an opening into a stream of a suspension liquid which is substantially immiscible. with the release agent, and cutting off equal bodies from the extruded mass when it leaves the opening, whereby the pulp bodies are suspended in the liquid, cannetecluiat thereof, both the suspension liquid and the pulp are brought to the strands in a regulated amount, so that the ratio between suspension liquid and pulp is kept substantially constant during the process and that the suspension liquid with the pulp bodies suspended therein is led to a distillation apparatus equipped with a stirrer and that the suspended pulp bodies are then rounded and hardened. per se edge salt in the distillation apparatus.

2. A method according to claim 1, can be characterized in that the pulp contains water before the extrusion and that the suspension liquid comprises water.

3. A method according to claim 1, characterized in that an insoluble additive is distributed in the pulp before its extraction.

4. A method according to claim 3, characterized in that the additive is water and that the suspension liquid consists of water containing a solid substance, which is insoluble in both the mass and the suspension liquid.

5. A method according to claim 1 or 2, characterized in that the suspension is derived continuously from the stalk where the pulp is divided, and that the ratio between pulp and suspension liquid next to said stable is substantially the same as the ratio between pulp and suspension liquid in the finished suspension .

6. A method according to any one of the preceding patent claims, characterized in that the suspension is kept at a temperature below that at which the pulp bodies are tacky after the suspension and before rounding. Cited publications: Patentskrifter 'ran Sverige 145919; France 1,050,238; USA 2 027 114.