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United States Patent (19) 11) 4,039,640 Leneve: 45) Aug United States Patent (19) 11) 4,039,640 Leneve: 45) Aug. 2, 1977 54 MOLDABLE COMPOSITIONS 3,673,286 6/1972 Remaly et al. .................. 264/3 B X COMPRISING POLY WINYL NITRATE 3,779,820 12/1973 Stevely et al. ............ 102/DIG. X 75 Inventor: Louis J. Leneveu, Pont de Buis, OTHER PUBLICATIONS France Akiyama et al., Chem. Abst., 72, Abst. No. 3982u. 73 Assignee: Societe Nationale des Poudres et (1970). Explosifs, France Primary Examiner-Peter A. Nelson 21) Appl. No.: 711,717 Attorney, Agent, or Firm-Bucknam and Archer 22 Filed: Aug. 5, 1976 57 ABSTRACT Related U.S. Application Data A mouldable thermoplastic composition comprises (i) polyvinyl nitrate, (ii) nitrocellulose and/or polyvinyl 62) Division of Ser. No. 491,619, July 24, 1974, abandoned. acetate and (iii) 2-nitro-diphenylamine and may be used 30 Foreign Application Priority Data to form combustible articles such as cartridge cases. Preferably, the composition comprises from 30 to 90% Aug. 9, 1973 France ................................ 73.291.86 by weight of polyvinyl nitrate based on the total weight Dec. 4, 1973 France ................................ 73.43246 of components (i) and (ii). The composition may com 5ll Int. Cl’.............................................. CO6B 21/OO prise up to about 30% by weight, based on the weight of 52 U.S.C. ................................... 264/3 B; 264/3 E; components (i) and (ii), of at least one additive selected 149/92; 149/100 from cellulose acetate, dinitrotoluene, phthalates, non 58) Field of Search .............. 264/3 R, 3 B, 3 D, 3 E; volatile esters, heterocyclic ketones, ureas and ABS 149/19.7, 19.8, 19.9, 19.91, 88,92, 100; copolymers. 102/DIG. 1 The combustible articles may be formed by compres (56) References Cited sion moulding or injection moulding. Preferably the mouldable composition is formed into granules using U.S. PATENT DOCUMENTS the “with solvent' technique for making single base 3,078,200 2/1963 Preckel .................................. 149/96 propellants, and the granules are mixed with a porous 3,422,170 1/1969 Brooks et al. ....................... 264/3 R powder comprising nitrocellulose prior to being 3,428,502 2/1969 Evans .............................. 264/3 RX moulded to form the combustible article. 3,447,983 6/1969 Camp et al...................... 264/3 RX 3,563,977 2/1971 Cucinotta ........................ 264/3 DX 3,669,924 6/1972 Daume et al. ................ 149/19.91 X 7 Claims, No Drawings 4,039,640 2 (for example, kraft), the potential of which is increased MOLDABLE COMPOSITIONS COMPRISING by adding crystalline explosives such as pentaerythritol POELYWNYL NTRATE tetranitrate, hexogen and octogen. However, the use of This is a division of applicaton Ser. No. 491,619, filed such explosives makes the preparation of the cartridge a July 24, 1974. Ser. No. 491,619 has now been abandoned delicate and long procedure because the entire manu in favor of a continuation applicaton Ser. No. 716,271 facturing process is carried out in aqueous media and filed Aug. 20, 1976. requies prolonged drying at the end of the manufactur The present invention relates to mouldable composi ing process. Another technique, described in French tions comprising polyvinyl nitrate. The compositions Pat. No. 2,103,794, comprises compressing a synthetic may be employed in the manufacture of combustible 10 foam made of polyvinyl actal, polyurethane or polysty articles, such as cartridge cases, mortar shell ends or rene, but this technique is restricted to the particular detonator tubes which have a very high potential and materials just mentioned because it is restricted to the thus contribute energy for propelling a self-propelled use of foams, and thus cannot employ a vinyl compound projectile of which the combustible article forms a part. which is highly energizing but cannot readily be made The thermoplastic properties of polyvinyl nitrate and 15 in the form of a foam, such as polyvinyl nitrate. its value in manufacturing moulded articles have been We have now developed certain mouldable composi described in French Pat. No. 911,759, but the energiz tions which are highly energising and which may be ing properties of these articles were not discussed in this used to form wholly combustible articles which, during patent and the patent does not contain any indication as combustion of the article, generate a substantial amount to the nature of the mouldable composition to be used 20 of energy which can be used to assist the propulsion of for a particular application. a projectile with which the article is associated. The desirability of combustible articles in the fields of According to the invention, there is provided a self-propulsion and artillery has long been apparent. In mouldable thermoplastic composition which comprises the field of self-propulsion, for example, the metal fins (i) polyvinyl nitrate, (ii)nitrocellulose and/or polyvinyl or certain metal parts of the stabiliser assembly add to 25 actate, and (iii) 2-nitro-diphenylamine. the weight of the article for the entire duration of the The invention also comprises a method of making a flight, although they are useful only at the start of the combustible article from a composition according to the trajectory, and require an increase in the powder charge invention, which comprises forming granules of a in order to effect their propulsion. In the field of artil mouldable thermoplastic composition which comprises lery, it has been found that the accumulation of empty 30 (i) polyvinyl nitrate, (ii) at least one material selected cartridge cases in a tank poses problems, both because from the group consisting of nitrocellulose and polyvi the empty cases clutter up the space in the tank, and nyl acetate, and (iii) 2-nitro-diphenylamine, using the because the cartridge cases also contain gases produced "with solvent' technique for making single base propel by the combustion of the powder, which pose toxicity lants, and moulding the granules so formed to produce problems for the occupants of the tank. These problems 35 the combustible article. are far from negligible, because a lowering in the effi The use of polyvinyl nitrate is advantageous in that, in ciency of military personnel in a tank in which a large contrast to nitrocellulose, polyvinyl nitrate softens quantity of empty cartridge cases has accumulated, has when hot, and since the decomposition temperature is been observed. markedly higher than the temperature at which soften It is known to make combustible articles, especially 40 ing starts, the product is easy to work with using injec combustible cartridge cases, by replacing a part only of tion moulding techniques. the metal casing by a combustible composition. Thus Since polyvinyl nitrate possesses poor mechanical French Pat. No. 1,349,818 describes cartridge cases strength, it is not used alone, but in admixture with made in two parts, namely a component made from a nitrocellulose and/or polyvinyl acetate, the proportion combustible material, namely nitrated cellulose, and a 45 by weight of polyvinyl nitrate preferably being from 30 metal base. A serious problem with this arrangement is to 90%. When more than 90% of polyvinyl nitrate is the difficulty of obtaining reliable joining of the metal used, the product possesses inadequate mechanical and the nitrocellulose, and, of course, such cartridge strength for some purposes and does not sufficiently cases are only partly combustible since they still contain retain its shape after moulding, whilst if less than 30% a metal component. French Pat. No. 1,573,822 describes 50 of polyvinyl nitrate is used, either the difference be consumable rocket fins which are destroyed during the tween the decomposition temperature and the softening flight of the machine, but these fins, which are made of temperature becomes too small (when nitrocellulose is a fusible metal, of a solid propulsion material which is present), or the heat of combustion decreases too much not described in the patent, or of an inert plastics mate (when polyvinyl acetate is present). rial, do not, on being consumed, contribute energy to 55 When nitrocellulose is used, a nitrocellulose with a propel the rocket. low nitrogen content is preferably employed. The An attempt has been made to manufacture combusti greater the nitrogen content of the nitrocellulose, the ble cartridge case bases made of a readily combustible smaller the difference between the temperature at Synthetic material. Such a proposal is described in which softening starts and the decomposition tempera French Pat. No. 1,499,078, but no mention is made in 60 ture. this patent of the use of a high energy thermoplastic The mechanical properties of polyvinyl nitrate are material, such polyvinyl nitrate. such that it is not desirable to manufacture the combus Attempts have also been made to use materials with a tible article from polyvinyl nitrate directly, but, rather, high energy of combustion so that the combustion of it is much preferred to proceed in two stages. In a first the article would provide energy which could be used 65 stage, small granules of the mouldable composition of for assisting propulsion of the projectile. One technique, the invention are manufactured and we have found, described in French Pat. No. 2,003,848, comprises us surprisingly, that it is possible to manufacture these ing, as the combustible material, a fibrous cellulosic base granules using the well-known “with solvent' tech 4,039,640 3. 4. nique for preparing single-base powders, the so-called
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