RU2280635C2 - Method of production of the spherical powder for the 9 mm cartridge - Google Patents

Abstract

FIELD: chemical industry; methods of production of the spherical powders for the cartridges to the small arms.

SUBSTANCE: the invention is pertaining to the field of chemical industry and presents the method of production of the spherical powder for the 9 mm cartridges to the small arms providing for stirring in the water of the components of the powder - nitrocellulose, the stabilizing agents, nitroglycerine, preparation of the powdery varnish in ethyl-acetate, the dispersion of the powdery varnish with simultaneous introduction of the emulsifiers and the SAS, then - introduction of the salt of Na₂SO₄ for dehydration, removal of ethyl-acetate, washdown, the grading and drying of the powder components. At the stirring of the components they additionally introduce the technical carbon. The powder varnish is dispersed at the mixer rotational speed of 190 minute^-1. As the nitrocellulose use the high- nitrogen pyroxylin with conditional viscosity of 5-12°Э, and as the SAS use dinitrogen salt of the diethyl ether N-γ- decyloxipropyl-N-(β-carboxy-β-propyl-sulfopropionel) aspartic acid. The invention allows to produce the fine, dense, finely combined spherical powder.

EFFECT: the invention ensures production of the fine, dense, finely combined spherical powder.

1 tbl, 10 ex

Description

The invention relates to the production of spherical powders for cartridges for small arms.

Known methods for producing fine summary powders for cartridges for sports and hunting weapons: pyroxylin powder "Falcon" (GOST 22781-77) Gindich V.I. Technology of pyroxylin powders. - t.2, Kazan, 1995, p. 319 and nitroglycerin powder (RF patent 2192405, application 2000124044 from 09/19/2000, IPC 7 C 06 V 24/25). The manufacture of these powders is carried out according to the existing hydropress technology.

The disadvantages of these methods is that, firstly, the resulting powder due to the low bulk density (0.500 kg / dm ³ ) and their poor flowability associated with the shape of the powder elements (plate) are not high-tech when assembling cartridges on automatic rotor lines ( ARL); secondly, the equipment used in the technological process (rollers, cutting machines) is metal-intensive and energy-intensive, and, in addition, rolling is a fire hazardous operation.

Known methods for producing spherical powder by emulsion technology (US patent 3917767, C 06 V 21/00 from 04.11.1975, RF patent 1727375, application 4804112 from 19.03.90, MKI 5 C 06 V 21/00; RF patent 2201912, application 2001107710 dated 03.22.2001, IPC 7 C 06 B 21/00, 25/18), the main stages of which (up to 90%) occur in the aquatic environment using simple capacitive equipment with mixers, which increases the level of production safety.

These technical solutions describe methods for producing gunpowders, which contain the following main stages of the process:

- mixing of the components in 2.5-20.0 volume parts of water per one part of the components;

- preparation of powder varnish or limited swelling of the elements of the powder in the case of using obsolete powders as raw materials with an expired warranty period of storage in 1.9-5.0 volume parts of ethyl acetate per one part of the components;

- dispersion of powder varnish in the presence of 0.4-2.0 wt.% emulsifier to water;

- dehydration of the obtained elements by entering 0-1.2 wt.% to water salt Na ₂ SO ₄ ;

- removal of ethyl acetate by distillation at a temperature of up to 92-94 ° C in the reactor.

Gunpowder obtained by these methods are also characterized by low bulk density (0.400-0.600 kg / DM ³ ). In addition, the powder elements are large (diameter up to 2 mm) and have a shape from spherical to ellipsoidal.

Spherical gunpowder with such characteristics does not provide ballistic requirements for 9 mm pistol cartridges.

The closest way to the proposed technical solution is an emulsion method for producing a dibasic spherical powder, which can be used in weapons with a low maximum pressure, according to the patent US 3917767 A, 04.11.1975, IPC 7 C 06 V 21/00, MKI C 06 tv 21 / 00 - prototype. The method includes:

- mixing in 10-20 vol. parts of water nitrocellulose, stabilizers 5-20 wt.% nitroglycerin and dinitroglycol;

- preparation of powder varnish with 2.5-5.0 vol. parts of ethyl acetate (EA) at a stirrer speed of 80 min ^-1 ;

- dispersing the varnish into particles by adding 0.2 wt.% emulsifier to water and 1.3 wt.% to water, Na ₂ SO ₄ salt, while reducing the stirrer speed to 54 min ^-1 ;

- stop mixing for 60 minutes with the formation of varnish;

- dispersion of varnish into particles with the introduction of 0.2 wt.% emulsifier to water;

- dehydration of particles with the introduction of 0.6-1.2 wt.% salt of Na ₂ SO ₄ to water at a stirring speed of 54 min ^-1 ;

- removal of EA by distillation at temperatures up to 99 ° C;

- washing, sorting and drying the obtained powder elements.

The powder elements obtained by this method are large, have a spherical shape and are characterized by a low bulk density of 0.400-0.600 g / cm ³ due to the large volume of water used and the presence of adhesion of varnish particles in the presence of Na ₂ SO ₄ salt, performing at this stage of the process the role of the blowing agent. In a large volume of water, the varnish particles do not experience the resistance of the aqueous medium with stirring and they acquire a spherical shape, which does not undergo changes during the removal of ethyl acetate. The use of highly porous powder with a high concentration of nitroglycerin obtained by this method, for example, in a 9 mm pistol cartridge, leads to a sharp increase in the average maximum pressure even with a small charge mass.

The objective of the invention is to obtain emulsion technology of fine, dense, fine spherical powder.

To achieve the technical result in the proposed method, which includes mixing in water components of the powder - nitrocellulose, stabilizers, nitroglycerin, preparing powder varnish in ethyl acetate, dispersing the powder varnish with the simultaneous introduction of emulsifiers, then Na ₂ SO ₄ salt for dehydration, removing ethyl acetate, washing, sorting and drying of powder elements, additionally, while mixing the components, 0.1-0.2 wt.% technical carbon is introduced, the components are mixed in 2.5-3.5 volume parts x water for one part of the components, the preparation of powder varnish is carried out in 1.7-4.0 volume parts of EA for one part of the components, the powder varnish is dispersed with 0.8-5.0 wt.% of emulsifiers added to water at a stirrer speed of 190 min ^-1 , while simultaneously with the introduction of emulsifiers, 0.1-0.2% surfactant is additionally added to wt.% to water, Na ₂ SO ₄ salt is administered in an amount of 0.5-2.5 wt.% to water, As nitrocellulose, high-nitrogen pyroxylin with a nominal viscosity of 5-12 ° O is used, and N-γ-decyloxypropyl-N- (β-carb) disodium salt of diethyl ether is used. xi-β-sulfopropionel) aspartic acid.

Reducing the size of the powder elements and the thickness of the burning arch is achieved by using pyroxylin with a nominal viscosity of 5-12 ° O, which provides the elements with a minimum mass after removal of ethyl acetate; using technical carbon as an additional dispersant along with an emulsifier; using a highly effective surfactant that facilitates the dispersion process by reducing interfacial tension; a decrease in the volume of water and an increase in the frequency of rotation of the stirrer to 190 min ^-1 , leading to an increase in the friction forces from the side of the water and the forces of hydrodynamic effects between themselves. As a result, the resulting small varnish particles undergo deformation and flatten, acquiring a shape close to the disk.

Input salt Na ₂ SO ₄ in the indicated concentrations provides a given density of the powder.

The proposed method can be implemented in the production of regular spherical powders on existing equipment, while the productivity of the formation phase increases due to the possibility of increasing the reactor load by 3.5 times as a result of reducing the dosage of water from 10-20 volume parts to 2.5-3, 5 parts by the proposed method.

The practical feasibility and technical result achieved are confirmed by examples of the specific production of gunpowder and the results of their physicochemical and ballistic tests as part of a 9 mm high-power pistol cartridge (see table).

Table
The characteristics of the process and gunpowder manufactured by the developed and known methods. Name of indicator Indicator value pr.1 pr.2 pr 3 pr.4 pr 5 pr.6 pr 7 pr 8 pr.9 Project 10 Prototype 1. The viscosity of high-nitrogen pyroxylin, ° E 5 8.5 12 2.0 1,5 8.5 8.5 8.5 8.5 8.5 - 2. Technical carbon, wt.% 0.1 0.15 0.2 0.15 0.15 0.15 0.15 - 0.15 0.15 - 3. The amount of water, volumetric part 2,5 3.0 3,5 3.0 3,5 4,50 3.0 3.0 3.0 3.0 10-20 4. The amount of ethyl acetate, vol. part 1.7 2.85 4.0 2.85 4.0 4.0 2.85 2.85 2.85 4,5 2.5-5.0 5. The concentration of the emulsifier wt.% To water 0.8 2.9 5,0 2.9 2.9 2.9 2.9 2.9 2.9 2.25 0.4 6. The concentration of surfactants, wt.% To water 0.1 0.15 0.2 0.15 0.15 0.15 0.15 - 0.15 0.15 - 7. The concentration of Na ₂ SO ₄ to water for dehydration, wt.% To water 0.5 1,5 2,5 1,5 1,5 1,5 0.2 1,5 1,5 1,5 0.6-1.2 8. The frequency of rotation of the mixer, min ^-1 190 190 190 190 190 190 190 190 150 190 50-90 9. Geometric dimensions, average: the thickness of the burning arch, 0.20 0.13 0.05 0.40 Besf.eleme 0.35 0.18 0.27 0.22 0.25 Krupn diameter mm 0.40 0.36 0.28 0.55 nt. 0.50 0.39 0.43 0.48 0.35 sph.el. 10. Bulk density, g / cm ³ 0,900 1,0 1,1 0.95 - 0.960 0.810 0.980 0,990 0.970 0.400- 0,600 11. Ballistic characteristics of a 9 mm pistol cartridge - mass of charge, g 0.46 0.42 0.40 0.52 - 0.49 0.38 0.48 0.47 0.36 0.32 - average bullet flight speed, m / s 476 479 485 462 - 450 437 460 457 449 410 - the maximum average pressure of the powder gases kgf / cm ² 1365 1380 1410 1310 - 1260 1610 1270 1320 1540 1950 Note: Requirements for 9 mm cartridge; charge mass not more than 0.48 g; the average speed of the bullet 470-490 m / s, the average maximum pressure of 1450 kgf / cm ² .

Example 1

2.5 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 5 ° O, stability stabilizer, nitroglycerin and 0.1% technical carbon are charged. Stirring is carried out and 1.7 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with 0.8 wt.% Water added to the emulsifier water and surfactant added in an amount of 0.1 wt.% Water, at a stirrer speed of 190 ^-1 min and then the Na ₂ SO ₄ salt is introduced into the dehydration the amount of 0.5 wt.% to water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 2

3.0 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 8.5 ° O, stability stabilizer, nitroglycerin and 0.15% technical carbon are charged. Stirring is carried out and 2.85 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with the addition of 2.9 wt.% To the emulsifier water and the introduction of a surfactant in the amount of 0.15 wt.% To water at a stirrer speed of 190 ^-1 min and then Na ₂ SO ₄ salt is introduced into the dehydration in the amount 1.5 wt.% To water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 3

3.5 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 12.0 ° O, stability stabilizer, nitroglycerin and 0.2% technical carbon are charged. Stirring is carried out and 4.0 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with the introduction of 5.0 wt.% To the emulsifier water and the introduction of a surfactant in an amount of 0.2 wt.% To water at a stirrer speed of 190 ^-1 min and then Na ₂ SO ₄ salt is introduced into the dehydration in the amount 2.5 wt.% To water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 4

3.0 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 2.0 ° O, stability stabilizer, nitroglycerin and 0.15% technical carbon are charged. Stirring is carried out and 2.85 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with the addition of 2.9 wt.% To the emulsifier water and the introduction of a surfactant in the amount of 0.15 wt.% To water at a stirrer speed of 190 ^-1 min and then Na ₂ SO ₄ salt is introduced into the dehydration in the amount 1.5 wt.% To water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 5

3.5 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 15.0 ° O, stability stabilizer, nitroglycerin and 0.15% technical carbon are charged. Stirring is carried out and 4.0 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with the addition of 2.9 wt.% To the emulsifier water and the introduction of a surfactant in the amount of 0.15 wt.% To the water of the components at a stirrer speed of 190 ^-1 min and then the Na ₂ SO ₄ salt is introduced into the dehydration the amount of 1.5 wt.% to water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 6

4.0 volumetric parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 8.5 ° O, stability stabilizer, nitroglycerin and 0.15% technical carbon are charged. Stirring is carried out and 4.0 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with the addition of 2.9 wt.% To the emulsifier water and the introduction of a surfactant in the amount of 0.15 wt.% To water at a stirrer speed of 190 ^-1 min and then Na ₂ SO ₄ salt is introduced into the dehydration in the amount 1.5 wt.% To water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 7

3.0 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 8.5 ° O, stability stabilizer, nitroglycerin and 0.15% technical carbon are charged. Stirring is carried out and 2.85 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with the addition of 2.9 wt.% To the emulsifier water and the introduction of a surfactant in the amount of 0.15 wt.% To water at a stirrer speed of 190 ^-1 min and then Na ₂ SO ₄ salt is introduced into the dehydration in the amount 0.2 wt.% To water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 8

3.0 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 8.5 ° O, stability stabilizer, nitroglycerin and 0.15% technical carbon are charged. Stirring is carried out and 2.85 volume parts of ethyl acetate are introduced. After the preparation of the powder varnish, dispersion is carried out with the addition of 2.9 wt.% Emulsifier water to the agitator at a stirrer speed of 190 ^-1 min and then the Na ₂ SO ₄ salt is introduced into the dehydration in an amount of 1.5 wt.% To water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 9

3.0 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 8.5 ° O, stability stabilizer, nitroglycerin and 0.15% technical carbon are charged. Stirring is carried out and 2.85 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with the addition of 2.9 wt.% To the emulsifier water and the introduction of a surfactant in the amount of 0.15 wt.% To water at a stirrer speed of 190 ^-1 min and then Na ₂ SO ₄ salt is introduced into the dehydration in the amount 1.5 wt.% To water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

Example 10

3.0 volume parts of water are poured into the reactor, the mixer is turned on, and pyroxylin with a viscosity of 8.5 ° O, stability stabilizer, nitroglycerin and 0.15% technical carbon are charged. Stirring is carried out and 4.5 volume parts of ethyl acetate are introduced. After preparation of the powder varnish, dispersion is carried out with the introduction of 2.25 wt.% Water emulsifier and the introduction of surfactants in the amount of 0.15 wt.% Water, with a stirrer speed of 190 ^-1 min and then Na ₂ SO ₄ salt is introduced into the dehydration in the amount 1.5 wt.% To water. Next, ethyl acetate is removed from the powder elements, washed, sorted and the powder dried.

In experiments 1-3, the technical result is achieved: the method developed by the authors ensures the production of fine powder by emulsion technology with a bulk density of up to 1,100 kg / dm ³ , a burning arch thickness of 0.05-0.20 mm, and a diameter of 0.28-0.40 mm fulfilling ballistic requirements for a 9 mm pistol cartridge of increased power in terms of bullet speed and average maximum pressure for a given charge mass.

A decrease in the nominal viscosity of pyroxylin below the lower limit (D.4), the exclusion of surfactants (D.8), a decrease in the speed of the stirrer (D.9) and an increase in water above the upper limit (D.6) result in powder elements with a large burning thickness arch, as a result of the powder does not provide requirements for the magnitude of the charge mass to 9 mm pistol cartridge.

Gunpowder varnish obtained using pyroxylin with a viscosity higher than the upper limit (pr 5) becomes non-technological due to its high viscosity and heterogeneity. When dispersing varnish with such properties, shapeless powder elements are obtained.

When implementing a process with a reduced salt concentration of Na ₂ SO ₄ below the lower limit (pr. 7), the powder turns out to be low in density and becomes unsuitable for a 9 mm pistol cartridge due to the high maximum average pressure, which develops the powder even at a low charge mass.

With an increase in the volumetric part of EA over 4.0, the powder elements are obtained closer in shape to spherical, which leads to a decrease in the mass of the charge and an increase in the average maximum pressure (Project 10).

The decrease in the volume of water less than 2.5 complicates the process of mixing the components and leads to a heterogeneous powder varnish.

Carrying out a process with an increased concentration of technical carbon above the upper limit is impractical from an economic point of view.

Claims (1)

A method for producing spherical gunpowder for a 9 mm cartridge, including mixing in water components of gunpowder - nitrocellulose, stabilizers, nitroglycerin, preparing powder varnish in ethyl acetate, dispersing the powder varnish with the introduction of emulsifiers, then Na ₂ SO ₄ salt for dehydration, removing ethyl acetate, washing, sorting and drying the powder elements, characterized in that when mixing the components an additional 0.1-0.2 wt.% technical carbon is added, the components are mixed in 2.5-3.5 vol.h. water for one part of the components, the preparation of powder varnish lead in 1.7-4.0 vol.h. ethyl acetate on one part of the components, disperse the powder varnish with the introduction of 0.8-5.0 wt.% emulsifiers to water with a stirrer speed of 190 min ^-1 , while simultaneously with the introduction of emulsifiers an additional 0.1-0.2 wt. % to water surfactant, Na ₂ SO ₄ salt is introduced in an amount of 0.5-2.5 wt.% to water, high nitrogen pyroxylin with a nominal viscosity of 5-12 ° O is used as nitrocellulose, and disodium salt of diethyl ether is used as surfactant N-γ-decyloxypropyl-N- (β-carboxy-β-sulfopropionel) aspartic acid.