Method of recovering oxide of a metal component from mixed explosive

FIELD: explosives.

SUBSTANCE: invention concerns physicochemical analysis and can be used in production of explosives to determine content of metal component. Proposed method of recovering oxide of a metal component from mixed explosives belonging to nitramine class comprises converting mixed explosive into nonexplosive form by decomposing it through treatment with alkali reagent followed by oxidation of metal component to metal oxide by heat treatment of resulting material in air at 800-1100°C for 2-4 h.

EFFECT: increased degree of recovery of metal components.

3 cl

 

The invention relates to physico-chemical analysis and can be used for analysis in the production of mixed explosives (e), in particular, to determine the content of the metal component in the composite EXPLOSIVES used in electric detonators and explosive devices.

There is a method of determining the content of total zirconium (TU-4-376-76. Powder of zirconium nitrilimines). The method is based on determining the change in mass in the combustion of zirconium to zirconium dioxide.

The addition of zirconium, weighted with an accuracy of 0.0002 g, placed in pre-annealed and weighed crucible. The crucible with the sample Zirconia calcined at a temperature of 800-850°C for one hour, resulting in the oxidation of zirconium to zirconium dioxide. After that, the crucible is transferred to a desiccator, cooled and weighed.

The zirconium content (X1) in percent is determined by the formula:

where m2- weight of crucible with residue on ignition, g;

m1- the mass of the crucible, g;

m is the mass of powder of zirconium, g;

0.7403 - multiplier Zirconia in the Zirconia.

This method allows high accuracy to determine the content of total zirconium, however, cannot be applied in the analysis of mixtures of EXPLOSIVES with a metal component, as is the agrevanie explosive mixtures may occur flash and release of explosives, contained in explosive mixtures. The emission of explosives may result in the emission of particles of a metal component and lead to a reduced result in the determination of metal content in composite EXPLOSIVES.

The closest in technical essence to the claimed method is the extraction of alumina from rocket fuel containing polymer binder, aluminum and oxidizer (potassium perchlorate, HMX, RDX, nitroglycerine) (U.S. Patent No. 5331106, IPC606 In 21/00, publ. 19.07.94). The method is based on the translation of rocket fuel in non-explosive form by removing oxidant extraction with water and the production of a material containing not more than 15% of the oxidizer, with subsequent thermal treatment at a temperature of 1000-1100°With this material in a reducing atmosphere, with the aim of highlighting aluminum oxide.

In the extraction process oxidant possible partial loss of aluminum included with rocket fuel.

The disadvantage of this method is that the ablation of aluminum particles in the extraction process oxidant does not completely remove the aluminum from rocket fuel, it is therefore impossible its quantitative determination in the original substance. In addition, the heat treatment of the material is carried out in a reducing atmosphere (in the combustion chamber is added to the fuel), the fact significantly complicates the process of heat treatment.

The objective of the invention is to increase the degree of extraction of the metal oxide component of the composite EXPLOSIVES and, as a consequence, improving the accuracy of determining the initial content of the metal component in the composite EXPLOSIVES.

Using the proposed method provides the following technical result:

- the possibility to quantify the metal component in the composite EXPLOSIVES with a relative error no more than 3.7% and the application of this method in analytical chemistry;

security analysis is a powerful highly sensitive EXPLOSIVES;

- simplicity and low cost of analysis through the use of standard low-cost equipment;

- opportunity analysis composite EXPLOSIVES containing nanopowders of metals.

To achieve the technical result in the well-known method for extracting metal oxide component of explosive mixtures, which consists in the translation of composite EXPLOSIVES belonging to the class of nitramines, non-explosive form with subsequent oxidation of the metal component to a metal oxide by thermal processing of the material obtained according to the invention composite EXPLOSIVES transferred to non-explosive form decomposition by treatment with an alkaline reagent, and heat treatment is carried out at a temperature of 800-1100°C in air for 2-4 hours. To simplify and p is increasing the accuracy of the analysis it is desirable to use an alkaline reagent, fully gazifitsiruyutsya during heat treatment. As the alkaline reagent may be used ammonia solution concentration of 10-25% by weight.

The amount of metal component (X1) is determined by the formula:

where m2- weight of crucible with residue after heat treatment, g;

m1- the mass of the crucible, g;

m is the mass of explosive mixtures, g;

k is the calibration factor.

The decomposition of explosive mixtures belonging to the class of nitramines, by treating it with an alkaline component instead of extracting water minimizes loss of the metallic component, and conducting heat treatment at a temperature of 800-1100°C for 2-4 hours allows you to select from the products of decomposition of the metal oxide. The heat treatment parameters are chosen experimentally, under these conditions, the curve of the oxidation goes on the plateau and the oxidation process is stopped. Greatly simplified method of heat treatment (heat treatment is conducted in air and at a wider temperature range), allowing you to use existing standard equipment (muffle furnace).

The essence of the proposed method consists in the following. In composite EXPLOSIVES belonging to the class of nitramines add alkaline reagent, resulting in a contained explosive Razlog which is translated in non-explosive form, forming decomposition products, disappearing without a trace during further heat treatment. As the alkaline reagent is used ammonia solution concentration of 10-25% by weight.

The operation of the transfer of EXPLOSIVES in non-explosive form in this way allows you to fully maintain the metal component and extract it in the form of oxide, which, in turn, allows you to completely isolate the metal oxide and to determine the exact content of the metal component in the composite EXPLOSIVES.

The claimed method is as follows.

Determine the calibration factor.

The calibration factor is a multiplier of metal oxide on the metal taking into account the possibility of incomplete oxidation of the metal powder (degree of oxidation of the metal depends on the content in the powder of the coarse fraction, which may differ from batch to batch of powder metal).

The calibration factor is determined by analysis of reference compounds at several points within the range of the designated contents. Typically, the value of the calibration coefficient, a lot depends on the actual metal content, and varies from batch to batch. In the preparation of reference compounds to prevent loss of components of explosive mixtures, the batching and mixing of the components takes place directly in the crucible.

1. Sample of explosive composition, weighted with an accuracy of 0.0005 g, placed in pre-annealed and weighed crucibles.

2. For the decomposition of the explosive component in explosive mixtures in each crucible add ammonia solution, mixed and incubated for 60 minutes.

3. The contents of the crucible is dried to remove the liquid products of the decomposition of the CENTURY, after which the crucible is placed in a cold muffle furnace, slowly heat the working volume of the furnace with the crucible to a temperature of 800-1100°C, maintain the crucibles within 2-4 hours, resulting in gasification of the remaining decomposition products CC and the oxidation of the metal to its oxide.

4. The crucible is transferred to a desiccator, cooled and weighed.

Fraction of total mass of metal in % in explosive mixtures is determined by the formula:

where m2- weight of crucible with residue on ignition, g;

m1- the mass of the crucible, g;

m is the mass of explosive mixtures, ,

The method is tested on mixtures of CENTURIES of class nitramines (bis-trinitrophenylmethylnitramine, cyclotrimethylenetrinitramine (RDX), an intimate (HMX) with aluminum nanopowder (ultrafine aluminium and zirconium nitratereductor.

The content of metal component ranged from 2 to 30 percent by weight.

The experiments showed that the proposed JV the property allows you to extract the metal oxide component of the composite EXPLOSIVES and to determine the metal content in composite EXPLOSIVES with a relative error no more than 3.7%.

1. The method of extraction of the metal oxide component of mixed explosives, consisting in the transfer of mixed explosives in non-explosive form with subsequent oxidation of the metal component to a metal oxide by thermal processing of the received data, wherein the mixed explosive substance belonging to the class of nitramines, transferred to non-explosive form decomposition by treatment with an alkaline reagent, and heat treatment is carried out at a temperature of 800-1100°C in air for 2-4 hours

2. The method according to claim 1, characterized in that as the alkaline reagent is used ammonia solution concentration of 10-25% by weight.

3. The method according to claim 1, wherein after the heat treatment determines the amount of metal component according to the formula

where m2- weight of crucible with residue on ignition, g;

m1- the mass of the crucible, g;

m is the mass of mixed explosives, g;

k is the calibration factor.



 

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