Method of producing potassium picrate

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing potassium picrate by reacting picric acid with potassium carbonate, characterised by that picric acid is used as a solution in ethyl alcohol with concentration of (5.5-7.5)%, potassium carbonate is used as a water solution with concentration (9.0-11.0)%, the reagents are loaded with weight ratio of picric acid solution to potassium carbonate solution ranging from 3.0 to 5.5, and the reaction is carried out at temperature (17-40)°C. The disclosed method enables to obtain potassium picrate at low temperature (up to 40°C) using minimal equipment, which improves technological effectiveness of the process and ensures output of the end product of up to 95%. The end product meets all standard technical documentation requirements for colour, weight ratio of potassium and water-insoluble impurities and grain size. Potassium picrate obtained this way can be used in production of primers.

EFFECT: high technological effectiveness of the process and output of the end product of up to 95%.

2 cl, 14 ex, 1 tbl

 

The invention relates to methods for explosives, in particular to methods for picrate potassium, which because of its properties can be used in the production of means of initiation (SI).

It is known [Chemical encyclopedia. - M.: Great Russian encyclopedia, 1992, Vol.3, s]that the picrate of metals is produced by interaction of picric acid with oxides, hydroxides or carbonates of the metals.

In [R. Mc.Guchan. Improvements in primary explosive compositions and their manufacture. Proceedings of the 10-th symposium on explosives and pyrotechnics. - 14-16 February 1979, San Francisco, California, USA, Franklin Research Center, p.1-1÷1-12] is the technological process of production of picrate potassium RD 1369, based on the following two-stage reaction is conducted in the aquatic environment:

Because in this technological scheme is used almost saturated solution of picrate sodium, it is impossible to increase the concentration of the solution and accordingly, the output of the finished product (as pointed out by the authors, theoretical yield is 72%).

In the same paper describes the technological process of manufacturing of picrate potassium RD M, based on the following two-stage reaction is conducted in the aquatic environment:

Since this method of obtaining used pre paracrystalline the Oia picric acid, the yield was increased to 82.5%. But the percentage yield insufficient and its maintenance is quite complex: requires recrystallization of picric acid in the presence of crystalline and catalyst modifier.

In this work provides a way of obtaining picrate potassium, which is based on a reaction between picric acid with potassium hydroxide in aqueous medium and in the presence of a crystal modifier. As the authors state, it is possible to increase the yield, but the quality was worse than picrate potassium, obtained according to the technological scheme RD 1369.

The closest technical solution adopted for the prototype is the way to get picrate potassium, described in [AG Horst. Chemistry and technology of nitro compounds. M: Barongis, 1940, s], which States that the potassium picrate obtained by adding potassium carbonate to the hot solution of picric acid according to the following scheme:

2C6H2(NO2)3OH+K2CO3→2C6H2(NO2)3OK+H2O+CO2

When heated to 100°C is performed before the termination of allocation of coal acid. Upon cooling of the solution being crystallized potassium picrate.

The current normative-technical documentation on the potassium picrate, namely that 3-75.10103-9-91, ustanavlivaetsya indicators which must satisfy the finished product. Among the main indicators should indicate the following: color (yellow), the content in the product mass fraction of potassium (14,6±0.2%) and water-insoluble impurities (0,0-0,1%), and grain size of the obtained product should be no more than 110±20 microns.

The method adopted for the prototype allows for maximum yield up to 88% and to obtain a product that meets the requirements of TU 3-75.10103-9-91. However, the synthesis of picrate potassium in the method prototype is carried out at high temperature (100°C), which requires specific equipment (heated reactor). But with the increase in temperature increases the solubility of picrate potassium in water. So, if at 15°C the solubility of picrate of potassium in 100 g of water is 0,0049 g, at 100°C the solubility of picrate of potassium in 100 g of water is increased to 7.14,

Therefore, to reduce the losses of the finished product by cooling the mother liquor in the method-prototype introduces an additional operation of crystallization with the use of the mold.

An object of the invention is to develop a method of obtaining picrate potassium, satisfying the requirements of TU 3-75.10103-9-91 color, content mass fraction of potassium and water-insoluble impurities, the grain size of the obtained product. This synthesis should be carried out at low the temperatures and ensure that the finished product up to 95% using a minimum amount of equipment, that will improve the manufacturability of the process.

The task is solved in that the potassium picrate produced by interaction of picric acid with a compound of potassium, with picric acid is used as a solution in ethanol at a concentration of (5,5÷7,5) %, potassium carbonate is used as an aqueous solution at a concentration of (9,0÷11,0) %, reagents loaded when the mass ratio of the solution of picric acid by weight of solution of potash from 3.0 to 5.5, and the reaction is carried out in the temperature range (17÷40)°C. After receiving the product is subjected to three washing with water and once with alcohol.

The sequence of operations in accordance with the inventive method allows to obtain the potassium picrate, satisfying the requirements of TU 3-75.10103-9-91 color, content mass fraction of potassium and water-insoluble impurities, the grain size of the obtained product. This synthesis is carried out at temperatures up to 40°C in a normal pot synthesis without heating, which improves the manufacturability of the process. Yield up to 95%.

The essence of the proposed method and the results can be illustrated by examples presented in the table. As follows from the data table, prototype method provides receiving picrate potassium (arr. 1) with satisfactory results in terms of color, content mass fraction of potassium is water-insoluble impurities, the grain size of the obtained product with a yield of 88%. The selected modes of obtaining picrate potassium by the proposed method without three times washing the resulting product with water and once with alcohol (arr. 10÷12) also provide the product with the desired characteristics, the yield of the finished product reaches 94%, higher than that of the prototype method. Application three times washing the resulting product with water and once with alcohol (arr. 13÷15) allows to increase the yield up to 95% and reduce the amount of water-insoluble impurities to a minimum.

Thus, the developed method of obtaining picrate potassium, which allows to obtain a product with the required parameters for color, content mass fraction of potassium and water-insoluble impurities, the grain size of the obtained product. Synthesis of the proposed method is carried out at low temperatures in a normal pot synthesis that does not require heating of the reaction mixture and crystallization of the product, and the product yield is up to 95%.

Table
The results of the analysis of the obtained samples picrate potassium
No. sampleConcentrat what I picric acid in ethanol, %The concentration of the aqueous solution of carbonate of potassium, %The ratio of the weight of the solution of picric acid by weight of solution of potashThe temperature of the synthesis,°CColorMass fraction of potassium, %Mass fraction of water-insoluble impurities, %Yield, %The grain size of the finished product, microns
1---95yellow14,50,0388100
2of 5.411,04,030yellow14.4V0,16--
35,58,94,030yellow0,12--
47,610,04,030yellow14.4V0,13--
57,411.14,030yellow14,30,11--
65,59,02,930yellow14.4V0,12--
77,511,05,630yellow14,30,11--
86,510,04,016yellow-brown14,20,21--
96,510,04,041yellow14,30,11-
105,511,03,017yellow14,50,0491100
116,510,04,030yellow14.4V0,0293120
127,59,05,5 40yellow14,70,0694110
135,511,03,017yellow14,60,00494110
146,510,04,030yellow14.4V0,00395100
157,59,05,540yellow14,50,00695110

1. The method of obtaining picrate potassium by reacting picric acid with potassium carbonate, characterized in that picric acid is used as a solution in ethanol at a concentration of (5,5÷7,5)%, potash use is as an aqueous solution at a concentration of (9,0÷11,0)%, the reagents are loaded when the mass ratio of the solution of picric acid by weight of solution of potash from 3.0 to 5.5, and the reaction is carried out in the temperature range (17÷40)°C.

2. The method of obtaining picrate potassium according to claim 1, characterized in that after receiving the product is subjected to three washing with water and once with alcohol.



 

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