Method for production of granulated sodium arsenite

FIELD: technological processes.

SUBSTANCE: invention relates to the field of chemical technology and may be used to produce granulated sodium arsenite in processing of reaction mass produced at the stage of alkaline hydrolysis of lewisite. Liquid reaction mass is exposed to continuous convective spraying drying in fluidised bed. Process is carried out at the temperature of layer 70150C and at underpressure of 10200 mbar, and nitrogen is used as fluidised and spraying agent.

EFFECT: invention provides for hardware and structurally simple, technologically and ecologically safe process applicable for large-capacity production of granulated sodium arsenite suitable for long-term storage.

3 cl, 1 dwg

 

The invention relates to the field of chemical technology and can be used to obtain a granulated sodium arsenite by processing the reaction mixture obtained from stage alkaline hydrolysis of lewisite.

Granular sodium arsenite can be used as raw materials for obtaining the oxide of arsenic (III)metal arsenic, arsina cars arsenic, etc.

A known method of producing sodium arsenite in the form of solid particles in the size range of 0.11 mm and containing less than 3% moisture in the vacuum cylinder drier, giving it a 67% solution of sodium arsenite (Posin ON the Technology of mineral fertilizers. 4-th edition. part 2. - L.: Chemistry, s, 1974).

The main disadvantage of this method is the low performance of the vacuum roller dryers are suitable to use only the small-capacity production (Lykov MV Drying in the chemical industry. - M.: Chemistry, s, 1970).

The closest technical solution is selected as the prototype of the present invention is a method of producing sodium arsenite by processing the reaction mixture obtained from stage alkaline hydrolysis of lewisite, evaporation-drying in a rotary vacuum dryer at 74125C and a pressure of 0.40.6 ATM using additives 8,015,0% (wt.) 1,1,2,2-tetrachlorethane and 0,51,0% (wt.) montmorillonite clay (Patent P is 2209103 from 27.07.2003,).

The disadvantages of this method, which hinders its application in large industrial scale, are the periodicity of the process, and the process 1,1,2,2-tetrachlorethane. The main disadvantages of periodic process is downtime of the process equipment during loading of raw material and unloading of the product, as well as the volatility of the technological mode at the beginning and end of the processing cycle. Also, when interacting 1,1,2,2-tetrachlorethane with the reaction mass can flow process dehydrochlorinating with the formation of trichloroethylene, whose flash point is only 32C. This fact significantly reduces the security of the process of obtaining granulated sodium arsenite during the processing of the reaction mixture by the above method.

The aim of the invention is to create a simple from the point of view of hardware design, technologically and environmentally friendly continuous process, applicable for large-scale production of granular sodium arsenite suitable for long-term storage.

The method consists in using, to obtain a granulated sodium arsenite, convective process spray drying in the fluidized bed. Moreover, the process occurs at a temperature of layer 70150C and under a vacuum of 0200 mbar, and as pseudoviruses agent, nitrogen is used.

The technology of the method consists in the following. The spray dryer fluidized bed of the gas grill fall asleep seed material in powder form of sodium chloride or reture of sodium arsenite. Further, in a gas grill, bottom, serves pseudoviruses agent, which is nitrogen, at a temperature of 150280C. After the layer of the seed went in fluidized condition, start by spraying through a mechanical injector to apply to the layer of the reaction mass, which has a temperature of ~20C (nozzle nozzle pointing upward, the pressure of nitrogen in the sputtering 1,52 bar). The temperature in the layer is maintained in the range of 70150C, and the apparatus in which the process operates under a vacuum of 10 to 200 mbar. Exhaust process gas passes through the drying system and clean and again goes into the dryer as pseudoviruses agent. The finished granules in the size range 15 mm continuously removed from the dryer through line discharge of product.

The figure schematically shows the installation, which was implemented this method. The basic geometrical parameters of the setup are as follows: the diameter of the drying chamber is 160 mm, the height of the cylindrical part is 450 mm, the diameter of the holes naturally re EDI - 0,4 mm

The device operates as follows.

Pseudoviruses agent 1 is supplied through the gas grill apparatus 10 from the bottom up. In the working area of the device 7 is granular, rolling, fluid condition during the passage through it of the process gas stream. In the zone of separation 8 gas flow rate decreases due to the expansion of the walls of the apparatus, and a preliminary separation of fine particles and dust. Exhaust process gas 3 exit from the apparatus in its upper part and, after additional dust in the cyclone 11, is fed into the drying system and fine cleaning, after which, re-enters the drying chamber as a spray and pseudoviruses agents. Separated in the cyclone dust continuously withdrawn through the cellular drum gateway 12 back into the fluidized bed.

Using a mechanical injector reaction mass 4 is sprayed directly into the fluidized bed.

Through the screen 9 from the process continuously selected product. Design screen allows you to select granules of a given size. It is implemented as follows: the compressed nitrogen 2 is fed through a sifter bottom-up flow rate is adjusted so that only granules 6, the falling speed which is higher than the flow velocity of the upward when ATAGO nitrogen, can pass through the screen and get into the tank with the final product. Granules 5 speed falls below the speed of the upward flow, come back into the fluidized bed.

Tests of the proposed method for granulated sodium arsenite conducted in the range of the following process parameters:

- quantity of seed 0,351.5 kg;

- consumption pseudoviruses agent 65110 m3/h;

the flow of the reaction mass 0,85.2 kg/h;

- temperature pseudoviruses agent 150280C;

the temperature in the fluidized bed 70150C.

The following results are obtained:

- the amount of product 0,251.8 kg/h;

- humidity product 0,41%;

- granulometric composition of the product is 8090% of the granules in the size range 15 mm

When the temperature of the layer below 70C in our experiments we observed the formation of wet agglomerates in the gas distribution grid, which, in turn, led to the destruction of the fluidized bed, emergency stop and the cleaning apparatus. When the bed temperature above 150C was observed active dust formation and, consequently, the lack of growth of the granules.

The use of nitrogen as a spray and pseudoviruses agents prevents oxidation of arsenic.

The process under a vacuum of 10200 mbar prevents the accumulation of arsenic in the area of work is his premises, what makes the process environmentally friendly.

Information about the use of the process of convective spray drying in the fluidized bed to obtain a suitable for long-term storage of granulated sodium arsenite is not available.

The associated analysis of the proposed solutions with the prototype shows that the proposed method is distinguished by the use of a continuous process of convective spray drying in the fluidized bed to obtain a suitable for long-term storage of granulated sodium arsenite.

1. A method of obtaining a granulated sodium arsenite, characterized in that the liquid reaction mass obtained from step alkaline hydrolysis of lewisite, is subjected to continuous convective spray-dried in the fluidized bed at a temperature of layer 70150C and under a vacuum of 10 to 200 mbar, with ongoing selection of granules in the size range 15 mm and a moisture content of 0.41 wt.%, and as a spray and pseudoviruses agent using nitrogen.

2. The method according to claim 1, characterized in that formed during the drying-granulation dust fraction after separation from the flow of exhaust process gas back into the process as Remora.

3. The method according to claim 1, characterized in that nitrogen is used as pseudoviruses and spray agent, PR is IDA purification system from dust fraction and drying system, circulates in the system in a closed loop.



 

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