RU83774U1 - TECHNOLOGICAL LIMIT FOR PRODUCING PANAOXIDE OF VANADIUM - Google Patents

Abstract

Technological redistribution for the production of vanadium pentoxide, including a reactor with a stirrer for alkaline treatment of vanadium oxytrichloride, hermetically connected to the transported capacity of the initial vanadium oxytrichloride and connected in series with the dispenser and the tank for the preparation and supply of sodium hydroxide solution, the ammonium metavanadate crystallizer tank is connected to the ammonium chloride dispenser and a tank for preparing a solution of ammonium chloride, filter-1 to isolate the precipitate of ammonium metavanadate from the suspension and wash it, ammonium metavanadate sediment recovery tank connected to filter-1, a calcining furnace, mother liquor collection tank and ammonium metavanadate recovery tank, vanadium-containing wastewater treatment solution - mother liquors and ammonium metavanadate treatment connected via an iron dispenser tank (II) -containing solutions, a dispenser and a tank for preparing and supplying a solution of sodium hydroxide, filter-2 for separation of iron (II and III) oxyhydrates from the pulp with vanadium impurities, characterized in that the pipe the lower discharge of the reactor for alkaline treatment of vanadium oxytrichloride is directed through the pump and shut-off and control valves to filter-3, the trough of which is connected to a collector of titanium cake, a precipitate of titanium oxyhydrate, through the discharge distributing device, the outlet of which is directed to a heated tank with a stirrer for titanium repulpation cake, on the lid of the tank there is a nozzle for connecting a sodium hydroxide solution to the dispenser, the discharge of pulp from this tank through the pump is directed to filter-3, the output of the solid phase

Description

The proposed utility model relates to the field of metallurgy and chemical technology and can be used at chemical and metallurgical enterprises to obtain commercial vanadium pentoxide from vanadium-containing raw materials, in particular from technical vanadium oxytrichloride (30-90% VOCl ₃ + 70-10% TiCl ₄ ), formed in titanium production during the purification of technical titanium tetrachloride (TiCl ₄ ) from vanadium compounds.

The well-known "Production line for the production of vanadium pentoxide" (Certificate PM PM No. 23292 according to the application No. 2001130623/20 with priority from 11/16/2001. Regist. And published. 06/10/2002. Bull. No. 16), including: a reactor for leaching technical vanadium pentoxide, an alkali solution tank, a suction filter to separate insoluble residue, a crystallizer reactor, a filter press and an ammonia metavanadate decomposition furnace — NH ₄ VO ₃ to produce vanadium pentoxide — V ₂ O ₅ ; an insoluble residue leach reactor equipped with a sodium hypochlorite dosing tank.

The well-known "Production line" provides the production of commercial vanadium pentoxide from technical V ₂ O ₅ containing impurities of other metals - iron, manganese, etc.

The disadvantage of this well-known technical solution is the lack of equipment for the production of V ₂ O ₅ from technical vanadium oxytrichloride in the "Technological line".

Of the known analogues, the closest in technical essence and the achieved technical result is the well-known

"Hardware and technology complex for the production of vanadium pentoxide" (RF Patent ПМ No. 74636 according to application No. 2008105007 with priority from 02/11/2008. Register and publ. 10.07.2008. Bull. No. 19) - adopted as a PROTOTYPE.

The technical solution according to the prototype includes the following main technological equipment: a reactor for alkaline treatment of the initial vanadium-containing materials, hermetically connected to the transported container with vanadium oxytrichloride, the output of vanadium oxytrichloride from the transported tank through the shut-off and control valves is directed to a switchgear located in the reactor below the level mixers; a reactor with a stirrer for alkaline treatment of the starting vanadium-containing materials, connected to a tank for preparing and supplying a solution of sodium hydroxide, a crystallizer tank of ammonium metavanadate, having connections with a series-installed metering tank and a storage tank for preparing and supplying a solution of ammonium chloride, the lid of the crystallizer tank has a loading hatch in which the outlet from the sodium chloride collection hopper is directed; after filter-1, a ammonium metavanadate-recovery tank is installed; OR for neutralization and neutralization of vanadium-containing wastewater, connected through a batcher to a collection tank of iron (II) -containing solutions and a tank for preparing and supplying a solution of sodium hydroxide, a reactor for neutralizing and neutralizing vanadium-containing wastewater is connected to a filter-2 for separation from the pulp precipitate of iron oxyhydrates (II-III) with impurities of vanadium compounds.

The technical solution according to the prototype provides the production of commercial vanadium pentoxide from commercial vanadium oxytrichloride (99.0-99.9% VOCl ₃ ) and makes it possible to neutralize wastewater - waste water generated by the production of vanadium pentoxide - mother liquors and wastes of ammonium metavanadate.

The disadvantage of the technical solution - "Hardware-technological complex for producing vanadium pentoxide" according to the prototype is the lack of the necessary equipment for the production of commercial vanadium pentoxide from technical vanadium oxytrichloride, containing in addition to vOCl ₃ up to 10-70% titanium tetrachloride - TiCl ₄ .

The objective of the proposed utility model is the creation of a new technological redistribution, the combination of equipment of which makes it possible to obtain commercial vanadium pentoxide from technical vanadium oxytrichloride.

The technical result that can be obtained by implementing the proposed utility model is the separation of vanadium from related impurities - titanium compounds, the content of which in the feedstock - technical VOCl ₃ can range from 10 to 70%.

The problem is solved with the achievement of the above technical result by the proposed utility model - “Technological redistribution for the production of vanadium pentoxide”, including a reactor (1) with a stirrer for alkaline treatment of vanadium oxytrichloride, hermetically connected to the transported tank (2) of the initial technical vanadium oxytrichloride, connected in series with a dispenser (3) and a tank for preparing and supplying a sodium hydroxide solution (4), a crystallizer tank (5) of ammonium metavanadate is connected to a chlorine dispenser and ammonium (6-1) and the tank (6-2) for solution NH ₄ Cl, 1-filter (7) to separate the precipitate from the ammonium metavanadate slurry and washing tank repulpator (8) precipitate ammonium metavanadate, coupled with filter-1, a calcining furnace (9), a collection tank (10) of mother liquors and an ammonium metavanadate feed, a reactor (11) for neutralizing vanadium-containing wastewater - mother liquors and an ammonium metavanadate feed connected through a dispenser (12) to the tank - a collector (13) of iron (II) -containing solutions, a dispenser (3) and a tank (4) for preparing and supplying eniya hydroxide solution

sodium, filter-2 for the precipitation of iron (II and III) oxyhydrates from the pulp with vanadium impurities. New in the proposed technical solution is that the lower discharge pipe of the reactor (1) for alkaline treatment of vanadium oxytrichloride is directed through a pump (not shown in the figure) and shut-off and control valves to filter-3 (15), the trough (16) of which the unloading and distribution device (17) is connected to the collector (18) of the titanium cake - a precipitate of titanium oxyhydrate, the outlet of which is directed to a heated tank (19) with a stirrer for repulping the titanium cake, on the tank cover there is a nozzle for connection to the dispenser (3) of the solution hydrox sodium ida, draining the pulp from this tank through a pump (not shown in the figure) is directed to filter-3 (15), the output of the sodium metavanadate solution purified from the solid phase from filter-3 is directed to a prefabricated-averaging tank (19) connected to ammonium metavanadate crystallizer tank (5).

IMPLEMENTATION OF THE SUGGESTED USEFUL MODEL

The proposed technical solution - "Technological redistribution for the production of vanadium pentoxide" works and is operated as follows.

Sodium hydroxide solution (20-200 g / dm ³ ) of sodium hydroxide is pumped (or by gravity) into a reactor (1) with a mixer from a dispenser (3) connected to a tank (4) and then, when the mixer is switched on, through a switchgear from a transported tank ( 2) serves technical vanadium oxytrichloride (30-90% VOCl ₃ + 10-70% TiCl ₄ ). The feed rate is regulated by valves. In the reactor (1), "decomposition" of vanadium oxytrichloride occurs with the formation of a sodium vanadate solution.

and precipitation of titanium oxyhydrate:

The resulting pulp is fed (pumped) to filter-3 (15), which is mainly used as a filter press. A solution of sodium metavanadate (NaVO ₃ ), purified from the solid phase - suspended particles of titanium cake - titanium oxyhydrate, is collected in a collection-averaging tank (20) equipped with a stirrer. Titanium cake - a precipitate of titanium oxyhydrate with impurities of vanadium compounds is discharged from filter-3 (15) into a trough (16), from where this precipitate enters a collector (18) through a discharge and distribution device (18), from which the precipitate is sent to a heated tank ( 18) with a stirrer for repulping titanium cake - a precipitate of titanium oxyhydrate in a solution of sodium hydroxide - in order to recover vanadium compounds (NaVO ₃ ) from the precipitate. Repulpation is carried out at W: T = 2-5, T = 60-80 ° for 0.5-2 hours. The pulp is then pumped (the pump in the figure is not shown) to filter-3 (15) a solution of sodium metavanadate, purified from the precipitate - titanium oxyhydrate from filter-3 (15), is collected in a collection-averaging tank (20), from which the combined and averaged NaVO ₃ solution enters the crystallization tank (5) of ammonium metavanadate, the precipitate of titanium oxyhydrate on the filter, if necessary, washed with sodium hydroxide solution and / or water, then this precipitate is discharged from filter-3 (15) into the trough (16) and through discharge the distribution device is loaded into the collection (18). From this collection (18), the sediment is then shipped for further processing and disposal.

When the stirrer is on, a solution of ammonium chloride is supplied from the flow-storage tank — the tank for preparing the NH ₄ Cl solution (6–2) through the batcher (6–1). The resulting suspension is cooled and aged, as a result of which a crystalline precipitate of ammonium metavanadate is precipitated from the solution into the solid phase:

The suspension is then fed to filter-1 (7), for which suction filters, filter presses (manual and / or

automatic), drum vacuum filters, etc. The precipitate of ammonium metavanadate is separated from the mother liquor, which is collected in a collection tank (10). The precipitate on filter-1 (7) is washed with a diluted (1-3%) solution of ammonium chloride, in an amount of 2-3 volumes per 1 volume of precipitate. Promotions are collected in a collection tank (10). Then the precipitate from filter-1 (7) is discharged into the tank-repulpator (8), into which a diluted (1-3%) solution of ammonium chloride is preliminarily poured (pumped). The precipitate NH ₄ VO _{3 is} repulped at a ratio of W: T = (3-10): 1, the suspension is pumped onto filter-1 (7), the filtrate is collected in a collection tank (10). The precipitate on filter-1 (7) is again washed with a diluted (1-3%) solution of ammonium chloride. All promotions are collected in a collection tank (10). The washed (“washed” from sodium chloride) precipitate of NH ₄ VO _{3 is} discharged from filter-1 (7) and loaded into a calcining furnace (9), which is mainly used as a cylindrical rotary furnace installed at a slight (3-5 °) slope to the horizontal axis and having along the entire length several heating and calcining zones with different temperatures from 100-150 ° C to 500-550 ° C. As the NH ₄ VO ₃ precipitate passes from the “inlet” (loading hatch) to the exit (to the unloading device), ammonium metavanadate decomposes to produce marketable powdered vanadium pentoxide.

In this case, the released ammonia is mainly oxidized to nitrogen. Vanadium pentoxide in this case, apparently, plays the role of a catalyst. At the end of the calcination process, the resulting commercial vanadium pentoxide is discharged from the calcination furnace (9), packaged in airtight containers (bags) and shipped to consumers.

To neutralize from vanadium all vanadium-containing wastewater generated at the Peredelka - mother liquors, the washer, combined in the collection tank (10), is pumped into the reactor (11), then, with the stirrer turned on, it is sequentially supplied from the batcher (12) and

a collection tank (13) a solution of ferrous iron salt — FeCl ₂ or FeSO _4, and then a sodium hydroxide solution from a dispenser (6-1) and a tank (6-2). The pulp in the reactor (11) is mixed and pumped onto filter-2 (14). The precipitate of iron oxyhydrates (II and III) containing vanadium extracted from the pulp is separated from the purified (neutralized) solution from vanadium chloride (NaCl, NH ₄ Cl) solution, washed on the filter with water, discharged from filter-2 (14) and sent to recycling and disposal. The filtrate and wastewater purified from vanadium are discharged into the sewer.

TECHNOLOGICAL LIMIT FOR PRODUCING PANAOXIDE OF VANADIUM

1. a reactor with a stirrer for alkaline treatment of the initial technical vanadium oxytrichloride;

2. a transporting container with the original technical vanadium oxytrichloride;

3. dispenser of sodium hydroxide solution;

4. a tank with a stirrer for preparing a solution of sodium hydroxide;

5. a crystallizer tank of ammonium metavanadate;

6-1. ammonium chloride dispenser;

6-2. a tank for preparing a solution of ammonium chloride;

7. Filter-1 (Ф-1) for isolating ammonium metavanadate from the suspension and washing it;

8. tank-repulpator with an agitator for the repulpation of ammonium metavanadate;

9. calcination furnace-1;

10. tank-collection of vanadium-containing mother liquors and promotion of ammonium metavanadate;

11. A reactor with a stirrer for neutralizing wastewater (wastewater) and mother liquors from vanadium and promoting ammonium metavanadate;

12. dispenser of iron (II) -containing solutions;

13. a collection tank of iron (II) -containing solutions, for example, solutions containing FeCl ₂ and / or FeSO ₄ ;

14. filter-2, for example, a filter press (F-2) for separating from the pulp a precipitate of iron oxyhydrate with impurities of vanadium compounds;

15. filter-3, for example, a filter press (Ф-3) for separation from the pulp after alkaline (NaOH) treatment of technical vanadium oxytrichloride (VOCl ₃ + TiCl ₄ ) “titanium cake” - a precipitate of titanium oxyhydrate with impurities of vanadium compounds (mainly NaVO ₃ );

16. trough filter-3 (filter press (F-3);

17. unloading and distribution device trough filter-3;

18. a collection of titanium cake - a precipitate of titanium oxyhydrate with impurities of vanadium compounds;

19. a heated tank with a stirrer for the repulpation of titanium cake in a solution of sodium hydroxide - for additional extraction of vanadium from the precipitate - titanium oxyhydrate;

20. prefabricated averaging tank with a solution of sodium metavanadate.

Claims (1)

Technological redistribution for the production of vanadium pentoxide, including a reactor with a stirrer for alkaline treatment of vanadium oxytrichloride, hermetically connected to the transported capacity of the initial vanadium oxytrichloride and connected in series with the dispenser and the tank for the preparation and supply of sodium hydroxide solution, the ammonium metavanadate crystallizer tank is connected to the ammonium chloride dispenser and a tank for preparing a solution of ammonium chloride, filter-1 to isolate the precipitate of ammonium metavanadate from the suspension and wash it, ammonium metavanadate sediment recovery tank connected to filter-1, a calcining furnace, mother liquor collection tank and ammonium metavanadate recovery tank, vanadium-containing wastewater treatment solution - mother liquors and ammonium metavanadate treatment connected via an iron dispenser tank (II) -containing solutions, a dispenser and a tank for the preparation and supply of sodium hydroxide solution, filter-2 for separation of iron (II and III) oxyhydrates from the pulp with vanadium impurities, characterized in that the pipe the lower discharge of the reactor for alkaline treatment of vanadium oxytrichloride is directed through the pump and shut-off and control valves to filter-3, the trough of which is connected to a collector of titanium cake, a precipitate of titanium oxyhydrate, through the discharge-distributing device, the outlet of which is directed to a heated tank with a stirrer for titanium repulpation cake, on the lid of the tank there is a pipe for connecting a sodium hydroxide solution to the dispenser, the discharge of pulp from this tank through the pump is directed to filter-3, the output of p the solution of sodium metavanadate from filter-3 is directed to a prefabricated-averaging tank connected to a crystallization tank of ammonium metavanadate.