RU83497U1 - PRODUCTION DEPARTMENT FOR PROCESSING VANADIUM OXYTICHLORIDE WITH THE PRODUCTION OF VANADIUM PENTAOXIDE - Google Patents

Abstract

The proposed utility model relates to the field of chemical technology of inorganic substances, in particular to production technological departments, sections, complexes for the processing of technical vanadium oxytrichloride (VOCl ₃ + TiCl ₄ ) to produce marketable products - commercial vanadium pentoxide and by-products derived from industrial wastes. The objective of the proposed utility model is the creation of a new “Production Department”, the combination of equipment of which makes it possible to obtain commercial vanadium pentoxide from technical vanadium oxytrichloride and allows us to convert titanium-vanadium-containing production wastes into a form suitable for sale by consumers. The technical result that can be obtained by implementing the proposed technical solution is a high degree of purification of vanadium from titanium impurities. The problem is solved with the achievement of the above technical result by the proposed technical solution - “Production Department for the processing of vanadium oxytrichloride to obtain vanadium pentoxide”, which includes the following main equipment, technologically interconnected: a transportable container with the original vanadium oxytrichloride, hermetically connected through shut-off and control valves a reactor equipped with a stirrer and a distribution device for supplying vanadium oxytrichloride p d layer sodium hydroxide solution below the level of the agitator, the reactor for decomposition of vanadium oxytrichloride coupled to sequentially set the dispenser and tank

preparing a sodium hydroxide solution, an ammonium metavanadate crystallizer tank equipped with a stirrer and equipped with a nozzle for supplying ammonium chloride, filter-1 for isolating and washing the ammonium metavanadate precipitate from the suspension, an ammonium metavanadate recovery tank, the lower discharge of which is directed to filter-1 after filter-1, a calcining furnace and a collection tank of mother liquors and an ammonium metavanadate pump connected to a reactor with a stirrer for neutralizing vanadium are installed to isolate ammonium metavanadate from the suspension containing solutions and wastewater, there are nozzles on the reactor lid, one of which is connected to the dispenser and a tank with a solution containing iron (II) chloride, the other nozzle is connected to the dispenser and the tank for the preparation of sodium hydroxide solution, the lower discharge pipe of the reactor has a connection through a pump with a filter press-2 for the separation of iron (II and III) oxyhydrates from the pulp with impurities of vanadium compounds. New in the proposed technical solution is that after the reactor for the decomposition of vanadium oxytrichloride, a filter press 3 is installed to separate titanium oxyhydrate from the sludge, the trough filter press 3 has a discharge hatch equipped with a shut-off device connecting the filter press 3 and a titanium oxyhydrate precipitate sedimentation tank having connections to the filter press-3 and the sodium hydroxide solution dispenser, the output of the sodium metavanadate solutions purified from the precipitate is directed to a collection container connected with a tank for crystallization of ammonium metavanadate, the discharge hatch of the filter press-3 trough through a shut-off switchgear is connected to a collection of wet washed sludge of titanium oxyhydrate technologically connected to a drying chamber installed in series, a calcining furnace equipped with a discharge device, a storage hopper and filling machine.

Description

The proposed utility model relates to the field of chemical technology of inorganic substances, in particular to production technological departments, sections, complexes for the processing of technical vanadium oxytrichloride (VOCl ₃ + TiCl ₄ ) to produce marketable products - commercial vanadium pentoxide and by-products derived from industrial wastes.

A technical solution is known - "Technological line for the production of vanadium pentoxide" (RF Patent for PM No. 41719 according to application No. 2004116516/22 with priority dated June 1, 2004. Registered and published on November 30, 2004. Bull. No. 31; IPC ⁷ С01G 31/02 $ С22В 34/22).

The well-known "Technological line" includes: a reactor for leaching technical vanadium pentoxide, an alkali solution tank, a suction filter to separate insoluble residue, a crystallization reactor, a filter press, and an ammonium metavanadate decomposition furnace; an insoluble residue leach reactor equipped with a sodium hypochlorite dosing tank; a neutralizing tank equipped with a metering tank of a reducing solution, an absorber with a fluidized nozzle and a circulation tank with an alkaline solution.

A well-known technical solution allows to obtain commercial vanadium pentoxide from intermediates - rough vanadium pentoxide, containing in addition to V ₂ O ₅ impurities of oxides and oxyhydrates of other elements - iron, manganese, silicon, calcium, magnesium, aluminum, etc.

A disadvantage of the well-known "Technological line" is the lack of the necessary equipment for processing technical vanadium oxytrichloride containing 30-90% V ₂ O ₅ and up to 10-70% TiCl ₄ .

Of the known analogues, the closest in technical essence and the technical result achieved is the well-known "Hardware and technological complex for the production of vanadium pentoxide" (RF Patent ПМ No. 74636 by application No. 2008105007 with prior. Dated 11.02.2008. Reg. And publ. July 10, 2008, Bull. No. 19) - adopted as a PROTOTYPE.

The technical solution for the prototype includes the following main technological equipment: a reactor for alkaline treatment of the initial vanadium-containing materials, which is hermetically connected to a transported container with vanadium oxytrichloride, and the outlet of vanadium oxytrichloride from the transported tank is directed through a shut-off and control valve to a switchgear located in the reactor below the mixer. A reactor with a stirrer for alkaline treatment of the starting vanadium-containing materials is connected to a tank for preparing and supplying a solution of sodium hydroxide, a crystallization tank of ammonium metavanadate, having a connection with a series-installed metering tank and a storage tank for preparing and supplying a solution of ammonium chloride, on the lid 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, a pipe the bottom drain of the suspension of which has a connection with a filter-1, for separating the precipitate of ammonium metavanadate from the suspension and washing it, a calcining furnace, a collection tank of mother liquors and an ammonium metavanadate feed, a reactor for neutralizing and neutralizing vanadium-containing wastewater, connected through a dispenser to the tank a collection of iron (II) containing solutions and a tank for the preparation and supply of a solution of sodium hydroxide, a reactor for neutralization and neutralization

vanadium-containing wastewater is connected to filter-2 to separate iron (II and III) oxyhydrates from the pulp 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) from the production of vanadium pentoxide — mother liquors and wastes of ammonium metavanadate.

The disadvantage of the technical solution - "Instrumentation line" according to the prototype is the lack of the necessary equipment to produce commercial vanadium pentoxide from technical vanadium oxytrichloride, containing in addition to VOCl ₃ up to 10-70% titanium tetrachloride - TiCl ₄ .

Another disadvantage of the technical solution known from the prototype is that the equipment included in the “Technological line” does not provide for the possibility of processing the resulting production waste.

The objective of the proposed utility model is the creation of a new “Production Department”, the combination of equipment of which makes it possible to obtain commercial vanadium pentoxide from technical vanadium oxytrichloride and allows us to convert titanium-vanadium-containing production wastes into a form suitable for sale by consumers.

The technical result that can be obtained by implementing the proposed technical solution is a high degree of purification of vanadium from titanium impurities.

The problem is solved with the achievement of the above technical result by the proposed technical solution - "Production Department for the processing of vanadium oxytrichloride to obtain vanadium pentoxide", including the following main

equipment technologically interconnected: a transportable container (1) with the original technical vanadium oxytrichloride, tightly connected through shut-off and control valves to a reactor (2) equipped with a stirrer and a distribution device (3) for supplying vanadium oxytrichloride under a layer of sodium hydroxide solution below the level mixers, a reactor (2) for the decomposition of vanadium oxytrichloride is connected to a sequentially installed batcher (4) and a tank (5) for preparing a solution of sodium hydroxide, a crystallizer tank (6) m ammonium etavanadate equipped with a stirrer and equipped with a nozzle (7) for supplying ammonium chloride, filter-1 (8) for isolating and washing the ammonium metavanadate precipitate from the suspension, and a ammonium metavanadate recovery tank (9), the lower discharge of which is directed to the filter 1 (8), after filter-1 (8), a calcining furnace (10) and a collection tank (11) of mother liquors and an ammonium metavanadate prompter connected to a reactor with a stirrer for neutralizing vanadium-containing solutions and wastewater were installed to separate ammonium metavanadate from the suspension on the lid the reactor has nozzles, one of which is connected to the dispenser (13) and the tank (14) with a solution containing iron (II) chloride, the other nozzle is connected to the dispenser (4) and the tank for the preparation of sodium hydroxide solution (5), the lower discharge nozzle the reactor (12) is connected through a pump with a filter press-2 (16) to separate iron (II and III) oxyhydrates from the pulp with impurities of vanadium compounds. New in the proposed technical solution is that after reactor-3 (17) to separate titanium oxyhydrate from the pulp, the trough (18) of filter-3 (17) has an unloading hatch (19) equipped with a shut-off and distribution device (20), connecting the filter-3 (17) and the tank-repulpator (21) of the precipitate of titanium oxyhydrate, having a connection to the filter press-3 (17) and the batcher (4) of the sodium hydroxide solution, the output of the sodium metavanadate solutions purified from the sediment is directed to the capacity (22),

connected to the ammonium metavanadate crystallization tank, the discharge hatch (19) of the filter-3 trough (17) through a shut-off distribution device (20) is connected to a collector (23) of a wet washed precipitate of titanium oxyhydrate, which is technologically connected to a drying chamber (24) ), a calcining furnace (25) equipped with an unloading device, a storage hopper (27) and a filling machine (28).

IMPLEMENTATION OF THE SUGGESTED USEFUL MODEL

The proposed technical solution - "Production Department for the processing of vanadium oxytrichloride to obtain vanadium pentoxide" works and is operated as follows (see. Fig.).

Sodium hydroxide solution (20-200 g / dm ³ ) of sodium hydroxide is pumped (or by gravity) into a reactor (2) with a mixer from a dispenser (4) connected to a tank (5) and then, with the mixer switched on, through a switchgear (3) from the transported container (1) serves technical vanadium oxytrichloride (30-90% VOCl ₃ + 10-70% TiCl ₄ ). The feed rate is regulated by valves. In the reactor (2), the “decomposition” of technical vanadium oxytrichloride occurs with the formation of pulp — a solution of sodium vanadate — NaVO ₃ and a fine precipitate of titanium oxyhydrates: TiO (OH) ₂ , Ti (OH) ₄ , TiO ₂ , H ₂ O, etc. the pulp from the reactor (2) is pumped through the bottom discharge pipe with a pump (not shown in the figure) to filter-3 (17), which is mainly used as a filter press. The sodium metavanadate filtrate solution - NaVO _{3 is} sent to a collection container (22). After filling the filter with sediment, the latter is dumped into the trough (18) and then, through a shut-off and distribution device, it is fed to the recovery tank (21), into which sodium hydroxide solution and pulp in the recovery tank (21) are preliminarily filled ) incubated with continuous stirring at 60-90 ° C for 0.5-2

hours for additional extraction of vanadium compounds from the precipitate phase into the solution. At the end of the repulpation, the pulp from the repulpator tank (21) is pumped onto filter-3 (17) with a pump, the sodium metavanadate solution is separated from the sediment and sent to the collection and delivery tank (22), the sediment is discharged from filter-3 (17) first into the trough (18) and then to the collection (23) of a wet precipitate of titanium oxyhydrate with impurities of vanadium compounds. From this collection (23), the precipitate is sent to a sequentially installed drying chamber (24) for dewatering the precipitate, then to a calcining furnace (25). From a calcining furnace (25), the resulting titanium dioxide with impurities (up to 5-10% V ₂ O ₅ ) is discharged through a discharge device (26) into a storage hopper (27), from which the sediment is packed into bags through a filling machine (28) and shipped to consumers, for example, enterprises producing titanium sponge - magnetothermal reduction of titanium tetrachloride. In particular, the resulting titanium dioxide, containing up to 5-10 V ₂ O ₅ , is sent together with ilmenite and / or ilmenorutil concentrate to the ore-thermal furnace (RTP) for reductive ore-smelting. According to another disposal option, the resulting titanium dioxide is used for the preparation of the charge — together with titanium slag for chlorination in the melt of sodium and / or potassium chlorides to produce titanium tetrachloride and technical vanadium oxytrichloride.

To obtain commercial vanadium pentoxide, a solution of sodium metavanadate - NaVO ₃ , purified from titanium compounds, is pumped from a collection container (22) into the crystallization tank (6) of ammonium metavanadate, into which, with the stirrer turned on, the calculated amount of chloride is supplied through the pipe (7) ammonium - either in solid form or in the form of a solution. The resulting suspension, if necessary, is cooled and maintained, as a result of which a crystalline precipitate of ammonium metavanadate - NH ₄ VO _{3 is} precipitated from the solution into the solid phase.

The suspension is then fed to filter-1 (8), for which suction filters, filter presses (manual and / or automatic), drum vacuum filters, etc. can be used. The precipitate of ammonium metavanadate is separated from the mother liquor, which is collected in a collection tank (11). The precipitate on filter-1 (8) 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 (11). Then the precipitate from filter-1 (8) is discharged into a tank-repulpator (9), 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 (8), the filtrate is collected in a collection tank (11). The precipitate on filter-1 (8) is again washed with a diluted (1-3%) solution of ammonium chloride. All promotions are collected in a collection tank (11). The washed (washed off from sodium chloride) NH ₄ VO ₃ precipitate is discharged from filter-1 and loaded into a calcining furnace, which is mainly used as a cylindrical rotary furnace installed at a slight (3-5 °) slope to the horizontal axis and having the entire length of several heating and calcination zones and various temperatures from 100-150 ° C to 500-550 ° C. As the NH ₄ VO ₃ precipitate passes from the loading hatch to the unloading unit, ammonium metavanadate decomposes to produce marketable powdered vanadium pentoxide. At the end of the calcination process, the obtained commercial vanadium pentoxide is discharged from the calcination furnace (10), packaged in bags, and shipped to consumers.

In order to neutralize all vanadium-containing wastewater generated from the vanadium, the mother liquors, the wastewater, the combined effluent from the collection tank (11) are pumped into the reactor (12), then, with the stirrer turned on, it is sequentially fed from the batcher (13) and the collection tank ( 14) a solution of a salt of ferrous iron — FeCl ₂ and / or FeSO ₄ , after which a hydroxide solution is supplied from the dispenser (4) and the tank (5)

sodium. The pulp in the reactor (12) is mixed and pumped onto filter-2 (16). The precipitate of iron oxyhydrate containing vanadium extracted from the effluent 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 (16) and sent for further processing and disposal. The filtrate and wastewater purified from vanadium are collected in a collector (15) and then, after a chemical control analysis, they are discharged into the sewer.

Production department for the processing of vanadium oxytrichloride to obtain vanadium pentoxide

1. transported container with the original technical vanadium oxytrichloride;

2. a reactor equipped with a stirrer for the decomposition of vanadium oxytrichloride;

3. a distribution device for supplying the initial technical vanadium oxytrichloride under a layer of sodium hydroxide solution, below the level of the mixer;

4. dispenser of sodium hydroxide solution;

5. tank for the preparation of sodium hydroxide solution;

6. crystallization tank of ammonium metavanadate;

7. a pipe for feeding ammonium chloride into the crystallizer tank (6);

8. Filter-1 (Ф-1) for isolating ammonium metavanadate from the suspension;

9. ammonium metavanadate sediment recovery tank;

10. calcining furnace for calcining ammonium metavanadate to obtain vanadium pentoxide;

11. tank-collection of uterine solutions and promotion of ammonium metavanadate;

12. reactor for the neutralization of vanadium-containing solutions and promoter - mother liquors and promoter of ammonium metavanadate;

13. dispenser of solutions of chloride and / or iron sulfate;

14. a tank for the preparation and / or storage of initial solutions of chloride and / or iron sulfate;

15. a collection of wastewater purified from vanadium;

16. filter-2 (F-2) for the precipitation of iron (II and III) oxyhydrates from the pulp with impurities of vanadium compounds;

17. filter-3 to isolate titanium oxyhydrate from the pulp;

18. trough filter -3;

19. unloading hatch trough (18) of filter-3 (17);

20. shut-off and control switchgear;

21. heated tank-repulpator with a stirrer for repulping titanium oxyhydrate;

22. collection capacity of sodium metavanadate solutions;

23. a collection of wet sediment titanium oxyhydrate;

24. drying chamber precipitate titanium oxyhydrate;

25. calcination furnace of titanium oxyhydrate with impurities of vanadium compounds;

26. unloading device of a calcining furnace;

27. bunker storage of calcined sediment - titanium dioxide with impurities (up to 5-10%) of vanadium pentoxide;

28. filling machine.

Claims (1)

Production department for processing vanadium oxytrichloride to produce vanadium pentoxide, including a transported tank with the original vanadium oxytrichloride, tightly connected through shut-off and control valves with a reactor equipped with a stirrer and a distribution device for supplying vanadium oxytrichloride under a layer of sodium hydroxide solution below the level of the mixer, a reactor for decomposition vanadium oxytrichloride is connected to a sequentially installed dispenser and a tank for preparing a solution of hydroxide n atria, an ammonia metavanadate crystallizer tank equipped with a stirrer and equipped with a nozzle for supplying ammonium chloride, filter-1 for isolating and washing the ammonium metavanadate precipitate from the suspension, an ammonium metavanadate-recovery tank, the lower discharge of which is directed to filter-1, after the filter -1 to isolate ammonium metavanadate from the suspension, a calcining furnace and a collector tank for mother liquors and an ammonium metavanadate feed connected to a reactor with a stirrer for neutralizing vanadium-containing solutions and wastewater are installed , on the reactor cover there are nozzles, one of which is connected to the dispenser and the tank with the solution containing iron (II) chloride, the other nozzle is connected to the dispenser and the tank for the preparation of the sodium hydroxide solution, the lower drain port of the reactor has a connection through the pump to the filter press 2 for separating the precipitate of iron (II and III) oxyhydrates with impurities of vanadium compounds, characterized in that a filter press 3 is installed after the reactor for the decomposition of vanadium oxytrichloride to precipitate titanium oxyhydrate from the pulp, This filter press-3 has a discharge hatch equipped with a shut-off device connecting the filter press 3 and the titanium oxyhydrate precipitate recovery tank, having connections to the filter press-3 and the sodium hydroxide solution dispenser, the output of the metavanadate solution purified from the sediment sodium is sent to a collection container connected to a tank for crystallization of ammonium metavanadate, the discharge hatch of the filter press-3 trough through a shut-off switchgear is connected to a wet washed sediment collector and titanium oxyhydrate, technologically connected to a drying chamber installed in series, a calcining furnace equipped with an unloading device, a storage hopper and a filling machine.