RU83505U1 - SYSTEM OF TECHNOLOGICAL EQUIPMENT FOR PROCESSING VANADIUM OXYTICHLORIDE WITH PRODUCTION OF VANADIUM PENTAOXIDE - Google Patents

Abstract

A system of technological equipment for processing vanadium oxytrichloride to produce vanadium pentoxide, including a reactor with a stirrer for alkaline treatment of vanadium oxytrichloride, hermetically connected to a transported tank of the initial technical vanadium oxytrichloride, connected in series with a batcher and a tank for the preparation and supply of sodium hydroxide solution, a metavanadate crystallizer tank ammonia connected to an ammonium chloride dispenser and an NH4Cl solution preparation tank, filter-1 for isolation from a suspension of ammonium metavanadate sludge and its washing, a ammonium metavanadate sludge repulpator tank connected to filter-1, a calcining furnace, a mother liquor collection tank and an ammonium metavanadate recovery vessel, a vanadium-containing wastewater neutralization reactor uterine solutions and ammonia methavanadate connected through a dispenser to a collection tank of iron (II) -containing solutions, a dispenser and a tank for preparing and supplying a solution of sodium hydroxide, filter-2, for the precipitation of iron oxyhydrates from the pulp (II and III) with vanadium impurities, characterized in that the lower discharge pipe of the reactor for alkaline treatment of vanadium oxytrichloride is directed through a pump and shut-off and control valves to filter-3, the trough of which is connected to a collector of titanium cake-precipitate of titanium oxyhydrate through a discharge-distributing device, the outlet from which is directed to a heated tank with a stirrer for repulping titanium cake, on the tank cover there is a pipe for connecting sodium hydroxide solution to the dispenser, draining the pulp from the tank through a pressure pump

Description

The proposed utility model relates to the field of hydrometallurgy and chemical technology of inorganic substances, in particular to technological equipment - systems, complexes, sections, compartments, etc., for the production of oxyhydrates and metal oxides and can be specifically used in chemical and metallurgical enterprises to obtain of commercial vanadium pentoxide from the initial technical vanadium oxytrichloride (VOCI ₃ + TiCI ₄ ) formed at titanium-magnesium enterprises in the process of purification of technical titanium tetrachloride from vanadium compounds.

A technical solution is known - “Technological Department for the Production of Metal Oxides” (Patent for PM No. 72964 according to the application No. 2007148250/22 with priority dated 12.24.2007. Regist. And publ. 10.08.2008. Bull. No. 13), including the following technological equipment:

- transported tank with initial metal chlorides;

- a container for the preparation and dosage of the initial chloride solutions, equipped with a stirrer;

- filtering equipment;

- tank collection of the mother liquor;

- tank-repulpator;

- a drying chamber;

- calcining furnace;

- hopper-collection of finished products;

- filling machine;

- tank collection promvlod oxides of niobium and / or tantalum;

- hydrochloric acid metering tank;

- consumable container with ammonia water;

- bubbler of compressed air;

- dispersant;

- dosing tank of an aqueous solution of high molecular weight surfactants (surfactants);

- distilled water distribution line;

- spray dryer;

- cyclone;

- pipelines, pumps, shut-off and control valves,

- instrumentation, automation, etc.

The known technical solution provides highly dispersed, uniform in size oxides of niobium and tantalum from the starting metal chlorides — niobium oxytrichloride — NbOCI ₃ and tantalum pentachloride — TaCl ₅ . However, the equipment that is part of the well-known "technological department ..." does not allow to process technical vanadium oxytrichloride and obtain commercial vanadium pentoxide.

Of the known analogues, the closest in technical essence and the technical result achieved is the well-known "Hardware-technological complex for producing vanadium pentoxide" (Patent for PM No. 74636 by application No. 2008105007/22 with prior, dated 11.02.2008. Reg. And publ. 07/10/2008 Bull. No. 15 - 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 has a tight connection with 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 of the stirrer: a reactor with a stirrer for alkaline treatment of the initial vanadium-containing materials, connected to a tank for the preparation and supply of a sodium hydroxide solution, an ammonium metavanadate crystallizer tank, which has connections with a series-installed metering tank and a storage tank for preparation and supply of a solution of ammonium chloride; on the lid of the crystallizer tank there is a loading hatch in which the exit from the sodium chloride hopper is directed; after filter-1, an ammonium metavanadate recovery tank is installed, the lower discharge pipe of the suspension from which has a connection with filter-1 for separating the ammonium metavanadate precipitate from the suspension and washing it; calcining furnace for decomposition of NH ₄ VO ₃ to obtain marketable V ₂ O ₅ ; tank-collection of uterine solutions and promotion of ammonium metavanadate; a reactor for the neutralization and neutralization of vanadium-containing wastewater, connected through a dispenser to a collection tank of iron (II) -containing solutions and a tank for the preparation and supply of sodium hydroxide solution; a reactor for the neutralization and neutralization of vanadium-containing wastewater connected to a filter-2 to separate iron (II and III) oxyhydrates from the sludge 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 - "Hardware-technological line" according to the prototype is the lack of the necessary equipment to obtain 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 "System of technological equipment for the processing of vanadium oxytrichloride to produce commercial vanadium pentoxide."

The problem is solved with the achievement of the above technical result by the proposed utility model "System of technological equipment for the processing of vanadium oxytrichloride to obtain commercial vanadium pentoxide", including a reactor (1) with an agitator for alkaline treatment of vanadium oxytrichloride, hermetically connected to a transported tank (2) with the original technical vanadium oxytrichloride connected to a dispenser (3) and a tank for preparing and supplying a sodium hydroxide solution (4), a crystallization tank (5) ammonium tavanadate connected to an ammonium chloride dispenser (6-1) and a tank (6-2) for preparing an NPLtCl solution, a filter - 1 (7) for isolating and washing the ammonium metavanadate precipitate from the suspension, a recovery tank (8) an ammonium metavanadate precipitate connected to the filter - 1, a calcining furnace (9), a collection tank (10) of the mother liquor 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) ) with a collection tank (13) iron (II) -containing solutions, a dispenser (3) and a tank (4) for the preparation and supply of a sodium hydroxide solution, filter 2 (14) 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 the filter - 3 (15), the trough (16) of which the unloading and distribution device (17) is connected to the collector (18) of titanium cake - a precipitate of titanium oxyhydrate, exit

which is directed into a heated tank (19) with an agitator for repulping titanium cake, there is a pipe on the tank lid for connecting sodium hydroxide solution to the batcher (3), draining the pulp from the 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 the filter - 3 is directed to a prefabrication-averaging tank (19) connected to a reactor (1) for alkaline treatment of vanadium oxytrichloride, with a collection tank (10) of the mother liquor and ammonium metavanadate treatment filter trough - 2 have tons of connection with the loading unit (22) of the drying chamber (23) installed in series and the calcining furnace - 2 (24), the unloading unit of which has connections to the collection and metering hopper (25), the output of the calcined oxide deposit based on iron oxides ( III) and vanadium (V) is directed to the filling machine (26).

IMPLEMENTATION OF THE SUGGESTED USEFUL MODEL

The proposed technical solution - "System of technological equipment for the processing of vanadium oxytrichloride to obtain commercial 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 the reactor (1) with a mixer from a batcher (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) into a collector (18) from which the precipitate is sent to a heated tank (19) ) with a mixer 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 is not shown in the figure) to a filter-3 (15) solution of sodium metavanadate, purified from the precipitate - titanium oxyhydrate, from filter-3 (15) is collected in a collection-averaging tank (21), from which the combined and averaged the alkaline NaVO ₃ solution enters the reactor (1), the tank for the preparation of the sodium hydroxide solution (4) and the mother liquor collection tank and the ammonium metavanadate feed, the precipitate of titanium oxyhydrate on the filter-3 (15), if necessary, washed with sodium hydroxide and / or water, then this precipitate is discharged from filter-3 (15) into the trough (16) and through the unloading and 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 fed into the crystallizer tank (5) from the feed-storage tank - 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. can be used. 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). Washed (“washed” from sodium chloride) precipitate 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.

At the end of the calcination process, the obtained commercial vanadium pentoxide is discharged from the calcining furnace (9), packaged in a sealed container (bags) and shipped to consumers.

In order to neutralize all vanadium-containing wastewater formed from vanadium - mother liquors, industrial pumps, combined in the collection tank (10), they are pumped into the reactor (11), then, in this reactor, with the stirrer turned on, it is sequentially fed from the batcher

(12) and the collecting tank (13) a salt solution of ferrous iron - FeCl ₂ or FeSO _4, and then - from the dispenser (6-1) and the tank (6-2) solution of sodium hydroxide. The pulp in the reactor (11) is mixed and pumped onto filter-2 (14). The precipitate of iron oxyhydrates (II and III) containing vanadium recovered from the pulp is separated from the purified (neutralized) solution from vanadium chloride (NaCl, NH ₄ Cl), washed on the filter with water, the filtrate and wastewater are discharged into the sewer. The precipitate of iron oxyhydrate containing vanadium is discharged from filter-2 (14) into the trough (14.1) and then, through the loading unit (22), it is loaded into the drying chamber (23) installed in series - to dehydrate wet (40-80%) oxyhydrate (Fe -V) the precipitate, the dehydrated precipitate is then sent to the calcination furnace-2 (24), from which the calcined precipitate is iron oxide Fe ₂ O ₃ containing up to 5-10% V ₂ O _{5 is} discharged into the collection and metering hopper (25) , the exit from which is directed to the filling machine (26) for subsequent shipment to consumers at the Titanium Magnesium Plant for ore-thermal reduction smelting - together with ilmenite and / or ilmenorutil concentrate to produce cast iron and vanadium-enriched titanium slag, sent to the chlorination redistribution to obtain TiCI ₄ and technical VOCI ₄ containing TiCI ₄ .

HARDWARE AND TECHNOLOGICAL LINE FOR PROCESSING VANADIUM OXYTICHLORIDE FOR PRODUCING VANADIUM PENTAOXIDE FROM VANADIUM OXYTICHLORIDE

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

2 - transported container with the original technical vanadium oxytrichloride;

3 - dispenser of sodium hydroxide solution;

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

5 - crystallization tank of ammonium metavanadate;

6.1 - dispenser of a solution of ammonium chloride;

6.2 - tank for the preparation of a solution of ammonium chloride;

7 - filter (f-1) for separation of ammonium metavanadate from the suspension and washing it;

8 - tank-sedimentator sediment ammonium metavanadate;

9 - calcination furnace (PP-1);

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

11 - a reactor with a stirrer for neutralizing wastewater (effluent) water - mother liquors from vanadium and promoting ammonium metavanadate;

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

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

14 - filter-2 (filter press F-2) for the separation from the pulp of the precipitate of iron oxyhydrate with impurities of vanadium compounds;

14.1 - filter trough-2 for unloading and placing a wet precipitate of iron (III) oxyhydride with vanadium impurities;

15 - filter - 3 (filter press - 3) for isolation from the pulp - after alkaline treatment of technical vanadium oxytrichloride (VOCl ₃ + TiCl ₄ ), "titanium cake" - precipitate of titanium oxyhydrate with impurities of vanadium compounds (mainly NaVO ₃ );

16 - filter trough - 3;

17 - discharge - distribution device of the filter trough - 3;

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

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

20 - prefabricated - averaged capacity of sodium metavanadate solution;

21 is a collection tank of an alkaline solution of sodium metavanadate obtained after the repulpation of "titanium cake" - a precipitate of titanium oxyhydrate with impurities of vanadium compounds;

22 - loading node of the drying chamber (23);

23 - drying chamber (23) - for dehydration of wet (40-80%) sludge, with impurities of vanadium compounds;

shut-off and control switchgear;

24 - calcination furnace - 2 (PP-2) for heat treatment and calcination of the precipitate - based on iron oxide Fe ₂ O ₃ containing up to 5-10% V ₂ O ₅ ;

25 - prefabricated - dosing hopper of calcined sludge - based on iron oxide Fe ₂ O ₃ containing up to 5-10% V ₂ O ₅ ;

26 - filling machine oxide sludge to ensure the shipment of marketable products by the consumer.

Claims (1)

A system of technological equipment for processing vanadium oxytrichloride to produce vanadium pentoxide, including a reactor with a stirrer for alkaline treatment of vanadium oxytrichloride, hermetically connected to a transported tank of the initial technical vanadium oxytrichloride, connected in series with a batcher and a tank for the preparation and supply of sodium hydroxide solution, a metavanadate crystallizer tank ammonia connected to an ammonium chloride dispenser and a tank for preparing an NH ₄ Cl solution, filter-1 to isolate I am from a suspension of ammonium metavanadate sediment and washing it, a ammonium metavanadate sedimentation tank-changer connected to filter-1, a calcining furnace, a mother liquor collection tank and an ammonium metavanadate recovery vessel, a vanadium-containing wastewater neutralization and mother liquor treatment reactor ammonium connected through a dispenser to a collection tank of iron (II) -containing solutions, a dispenser and a tank for preparing and supplying a solution of sodium hydroxide, filter-2, to separate iron oxyhydrates from the pulp ( II and III) with vanadium impurities, characterized in that the lower discharge pipe of the reactor for alkaline treatment of vanadium oxytrichloride is directed through a pump and shut-off and control valves to filter-3, the trough of which is connected to a collector of titanium cake-precipitate of titanium oxyhydrate , the outlet of which is directed to a heated tank with an agitator for repulping titanium cake, there is a nozzle on the tank lid for connecting sodium hydroxide solution to the dispenser, draining the pulp from the tank through a pump avlen on filter-3, the output of the sodium metavanadate solution purified from the solid phase from the filter-3 is directed to a prefabricated-averaging vessel connected to the alkaline-treatment reactor for vanadium oxytrichloride, with a collection tank for the mother liquor and the passage of ammonium metavanadate, filter-2 connections with a loading unit, a drying chamber and a calcining furnace-2 installed in series, the unloading unit of which has connections to a collecting and metering hopper, the output of a calcined oxide deposit based on yellow oxides Sesa (III) and vanadium (V) are directed to the filling machine.