CN110054223B - Process and system for producing vanadium pentoxide by using waste furnace bricks - Google Patents
Process and system for producing vanadium pentoxide by using waste furnace bricks Download PDFInfo
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Abstract
A process and a system for producing vanadium pentoxide by using waste furnace bricks comprise: the process comprises a first-stage reaction tank, a high-level liquid storage tank, a filter press pump, a filter press, a belt conveyor, a second-stage reaction tank, a thickener and a vanadium precipitation tank, wherein the process comprises the following steps: adding a secondary leaching solution and industrial water into a primary reaction tank, adding waste furnace brick powder, adding a reactant for reaction to obtain a primary leaching solution, performing solid-liquid separation through a filter press to obtain a primary leaching solution, sending the primary leaching solution into a concentrator, overflowing supernatant of the concentrator into a vanadium precipitation tank, adding concentrated sulfuric acid into the vanadium precipitation tank to adjust the pH value, adding ammonium sulfate, continuously adding concentrated sulfuric acid to adjust the pH value, heating to a boiling reaction, performing solid-liquid separation on the reaction solution to obtain ammonium polyvanadate, and processing the ammonium polyvanadate into flaky vanadium pentoxide, wherein the vanadium content of the reaction solution is less than or equal to 0.2 g/L. The advantages are that: the vanadium solution is prepared by the reaction with the waste furnace bricks through a wet process, vanadium valuable elements are recovered, the solid waste furnace bricks are reused, and the method has leading and demonstration effects on energy conservation, emission reduction and development of circular economy.
Description
Technical Field
The invention belongs to the field of wet metallurgy, and particularly relates to a process and a system for producing vanadium pentoxide by using waste furnace bricks.
Background
In the process of producing vanadium pentoxide (flake) in domestic vanadium enterprises, high-quality ammonium polyvanadate or ammonium metavanadate is usually directly added into a melting furnace, ammonium polyvanadate or ammonium metavanadate is decomposed and melted at high temperature under 850-1150 ℃, and vanadium pentoxide liquid melted at high temperature is cooled and crystallized on a sheet casting machine to produce vanadium pentoxide (flake) products.
Because vanadium pentoxide (flake) is continuously produced at high temperature in a melting furnace, the working condition is relatively severe, the vanadium pentoxide belongs to an oxidizing and reducing amphoteric compound, clay bricks and high-alumina bricks of a furnace wall are severely eroded and washed for a long time through high-temperature molten liquid and radiant heat, the service life of the furnace wall is generally less than one year, and in extreme cases, the service life of the furnace wall is only as short as 5 months. In order to ensure the production requirement, at the moment, the furnace wall of the melting furnace needs to be dismantled, and a new furnace wall needs to be built again. After the furnace wall is dismantled, tens of tons of solid waste furnace bricks (V) without utilization value are generated2O53-16 percent of the total weight of the waste furnace bricks), the waste furnace bricks are usually required to be buried, and certain adverse effects are caused to the environment; few enterprises extract vanadium by roasting waste furnace bricks with a rotary kiln, but the process is complicated and high in cost, and smoke generated in the roasting process pollutes the environment.
Disclosure of Invention
The invention aims to solve the technical problem of providing a process and a system for producing vanadium pentoxide by using waste furnace bricks, wherein a vanadium solution is prepared by reacting with the waste furnace bricks through a wet process, valuable elements of vanadium are recovered, the solid waste furnace bricks are recycled, and the process and the system have leading and demonstration effects on energy conservation, emission reduction and development of circular economy.
The technical solution of the invention is as follows:
a process for producing vanadium pentoxide by using waste furnace bricks comprises the following specific steps:
(1) the method comprises the steps of adopting a waste furnace brick production system, opening a valve a at the bottom of a high-level liquid storage tank, adding a secondary leaching solution into a primary reaction tank, simultaneously opening a valve b of industrial water, supplementing normal-temperature industrial water, closing the valve a and the valve b, starting a stirring paddle on the primary reaction tank, opening a steam valve c, adding waste furnace brick powder, wherein the mass ratio of the total mass of the secondary leaching solution and the industrial water to the waste furnace brick powder is 3: 1-5: 1, adding a reactant, controlling the pH value to be 8.5-10.5, reacting at 70-95 ℃ for 120-180 min, closing the valve c when the analytic leaching solution is more than or equal to 20g/L and carrying out solid-liquid separation on the primary leaching solution through a filter press I to obtain a primary leaching solution and primary leaching slag; feeding the primary leaching solution into a thickener to obtain primary leaching slurry;
(2) opening an industrial water valve d, adding normal-temperature industrial water into a secondary reaction tank, closing the valve d, starting a stirring paddle of the secondary reaction tank, opening a steam valve e, returning primary leaching slag and primary leaching slurry into the secondary reaction tank from a discharge chute opening of a filter press I and a slurry outlet at the bottom of a thickener respectively, adding 3-5 times of the industrial water by mass as much as the primary leaching slag, adding a reactant, controlling the pH value to be 8.5-10.5, reacting at 70-95 ℃ for 60-90 min, analyzing vanadium contained in the secondary leaching slag by V2O5After the amount is less than or equal to 1.0 percent, carrying out solid-liquid separation on the secondary leaching solution through a filter press II to obtain a secondary leaching solution, and feeding the secondary leaching solution into a high-level liquid storage tank;
(3) overflowing the supernatant of the thickener into a vanadium precipitation tank, starting a stirring paddle of the vanadium precipitation tank, opening a concentrated sulfuric acid pipeline valve f, adding concentrated sulfuric acid into the vanadium precipitation tank, closing the valve f when the pH of the solution is 6, then adding ammonium sulfate according to the mass ratio of the mass of the ammonium sulfate to the mass of vanadium contained in the vanadium precipitation tank being 1.0: 1-1.2: 1, opening the concentrated sulfuric acid pipeline valve f, continuing to add the concentrated sulfuric acid, when the pH of the solution is 2, closing the valve f, opening a steam valve g, heating the solution to boiling, reacting for 35-60 min, analyzing and detecting that the vanadium content of the solution in the vanadium precipitation tank is less than or equal to 0.2g/L, closing the steam valve g, and carrying out solid-liquid separation on the vanadium precipitation solution through a filter press to obtain ammonium polyvanadate;
(4) decomposing and melting ammonium polyvanadate at 850-1150 ℃, and cooling and crystallizing the vanadium pentoxide molten liquid to obtain the flaky vanadium pentoxide product.
Further, in the step (1), the granularity of the waste furnace brick powder is 60-200 meshes, and the reactant is sodium carbonate or baking soda.
Further, in the step (2), the reactant is sodium carbonate or baking soda.
Further, the granularity of the waste furnace brick powder in the step (1) is 100-150 meshes, the reaction temperature is 80-90 ℃, the pH value is 9.0-9.5, and the reaction temperature in the step (2) is 80-90 ℃, and the pH value is controlled to be 9.0-9.5.
The utility model provides a system for produce vanadic anhydride with useless stove brick, includes one-level retort, thickener, second grade retort, heavy vanadium tank, its special character lies in: the liquid outlet of the first-stage reaction tank is communicated with the thickener through a pipeline, and a pressure filtration pump I and a pressure filter I are sequentially arranged on the pipeline between the first-stage reaction tank and the thickener; the liquid inlet of the first-stage reaction tank is communicated with the high-level liquid storage tank through a pipeline; an overflow port of the thickener is communicated with a vanadium precipitation tank through a pipeline, a liquid outlet at the bottom of the thickener is communicated with a secondary reaction tank through a pipeline, a liquid outlet of the secondary reaction tank is communicated with a high-level liquid storage tank through a pipeline, and a pressure filter pump II and a pressure filter II are sequentially arranged on the pipeline between the secondary reaction tank and the high-level liquid storage tank; a belt conveyor is arranged above a charging opening of the secondary reaction tank, a discharging slide opening of the belt conveyor is positioned right above the charging opening of the secondary reaction tank, and a discharging slide opening of the filter press I is positioned right above the belt conveyor; and a pressure filtration pump III and a pressure filter III are sequentially arranged on the outlet pipeline of the vanadium precipitation tank.
A valve a is arranged on a pipeline between the primary reaction tank and the high-level liquid storage tank; the top of the first-stage reaction tank is respectively connected with a first-stage reaction tank industrial water pipeline and a first-stage reaction tank steam pipeline, a valve b is arranged on the first-stage reaction tank industrial water pipeline, and a valve c is arranged on the first-stage reaction tank steam pipeline.
The top of the second-stage reaction tank is respectively connected with a second-stage reaction tank industrial water pipeline and a second-stage reaction tank steam pipeline, a valve d is arranged on the second-stage reaction tank industrial water pipeline, and a valve e is arranged on the second-stage reaction tank steam pipeline.
The top of the vanadium precipitation tank is respectively connected with a concentrated sulfuric acid pipeline and a vanadium precipitation tank steam pipeline, a valve f is arranged on the concentrated sulfuric acid pipeline, and a valve g is arranged on the vanadium precipitation tank steam pipeline.
The invention has the beneficial effects that:
(1) short process flow, convenient operation and good vanadium extraction effect.
The method has the advantages that the vanadium is extracted by utilizing the waste furnace bricks through wet reaction, dozens of sets of complex process equipment for extracting vanadium by using a rotary kiln fire method are greatly reduced, the vanadium extraction flow is short, the vanadium extraction equipment is few, and the vanadium extraction effect is better.
(2) The operation and maintenance cost is low, the energy consumption is low, and the unit cost is low.
The process and the system thereof do not need a rotary kiln to extract vanadium by a fire method, save a large amount of equipment, have low operation, maintenance and maintenance costs, save a large amount of fuel and electric power, do not discharge a large amount of flue gas generated by roasting in the rotary kiln, save energy and reduce emission, have low energy consumption and low unit cost.
(3) Harmful impurity ions are not generated in the leaching process, and the impurity removal process of the leaching solution is simple.
The process selects sodium carbonate or baking soda as a reactant, compared with acid-base leaching agents such as sulfuric acid, sodium hydroxide and the like, more harmful impurity ions such as silicon, iron, calcium, phosphorus, aluminum and the like are not generated in leaching solution, deep impurity removal is not needed in the leaching solution, the process is simple and practical, and impurity removal equipment is few.
Drawings
FIG. 1 is a schematic structural diagram of a system for producing vanadium pentoxide by using waste furnace bricks.
In the figure: 1-a first-stage reaction tank, 2-a high-level liquid storage tank, 3-a filter press pump I, 4-a filter press I, 5-a belt conveyor, 6-a second-stage reaction tank, 7-a filter press pump II, 8-a filter press II, 9-a concentrator, 10-a vanadium precipitation tank, 11-a filter press pump III, 12-a filter press III, 13-a first-stage reaction tank industrial water pipeline, 14-a first-stage reaction tank steam pipeline, 15-a second-stage reaction tank industrial water pipeline, 16-a second-stage reaction tank steam pipeline, 17-concentrated sulfuric acid pipeline and 18-a vanadium precipitation tank steam pipeline.
Detailed Description
Example 1
As shown in the figure, the process system for producing vanadium pentoxide by using waste furnace bricks comprises a first-stage reaction tank 1, wherein a liquid inlet of the first-stage reaction tank 1 is connected with a high-level liquid storage tank 2 through a pipeline, a liquid outlet of the first-stage reaction tank 1 is connected with a thickener 9 through a pipeline, and a pressure filtration pump I3 and a pressure filtration pump I4 are sequentially arranged on the pipeline between the first-stage reaction tank 1 and the thickener 9. An overflow port of the thickener 9 is connected with a vanadium precipitation tank 10 through a pipeline, and an outlet pipeline of the vanadium precipitation tank 10 is sequentially connected with a pressure filtration pump III 11 and a pressure filter III 12; a liquid outlet at the bottom of the thickener 9 is connected with a secondary reaction tank 6 through a pipeline, a liquid outlet of the secondary reaction tank 6 is communicated with the high-level liquid storage tank 2 through a pipeline, and a pressure filtration pump II 7 and a pressure filter II 8 are sequentially arranged on the pipeline between the secondary reaction tank 6 and the high-level liquid storage tank 2; a belt conveyor 5 is arranged above a charging opening of the secondary reaction tank 6, a discharging slide opening of the belt conveyor 5 is positioned right above the charging opening of the secondary reaction tank 6, and a discharging slide opening at the bottom of the filter press I4 is positioned right above the belt conveyor 5;
a valve a is arranged on a pipeline between the primary reaction tank 1 and the high-level liquid storage tank 2; the top of the primary reaction tank 1 is respectively connected with a primary reaction tank industrial water pipeline 13 and a primary reaction tank steam pipeline 14, the primary reaction tank industrial water pipeline 13 is provided with a valve b, and the primary reaction tank steam pipeline 14 is provided with a valve c;
the top of the secondary reaction tank 6 is respectively connected with a secondary reaction tank industrial water pipeline 15 and a secondary reaction tank steam pipeline 16, the secondary reaction tank industrial water pipeline 15 is provided with a valve d, and the secondary reaction tank steam pipeline 16 is provided with a valve e;
the top of the vanadium precipitation tank 10 is respectively connected with a concentrated sulfuric acid pipeline 17 and a vanadium precipitation tank steam pipeline 18, a valve f is arranged on the concentrated sulfuric acid pipeline 17, and a valve g is arranged on the vanadium precipitation tank steam pipeline 18.
The process system for producing vanadium pentoxide by using the waste furnace bricks has the following operation processes: before the process system is started, all valves are in a closed state;
(1) opening a valve a at the bottom of the high-level liquid storage tank 2, adding the secondary leaching solution into the primary reaction tank 1, and simultaneously opening an industrial water valveDoor b, adding normal temperature industrial water, closing the valve a and the valve b, starting the stirring paddle on the first-stage reaction tank 1, opening the steam valve c, and adding waste furnace brick powder (with the granularity of 60 meshes) in V2O514.5 percent in terms of weight), the mass ratio of the total mass of the secondary leaching solution and the industrial water to the waste furnace brick powder is 3:1, soda is added, the reaction temperature is 95 ℃, the pH value is controlled to be 10.5 through the addition amount of the soda, the leaching solution is analyzed to contain vanadium for 120min to be 23.1g/L, a valve c is closed, the primary leaching solution is subjected to solid-liquid separation through a filter press I4, and primary leaching solution and primary leaching slag are obtained; feeding the primary leaching solution into a thickener 9 to obtain primary leaching slurry;
(2) opening an industrial water valve d, adding normal-temperature industrial water into a secondary reaction tank 6, closing the valve d, starting a stirring paddle of the secondary reaction tank 6, opening a steam valve e, returning primary leaching slag and primary leaching slurry into the secondary reaction tank 6 through a discharge chute of a filter press I4 and a slurry outlet at the bottom of a thickener 9 respectively, wherein the adding mass of the industrial water is 3 times of that of the primary leaching slag, adding sodium bicarbonate, controlling the pH value to be 8.5 through the adding amount of the sodium bicarbonate, reacting at the temperature of 95 ℃ for 90min, analyzing vanadium (V) contained in the secondary leaching slag2O50.9 percent of the total weight of the leaching solution, performing solid-liquid separation on the secondary leaching solution through a filter press II 8, and feeding the secondary leaching solution into a high-level liquid storage tank 2;
(3) overflowing the supernatant of the thickener 9 into a vanadium precipitation tank 10, starting a stirring paddle of the vanadium precipitation tank 10, and enabling the volume of the solution to be 15m3Analyzing a solution containing 22.8g/L of vanadium, opening a concentrated sulfuric acid pipeline valve f, adding concentrated sulfuric acid into a vanadium precipitation tank 10, adding ammonium sulfate according to the mass ratio of the ammonium sulfate to the vanadium (by weight of the vanadium) in the vanadium precipitation tank 10 of 1.0:1 when the pH value of the solution is 6, opening the concentrated sulfuric acid pipeline valve f, continuously adding concentrated sulfuric acid, closing the valve f when the pH value of the solution is 2, opening a steam valve g, heating the solution to boiling, reacting for 35min, analyzing and detecting that the solution in the vanadium precipitation tank 10 contains 0.2g/L of vanadium, closing the steam valve g, and performing solid-liquid separation on the vanadium precipitation solution through a filter press III 12 to obtain ammonium polyvanadate (V)2O5 98.4％、Si 0.1％、Fe 0.12％、P 0.012％)；
(4) Decomposing and melting ammonium polyvanadate at 1150 deg.C, cooling and crystallizing vanadium pentoxide molten liquidObtaining vanadium pentoxide (flake) product (V)2O5 98.2％、Si 0.16％、Fe 0.17％、P 0.013％)。
Example 2
The system for producing vanadium pentoxide by using waste furnace bricks is the same as that in example 1.
The process system for producing vanadium pentoxide by using the waste furnace bricks has the following operation processes: before the process system is started, all valves are in a closed state;
(1) opening a valve a at the bottom of a high-level liquid storage tank 2, adding a secondary leaching solution into a primary reaction tank 1, simultaneously opening an industrial water valve b, adding normal-temperature industrial water, closing the valve a and the valve b, starting a stirring paddle on the primary reaction tank 1, opening a steam valve c, and adding waste furnace brick powder (V in particle size of 200 meshes)2O513.2 percent in terms of mass ratio, the mass ratio of the total mass of the secondary leaching solution and the industrial water to the waste furnace brick powder is 5:1, baking soda is added, the reaction temperature is 70 ℃, the time is 180min, the pH value is controlled to be 8.5 through the addition amount of soda, the leaching solution is analyzed to contain 21.3g/L of vanadium, a valve c is closed, and the primary leaching solution is subjected to solid-liquid separation through a filter press I4 to obtain primary leaching solution and primary leaching slag; feeding the primary leaching solution into a thickener 9 to obtain primary leaching slurry;
(2) opening an industrial water valve d, adding normal-temperature industrial water into a secondary reaction tank 6, closing the valve d, starting a stirring paddle of the secondary reaction tank 6, opening a steam valve e, returning primary leaching slag and primary leaching slurry into the secondary reaction tank 6 through an I4 discharge chute and a slurry outlet at the bottom of a thickener 9 respectively, wherein the adding mass of the industrial water is 5 times of that of the primary leaching slag, adding sodium bicarbonate, controlling the pH value to be 10.5 by the adding amount of the sodium bicarbonate, reacting at the temperature of 70 ℃ for 60min, analyzing vanadium (V) contained in the secondary leaching slag2O50.8 percent of the total weight of the leaching solution, performing solid-liquid separation on the secondary leaching solution through a filter press II 8, and feeding the secondary leaching solution into a high-level liquid storage tank 2;
(3) overflowing the supernatant of the thickener 9 into a vanadium precipitation tank 10, starting a stirring paddle of the vanadium precipitation tank 10, and enabling the volume of the solution to be 20m3Analyzing the solution containing 20.5g/L vanadium, opening a concentrated sulfuric acid pipeline valve f, adding concentrated sulfuric acid into the vanadium precipitation tank 10, and when the pH value of the solution is 6, adding ammonium sulfate andadding ammonium sulfate into a vanadium precipitation tank 10, opening a concentrated sulfuric acid pipeline valve f, continuously adding concentrated sulfuric acid, closing the valve f when the pH value of the solution is 2, opening a steam valve g, heating the solution to boiling, reacting for 60min, analyzing and detecting that the solution in the vanadium precipitation tank 10 contains vanadium 0.10g/L, closing the steam valve g, and carrying out solid-liquid separation on the vanadium precipitation solution through a filter press III 12 to obtain ammonium polyvanadate (V)2O5 98.9％、Si 0.06％、Fe 0.14％、P 0.016％)；
(4) Decomposing and melting ammonium polyvanadate at 900 ℃, cooling and crystallizing vanadium pentoxide molten liquid to obtain vanadium pentoxide (sheet) product (V)2O5 98.7％、Si 0.10％、Fe 0.20％、P 0.016％)。
Example 3
The system for producing vanadium pentoxide by using waste furnace bricks is the same as that in example 1.
The process system for producing vanadium pentoxide by using the waste furnace bricks has the following operation processes: before the process system is started, all valves are in a closed state;
(1) opening a valve a at the bottom of a high-level liquid storage tank 2, adding a secondary leaching solution into a primary reaction tank 1, simultaneously opening an industrial water valve b, adding normal-temperature industrial water, closing the valve a and the valve b, starting a stirring paddle on the primary reaction tank 1, opening a steam valve c, and adding waste furnace brick powder (V in particle size) with the particle size of 100 meshes2O515.3 percent of the total mass of the secondary leaching solution and the industrial water and the mass ratio of the waste furnace brick powder is 4:1, adding soda ash, reacting at 80 ℃, controlling the pH value to be 9.5 by the addition amount of the soda ash, reacting for 150min, analyzing the leaching solution containing 24.1g/L of vanadium, closing a valve c, and carrying out solid-liquid separation on the primary leaching solution through a filter press I4 to obtain primary leaching solution and primary leaching slag; feeding the primary leaching solution into a thickener 9 to obtain primary leaching slurry;
(2) opening an industrial water valve d, adding normal-temperature industrial water into the secondary reaction tank 6, closing the valve d, starting a stirring paddle of the secondary reaction tank 6, opening a steam valve e, and returning the primary leaching slag and the primary leaching slurry into the secondary reaction tank 6 through the I4 discharge chute port and the slurry outlet at the bottom of the thickener 9 respectively, wherein the adding quality of the industrial water is that the primary leaching slurry is addedAdding sodium bicarbonate 4 times the weight of the leaching residue, controlling pH value to 9.5 by the addition amount of the sodium bicarbonate, reacting at 85 deg.C for 80min, and analyzing vanadium (V) contained in the secondary leaching residue2O50.7 percent of the total weight of the leaching solution, performing solid-liquid separation on the secondary leaching solution by a filter press II 8, and feeding the secondary leaching solution into a high-level liquid storage tank 2;
(3) overflowing the supernatant of the thickener 9 into a vanadium precipitation tank 10, starting a stirring paddle of the vanadium precipitation tank 10, and enabling the volume of the solution to be 15m3Analyzing solution containing 24.0g/L of vanadium, opening a concentrated sulfuric acid pipeline valve f, adding concentrated sulfuric acid into a vanadium precipitation tank 10, when the pH value of the solution is 6, adding ammonium sulfate into the vanadium precipitation tank 10 according to the mass ratio of the ammonium sulfate to vanadium (by weight of the vanadium) in 1.1:1, opening a concentrated sulfuric acid pipeline valve f, continuously adding concentrated sulfuric acid, when the pH value of the solution is 2, closing the valve f, opening a steam valve g, heating the solution to boiling, reacting for 50min, analyzing and detecting that the solution in the vanadium precipitation tank 10 contains 0.18g/L of vanadium, closing the steam valve g, and performing solid-liquid separation on the vanadium precipitation solution through a filter press III 12 to obtain ammonium polyvanadate (V is vanadium) (the content is 24.0 g/L)2O5 99.2％、Si 0.06％、Fe 0.06％、P 0.011％)；
(4) Decomposing and melting ammonium polyvanadate at 850 ℃, cooling and crystallizing vanadium pentoxide molten liquid to obtain vanadium pentoxide (flake) product (V)2O5 98.92％、Si 0.08％、Fe 0.09％、P 0.011％)。
Example 4
The system for producing vanadium pentoxide by using waste furnace bricks is the same as that in example 1.
The process system for producing vanadium pentoxide by using the waste furnace bricks has the following operation processes: before the process system is started, all valves are in a closed state;
(1) opening a valve a at the bottom of a high-level liquid storage tank 2, adding a secondary leaching solution into a primary reaction tank 1, simultaneously opening an industrial water valve b, adding normal-temperature industrial water, closing the valve a and the valve b, starting a stirring paddle on the primary reaction tank 1, opening a steam valve c, and adding waste furnace brick powder (with the particle size of 150 meshes in V)2O515.6 percent of the total mass of the secondary leaching solution and the industrial water and the mass ratio of the waste furnace brick powder is 4:1, adding sodium bicarbonate, reacting at the temperature of 90 ℃, controlling the pH value to be 9.0 by the addition of soda ash, and reactingAnalyzing the leaching solution containing vanadium for 130min, closing a valve c, and carrying out solid-liquid separation on the primary leaching solution through a filter press I4 to obtain a primary leaching solution and primary leaching slag; feeding the primary leaching solution into a thickener 9 to obtain primary leaching slurry;
(2) opening an industrial water valve d, adding normal-temperature industrial water into a secondary reaction tank 6, closing the valve d, starting a stirring paddle of the secondary reaction tank 6, opening a steam valve e, returning primary leaching slag and primary leaching slurry into the secondary reaction tank 6 through an I4 discharge chute and a slurry outlet at the bottom of a thickener 9 respectively, wherein the adding mass of the industrial water is 3.5 times of that of the primary leaching slag, adding sodium carbonate, controlling the pH value to be 9.0 by the adding amount of the sodium carbonate, reacting at the temperature of 90 ℃ for 80min, analyzing vanadium (V) contained in the secondary leaching slag2O50.7 percent of the total weight of the leaching solution, performing solid-liquid separation on the secondary leaching solution by a filter press II 8, and feeding the secondary leaching solution into a high-level liquid storage tank 2;
(3) overflowing the supernatant of the thickener 9 into a vanadium precipitation tank 10, starting a stirring paddle of the vanadium precipitation tank 10, and enabling the volume of the solution to be 15m3Analyzing a solution containing 22.8g/L of vanadium, opening a concentrated sulfuric acid pipeline valve f, adding concentrated sulfuric acid into a vanadium precipitation tank 10, when the pH value of the solution is 6, adding ammonium sulfate into the vanadium precipitation tank 10 according to the mass ratio of the ammonium sulfate to the vanadium (by the weight of the vanadium) in 1.0:1, opening a concentrated sulfuric acid pipeline valve f, continuously adding concentrated sulfuric acid, when the pH value of the solution is 2, closing the valve f, opening a steam valve g, heating the solution to boiling, reacting for 45min, analyzing and detecting that the vanadium content of the solution in the vanadium precipitation tank 10 is 0.19g/L, closing the steam valve g, and performing solid-liquid separation on the vanadium precipitation solution through a filter press III 12 to obtain ammonium polyvanadate (V is vanadium-containing)2O5 98.9％、Si 0.09％、Fe 0.07％、P 0.008％)；
(4) Decomposing and melting ammonium polyvanadate at 1000 ℃, cooling and crystallizing vanadium pentoxide molten liquid to obtain vanadium pentoxide (sheet) product (V)2O5 98.7％、Si 0.12％、Fe 0.13％、P 0.011％)。
The above description is only exemplary of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A process for producing vanadium pentoxide by using waste furnace bricks is characterized by comprising the following steps:
the method comprises the following specific steps:
(1) the system for producing the vanadium pentoxide by adopting the waste furnace bricks comprises a primary reaction tank, a thickener, a secondary reaction tank and a vanadium precipitation tank, wherein a liquid outlet of the primary reaction tank is communicated with the thickener through a pipeline, and a pressure filtration pump I and a pressure filter I are sequentially arranged on the pipeline between the primary reaction tank and the thickener; the liquid inlet of the first-stage reaction tank is communicated with the high-level liquid storage tank through a pipeline; an overflow port of the thickener is communicated with a vanadium precipitation tank through a pipeline, a liquid outlet at the bottom of the thickener is communicated with a secondary reaction tank through a pipeline, a liquid outlet of the secondary reaction tank is communicated with a high-level liquid storage tank through a pipeline, and a pressure filter pump II and a pressure filter II are sequentially arranged on the pipeline between the secondary reaction tank and the high-level liquid storage tank; a belt conveyor is arranged above a charging opening of the secondary reaction tank, a discharging slide opening of the belt conveyor is positioned right above the charging opening of the secondary reaction tank, and a discharging slide opening of the filter press I is positioned right above the belt conveyor; a pressure filtration pump III and a pressure filter III are sequentially arranged on the outlet pipeline of the vanadium precipitation tank;
opening a valve a at the bottom of a high-level liquid storage tank, adding a secondary leaching solution into a primary reaction tank, simultaneously opening an industrial water valve b, supplementing normal-temperature industrial water, closing the valve a and the valve b, starting a stirring paddle on the primary reaction tank, opening a steam valve c, adding waste furnace brick powder, controlling the mass ratio of the total mass of the secondary leaching solution and the industrial water to the mass of the waste furnace brick powder to be 3: 1-5: 1, adding a reactant, controlling the pH value to be 8.5-10.5, reacting at 70-95 ℃ for 120-180 min, closing the valve c when the analytic leaching solution contains more than or equal to 20g/L of vanadium, and carrying out solid-liquid separation on the primary leaching solution through a filter press I to obtain a primary leaching solution and primary leaching slag; feeding the primary leaching solution into a thickener to obtain primary leaching slurry;
the granularity of the waste furnace brick powder is 60-200 meshes, and the reactant is sodium carbonate or baking soda;
(2) opening an industrial water valve d, adding normal-temperature industrial water into a secondary reaction tank, closing the valve d, starting a stirring paddle of the secondary reaction tank, opening a steam valve e, returning primary leaching slag and primary leaching slurry into the secondary reaction tank from a discharge chute opening of a filter press I and a slurry outlet at the bottom of a thickener respectively, adding 3-5 times of the industrial water by mass as much as the primary leaching slag, adding a reactant, controlling the pH value to be 8.5-10.5, reacting at 70-95 ℃ for 60-90 min, analyzing vanadium contained in the secondary leaching slag by V2O5After the amount is less than or equal to 1.0 percent, carrying out solid-liquid separation on the secondary leaching solution through a filter press II to obtain a secondary leaching solution, and feeding the secondary leaching solution into a high-level liquid storage tank;
the reactant is sodium carbonate or baking soda;
(3) overflowing the supernatant of the thickener into a vanadium precipitation tank, starting a stirring paddle of the vanadium precipitation tank, opening a concentrated sulfuric acid pipeline valve f, adding concentrated sulfuric acid into the vanadium precipitation tank, closing the valve f when the pH of the solution is 6, then adding ammonium sulfate according to the mass ratio of the mass of the ammonium sulfate to the mass of vanadium contained in the vanadium precipitation tank being 1.0: 1-1.2: 1, opening the concentrated sulfuric acid pipeline valve f, continuing to add the concentrated sulfuric acid, when the pH of the solution is 2, closing the valve f, opening a steam valve g, heating the solution to boiling, reacting for 35-60 min, analyzing and detecting that the vanadium content of the solution in the vanadium precipitation tank is less than or equal to 0.2g/L, closing the steam valve g, and carrying out solid-liquid separation on the vanadium precipitation solution through a filter press to obtain ammonium polyvanadate;
(4) decomposing and melting ammonium polyvanadate at 850-1150 ℃, and cooling and crystallizing the vanadium pentoxide molten liquid to obtain the flaky vanadium pentoxide product.
2. The process for producing vanadium pentoxide from waste furnace bricks as claimed in claim 1, wherein: the granularity of the waste furnace brick powder in the step (1) is 100-150 meshes, the reaction temperature is 80-90 ℃, the pH value is 9.0-9.5, and the reaction temperature in the step (2) is 80-90 ℃, and the pH value is controlled to be 9.0-9.5.
3. The process for producing vanadium pentoxide from waste furnace bricks as claimed in claim 1, wherein: a valve a is arranged on a pipeline between the primary reaction tank and the high-level liquid storage tank; the top of the first-stage reaction tank is respectively connected with a first-stage reaction tank industrial water pipeline and a first-stage reaction tank steam pipeline, a valve b is arranged on the first-stage reaction tank industrial water pipeline, and a valve c is arranged on the first-stage reaction tank steam pipeline.
4. The process for producing vanadium pentoxide from waste furnace bricks as claimed in claim 1, wherein: the top of the second-stage reaction tank is respectively connected with a second-stage reaction tank industrial water pipeline and a second-stage reaction tank steam pipeline, a valve d is arranged on the second-stage reaction tank industrial water pipeline, and a valve e is arranged on the second-stage reaction tank steam pipeline.
5. The process for producing vanadium pentoxide from waste furnace bricks as claimed in claim 1, wherein: the top of the vanadium precipitation tank is respectively connected with a concentrated sulfuric acid pipeline and a vanadium precipitation tank steam pipeline, a valve f is arranged on the concentrated sulfuric acid pipeline, and a valve g is arranged on the vanadium precipitation tank steam pipeline.
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| CN1724405A (en) * | 2005-06-28 | 2006-01-25 | 贵州宏福实业开发有限总公司 | Process for treating and controlling acid waste water containing fluorine |
| CN1752021A (en) * | 2004-09-24 | 2006-03-29 | 刘亚光 | Method of producing ranadium pentoxide using vanadium containing waste catalyst |
| CN101898793A (en) * | 2010-07-28 | 2010-12-01 | 攀钢集团冶金工程技术有限公司 | Leaching method of vanadium-containing clinker |
| CN106399694A (en) * | 2016-10-08 | 2017-02-15 | 河钢股份有限公司承德分公司 | Method for synchronously extracting vanadium and aluminum from waste vanadium oxide smelter refractory brick |
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| CN1752021A (en) * | 2004-09-24 | 2006-03-29 | 刘亚光 | Method of producing ranadium pentoxide using vanadium containing waste catalyst |
| CN1724405A (en) * | 2005-06-28 | 2006-01-25 | 贵州宏福实业开发有限总公司 | Process for treating and controlling acid waste water containing fluorine |
| CN101898793A (en) * | 2010-07-28 | 2010-12-01 | 攀钢集团冶金工程技术有限公司 | Leaching method of vanadium-containing clinker |
| CN106399694A (en) * | 2016-10-08 | 2017-02-15 | 河钢股份有限公司承德分公司 | Method for synchronously extracting vanadium and aluminum from waste vanadium oxide smelter refractory brick |
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Effective date of registration: 20211217 Address after: 121000 Taihe 59, Taihe District, Jinzhou, Liaoning Patentee after: Jinzhou Vanadium Industry Co.,Ltd. Address before: 121005 alloy No. 59, Taihe District, Liaoning, Jinzhou Patentee before: CITIC JINZHOU METAL Co.,Ltd. |