CN110467222B - Method for preparing vanadium pentoxide - Google Patents
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Abstract
A method for preparing vanadium pentoxide belongs to the field of vanadium pentoxide production, and comprises the following steps: (A) pouring the ore pulp into a reaction kettle, stirring along the middle to form a pit, pouring concentrated sulfuric acid into the pit, uniformly stirring, and curing at constant temperature to obtain a first reactant; (B) the first reactant is subjected to multi-stage countercurrent leaching separation to obtain a solid phase and a liquid phase; (C) adding ammonium bicarbonate into the liquid phase, and performing solid-liquid separation to obtain a first solution; (D) adding an oxidant into the first solution for oxidation, carrying out ion exchange enrichment on the first solution to obtain a second solution, and eluting the second solution by using a sodium hydroxide solution to obtain an eluent; (E) adding a magnesium chloride solution into the eluent to obtain a third solution; (F) and adding ammonium sulfate into the third solution, performing centrifugal separation to obtain ammonium metavanadate, and finally performing decomposition reaction on the ammonium metavanadate to obtain vanadium pentoxide.
Description
Technical Field
The invention relates to the field of vanadium pentoxide production, in particular to a method for preparing vanadium pentoxide.
Background
Vanadium is a non-ferrous metal, and vanadium pentoxide is widely used in the industries of metallurgy, chemical industry and the like, and is mainly used for smelting ferrovanadium. The catalyst is used as an alloy additive and accounts for more than 80 percent of the total consumption of vanadium pentoxide, is used as a catalyst of organic chemical engineering, namely a catalyst, and accounts for about 10 percent of the total amount, and is used as an inorganic chemical, a chemical reagent, enamel, a magnetic material and the like in other places, and accounts for about 10 percent of the total amount.
At present, two methods for extracting vanadium pentoxide from stone coal by using sulfuric acid are mainly used, one method is a dilute acid heating extraction method, the production period of the method is long, 9-12 hours are needed, the energy consumption is high, and the impurities in an extracting solution are more; the other method is a solid mineral powder mixed concentrated acid heap leaching method, the method has longer period, needs at least 5-7 days, occupies large production area, and has severe production environment and great pollution.
For example, application numbers are: CN201410520118.7 discloses a method for preparing vanadium pentoxide, which comprises crushing and grinding dry stone coal with low water content to 80 meshes, mixing with concentrated sulfuric acid and water in a certain proportion, and directly heap leaching in open air. Fermenting at constant temperature for 7-10 days, adding water, leaching, and performing solid-liquid separation. Obtaining pickle liquor containing vanadium. Adding ammonium bicarbonate into the vanadium-containing pickle liquor to prepare ammonium alum, and removing aluminum. Then the separation liquid is subjected to ion exchange to enrich vanadium in the solution. After being eluted by alkali liquor, the ammonium metavanadate is prepared by removing impurities and adding ammonium chloride or ammonium sulfate, and finally vanadium pentoxide is obtained by high-temperature calcination.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides the method for preparing the vanadium pentoxide, which can eliminate dust pollution, reduce the production cost and has short production period.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing vanadium pentoxide comprises the following steps:
(A) grinding stone coal by a wet grinding ball mill, simultaneously controlling the water addition amount to obtain ore pulp containing 30-40% of water, pouring the ore pulp into a reaction kettle, stirring along the middle to form a pit, pouring concentrated sulfuric acid into the pit, uniformly stirring, and curing at constant temperature for 4-6 h to obtain a first reactant;
(B) carrying out multi-stage countercurrent leaching separation on the first reactant at normal temperature to obtain a solid phase and a liquid phase, wherein the solid phase is ore tailings with the water content of less than 20% by mass, and the liquid phase is a vanadium-containing acid solution;
(C) adding a certain amount of ammonium bicarbonate or ammonium sulfate into the liquid phase, and performing solid-liquid separation to obtain ammonium alum crystals and a first solution;
(D) adjusting the pH value of the first solution to 2.0-2.5, adding an oxidant for oxidation, and performing ion exchange enrichment to obtain a vanadium-containing barren solution and a second solution, wherein the second solution is an eluent obtained by eluting with a sodium hydroxide solution;
(E) adjusting the pH value of the second solution to 8.5-9.5, and adding the second solution in a mass ratio of 1: reacting 0.12 of 20% magnesium chloride solution at the temperature of 80-100 ℃ for 2 hours, and filtering to obtain a third solution;
(F) adding vanadium to ammonium in a molar ratio of 1: 1.2, stirring and reacting for 2 hours at the temperature of 40-60 ℃, centrifugally separating to obtain ammonium metavanadate and vanadium precipitation mother liquor, and finally, carrying out decomposition reaction on the ammonium metavanadate to obtain vanadium pentoxide.
The method is between two methods in the prior art, concentrated sulfuric acid and ore pulp are cured in a reaction kettle, the curing time is short, wet grinding is adopted, and the concentrated sulfuric acid and the ore pulp are cured in the reaction kettle, so that no dust is generated; the ore pulp is stirred to form a pit at the center of the ore pulp, and the pit is used for pouring concentrated sulfuric acid, so that the concentrated sulfuric acid cannot be sputtered when being added, and the mixing of the concentrated sulfuric acid and the ore pulp can be accelerated; multistage countercurrent leaching refers to a process in which multistage leaching is carried out in a multistage series of equipment. Each stage includes a primary leaching chamber and a secondary leaching chamber. The solid phase is provided in the leaching chamber for contact with a leaching agent which is releached when in contact with the receiver in the releaching chamber. The leachant is suitably cross-flowed in the same stage to the donor and acceptor phases, with the donor and acceptor phases being counter-flowed through some or all of the stages, and multi-stage counter-current leaching is known in the art and will not be described in any greater detail herein.
The first solution, the second solution and the third solution are all vanadium-containing solutions, and the ion exchange equipment is an ion exchange column, which is a columnar pressure container for carrying out ion exchange reaction and is exchange equipment for ion exchange by a column method. Is often used in laboratories and industry. The method can be divided into three types of in-vivo regeneration mixed bed, in-vitro regeneration mixed bed and anion resin outward transfer regeneration mixed bed according to a regeneration mode, and can be divided into a laboratory ion exchange column and an industrial ion exchange column in the application range, wherein the ion exchange column can generate two solutions, one is a saturated second solution, the other is a vanadium-containing barren solution, the vanadium-containing barren solution contains a large amount of metal impurities, and the vanadium-containing barren solution can be returned to the step (A) for water use after further reaction.
Further, in the step (A), the stone coal is ground to be smaller than 100 meshes by a wet grinding ball mill, the grinding can reduce the curing time, and under the condition of a certain temperature, the curing time of the stone coal is shorter as the stone coal is smaller within a range smaller than 100 meshes, and when the stone coal is larger than 100 meshes, the curing time of the stone coal is certain and is not reduced as the stone coal becomes smaller.
Further, the ore pulp and concentrated sulfuric acid in the step (A) are cured for 5-6 hours at the temperature of 110-120 ℃ to obtain a first reactant.
Further, the ore pulp containing 30% -40% of water in the step (A) is processed through a ceramic filter to obtain 15% -20% of wet ore powder, the wet ore powder and concentrated sulfuric acid are cured for 4-5 hours at the temperature of 120-130 ℃ to obtain a first reactant, the ceramic filter is the prior art, redundant description is omitted, and the curing time of water in the ore pulp in the subsequent curing process can be further shortened.
Further, the molar ratio of ammonium ions in the ammonium bicarbonate or ammonium sulfate added in the step (C) to aluminum ions in the liquid phase is 1.2-1.5: 1, Al in liquid phase2（SO4）3Is easy to react with Na+，K+，NH4 +Plasma generates composite salt, so ammonium bicarbonate or ammonium sulfate is added into liquid phase, and the ammonium bicarbonate or ammonium sulfate can be mixed with Al2（SO4）3Reacting to generate aluminum ammonium sulfate, cooling and crystallizing the aluminum ammonium sulfate to obtain the ammonium alum, wherein the molecular formula of the ammonium alum is as follows: NH (NH)4Al（SO4）2·12H2O, so that the molar ratio of the added ammonium ions to the aluminum ions in the liquid phase is preferably 1.2-1.5: 1 ensures the reaction is complete.
And (3) further, adding calcium oxide into the vanadium-containing barren solution enriched by the ion exchange column in the step (D), adjusting the pH value to 6.0-7.0, returning to the multi-stage countercurrent leaching in the step (B) for recycling, wherein the cured first reactant is in a solid-liquid mixed viscous state, and the treated vanadium-containing barren solution can dilute the first reactant, promote partial dissolution and facilitate the multi-stage countercurrent leaching.
Further, after deamination is performed on the vanadium precipitation mother liquor obtained by centrifugal separation in the step (F) through a degassing membrane, returning to the ore grinding link in the step (A) for application, wherein the vanadium precipitation mother liquor is only water actually and contains a part of ammonia, and the ammonia in the vanadium precipitation mother liquor is removed through the degassing membrane and can be returned to the step (A) for use as water; the degassing membrane is a membrane separation product for removing gases in liquid, such as carbon dioxide, oxygen and ammonia nitrogen, by using the principle of diffusion. The degassing membrane contains a large number of hollow fibers, the walls of which have tiny pores through which water molecules cannot pass, but through which gas molecules can pass. When the degassing device works, water flows through the hollow fibers under certain pressure, and the gas is continuously pumped away from the outside of the hollow fibers under the action of the vacuum pump to form certain negative pressure, so that the gas in the water continuously overflows from the water through the hollow fibers, the aim of removing the gas in the water is fulfilled, and the degassing membrane is internally provided with a large number of hollow fibers so as to enlarge the area of a gas-liquid interface and accelerate the degassing speed.
Further, in the step (F), a calcination manner is adopted for decomposition reaction of ammonium metavanadate, the calcination temperature is 500-550 ℃, the reaction time is 2-3 hours, the ammonium metavanadate is decomposed to generate vanadium pentoxide, water and ammonia gas, and calcination of ammonium metavanadate to prepare vanadium pentoxide is prior art and is not described herein in detail.
Further, in the step (F), an electric heating mode is adopted for decomposition reaction of ammonium metavanadate, the ammonium metavanadate is decomposed to generate vanadium pentoxide, water and ammonia gas, and the preparation of the vanadium pentoxide by electric heating is more environment-friendly.
And (3) further, absorbing ammonia gas generated by decomposing the ammonium metavanadate with sulfuric acid to obtain ammonium sulfate salt, dissolving the ammonium sulfate salt, returning the dissolved ammonium sulfate salt to the step (F) to react with the third solution, and recycling the generated ammonia gas to prevent the generation of waste gas.
The invention has the beneficial effects that: according to the invention, the ore pulp with a certain water content is pumped into the reaction kettle, the center of the ore pulp is stirred to form a pit, concentrated sulfuric acid is added, and the pit is cured at a certain temperature under stirring, so that the whole production period is greatly shortened, the sealing operation is carried out, and the continuous production is realized; continuous multi-stage countercurrent leaching is adopted, the efficiency is high, the operation is convenient, the cost is reduced, the labor intensity is reduced, and the operation environment is greatly improved.
The lean solution containing vanadium and the vanadium precipitation mother solution generated by the method can be returned to a system for cyclic utilization after being treated, so that the whole method does not generate wastewater, and the environmental pollution is reduced; the ammonia gas generated by decomposing the ammonium metavanadate to prepare the vanadium pentoxide reacts with the sulfuric acid to obtain ammonium sulfate salt, and the ammonium sulfate salt can be returned to the system for cyclic utilization after being dissolved, so that the whole method does not generate waste gas, and the atmospheric pollution is reduced.
At present, the mining is generally carried out by adopting hole mining, mineral aggregates are wet aggregates with high water content, and the invention can directly carry out wet grinding by the wet aggregates without dehumidification, thereby reducing investment, eliminating dust pollution and lowering production cost; the ore pulp is cured in the reaction kettle to replace the original open-air heap leaching fermentation, so that the problems of large occupied area, long working time, environmental pollution and the like are solved, and the production cost is reduced.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The method for preparing vanadium pentoxide comprises the following steps:
step (A): grinding stone coal by a wet grinding ball mill to be smaller than 100 meshes, simultaneously controlling the water addition amount to obtain ore pulp containing 40% of water, pouring the ore pulp into a reaction kettle, stirring at the center to form a pit, adding concentrated sulfuric acid into the pit, uniformly stirring, curing at constant temperature for 6 hours, and obtaining a first reactant, wherein the temperature is 120 ℃;
step (B): carrying out multi-stage countercurrent leaching separation on the first reactant at normal temperature to obtain a solid phase and a liquid phase, wherein the solid phase is ore tailings with the water content of less than 20% by mass, and the liquid phase is a vanadium-containing acid solution;
step (C): adding a certain amount of ammonium bicarbonate or ammonium sulfate into the liquid phase, wherein the molar ratio of ammonium ions to aluminum ions in the liquid phase is 1.2-1.5: 1, obtaining ammonium alum crystals and a first solution through solid-liquid separation;
step (D): adjusting the pH value of the first solution to 2.0-2.5, adding an oxidant for oxidation, and performing ion exchange enrichment to obtain a vanadium-containing barren solution and a second solution, wherein the second solution is an eluent obtained by eluting with a sodium hydroxide solution; adding calcium oxide into the vanadium-containing barren solution, adjusting the pH value to 6.0-7.0, and returning to the multi-stage countercurrent leaching in the step (B) for recycling;
a step (E): adjusting the pH value of the second solution to 8.5-9.5, and adding the second solution in a mass ratio of 1: reacting 0.12 of 20% magnesium chloride solution at the temperature of 80-100 ℃ for 2 hours, and filtering to obtain a third solution;
step (F): adding vanadium to ammonium in a molar ratio of 1: 1.2, stirring and reacting at 40-60 ℃ for 2h, performing centrifugal separation to obtain ammonium metavanadate and a vanadium precipitation mother solution, removing ammonia from the vanadium precipitation mother solution through a degassing membrane, returning to the ore grinding step in the step (A) for use, finally performing decomposition reaction on the ammonium metavanadate to obtain vanadium pentoxide, performing decomposition reaction on the ammonium metavanadate to obtain vanadium pentoxide by adopting a calcination mode, wherein the calcination temperature is 500-550 ℃, the reaction time is 2-3 h, the ammonium metavanadate is decomposed to generate vanadium pentoxide, water and ammonia gas, absorbing the generated ammonia gas with sulfuric acid to obtain ammonium sulfate, dissolving the ammonium sulfate, and returning to the step (F) to react with the third solution.
Example 2
This example differs from example 1 in that: in the step (A), the water adding amount is controlled to obtain ore pulp with water content of 30%, concentrated sulfuric acid is added into the ore pulp in a reaction kettle, the ore pulp is uniformly stirred and cured at constant temperature for 5 hours, and the temperature is 120 ℃ to obtain a first reactant.
Example 3
This example differs from example 1 in that: in the step (A), the water adding amount is controlled to obtain ore pulp with the water content of 30%, the ore pulp with the water content of 30% is filtered by a ceramic filter to obtain wet ore powder with the water content of 20%, and the wet ore powder and concentrated sulfuric acid are aged for 5 hours at the temperature of 120 ℃ to obtain a first reactant.
Example 4
This example differs from example 1 in that: in the step (A), the water adding amount is controlled to obtain ore pulp with the water content of 30%, the ore pulp with the water content of 30% is filtered by a ceramic filter to obtain wet ore powder with the water content of 15%, and the wet ore powder and concentrated sulfuric acid are aged for 4 hours at the temperature of 120 ℃ to obtain a first reactant.
Example 5
This example differs from example 1 in that: in the step (A), the ore pulp is poured into a reaction kettle, and then concentrated sulfuric acid is directly poured into the reaction kettle, wherein the curing temperature is 110 ℃, and other conditions are the same.
Experimental example 1
The first reactant of the embodiments 1 to 4 of the present invention is detected, and the specific detection results are shown in the following table 1:
TABLE 1 ripening results for the first reactant
Comparative examples 1 to 10 in the table are comparative experiments according to examples 1 to 5, the comparative example 1 is compared with the comparative example 5, a pit is formed in ore pulp by stirring, and concentrated sulfuric acid is poured into the pit to improve a certain curing degree; generally speaking, when the water content of the ore pulp is 30-40%, the curing time is 5-6 h at the preferred temperature of 110-120 ℃, and when the water content of the ore pulp is 15-20%, the curing time is 4-5 h at the preferred temperature of 120-130 ℃.
Example 6
This example differs from example 1 in that: in the step (F), the ammonium metavanadate is decomposed to generate vanadium pentoxide, water and ammonia gas by adopting an electric heating mode; compared with calcination, the electric heating mode is more environment-friendly, waste such as calcination waste gas and waste residue can not be generated, and the factory environment is further optimized.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (10)
1. The method for preparing vanadium pentoxide is characterized by comprising the following steps:
(A) grinding stone coal by a wet grinding ball mill, simultaneously controlling the water addition amount to obtain ore pulp containing 30-40% of water, pouring the ore pulp into a reaction kettle, stirring along the middle to form a pit, pouring concentrated sulfuric acid into the pit, uniformly stirring, and curing at constant temperature for 4-6 h to obtain a first reactant;
(B) carrying out multi-stage countercurrent leaching separation on the first reactant at normal temperature to obtain a solid phase and a liquid phase, wherein the solid phase is ore tailings with the water content of less than 20% by mass, and the liquid phase is a vanadium-containing acid solution;
(C) adding a certain amount of ammonium bicarbonate or ammonium sulfate into the liquid phase, and performing solid-liquid separation to obtain ammonium alum crystals and a first solution;
(D) adjusting the pH value of the first solution to 2.0-2.5, adding an oxidant for oxidation, and performing ion exchange enrichment to obtain a vanadium-containing barren solution and a second solution, wherein the second solution is an eluent obtained by eluting with a sodium hydroxide solution;
(E) adjusting the pH value of the second solution to 8.5-9.5, and adding the second solution in a mass ratio of 1: reacting 0.12 of 20% magnesium chloride solution at the temperature of 80-100 ℃ for 2 hours, and filtering to obtain a third solution;
(F) adding vanadium to ammonium in a molar ratio of 1: 1.2, stirring and reacting for 2 hours at the temperature of 40-60 ℃, centrifugally separating to obtain ammonium metavanadate and vanadium precipitation mother liquor, and finally, carrying out decomposition reaction on the ammonium metavanadate to obtain vanadium pentoxide.
2. The method for producing vanadium pentoxide according to claim 1, wherein: in the step (A), the stone coal is ground to be less than 100 meshes by a wet grinding ball mill.
3. The method for producing vanadium pentoxide according to claim 1 or 2, wherein: and (B) curing the ore pulp and concentrated sulfuric acid in the step (A) for 5-6 h at the temperature of 110-120 ℃ to obtain a first reactant.
4. The method for producing vanadium pentoxide according to claim 1 or 2, wherein: and (B) enabling the ore pulp containing 30-40% of water in the step (A) to pass through a ceramic filter to obtain 15-20% of wet ore powder, and curing the wet ore powder and concentrated sulfuric acid at the temperature of 120-130 ℃ for 4-5 hours to obtain a first reactant.
5. The method for producing vanadium pentoxide according to claim 1 or 2, wherein: the molar ratio of ammonium ions in the ammonium bicarbonate or ammonium sulfate added in the step (C) to aluminum ions in the liquid phase is 1.2-1.5: 1.
6. the method for producing vanadium pentoxide according to claim 1 or 2, wherein: and (D) adding calcium oxide into the vanadium-containing barren solution enriched by the ion exchange column in the step (D), adjusting the pH value to 6.0-7.0, and returning to the step (B) for multi-stage countercurrent leaching for recycling.
7. The method for producing vanadium pentoxide according to claim 1 or 2, wherein: and (D) after deaminizing by a degassing membrane, returning the vanadium precipitation mother liquor obtained by centrifugal separation in the step (F) to the step (A) for ore grinding link application.
8. The method for producing vanadium pentoxide according to claim 1, wherein: in the step (F), the decomposition reaction of the ammonium metavanadate adopts a calcining mode, the calcining temperature is 500-550 ℃, the reaction time is 2-3 h, and the ammonium metavanadate is decomposed to generate vanadium pentoxide, water and ammonia gas.
9. The method for producing vanadium pentoxide according to claim 1, wherein: and (F) decomposing the ammonium metavanadate in the step (F) by adopting an electric heating mode to generate vanadium pentoxide, water and ammonia gas.
10. The method for producing vanadium pentoxide according to claim 8 or 9, wherein: and (D) absorbing ammonia gas generated by decomposing the ammonium metavanadate with sulfuric acid to obtain ammonium sulfate, dissolving the ammonium sulfate, and returning to the step (F) to react with the third solution.
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| CN101275187A (en) * | 2007-03-26 | 2008-10-01 | 吉首大学 | Process for extracting vanadium by stone coal wet method |
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