CN111534698A - Method for preparing vanadium product from sodium vanadium solution without ammonium precipitation - Google Patents
Method for preparing vanadium product from sodium vanadium solution without ammonium precipitation Download PDFInfo
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- CN111534698A CN111534698A CN202010537743.8A CN202010537743A CN111534698A CN 111534698 A CN111534698 A CN 111534698A CN 202010537743 A CN202010537743 A CN 202010537743A CN 111534698 A CN111534698 A CN 111534698A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- C—CHEMISTRY; METALLURGY
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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Abstract
The invention provides a method for preparing a vanadium product by ammonium-free vanadium precipitation of a sodium vanadium solution. The method comprises the following steps: step a: adding the sodium vanadium solution into organic acid, adjusting the pH value to 6-8, and hydrolyzing to precipitate vanadium; step b: carrying out solid-liquid separation on the mixture obtained by the reaction, and calcining the separated solid; step c: and grinding, washing and drying the calcined product to obtain a vanadium product. The vanadium product prepared by the method has the vanadium precipitation rate of over 98 percent and the vanadium content of over 56 percent. The method does not need an ammonia-containing vanadium precipitation agent, thereby reducing ammonia pollution; after the vanadium is precipitated, the supernatant liquid of the precipitated vanadium is beneficial to wastewater treatment because of no ammonium. In addition, the method has the advantages of simple process, low equipment requirement, convenient operation, wide application range, low cost and good social and economic benefits.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a method for preparing a vanadium product from a sodium vanadium solution without ammonium precipitation.
Background
The vanadium slag is mainly from molten iron vanadium extraction, the vanadium slag vanadium extraction process mainly comprises sodium salt roasting vanadium extraction and calcification roasting vanadium extraction, the vanadium solution obtained by the method mainly adopts acidic ammonium salt vanadium precipitation, the yield of the acidic ammonium salt vanadium precipitation is high, the quality of the vanadium product meets the quality standard requirement, but the following defects exist: on one hand, in the process of using ammonium salt to precipitate vanadium, a large amount of ammonia overflows to cause the severe working environment of the vanadium precipitation process, and in addition, a part of ammonium salt enters a wastewater system, so that the ammonia nitrogen content in wastewater is higher, the wastewater treatment cost is high, and if the ammonium salt is directly discharged, the environment can be greatly polluted; on the other hand, ammonium polyvanadate is generally obtained by vanadium precipitation, and the vanadium pentoxide product can be obtained only by calcining at about 500 ℃ and burning off ammonium therein.
In the prior art, ammonium-free vanadium precipitation is also started, a novel vanadium precipitation agent is generally adopted for vanadium precipitation, vanadium dioxide with low price is formed by reaction at a certain temperature, or the vanadium in the vanadium precipitation agent is precipitated in a poly-vanadic acid form, and the poly-vanadic acid is hydrolyzed into vanadium pentoxide and precipitated along with the reduction of acidity.
For example, patent document CN108531753A discloses a method for precipitating vanadium from vanadium shale without ammonium, which comprises the following steps: step 1), mixing a vanadium precipitation agent with a vanadium-rich liquid, and then adjusting the pH of the mixed liquid to 0.7-1.0 to obtain a liquid to be reacted; the vanadium-rich liquid is a liquid which is obtained by roasting, acid leaching, extracting and back extracting the vanadium shale, has a vanadium concentration of 10-45 g/L and a vanadium valence state of + 5; the molar ratio of the vanadium precipitation agent to vanadium in the vanadium-rich liquid is 1.0-2.0; step 2), reacting the solution to be reacted obtained in the step 1) at the temperature of 180-240 ℃ for 3-12 hours, and naturally cooling to obtain slurry; and 3) carrying out solid-liquid separation on the slurry obtained in the step 2) to obtain a solid and a liquid, and carrying out vacuum drying on the solid at the temperature of 60-100 ℃ to obtain a vanadium dioxide product. The invention adopts an ammonium-free vanadium precipitation agent for hydrothermal reaction to obtain a vanadium dioxide product.
Patent document CN106337135A discloses a novel method for producing vanadium pentoxide by ammonium-free vanadium precipitation. Oxidizing tetravalent vanadium in a back extraction liquid obtained after acid leaching, extraction and back extraction of raw ore in a vanadium extraction process into pentavalent vanadium to form a pentavalent vanadium supersaturated system, crystallizing poly-vanadic acid precipitate, or roasting, acid leaching, ion exchange or extracting and back extracting ore or vanadium slag to obtain a high-concentration vanadium-containing solution, uniformly stirring while keeping the temperature, adding a novel vanadium precipitation agent to precipitate poly-vanadic acid continuously, generating more insoluble vanadium pentoxide hydrate precipitate due to the reduction of acid concentration, separating a mother solution with high impurity content through solid-liquid separation to obtain a powdery vanadium pentoxide hydrate, and calcining the product to obtain vanadium pentoxide.
However, the existing ammonium-free vanadium precipitation method has poor effect for various reasons such as process, cost and the like, and still has room for further improvement.
Disclosure of Invention
The invention aims to overcome the defects that the ammonia nitrogen in the waste water exceeds the standard and the ammonia gas is discharged in the calcining process of the product in the existing ammonium salt vanadium precipitation process and solve the problem of low vanadium precipitation rate, and provides the method for preparing the vanadium product by using the sodium vanadium solution without ammonium vanadium precipitation, which is environment-friendly and high in vanadium precipitation rate.
Based on the purposes, the invention adopts the following technical scheme:
a method for preparing a vanadium product from a sodium vanadium solution without ammonium precipitation comprises the following steps:
step a: adding the sodium vanadium solution into organic acid, adjusting the pH value to 6-8, and hydrolyzing to precipitate vanadium;
step b: carrying out solid-liquid separation on the mixture obtained by the reaction, and calcining the separated solid;
step c: and grinding, washing and drying the calcined product to obtain a vanadium product.
According to one embodiment of the invention, in step a, the organic acid used is formic acid and/or acetic acid.
According to one embodiment of the invention, in step a, the reaction temperature is room temperature.
According to one embodiment of the invention, in step a, the sodium vanadium solution is added to the organic acid under stirring.
According to one embodiment of the invention, in the step a, the stirring is continued for 60-120 minutes after the pH is adjusted to 6-8.
According to an embodiment of the invention, in the step b, the calcination temperature is 150-350 ℃ and the calcination time is 30-50 min.
According to one embodiment of the invention, in step b, the solid separated from the solid-liquid is directly calcined.
According to one embodiment of the invention, in step c, the calcined product is ground to-60 mesh.
According to one embodiment of the invention, in step c, washing is performed with water, and the liquid-solid ratio of washing is 0.5: 1, the liquid-solid ratio is the ratio of the mL number of water to the g number of the object to be washed, and the washing is carried out for three times.
According to one embodiment of the invention, the concentration of vanadium in the sodium vanadium solution is 18-80 g/L.
By adopting the technical scheme, the invention at least has the following beneficial effects:
the method of the invention adopts organic acid such as formic acid and/or acetic acid as vanadium precipitation agent to carry out hydrolysis vanadium precipitation on the sodium vanadium solution, the whole method process is environment-friendly and economic, no toxic and harmful gas is discharged, and the recovery rate of vanadium products is high. In addition, the method has the advantages of simple process, low equipment requirement, convenient operation, wide application range and low cost.
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FIG. 1 shows a process flow diagram of a method for preparing a vanadium product from a sodium vanadium solution without ammonium precipitation of vanadium according to the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
As shown in fig. 1, the invention provides a method for preparing a vanadium product from a sodium vanadium solution without ammonium precipitation, which comprises the following steps:
step a: adding the sodium vanadium solution into organic acid, adjusting the pH value to 6-8, and hydrolyzing to precipitate vanadium;
step b: carrying out solid-liquid separation on the mixture obtained by the reaction, and calcining the separated solid;
step c: and grinding, washing and drying the calcined product to obtain a vanadium product.
The source of the sodium vanadium solution is not particularly limited, and the sodium vanadium solution can be vanadium slag obtained after sodium roasting or vanadium leaching solution of stone coal. In general, the sodium vanadium solution contains impurities such as phosphorus, titanium, calcium, magnesium, silicon, iron, aluminum, calcium, and chromium in addition to sodium and vanadium. The concentration of vanadium in the sodium vanadium solution is not particularly limited in the present invention as long as vanadium can be recovered therefrom, and in such a case, the concentration of vanadium in the sodium vanadium solution may be more than 1g/L, preferably 10 to 80 g/L. In the sodium vanadium solution, vanadium exists in the form of pentavalent vanadium. The initial pH of the sodium vanadium solution is 9-11.
In step a, the organic acid used is formic acid and/or acetic acid. Wherein, the formic acid can adopt 85 to 88 mass percent of formic acid, and the acetic acid can adopt 36 to 99.5 mass percent of acetic acid. In the step a, the sodium vanadium solution is added into the organic acid under the condition of stirring so as to keep the solution in a homogeneous system. The stirring conditions in the present invention are not particularly limited, and stirring conditions known to those skilled in the art can be used. The tool for stirring in the present invention is not particularly limited, and may be a stirring tool known to those skilled in the art, and for example, a magnetic stirring bar, a power-assisted electric stirrer, or the like may be used. In the step a, the vanadium liquid is used as a regulator to regulate the end point pH to be 6-8, so that the consumption of formic acid or acetic acid is minimum, and the vanadium precipitation rate is high. If the pH is less than 5, on one hand, the acid consumption is greatly increased, the cost is high, and on the other hand, the acidity is too strong, so that the generated vanadium pentoxide is easily dissolved, and the vanadyl formate/vanadyl acetate and the sodium formate/sodium acetate coexist in a liquid form; if the pH is too high, the precipitation of vanadium is poor and it is possible that some of the sodium vanadate in the solution is not converted into precipitable vanadium species. In the step a, after the pH is adjusted to 6-8, stirring is continued for a certain time, which is beneficial to fully reacting under the pH condition. The time for continuing stirring is preferably 60 to 120 minutes. The reaction temperature in step a was room temperature. After the hydrolysis vanadium precipitation reaction is finished, a layered system comprising an upper layer liquid and a precipitate can be obtained, and the vanadium precipitation rate is obtained by calculating the percentage of the difference between the total vanadium content of the initial sodium vanadium solution and the vanadium content in the upper layer liquid after the reaction in the total vanadium content.
And in the step b, performing solid-liquid separation on the mixture obtained by the reaction by adopting a conventional filtration mode. The separated solid is directly calcined without washing, so that the process is simplified. In the step b, the calcining temperature is 150-350 ℃, and the calcining time is 30-50 min.
In step c, the calcined product is ground through-60 mesh and washed with water to wash out sodium carbonate, sodium acetate, etc. from the product. Liquid-solid ratio in washing 0.5: 1, the liquid-solid ratio is the ratio of the mL number of water to the g number of the object to be washed, preferably washing for three times in total, and then drying the washed product to obtain the vanadium product. The obtained vanadium product is vanadium pentoxide or a mixture of the vanadium pentoxide and the vanadium trioxide. The washing water after washing can be returned to be used for clinker leaching.
In the hydrolysis vanadium precipitation reaction process, sodium vanadate reacts with formic acid/acetic acid to generate vanadium pentoxide and sodium vanadyl formate/sodium vanadyl acetate, and the vanadium pentoxide and the sodium vanadyl formate/sodium vanadyl acetate are precipitated by coprecipitation; in the subsequent calcining process, the sodium vanadyl formate/sodium vanadyl acetate are heated to decompose, vanadium pentoxide and sodium formate/sodium acetate are obtained again, and simultaneously partial formate/acetate possibly mixed with the sodium vanadyl formate/acetate are decomposed into carbon monoxide, so that the vanadium has a certain reduction effect, and partial low-valence vanadium trioxide is contained in the product; when the vanadium pentoxide is washed by water, the sodium formate/sodium acetate enters water washing liquid, so that the vanadium pentoxide with higher purity is obtained.
Specific examples of the present invention are given below.
Example 1
Pouring the sodium vanadium solution (18g/L) into acid (formic acid), and adding the vanadium solution into the acid while stirring; adjusting pH to 6, and stirring for 60 min; filtering, and calcining at 150 deg.C for 30 min; grinding to 60 meshes, and the liquid-solid ratio is 0.5: 1, washing for three times and drying. The vanadium content in the supernatant fluid is 0.3g/L, the vanadium precipitation rate is 98.33 percent, and the V content in the obtained vanadium product is 56.3 percent.
Example 2
Pouring 45/L of sodium vanadium solution into acid (acetic acid), and adding the vanadium solution into the acid while stirring; adjusting pH to 7.2, and stirring for 100 min; filtering, and calcining at 250 deg.C for 40 min; grinding to 60 meshes, and the liquid-solid ratio is 0.5: 1, washing for three times and drying. The content of vanadium in the supernatant fluid is 0.35g/L, the vanadium precipitation rate is 99.22%, and the content of V in the obtained vanadium product is 56.45%.
Example 3
Pouring the sodium vanadium solution (80g/L) into acid (formic acid and acetic acid), and adding the vanadium solution into the acid while stirring; adjusting pH to 8, and stirring for 120 min; filtering, and calcining at 350 deg.C for 50 min; grinding to 60 meshes, and the liquid-solid ratio is 0.5: 1, washing for three times and drying. The vanadium content in the supernatant fluid is 0.40g/L, the vanadium precipitation rate is 99.5 percent, and the V content in the obtained vanadium product is 56.18 percent.
Example 4
Pouring the sodium vanadium solution (18g/L) into acid (formic acid), and adding the vanadium solution into the acid while stirring; adjusting pH to 6, and stirring for 60 min; filtering, and calcining at 200 deg.C for 30 min; grinding to 60 meshes, and the liquid-solid ratio is 0.5: 1, washing for three times and drying. The vanadium content in the supernatant liquid is 0.32g/L, the vanadium precipitation rate is 98.5 percent, and the V content in the obtained vanadium product is 56.2 percent.
Example 5
Pouring the sodium vanadium solution (18g/L) into acid (formic acid), and adding the vanadium solution into the acid while stirring; adjusting pH to 6, and stirring for 60 min; filtering, and calcining at 300 deg.C for 30 min; grinding to 60 meshes, and the liquid-solid ratio is 0.5: 1, washing for three times and drying. The vanadium content in the supernatant liquid is 0.24g/L, the vanadium precipitation rate is 99.03%, and the V content in the obtained vanadium product is 56.42%.
According to the embodiment, the vanadium precipitation rate of the vanadium product prepared by the method can reach more than 98%, and the vanadium content of the prepared vanadium product reaches more than 56%. In addition, the method does not need an ammonia-containing vanadium precipitation agent, thereby reducing ammonia pollution; after the vanadium is precipitated, the supernatant liquid of the precipitated vanadium is beneficial to wastewater treatment because of no ammonium. In addition, the method has the advantages of simple process, low equipment requirement, convenient operation, wide application range, low cost and good social and economic benefits.
The above is an exemplary embodiment of the present disclosure, and the order of disclosure of the above embodiment of the present disclosure is only for description and does not represent the merits of the embodiment. It should be noted that the discussion of any embodiment above is exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to those examples, and that various changes and modifications may be made without departing from the scope, as defined in the claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of an embodiment of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (10)
1. A method for preparing a vanadium product from a sodium vanadium solution without ammonium precipitation is characterized by comprising the following steps:
step a: adding the sodium vanadium solution into organic acid, adjusting the pH value to 6-8, and hydrolyzing to precipitate vanadium;
step b: carrying out solid-liquid separation on the mixture obtained by the reaction, and calcining the separated solid;
step c: and grinding, washing and drying the calcined product to obtain a vanadium product.
2. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation is characterized in that in the step a, the organic acid is formic acid and/or acetic acid.
3. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation of vanadium according to claim 2, wherein in the step a, the reaction temperature is room temperature.
4. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation is characterized in that in the step a, the sodium vanadium solution is added into the organic acid under the condition of stirring.
5. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation is characterized in that in the step a, the stirring is continued for 60-120 minutes after the pH is adjusted to 6-8.
6. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation is characterized in that in the step b, the calcining temperature is 150-350 ℃ and the calcining time is 30-50 min.
7. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation of vanadium, which is characterized in that in the step b, the solid after solid-liquid separation is directly calcined.
8. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation is characterized in that in the step c, the calcined product is ground to be minus 60 meshes.
9. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation is characterized in that in the step c, water is used for washing, and the liquid-solid ratio of washing is 0.5: 1, washing three times, wherein the liquid-solid ratio is the ratio of the mL number of water to the g number of the object to be washed.
10. The method for preparing the vanadium product from the sodium vanadium solution without ammonium precipitation is characterized in that the concentration of vanadium in the sodium vanadium solution is 18-80 g/L.
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Application publication date: 20200814 |