CN115010174B - Separation method of low-grade vanadium slag - Google Patents
Separation method of low-grade vanadium slag Download PDFInfo
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- CN115010174B CN115010174B CN202210773249.0A CN202210773249A CN115010174B CN 115010174 B CN115010174 B CN 115010174B CN 202210773249 A CN202210773249 A CN 202210773249A CN 115010174 B CN115010174 B CN 115010174B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The application particularly relates to a separation method of low-grade vanadium slag, belonging to the field of alumina production. A separation method of low-grade vanadium slag comprises the following steps: obtaining n parts of low-grade vanadium slag; respectively carrying out m times of reverse washing and m times of filtering on n parts of low-grade vanadium precipitation slag to respectively obtain n parts of m times of filtrate and n parts of vanadium removal filter cakes; cooling and recrystallizing the filtrate of the 1 time to obtain high-grade vanadium slag; and dissolving, filtering and evaporating to crystallize the vanadium-removed filter cake with new water to obtain sodium oxalate crystals. The method can separate high-grade vanadium slag from low-grade vanadium slag with high sodium oxalate content, and then obtain sodium oxalate crystals by dissolving, filtering and evaporating and crystallizing the vanadium removal filter cake, thereby realizing the effective separation of vanadium salt and sodium oxalate in the low-grade vanadium slag.
Description
Technical Field
The application belongs to the field of alumina production, and particularly relates to a separation method of low-grade vanadium slag.
Background
In the process of producing alumina by the Bayer process, organic matters and vanadium-containing minerals in the ore continuously enter the alumina production flow in the ore leaching process. Part of organic matters are continuously accumulated and degraded in the process, are gradually converted into sodium oxalate, and are converted into vanadium salt after being reacted with alkali, and are continuously accumulated in the process. After the two impurities are accumulated to a certain concentration in the process, the impurities are crystallized and separated out in the decomposition process, so that the operation of the alumina production process and the yield and quality of alumina products are seriously influenced. Therefore, in the process of producing alumina from bauxite with high contents of both organics and vanadium-containing minerals, means are required to remove both impurities from the production system.
At present, most of aluminum oxide flows adopt crystallization methods to remove sodium oxalate and vanadium salt respectively. The crystallization precipitation of sodium oxalate and vanadium salt can be realized by optimizing the process conditions, and the obtained crystallization salt removal filter cake is low-grade vanadium precipitation slag, and the main components of the filter cake are sodium oxalate and vanadium salt, and simultaneously, the filter cake also contains a small amount of other impurity components such as aluminum hydroxide, phosphorus salt and the like. But V is caused by the existence of sodium oxalate in the vanadium slag 2 O 5 The content of the vanadium salt is low, and the necessary technical means are needed to realize the high-efficiency separation of the vanadium salt and sodium oxalate in the crystallization salt removal filter cake, and meanwhile, the high-grade vanadium precipitation slag and oxalate products are obtained.
The separation of sodium oxalate and vanadium salt in the salt removal filter cake by crystallization is not involved in the currently known technology. Therefore, for the special filter cake with vanadium salt and sodium oxalate in the salt removal filter cake and the higher content of sodium oxalate, when vanadium is recovered independently, the existence of sodium oxalate can seriously obstruct the recovery of vanadium, and when sodium oxalate is recovered, if vanadium salt exists in the sodium oxalate removal filter cake, in the solution system of the method, the vanadium salt and sodium oxalate are also dissolved into the solution together, and co-crystallized and separated out with sodium oxalate in the solution recrystallization process, so that high-purity sodium oxalate crystals cannot be obtained.
Disclosure of Invention
The application aims to provide a separation method of low-grade vanadium slag, which aims to solve the technical problem that the prior art cannot effectively separate vanadium salt and sodium oxalate in the low-grade vanadium slag.
The embodiment of the application provides a separation method of low-grade vanadium slag, which comprises the following steps:
obtaining n parts of low-grade vanadium slag, wherein n is an integer more than or equal to 2;
respectively carrying out m times of reverse washing and m times of filtering on n parts of the low-grade vanadium precipitation slag to respectively obtain n parts of m times of filtrate and n parts of vanadium removal filter cakes, wherein m is an integer more than or equal to 2;
cooling and recrystallizing the filtrate of the 1 time to obtain high-grade vanadium slag;
mixing the vanadium-removed filter cake with fresh water, dissolving, filtering, evaporating and crystallizing to obtain sodium oxalate crystals;
wherein:
the m-1 th reverse washing of the low-grade vanadium slag is adopted as a washing liquid, and the m-th filtrate obtained by the m-1 th reverse washing of the low-grade vanadium slag is adopted as a washing liquid;
and (3) carrying out the m-th reverse washing on the low-grade vanadium slag, wherein water is used as washing liquid.
Optionally, the liquid-solid mass ratio of the washing liquid to the washed object is (3-5): 1.
Optionally, the temperature of the washing liquid is 35-85 ℃.
Optionally, the temperature of the washing liquid is 65-85 ℃.
Optionally, the time of the reverse washing is 10-60min.
Optionally, the end temperature of the cooling recrystallization is 15-35 ℃.
Alternatively, m is 2-4.
Optionally, the low-grade vanadium slag comprises the following components in percentage by mass after being dried at 105 ℃:
vanadium pentoxide: 5-10%, sodium oxalate: 30-60%, aluminum hydroxide: 5% -10%.
Optionally, the following components in percentage by mass:
the components of the high-grade vanadium slag after being dried at 105 ℃ comprise: vanadium pentoxide: more than or equal to 20 percent, sodium oxalate: less than or equal to 2 percent;
the vanadium removal filter cake comprises the following components: vanadium pentoxide: less than or equal to 0.5 percent, sodium oxalate: 85-92%.
One or more technical solutions in the embodiments of the present application at least have the following technical effects or advantages:
according to the separation method of the low-grade vanadium precipitation slag, according to the difference of the dissolution speed and the solubility of sodium oxalate and vanadium salt in the vanadium precipitation slag in alkaline solutions with the same temperature and the principle that the dissolution speed of the vanadium salt in the vanadium precipitation slag in a reverse washing process is larger than that of sodium oxalate, the vanadium salt in the vanadium precipitation slag is fully dissolved into filtrate by utilizing the steps defined by the method, and most of sodium oxalate crystals are left in a filter cake; and the solubility of the vanadium salt in the alkaline solution is far less than that of sodium oxalate according to the same temperature, so that the vanadium salt in the solution is more sensitive to temperature and is easy to crystallize and precipitate because the vanadium salt reaches the saturated concentration in the process of cooling the solution. Sodium oxalate in the solution does not reach a saturated state, and basically does not crystallize and separate out in the process of cooling the solution. And cooling and recrystallizing the filtrate to crystallize and separate out vanadium salt in the filtrate, thereby obtaining high-grade vanadium precipitation slag. Undissolved sodium oxalate enters a solid phase, and sodium oxalate crystals are obtained after dissolution, filtration and evaporative crystallization of new water, so that the effective separation of vanadium salt and sodium oxalate in the low-grade vanadium precipitation slag is realized.
The foregoing description is only an overview of the present application, and is intended to be implemented in accordance with the teachings of the present application in order that the same may be more clearly understood and to make the same and other objects, features and advantages of the present application more readily apparent.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a separation method of low-grade vanadium slag.
Detailed Description
The advantages and various effects of the present application will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the application, not to limit the application.
Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification will control. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present application. For example, room temperature may refer to a temperature in the range of 10 to 35 ℃.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present application are commercially available or may be prepared by existing methods.
The technical scheme of the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
according to an exemplary embodiment of the present application, there is provided a separation method of low-grade vanadium slag, including the steps of:
s1, obtaining n parts of low-grade vanadium slag, wherein n is an integer more than or equal to 2.
S2, respectively carrying out m times of reverse washing and m times of filtering on n parts of the low-grade vanadium precipitation slag to respectively obtain n parts of m times of filtrate and n parts of vanadium removal filter cakes, wherein m is an integer more than or equal to 2.
S3, cooling and recrystallizing the filtrate for 1 time to obtain high-grade vanadium slag.
S4, mixing the vanadium removal filter cake with fresh water, dissolving, filtering, evaporating and crystallizing to obtain sodium oxalate crystals.
Wherein:
the m-1 th reverse washing of the low-grade vanadium slag is adopted as a washing liquid, and the m-th filtrate obtained by the m-1 th reverse washing of the low-grade vanadium slag is adopted as a washing liquid;
and (3) carrying out the m-th reverse washing on the low-grade vanadium slag, wherein water is used as washing liquid.
According to the separation method of the low-grade vanadium precipitation slag, according to the difference of the dissolution speed and the solubility of sodium oxalate and vanadium salt in the vanadium precipitation slag in alkaline solution with the same temperature and the principle that the dissolution speed of the vanadium salt in the vanadium precipitation slag in a reverse washing process is greater than that of sodium oxalate, the vanadium salt in the vanadium precipitation slag is completely dissolved into filtrate by utilizing the steps defined by the method, and most of sodium oxalate crystals are remained in a filter cake; and then according to the fact that the solubility of vanadium salt in alkaline solution at the same temperature is far smaller than that of sodium oxalate, cooling and recrystallizing filtrate to enable the vanadium salt in a saturated state in the solution to be crystallized and separated out, and obtaining high-grade vanadium precipitation slag. And sodium oxalate in the solution does not reach a saturated state, and basically does not crystallize and separate out in the process of cooling the solution. Undissolved sodium oxalate enters a solid phase, and sodium oxalate crystals are obtained after dissolution, filtration and evaporative crystallization of new water, so that the effective separation of vanadium salt and sodium oxalate in the low-grade vanadium precipitation slag is realized.
The (n) th part of the raw material is subjected to the (m-1) th reverse washing, and the (m) th filtrate obtained by the (n-1) th reverse washing of the raw material is used as washing liquid, so that on one hand, the water for the reverse washing (namely, the filtrate) is fully utilized, and the water resource is saved; on the other hand, the method aims to enrich the product in the filtrate for multiple times, so that the product in the filtrate is not wasted, and the yield of the product is ensured.
As an alternative embodiment, the liquid-solid mass ratio of the washing liquid to the washed object is (3-5): 1.
As an alternative embodiment, the temperature of the wash solution is 35-85 ℃.
Preferably, the temperature of the wash solution is 65-85 ℃.
As an alternative embodiment, the reverse washing time is 10-60min.
As an alternative embodiment, the end point temperature of the reduced temperature recrystallization is 15-35 ℃.
As an alternative embodiment, m is 2-4.
As an optional implementation manner, the low-grade vanadium slag comprises the following components in percentage by mass after being dried at 105 ℃: vanadium pentoxide: 5-10%, sodium oxalate: 30-60%, aluminum hydroxide: 5% -10%.
As an alternative embodiment, the following percentages are by mass:
the components of the high-grade vanadium slag after being dried at 105 ℃ comprise: vanadium pentoxide: more than or equal to 20 percent, sodium oxalate: less than or equal to 2 percent;
the vanadium removal filter cake comprises the following components: vanadium pentoxide: less than or equal to 0.5 percent, sodium oxalate: 85-92%.
The present application will be described in detail with reference to examples, comparative examples and experimental data.
Example 1
The separation method of the low-grade vanadium slag comprises the following steps:
s1, 6 parts of low-grade vanadium slag is obtained, and the low-grade vanadium slag is dried at 105 ℃ and comprises the following components in percentage by mass: vanadium pentoxide: 5-10%, sodium oxalate: 30-60%.
S2, respectively carrying out 2 times of reverse washing and 2 times of filtering on 6 parts of low-grade vanadium slag to respectively obtain 6 parts of 1-time filtrate, 6 parts of 2-time filtrate and 6 parts of vanadium removal filter cake, wherein the mass percentages are as follows: the 6 parts of vanadium removal filter cake comprises the following components: average content of vanadium pentoxide: 0.12 percent of sodium oxalate average content: 91.17%.
S3, cooling and recrystallizing 6 parts of 1-time filtrate respectively to obtain 6 parts of high-grade vanadium slag, wherein the mass percentages are as follows: the 6 parts of high-grade vanadium slag after being dried at 105 ℃ comprises the following components: average content of vanadium pentoxide: 24.79%, average content of sodium oxalate: 1.10%.
Wherein:
the final temperature of the cooling recrystallization is 35 ℃;
the liquid-solid mass ratio of the washing liquid to the washed object is 3:1;
the temperature of the washing liquid is 85 ℃;
the reverse washing time was 10min.
S4, mixing the vanadium removal filter cake with new water, dissolving, filtering, evaporating and crystallizing to obtain sodium oxalate crystals.
Wherein:
the 1 st reverse washing of the nth part of low-grade vanadium slag adopts 2 times of filtrate obtained by the 2 nd reverse washing of the nth-1 st part of raw materials as washing liquid, wherein n=2, 3, 4, 5 and 6;
and 6 parts of the low-grade vanadium slag are reversely washed for the 2 nd time, and water is used as washing liquid.
Example 2
The separation method of the low-grade vanadium slag is provided, and only differs from the embodiment 1 in that:
the final temperature of the cooling recrystallization is 15 ℃;
the weight percentage is as follows:
the 6 parts of vanadium removal filter cake comprises the following components: average content of vanadium pentoxide: 0.09%, average content of sodium oxalate: 90.24%;
the 6 parts of high-grade vanadium slag after being dried at 105 ℃ comprises the following components: average content of vanadium pentoxide: 23.09%, average content of sodium oxalate: 1.81%.
Example 3
The separation method of the low-grade vanadium slag is provided, and only differs from the embodiment 1 in that:
the final temperature of the cooling recrystallization is 15 ℃;
the temperature of the washing liquid is 65 ℃;
the time of the reverse washing is 30min;
the weight percentage is as follows:
the 6 parts of vanadium removal filter cake comprises the following components: average content of vanadium pentoxide: 0.14%, average content of sodium oxalate: 88.94%;
the 6 parts of high-grade vanadium slag after being dried at 105 ℃ comprises the following components: average content of vanadium pentoxide: 23.51%, average content of sodium oxalate: 1.38%.
Example 4
The separation method of the low-grade vanadium slag is provided, and only differs from the embodiment 1 in that:
the liquid-solid mass ratio of the washing liquid to the washed object is 4:1;
the final temperature of the cooling recrystallization is 15 ℃;
the temperature of the washing liquid is 65 ℃;
the time of the reverse washing is 30min;
the weight percentage is as follows:
the 6 parts of vanadium removal filter cake comprises the following components: average content of vanadium pentoxide: 0.18%, average content of sodium oxalate: 91.26%;
the 6 parts of high-grade vanadium slag after being dried at 105 ℃ comprises the following components: average content of vanadium pentoxide: 23.92%, average content of sodium oxalate: 0.93%.
Example 5
The separation method of the low-grade vanadium slag is provided, and only differs from the embodiment 1 in that:
s2, respectively carrying out reverse washing and 3 times of filtering on 6 parts of low-grade vanadium slag to respectively obtain 6 parts of 1-time filtrate, 6 parts of 2-time filtrate, 6 parts of 3-time filtrate and 6 parts of vanadium removal filter cakes;
the liquid-solid mass ratio of the washing liquid to the washed object is 4:1;
the final temperature of the cooling recrystallization is 15 ℃;
the temperature of the washing liquid is 35 ℃;
the reverse washing time is 60min;
the weight percentage is as follows:
the 6 parts of vanadium removal filter cake comprises the following components: average content of vanadium pentoxide: 0.45%, average content of sodium oxalate: 85.48%;
the 6 parts of high-grade vanadium slag after being dried at 105 ℃ comprises the following components: average content of vanadium pentoxide: 21.92%, average content of sodium oxalate: 1.59%;
the 1 st reverse washing of the nth part of low-grade vanadium slag adopts 2 times of filtrate obtained by the 2 nd reverse washing of the nth-1 st part of raw materials as washing liquid, wherein n=2, 3, 4, 5 and 6; the 2 nd reverse washing of the nth part of low-grade vanadium slag adopts 3 times filtrate obtained by the 3 rd reverse washing of the nth-1 st part of raw materials as washing liquid, and n=2, 3, 4, 5 and 6;
and (3) carrying out reverse washing on 6 parts of low-grade vanadium slag for the 3 rd time, wherein water is used as washing liquid.
Example 6
The separation method of the low-grade vanadium slag is provided, and only differs from the embodiment 1 in that:
s3, respectively carrying out reverse washing and 4 times of filtering on 6 parts of low-grade vanadium slag to respectively obtain 6 parts of 1-time filtrate, 6 parts of 2-time filtrate, 6 parts of 3-time filtrate, 6 parts of 4-time filtrate and 6 parts of vanadium removal filter cakes;
the liquid-solid mass ratio of the washing liquid to the washed object is 5:1;
the final temperature of the cooling recrystallization is 15 ℃;
the temperature of the washing liquid is 35 ℃;
the reverse washing time is 60min;
the weight percentage is as follows:
the 6 parts of vanadium removal filter cake comprises the following components: average content of vanadium pentoxide: 0.36% of sodium oxalate average content: 87.96%;
the 6 parts of high-grade vanadium slag after being dried at 105 ℃ comprises the following components: average content of vanadium pentoxide: 22.46%, average content of sodium oxalate: 1.33%;
the 1 st reverse washing of the nth part of low-grade vanadium slag adopts 2 times of filtrate obtained by the 2 nd reverse washing of the nth-1 st part of raw materials as washing liquid, wherein n=2, 3, 4, 5 and 6; the 2 nd reverse washing of the nth part of low-grade vanadium slag adopts 3 times filtrate obtained by the 3 rd reverse washing of the nth-1 st part of raw materials as washing liquid, and n=2, 3, 4, 5 and 6;
and (3) carrying out reverse washing on 6 parts of low-grade vanadium slag for the 3 rd time, wherein water is used as washing liquid.
Finally, it is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (5)
1. The separation method of the low-grade vanadium slag is characterized by comprising the following steps of:
obtaining n parts of low-grade vanadium slag, wherein n is an integer more than or equal to 2;
respectively carrying out m times of reverse washing and m times of filtering on n parts of the low-grade vanadium precipitation slag to respectively obtain n parts of m times of filtrate and n parts of vanadium removal filter cakes, wherein m is an integer more than or equal to 2;
cooling and recrystallizing the filtrate of the 1 time to obtain high-grade vanadium slag;
mixing the vanadium-removed filter cake with fresh water, dissolving, filtering, evaporating and crystallizing to obtain sodium oxalate crystals;
wherein:
the m-1 th reverse washing of the low-grade vanadium slag is adopted as a washing liquid, and the m-th filtrate obtained by the m-1 th reverse washing of the low-grade vanadium slag is adopted as a washing liquid;
the mth reverse washing of the low-grade vanadium slag adopts new water as washing liquid;
the temperature of the washing liquid is 35-85 ℃, the time of the reverse washing is 10-60min, the end temperature of the cooling recrystallization is 15-35 ℃, and the components of the low-grade vanadium slag after being dried at 105 ℃ comprise the following components in percentage by mass:
vanadium pentoxide: 5-10%, sodium oxalate: 30-60%, aluminum hydroxide: 5% -10%.
2. The method for separating low-grade vanadium slag according to claim 1, wherein the ratio of the liquid to the solid of the washing liquid to the object to be washed is (3-5): 1.
3. The method for separating low-grade vanadium slag according to claim 1, wherein the temperature of the washing liquid is 65-85 ℃.
4. The method for separating low-grade vanadium slag according to claim 1, wherein m is 2 to 4.
5. The method for separating low-grade vanadium slag according to claim 1, which is characterized by comprising the following steps of:
the components of the high-grade vanadium slag after being dried at 105 ℃ comprise: vanadium pentoxide: more than or equal to 20 percent, sodium oxalate: less than or equal to 2 percent;
the vanadium removal filter cake comprises the following components: vanadium pentoxide: less than or equal to 0.5 percent, sodium oxalate: 85-92%.
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