CN116640936B - Method for producing high-grade vanadium concentrate - Google Patents
Method for producing high-grade vanadium concentrate Download PDFInfo
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- CN116640936B CN116640936B CN202310614054.6A CN202310614054A CN116640936B CN 116640936 B CN116640936 B CN 116640936B CN 202310614054 A CN202310614054 A CN 202310614054A CN 116640936 B CN116640936 B CN 116640936B
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 67
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000012141 concentrate Substances 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims abstract description 116
- 229940039790 sodium oxalate Drugs 0.000 claims abstract description 116
- 239000012452 mother liquor Substances 0.000 claims abstract description 76
- 238000001556 precipitation Methods 0.000 claims abstract description 49
- 238000002425 crystallisation Methods 0.000 claims abstract description 33
- 150000003681 vanadium Chemical class 0.000 claims abstract description 31
- 238000004131 Bayer process Methods 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 230000008025 crystallization Effects 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 27
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 239000010413 mother solution Substances 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 28
- 239000003518 caustics Substances 0.000 claims description 27
- 239000003513 alkali Substances 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 description 12
- 239000002002 slurry Substances 0.000 description 12
- 238000003825 pressing Methods 0.000 description 11
- 238000000605 extraction Methods 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 238000011085 pressure filtration Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 229910001570 bauxite Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- DNWNZRZGKVWORZ-UHFFFAOYSA-N calcium oxido(dioxo)vanadium Chemical compound [Ca+2].[O-][V](=O)=O.[O-][V](=O)=O DNWNZRZGKVWORZ-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009439 industrial construction Methods 0.000 description 1
- 238000009440 infrastructure construction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
Classifications
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
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Abstract
The application relates to the field of vanadium concentrate preparation, in particular to a method for producing high-grade vanadium concentrate; the method comprises the following steps: adding a sodium oxalate remover into Bayer process seed precipitation mother liquor to perform sodium oxalate removal reaction, and then performing solid-liquid separation to obtain mother liquor after sodium oxalate removal; evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystal into the concentrated mother solution for crystallization reaction, and carrying out solid-liquid separation to obtain high-grade vanadium concentrate. Sodium oxalate impurity is removed by adding sodium oxalate remover into Bayer process seed precipitation mother liquor, primary purification of Bayer process seed precipitation mother liquor is realized, concentration of sodium oxalate in the mother liquor is reduced, and then the mother liquor after sodium oxalate removal is concentrated and cooled for vanadium precipitation, so that crystallization precipitation of sodium oxalate in the vanadium precipitation process can be avoided, and vanadium concentrate with high vanadium pentoxide content is obtained.
Description
Technical Field
The application relates to the field of preparation of vanadium concentrates, in particular to a method for producing high-grade vanadium concentrates.
Background
In the process of alumina production by taking high vanadium bauxite as a raw material, vanadium-containing minerals in the bauxite belong to harmful impurities, and when the vanadium-containing minerals reach a certain concentration, adverse effects can be caused on a production system. However, vanadium is used as a rare element, plays an important role in the fields of national defense construction, major infrastructure construction, new energy sources and the like, is one of essential basic materials and strategic materials for national defense and industrial construction, and is also a strategic material focused on by countries around the world.
In recent years, some alumina manufacturers have been focusing on the extraction and recovery of vanadium resources from bauxite. In view of the extraction of vanadium in the alumina process, the currently known methods include adsorption extraction, precipitation, crystallization and the like. The crystallization method has the advantages of simple technology and strong operability, and is widely applied to the extraction of vanadium in enterprises.
However, for precipitating vanadium by crystallization, sodium oxalate, sodium carbonate and other various impurities exist in the production flow of alumina, and some impurities such as sodium oxalate and the like and vanadium salt have the same crystallization process, when the concentration of sodium oxalate in the solution is higher, sodium oxalate and vanadium salt are easy to separate out synchronously, the sodium oxalate content in the obtained salt removal filter cake is too high, and the content of vanadium pentoxide is lower, so that the recovery value of vanadium in the filter cake is not great. Therefore, how to provide a method for producing high-grade vanadium concentrate so as to greatly improve the content of vanadium pentoxide in the vanadium precipitation filter cake is a technical problem which needs to be solved at present.
Disclosure of Invention
The application provides a method for producing high-grade vanadium concentrate, which aims to solve the technical problem that the content of vanadium pentoxide is low due to the fact that the content of sodium oxalate is too high in the prior art.
In a first aspect, the present application provides a method of producing high grade vanadium concentrate, the method comprising:
adding a sodium oxalate remover into Bayer process seed precipitation mother liquor to perform sodium oxalate removal reaction, and then performing solid-liquid separation to obtain mother liquor after sodium oxalate removal;
evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystal into the concentrated mother solution for crystallization reaction, and carrying out solid-liquid separation to obtain high-grade vanadium concentrate.
Optionally, the caustic alkali concentration of the Bayer process seed precipitation mother liquor is less than or equal to 170g/L, and the temperature of the Bayer process seed precipitation mother liquor is 30-60 ℃.
Optionally, the adding amount of the sodium oxalate remover is 3 g/L-10 g/L.
Optionally, the reaction time for removing sodium oxalate is 4-10 hours.
Optionally, the caustic concentration of the concentrated mother liquor is 190g/L to 240g/L.
Optionally, the temperature of the cooling end point is 25-60 ℃.
Optionally, the crystallization reaction time is 5-15 h.
Optionally, adding a sodium oxalate remover into the bayer process seed precipitation mother liquor to perform a sodium oxalate removal reaction, and performing solid-liquid separation to obtain a mother liquor after sodium oxalate removal, wherein the method comprises the following steps:
Adding a sodium oxalate removing agent into Bayer process seed precipitation mother liquor to perform sodium oxalate removal reaction, and then performing solid-liquid separation to respectively obtain mother liquor after sodium oxalate removal and sodium oxalate removal seed crystal;
And recycling the sodium oxalate removal seed crystal.
Optionally, evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystal into the concentrated mother solution for crystallization reaction, and performing solid-liquid separation to obtain high-grade vanadium concentrate, and the method comprises the following steps:
Evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystals into the concentrated mother solution for crystallization reaction, and carrying out solid-liquid separation to obtain high-grade vanadium concentrate and separation solution respectively;
the separated solution is used as a raw material for alumina production.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the method for producing the high-grade vanadium concentrate, provided by the embodiment of the application, the sodium oxalate removing agent is added into the Bayer process seed precipitation mother liquor to remove sodium oxalate impurities, so that the Bayer process seed precipitation mother liquor is primarily purified, the concentration of sodium oxalate is reduced, then the evaporation concentration and the cooling are carried out, the concentration of sodium oxalate can be further reduced, and finally the Bayer process seed precipitation mother liquor is separated out for crystallization through the vanadium salt seed crystal, and due to the low content of sodium oxalate, the low-concentration sodium oxalate is difficult to react with vanadium salt in the crystallization process, so that the vanadium concentrate with high vanadium pentoxide content is obtained.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the application or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, and it will be obvious to a person skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic flow chart of a method for producing high-grade vanadium concentrate according to an embodiment of the present application.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
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 inventive thinking of the application is:
Aiming at the extraction of vanadium in an alumina process, the currently known methods comprise an adsorption extraction method, a precipitation method, a crystallization method and the like, wherein the adsorption extraction method needs to use an adsorbent such as an ion exchange resin with high price, the targeting ion exchange resin aiming at vanadium is not commercially applied at the present stage, and meanwhile, the problems of high desorption difficulty, low efficiency and the like of the vanadium after the vanadium is adsorbed by the resin exist, so that the related research only stays in a laboratory stage; the precipitation method is to add lime into the mother liquor to precipitate vanadium in the solution. The method has the defects that the addition of lime can cause a great deal of loss of aluminum in the sodium aluminate solution, and the obtained calcium vanadate precipitate has higher cost when vanadium is recovered; the crystallization method is characterized in that the equilibrium concentration of vanadium salt in sodium aluminate solution is reduced along with the increase of the caustic alkali concentration of the solution and the decrease of the solution temperature, and the vanadium salt in the solution is crystallized and separated out by increasing the caustic alkali concentration of the solution, decreasing the solution temperature and adding seed crystals. The method has simple process technology and strong operability, and is applied to some alumina enterprises in China at present.
However, in the crystallization method for precipitating vanadium, sodium oxalate, sodium carbonate and other various impurities exist in the production flow of alumina, and some impurities such as sodium oxalate and the like have the same crystallization process with vanadium salt, namely the higher the caustic alkali concentration of the solution is, the lower the crystallization temperature is, and the higher the precipitation rate of sodium oxalate and vanadium salt in the solution is. Therefore, when the concentration of sodium oxalate in the solution is higher, sodium oxalate is easy to be synchronously separated out with vanadium salt, the content of sodium oxalate in the obtained salt removal filter cake is too high, and the content of vanadium pentoxide is lower, so that the recovery value of vanadium in the filter cake is not great. Therefore, how to provide a method for producing high-grade vanadium concentrate so as to greatly improve the content of vanadium pentoxide in the vanadium precipitation filter cake is a technical problem which needs to be solved at present.
As shown in fig. 1, an embodiment of the present application provides a method for producing high-grade vanadium concentrate, the method comprising:
S1, adding a sodium oxalate remover into Bayer process seed precipitation mother liquor to perform sodium oxalate removal reaction, and then performing solid-liquid separation to obtain mother liquor after sodium oxalate removal;
S2, evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystals into the concentrated mother solution for crystallization reaction, and carrying out solid-liquid separation to obtain high-grade vanadium concentrate.
In some alternative embodiments, the bayer process seed precipitation liquor has a caustic concentration of 170g/L or less and a temperature of 30 ℃ to 60 ℃.
In the embodiment of the application, the specific caustic alkali and the specific temperature of the Bayer process seed precipitation mother liquor are controlled, so that the mother liquor can fully react with the sodium oxalate remover, thereby effectively reducing the concentration of sodium oxalate in the mother liquor, and conveniently obtaining vanadium concentrate with high vanadium pentoxide content from the mother liquor after sodium oxalate removal.
In some alternative embodiments, the sodium oxalate removal agent is added in an amount of 3g/L to 10g/L.
In the embodiment of the application, the specific addition amount of the sodium oxalate remover is controlled, so that the concentration of sodium oxalate in the mother liquor can be effectively reduced, the subsequent crystallization reaction of the mother liquor and the vanadium salt seed crystal is convenient, and the vanadium concentrate with high vanadium pentoxide content is obtained.
In some alternative embodiments, the time for the sodium oxalate removal reaction is from 4 hours to 10 hours.
In the embodiment of the application, the specific time of the sodium oxalate removal reaction is controlled, so that the sodium oxalate and the sodium oxalate removal agent in the mother liquor are fully reacted, thereby obtaining the mother liquor with low sodium oxalate concentration, and vanadium concentrate with high vanadium pentoxide content is conveniently obtained from the mother liquor after sodium oxalate removal.
In some alternative embodiments, the concentrated mother liquor has a caustic concentration of 190g/L to 240g/L.
In the embodiment of the application, the specific caustic alkali concentration of the concentrated mother liquor is controlled, so that the mother liquor and the vanadium salt seed crystal are fully reacted, and the high-grade vanadium concentrate is obtained.
In some alternative embodiments, the reduced temperature is at an endpoint temperature of 25 ℃ to 60 ℃.
In the embodiment of the application, the specific end point temperature of the cooling is controlled, so that the temperature of the mother solution is suitable, and the mother solution can fully react with the vanadium salt seed crystal, thereby obtaining high-grade vanadium concentrate.
In some alternative embodiments, the crystallization reaction is for a period of time ranging from 5 hours to 15 hours.
In the embodiment of the application, the specific time of the crystallization reaction is controlled, so that the mother liquor and the vanadium salt seed crystal are fully reacted, and the high-grade vanadium concentrate is obtained.
In some alternative embodiments, the adding a sodium oxalate remover to the bayer process seed precipitation mother liquor to perform a sodium oxalate removal reaction, and then performing solid-liquid separation to obtain a mother liquor after sodium oxalate removal, including the steps of:
Adding a sodium oxalate removing agent into Bayer process seed precipitation mother liquor to perform sodium oxalate removal reaction, and then performing solid-liquid separation to respectively obtain mother liquor after sodium oxalate removal and sodium oxalate removal seed crystal;
And recycling the sodium oxalate removal seed crystal as a sodium oxalate removal agent.
In the embodiment of the application, the solid phase and the liquid phase after the sodium oxalate removal reaction are separated, so that the mother solution with low sodium oxalate concentration can be obtained, and the separated solid phase can be used as a sodium oxalate removal agent, so that the recycling of the reagent is realized.
In some alternative embodiments, evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystal into the concentrated mother solution for crystallization reaction, and performing solid-liquid separation to obtain high-grade vanadium concentrate, including the steps of:
Evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystals into the concentrated mother solution for crystallization reaction, and carrying out solid-liquid separation to obtain high-grade vanadium concentrate and separation solution respectively;
the separated solution is used as a raw material for alumina production.
In the embodiment of the application, the solid phase and the liquid phase after the crystallization reaction are separated, so that the solid phase of the high-grade vanadium concentrate and the liquid phase of the alumina mother solution with low sodium oxalate concentration and low vanadium concentration can be obtained, and the liquid phase can be used as a raw material for alumina production, so that a purer alumina production raw material can be obtained.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. The experimental procedures, which are not specified in the following examples, are generally determined according to national standards. If the corresponding national standard does not exist, the method is carried out according to the general international standard, the conventional condition or the condition recommended by the manufacturer.
Example 1
Selecting Bayer process seed precipitation mother liquor of an alumina plant, wherein the caustic alkali concentration is 145g/L, cooling to 30 ℃, adding 3g/L sodium oxalate remover into the mother liquor, carrying out pressure filtration on slurry after 4 hours of reaction to realize solid-liquid separation, and detecting that the sodium oxalate concentration in the mother liquor is reduced from 4.77g/L to 1.95g/L;
And continuously concentrating the filtrate obtained after filter pressing until the caustic alkali concentration of the solution is 192g/L, cooling to 25 ℃, adding vanadium salt seed crystals, crystallizing for 5 hours, pumping the slurry into a settling tank, performing filter pressing on the underflow of the settling tank to obtain vanadium concentrate with the V 2O5 content of 28.35% and the sodium oxalate content of 0.38%, and returning the overflow of the settling tank and the filtrate of the filter press to the alumina production flow.
Example 2
Example 2 and example 1 were compared, and the difference between example 2 and example 1 is that:
selecting Bayer process seed precipitation mother liquor of an alumina plant, wherein the caustic alkali concentration is 145g/L, adding 10g/L sodium oxalate remover into the mother liquor after cooling to 60 ℃, carrying out pressure filtration on slurry after reacting for 10 hours to realize solid-liquid separation, and detecting that the sodium oxalate concentration in the mother liquor is reduced from 4.69g/L to 1.83g/L;
Continuously concentrating the filtrate obtained after filter pressing until the caustic alkali concentration of the solution is 210g/L, cooling to 40 ℃, adding vanadium salt seed crystals, crystallizing for 10 hours, pumping the slurry into a settling tank, performing filter pressing on the underflow of the settling tank to obtain vanadium concentrate with the V 2O5 content of 27.98% and the sodium oxalate content of 0.54%, and returning the overflow of the settling tank and the filtrate of the filter press to the alumina production flow.
Example 3
Example 3 was compared with example 1, and the difference between example 3 and example 1 was:
Selecting a Bayer process seed precipitation mother liquor of an alumina plant, wherein the caustic alkali concentration is 165g/L, adding 10g/L sodium oxalate remover into the mother liquor after cooling to 40 ℃, carrying out pressure filtration on slurry after reacting 10 to realize solid-liquid separation, and detecting that the sodium oxalate concentration in the mother liquor is reduced from 4.23g/L to 1.45g/L;
continuously concentrating the filtrate obtained after filter pressing until the caustic alkali concentration of the solution is 238g/L, cooling to 60 ℃, adding vanadium salt seed crystals, crystallizing for 15 hours, pumping the slurry into a settling tank, performing filter pressing on the underflow of the settling tank to obtain vanadium concentrate with V 2O5 content of 26.92% and sodium oxalate content of 0.73%, and returning the overflow of the settling tank and the filtrate of the filter press to the alumina production flow.
Example 4
Selecting Bayer process seed precipitation mother liquor of an alumina plant, wherein the caustic alkali concentration is 168g/L, adding 10g/L sodium oxalate remover into the mother liquor after cooling to 30 ℃, carrying out pressure filtration on slurry after reacting for 6 hours to realize solid-liquid separation, and detecting that the sodium oxalate concentration in the mother liquor is reduced from 4.31g/L to 1.29g/L;
Continuously concentrating the filtrate obtained after filter pressing until the caustic alkali concentration of the solution is 240g/L, cooling to 40 ℃, adding vanadium salt seed crystals, crystallizing for 10 hours, pumping the slurry into a settling tank, performing filter pressing on the underflow of the settling tank to obtain vanadium concentrate with the V 2O5 content of 26.59% and the sodium oxalate content of 0.79%, and returning the overflow of the settling tank and the filtrate of the filter press to the alumina production flow.
Comparative example 1
The Bayer process seed precipitation mother liquor of an alumina plant is selected, the caustic alkali concentration of the seed precipitation mother liquor is 145g/L, the sodium oxalate concentration of the seed precipitation mother liquor is 4.77g/L, the seed precipitation mother liquor is directly concentrated to the caustic alkali concentration of the solution of 194g/L, the temperature is reduced to 25 ℃, then vanadium salt seed crystals are added, the slurry is pumped into a settling tank after 5 hours of crystallization, the underflow of the settling tank is subjected to filter pressing to obtain vanadium concentrate with the V 2O5 content of 14.47% and the sodium oxalate content of 11.95%, and the overflow of the settling tank and the filtrate of a filter press are returned to the alumina production flow.
Comparative example 2
The Bayer process seed precipitation mother liquor of an alumina plant is selected, the caustic alkali concentration of the seed precipitation mother liquor is 145g/L, the sodium oxalate concentration of the seed precipitation mother liquor is 4.69g/L, the caustic alkali concentration of the solution is 210g/L, the temperature is reduced to 40 ℃, vanadium salt seed crystals are added, the slurry is pumped into a settling tank after crystallization for 10 hours, the underflow of the settling tank is subjected to filter pressing to obtain vanadium concentrate with V 2O5 content of 13.35% and sodium oxalate content of 20.44%, and the overflow of the settling tank and the filtrate of a filter press are returned to the alumina production flow.
Comparative example 3
The Bayer process seed precipitation mother liquor of an alumina plant is selected, the caustic alkali concentration of the seed precipitation mother liquor is 165g/L, the sodium oxalate concentration of the seed precipitation mother liquor is 4.23g/L, the seed precipitation mother liquor is directly concentrated to the caustic alkali concentration of the solution of 238g/L, the temperature is reduced to 60 ℃, vanadium salt seed crystals are added, the slurry is pumped into a settling tank after 15 hours of crystallization, the underflow of the settling tank is subjected to filter pressing to obtain vanadium concentrate with V 2O5 content of 12.26% and sodium oxalate content of 16.54%, and the overflow of the settling tank and the filtrate of a filter press are returned to the alumina production flow.
Comparative example 4
Seed precipitation mother liquor of Bayer process in certain alumina plant is selected, the caustic alkali concentration is 168g/L, the sodium oxalate concentration is 4.31g/L, seed precipitation mother liquor is directly concentrated to the caustic alkali concentration of 240g/L, vanadium salt seed crystal is added after the temperature is reduced to 40 ℃, the slurry is pumped into a settling tank after 10 hours of crystallization, the underflow of the settling tank is filtered and pressed to obtain vanadium concentrate with V 2O5 content of 10.33% and sodium oxalate content of 35.77%, and the overflow of the settling tank and the filtrate of a filter press are returned to the alumina production flow.
In summary, the method provided by the embodiment of the application primarily purifies the mother liquor by removing sodium oxalate in the seed precipitation mother liquor, and then carries out evaporation concentration and cooling crystallization on the mother liquor after removing sodium oxalate to precipitate vanadium, thereby obtaining vanadium concentrate with vanadium pentoxide content of more than 25% and sodium oxalate content of less than 1.0%, and further obtaining vanadium concentrate with high vanadium pentoxide content.
Various embodiments of the application may exist in a range of forms; it should be understood that the description in a range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the application; it is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1,2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
In the present application, unless otherwise specified, terms such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present specification, the terms "include", "comprising" and the like mean "including but not limited to".
Relational terms such as "first" and "second", and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Herein, "and/or" describing an association relationship of an association object means that there may be three relationships, for example, a and/or B, may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. Herein, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
The foregoing is only a specific embodiment of the application to enable those skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (3)
1. A method of producing a high grade vanadium concentrate, the method comprising:
adding a sodium oxalate remover into Bayer process seed precipitation mother liquor to perform sodium oxalate removal reaction, and then performing solid-liquid separation to obtain mother liquor after sodium oxalate removal;
Evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystals into the concentrated mother solution for crystallization reaction, and carrying out solid-liquid separation to obtain high-grade vanadium concentrate, wherein the content of vanadium pentoxide in the high-grade vanadium concentrate is more than 25% and the content of sodium oxalate is less than 1.0%;
The caustic alkali concentration of the Bayer process seed precipitation mother liquor is less than or equal to 170g/L, the concentration of sodium oxalate in the Bayer process seed precipitation mother liquor is 4.77g/L, 4.69g/L, 4.23g/L or 4.31g/L, and the temperature of the Bayer process seed precipitation mother liquor is 30-60 ℃;
the adding amount of the sodium oxalate remover is 3 g/L-10 g/L;
the reaction time of removing sodium oxalate is 4-10 hours;
the concentration of caustic alkali in the concentrated mother liquor is 190 g/L-240 g/L;
the temperature of the cooling end point is 25-60 ℃;
Adding a sodium oxalate remover into Bayer process seed precipitation mother liquor to perform sodium oxalate removal reaction, and then performing solid-liquid separation to obtain mother liquor after sodium oxalate removal, wherein the method comprises the following steps:
Adding a sodium oxalate removing agent into Bayer process seed precipitation mother liquor to perform sodium oxalate removal reaction, and then performing solid-liquid separation to respectively obtain mother liquor after sodium oxalate removal and sodium oxalate removal seed crystal;
And recycling the sodium oxalate removal seed crystal as the sodium oxalate removal agent.
2. The method according to claim 1, wherein the crystallization reaction time is 5 to 15 hours.
3. The method of claim 1, wherein evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystal into the concentrated mother solution for crystallization reaction, and performing solid-liquid separation to obtain high-grade vanadium concentrate, comprising the steps of:
Evaporating and concentrating the mother solution after removing sodium oxalate, cooling, adding vanadium salt seed crystals into the concentrated mother solution for crystallization reaction, and carrying out solid-liquid separation to obtain high-grade vanadium concentrate and separation solution respectively;
the separated solution is used as a raw material for alumina production.
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| CN1887724A (en) * | 2006-07-14 | 2007-01-03 | 山东铝业股份有限公司 | Method of extracting vanadium from aluminium producing Bayer process |
| CN101302022A (en) * | 2008-06-30 | 2008-11-12 | 中国铝业股份有限公司 | Method for removing sodium oxalate from industrial sodium aluminate solution |
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| AU661486B2 (en) * | 1991-07-19 | 1995-07-27 | Particle Engineered Hydrates Pty Ltd | Recovery of vanadium and aluminium values |
| CN111573699A (en) * | 2020-05-22 | 2020-08-25 | 中国铝业股份有限公司 | Method for removing sodium oxalate in production process of aluminum oxide |
| CN115010174B (en) * | 2022-07-01 | 2023-09-26 | 中国铝业股份有限公司 | Separation method of low-grade vanadium slag |
| CN115448339A (en) * | 2022-08-29 | 2022-12-09 | 中铝郑州有色金属研究院有限公司 | Crude liquid purifying agent, preparation method thereof and application method thereof in alumina production process |
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| CN1887724A (en) * | 2006-07-14 | 2007-01-03 | 山东铝业股份有限公司 | Method of extracting vanadium from aluminium producing Bayer process |
| CN101302022A (en) * | 2008-06-30 | 2008-11-12 | 中国铝业股份有限公司 | Method for removing sodium oxalate from industrial sodium aluminate solution |
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