CN119972340A - Comprehensive recovery method of tantalum, niobium and tin from lithium slag - Google Patents

Comprehensive recovery method of tantalum, niobium and tin from lithium slag Download PDF

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Publication number
CN119972340A
CN119972340A CN202510177090.XA CN202510177090A CN119972340A CN 119972340 A CN119972340 A CN 119972340A CN 202510177090 A CN202510177090 A CN 202510177090A CN 119972340 A CN119972340 A CN 119972340A
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niobium
tantalum
tin
tailings
concentrate
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邓星星
殷志刚
张�杰
易鹏
何芋崎
高宜宝
卢茜
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Tianqi Lithium Corp
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Tianqi Lithium Corp
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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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Abstract

The invention relates to a comprehensive recovery method of lithium slag, in particular to a method for recovering tantalum, niobium and tin rare metal elements from lithium slag, and belongs to the technical field of lithium slag recovery. The invention solves the technical problem of providing a method for comprehensively recovering tantalum, niobium and tin from lithium slag with high recovery rate. According to the method, firstly, lithium slag is pulpified, classified and tailings are thrown, and then, the steps of gravity separation, grinding and magnetic separation are carried out on different particle sizes to obtain the tantalum-niobium-tin concentrate, so that the ore dressing cost can be greatly reduced, the separating efficiency can be improved, the loss of the tantalum-niobium-tin concentrate in the tailings in the fine particle size can be reduced, and the recovery rate of tantalum-niobium-tin can be improved. And the concentrate subjected to grading and tailing discarding is subjected to gravity separation by adopting different bed surface differential shaking tables according to different granularity, so that the grade and recovery rate of the tantalum-niobium-tin concentrate can be greatly improved, and the loss rate of fine-fraction tantalum-niobium-tin minerals in the gravity separation tailings of the shaking tables is reduced. The method can effectively separate the tantalum niobium tin, obtain the high-quality tantalum niobium concentrate and tin concentrate, and has high recovery rate.

Description

Method for comprehensively recovering tantalum, niobium and tin from lithium slag
Technical Field
The invention relates to a comprehensive recovery method of lithium slag, in particular to a method for recovering tantalum, niobium and tin rare metal elements from lithium slag, and belongs to the technical field of lithium slag recovery.
Background
Spodumene is an important lithium mineral, and the main component is lithium aluminosilicate, which is usually accompanied by valuable metals such as tantalum, niobium, tin and the like. With the wide application of lithium ion batteries, the demand of lithium is greatly increased, and the lithium extraction technology of spodumene is rapidly developed. The spodumene is used for extracting lithium, each time 1 ton of lithium carbonate is produced, 8-10 tons of lithium slag is produced, more than 500 ten thousand tons of spodumene smelting slag are produced per year in China calculated by the current lithium salt productivity, the (Ta+Nb) 2O5 content in the lithium slag is 100-180 ppm, the Sn content is 100-200 ppm, and the lithium slag has higher economic value even though the content of tantalum-niobium-tin elements is lower, and rare metals tantalum-niobium-tin in the lithium slag can be recycled economically and efficiently.
The analysis data of the main chemical components in a certain lithium slag are shown in table 1.
TABLE 1 analysis data of main chemical components in lithium slag
Component (A) SO3 Fe2O3 Al2O3 SiO2 Li2O K2O Na2O CaO
Content (%) 6.82 0.90 20.22 52.08 0.32 0.50 0.28 5.25
Component (A) MgO Ta2O5 Nb2O5 Sn B2O3 P2O5 TiO2 Loss on ignition
Content (%) 0.22 0.008 0.006 0.02 0.24 0.23 0.09 9.69
According to the research of lithium slag technology mineralogy, the lithium slag has low tantalum-niobium-tin content, the tantalum-niobium-tin is distributed and dispersed in each grain-level mineral, about 30% of the tantalum-niobium-tin mineral is distributed in the grain-level mineral below 20 mu m, and most of the tantalum-niobium-tin mineral in the lithium slag is wrapped by glass phase or is generated together with the glass phase, which is one of the main differences between the lithium slag and the original tantalum-niobium-tin mineral, and the complex embedding property of the tantalum-niobium-tin mineral in the lithium slag is the main reason for the great difficulty of recovering the tantalum-niobium-tin metal from the lithium slag.
For valuable metal recovery in lithium slag, the prior art mainly adopts methods of wet leaching, pyrometallurgy and the like. The wet leaching is to make the lithium slag contact with acid or alkali leaching agent to dissolve valuable metal in the solution, and then to recover valuable metal through extraction, precipitation and other processes. Pyrometallurgy is the melting of lithium slag at high temperatures, followed by the recovery of valuable metals by electrolysis or other means. The prior art has the problems of the prior lithium slag recovery valuable metal technology. First, existing methods such as wet leaching and pyrometallurgy generally require a large amount of chemical reagents and energy, are relatively costly, and are difficult to implement for large-scale industrial applications. Second, these methods may generate a large amount of waste water and waste gas during the recovery of valuable metals, which may pollute the environment. Finally, because the content of low-content valuable metals in the lithium slag is low, the conventional beneficiation method is difficult to realize high-efficiency recovery, and the recovery rate of the valuable metals is low, so that the resource waste is serious. Therefore, how to recycle low-content valuable metals in lithium slag with low cost and environmental protection is a problem to be solved in the current field.
Patent CN113976309A, CN117065916A, CN117165787A, CN116532235A relates to recycling of rare metal tantalum niobium in lithium slag, and is mainly recycled by adopting a magnetic separation and reselection process. Patent CN114226413a discloses a method for recovering tantalum and niobium from lithium slag by adopting floatation and gravity separation. The process has the advantages that the recovery rate of tantalum and niobium is low, the tantalum and niobium in the fine particle grade are difficult to recover, tin is not separated and recovered, the waste of tin resources is caused, high-quality tantalum and niobium concentrate is difficult to obtain, meanwhile, the rare metal tantalum and niobium and tin content in the raw materials is extremely low, the raw materials are directly subjected to a method for pre-enriching tantalum and niobium by magnetic separation or floatation, the treatment capacity is large, the separation cost is high, and the economy is poor.
Disclosure of Invention
Aiming at the defects, the invention solves the technical problem of providing a method for comprehensively recovering tantalum, niobium and tin from lithium slag with high recovery rate.
According to the method for comprehensively recovering tantalum, niobium and tin from lithium slag, the lithium slag is pulped and then classified to obtain coarse-size-fraction slurry and fine-size-fraction slurry, and then the coarse-size-fraction slurry and the fine-size-fraction slurry are subjected to tail discarding and reselection respectively to obtain the tantalum, niobium and tin mixed concentrate.
In one embodiment of the invention, the method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following steps:
s1, pulping, namely uniformly mixing water and lithium slag to obtain a slurry;
S2, grading, namely grading the slurry obtained in the step S1 to obtain coarse-fraction slurry and fine-fraction slurry respectively;
s3, performing coarse-grain-level slurry tailing discarding, namely performing tailing discarding on the coarse-grain-level slurry obtained in the step S2 to obtain coarse-grain-level tailing discarding concentrate and coarse-grain-level tailing discarding concentrate;
S4, fine-fraction sizing agent tailing discarding, namely performing tailing discarding on the fine-fraction sizing agent obtained in the step S2 to obtain fine-fraction tailing discarding concentrate and fine-fraction tailing discarding tailings;
s5, carrying out gravity separation on the coarse-fraction tailings, namely carrying out tantalum-niobium-tin gravity separation on the coarse-fraction tailings obtained in the step S3 to obtain gravity separation concentrate A, gravity separation middling A and gravity separation tailings A;
S6, performing gravity separation on the fine-fraction tailing-off concentrate, namely performing tantalum-niobium-tin gravity separation on the fine-fraction tailing-off concentrate in the step S4 to obtain gravity separation concentrate B, gravity separation middling B and gravity separation tailing B;
and S7, merging concentrate, namely merging the gravity concentrate A in the step S5 and the gravity concentrate B in the step S6 to obtain the tantalum-niobium-tin mixed concentrate.
In one embodiment of the present invention, in the step S1, the mass concentration of the slurry is 10% -60%. In some specific embodiments, in the step S1, the mass concentration of the slurry is 20% -40%.
In some embodiments of the invention, in the step S2, equipment adopted in classification comprises one or a combination of a hydrocyclone, a high-frequency vibration fine screen and a spiral classifier, wherein the classified granularity is 74-150 mu m.
In some embodiments of the present invention, in step S3, the equipment used for tail casting includes one or a combination of several of spiral chute, blanket machine, cloth laying chute, jigger. In some embodiments of the invention, the tailing removal rate of the tail-casting in the step S3 is 20% -98%. In some specific embodiments, the tailing discarding rate of the tailing discarding in the step S3 is 50% -90%.
In some embodiments of the invention, in step S4, the equipment used for tail casting includes one or a combination of several of spiral chute, blanket machine, cloth laying chute and jigger. In some embodiments of the invention, the tailing removal rate of the tail-casting in the step S4 is 20% -98%. In some specific embodiments, the tailing removal rate of the tail-casting in the step S4 is 50% -90%. In the step S5 and the step S6, the equipment adopted by the reselection respectively comprises one or a combination of a plurality of compound bed surface shaking tables, fine sand shaking tables, slurry shaking tables, suspension vibration cone concentrating machines and centrifuges.
In some embodiments of the present invention, in step S5 and step S6, the equipment used for reselection includes one or a combination of several of a composite bed surface cradle, a fine sand cradle, a slurry cradle, a suspension vibration cone concentrator, and a centrifuge, respectively.
In one embodiment of the invention, the method for comprehensively recovering tantalum, niobium and tin from lithium slag further comprises at least one of the following steps:
s8, carrying out treatment on the reselected middling A, namely concentrating and grinding the reselected middling A in the step S5, and returning to the step S4 for tail discarding after grinding;
s9, re-selecting the middling ore B, namely returning the re-selecting middling ore B in the step S6 to the step S4 for tail discarding.
In one embodiment of the invention, in the step S8, equipment adopted by concentration comprises one or a combination of a cyclone, a thickener and a thickener, grinding comprises one or a combination of ball mill grinding, vertical mill grinding and tower mill grinding, and the content of grinding fineness of 74 μm or less is 50% -100%. In a preferred embodiment, the content of the ore having a fineness of 74 μm or less is 80% to 95%.
In one embodiment of the invention, the method for comprehensively recovering tantalum, niobium and tin from lithium slag further comprises the steps of grinding and magnetic separation of the obtained tantalum, niobium and tin mixed concentrate to obtain tantalum, niobium concentrate and tin concentrate.
In one embodiment of the invention, the method for comprehensively recovering tantalum, niobium and tin from lithium slag specifically comprises the following steps:
s10, grinding, namely grinding the tantalum-niobium-tin mixed concentrate obtained in the step S7 to obtain fine-fraction tantalum-niobium-tin mixed concentrate;
S11, magnetically separating the fine-fraction tantalum-niobium-tin mixed concentrate obtained in the step S10 by strong magnetic separation to obtain a magnetic material and a non-magnetic material respectively, filtering to obtain tantalum-niobium concentrate and tin concentrate respectively, and enabling filtrate to enter a water return tank for recycling;
s12, tailings treatment, namely combining coarse-fraction tailings, fine-fraction tailings, gravity tailings A and gravity tailings B, filtering, taking filter residues as total tailings, and recycling filtrate in a backwater pool.
In a specific embodiment, in step S10, the grinding includes one or a combination of several of ball milling, vertical milling, tower milling. In one embodiment of the present invention, the fineness of the ground ore is 38 μm or less and the content thereof is 30 to 95%. In a preferred embodiment, the fineness of the ground ore is not more than 38 μm and the content is 70% -90%.
In a specific embodiment, in step S11, the apparatus used for strong magnetic separation includes one or a combination of several of a high gradient magnetic separator, a drum magnetic separator and a belt magnetic separator. In one embodiment of the invention, the magnetic field strength of the strong magnetic separation is 0.3T-1.5T. In a preferred embodiment, the magnetic field strength of the ferromagnetic separation is 0.8t to 1.2t.
In a specific embodiment, in the step S11 and the step S12, the filtering equipment comprises one or a combination of a plurality of ceramic filters, disc filters and plate-and-frame filter presses.
In one embodiment of the present invention, the recycling rate of the recycled water in both the step S11 and the step S12 is 100%.
Compared with the prior art, the invention has the following beneficial effects:
According to the method, firstly, the lithium slag is pulpified, classified and tailings are thrown, then the steps of re-selection, grinding and magnetic separation are carried out to obtain tantalum niobium tin concentrate, the lithium slag is presorted and tailings are thrown, and different tailings throwing equipment is selected for different particle grades, so that the feeding and feeding amount of tantalum niobium tin during deep enrichment can be greatly reduced, the beneficiation cost is reduced, the separation efficiency is improved, the loss of micro-particle-grade tantalum niobium tin concentrate in tailings can be reduced, and the recovery rate of tantalum niobium tin is improved. And the concentrate subjected to grading and tailing discarding is subjected to gravity separation by adopting different bed surface differential shaking tables according to different granularity, so that the grade and recovery rate of the tantalum-niobium-tin concentrate can be greatly improved, and the loss rate of fine-fraction tantalum-niobium-tin minerals in the gravity separation tailings of the shaking tables is reduced.
The method can effectively separate the tantalum, niobium and tin, so that the Sn content in the tantalum and niobium concentrate is less than 5%, the Ta 2O5 in the tin concentrate is less than 3%, and the Ta content (calculated by oxide) in the tin concentrate is less than 5%, the method can obtain high-quality tantalum and niobium concentrate and tin concentrate, the recovery rate is high, the Ta 2O5 grade of the tantalum and niobium concentrate is more than or equal to 20%, the Ta recovery rate is more than or equal to 60%, the Nb 2O5 grade is more than or equal to 14%, the Nb recovery rate is more than or equal to 55%, the Sn grade of the tin concentrate is more than or equal to 55%, and the tin recovery rate is more than or equal to 60%.
Drawings
FIG. 1 is a process flow diagram of a method for comprehensively recovering tantalum, niobium and tin from lithium slag in an embodiment of the invention.
Detailed Description
According to the method for comprehensively recovering tantalum, niobium and tin from lithium slag, the lithium slag is pulped and then classified to obtain coarse-size-fraction slurry and fine-size-fraction slurry, and then the coarse-size-fraction slurry and the fine-size-fraction slurry are subjected to tail discarding and reselection respectively to obtain the tantalum, niobium and tin mixed concentrate.
According to the method, the tailings are subjected to tailings discarding after being classified in advance, different tailings discarding equipment can be adopted for efficiently discarding the tailings aiming at the materials with different sizes, firstly, the processing capacity of the subsequent reselection process can be greatly reduced, the sorting efficiency of tantalum, niobium and tin is improved, secondly, the loss rate of tantalum, niobium and tin metals in tailings can be obviously reduced by adopting the corresponding tailings discarding equipment according to different mineral sizes, the loss rate of tantalum, niobium and tin metals in the tailings is less than 15%, if the lithium slag is not subjected to the tailings discarding treatment in advance in a classified manner, the loss rate of the tantalum, niobium and tin minerals with the fine size in the tailings discarding stage is high, the overall recovery rate of tantalum, niobium and tin is lower by 5-10%, and the main reason is that the content of the tantalum, niobium and tin minerals with the fine size in the tailings are distributed and dispersed in each size stage of the lithium slag, and the fine size tantalum, niobium and tin minerals are easy to be discarded together with coarse size gangue minerals in the tailings discarding process.
In addition, the concentrate after classified tailing discarding can be reselected by adopting different bed surfaces according to different granularity, so that the grade and recovery rate of the tantalum-niobium-tin concentrate can be greatly improved, and the loss rate of fine-grained tantalum-niobium-tin minerals in the tailing reselected by the cradle can be reduced. If the coarse and fine grain differential shaking table reselection is not carried out, the fine grain tantalum-niobium-tin minerals and the coarse grain gangue minerals cannot form zonation and enter the shaking table tailings for loss.
In some embodiments of the invention, the method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following steps:
s1, pulping, namely uniformly mixing water and lithium slag to obtain a slurry;
S2, grading, namely grading the slurry obtained in the step S1 to obtain coarse-fraction slurry and fine-fraction slurry respectively;
s3, performing coarse-grain-level slurry tailing discarding, namely performing tailing discarding on the coarse-grain-level slurry obtained in the step S2 to obtain coarse-grain-level tailing discarding concentrate and coarse-grain-level tailing discarding concentrate;
S4, fine-fraction sizing agent tailing discarding, namely performing tailing discarding on the fine-fraction sizing agent obtained in the step S2 to obtain fine-fraction tailing discarding concentrate and fine-fraction tailing discarding tailings;
s5, carrying out gravity separation on the coarse-fraction tailings, namely carrying out tantalum-niobium-tin gravity separation on the coarse-fraction tailings obtained in the step S3 to obtain gravity separation concentrate A, gravity separation middling A and gravity separation tailings A;
S6, performing gravity separation on the fine-fraction tailing-off concentrate, namely performing tantalum-niobium-tin gravity separation on the fine-fraction tailing-off concentrate in the step S4 to obtain gravity separation concentrate B, gravity separation middling B and gravity separation tailing B;
and S7, merging concentrate, namely merging the gravity concentrate A in the step S5 and the gravity concentrate B in the step S6 to obtain the tantalum-niobium-tin mixed concentrate.
And S1, pulping, namely uniformly mixing water and lithium slag to obtain a slurry. Clear water or backwater and lithium slag can be adopted for mixing, stirring and pulping. In one embodiment of the present invention, the mass concentration of the slurry is 10% -60%. In some specific embodiments, the mass concentration of the slurry is 20% -40%.
And S2, grading, namely grading the slurry obtained in the step S1 to obtain coarse-fraction slurry and fine-fraction slurry respectively. In this step, classification may be performed by using one or a combination of a hydrocyclone, a high-frequency vibrating fine screen, and a spiral classifier.
In some embodiments of the invention, the graded particle size is 74 μm to 150 μm. That is, classification may take any one of values of 74 μm to 150 μm as a criterion for classification, for example, a classified particle size of 74 μm, that is, particles having a particle size of 74 μm or more are coarse particles, particles having a particle size of less than 74 μm are fine particles, another example, a classified particle size of 150 μm, that is, particles having a particle size of 150 μm or more are coarse particles, particles having a particle size of less than 150 μm are fine particles, another example, a classified particle size of 100 μm, that is, particles having a particle size of 100 μm or more are coarse particles, particles having a particle size of less than 100 μm are fine particles, and so on, a classified particle size may be 75 μm, 80 μm, 85 μm, 90 μm, 95 μm, 100 μm, 105 μm, 110 μm, 115 μm, 120 μm, 125 μm, 130 μm, 135 μm, 140 μm, 145 μm, 150 μm, and so on.
And S3, performing tail discarding on the coarse-grain sizing agent obtained in the step S2 to obtain coarse-grain tail discarding concentrate and coarse-grain tail discarding tailings.
In some embodiments of the present invention, the equipment used for the tail-casting in step S3 includes one or a combination of several of a spiral chute, a blanket machine, a cloth laying chute, and a jigger. In some embodiments of the invention, the tailing removal rate of the tail-casting in the step S3 is 20% -98%. In some specific embodiments, the tailing discarding rate of the tailing discarding in the step S3 is 50% -90%.
And S4, fine-fraction slurry tailing discarding, namely performing tailing discarding on the fine-fraction slurry obtained in the step S2 to obtain fine-fraction tailing discarding concentrate and fine-fraction tailing discarding tailings.
And S4, the tail is thrown, and the adopted equipment and the specific tailing throwing rate can be the same as or different from those of the step S3. In some embodiments of the present invention, the equipment used for the tail-casting in step S4 includes one or a combination of several of a spiral chute, a blanket machine, a cloth laying chute, and a jigger. In some embodiments of the invention, the tailing removal rate of the tail-casting in the step S4 is 20% -98%. In some specific embodiments, the tailing removal rate of the tail-casting in the step S4 is 50% -90%.
And S5, carrying out gravity separation on the coarse-fraction tailing-off concentrate, and carrying out tantalum-niobium-tin gravity separation on the coarse-fraction tailing-off concentrate in the step S3 to obtain gravity separation concentrate A, gravity separation middling A and gravity separation tailing A. In some embodiments of the present invention, the equipment used in the step S5 reselection includes one or a combination of several of a composite bed surface cradle, a fine sand cradle, a slurry cradle, a suspension vibration cone concentrator, and a centrifuge, respectively.
And S6, performing gravity separation on the fine-fraction tailing-discarding concentrate, and performing tantalum-niobium-tin gravity separation on the fine-fraction tailing-discarding concentrate in the step S4 to obtain gravity separation concentrate B, gravity separation middling B and gravity separation tailing B. In some embodiments of the present invention, the equipment used in the step S6 reselection includes one or a combination of several of a composite bed surface cradle, a fine sand cradle, a slurry cradle, a suspension vibration cone concentrator, and a centrifuge, respectively.
And S7, merging the concentrates, and merging the gravity concentrate A in the step S5 and the gravity concentrate B in the step S6 to obtain the tantalum-niobium-tin mixed concentrate.
In one embodiment of the invention, the method for comprehensively recovering tantalum, niobium and tin from lithium slag further comprises at least one of the following steps:
s8, carrying out treatment on the reselected middling A, namely concentrating and grinding the reselected middling A in the step S5, and returning to the step S4 for tail discarding after grinding;
s9, re-selecting the middling ore B, namely returning the re-selecting middling ore B in the step S6 to the step S4 for tail discarding.
And (3) treating the gravity concentrate A or the gravity concentrate B, so that part of resources can be recovered. Wherein, the S8 step is the treatment of the gravity center A, and the S9 step is the treatment of the gravity center B. In one embodiment of the invention, in the step S8, equipment adopted by concentration comprises one or a combination of a cyclone, a thickener and a thickener, grinding comprises one or a combination of ball mill grinding, vertical mill grinding and tower mill grinding, the mineral content with the grinding fineness of less than 74 μm is 50% -100%, and in a preferred embodiment, the mineral content with the grinding fineness of less than 74 μm is 80% -95%.
In one embodiment of the invention, the method for comprehensively recovering tantalum, niobium and tin from lithium slag further comprises the steps of grinding and magnetic separation of the obtained tantalum, niobium and tin mixed concentrate to obtain tantalum, niobium concentrate and tin concentrate.
In one embodiment of the invention, the method for comprehensively recovering tantalum, niobium and tin from lithium slag specifically comprises the following steps:
s10, grinding, namely grinding the tantalum-niobium-tin mixed concentrate obtained in the step S7 to obtain fine-fraction tantalum-niobium-tin mixed concentrate;
S11, magnetically separating the fine-fraction tantalum-niobium-tin mixed concentrate obtained in the step S10 by strong magnetic separation to obtain a magnetic material and a non-magnetic material respectively, filtering to obtain tantalum-niobium concentrate and tin concentrate respectively, and enabling filtrate to enter a water return tank for recycling;
s12, tailings treatment, namely combining coarse-fraction tailings, fine-fraction tailings, gravity tailings A and gravity tailings B, filtering, taking filter residues as total tailings, and recycling filtrate in a backwater pool.
Through the steps S10-S12, the tantalum-niobium-tin mixed concentrate can be respectively recovered from the tantalum-niobium-tin mixed concentrate. Because the lithium slag and the primary ore are greatly different, most of tantalum-niobium-tin ore in the lithium slag is wrapped or continuously generated by glass phase substances, the mutual content of tantalum-niobium-tin in the concentrate after direct magnetic separation is high, and because tin in the tantalum-niobium concentrate and tantalum-niobium in the tin concentrate are often unable to be independently priced, so that resources are lost, the invention provides a fine grinding-strong magnetic process which can effectively separate tantalum-niobium-tin to obtain higher-quality tantalum-niobium concentrate and tin concentrate, wherein the Sn content in the tantalum-niobium concentrate is less than 5%, and Ta 2O5% in the tin concentrate is less than 3%.
And S10, grinding, namely grinding the tantalum-niobium-tin mixed concentrate in the step S7 to obtain fine-fraction tantalum-niobium-tin mixed concentrate. Grinding, which is commonly used in the art, is suitable for use in the present invention. In one embodiment, milling comprises one or a combination of several of ball milling, vertical milling, tower milling. In one embodiment of the present invention, the fineness of the ground ore is 38 μm or less and the content thereof is 30 to 95%. In a preferred embodiment, the fineness of the ground ore is not more than 38 μm and the content is 70% -90%.
And S11, carrying out magnetic separation, namely carrying out strong magnetic separation on the fine-fraction tantalum-niobium-tin mixed concentrate obtained in the step S10 to obtain a magnetic material and a non-magnetic material respectively, filtering to obtain tantalum-niobium concentrate and tin concentrate respectively, and enabling filtrate to enter a water return tank for recycling.
In one embodiment of the invention, the equipment used for the strong magnetic separation comprises one or a combination of a plurality of high-gradient magnetic separators, cylindrical magnetic separators and belt magnetic separators.
In one embodiment of the invention, the magnetic field strength of the strong magnetic separation is 0.3T-1.5T. In a preferred embodiment, the magnetic field strength of the ferromagnetic separation is 0.8t to 1.2t.
The filtering in step S11 may also be performed by a filtering method conventional in the art, and in some embodiments, the filtering apparatus includes one or a combination of several of a ceramic filter, a disc filter, and a plate-and-frame filter press.
And S12, tailings treatment, namely merging coarse-fraction tailings, fine-fraction tailings, gravity tailings A and gravity tailings B, filtering, taking filter residues as total tailings, and recycling filtrate in a water return tank. The filtering in this step may be the same as or different from the filtering in step S11, and in some embodiments, the filtering device includes one or a combination of several of a ceramic filter, a disc filter, and a plate-and-frame filter press.
In one embodiment of the present invention, the recycling rate of the recycled water in both the step S11 and the step S12 is 100%.
The following describes the invention in more detail with reference to examples, which are not intended to limit the invention thereto. The lithium slag used in the examples is shown in table 1.
Example 1
As shown in FIG. 1, the method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding clear water into the lithium slag to stir and pulping to prepare slurry with the mass concentration of 20%, and then, entering a hydrocyclone to perform pre-classification to obtain coarse-fraction slurry and fine-fraction slurry, wherein the classification granularity is 74 mu m;
(2) Carrying out tail-throwing operation on the coarse-grain-level slurry by adopting a spreading chute to obtain coarse-grain-level tail-throwing concentrate and coarse-grain-level tail-throwing tailings, wherein the tail-throwing rate of operation is 80%;
(3) Carrying out tail-casting operation on the fine-fraction slurry by adopting a blanket machine to obtain fine-fraction tail-casting concentrate and fine-fraction tail-casting tailings, wherein the operation tailing-casting rate is 80%;
(4) The coarse fraction tailing-throwing concentrate is subjected to gravity separation by adopting a mineral sand table to obtain coarse fraction tantalum-niobium-tin mixed concentrate, coarse fraction middling of the table and coarse fraction tailing of the table, grinding the coarse-grain middlings of the shaking table by adopting a ball mill until the content of the middlings is 80% below 74 mu m, and returning the middlings to the blanket machine for tail-throwing operation;
(5) The fine fraction tailing-throwing concentrate is subjected to gravity concentration by adopting a slurry type shaking table to obtain fine fraction tantalum-niobium-tin mixed concentrate, fine fraction middling and fine fraction tailing;
(6) Combining the coarse-grain tantalum-niobium-tin mixed concentrate and the fine-grain tantalum-niobium-tin mixed concentrate, and grinding by adopting a ball mill, wherein the grinding fineness is less than 38 mu m and the content is 70%;
(7) Carrying out high-intensity magnetic separation on the finely ground tantalum-niobium-tin mixed concentrate by adopting a high-gradient magnetic separator, wherein the magnetic field strength is 0.8T, respectively obtaining magnetic materials and non-magnetic materials, filtering to obtain tantalum-niobium concentrate and tin concentrate, and carrying out water return Chi Huiyong on filtrate;
(8) And combining and filtering all tailings to obtain total tailings, and enabling filtrate to enter a water return tank for recycling.
Example 2
As shown in FIG. 1, the method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding the lithium slag into backwater, stirring and pulping to prepare slurry with the mass concentration of 25%, and then, entering a spiral classifier for pre-classification to obtain coarse-fraction slurry and fine-fraction slurry, wherein the classification granularity is 100 mu m;
(2) Carrying out tail-casting operation on the coarse-grain slurry by adopting a waterfall chute to obtain coarse-grain tail-casting concentrate and coarse-grain tail-casting tailings, wherein the operation tailing-casting rate is 70%;
(3) Carrying out tail-casting operation on the fine-fraction slurry by adopting a blanket machine to obtain fine-fraction tail-casting concentrate and fine-fraction tail-casting tailings, wherein the operation tailing-casting rate is 85%;
(4) Re-selecting coarse-grain-level tailing-throwing concentrate by adopting a composite bed surface shaking table to obtain coarse-grain-level tantalum-niobium-tin mixed concentrate, shaking table coarse-grain-level middling and shaking table coarse-grain-level tailing, grinding the shaking table coarse-grain-level middling by adopting a ball mill until the content of the shaking table coarse-grain-level middling is 85% below 74 mu m, and returning to the blanket machine tailing-throwing operation;
(5) The fine fraction tailing-throwing concentrate is subjected to gravity concentration by adopting a slurry type shaking table to obtain fine fraction tantalum-niobium-tin mixed concentrate, fine fraction middling and fine fraction tailing;
(6) Combining the coarse-grain tantalum-niobium-tin mixed concentrate and the fine-grain tantalum-niobium-tin mixed concentrate, and grinding by a vertical mill, wherein the grinding fineness is less than 38 mu m and the content is 75%;
(7) Carrying out high-intensity magnetic separation on the finely ground tantalum-niobium-tin mixed concentrate by adopting a drum-type high-intensity magnetic separator, wherein the magnetic field intensity is 1.0T, respectively obtaining magnetic materials and non-magnetic materials, filtering to obtain tantalum-niobium concentrate and tin concentrate, and carrying out water return Chi Huiyong on filtrate;
(8) And combining and filtering all tailings to obtain total tailings, and enabling filtrate to enter a water return tank for recycling.
Example 3
As shown in FIG. 1, the method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding the lithium slag into backwater, stirring and pulping to prepare slurry with the mass concentration of 30%, and then, entering a high-frequency vibrating screen for pre-grading to obtain coarse-size slurry and fine-size slurry, wherein the grading granularity is 150 mu m;
(2) Carrying out tail-casting operation on the coarse-grain-grade slurry by adopting a spiral chute to obtain coarse-grain-grade tail-casting concentrate and coarse-grain-grade tail-casting tailings, wherein the tail-casting rate of operation tailings is 50%;
(3) Carrying out tail-casting operation on the fine-fraction slurry by adopting a blanket machine to obtain fine-fraction tail-casting concentrate and fine-fraction tail-casting tailings, wherein the operation tailing-casting rate is 90%;
(4) The coarse fraction tailing-throwing concentrate is subjected to gravity separation by adopting a mineral sand table to obtain coarse fraction tantalum-niobium-tin mixed concentrate, coarse fraction middling of the table and coarse fraction tailing of the table, grinding the coarse fraction middlings of the shaking table by adopting a ball mill until the content of the middlings is 90% below 74 mu m, and returning the middlings to the blanket machine for tail-throwing operation;
(5) The fine fraction tailing-throwing concentrate is subjected to gravity concentration by adopting a slurry type shaking table to obtain fine fraction tantalum-niobium-tin mixed concentrate, fine fraction middling and fine fraction tailing;
(6) Combining the coarse-grain tantalum-niobium-tin mixed concentrate and the fine-grain tantalum-niobium-tin mixed concentrate, and grinding by a vertical mill, wherein the grinding fineness is less than 38 mu m and the content is 80%;
(7) Carrying out high-intensity magnetic separation on the finely ground tantalum-niobium-tin mixed concentrate by adopting a high-gradient magnetic separator, wherein the magnetic field strength is 1.2T, respectively obtaining magnetic materials and non-magnetic materials, filtering to obtain tantalum-niobium concentrate and tin concentrate, and carrying out water return Chi Huiyong on filtrate;
(8) And combining and filtering all tailings to obtain total tailings, and enabling filtrate to enter a water return tank for recycling.
Example 4
As shown in FIG. 1, the method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding the lithium slag into backwater, stirring and pulping to prepare slurry with the mass concentration of 35%, and then entering a hydrocyclone for pre-grading to obtain coarse-fraction slurry and fine-fraction slurry, wherein the grading granularity is 74 mu m;
(2) Performing tail-casting operation on the coarse-grain-level slurry by adopting a spiral chute to obtain coarse-grain-level tail-casting concentrate and coarse-grain-level tail-casting tailings, wherein the operation tailing-casting rate is 80%;
(3) Carrying out tail-casting operation on the fine-fraction slurry by adopting a blanket machine to obtain fine-fraction tail-casting concentrate and fine-fraction tail-casting tailings, wherein the operation tailing-casting rate is 90%;
(4) The coarse fraction tailing-throwing concentrate is subjected to gravity separation by adopting a mineral sand table to obtain coarse fraction tantalum-niobium-tin mixed concentrate, coarse fraction middling of the table and coarse fraction tailing of the table, grinding the coarse fraction middlings of the shaking table by adopting a ball mill until the content of the middlings is 95% below 74 mu m, and returning the middlings to the blanket machine for tail-throwing operation;
(5) The fine fraction tailing-throwing concentrate is subjected to gravity concentration by adopting a composite bed surface shaking table to obtain fine fraction tantalum-niobium-tin mixed concentrate, fine fraction middling and fine fraction tailing;
(6) Combining the coarse-grain tantalum-niobium-tin mixed concentrate and the fine-grain tantalum-niobium-tin mixed concentrate, and grinding by adopting a tower mill, wherein the grinding fineness is less than 38 mu m and the content is 85%;
(7) Carrying out high-intensity magnetic separation on the tantalum-niobium-tin mixed concentrate after grinding by adopting a belt type high-intensity magnetic separator, wherein the magnetic field intensity is 1.0T, respectively obtaining magnetic materials and non-magnetic materials, filtering to obtain tantalum-niobium concentrate and tin concentrate, and carrying out water return Chi Huiyong on filtrate;
(8) And combining and filtering all tailings to obtain total tailings, and enabling filtrate to enter a water return tank for recycling.
Example 5
As shown in FIG. 1, the method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding the lithium slag into backwater, stirring and pulping to prepare slurry with the mass concentration of 40%, and then entering a hydrocyclone for pre-grading to obtain coarse-fraction slurry and fine-fraction slurry, wherein the grading granularity is 74 mu m;
(2) Performing tail-casting operation on the coarse-grain-level slurry by adopting a spiral chute to obtain coarse-grain-level tail-casting concentrate and coarse-grain-level tail-casting tailings, wherein the operation tailing-casting rate is 80%;
(3) Carrying out tail-casting operation on the fine-fraction slurry by adopting a blanket machine to obtain fine-fraction tail-casting concentrate and fine-fraction tail-casting tailings, wherein the operation tailing-casting rate is 90%;
(4) The coarse fraction tailing-throwing concentrate is subjected to gravity separation by adopting a mineral sand table to obtain coarse fraction tantalum-niobium-tin mixed concentrate, coarse fraction middling of the table and coarse fraction tailing of the table, grinding the coarse-grain middlings of the shaking table by adopting a ball mill until the content of the middlings is 90 percent below 74 mu m, and returning the middlings to the blanket machine for tail-throwing operation;
(5) The fine fraction tailing-throwing concentrate is subjected to gravity concentration by adopting a slurry type shaking table to obtain fine fraction tantalum-niobium-tin mixed concentrate, fine fraction middling and fine fraction tailing;
(6) Combining the coarse-grain tantalum-niobium-tin mixed concentrate and the fine-grain tantalum-niobium-tin mixed concentrate, and grinding by adopting a ball mill, wherein the content of the grinding fineness is less than 38 mu m and is 90%;
(7) Carrying out high-intensity magnetic separation on the finely ground tantalum-niobium-tin mixed concentrate by adopting a high-gradient magnetic separator, wherein the magnetic field strength is 1.2T, respectively obtaining magnetic materials and non-magnetic materials, filtering to obtain tantalum-niobium concentrate and tin concentrate, and carrying out water return Chi Huiyong on filtrate;
(8) And combining and filtering all tailings to obtain total tailings, and enabling filtrate to enter a water return tank for recycling.
Comparative example 1
The method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding clear water into the lithium slag, stirring and pulping to prepare slurry with the mass concentration of 30%;
(2) Performing tail discarding on the slurry by adopting high-gradient strong magnetic separation, wherein the magnetic field strength is 1.5T, and obtaining magnetic concentrate and magnetic tailings, and the yield of the magnetic tailings is 80%;
(3) The magnetic concentrate is subjected to gravity separation by adopting a composite bed surface shaking table to obtain tantalum-niobium-tin mixed concentrate, middling and tailings, and the middling is returned to the magnetic separation tailing discarding operation;
(4) And carrying out high-intensity magnetic separation on the tantalum-niobium-tin mixed concentrate by adopting a high-gradient magnetic separator, wherein the magnetic field strength is 1.0T, and respectively obtaining the tantalum-niobium concentrate and the tin concentrate.
Comparative example 2
The method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding clear water into the lithium slag, stirring and pulping to prepare slurry with the mass concentration of 30%;
(2) Pumping the slurry into a flotation machine, adding 200g/t of styrene phosphoric acid serving as a tantalum-niobium flotation reagent, performing tantalum-niobium flotation by adopting a 1-coarse 2-sweep 3-fine process, wherein a flotation foam product is tantalum-niobium-tin rough concentrate, and a flotation underflow is tailings;
(3) The tantalum-niobium rough concentrate is subjected to gravity separation by adopting a composite bed surface table to obtain tantalum-niobium-tin concentrate, middling and tailings, and the middling is returned to flotation operation;
(4) And carrying out high-intensity magnetic separation on the tantalum-niobium-tin mixed concentrate by adopting a high-gradient magnetic separator, wherein the magnetic field strength is 1.0T, and respectively obtaining the tantalum-niobium concentrate and the tin concentrate.
Comparative example 3
The method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding clear water into the lithium slag, stirring and pulping to prepare slurry with the mass concentration of 30%;
(2) Performing tail-casting operation on the slurry by adopting a spiral chute to obtain tail-casting concentrate and tail-casting tailings, wherein the tail-casting rate is 80%;
(3) Gravity separation is carried out on the tailing-throwing concentrate by adopting a composite bed surface shaking table to obtain tantalum-niobium-tin mixed concentrate, shaking table middlings and shaking table tailings, the shaking table middlings are ground by adopting a ball mill until the content of the middlings is 80% below 74 mu m, and then the middlings return to spiral chute tailing-throwing operation;
(4) And carrying out high-intensity magnetic separation on the tantalum-niobium-tin mixed concentrate by adopting a high-gradient magnetic separator, wherein the magnetic field strength is 1.0T, and respectively obtaining the tantalum-niobium concentrate and the tin concentrate.
Comparative example 4
The method for comprehensively recovering tantalum, niobium and tin from lithium slag comprises the following implementation steps:
(1) Adding clear water into the lithium slag, stirring and pulping to prepare slurry with the mass concentration of 30%;
(2) Performing tail-casting operation on the slurry by adopting a spiral chute to obtain tail-casting concentrate and tail-casting tailings, wherein the tail-casting rate is 80%;
(3) Gravity separation is carried out on the tailing-throwing concentrate by adopting a composite bed surface shaking table to obtain tantalum-niobium-tin mixed concentrate, shaking table middlings and shaking table tailings, the shaking table middlings are ground by adopting a ball mill until the content of the middlings is 80% below 74 mu m, and then the middlings return to spiral chute tailing-throwing operation;
(4) Grinding the tantalum-niobium-tin mixed concentrate by adopting a vertical mill, wherein the grinding fineness is less than 38 mu m and the content is 90%;
(5) And carrying out high-intensity magnetic separation on the finely ground tantalum-niobium-tin mixed concentrate by adopting a high-gradient magnetic separator, wherein the magnetic field strength is 1.0T, and respectively obtaining the tantalum-niobium concentrate and the tin concentrate.
The component contents of the tantalum-niobium concentrate and the tin concentrate obtained in examples and comparative examples were measured, and the results thereof are shown in Table 2.
Table 2 tantalum niobium tin index for examples and comparative examples
As can be seen from the comparison between examples 1-5 and comparative example 1, the recovery rate of tin can be higher by adopting the gravity separation tail-out process than the magnetic separation tail-out process, and the loss of tin in the tail-out process is larger due to the fact that part of cassiterite in the lithium slag is non-magnetic. The recovery rate of tantalum and niobium in the magnetic separation and tail discarding process is lower.
As can be seen from the comparison of examples 1-5 and comparative example 2, the recovery rate of tantalum, niobium and tin is far lower than that of the examples by adopting the floatation process for optimized enrichment, and the main reason is that the lithium slag is the product of spodumene subjected to high-temperature roasting and acid leaching to leach lithium, so that the physical and chemical properties of the surface of the tantalum, niobium and tin ore are changed after the lithium is extracted, and the floatation recovery rate is lower.
Through examples 1-5 and comparative example 3, the tantalum-niobium-tin concentrate is separated by adopting fine grinding and magnetic separation processes, so that the mutual content of tantalum-niobium and tin in the tantalum-niobium concentrate and the tin concentrate can be reduced, and the tantalum-niobium concentrate with Sn being less than 5% and the tin concentrate with Ta2O5 being less than 3% are obtained.
As can be seen from the comparison of examples 1-5 and comparative example 4, the recovery rate of the tantalum-niobium-tin mixed concentrate can be improved by 5-10% by adopting the process of pre-grading and re-selecting the tail-casting compared with the non-grading direct tail-casting process in comparative example 4.

Claims (9)

1.锂渣综合回收钽铌锡的方法，其特征在于：先将锂渣制浆后进行分级，得到粗粒级浆料和细粒级浆料，再分别对粗粒级浆料和细粒级浆料进行抛尾和重选，得到钽铌锡混合精矿。1. A method for comprehensive recovery of tantalum, niobium and tin from lithium slag, characterized in that: the lithium slag is first pulped and then classified to obtain coarse-grained slurry and fine-grained slurry, and then the coarse-grained slurry and the fine-grained slurry are respectively subjected to tailings discarding and gravity separation to obtain a tantalum, niobium and tin mixed concentrate. 2.根据权利要求1所述的锂渣综合回收钽铌锡的方法，其特征在于：具体包括以下步骤：2. The method for comprehensive recovery of tantalum, niobium and tin from lithium slag according to claim 1 is characterized in that it specifically comprises the following steps: S1、制浆：将水和锂渣混匀，得到浆料；S1. Slurrying: mixing water and lithium slag to obtain slurry; S2、分级：将S1步骤的浆料进行分级，分别得到粗粒级和细粒级的浆料；S2, classification: Classifying the slurry in step S1 to obtain coarse-grained and fine-grained slurries respectively; S3、粗粒级浆料抛尾：将S2步骤所述的粗粒级浆料进行抛尾，得到粗粒级抛尾精矿和粗粒级抛尾尾矿；S3, coarse-grained slurry tailings disposal: the coarse-grained slurry described in step S2 is subjected to tailings disposal to obtain coarse-grained tailings concentrate and coarse-grained tailings; S4、细粒级浆料抛尾：将S2步骤所述的细粒级浆料进行抛尾，得到细粒级抛尾精矿和细粒级抛尾尾矿；S4, fine-grained slurry tailings disposal: the fine-grained slurry described in step S2 is subjected to tailings disposal to obtain fine-grained tailings concentrate and fine-grained tailings disposal; S5、粗粒级抛尾精矿重选：将S3步骤所述的粗粒级抛尾精矿进行钽铌锡重选，得到重选精矿A、重选中矿A和重选尾矿A；S5, coarse-grained tailings concentrate gravity separation: the coarse-grained tailings concentrate described in step S3 is subjected to tantalum, niobium and tin gravity separation to obtain gravity separation concentrate A, gravity separation ore A and gravity separation tailings A; S6、细粒级抛尾精矿重选：将S4步骤所述的细粒级抛尾精矿进行钽铌锡重选，得到重选精矿B、重选中矿B和重选尾矿B；S6, gravity separation of fine-grained tailings concentrate: The fine-grained tailings concentrate described in step S4 is subjected to gravity separation of tantalum, niobium and tin to obtain gravity separation concentrate B, gravity separation ore B and gravity separation tailings B; S7、精矿合并：将S5步骤所述的重选精矿A和S6步骤所述的重选精矿B合并，得到钽铌锡混合精矿。S7. Concentrate merging: The gravity-separated concentrate A described in step S5 and the gravity-separated concentrate B described in step S6 are combined to obtain a tantalum, niobium and tin mixed concentrate. 3.根据权利要求2所述的锂渣综合回收钽铌锡的方法，其特征在于：S1步骤中，所述浆料的质量浓度为10％～60％；优选所述浆料的质量浓度为20％～40％；3. The method for comprehensive recovery of tantalum, niobium and tin from lithium slag according to claim 2, characterized in that: in step S1, the mass concentration of the slurry is 10% to 60%; preferably, the mass concentration of the slurry is 20% to 40%; S2步骤中，分级采用的设备包括水力旋流器、高频振动细筛、螺旋分级机的一种或几种组合；分级的粒度为74μm～150μm；In step S2, the equipment used for classification includes one or a combination of a hydrocyclone, a high-frequency vibrating fine screen, and a spiral classifier; the particle size of the classification is 74 μm to 150 μm; S3步骤中，抛尾采用的设备包括螺旋溜槽、毛毯机、铺布溜槽、跳汰机的一种或几种组合；抛尾的尾矿抛除率为20％～98％；优选抛尾的尾矿抛除率为50％～90％；In step S3, the equipment used for tailings removal includes one or a combination of a spiral chute, a blanket machine, a cloth chute, and a jig; the tailings removal rate of tailings removal is 20% to 98%; preferably, the tailings removal rate of tailings removal is 50% to 90%; S4步骤中，抛尾采用的设备包括螺旋溜槽、毛毯机、铺布溜槽、跳汰机的一种或几种组合；抛尾的尾矿抛除率为20％～98％；优选抛尾的尾矿抛除率为50％～90％；In step S4, the equipment used for tailings removal includes one or a combination of a spiral chute, a blanket machine, a cloth chute, and a jig; the tailings removal rate of tailings removal is 20% to 98%; preferably, the tailings removal rate of tailings removal is 50% to 90%; S5步骤和S6步骤中，重选采用的设备分别包括复合床面摇床、细砂摇床、矿泥摇床、悬振圆锥选矿机、离心机中的一种或几种组合。In step S5 and step S6, the equipment used for gravity separation includes one or a combination of a composite bed shaking table, a fine sand shaking table, a sludge shaking table, a suspended vibration cone concentrator, and a centrifuge. 4.根据权利要求2所述的锂渣综合回收钽铌锡的方法，其特征在于：还包括以下步骤中的至少一个：4. The method for comprehensive recovery of tantalum, niobium and tin from lithium slag according to claim 2, characterized in that it also includes at least one of the following steps: S8、重选中矿A处理：将S5步骤所述的重选中矿A进行浓缩、磨矿，磨细后返回至S4步骤进行抛尾；S8, treatment of the gravity separation ore A: concentrating and grinding the gravity separation ore A described in step S5, and returning the ground ore to step S4 for tailings discarding; S9、重选中矿B处理：将S6步骤所述的重选中矿B，返回至S4步骤进行抛尾。S9, processing of the re-selected ore B: returning the re-selected ore B described in step S6 to step S4 for tailings discarding. 5.根据权利要求4所述的锂渣综合回收钽铌锡的方法，其特征在于：5. The method for comprehensive recovery of tantalum, niobium and tin from lithium slag according to claim 4, characterized in that: S8步骤中，浓缩采用的设备包括旋流器、浓缩机、浓密机的一种或几种组合；磨矿包括球磨磨矿、立磨磨矿、塔磨磨矿的一种或几种组合；磨矿细度为74μm以下的含量为50％～100％，优选74μm以下的含量为80％～95％。In step S8, the equipment used for concentration includes one or a combination of a cyclone, a concentrator, and a thickener; the grinding includes one or a combination of ball grinding, vertical grinding, and tower grinding; the content of grinding fineness below 74 μm is 50% to 100%, and preferably the content below 74 μm is 80% to 95%. 6.根据权利要求1或2所述的锂渣综合回收钽铌锡的方法，其特征在于：还包括将得到的钽铌锡混合精矿进行磨矿、磁选，得到钽铌精矿和锡精矿。6. The method for comprehensive recovery of tantalum, niobium and tin from lithium slag according to claim 1 or 2 is characterized by: it also includes grinding and magnetic separation of the obtained tantalum, niobium and tin mixed concentrate to obtain tantalum, niobium and tin concentrate. 7.根据权利要求6所述的锂渣综合回收钽铌锡的方法，其特征在于：具体包括以下步骤：7. The method for comprehensive recovery of tantalum, niobium and tin from lithium slag according to claim 6, characterized in that it specifically comprises the following steps: S10、磨矿：将钽铌锡混合精矿进行磨矿，得到细粒级钽铌锡混合精矿；S10, grinding: grinding the tantalum, niobium and tin mixed concentrate to obtain a fine-grained tantalum, niobium and tin mixed concentrate; S11、磁选：将S10步骤所述的细粒级钽铌锡混合精矿进行强磁磁选，分别得到磁性料和非磁性料，过滤后分别得到钽铌精矿和锡精矿，滤液进入到回水池进行循环利用；S11, magnetic separation: subjecting the fine-grained tantalum, niobium and tin mixed concentrate described in step S10 to strong magnetic separation to obtain magnetic material and non-magnetic material respectively, and filtering to obtain tantalum and niobium concentrate and tin concentrate respectively, and the filtrate enters the return water pool for recycling; S12、尾矿处理：将粗粒级抛尾尾矿、细粒级抛尾尾矿、重选尾矿A和重选尾矿B合并进行过滤，滤渣作为总尾矿，滤液进入到回水池循环利用。S12. Tailings treatment: The coarse-grained tailings, fine-grained tailings, gravity-separation tailings A and gravity-separation tailings B are combined and filtered, and the filter residue is used as the total tailings. The filtrate enters the recycle pool for recycling. 8.根据权利要求7所述的锂渣综合回收钽铌锡的方法，其特征在于：8. The method for comprehensive recovery of tantalum, niobium and tin from lithium slag according to claim 7, characterized in that: S10步骤中，磨矿包括球磨磨矿、立磨磨矿、塔磨磨矿的一种或几种组合；磨矿的细度为38μm以下含量为30～95％，优选磨矿的细度38μm以下含量为70％～90％；In step S10, the grinding includes one or a combination of ball milling, vertical milling, and tower milling; the grinding fineness is below 38 μm and the content is 30-95%, preferably the grinding fineness is below 38 μm and the content is 70%-90%; S11步骤中，强磁磁选采用的设备包括高梯度磁选机、筒式磁选机、带式磁选机的一种或几种组合；强磁磁选的磁场强度为0.3T～1.5T，优选强磁磁选的磁场强度为0.8T～1.2T；In step S11, the equipment used for high-intensity magnetic separation includes one or a combination of high-gradient magnetic separator, drum magnetic separator, and belt magnetic separator; the magnetic field strength of the high-intensity magnetic separation is 0.3T to 1.5T, and preferably the magnetic field strength of the high-intensity magnetic separation is 0.8T to 1.2T; S11步骤和S12步骤中，过滤采用的设备分别包括陶瓷过滤机、盘式过滤机、板框压滤机中的一种或几种组合。In step S11 and step S12, the filtering equipment used includes one or a combination of ceramic filter, disc filter, plate and frame filter press. 9.根据权利要求7所述的锂渣综合回收钽铌锡的方法，其特征在于：S11步骤和S12步骤中，回水的循环利用率为100％。9. The method for comprehensive recovery of tantalum, niobium and tin from lithium slag according to claim 7, characterized in that in steps S11 and S12, the recycling rate of returned water is 100%.
CN202510177090.XA 2025-02-18 2025-02-18 Comprehensive recovery method of tantalum, niobium and tin from lithium slag Pending CN119972340A (en)

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Citations (8)

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Publication number Priority date Publication date Assignee Title
CN103846154A (en) * 2012-12-05 2014-06-11 核工业北京地质研究院 Method of recycling tin, niobium and tantalum from smelted tailings
CN108147658A (en) * 2018-01-17 2018-06-12 税欣 A kind of high-valued method of comprehensive utilization of lithium slag
CN113083510A (en) * 2021-04-07 2021-07-09 宜春市金地锂业有限公司 Method for efficiently recycling tantalum, niobium and tin from lepidolite ore
CN113976309A (en) * 2021-12-01 2022-01-28 天齐创锂科技(深圳)有限公司 Method for comprehensively recovering lithium, tantalum-niobium, silicon-aluminum micro powder, iron ore concentrate and gypsum from lithium slag
CN116510885A (en) * 2023-04-27 2023-08-01 湖南紫金锂业有限公司 Classification and separation method for comprehensive recovery of lithium, tin and tungsten from lithium polymetallic ore
CN116832957A (en) * 2023-07-11 2023-10-03 长沙有色冶金设计研究院有限公司 Mineral separation method of lepidolite ore
CN118698721A (en) * 2024-07-24 2024-09-27 中南大学 Iron lithium mica collector, method for efficient comprehensive recovery of low-grade lithium tungsten tin polymetallic ore
CN119259240A (en) * 2024-09-24 2025-01-07 宜春江理锂电新能源产业研究院 A method for comprehensive recovery of tantalum, niobium and tin from lithium mica flotation tailings

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103846154A (en) * 2012-12-05 2014-06-11 核工业北京地质研究院 Method of recycling tin, niobium and tantalum from smelted tailings
CN108147658A (en) * 2018-01-17 2018-06-12 税欣 A kind of high-valued method of comprehensive utilization of lithium slag
CN113083510A (en) * 2021-04-07 2021-07-09 宜春市金地锂业有限公司 Method for efficiently recycling tantalum, niobium and tin from lepidolite ore
CN113976309A (en) * 2021-12-01 2022-01-28 天齐创锂科技(深圳)有限公司 Method for comprehensively recovering lithium, tantalum-niobium, silicon-aluminum micro powder, iron ore concentrate and gypsum from lithium slag
CN116510885A (en) * 2023-04-27 2023-08-01 湖南紫金锂业有限公司 Classification and separation method for comprehensive recovery of lithium, tin and tungsten from lithium polymetallic ore
CN116832957A (en) * 2023-07-11 2023-10-03 长沙有色冶金设计研究院有限公司 Mineral separation method of lepidolite ore
CN118698721A (en) * 2024-07-24 2024-09-27 中南大学 Iron lithium mica collector, method for efficient comprehensive recovery of low-grade lithium tungsten tin polymetallic ore
CN119259240A (en) * 2024-09-24 2025-01-07 宜春江理锂电新能源产业研究院 A method for comprehensive recovery of tantalum, niobium and tin from lithium mica flotation tailings

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