CN114752785B - Application of inorganic adsorbent and continuous fluid separation combined process in brine lithium extraction - Google Patents
Application of inorganic adsorbent and continuous fluid separation combined process in brine lithium extraction Download PDFInfo
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- CN114752785B CN114752785B CN202210382177.7A CN202210382177A CN114752785B CN 114752785 B CN114752785 B CN 114752785B CN 202210382177 A CN202210382177 A CN 202210382177A CN 114752785 B CN114752785 B CN 114752785B
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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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
- 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
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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Abstract
The invention discloses an application of an inorganic adsorbent and continuous fluid separation combined process in extracting lithium from brine, wherein lithium-containing brine enters the adsorbent to be separated from magnesium, sodium and potassium components in raw materials through a continuous fluid separation system filled with inorganic ion adsorbent filler, and lithium ions on the adsorbent filler are eluted through an analytical agent to obtain a high-concentration lithium-rich solution. The continuous fluid separation system is internally provided with a plurality of separation units, each separation unit is filled with manganese adsorbent filler, and comprises an exchange area, an exchange water washing area, an acid regeneration analysis area and a water acid washing area; the exchange area, the exchange water washing area, the acid regeneration analysis area and the water washing acid area are sequentially arranged along the circumference clockwise direction; the invention achieves the purposes of reducing production cost, simplifying production method, shortening production period, increasing lithium-magnesium ratio and increasing total yield.
Description
Technical Field
The invention relates to the technical field of product fluid separation, in particular to application of an inorganic adsorbent and continuous fluid separation combined process in brine lithium extraction.
Background
Lithium is a novel clean energy source, is an important raw material for power batteries, and has huge market demand space. Global lithium resources are statistically divided into two major categories, salt lake resources and ore resources. Wherein, lithium resources in the salt lake brine and the underground brine account for more than 60 percent. The salt lake brine mainly utilizes a salt field to separate a large amount of sodium salt and potassium salt through solar evaporation due to coexistence of lithium and a large amount of sodium, potassium, magnesium and other components, the lithium is enriched in evaporation mother liquor, and a large amount of lithium resources are lost due to entrainment of a large amount of sodium salt, potassium salt and other solids. The lithium manganate adsorbent, the lithium titanate adsorbent and the aluminum adsorbent inorganic ion adsorbent are ion sieves with memory effect, have the characteristics of high selectivity, high efficiency and the like, and can solve the problem of separating lithium from a large amount of magnesium, sodium, potassium and other components in brine. Realize direct separation and extraction of lithium from salt lake brine to prepare lithium carbonate and other lithium salt products. The adsorption extraction technology generally adopts column type device equipment, and because the adsorbent is huge in volume and multiple columns are connected in series or in parallel according to the process requirement, the adsorption analysis operation state of each column needs to be continuously changed and switched in continuous operation, so that the equipment connecting pipeline is complex, and the control difficulty is high. Aiming at the defects of the existing lithium extraction technology, the invention combines the high-efficiency inorganic lithium ion adsorbent with the novel continuous ion exchange system, establishes a combined technology of separating the inorganic lithium ion adsorbent from continuous fluid, is used for directly extracting lithium from salt lake brine and underground brine, and the application of the technology can promote the efficiency of extracting lithium from salt lake to be greatly improved, and the cost is hopeful to be further reduced.
Disclosure of Invention
The invention aims to provide an application of an inorganic adsorbent and continuous fluid separation combined process in extracting lithium from brine, so as to achieve the purposes of reducing production cost, simplifying production method, shortening production period, increasing lithium-magnesium ratio and increasing total yield.
The invention is realized by the following technical scheme:
an application of an inorganic adsorbent and continuous fluid separation combined process in extracting lithium from brine, wherein: the lithium-containing brine is separated from magnesium, sodium and potassium components in raw materials by a continuous fluid separation system filled with inorganic ion adsorbent filler, and lithium ions on the adsorbent filler are eluted by an analytical agent to obtain a high-concentration lithium-rich solution.
Further, a plurality of separation units are arranged in the continuous fluid separation system, each separation unit is filled with manganese adsorbent filler, and the continuous fluid separation system comprises an exchange area, an exchange water washing area, an acid regeneration analysis area and a water acid washing area; the exchange area, the exchange water washing area, the acid regeneration analysis area and the water washing acid area are sequentially arranged along the circumference clockwise direction.
Further, the exchange area adopts a combination mode of serial connection and parallel connection for feeding, lithium ions in brine are adsorbed, and the feed liquid firstly enters a first group of parallel columns to be fully contacted with the manganese adsorbent; the tail liquid containing a small amount of lithium ions flows out into the subsequent parallel columns to be subjected to secondary adsorption, so that the finally discharged adsorption tail liquid only contains a small amount of lithium or does not contain lithium.
Further, after the brine is exchanged by the manganese-based adsorbent, the adsorbent loses the exchange capacity and needs to be regenerated and resolved, and as the brine stock solution still remains in the column, the raw materials in the column need to be washed out; the exchange water washing area adopts a mode that a plurality of columns are connected in series to carry out gradient water washing, and dilute materials washed out by water are put on the columns again or enter raw material liquid to dilute the raw material liquid, so that crystallization precipitation can not occur in the process.
Further, the acid regeneration analysis area and the water acid washing area adopt a reverse analysis mode, so that the resin is in a semi-fluidization state in the analysis process, the analysis speed is improved, and the dissolution loss of the resin is reduced; after the resin is resolved, the resolving agent is rapidly discharged out of the system, and the residual resolving agent is cleaned by water.
Further, the inorganic ion adsorbent is a lithium manganate adsorbent, and the adsorbent adopts a granulation technology, so that the density and the particle size of the adsorbent are required to meet the requirement that the adsorbent forms a semi-fluidization working state in a continuous fluid separation system.
Further, the resolving agent comprises dilute solution of sulfuric acid and hydrochloric acid, and the concentration range is 0.0-2.0mol/L.
Further, the continuous fluid separation system can meet the requirements of rapid loading and unloading of manganese-based adsorbents.
The invention has the beneficial effects that:
(1) The production cost is reduced, the production method is simplified, the production period is shortened, the lithium-magnesium ratio of the product is increased, the lithium-magnesium ratio can be increased to 4:1 from the original 1:1, the total yield is increased, and the total yield of the system can be increased by more than 10%.
(2) The continuous fluid separation system has the following advantages:
1) Because of continuous operation, the components and the concentration of the product are kept stable, and the downstream working section is convenient to be matched.
2) The device is compact and easy to install in any position.
3) The consumption of the regenerant is greatly reduced, and the consumption of the washing water can be saved by 50-60% at most.
4) The rotation speed can be automatically adjusted according to the change of the mass and the flow of the flowing fluid according to the requirement of the production process; thus ensuring an economically optimal operation.
5) The flow direction of the fluid may be coupled in a counter-current or co-current manner, depending on the convenience of the production process.
6) Because a plurality of separation units are adopted, the production method flow can be flexibly changed.
Drawings
FIG. 1 is a schematic diagram of a continuous fluid separation system for lithium extraction process according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a continuous fluid separation system according to an embodiment of the present invention;
FIG. 3 is a table of example 1 for extracting lithium from brine in accordance with an embodiment of the invention;
FIG. 4 is a table of example 2 for extracting lithium from brine in accordance with an embodiment of the invention;
fig. 5 is a table of example 3 for extracting lithium from brine in accordance with an embodiment of the invention.
Description of the embodiments
The present invention will now be described in detail with reference to the drawings and the detailed description thereof, wherein the invention is illustrated by the schematic drawings and the detailed description thereof, which are included to illustrate and not to limit the invention.
It should be noted that all directional indicators (such as up, down, left, right, front, back, upper, lower, top, bottom … …) in the embodiments of the present invention are merely used to explain the relative positional relationship, movement, etc. between the components in a particular posture (as shown in the drawings), and if the particular posture is changed, the directional indicators are correspondingly changed.
In the present invention, unless explicitly specified and limited otherwise, the term "connected" is to be construed broadly, and for example, "connected" may be either fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
Furthermore, descriptions such as those referred to as "first," "second," and the like, are provided for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implying an order of magnitude of the indicated technical features in the present disclosure. Thus, a feature defining "a first", "a second" may include at least one such feature, either explicitly or implicitly; in addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
As shown in fig. 1 and 2, an inorganic adsorbent and continuous fluid separation combined process is used for extracting lithium from brine, wherein: the lithium-containing brine is separated from magnesium, sodium and potassium components in raw materials by a continuous fluid separation system filled with inorganic ion adsorbent filler, and lithium ions on the adsorbent filler are eluted by an analytical agent to obtain a high-concentration lithium-rich solution. Compared with the existing brine lithium extraction production method, the method has the defects of complicated steps, low yield, high cost, and the like, and is based on the advantages of large adsorption capacity of the manganese adsorbent and advanced separation method of the continuous fluid separation device, so that the brand new brine lithium extraction production method is provided, and the purposes of reducing the production cost, simplifying the production method, shortening the production period, increasing the lithium-magnesium ratio and increasing the total yield are achieved.
Specifically, in the scheme of the embodiment, a plurality of separation units are arranged in the continuous fluid separation system, each separation unit is filled with manganese adsorbent filler, and the continuous fluid separation system comprises an exchange area, an exchange water washing area, an acid regeneration analysis area and a water acid washing area; the exchange area, the exchange water washing area, the acid regeneration analysis area and the water washing acid area are sequentially arranged along the circumference clockwise direction.
Specifically, in the scheme of the embodiment, the exchange area adopts a combination mode of serial connection and parallel connection for feeding, lithium ions in brine are adsorbed, and the feed liquid firstly enters a first group of parallel columns to be fully contacted with the manganese adsorbent; the tail liquid containing a small amount of lithium ions flows out into the subsequent parallel columns to be subjected to secondary adsorption, so that the finally discharged adsorption tail liquid only contains a small amount of lithium or does not contain lithium. The exchange area can furthest improve the feeding flow through ingenious combination of the series-parallel connection of the columns, and simultaneously ensure the adsorption capacity of the resin, thereby improving the utilization efficiency and the utilization rate of the resin.
Specifically, in the scheme of the embodiment, after brine is exchanged by the manganese-based adsorbent, the adsorbent loses the exchange capacity and needs to be regenerated and resolved, and as the brine stock solution still remains in the column, the raw materials in the column need to be washed out; the exchange water washing area adopts a mode that a plurality of columns are connected in series to carry out gradient water washing, and dilute materials washed out by water are put on the columns again or enter raw material liquid to dilute the raw material liquid, so that the crystallization precipitation in the process is avoided, and the production is influenced. Through the multistage series connection mode, the water washing amount can be effectively reduced, and meanwhile, the cleaning is ensured to be complete.
Specifically, in the solution of this embodiment, the acid regeneration analysis area and the acid washing area use a reverse analysis mode, so that the resin is in a semi-fluidization state in the analysis process, thereby improving the analysis speed and reducing the dissolution loss of the resin; after the resin is resolved, the resolving agent is rapidly discharged out of the system, and the residual resolving agent is cleaned by water, so that the contact time of the resolving agent and the resin is reduced, and the dissolution loss of the resin is reduced.
Specifically, in this embodiment, the inorganic ion adsorbent refers to a lithium manganate adsorbent, and the adsorbent adopts a granulation technology, so that the density and the particle size of the adsorbent are required to satisfy the semi-fluidization working state formed in a continuous fluid separation system.
Specifically, in this embodiment, the resolving agent includes dilute solution of sulfuric acid and hydrochloric acid, and the concentration range is 0.0-2.0mol/L.
Specifically, in the embodiment, the continuous fluid separation system can meet the requirements of rapid filling and disassembly of the manganese-based adsorbent.
Specifically, the implementation method of the invention comprises the following steps: the continuous fluid separation device filled with the manganese series adsorbent is adopted to carry out advanced separation, the functions of the steps of adsorption, multistage membrane and the like in the traditional method are replaced, and lithium is extracted from brine. The design production method comprises the following steps:
continuous fluid separation device for filling manganese series adsorbent, namely lithium-rich liquid, of lithium-containing brine enters downstream working section
The specific method is that the lithium-containing brine passes through a separation unit in a continuous fluid separation device filled with manganese-based adsorbent. In the continuous fluid separation unit, lithium and hydrogen ions on the manganese-based adsorbent are exchanged, and the effluent is waste liquid after adsorption exchange. The exchanged adsorbent enters a regeneration analysis zone along with the rotation of the system, and is subjected to regeneration analysis of dilute acid in the regeneration zone to obtain lithium-rich liquid. The manganese adsorbent after water washing again enters the exchange area again to continuously adsorb lithium.
The manganese adsorbent and continuous fluid separation device technology used in the method of the invention realizes the multistage membrane method production process in the traditional production in a continuous production method, continuously feeds and continuously outputs products, and completely innovates the traditional technology. In the invention, a plurality of intermediate links in the traditional production method are omitted. Meanwhile, due to the continuous operation of the continuous fluid separation device, the fluid distribution valves are sequentially switched, and each separation unit sequentially pumps liquid with different media according to the method design, such as: raw materials, water, different chemical reagents, etc.
As shown in fig. 1 and 2, the invention adopts a manganese adsorbent and a continuous fluid separation device, and organically combines the two products for extracting lithium from brine.
In the production method, manganese adsorbent filler and a continuous fluid separation device are combined to replace the original multi-section membrane combination process, the product yield in the step can reach more than 95%, and the lithium-magnesium ratio of the product can reach more than 4:1, as shown in figures 3 to 5;
compared with the prior art, the invention has the advantages that:
in a combined process of manganese-based sorbent and continuous fluid separation. Compared with other adsorbents, the adsorption capacity is larger and is about 300 percent larger than that of other adsorbents; the equipment investment scale is smaller, the equipment investment scale is about 60 percent smaller than that of other adsorbents, the adsorbent usage amount is less, and the adsorbent usage amount is about 60 percent smaller than that of other adsorbents. Meanwhile, the occupied area of the system is reduced by about 60%; the product yield is improved by 10%; the lithium-magnesium ratio of the product is improved by 300 percent.
The foregoing has described in detail the technical solutions provided by the embodiments of the present invention, and specific examples have been applied to illustrate the principles and implementations of the embodiments of the present invention, where the above description of the embodiments is only suitable for helping to understand the principles of the embodiments of the present invention; meanwhile, as for those skilled in the art, according to the embodiments of the present invention, there are variations in the specific embodiments and the application scope, and the present description should not be construed as limiting the present invention.
Claims (4)
1. The application of the inorganic adsorbent and continuous fluid separation combined process in extracting lithium from brine is characterized in that: the lithium-containing brine enters an adsorbent to be separated from magnesium, sodium and potassium components in raw materials through a continuous fluid separation system filled with inorganic ion adsorbent fillers, and then lithium ions on the adsorbent fillers are eluted through an analytical agent to obtain a high-concentration lithium-rich solution; the continuous fluid separation system is internally provided with a plurality of separation units, each separation unit is filled with manganese adsorbent filler, and comprises an exchange area, an exchange water washing area, an acid regeneration analysis area and a water acid washing area; the exchange area, the exchange water washing area, the acid regeneration analysis area and the water washing acid area are sequentially arranged along the circumference clockwise direction; the exchange area adopts a combination mode of serial connection and parallel connection for feeding, lithium ions in brine are adsorbed, and the feed liquid firstly enters a first group of parallel columns to be fully contacted with the manganese adsorbent; the tail liquid containing a small amount of lithium ions flows out into a subsequent parallel column to be subjected to secondary adsorption, so that the finally discharged adsorption tail liquid only contains a small amount of lithium or does not contain lithium; the inorganic ion adsorbent is a lithium manganate adsorbent.
2. The use of an inorganic adsorbent and continuous fluid separation combined process according to claim 1 for brine extraction of lithium, characterized in that: after the brine is exchanged by the manganese-series adsorbent, the adsorbent loses the exchange capacity and needs to be regenerated and resolved, and as the brine stock solution still remains in the column, the raw materials in the column need to be washed out; the exchange water washing area adopts a mode that a plurality of columns are connected in series to carry out gradient water washing, and dilute materials washed out by water are put on the columns again or enter raw material liquid to dilute the raw material liquid, so that crystallization precipitation can not occur in the process.
3. The use of an inorganic adsorbent and continuous fluid separation combined process according to claim 2 for brine extraction of lithium, characterized in that: the acid regeneration analysis area and the water acid washing area adopt a reverse analysis mode, so that the resin is in a semi-fluidization state in the analysis process, the analysis speed is improved, and the dissolution loss of the resin is reduced; after the resin is resolved, the resolving agent is rapidly discharged out of the system, and the residual resolving agent is cleaned by water.
4. The use of an inorganic adsorbent and continuous fluid separation combined process according to claim 1 for brine extraction of lithium, characterized in that: the continuous fluid separation system satisfies rapid loading and unloading of manganese-based adsorbents.
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| WO2015096549A1 (en) * | 2013-12-26 | 2015-07-02 | 江苏久吾高科技股份有限公司 | Process and apparatus for extracting battery grade lithium from brine |
| JP2019099901A (en) * | 2017-12-05 | 2019-06-24 | ティーエムシー株式会社 | Method for recovering lithium from lithium-containing solution |
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| CN112695211A (en) * | 2020-12-01 | 2021-04-23 | 西安蓝深环保科技有限公司 | Continuous ion exchange method for separating lithium from salt lake brine |
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| DE112011103839B4 (en) * | 2010-11-19 | 2016-08-18 | Central South University | Process and apparatus for separating lithium from magnesium and accumulating lithium in brine |
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| WO2015096549A1 (en) * | 2013-12-26 | 2015-07-02 | 江苏久吾高科技股份有限公司 | Process and apparatus for extracting battery grade lithium from brine |
| JP2019099901A (en) * | 2017-12-05 | 2019-06-24 | ティーエムシー株式会社 | Method for recovering lithium from lithium-containing solution |
| CN111826524A (en) * | 2020-07-13 | 2020-10-27 | 礼思(上海)材料科技有限公司 | Method for extracting lithium from salt lake brine by using adsorbent |
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