CN102031368B - Continuous ion exchange device and method for extracting lithium from salt lake brine - Google Patents
Continuous ion exchange device and method for extracting lithium from salt lake brine Download PDFInfo
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Abstract
The invention discloses a continuous ion exchange device for extracting lithium from salt lake brine, comprising resin, a plurality of resin columns used for loading the resin, a feeding main pipe which is communicated with the upper end of each resin column and a discharge main pipe which is communicated with the lower end of each resin column, wherein the resin columns are sequentially connected in series by a serial pipeline to form an adsorption resin column group, a rapid leaching resin column group and a leaching resin column group which are in sequential mobile circulation running, andeach feeding branch pipe and each discharge branch pipe are respectively provided with a control valve used for harmoniously controlling the transformation process of realizing ion exchange, washing,leaching and resin in turn among the resin column groups. Compared with the traditional fixed bed adsorption technology, the invention has the advantages of simple equipment, convenient operation, high automation degree, small usage amount of resin, high utilization ratio, stable product concentration and high concentration of qualified liquid.
Description
Technical field
The present invention relates to a kind of continuous ion exchange unit, be specifically related to a kind of continuous ion exchange unit that from salt lake brine, extracts lithium, the invention still further relates to the continuous ionic switching method of utilizing this device from salt lake brine, to extract lithium.
Background technology
Metallic lithium and compound thereof have the major application prospect aspect the energy and the novel material, salt lake brine is put forward the main direction that lithium will become 21 century lithium salts production.The lithium resource of occurring in nature is mainly composed and is stored in granitic pegmatite-type mineral deposit, salt lake brine, seawater and the GEOTHERMAL WATER.According to statistics, salt lake brine lithium resource reserves account for 70～80% of lithium resource total amount, therefore salt lake brine is carried lithium will become the main path that lithium salts is produced, and the lithium salts product (in Quilonum Retard) that the whole world produces from bittern has accounted for more than 85% of lithium product population.
From salt lake brine, extract the technology method of lithium salts both at home and abroad, be summed up and mainly contain the precipitator method, extraction process, ion exchange adsorption, carborization, calcining leaching method, Xu Shi method and electroosmose process etc.Wherein the precipitator method, extraction process, absorption method and carborization are studied extensively and deeply, are become main salt lake brine and put forward the lithium method, from bittern, extract lithium salts industrial generally all be to adopt evaporate-crystallization-precipitation, its finished product all are Quilonum Retards.Precipitator method feasible process, but technical process is long, the material cycling amount is large, needs repeatedly calcining to filter, and operation steps is numerous and diverse, and last resulting lithium leaching liquid concentration is low, and it is concentrated needs to consume a large amount of power costs.The extraction process rate of recovery is high, but long flow path, equipment corrosion is serious, and production cost is high, and the realization industrialization is had any problem.The resin absorption rule is to use lithium ion exchanged sorbent material such as titanium dioxide, metal phosphate, compound stibnate and aluminium salt type sorbent material and organic ion exchange resin etc. optionally to process the salt lake brine of high Mg/Li ratio, utilization is adsorbed lithium ion to the sorbent material of the selective absorption of lithium ion, again lithium ion is eluted, reach the purpose that lithium ion separates with other foreign ion.This method technique is simple, and the rate of recovery is high, and selectivity is good, has compared larger superiority with other method.Therefore the Chaidamu Basin, Qinghai Province that has global bittern lithium resource 79% in China is promoted absorption method such as salt lake one bands such as platform gill lake, Yi Liping, Cha Er sweat and large Chai Dan and is produced the technique of lithium significant aspect economic worth and the environmental protection.
Chinese patent CN1511964 discloses a kind of absorption method from the method for extracting lithium from salt lake brine, and be applicable to Qinghai and contain that lithium salts lake bittern water and salt pan are concentrated to contain the old halogen of lithium, and the technological process of from Qinghai Salt Lake Bittern, producing Quilonum Retard and lithium chloride.But it is not elaborated to the specific embodiment of absorption method, and the process of absorption method take for the fixed bed pattern, cause the resin utilization ratio low, product concentration low water usage amount is large etc.
Summary of the invention
The technical problem that the present invention solves is that existing preventing fixed bed adsorber extracts lithium in the bittern from the salt lake technique exists the resin utilization ratio low, the problem that product concentration is low and water is large the invention provides a kind of continuous ion exchange unit that extracts lithium from salt lake brine.
For achieving the above object, a kind of continuous ion exchange unit that from salt lake brine, extracts lithium, comprise resin, be used for loading a plurality of resin columns of resin, reach the discharge header pipe that is communicated with the resin column lower end with the charging house steward who is communicated with on the resin column, described resin column is provided with five at least, be connected in series successively by series pipe between the described resin column, and form the adsorption resin column group of ordinal shift cycle operation, quick drip washing resin column group and drip washing resin column group;
Described charging house steward comprises bittern charging house steward, quick drip washing charging house steward and drip washing charging house steward, described discharge header pipe comprises bittern discharge header pipe, drip washing discharge header pipe and quick drip washing discharge header pipe, is respectively equipped with the feed-inputing branched pipe that is communicated with the charging house steward and the discharging arm that is communicated with described discharge header pipe on described each resin column;
Described feed-inputing branched pipe comprises bittern feed-inputing branched pipe, quick drip washing feed-inputing branched pipe and drip washing feed-inputing branched pipe, and described bittern feed-inputing branched pipe, quick drip washing feed-inputing branched pipe and drip washing feed-inputing branched pipe are respectively with described bittern charging house steward, fast drip washing charging house steward and one by one corresponding connection of drip washing charging house steward;
Described discharging arm comprises bittern discharging arm, drip washing discharging arm and quick drip washing discharging arm, with described bittern discharge header pipe, drip washing discharge header pipe and fast one by one corresponding connection of drip washing discharge header pipe, described qualifying liquid is by exporting in the described drip washing discharge header pipe respectively for described bittern discharging arm, drip washing discharging arm and quick drip washing discharging arm;
Be respectively equipped with control valve on described each feed-inputing branched pipe, discharging arm and the series pipe, be used for periodically controlling each resin column group and between a plurality of resin columns, realize synchronously ion-exchange, quick drip washing and lessivation.
The quantity of described drip washing resin column group is at least two groups, and the quantity of the quantity of the drip washing feed-inputing branched pipe on the described resin column and drip washing discharging arm equates with the group number of described drip washing resin column group;
Described drip washing charging house steward's quantity, the quantity of drip washing discharge header pipe equate with the group number of described drip washing resin column group respectively;
Described drip washing charging house steward comprises wash feed house steward and at least one backflow charging house steward, described drip washing discharge header pipe comprises qualifying liquid discharge header pipe and at least one backflow discharge header pipe, and described backflow discharge header pipe and backflow charging house steward connect one to one with surge tank by pipeline.
Described drip washing resin column group arranges three groups, is respectively the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group, wherein,
The series connection resin column quantity of described adsorption resin column group is at least 2;
The series connection resin column quantity of described quick drip washing resin column group is at least 1;
The series connection resin column quantity of described the first drip washing resin column group is at least 2;
The series connection resin column quantity of described the second drip washing resin column group is at least 2;
The series connection resin column quantity of described the 3rd drip washing resin column group is at least 2;
Export in the qualifying liquid discharge header pipe of described qualifying liquid by the last step resin of described the 3rd drip washing resin column group.
Described resin is the organic ion exchange resin, mineral ion exchange resin and sorbent material, aluminum salt adsorbent, ion(ic)sieve oxide adsorbent, a kind of without in the sorbent material of unformed hydroxide.
Described control valve is magnetic valve or pneumavalve, and described control valve is used for periodically controlling the keying of the control valve on described feed-inputing branched pipe, discharging arm and the series pipe by the PLC time variable control.
The present invention also provides a kind of continuous ionic switching method of extracting lithium from salt lake brine, comprises the steps:
Step 1: a plurality of resin columns are connected in series successively, formation flows to five groups of resin column groups of identical and running capable of circulation, is followed successively by the first drip washing resin column group, quick drip washing resin column group, adsorption resin column group, the 3rd drip washing resin column group and the second drip washing resin column group;
Step 2: salt lake brine is input in the polymeric adsorbent group post, washings is inputed to respectively in the first drip washing resin column group and the quick drip washing resin column group, leacheate in the first drip washing resin column group is back in the second drip washing resin column group by surge tank and as the feeding liquid of the second drip washing resin column group, the leacheate in described the second drip washing resin column group is back in the 3rd drip washing resin column group and as the feeding liquid of the 3rd drip washing resin column group by secondary drip washing surge tank and finishes synchronously the quick drip washing of lithium ion exchanged, resin column and the washing process of resin column;
Step 3: behind a upper end cycle, make five groups of resin column groups between a plurality of resin columns, carry out the combination of next cycle by the control valve that switches on the resin column;
Step 4: salt lake brine and washings are input to respectively in the adsorption resin column group of next cycle, quick drip washing resin column group and the first drip washing resin column group, finish synchronously the lithium ion exchanged of next cycle, quick drip washing and the resin column washing process of resin column, export in the last step resin column of qualifying liquid by the 3rd drip washing resin column group in each cycle.
First step resin column in the quick drip washing resin column group in the described step 4 is the first step resin column in the upper cycle adsorption resin column group; The last step resin column of described adsorption resin column group is the first step resin column in upper cycle the 3rd drip washing resin column group; Last step resin column in described the first drip washing resin column group was the first step resin column in the quick drip washing resin column group of the upper cycle.
Described salt lake brine is from the top feed liquor of adsorption resin column group, described washings is respectively from the top feed liquor of described quick drip washing resin column group and the first drip washing resin column group, and described top feed liquor is flowed through after the resin column group of appointment and in the bottom of its last step resin column fluid;
The leacheate of described the first drip washing resin column group is by the bottom output of its last step resin column, and as the top feeding liquid of the second drip washing resin column group, the leacheate of described the second drip washing resin column group is by the bottom output of its last step resin column, and as the top feeding liquid of the 3rd drip washing resin column group, qualifying liquid is by the bottom output of the last step resin column of the 3rd drip washing resin column group.
The treatment rate of the salt lake brine in the described adsorption resin column group is 5-10BV/h, treatment capacity: 20-60BV;
The treatment rate of the washings in the described quick drip washing resin column group is 5-20BV/h, treatment capacity 2-4BV;
The treatment rate of the washings in described the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group is 3-5BV/h, treatment capacity 2-6BV;
The time that the wherein said control valve cycle switches is 2-12h.
Magnesium lithium mass concentration ratio is 10-15 in the top feeding liquid of described the second drip washing resin column group, and magnesium lithium mass concentration ratio is 5-10 in the out-feed liquid of its underpart; The magnesium lithium mass concentration ratio of the qualifying liquid of exporting in the last step resin column by described the 3rd drip washing resin column group is＜5.
The temperature of the salt lake brine in the described adsorption resin column group is 20-100 ℃;
Washings in described rapid resin post group, the first resin column group is 20-50 ℃ deionized water.
The present invention extracts lithium from salt lake brine continuous ionic exchange process adopts the continuous ionic exchange system, resin position in continuous ion exchange unit is motionless, switching by the automatic control system valve, make the simultaneously property performance period absorption of different zones resin, fast drip washing and drip washing, autocontrol valve is pneumavalve or magnetic valve, adopts the PLC time variable control.
Particularly, method of the present invention can realize by following technique measures: adsorption zone: the operation of n1 post, and salt lake brine enters from resin column top, and the bottom goes out.Superficial linear velocity is controlled at 10-30m/h
Fast drip washing: the operation of n2 post, deionized water enters from resin column top, and the bottom goes out.
For the first time drip washing: the operation of n3 post, deionized water enters from resin column top, and the bottom goes out.
For the second time drip washing: the operation of n4 post, for the first time drip washing goes out leacheate and enters from resin column top, and the bottom goes out.
For the third time drip washing: the operation of n5 post, for the second time drip washing goes out leacheate and enters from resin column top, and the bottom goes out.
Be total to n resin column in the system, in the section, n1 post adsorbs at one time, n2 the quick drip washing of post, n3 for the first time drip washing of post, n4 for the second time drip washing of post, n5 for the third time drip washing of post.Each resin column carries out periodic working cycle.Wherein, n=n1+n2+n3+n4+n5, n1 〉=2, n2 〉=1, n3 〉=2, n4 〉=2, n5 〉=2.
Adsorption zone process described in the present invention may further comprise the steps: n1 post series operation, salt lake brine by resin column top enter fully exchange with resin after, go out from first step resin column end opening, enter from second stage resin column is suitable for reading more afterwards, process is carried out according to this, until go out from n1 resin column end opening, effluent liquid turns back to and shines in the salt pond.Temperature: 20-100 ℃, treatment rate 5-10BV/h, treatment capacity: 40-60BV
Quick lessivation described in the present invention may further comprise the steps: deionized water enters from resin column top, and salt lake brine residual in the resin is gone out.Temperature: 20-50 ℃, treatment rate: 20BV/H, treatment capacity 2BV-4BV
The lessivation first time described in the present invention may further comprise the steps: deionized water enters from resin column top, and the bottom goes out.To wash out with the weak magnesium of resin-bonded power in the resin.Temperature: 20-50 ℃, treatment rate: 3-5BV/h, treatment capacity 2BV-6BV collects the magnesium lithium content than the leacheate during as second time drip washing for the leacheate of 10-15.
The lessivation second time described in the present invention may further comprise the steps: the leacheate that fs drip washing goes out enters from resin column top, and the bottom goes out.The magnesium that bonding force in the resin is weak continues to wash out.Temperature: 20-50 ℃, the leacheate when treatment rate: 3-5BV/h, collection magnesium lithium content compare for for the third time drip washing of leacheate conduct of 5-10.
For the third time lessivation described in the present invention may further comprise the steps: the leacheate that subordinate phase drip washing goes out enters from resin column top, and the bottom goes out.The lithium that adsorbs in the resin is washed out.Temperature: 20-50 ℃, treatment rate: 3-5BV/h collects the leacheate of magnesium lithium content＜5 as the qualifying liquid of lithium.
More than absorption, lessivation is carried out synchronously, and periodically carries out the switching of valve.Each resin column is finished above institute in steps through the circulation in a week.
Method of the present invention adopts continuous ion exchange apparatus targetedly, and adsorption process is adopted the series connection absorption mode, has improved the service efficiency of resin, makes the resin state that at utmost reaches capacity.Adsorb saturated afterwards resin by quick drip washing and speed change drip washing pattern, the usage quantity of eluent is reduced, and increased the concentration of drip washing fluid.Compare with existing ADSORPTION IN A FIXED BED technology, it is simple, easy to operate to have equipment, and level of automation is high, and the resin usage quantity is few, and utilization ratio is high, and product concentration is stable and qualifying liquid concentration is high.
Description of drawings
Fig. 1 is the process flow sheet of continuous ionic exchange process of the present invention;
Fig. 2 is the continuous ionic exchange process device of Fig. 1;
Fig. 3 is PLC time variable control wiring diagram of the present invention.
Among the figure:
1. wash feed arm 2. quick drip washing feed-inputing branched pipes
3. bittern feed-inputing branched pipe 4. second backflow feed-inputing branched pipes
5. the first backflow feed-inputing branched pipe 6. first backflow discharging arms
7. quick drip washing discharging arm 8. bittern discharging arms
9. qualifying liquid discharging arm 10. second backflow discharging arms
11. pneumavalve/magnetic valve 12. resin columns
13. wash feed house steward 14. quick drip washing charging house stewards
15. bittern charging house steward 16. second backflow charging house stewards
17. the first backflow charging house steward 18. first backflow discharge header pipe
19. quick drip washing discharge header pipe 20. bittern discharge header pipe
21. qualifying liquid discharge header pipe 22. second backflow discharge header pipe
23. series pipe
Embodiment
The present invention is further described below in conjunction with embodiment, but does not limit the present invention.
A kind of continuous ion exchange unit that from salt lake brine, extracts lithium of the present invention, comprise resin, be used for loading a plurality of resin columns of resin, reach the discharge header pipe that is communicated with the resin column lower end with the charging house steward who is communicated with on the resin column, described resin column is provided with five at least, be connected in series successively by series pipe between the resin column, and form the adsorption resin column group of ordinal shift cycle operation, quick drip washing resin column group and drip washing resin column group; The quantity of drip washing resin column group wherein is at least two groups, the charging house steward comprises bittern charging house steward, quick drip washing charging house steward and drip washing charging house steward, discharge header pipe comprises bittern discharge header pipe, drip washing discharge header pipe and quick drip washing discharge header pipe, is respectively equipped with the feed-inputing branched pipe that is communicated with the charging house steward and the discharging arm that is communicated with discharge header pipe on each resin column; Feed-inputing branched pipe comprises bittern feed-inputing branched pipe, quick drip washing feed-inputing branched pipe and drip washing feed-inputing branched pipe, and bittern feed-inputing branched pipe, quick drip washing feed-inputing branched pipe and drip washing feed-inputing branched pipe are respectively with bittern charging house steward, fast drip washing charging house steward and one by one corresponding connection of drip washing charging house steward; The discharging arm comprises bittern discharging arm, drip washing discharging arm and quick drip washing discharging arm, with bittern discharge header pipe, drip washing discharge header pipe and fast one by one corresponding connection of drip washing discharge header pipe, qualifying liquid is by exporting in the drip washing discharge header pipe respectively for bittern discharging arm, drip washing discharging arm and quick drip washing discharging arm.
Be respectively equipped with control valve on described each feed-inputing branched pipe, discharging arm and the series pipe, be used for periodically controlling each resin column group and between a plurality of resin columns, realize synchronously ion-exchange, quick drip washing and lessivation.
The quantity of drip washing resin column group is at least two groups, the quantity of the quantity of the drip washing feed-inputing branched pipe on the resin column and drip washing discharging arm equates that with the group number of described drip washing resin column group the quantity of drip washing charging house steward's quantity, drip washing discharge header pipe equates with the group number of drip washing resin column group respectively; Drip washing charging house steward comprises wash feed house steward and at least one backflow charging house steward, the drip washing discharge header pipe comprises qualifying liquid discharge header pipe and at least one backflow discharge header pipe, and backflow discharge header pipe and backflow charging house steward connect one to one with surge tank by connecting pipeline.
When drip washing resin column group arranges three groups, namely be respectively the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group, wherein, the series connection resin column quantity of adsorption resin column group is at least 2, the series connection resin column quantity of drip washing resin column group is at least 1 fast, the series connection resin column quantity of the first drip washing resin column group is at least 2, the series connection resin column quantity of the second drip washing resin column group is at least 2, the series connection resin column quantity of the 3rd drip washing resin column group is at least 2, exports in the qualifying liquid discharge header pipe of qualifying liquid by the last step resin of described the 3rd drip washing resin column group.
Resin is the organic ion exchange resin, mineral ion exchange resin and sorbent material, aluminum salt adsorbent, ion(ic)sieve oxide adsorbent, a kind of without in the sorbent material of unformed hydroxide.Control valve is magnetic valve or pneumavalve, and control valve is used for periodically controlling the keying of the control valve on described feed-inputing branched pipe, discharging arm and the series pipe by the PLC time variable control.
As shown in Figure 3, all corresponding process controls are carried out relevant operation by the CPU in the PLC system.Each pillar operating unit is divided into absorption, fast drip washing, the first drip washing, five steps of the second drip washing and the 3rd drip washing are continuous, each step is continuous to be divided into again into salt lake brine (washings, leacheate, leacheate and secondary leacheate) and to start (closing), valve open (closing), sensor starts (cutting out) three and column unit.At a time, all pillars are in operation absorption, fast drip washing, the first drip washing, a certain step in the second drip washing and the 3rd drip washing step.As take the 1# post as example, give 1# post absorption instruction by CPU, this moment, sensor obtained advancing salt lake brine valve signal after the order of CPU, advanced the salt lake brine valve open.After preset time, CPU gives 1# post absorption END instruction, and this moment, sensor obtained advancing salt lake brine valve signal after the order of CPU, advanced the salt lake brine valve closes, and absorption finishes, and with this signal feedback to CPU.This moment, CPU gave the 1# post quick drip washing instruction, and this moment, sensor obtained advancing the wash fluid valve gating signal after the order of CPU, advanced the washings valve and opened.After preset time, CPU gives the 1# post and washs fast END instruction, this moment, sensor obtained advancing leacheate valve signal after the order of CPU, advance the leacheate valve open, after preset time, CPU gives the 1# post the first drip washing END instruction, and this moment, sensor obtained advancing leacheate valve signal one time after the order of CPU, advance the leacheate valve open one time, the first drip washing finishes.After preset time, CPU gives the 1# post the first drip washing END instruction, this moment, sensor obtained advancing secondary leacheate valve signal after the order of CPU, advanced secondary leacheate valve open, and the second drip washing finishes, after preset time, CPU gives the 1# post the second drip washing END instruction, and this moment, sensor obtained advancing secondary leacheate valve signal after the order of CPU, advanced secondary leacheate valve closes, the 3rd drip washing finishes, and the 1# post begins next algorithm.The control principle of other posts is identical with the 1# post with step.
The quantity of set drip washing resin column group is 3 groups among Fig. 1,2, be respectively the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group, the bittern feed-inputing branched pipe that is communicated with it, quick drip washing feed-inputing branched pipe, wash feed arm, the first backflow feed-inputing branched pipe and the second backflow feed-inputing branched pipe of being provided with suitable for reading of each resin column, the end opening of each resin column is provided with the bittern discharging arm that is communicated with it, quick drip washing discharging arm, the first backflow discharging arm, the second backflow discharging arm and qualifying liquid discharging arm; Charging house steward wherein comprises bittern charging house steward, quick drip washing charging house steward, wash feed house steward, the first backflow charging house steward and the second backflow charging house steward, discharge header pipe comprises bittern discharge header pipe, quick drip washing discharge header pipe, the first backflow discharge header pipe, the second backflow discharge header pipe and qualifying liquid discharge header pipe, wherein the first backflow discharge header pipe, the first backflow charging house steward are connected with surge tank respectively, and the second backflow discharge header pipe, the second backflow charging house steward are connected with the another one surge tank respectively.
Wherein, the series connection resin column quantity of adsorption resin column group is 3; The series connection resin column quantity of drip washing resin column group is 1 fast; The series connection resin column quantity of the first drip washing resin column group is 2, and the series connection resin column quantity of the second drip washing resin column group is 2, and the series connection resin column quantity of the 3rd drip washing resin column group is at least 2;
Export in the qualifying liquid discharge header pipe of qualifying liquid by the last step resin of the 3rd drip washing resin column group.
The present invention also provides a kind of continuous ionic switching method of extracting lithium from salt lake brine, comprises the steps:
Step 1: a plurality of resin columns are connected in series successively, formation flows to five groups of resin column groups of identical and running capable of circulation, is followed successively by the first drip washing resin column group, quick drip washing resin column group, adsorption resin column group, the 3rd drip washing resin column group and the second drip washing resin column group;
Step 2: salt lake brine is input in the polymeric adsorbent group post, deionized water is inputed to respectively in the first drip washing resin column group and the quick drip washing resin column group, leacheate in the first drip washing resin column group is back in the second drip washing resin column group by surge tank and as the feeding liquid of the second drip washing resin column group, leacheate in the second drip washing resin column group is back in the 3rd drip washing resin column group by the secondary buffer tank and as the feeding liquid of the 3rd drip washing resin column group, finishes synchronously the quick drip washing of lithium ion exchanged, resin column and the washing process of resin column;
Step 3: behind a upper end cycle, make five groups of resin column groups between a plurality of resin columns, carry out the combination of next cycle by the control valve that switches on the resin column;
Step 4: salt lake brine and deionized water are input to respectively in the adsorption resin column group of next cycle, quick drip washing resin column group and the first drip washing resin column group, finish synchronously the lithium ion exchanged of next cycle, quick drip washing and the resin column washing process of resin column, export in the last step resin column of qualifying liquid by the 3rd drip washing resin column group in each cycle.
Wherein the first step resin column in the quick drip washing resin column group in the step 4 is the first step resin column in the upper cycle adsorption resin column group; The last step resin column of adsorption resin column group is the first step resin column in upper cycle the 3rd drip washing resin column group; Last step resin column in described the first drip washing resin column group was the first step resin column in the quick drip washing resin column group of the upper cycle.
As shown in table 1, the continuous ion exchage extracting process from Lithium from Salt Lake Brine of the present invention adopts continuous ion exchange apparatus to extract lithium from salt lake brine, has adopted the operator scheme of series connection continous way.
Table 1: resin column different zones function step run table
The described method of present embodiment comprises the steps:
The resin of resin column adopts ion-sieve type sorbent material seplite LXL-10A (Xi'an Lanxiao Sci-Tech Co., Ltd.), and the magnesium lithium content was than 432: 1 in the initial salt lake brine.
As shown in drawings, each resin column is in the following different resins post group, take the period 1 as example:
1#, 2# post: the first drip washing resin column group 3# post: quick drip washing resin column group
4#, 5#, 6# post: adsorption resin column group 7#, 8# post: the 3rd drip washing resin column group
9#, 10# post: the second drip washing resin column group
4#, 5#, 6# post: adsorption resin column group.4#, 5#, 6# post are the drag flow series operation, salt lake brine enters the 4# post bittern feed-inputing branched pipe suitable for reading from bittern charging house steward, successively by 5# post and 6# post, the bittern discharging arm by 6# post end opening enters in the bittern discharge header pipe at last through series pipe, finally enters and shines in the salt pond.Whole adsorption process, Lithium from Salt Lake Brine is through after the three grade resins absorption, and the concentration of lithium is reducing gradually, until the concentration of 4# post end opening lithium is with after the import lithium concentration is consistent, think that namely resin reaches capacity, switch the 4# post through valve and enter into quick drip washing resin column group.Feeding rate: 10BV/h, charging total amount 40BV, residence time 240min.
3# post: quick drip washing resin column group.Deionized water is from quick drip washing charging house steward enters quick drip washing feed-inputing branched pipe with the connection suitable for reading of 3# post, quick drip washing discharging arm through end opening enters quick drip washing house steward, then be back to and shine the salt pond, the a large amount of salt lake brines that farthest will remain in the resin are removed, and can flush away and the magnesium of resin-bonded power a little less than relatively.Deionized water speed: 20BV/h, charging total amount 3BV, residence time 240min.Consider the particular requirement of quick drip washing, drip washing needs total time to only have 9min fast.Therefore, behind this end of processing, resin was in waiting status after drip washing resin column group finished fast.After total system 240min finishes fully, switch again and enter next cycle.
1#, 2# post: the first drip washing resin column group.Through the lithium stronger with the weak magnesium of resin-bonded power and bonding force arranged on the resin after the quick drip washing.Deionized water enters wash feed arm with the connection suitable for reading of 1# post by the wash feed house steward, and it is suitable for reading to enter the 2# post through series pipe, and is entered in the first backflow discharge header pipe by the first backflow discharging arm of end opening, then enters in the surge tank of a drip washing; When wherein magnesium and lithium were gone out by drip washing simultaneously, the concentration of magnesium will be higher than lithium, and the speed of deionized water is at 3Bv/h, total amount 6BV, and magnesium lithium mass concentration ratio is 13, the residence time: 240min.
9#, 10# post: the second drip washing resin column group.After the first drip washing resin column group, minimizing is more relatively for the magnesium of combination on the resin, and the lithium minimizing is less.Therefore, effluent liquid by using the first drip washing resin column group is as the leacheate of the second drip washing resin column group, the leacheate of the second drip washing resin column group is flowed out by 10# resin column end opening, and enter in the surge tank of secondary drip washing through the second backflow discharge header pipe, the effluent liquid magnesium of the second drip washing resin column group and the concentration of lithium are improving gradually.The speed of leacheate: 5BV/h, total amount 6BV, magnesium lithium mass concentration ratio is 7, residence time 240min.
7#, 8# post: the 3rd drip washing resin column group.Magnesium through combination on the resin after the two-stage drip washing has reduced often, and the content of lithium increases relatively.Effluent liquid by using the second drip washing resin column group is as the leacheate of the 3rd drip washing resin column group, and the qualifying liquid concentration that is flowed out by the qualifying liquid discharging arm of the 3rd drip washing resin column group last step increases, and the purity of lithium also is improved.The speed of leacheate: 5BV/h, total amount 6BV, magnesium lithium mass concentration ratio is 2, residence time 240min, the extraction yield of Lithium from Salt Lake Brine are 91%.
After the period 1 finished, the resin column in each resin column group passed through each control valve of PLC time variable control, thereby makes each in order translation of resin column group, finishes next cycle.
The temperature of the salt lake brine in the adsorption resin column group is 20-100 ℃, and the washings in rapid resin post group, the first resin column group is 20-50 ℃ deionized water.
Embodiment 2
With embodiment 1 difference be:
The resin of resin column adopts ion-sieve type sorbent material seplite LXL-10B (Xi'an Lanxiao Sci-Tech Co., Ltd.), the magnesium lithium content was than 432: 1 in the initial salt lake brine, the treatment rate of the salt lake brine in the adsorption resin column group of salt lake brine is 5BV/h, treatment capacity: 40BV, the treatment rate of the deionized water in the drip washing resin column group is 10BV/h fast, treatment capacity 2BV; The treatment rate of the washings in the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group is 3BV/h, treatment capacity 2BV.
The time 480min that switches of control valve cycle wherein.
Magnesium lithium mass concentration ratio is 12: 1 in the top feeding liquid of the second drip washing resin column group, magnesium lithium mass concentration ratio is 6: 1 in the out-feed liquid of its underpart, the magnesium lithium mass concentration ratio of the qualifying liquid of exporting in the last step resin column by described the 3rd drip washing resin column group is 3: 1, and the extraction yield of Lithium from Salt Lake Brine is 90.3%.
Embodiment 3
With embodiment 1 difference be:
The resin of resin column adopts Amberlite IR-120B (U.S.'s ROHM AND HAAS), the magnesium lithium content was than 432: 1 in the initial salt lake brine, the treatment rate of the salt lake brine in the adsorption resin column group is 6BV/h, treatment capacity: 50BV, the treatment rate of the deionized water in the drip washing resin column group is 15BV/h fast, treatment capacity 4BV; The treatment rate of the washings in the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group is 4BV/h, treatment capacity 6BV.
The time 500min that switches of control valve cycle wherein.
Magnesium lithium mass concentration ratio is 13.5: 1 in the top feeding liquid of the second drip washing resin column group, and magnesium lithium mass concentration ratio is 7.3: 1 in the out-feed liquid of its underpart; The magnesium lithium mass concentration ratio of the qualifying liquid of exporting in the last step resin column by described the 3rd drip washing resin column group is 5: 1, and the extraction yield of Lithium from Salt Lake Brine is 89.3%.
Embodiment 4
With embodiment 1 difference be:
The resin of resin column adopts unformed oxyhydroxide sorbent material (testing laboratory of Xi'an Lanxiao Sci-Tech Co., Ltd. is synthetic), unformed oxyhydroxide sorbent material wherein is take aluminium type sorbent material as representative, rear and carbon dioxide reaction forms amorphous hydroted alumina Al (OH) with the sodium aluminate dilution
2.8(C03)
0.1.xH20.The magnesium lithium content was than 510: 1 in the initial salt lake brine, and the treatment rate of the salt lake brine in the adsorption resin column group is 8BV/h, treatment capacity: 60BV, and the treatment rate of the deionized water in the drip washing resin column group is 12BV/h fast, treatment capacity 3BV; The treatment rate of the washings in the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group is 4.5BV/h, treatment capacity 5BV.
The time 450min that switches of control valve cycle wherein.
Magnesium lithium mass concentration ratio is 12.7: 1 in the top feeding liquid of the second drip washing resin column group, and magnesium lithium mass concentration ratio is 8: 1 in the out-feed liquid of its underpart; The magnesium lithium mass concentration ratio of the qualifying liquid of exporting in the last step resin column by described the 3rd drip washing resin column group is 3.7: 1, and the extraction yield of Lithium from Salt Lake Brine is 87.6%.
Embodiment 5
With embodiment 1 difference be:
The resin of resin column adopts aluminum salt adsorbent, and aluminum salt adsorbent wherein is that LiCl inserts the compound L iCl2A1 (OH) that generates among the AI (OH) 3
3NH20 (testing laboratory of Xi'an Lanxiao Sci-Tech Co., Ltd. is synthetic), the magnesium lithium content was than 510: 1 in the initial salt lake brine, the treatment rate of the salt lake brine in the adsorption resin column group is 10BV/h, treatment capacity: 20BV, the treatment rate of the deionized water in the drip washing resin column group is 15BV/h fast, treatment capacity 4BV; The treatment rate of the washings in the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group is 5BV/h, treatment capacity 3BV.
The time 120min that switches of control valve cycle wherein.
Magnesium lithium mass concentration ratio is 12.8: 1 in the top feeding liquid of the second drip washing resin column group, and magnesium lithium mass concentration ratio is 6.5: 1 in the out-feed liquid of its underpart; The magnesium lithium mass concentration ratio of the qualifying liquid of exporting in the last step resin column by described the 3rd drip washing resin column group is 4.8: 1, and the extraction yield of Lithium from Salt Lake Brine is 88.2%.
Obviously, above-described embodiment only is for example clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.And the apparent variation of being extended out thus or change still are among the protection domain of the invention.
Claims (11)
1. continuous ion exchange unit that extracts lithium from salt lake brine comprises resin, is used for loading a plurality of resin columns of resin, the charging house steward who is communicated with the resin column upper end and the discharge header pipe that is communicated with the resin column lower end, it is characterized in that:
Described resin column is provided with five at least, is connected in series successively by series pipe between the described resin column, and forms the adsorption resin column group of ordinal shift cycle operation, quick drip washing resin column group and drip washing resin column group;
Described charging house steward comprises bittern charging house steward, quick drip washing charging house steward and drip washing charging house steward, described discharge header pipe comprises bittern discharge header pipe, drip washing discharge header pipe and quick drip washing discharge header pipe, is respectively equipped with the feed-inputing branched pipe that is communicated with the charging house steward and the discharging arm that is communicated with described discharge header pipe on described each resin column;
Described feed-inputing branched pipe comprises bittern feed-inputing branched pipe, quick drip washing feed-inputing branched pipe and drip washing feed-inputing branched pipe, and described bittern feed-inputing branched pipe, quick drip washing feed-inputing branched pipe and drip washing feed-inputing branched pipe are respectively with described bittern charging house steward, fast drip washing charging house steward and one by one corresponding connection of drip washing charging house steward;
Described discharging arm comprises bittern discharging arm, drip washing discharging arm and quick drip washing discharging arm, with described bittern discharge header pipe, drip washing discharge header pipe and fast one by one corresponding connection of drip washing discharge header pipe, qualifying liquid is by exporting in the described drip washing discharge header pipe respectively for described bittern discharging arm, drip washing discharging arm and quick drip washing discharging arm;
Be respectively equipped with control valve on described each feed-inputing branched pipe, discharging arm and the series pipe, be used for periodically controlling each resin column group and between a plurality of resin columns, realize synchronously ion-exchange, quick drip washing and lessivation.
2. the continuous ion exchange unit that extracts lithium from salt lake brine according to claim 1 is characterized in that:
The quantity of described drip washing resin column group is at least two groups, and the quantity of the quantity of the drip washing feed-inputing branched pipe on the described resin column and drip washing discharging arm equates with the group number of described drip washing resin column group;
Described drip washing charging house steward's quantity, the quantity of drip washing discharge header pipe equate with the group number of described drip washing resin column group respectively;
Described drip washing charging house steward comprises wash feed house steward and at least one backflow charging house steward, described drip washing discharge header pipe comprises qualifying liquid discharge header pipe and at least one backflow discharge header pipe, and described backflow discharge header pipe and backflow charging house steward connect one to one with surge tank by pipeline.
3. the continuous ion exchange unit that from salt lake brine, extracts lithium according to claim 2, it is characterized in that: described drip washing resin column group arranges three groups, be respectively the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group, wherein
The series connection resin column quantity of described adsorption resin column group is at least 2;
The series connection resin column quantity of described quick drip washing resin column group is at least 1;
The series connection resin column quantity of described the first drip washing resin column group is at least 2;
The series connection resin column quantity of described the second drip washing resin column group is at least 2;
The series connection resin column quantity of described the 3rd drip washing resin column group is at least 2;
Export in the qualifying liquid discharge header pipe of described qualifying liquid by the last step resin of described the 3rd drip washing resin column group.
4. it is characterized in that according to claim 1 and 2 or the 3 described continuous ion exchange units that from salt lake brine, extract lithium:
Described resin is the organic ion exchange resin, mineral ion exchange resin and sorbent material, aluminum salt adsorbent, ion(ic)sieve oxide adsorbent, a kind of in the unformed oxyhydroxide sorbent material.
5. it is characterized in that according to claim 1 and 2 or the 3 described continuous ion exchange units that from salt lake brine, extract lithium:
Described control valve is magnetic valve or pneumavalve, and described control valve is used for periodically controlling the keying of the control valve on described feed-inputing branched pipe, discharging arm and the series pipe by the PLC time variable control.
6. a continuous ionic switching method of extracting lithium from salt lake brine is characterized in that comprising the steps:
Step 1: a plurality of resin columns are connected in series successively, formation flows to five groups of resin column groups of identical and running capable of circulation, is followed successively by the first drip washing resin column group, quick drip washing resin column group, adsorption resin column group, the 3rd drip washing resin column group and the second drip washing resin column group;
Step 2: salt lake brine is input in the polymeric adsorbent group post, washings is inputed to respectively in the first drip washing resin column group and the quick drip washing resin column group, leacheate in the first drip washing resin column group is back in the second drip washing resin column group by drip washing surge tank and as the feeding liquid of the second drip washing resin column group, leacheate in described the second drip washing resin column group is back in the 3rd drip washing resin column group by secondary drip washing surge tank and as the feeding liquid of the 3rd drip washing resin column group, finishes synchronously lithium ion exchanged, the quick drip washing of resin column and the washing process of resin column;
Step 3: behind a upper end cycle, make five groups of resin column groups between a plurality of resin columns, carry out the combination of next cycle by the control valve that switches on the resin column;
Step 4: salt lake brine and washings are input to respectively in the adsorption resin column group of next cycle, quick drip washing resin column group and the first drip washing resin column group, finish synchronously the lithium ion exchanged of next cycle, the quick drip washing of resin column and the washing process of resin column, export in the last step resin column of qualifying liquid by the 3rd drip washing resin column group in each cycle.
7. the continuous ionic switching method of extracting lithium from salt lake brine according to claim 6 is characterized in that:
First step resin column in the quick drip washing resin column group in the described step 4 is the first step resin column in the upper cycle adsorption resin column group;
The last step resin column of described adsorption resin column group is the first step resin column in upper cycle the 3rd drip washing resin column group; Last step resin column in described the first drip washing resin column group was the first step resin column in the quick drip washing resin column group of the upper cycle.
8. it is characterized in that according to claim 6 or the 7 described continuous ionic switching methods of from salt lake brine, extracting lithium:
Described salt lake brine is from the top feed liquor of adsorption resin column group, described washings is respectively from the top feed liquor of described quick drip washing resin column group and the first drip washing resin column group, and described top feed liquor is flowed through after the resin column group of appointment and in the bottom of its last step resin column fluid;
The leacheate of described the first drip washing resin column group is by the bottom output of its last step resin column, and as the top feeding liquid of the second drip washing resin column group, the leacheate of described the second drip washing resin column group is by the bottom output of its last step resin column, and as the top feeding liquid of the 3rd drip washing resin column group, qualifying liquid is by the bottom output of the last step resin column of the 3rd drip washing resin column group.
9. the continuous ionic switching method of extracting lithium from salt lake brine according to claim 8 is characterized in that:
The treatment rate of the salt lake brine in the described adsorption resin column group is 5-10BV/h, treatment capacity 20-60BV;
The treatment rate of the washings in the described quick drip washing resin column group is 5-20BV/h, treatment capacity 2-4BV;
The treatment rate of the washings in described the first drip washing resin column group, the second drip washing resin column group and the 3rd drip washing resin column group is 3-5BV/h, treatment capacity 2-6BV;
The time 2-12h that the wherein said control valve cycle switches.
10. the continuous ionic switching method of extracting lithium from salt lake brine according to claim 9 is characterized in that:
Magnesium lithium mass concentration ratio is 10-15 in the top feeding liquid of described the second drip washing resin column group, and magnesium lithium mass concentration ratio is 5-10 in the out-feed liquid of its underpart; The magnesium lithium mass concentration ratio of the qualifying liquid of exporting in the last step resin column by described the 3rd drip washing resin column group is＜5.
11. the continuous ionic switching method of extracting lithium from salt lake brine according to claim 9 is characterized in that:
The temperature of the salt lake brine in the described adsorption resin column group is 20-100 ℃;
Washings in described rapid resin post group, the first resin column group is 20-50 ℃ deionized water.
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| CN108517421B (en) * | 2018-07-02 | 2020-10-16 | 西安蓝晓科技新材料股份有限公司 | Method for separating lithium and sodium in lithium and sodium-containing solution |
| CN109264835B (en) * | 2018-10-09 | 2021-08-06 | 天津科技大学 | Continuous electrochemical element extraction system |
| CN111041201A (en) | 2019-12-30 | 2020-04-21 | 西安蓝晓科技新材料股份有限公司 | Novel method for extracting lithium from salt lake brine |
| CN111197123A (en) * | 2020-01-15 | 2020-05-26 | 西安蓝晓科技新材料股份有限公司 | Novel method for separating lithium and sodium |
| CN113072081A (en) * | 2021-03-25 | 2021-07-06 | 四川恩特普环保科技有限公司 | Impurity removal process for lithium sulfate purification completion liquid |
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| CN116356144A (en) * | 2021-12-28 | 2023-06-30 | 比亚迪股份有限公司 | Method for extracting lithium from salt lake |
| CN118272670A (en) * | 2022-12-30 | 2024-07-02 | 西安蓝晓科技新材料股份有限公司 | Preparation method and application of adsorption unit for lithium recovery |
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| CN1243112C (en) * | 2002-12-27 | 2006-02-22 | 中国科学院青海盐湖研究所 | Process for extracting lithium from salt lake brine by adsorptive method |
| CN201825992U (en) * | 2010-10-29 | 2011-05-11 | 西安蓝晓科技有限公司 | Continuous ion exchange device extracting lithium from salt lake brine |
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