CN101654262A - Device for extracting lithium ions form brine - Google Patents
Device for extracting lithium ions form brine Download PDFInfo
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- CN101654262A CN101654262A CN200910195886A CN200910195886A CN101654262A CN 101654262 A CN101654262 A CN 101654262A CN 200910195886 A CN200910195886 A CN 200910195886A CN 200910195886 A CN200910195886 A CN 200910195886A CN 101654262 A CN101654262 A CN 101654262A
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Abstract
The invention relates to a device for extracting lithium ions from brine by adopting an ion sieve absorption method, which comprises a columnar cylinder body with one closed end, wherein one end of the outer side surface of the columnar cylinder body is provided with a feeding part and the other end of the outer side surface is provided with a discharging part; the closed end of the columnar cylinder body is provided with a waste liquid discharging part and an absorbent discharging part; the columnar cylinder body is internally provided with a stirring shaft, one end of the stirring shaft close to a feeding valve is provided with a plurality of stirring blades; one end of the stirring shaft close to the discharging part is provided with a plurality of turntables; one end of the inner sidesurface of the columnar cylinder body close to the discharging part is provided with a plurality of detachable fixing rings, and the fixing rings and the turntables are formed a turntable tower structure. The device can improve both the absorption quantity of the used absorbent and the absorption speed rate of the absorbent when lithium ions are extracted from the brine, thereby improving the efficiency of the whole production process.
Description
Technical field
The present invention relates to a kind of being used for, specifically, relate to a kind of ion(ic)sieve absorption method that adopts by the device that extracts lithium ion in the bittern from extract the device of lithium ion by water.
Background technology
Bittern (claiming bittern or bittern again), when referring generally to by salt water (seawater, salt lake saline etc.) salt manufacturing residual mother liquor.Contain compound, vitriol and the lithium resource etc. of a large amount of magnesium, potassium, sodium, can be used as the raw material that extracts sylvite, magnesium salts and bromide.
Lithium and compound thereof are strategic resources significant in national economy and the national defense construction, are " promoting world's progressive energy metal ".Along with the continuous exhaustion of the world to the growing of lithium demand and solid mineral resources, comprehensive exploitation and utilize the salt lake brine lithium resource to become the main flow of lithium industrial development.And being a kind of green salt lake brine that has prospect, the ion(ic)sieve absorption method puies forward the lithium method.
Extracting lithium ion at present from bittern mainly is to be achieved by employing " fixed-bed type adsorption-desorption device ", and its main defective is that sorbent material is (as MnO
2Ion(ic)sieve etc.) adsorptive capacity is on the low side.Tracing it to its cause, may be to adopt " fixed-bed type adsorption-desorption device " to carry out in the adsorption process reasons such as mass transfer effect contact surface relatively poor and/or bittern and sorbent material is less.Therefore, the adsorptive capacity that how to improve unit time internal adsorption agent just becomes technical problem underlying to be solved by this invention.
Summary of the invention
The object of the invention is, provides a kind of ion(ic)sieve absorption method that adopts by the device that extracts lithium ion in the bittern, overcomes to have defective in the prior art.
Device of the present invention, it comprises: the cylinder shape cylindrical shell of one one end sealing, be provided with feed pieces at described cylinder shape cylindrical shell outer side one end, be provided with the discharging parts at the described cylinder shape cylindrical shell outer side the other end;
Closed end at described cylinder shape cylindrical shell is provided with waste liquid discharging parts and sorbent material discharging parts;
In described cylinder shape cylindrical shell, be provided with stir shaft, be provided with several agitating vanes, be provided with several rotating disks at nearly discharging parts one end of described stir shaft at nearly feed pieces one end of described stir shaft;
Be provided with several dismountable " set collars " at nearly discharging parts one end of described cylinder shape cylindrical shell medial surface, described " set collar " constitutes the rotating disc contactor structure with described rotating disk.
In optimized technical scheme of the present invention, also be provided with circuit element with described cylinder shape cylindrical shell UNICOM at nearly feed pieces one end of described cylinder shape cylindrical shell outer side, also be provided with the baffling parts in nearly described circuit element one side of described cylinder shape cylindrical shell medial surface.
Description of drawings
Fig. 1 is the structural representation of device of the present invention.
Wherein: 1-agitator motor, 2-stir shaft, 3-cylinder shape cylindrical shell, 4-bleeder valve, 5-" set collar ", 6-rotating disk, 7-agitating vane, 8-baffle, 9-loop pipe, 10-feed valve, 11-waste liquid bleeder valve, 12-sorbent material bleeder valve.
Fig. 2 is the waste liquid bleeder valve 11 of device of the present invention and the sectional view of sorbent material bleeder valve 12.
Fig. 3 is the waste liquid bleeder valve 11 of device of the present invention and the vertical view of sorbent material bleeder valve 12.
Fig. 4 is the vertical view of agitating vane 7 described in Fig. 1.
Fig. 5 is the vertical view of " set collar " 5 described in Fig. 1.
Fig. 6 is the vertical view of rotating disk 6 described in Fig. 1.
Fig. 7 is for adopting different an adsorption devices, MnO
2The comparison diagram of particle adsorption effect
Wherein: X-coordinate is adsorption time (unit: hour), and ordinate zou is a lithium concentration (unit: mmole/gram).
Embodiment
In conjunction with the accompanying drawings, content of the present invention is further elaborated.
As shown in Figure 1:
The said adsorption-desorption device of the present invention, it comprises: the cylinder shape cylindrical shell 3 of one one end sealing, be provided with feed valve 10 at described cylinder shape cylindrical shell 3 outer sides one end, be provided with bleeder valve 4 at the described cylinder shape cylindrical shell 3 outer side the other ends, be provided with loop pipe 9 with described cylinder shape cylindrical shell 3 UNICOMs at nearly feed valve 10 1 ends of described cylinder shape cylindrical shell 3 outer sides;
Closed end at described cylinder shape cylindrical shell 3 is provided with waste liquid bleeder valve 11 and sorbent material bleeder valve 12;
In described cylinder shape cylindrical shell 3, be provided with stir shaft 2 (it links to each other with agitator motor 1), be provided with several agitating vanes 7, be provided with baffle 8 in nearly described loop pipe 9 one sides of described cylinder shape cylindrical shell 3 medial surfaces at nearly feed valve 10 1 ends of described stir shaft 2;
Nearly bleeder valve 4 one ends at described stir shaft 2 are provided with several rotating disks 6, are provided with several dismountable " set collars " 5 at nearly bleeder valve 4 one ends of described cylinder shape cylindrical shell 3 medial surfaces, and described " set collar " 5 constitutes the rotating disc contactor structure with described rotating disk 6.
In the present invention, will be called stirring area by zone between feed valve 10 to first " set collars " 5, and will be called settling section by first " set collar " 5 to zone between the bleeder valve 4.It (is H that the ratio of stirring area and the height of settling section is preferably 3: 2
Stirring area: H
Settling section=3: 2).
In described stirring area, agitating vane 7 on the stir shaft 2 can equidistantly be provided with (being that distance equates between each agitating vane 7) or non-equidistant setting (being that distance is unequal between each agitating vane 7), and agitating vane 7 recommends to use the pusher blade (see figure 4) of four oblique leaf formula axial flows with 45 degree inclination angles.
In described settling section, the internal diameter (Ф between " set collar " 5
1) should be greater than the diameter (Ф of rotating disk 6
2).
A kind of method that adopts adsorption-desorption device mentioned above to remove lithium ion in the bittern, it comprises the steps:
(1) takes by weighing 6g PVC (polymerization degree is 1000 ± 20) and be dissolved in the N-Methyl pyrrolidone (NMP) of 66ml, after the dissolving fully, add 20g powdery Li
4Mn
5O
12Presoma also stirs.Then this mixture is dropwise splashed in the deionized water, and complete with deionized water wash, and the particle that obtains is dry 12h in 105 ℃ of still airs.With the granular Li after the moulding
4Mn
5O
12Granular precursor is inserted in right amount in the HCl solution of 1mol/l of (H/Li=2, mol ratio) and is carried out pickling, and promptly obtaining median size is the granular MnO of 2mm
2Ion(ic)sieve.
With median size (diameter) is the MnO of 2mm
2The ion(ic)sieve particle is filled to stirring area through settling section, MnO
2The obstinate rate of ion(ic)sieve is controlled at 0.5%-5%, and the flow rate control of corresponding bittern is at 0.5ml/min-40ml/min;
(2) under normal temperature and pressure (1atm and 20 ℃～25 ℃), (the laboratory configuration is for containing Li with bittern
+Concentration is the LiCl solution of 10mmol/l, is 10.1 NH by the pH value
3H
2O and NH
4Cl buffered soln is demarcated) introduce stirring area by feed valve 10, to open and stir, stir speed (S.S.) is controlled to be 0.5m/s～2m/s, can observe MnO
2The ion(ic)sieve uniform particles is distributed in the stirring area, particle flow very fast (so, can make the solid-liquid two-phase reach abundant contact, liquid concentration unanimity in the stirring area, the existence of stirring makes mass transfer strengthen, and is more conducive to adsorption operations) in the loop pipe 9.No MnO in the settling section
2Ion(ic)sieve particle, liquid phase bittern flow through settling section stably and arrive bleeder valve 4.
Adsorb after 72 hours, close feed valve 10, treat particles settling, when bittern is clarified in the tower, discharge relict bittern in the towers by waste liquid bleeder valve 11.
(3) treat the bittern emptying after, close waste liquid bleeder valve 11, with MnO in the deionized water cleaning tower
2The ion(ic)sieve particle is still got rid of deionized waters by waste liquid bleeder valve 11 after cleaning is finished.
Close waste liquid bleeder valve 11, feed the hydrochloric acid of 1mol/l in the tower by feed valve 10, adsorbing Li
+MnO
2Particle carries out desorption manipulation, after 96 hours, repeats the discharge of waste liquid and the ion(ic)sieve particulate is cleaned.
Behind multiple adsorb-desorption manipulation, MnO
2After the reduction of ion(ic)sieve seed activity reaches work-ing life, then draw off by sorbent material bleeder valve 12.
Set forth the progressive of device of the present invention below by embodiment.
Embodiment
Under normal temperature and pressure (1atm and 20 ℃～25 ℃), with the MnO of same type and same amount
2Ion(ic)sieve particle (additive level of ion(ic)sieve is just the same) is a sorbent material, adopt fixed-bed type adsorption-desorption device (prior art) and device of the present invention to carry out from bittern, extracting the lithium ion experiment respectively, used bittern is disposed voluntarily by the laboratory that (laboratory configuration is for containing Li
+Concentration is the LiCl solution of 10mmol/l, is 10.1 NH by the pH value
3H
2O and NH
4Cl buffered soln is demarcated) lithium ion starting point concentration C wherein
0=10mmol/l gets u
0=2ml/min, stir speed (S.S.) is 0.5m/s in the described device, experimental result is seen Fig. 7.
As shown in Figure 7, in same 72 hours adsorption time, adopt sorbent material (MnO in the described device of invention
2The ion(ic)sieve particle) adsorptive capacity is 3.50mmol/g; And employing fixed-bed type adsorption-desorption device (prior art), the adsorptive capacity of its sorbent material is 3.18mmol/g.And the adsorption rate of sorbent material is also greater than the adsorption rate of sorbent material in the prior art in the device of the present invention.
In summary, adopt the described device of invention to carry out not only can improving sorbent used adsorptive capacity, and can improving adsorbents adsorb speed when extracting lithium ion in the bittern, thereby improve the efficient of whole process of production.
Claims (6)
1, a kind of ion(ic)sieve absorption method that adopts is by the device that extracts lithium ion in the bittern, and it comprises:
The cylinder shape cylindrical shell of one one end sealing is provided with feed pieces at described cylinder shape cylindrical shell outer side one end, is provided with the discharging parts at the described cylinder shape cylindrical shell outer side the other end;
Closed end at described cylinder shape cylindrical shell is provided with waste liquid discharging parts and sorbent material discharging parts;
In described cylinder shape cylindrical shell, be provided with stir shaft, be provided with several agitating vanes, be provided with several rotating disks at nearly discharging parts one end of described stir shaft at nearly feed valve one end of described stir shaft;
Be provided with several dismountable " set collars " at nearly discharging parts one end of described cylinder shape cylindrical shell medial surface, described " set collar " constitutes the rotating disc contactor structure with described rotating disk.
2, device as claimed in claim 1, it is characterized in that, also be provided with circuit element with described cylinder shape cylindrical shell UNICOM at nearly feed pieces one end of described cylinder shape cylindrical shell outer side, also be provided with baffling stopper part in nearly described circuit element one side of described cylinder shape cylindrical shell medial surface.
3, device as claimed in claim 1 or 2 is characterized in that, described device comprises:
The cylinder shape cylindrical shell (3) of one one end sealing, be provided with feed valve (10) at described cylinder shape cylindrical shell (3) outer side one end, be provided with bleeder valve (4) at described cylinder shape cylindrical shell (3) the outer side the other end, be provided with loop pipe (9) with described cylinder shape cylindrical shell (3) UNICOM at nearly feed valve (10) one ends of described cylinder shape cylindrical shell (3) outer side;
Closed end at described cylinder shape cylindrical shell (3) is provided with waste liquid bleeder valve (11) and sorbent material bleeder valve (12);
In described cylinder shape cylindrical shell (3), be provided with stir shaft (2), nearly feed valve (10) one ends at described stir shaft (2) are provided with several agitating vanes (7), are provided with baffle (8) in nearly described loop pipe (9) one sides of described cylinder shape cylindrical shell (3) medial surface;
Nearly bleeder valve (4) one ends at described stir shaft (2) are provided with several rotating disks (6), be provided with several dismountable " set collar " (5) at nearly bleeder valve (4) one ends of described cylinder shape cylindrical shell (3) medial surface, described " set collar " (5) constitute the rotating disc contactor structure with described rotating disk (6).
4, device as claimed in claim 3 is characterized in that, wherein will be called stirring area by feed valve (10) to zone between first " set collar " (5); To be called settling section to zone between the bleeder valve (4) by first " set collar " (5), stirring area is 3: 2 with the ratio of the height of settling section.
5, device as claimed in claim 3 is characterized in that, wherein internal diameter (the Φ between " set collar " (5)
1) greater than the diameter (Φ of rotating disk (6)
2).
6, device as claimed in claim 3 is characterized in that, wherein agitating vane (7) is for having the pusher blade of four oblique leaf formula axial flows at 45 degree inclination angles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101958869A CN101654262B (en) | 2009-09-18 | 2009-09-18 | Device for extracting lithium ions form brine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101958869A CN101654262B (en) | 2009-09-18 | 2009-09-18 | Device for extracting lithium ions form brine |
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| Publication Number | Publication Date |
|---|---|
| CN101654262A true CN101654262A (en) | 2010-02-24 |
| CN101654262B CN101654262B (en) | 2011-05-11 |
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ID=41708757
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101958869A Expired - Fee Related CN101654262B (en) | 2009-09-18 | 2009-09-18 | Device for extracting lithium ions form brine |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102918170A (en) * | 2010-11-26 | 2013-02-06 | 韩国地质资源研究院 | Apparatus and method for adsorbing and desorbing lithium ions using a ccd process |
| CN103517877A (en) * | 2010-11-17 | 2014-01-15 | 韩国地质资源研究院 | Method for preparing high-purity lithium carbonate from brine |
| CN104689858A (en) * | 2013-12-10 | 2015-06-10 | 上海空间电源研究所 | Preparation method of lithium manganate ion sieve separation membrane |
| CN104925836A (en) * | 2015-05-22 | 2015-09-23 | 中国科学院青海盐湖研究所 | Method for extracting lithium from lithium-containing brine |
| CN108236791A (en) * | 2016-12-23 | 2018-07-03 | 蔺钰桢 | A kind of micro- mixed dodge extracts efficient extraction plant and application method |
-
2009
- 2009-09-18 CN CN2009101958869A patent/CN101654262B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103517877A (en) * | 2010-11-17 | 2014-01-15 | 韩国地质资源研究院 | Method for preparing high-purity lithium carbonate from brine |
| CN103517877B (en) * | 2010-11-17 | 2016-06-01 | 韩国地质资源研究院 | The method being prepared high-purity lithium carbonate by saline |
| CN102918170A (en) * | 2010-11-26 | 2013-02-06 | 韩国地质资源研究院 | Apparatus and method for adsorbing and desorbing lithium ions using a ccd process |
| CN102918170B (en) * | 2010-11-26 | 2016-02-03 | 韩国地质资源研究院 | Utilize the lithium ion adsorption/desorption devices and methods therefor of counter-current decantation technique |
| CN104689858A (en) * | 2013-12-10 | 2015-06-10 | 上海空间电源研究所 | Preparation method of lithium manganate ion sieve separation membrane |
| CN104925836A (en) * | 2015-05-22 | 2015-09-23 | 中国科学院青海盐湖研究所 | Method for extracting lithium from lithium-containing brine |
| CN108236791A (en) * | 2016-12-23 | 2018-07-03 | 蔺钰桢 | A kind of micro- mixed dodge extracts efficient extraction plant and application method |
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| Publication number | Publication date |
|---|---|
| CN101654262B (en) | 2011-05-11 |
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Granted publication date: 20110511 Termination date: 20210918 |