CN104383901B - A kind of method recovering lithium adsorbent performance - Google Patents
A kind of method recovering lithium adsorbent performance Download PDFInfo
- Publication number
- CN104383901B CN104383901B CN201410725724.2A CN201410725724A CN104383901B CN 104383901 B CN104383901 B CN 104383901B CN 201410725724 A CN201410725724 A CN 201410725724A CN 104383901 B CN104383901 B CN 104383901B
- Authority
- CN
- China
- Prior art keywords
- lithium
- ammonium salt
- solution
- adsorbent
- lithium adsorbent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of method recovering lithium adsorbent performance, first ammonium salt and salt-free water are sufficiently mixed, stir formation ammonium salt solution stock solution, described ammonium salt solution stock solution and described salt-free water being sufficiently mixed and being configured to concentration is 100kg/m3To 150kg/m3The first ammonium salt solution；Then it is (50～240) by volume ratio: it is 0.6kg/m that the described salt-free water of 1.0 and described first ammonium salt solution are hybridly prepared into concentration mutually3To 2.0kg/m3The second ammonium salt solution；Finally by described lithium adsorbent classification convection current saturated with absorption for described second ammonium salt solution through meeting the time of staying of technological requirement, until described lithium adsorbent makes the absorption property of himself be restored while resolving the lithium chloride of its absorption, the formation of lithium adsorbent inorganic salt is polluted in suppression simultaneously.The method that the present invention provides can solve the defect of lithium adsorbent hydraulic performance decline in operation, it is simple to control production cost and production capacity is stable.
Description
Technical field
The present invention relates to inorganic adsorbent field, particularly relate to absorption method and obtain from the lake bittern water containing lithium salts
The adsorbent longtime running of lithium be insoluble to water inorganic salt pollute after hydraulic performance decline, recover its performance
Method.
Background technology
Lithium resource in nature is mainly composed and is stored in granitic pegmatite-type mineral deposit, salt lake bittern, sea water
And in GEOTHERMAL WATER, owing to salt lake bittern resource is successively verified, salt lake bittern lithium resource reserves account for lithium
The 70%～80% of total resources (gross reserves about 1.466 × 107t).Wherein salt lake bittern lithium reserves
More than 3 × 106t, there is good resources supplIes and DEVELOPMENT PROSPECT.China's salt lithium resource reserves occupy
Third place in the world, is distributed mainly in the salt lake in Qinghai and Tibet, wherein Chaidamu Basin, Qinghai Province salt
The reserves of lake lithium resource rank first in the whole country, and have lithium chloride reserves about 15,000,000 tons.It is positioned at
The Cha Er Han Salt Lake LiCl reserves in the Caidamu Basin are 833.7 ten thousand tons, are the important lithium resources of China
Ground.This lake bittern water belongs to chloride type, after concentration in old halogen the most relatively low about 200ppm of lithium concentration～
300ppm, Mg/Li ratio is reduced to about 500, for this high Mg/Li ratio by thousands of in former halogen
Salt lake bittern, the exploitation optimum selection of lithium resource is the excellent suction selecting to have selective absorption lithium
Attached dose carries out separating magnesium and lithium.
Taking off the lithium carbonate produced of analysis by adsorbent is that a kind of important and indispensable industry is former
Material, is mainly used in the essential industry necks such as battery, lubricant, pottery, glass, air-conditioning, pharmacy
Territory.Lithium carbonate is the initial feed in anode material of lithium battery and electrolyte, is that lithium battery is most important
Raw material, along with the lithium battery demand in new-energy automobile field increases, new-energy automobile will drive
Lithium carbonate demand burst increases.
ZL01823738X discloses a kind of method and enforcement the method obtaining lithium chloride from saline solution
Equipment, its method is through loading the bed of lithium adsorbent containing lithium salts water, and lithium adsorbent selects to adsorb it
Lithium chloride molecule in saline, uses the lithium chloride adsorbed in duct in fresh water desorption lithium adsorbent,
Thus obtain rich lithium chloride solution.
The disclosed method obtaining lithium chloride from saline solution of ZL01823738X, the selective absorption of lithium carries
Take, by making in adsorption zone containing lithium salt and having lithium the adsorbent selecting absorption to transport in classification convection current
Disorder of internal organs contacts through certain adsorbent hydroxyl aluminum, it is ensured that lithium chloride is fully adsorbed full by adsorbent
With.The parsing of lithium chloride solution, carries out lithium chloride with salt-free water to adsorbent in classification convection current
The parsing of solution.
The defect that the method is applied in Salt-lake brine then at, after longtime running, lithium adsorbent has
The defect that absorption property declines.
Salt lake bittern is a kind of saline containing polyionic high concentration, and leading ion form has
Mg2+(magnesium ion), Na+(sodium ion), K+(potassium ion), Li+(lithium ion), Cl-(chlorine root from
Son, SO42-(sulfate ion), B (OR)3-(borate ion) etc., pH value is at 6-7, weak
Acid.Described method is during adsorption zone is adsorbed-resolved, and salt lake bittern is continuous in adsorption zone
Dilution, is affected by weak acid strong alkali salt in brine systems, is had weak acid strong alkali salt in salt dilution
Hydrolysis, described during salt pH value constantly rise, pH value is interval at 8.0-9.5.
Salt and salt-free water are certain during adsorbing in the convective motion of adsorption zone in stop contact process
In time, pH value has described hydrolysis at 8.0-9.5, with hydroxide precipitated product, institute
State precipitated product in adsorption zone, gradually adhere to lithium adsorbent surface, nano-pore in blocking adsorbent
Net, affects it and declines the selective absorption of lithium chloride in salt, lithium adsorbent absorption property.
Therefore, manufacturing enterprise, desirable to provide a kind of method recovering lithium adsorbent performance, solves to run
The defect of middle lithium adsorbent hydraulic performance decline, it is simple to control production cost and production capacity is stable.
Summary of the invention
To this end, the present invention proposes and a kind of can solve at least one of novel extensive of the problems referred to above
The method of multiple lithium adsorbent performance.
According to an aspect of the invention, it is provided a kind of method recovering lithium adsorbent performance, bag
Include following steps:
The preparation steps of ammonium salt solution: ammonium salt and salt-free water are sufficiently mixed, stir formation ammonium salt
Solution stock solution,
Described ammonium salt solution stock solution and described salt-free water being sufficiently mixed and being configured to concentration is 100
kg/m3To 150kg/m3The first ammonium salt solution；
Preparation steps for lithium adsorbent parsing solution:
It is (50～240) by volume ratio: the described salt-free water of 1.0 and described first ammonium salt solution phase
Being hybridly prepared into concentration is 0.6kg/m3To 2.0kg/m3The second ammonium salt solution；
Lithium adsorbent is used to resolve solution to the recovery of lithium adsorbent absorption property and suppression technique step
Rapid:
By described lithium adsorbent classification convection current saturated with absorption for described second ammonium salt solution through meeting
Technological requirement the time of staying, until described lithium adsorbent is lithium chloride same resolving its absorption
Time make the absorption property of himself be restored, simultaneously suppression pollute lithium adsorbent inorganic salt shape
Become.
Alternatively, according to an embodiment of the invention, solution pair is resolved using lithium adsorbent
In the recovery of lithium adsorbent absorption property and suppression processing step, keep described second ammonium salt solution
Temperature is at 20 DEG C to 40 DEG C.
The method recovering lithium adsorbent performance that the present invention provides uses one to recover lithium adsorbent absorption
The technique that performance and prevention lithium adsorbent absorption property decline, at least can solve the problem that and inhales with salt lake bittern
Attached carry in lithium technique, solve the contamination and plugging absorption duct owing to inorganic salt forms microscopic precipitate thing,
The defect of lithium adsorbent hydraulic performance decline in causing running.The method that the present invention provides is in industrial applications
In be beneficial to realize, its discharge product do not introduce any foreign ion, Cha Er Han Salt Lake is not caused
Any impact, belongs to environmental protection technique, is particularly suited for aluminum system lithium adsorbent and obtains from salt lake bittern
Obtain the recovery absorption property after lithium.
Accompanying drawing explanation
By reading the detailed description of hereafter preferred implementation, various other advantage and benefit pair
Will be clear from understanding in those of ordinary skill in the art.Accompanying drawing is only used for illustrating preferred implementation
Purpose, and be not considered as limitation of the present invention.And in whole accompanying drawing, with identical
Reference marks represents identical parts.The most in the accompanying drawings, the alphabetic flag after reference number refers to
Show multiple identical parts, when referring to these parts, its last alphabetic flag will be omitted.?
In accompanying drawing:
Fig. 1 shows a preferred embodiment of the invention process chart；
Fig. 2 shows that lithium adsorbent is with salt-free water and certain density ammonium salt solution as lithium adsorbent
Desorbed solution time, the PH change curve of desorbed solution in absorption resolving；
Fig. 3 shows under the conditions of different desorbed solutions (salt-free water and the salt-free water containing ammonium salt)
The change of lithium adsorbent surface contamination exponential quantity；
Fig. 4 shows industrialized unit 35# adsorption tower lithium adsorbent application salt-free water and joins in proportion
The ammonium salt water put change curve of lithium adsorbent adsorption capacity in the resolving of lithium；And
Fig. 5 shows a preferred embodiment of the invention process flow diagram.
Wherein: salt-free water 1, preparation ammonium salt solution storage tank 2,100kg/m3-150kg/m3Ammonium salt
Solution 3,0.6kg/m3-2.0kg/m3Ammonium salt solution 4, blender 5, adsorption zone 6, lithium chloride are molten
Liquid 7.
Detailed description of the invention
The invention provides many applicable creative concepts, this creativeness concept can substantial amounts of body
Now in concrete context.In the specific embodiment described in following embodiments of the present invention
It is only used as the exemplary illustration of the detailed description of the invention of the present invention, and does not constitute the scope of the invention
Limit.
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Carrying in lithium technique with salt lake bittern absorption, polluting owing to inorganic salt forms microscopic precipitate thing
Blocking absorption duct, lithium adsorbent hydraulic performance decline in causing running.In order to recover lithium adsorbent absorption
Performance and prevention lithium adsorbent absorption property decline, and the invention provides a kind of recovery lithium adsorbent
The method of energy.According to the process chart shown in Fig. 1, initially enter joining of S1100 ammonium salt solution
Step processed, subsequently enters S1200 and resolves the preparation steps of solution for lithium adsorbent, finally enter
S1300 uses lithium adsorbent to resolve solution to the recovery of lithium adsorbent absorption property and suppression technique step
Suddenly.
Specifically, the preparation steps of S1100 ammonium salt solution: ammonium salt and salt-free water are sufficiently mixed,
Stirring forms ammonium salt solution stock solution, described ammonium salt solution stock solution is sufficiently mixed with described salt-free water
Being configured to concentration is 100kg/m3To 150kg/m3The first ammonium salt solution.
Described ammonium salt includes ammonium chloride, ammonium carbonate or ammonium hydrogen carbonate etc..
Sodium chloride content≤100ppm in the water quality requirement of described salt-free water.
In this step, the preparation of the first ammonium salt solution be in container by described ammonium salt solution stock solution with
Described salt-free water is sufficiently mixed stirring, controls uniform temperature to ensure fully to dissolve.
S1200 resolves the preparation steps of solution for lithium adsorbent: be (50～240) by volume ratio:
It is 0.6kg/m that the described salt-free water of 1.0 and described first ammonium salt solution are hybridly prepared into concentration mutually3
To 2.0kg/m3The second ammonium salt solution.
Wherein, described salt-free water is (50～240) with the volume ratio of described first ammonium salt solution:
1.0, the described second ammonium salt solution concentration being configured to is 0.6kg/m3To 2.0kg/m3, these two skills
Art index must reach simultaneously.
In this step, produce within battery limit, resolve solution and the ammonium salt configured for lithium adsorbent
Solution uniformly mixes.Preferably, salt-free water is 50-160 with the ammonium salt solution control ratio of high concentration
To ensure that in solution bleed, ammonium salt concentration reaches 0.6kg/m3To 2.0kg/m3。
S1300 uses lithium adsorbent to resolve solution to the recovery of lithium adsorbent absorption property and suppression work
Skill step:
By described lithium adsorbent classification convection current saturated with absorption for described second ammonium salt solution through meeting
Technological requirement the time of staying, until described lithium adsorbent is lithium chloride same resolving its absorption
Time make the absorption property of himself be restored, simultaneously suppression pollute lithium adsorbent inorganic salt shape
Become.Alternatively, by described lithium adsorbent classification convection current saturated with absorption for described second ammonium salt solution
Through certain time of staying 3h.Lithium adsorbent is made while resolving the lithium chloride of lithium adsorbent absorption
Absorption property be restored, the inorganic salt polluting lithium adsorbent in this running is sent out with ammonium salt
Biochemical reaction, forms water-soluble inorganic matter, enters desorbed solution system.Apply the second ammonium salt
Resolve and lithium adsorbent adsorbing chlorinated lithium running ensures the pH value environment less than 8, its environment
Can suppress to pollute lithium adsorbent inorganic salt to be formed.
Lithium adsorbent is used to resolve solution to the recovery of lithium adsorbent absorption property and suppression at S1300
In processing step, keep the temperature of described second ammonium salt solution at 20 DEG C to 40 DEG C.That is, inhale at lithium
The temperature of ammonium salt solution 20 DEG C to 40 DEG C in attached dose of absorption, resolving.
Generally speaking, the method is characterized in that: select the solution containing ammonium salt to inhale as lithium
The attached dose of solution resolving lithium chloride, controls lithium adsorbent by ammonium salt solution and runs in absorption, parsing
During pH value environment, it is ensured that during described solution pH value be less than 8.
Second ammonium salt solution resolves the solution of lithium chloride, its concentration 0.6kg/m as lithium adsorbent3Extremely
2.0kg/m3, the temperature 20 DEG C of the second ammonium salt solution in lithium adsorbent absorption, resolving simultaneously
To 40 DEG C.
The recovery lithium adsorbent absorption property method that the present invention provides is beneficial to realize in industrial applications
And it being applied to industrialized production, the product of its discharge does not introduce any foreign ion, not to Cha Er
Antiperspirant salt lake has any impact, and belongs to environmental protection technique, and this technique is particularly suited for the lithium absorption of aluminum system
Agent obtains the recovery absorption property after lithium from salt lake bittern.
Method offer of the present invention being recovered lithium adsorbent performance below in conjunction with Fig. 5 explains:
1, the preparation of ammonium salt solution, by ammonium salt and salt-free water 1 in preparation ammonium salt solution storage tank 2
Being sufficiently mixed stirring, control uniform temperature and fully dissolve with guarantee, the first ammonium salt made is molten
The concentration of liquid 3 is 100kg/m3To 150kg/m3。
2, the finite concentration ammonium salt solution recovery technique to lithium adsorbent absorption property is used.
Producing within battery limit, resolving solution for lithium adsorbent and the first ammonium salt solution configured exists
Uniformly mixing in blender 5, salt-free water with the second ammonium salt solution control volume ratio of high concentration is
(50～240): 1.0, to ensure that in solution bleed, ammonium salt concentration reaches 0.6kg/m3To 2.0kg/m.
Described ammonium salt-containing solution is to adsorbing in saturated lithium chloride resolving in lithium adsorbent, one
Recovery to adsorbent performance simultaneously at a temperature of Ding.Specifically, lithium adsorbent absorption, solution
Analysis process is carried out in adsorption zone 6, and during this, the second ammonium salt solution temperature is maintained at 20 DEG C to 40
DEG C, finally give lithium chloride solution 7.
The method is characterized in that: select the solution containing ammonium salt to resolve chlorine as lithium adsorbent
Change the solution of lithium, control lithium adsorbent PH in absorption, parsing running by ammonium salt solution
Value environment, it is ensured that during described, solution pH value is less than 8.
In order to illustrate further the advantage of the method recovering lithium adsorbent performance that the present invention provides,
Inventor has also done volume of data and has been analyzed as follows:
Fig. 2 be lithium adsorbent in industrialized unit with salt-free water and certain density ammonium salt solution
During for the desorbed solution of lithium adsorbent, PH change curve in absorption resolving.In Fig. 2, vertical seat
Being designated as pH value in desorbed solution, abscissa is desorbed solution sample volume.PH curve table in salt-free water
Showing and do not add ammonium salt desorbed solution, lithium adsorbent adsorbs the pH value of solution in saturated rear resolving
More than 8；In ammonium salt solution, PH curve is to add ammonium salt in proportion to carry out solution in resolving
PH value is less than 8, destroys water-fast inorganic salt formation condition, makes the adsorptivity of lithium adsorbent
Can be recovered and kept.
Fig. 3 is that water-fast inorganic salt takes off analysis process in lithium adsorbent absorption in industrialized unit
In pollution index value to lithium adsorbent.Vertical coordinate is lithium adsorbent pollution index %, and abscissa is
Absorption de-analysis period.In Fig. 3 industrialized unit lithium adsorbent pollutant index change curve,
Front 1950 circulations apply salt-free water washing after stain index for lithium adsorbent in absorption resolving
Data Detection value, water-fast inorganic salt is in rising trend to adsorbent pollution index, pollute
Index reaches to tend to a more stable value when about 20；1950-2080 circulation is disguised for 35# tower industry
Put lithium adsorbent and with the addition of a certain proportion of ammonium salt solution after stain index in absorption resolving
Data Detection value, inorganic salt to the pollution index of adsorbent along with the increase of ammonium salt solution period
On a declining curve, pollution index is when less than 5, and lithium adsorbent absorption property has been restored and has set
Evaluation is consistent.
Fig. 4 is for showing industrialized unit 35# adsorption tower lithium adsorbent application salt-free water and in proportion
Ammonium salt water change curve of lithium adsorbent adsorption capacity in the resolving of lithium of configuration, vertical seat
Being designated as lithium adsorbent adsorption capacity, unit: mg/g, before abscissa, 1-28 circulation takes off for novel sorbents
Analysis period, when middle 1-34 circulation is 18-20 for pollution index, adsorbent de-analysis period,
Back segment 1-35 circulation is adsorbent de-analysis period, unit: individual after lithium adsorbent performance recovery.Before
1-28 circulation for No. 35 adsorption tower lithium adsorbents (novel sorbents) in industrialized unit with salt-free water is
During desorbed solution, lithium adsorbent absorption property during water-fast inorganic salt pollution index≤5 in operation
Statistical data, the absorption property value of its lithium adsorbent is in scope of design；In curve chart, second
Section curve 1-34 circulation is the inorganic salt pollution index of No. 35 adsorption tower lithium adsorbents of industrialized unit
For absorption property statistical data during 18-20, on a declining curve, its absorption property value is deposited with design load
In deviation；In curve chart, the 3rd section of curve: 1-35 circulation is No. 35 adsorption tower lithiums of industrialized unit
The adsorbent desorbed solution with certain density ammonium salt solution as lithium adsorbent is examined after running about 130 circulations
The statistical data of its absorption property when surveying inorganic salt pollution index≤5 in its lithium adsorbent, with necessarily
The ammonium salt solution of concentration is lithium adsorbent desorbed solution, and adsorbent performance is recovered.
Method offer of the present invention being recovered lithium adsorbent performance below in conjunction with Fig. 2-5 is entered further
Row is explained: taking the lithium adsorbent polluted by inorganic salt, described adsorbent includes water-fast inorganic
Salt 19.43%, is placed in commercial plant absorption examination post.Application Cha Er Han Salt Lake potash fertilizer produces discharge height
Mg/Li ratio try the adsorbent warp in classification convective motion in post containing lithium salt with described being filled in
Cross one section of adsorbent hydroxyl aluminum and contact, adsorb saturated.Make 0.6kg/m again3-2kg/m3Ammonium salt solution
The lithium adsorbent classification convection current saturated with described absorption resolves time of staying parsing through one section inhale
Lithium chloride in attached dose, repeats process about 112 circulation of described absorption-parsing.
De-analysis liquid pH value result during described industrialized unit absorption examination column operation as in figure 2 it is shown,
Meet PH in running environment and be less than 8；In described industrialized unit in lithium adsorbent detection data not
It is dissolved in the result of the inorganic salt pollution index of water as it is shown on figure 3, contaminated lithium adsorbent adsorptivity
Can with the lithium adsorbent absorption property result of variations of the water-fast inorganic salt of removing as shown in Figure 4.
The described method recovering contaminated lithium adsorbent performance is in the annual output using absorption method to produce
It is applied on the device of 10000 tons of high-purity high-quality lithium carbonate.Its application effect is consistent with experimental result.
Embodiment
Embodiment 1
Taking the aluminum system lithium adsorbent of the contaminants not being insoluble to water, described adsorbent includes
Pollution index is 0, is placed in laboratory adsorption examination post.Application Cha Er Han Salt Lake potash fertilizer produces discharge
High Mg/Li ratio containing lithium salt with the adsorbent 500ml being filled in trying in post at classification convective motion
Middle through one section of adsorption time, reapply 0.6kg/m3Ammonium salt solution, temperature controls at 30 DEG C, right
It carries out the lithium chloride in classification convection current Dissociative adsorption agent, resolves pH value environment in running,
Less than 8；Insoluble in water in lithium adsorbent is detected after repeating described absorption-resolving 112 circulation
Inorganic salt pollution index is less than 1.
It is, after salt-free water carries out 112 circulations of absorption parsing to lithium adsorbent, to detect lithium with desorbed solution
In adsorbent, water-fast inorganic salt pollution index is 15.
Using the solution containing ammonium salt is desorbed solution, can effectively suppress water insoluble at this concentration
Inorganic salt form the prevention pollution to lithium adsorbent, lithium adsorbent absorption property is at this running
In there is no downward trend.
Embodiment 2
Take the aluminum system lithium adsorbent of the contaminants being insoluble to water, described adsorbent pollution index
It is 19.47, is placed in laboratory adsorption examination post.Application Cha Er Han Salt Lake potash fertilizer produces the high magnesium of discharge
Passing through in classification convective motion with the adsorbent 500ml being filled in trying in post containing lithium salt of lithium ratio
One section of adsorption time, reapplies 1.3kg/m3Ammonium salt solution, temperature controls, at 30 DEG C, to carry out it
Lithium chloride in classification convection current Dissociative adsorption agent, after repeating described absorption-resolving 112 circulation
In detection lithium adsorbent, the inorganic salt pollution index of insoluble in water is less than 4.Make lithium adsorbent adsorptivity
Can be recovered.
Embodiment 3
Take the aluminum system lithium adsorbent of the contaminants being insoluble to water, described adsorbent pollution index
It is 20, is placed in laboratory adsorption examination post.Application Cha Er Han Salt Lake potash fertilizer produces the high magnesium lithium of discharge
Ratio containing lithium salt and the adsorbent 500ml being filled in trying in post in classification convective motion through one
Section adsorption time, reapplies 2kg/m3Ammonium salt solution, temperature controls, at 30 DEG C, it to be carried out classification
Lithium chloride in convection current Dissociative adsorption agent, detects after repeating described absorption-resolving 112 circulation
In lithium adsorbent, the inorganic salt pollution index of insoluble in water is less than 3.Lithium adsorbent absorption property is made to obtain
Arrive recovery.The inorganic salt polluting lithium adsorbent in this running occurs chemistry anti-with ammonium salt
Should, form water-soluble inorganic matter, enter desorbed solution system；The product of its discharge does not introduce appoints
What foreign ion, does not has any impact to Cha Er Han Salt Lake, belongs to environmental protection technique.
Embodiment 4
Take the aluminum system lithium adsorbent of the contaminants being insoluble to water, described adsorbent pollution index
It is 19.47, is placed in the absorption examination post of industrialized unit.Application Cha Er Han Salt Lake potash fertilizer produces discharge
High Mg/Li ratio containing lithium salt and be filled in trying the adsorbent 40M in post3At classification convective motion
Middle through one section of adsorption time, reapply 0.6kg/m3Ammonium salt solution, temperature controls at 40 DEG C, right
Its lithium chloride carried out in classification convection current Dissociative adsorption agent, repeats described absorption-resolving 120
Detecting the inorganic salt pollution index of insoluble in water in lithium adsorbent after circulation is less than 4.Make lithium adsorbent
Absorption property is recovered.
Embodiment 5
Take the aluminum system lithium adsorbent of the contaminants being insoluble to water, described adsorbent pollution index
It is 19.47, is placed in the absorption examination post of industrialized unit.Application Cha Er Han Salt Lake potash fertilizer produces discharge
High Mg/Li ratio containing lithium salt with the adsorbent 40M3 being filled in trying in post at classification convective motion
Middle through one section of adsorption time, reapply 0.6kg/m3Ammonium salt solution, temperature controls at 20 DEG C, right
Its lithium chloride carried out in classification convection current Dissociative adsorption agent, repeats described absorption-resolving 150
Detecting the inorganic salt pollution index of insoluble in water in lithium adsorbent after circulation is less than 5.
Embodiment 6: take the aluminum system lithium adsorbent of the contaminants being insoluble to water, described absorption
Agent pollution index is 16.28, is placed in the absorption examination post of industrialized unit.Application Cha Er Han Salt Lake potassium
Dividing with the adsorbent 40M3 being filled in trying in post containing lithium salt of the fertile high Mg/Li ratio producing discharge
Through one section of adsorption time in level convective motion, reapply 2kg/m3Ammonium salt solution, temperature controls
40 DEG C, it is carried out the lithium chloride in classification convection current Dissociative adsorption agent, repeat described absorption-parsed
Detecting the inorganic salt pollution index of insoluble in water in lithium adsorbent after journey about 110 circulation is less than 4.
In this running, pollute inorganic salt and the ammonium salt generation chemical reaction of lithium adsorbent, formed
Water-soluble inorganic matter, enters desorbed solution system；Its discharge product do not introduce any impurity from
Son, does not has any impact to Cha Er Han Salt Lake, belongs to environmental protection technique.
In order to further verify the method recovering lithium adsorbent performance that the present invention provides, inventor
Always according to the condition of embodiment 1-3, ammonium salt solution temperature is controlled 20 DEG C, 25 DEG C, 35 DEG C,
Tested at 40 DEG C；According to the condition of embodiment 4 and 6, ammonium salt solution temperature is controlled
20 DEG C, 25 DEG C, 30 DEG C, carried out experiment under conditions of 35 DEG C；According to the condition of embodiment 5,
Ammonium salt solution temperature is controlled 25 DEG C, 30 DEG C, 35 DEG C, tested under the conditions of 40 DEG C, real
Detect the inorganic salt pollution index of insoluble in water in lithium adsorbent after testing and be respectively less than 5.
Advantages of the present invention and beneficial effect: the present invention inhales as lithium with the ammonium salt solution of certain concentration
The attached dose of solution resolving lithium chloride, changes the hydrolysis form in described absorption, resolving,
Control the pH value during this, it is to avoid or remove absorption and carry lithium technique obtains lithium chloride solution
In operation, lithium adsorbent channel surfaces attachment inorganic salt water-insoluble is formed, thus suppresses lithium to adsorb
Agent absorption property declines and has recovered lithium adsorbent adsorptivity.
The present invention makes the production using absorption method to extract lithium chloride from salt lake brine with high magnesium-lithium ratio to have
Effect, stable carrying out, it is to avoid because lithium adsorbent hydraulic performance decline causes yield to reduce, production cost increases
The risk added.
It should be noted that above-described embodiment the present invention will be described rather than carries out the present invention
Limit, and those skilled in the art can set without departing from the scope of the appended claims
Count out alternative embodiment.In the claims, any reference marks between bracket should not will be located in
It is configured to limitations on claims.Word " comprises " not exclude the presence of and does not arranges in the claims
Element or step.Word "a" or "an" before being positioned at element does not excludes the presence of multiple
Such element.Word first, second and third use do not indicate that any order.Can
It is title by these word explanations.
Claims (1)
1. the method recovering lithium adsorbent performance, comprises the steps:
(S1100) preparation steps of ammonium salt solution: ammonium salt is sufficiently mixed with salt-free water, stirs
Form ammonium salt solution stock solution,
Described ammonium salt solution stock solution and described salt-free water being sufficiently mixed and being configured to concentration is 100
kg/m3To 150kg/m3The first ammonium salt solution；
(S1200) for the preparation steps of lithium adsorbent parsing solution:
It is (50～240) by volume ratio: the described salt-free water of 1.0 mixes with described first ammonium salt solution
It is 0.6kg/m that conjunction is configured to concentration3To 2.0kg/m3The second ammonium salt solution；
(S1300) lithium adsorbent is used to resolve solution to the recovery of lithium adsorbent absorption property and suppression
Processing step:
Keep the temperature of described second ammonium salt solution at 20 DEG C to 40 DEG C,
By described lithium adsorbent classification convection current saturated with absorption for described second ammonium salt solution through meeting
The time of staying of technological requirement, until described lithium adsorbent is while resolving the lithium chloride of its absorption
The absorption property making himself is restored, and the formation of lithium adsorbent inorganic salt is polluted in suppression simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410725724.2A CN104383901B (en) | 2014-12-03 | 2014-12-03 | A kind of method recovering lithium adsorbent performance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410725724.2A CN104383901B (en) | 2014-12-03 | 2014-12-03 | A kind of method recovering lithium adsorbent performance |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104383901A CN104383901A (en) | 2015-03-04 |
| CN104383901B true CN104383901B (en) | 2016-08-24 |
Family
ID=52601912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410725724.2A Active CN104383901B (en) | 2014-12-03 | 2014-12-03 | A kind of method recovering lithium adsorbent performance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104383901B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761249B (en) * | 2018-12-07 | 2021-07-27 | 开曼铝业（三门峡）有限公司 | Method and system for resolving lithium in lithium-rich adsorbent of alumina plant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257751A (en) * | 1999-12-23 | 2000-06-28 | 华南理工大学 | Process for preparing high-adsorptivity compound adsorbent of lithium chloride |
| CN102602966A (en) * | 2012-04-06 | 2012-07-25 | 华东理工大学 | Method for separating magnesium and lithium in salt lake brine and preparing lithium carbonate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH105585A (en) * | 1996-06-27 | 1998-01-13 | Toagosei Co Ltd | Lithium ion adsorbing agent |
-
2014
- 2014-12-03 CN CN201410725724.2A patent/CN104383901B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257751A (en) * | 1999-12-23 | 2000-06-28 | 华南理工大学 | Process for preparing high-adsorptivity compound adsorbent of lithium chloride |
| CN102602966A (en) * | 2012-04-06 | 2012-07-25 | 华东理工大学 | Method for separating magnesium and lithium in salt lake brine and preparing lithium carbonate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104383901A (en) | 2015-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chen et al. | Development of recovering lithium from brines by selective-electrodialysis: Effect of coexisting cations on the migration of lithium | |
| Lan et al. | Recycling of spent nitric acid solution from electrodialysis by diffusion dialysis | |
| CN103386299B (en) | A kind of non-woven group compound film for lithium isotope separation and preparation method thereof and the isotopic method of membrane chromatography separating Li | |
| Zhao et al. | Separating and recovering lithium from brines using selective-electrodialysis: Sensitivity to temperature | |
| CN101928828B (en) | Method for extracting lithium from salt lake brine by adsorption method | |
| Suren et al. | Uphill transport and mathematical model of Pb (II) from dilute synthetic lead-containing solutions across hollow fiber supported liquid membrane | |
| AU2011349335B2 (en) | Rhenium recovery | |
| CN103570048A (en) | Method for refining lithium from salt lake brine with high magnesium-lithium ratio | |
| CN104383901B (en) | A kind of method recovering lithium adsorbent performance | |
| CN109368670A (en) | A kind of method of the separation and enrichment of lithium | |
| AU2012241177B2 (en) | Enhanced staged elution of loaded resin | |
| CN110658143A (en) | Method for measuring contents of trace elements of bismuth, cadmium, chromium, copper, iron, lead, zinc, nickel, cobalt and manganese in high-concentration brine | |
| CN102643990B (en) | Method for removing trace Cu in high-purity Ni by chelate resin | |
| CN103502484A (en) | Method for recovering platinum group metals from industrial waste containing platinum group metals | |
| CN105523531A (en) | Production of electroplating-grade nickel aminosulfonate or electroplating-grade cobalt aminosulfonate through ion exchange method | |
| JP5662690B2 (en) | Method for producing ammonium tungstate aqueous solution | |
| CN109535474B (en) | Coated impregnating resin, preparation method thereof and application thereof in selective adsorption of rhenium in waste acid | |
| CN106086405A (en) | A kind of purifying and impurity-removing method of high salt Chloride System | |
| CN106048218A (en) | Purification and impurity removal method for lithium chloride mixed solution | |
| CN106507816B (en) | The method for extracting lithium from bittern | |
| CN103820652B (en) | Method for extracting strontium from mixed salt solution | |
| CN115806301A (en) | Method for preparing lithium carbonate from high-calcium type deep brine by adsorption method | |
| JP5648231B2 (en) | Purification method of alkaline aqueous solution | |
| CN105293526A (en) | Method for purifying iodine in saline water of ionic membrane caustic soda production process | |
| JP2013119487A (en) | Method for treating hydrosilicofluoric acid-containing liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |