CN107138126A - A kind of preparation method of lithium ion sieve adsorbant and the method for adsorbing lithium ion - Google Patents
A kind of preparation method of lithium ion sieve adsorbant and the method for adsorbing lithium ion Download PDFInfo
- Publication number
- CN107138126A CN107138126A CN201710585163.4A CN201710585163A CN107138126A CN 107138126 A CN107138126 A CN 107138126A CN 201710585163 A CN201710585163 A CN 201710585163A CN 107138126 A CN107138126 A CN 107138126A
- Authority
- CN
- China
- Prior art keywords
- lithium
- lithium ion
- ion sieve
- aluminum
- mother liquor
- 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.)
- Pending
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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Geochemistry & Mineralogy (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of lithium ion sieve adsorbant, comprise the steps of：Step 1, weigh containing manganese compound and lithium-containing compound mass ratio 6:1~14:1, it is well mixed in crucible, is placed in Muffle furnace 60~300min of roasting at 400~1000 DEG C, be down to room temperature, grinding obtains lithium type ion sieve；Step 2, with salt acid soak lithium type 6~18h of ion sieve that concentration is 0.5~3.0mol/L, it is placed on 12~30h of magnetic stirring apparatus Stirring, temperature control is at 45 50 DEG C during stirring, and mixing speed 500r/min is centrifuged, drying obtains form ion sieve, i.e. lithium ion sieve adsorbant.Preparation technology of the present invention is simple, and production cost is low, environmentally friendly；100% of lithium concentration in aluminum-extracted pulverized fuel ash circulating mother liquor can be reached using the amount of the lithium ion sieve adsorbant adsorbing and extracting lithium ion of the present invention, the adsorption rate to lithium is high.
Description
Technical field
The invention belongs to electrodeless metalloform-selective separation technology field, a kind of lithium ion sieve absorption is more particularly related to
The preparation method of agent and the method for adsorbing lithium ion.
Background technology
As economic continues to develop, the demand of lithium and its compound is also increasing, regardless of the daily life from people
The numerous areas such as work, aviation, medicine, chemical industry, high-energy battery and thermonuclear reaction, lithium and lithium salts are all widely used, and lithium has
High strategic value, the demand of current China's lithium has been far longer than 500t/a, and with more than 25% speed year by year
Increase, the storage level of lithium resource does not reach the demand in market much for a long time.To alleviate the lithium resource nervous office that supply falls short of demand
Face, extracts lithium also increasingly in coal in focus of the discovery of association lithium ore deposit for the moment as research, coal-fired product flyash in recent years
Attract attention.
Research finds in Zhungeer coal field and Shanxi riding comfort model coal the content super richening of association lithium and has reached association
The production-grade of lithium ore deposit；Meanwhile, to the product after riding comfort model coal combustion --- coal ash has carried out the measure of lithium content, finds coal
Lithium in ash has also reached associated minerals comprehensive reutilization production-grade；In addition, laboratory is also sent out by experimental study
The content of aluminum oxide is up to 47% in this existing coal ash, is high alumina coal ash, according to technique needs, and the recovery of lithium is after aluminium extraction
Carry out.To sum up, reclaiming lithium in flyash extraction aluminium circulating mother liquor from Zhungeer coal field and Shanxi riding comfort model will possess extensively
Wealthy development prospect, can not only alleviate the insufficient situation of lithium resource, can also be passed through for the circulation in coal resources field
The development of Ji and economies in transition provides new pattern, while the extraction research of lithium resource will provide important for following nuclear power station
Standby raw material.At present, not yet there is the relevant report that lithium is reclaimed from aluminum-extracted pulverized fuel ash circulating mother liquor.
The content of the invention
Circulated it is an object of the invention to provide a kind of preparation method of lithium ion sieve adsorbant and from aluminum-extracted pulverized fuel ash female
The method that lithium ion is adsorbed in liquid, the adsorption rate to lithium is high.
The present invention is achieved in that a kind of preparation method of lithium ion sieve adsorbant, and the method includes the steps of：
Step 1, weigh containing manganese compound and lithium-containing compound mass ratio 6:1~14:1, it is well mixed, is placed in crucible
60~300min is calcined in Muffle furnace at 400~1000 DEG C, room temperature is down to, grinding obtains lithium type ion sieve；
Step 2, with salt acid soak lithium type 6~18h of ion sieve that concentration is 0.5~3.0mol/L, it is placed on magnetic stirring apparatus
12~30h of Stirring, temperature control is at 45-50 DEG C during stirring, and mixing speed 500r/min is centrifuged, and drying obtains hydrogen
Type ion sieve, i.e. lithium ion sieve adsorbant.
Preferably, in step 1, the mass ratio containing manganese compound and lithium-containing compound weighed is 10:1, it is mixed in crucible
Close uniform, be placed in Muffle furnace and be calcined 120min at 900 DEG C, be down to room temperature, grinding obtains lithium type ion sieve；In step 2, use
1.5mol/L salt acid soak lithium type ion sieve 12h, be placed on magnetic stirrer 12h centrifugation, drying obtain Hydrogen from
Son sieve.
Described in step 1 is manganese dioxide containing manganese compound, and lithium-containing compound is lithium hydroxide.
The chemical formula of lithium type ion sieve described in step 1 is LiMn2O4。
Present invention also offers a kind of method that lithium ion is adsorbed in circulating mother liquor from aluminum-extracted pulverized fuel ash, the above-mentioned system of exploitation right
The lithium ion sieve adsorbant that Preparation Method is prepared adsorbs lithium ion from aluminum-extracted pulverized fuel ash circulating mother liquor.
Preferably, the method that lithium ion is adsorbed in a kind of above-mentioned circulating mother liquor from aluminum-extracted pulverized fuel ash, comprises the following steps：
Step 1, the appropriate lithium ion sieve adsorbant obtained by preparation added in aluminum-extracted pulverized fuel ash circulating mother liquor, during absorption
Between be 10~80min, centrifuge, the solid after being separated；
Step 2, the solid being centrifugally separating to obtain in step 1 eluted with 0.5~3.0mol/L hydrochloric acid, elution time is
20~60min, centrifuges, takes supernatant, produces the solution of enrichment lithium ion.
Preferably, in step 1, the ratio of the lithium ion sieve adsorbant of addition and aluminum-extracted pulverized fuel ash circulating mother liquor is 1：
1.6g/L。
Preferably, adsorption time is 30~60min, it is highly preferred that adsorption time is 40min.
Preferably, the solid being centrifugally separating to obtain is eluted with 1.0mol/L hydrochloric acid, elution time is 30min.
Beneficial effects of the present invention are as follows：
Lithium ion sieve adsorbant preparation technology prepared by the present invention is simple, and production cost is low, environmentally friendly；Use this hair
The amount of bright lithium ion sieve adsorbant adsorbing and extracting lithium ion can reach lithium concentration in aluminum-extracted pulverized fuel ash circulating mother liquor
100%, the adsorption rate to lithium is high；The method that lithium ion is adsorbed from aluminum-extracted pulverized fuel ash circulating mother liquor that the present invention is provided, operation
It is easy, it is easy to which that the implementation to lithium ion adsorbing and extracting, cost is low, and environmental pollution is small.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
The lithium type ion sieve SEM figures that Fig. 1 is prepared for the present invention.
The lithium type ion sieve X-ray diffractogram that Fig. 2 is prepared for the present invention.
The lithium type ion sieve schematic diagram that Fig. 3 is prepared for the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
A kind of preparation method of lithium ion sieve adsorbant provided in an embodiment of the present invention, prepared adsorbent is with dioxy
Change manganese is raw material, is sufficiently mixed with lithium hydroxide, and roasting at high temperature is prepared, and the method includes the steps of：
Step 1, weigh containing manganese compound and lithium-containing compound mass ratio 6:1~14:1, it is well mixed, is placed in crucible
60~300min is calcined in Muffle furnace at 400~1000 DEG C, room temperature is down to, grinding obtains lithium type ion sieve；
Step 2, with salt acid soak lithium type 6~18h of ion sieve that concentration is 0.5~3.0mol/L, it is placed on magnetic stirring apparatus
12~30h of Stirring, temperature control is at 45-50 DEG C during stirring, and mixing speed 500r/min is centrifuged, and drying obtains hydrogen
Type ion sieve, i.e. lithium ion sieve adsorbant.It is with the process main purpose of salt acid soak and stirring, allows Li+Room by H+
Instead of the skeleton of compound does not change so as to form the compound with certain rule after de- lithium, this to carry H+Change
Compound has imports the function that target lithium ion remembers identification to former, so in the case where different kinds of ions is co-existed in, with pair
Initially import the screening capacity of target lithium ion.
As a preferred scheme of the embodiment of the present invention, in step 1, weigh containing manganese compound and lithium-containing compound
Mass ratio is 10:1, it is well mixed in crucible, it is placed in Muffle furnace and is calcined 120min at 900 DEG C, be down to room temperature, grinding obtains lithium
Type ion sieve；In step 2, with 1.5mol/L salt acid soak lithium type ion sieve 12h, be placed on magnetic stirrer 12h from
The heart is separated, and drying obtains form ion sieve.
As a preferred scheme of the embodiment of the present invention, described in step 1 is manganese dioxide containing manganese compound, is closed containing lithiumation
Thing is lithium hydroxide.
In embodiments of the present invention, the chemical formula of the lithium type ion sieve described in step 1 is LiMn2O4。
Electronic microscope photos is carried out to above-mentioned prepared lithium type ion sieve, sample granularity has agglomeration, particle than more uniform
It is presented irregular polyhedron-shaped.
The embodiment of the present invention adsorbs the method for lithium ion, exploitation right in additionally providing a kind of circulating mother liquor from aluminum-extracted pulverized fuel ash
The lithium ion sieve adsorbant that above-mentioned preparation method is prepared adsorbs lithium ion from aluminum-extracted pulverized fuel ash circulating mother liquor.
In embodiments of the present invention, the method that lithium ion is adsorbed in a kind of above-mentioned circulating mother liquor from aluminum-extracted pulverized fuel ash, bag
Include following steps：
Step 1, the appropriate lithium ion sieve adsorbant obtained by preparation added in aluminum-extracted pulverized fuel ash circulating mother liquor, during absorption
Between be 10~80min, centrifuge, the solid after being separated；The procedure parameter is very easy to control, takes supernatant atom
Absorption spectrometer is determined, and the adsorption rate to lithium is very high.
Step 2, the solid being centrifugally separating to obtain in step 1 eluted with 0.5~3.0mol/L hydrochloric acid, elution time is
20~60min, centrifuges, takes supernatant, produces the solution of enrichment lithium ion.Supernatant is taken to be surveyed with Atomic Absorption Spectrometer
It is fixed, it is very high to the eluting rate of lithium.
It is used as a preferred scheme of the embodiment of the present invention, in step 1, the lithium ion sieve adsorbant and coal ash lifting of addition
The ratio of aluminium circulating mother liquor is 1：1.6g/L.
As a preferred scheme of the embodiment of the present invention, adsorption time is 30~60min, it is highly preferred that adsorption time is
40min。
As a preferred scheme of the embodiment of the present invention, by the solid being centrifugally separating to obtain 1.0mol/L salt pickling
De-, elution time is 30min.
In embodiments of the present invention, aluminum-extracted pulverized fuel ash circulating mother liquor used as follows gained：
(1) desiliconization ash is screened to 200 mesh with disintegrating machine attrition grinding, by quality proportioning 1.0:0.8:1.0 ratio claims
Take coal ash, Na2CO3And CaCO3Mixing, stirs and is placed in porcelain crucible, is placed on 1200 DEG C of roasting 1.5h of Muffle furnace, drops naturally
Temperature to 750 DEG C of constant temperature keep 20min, and cooling is taken out.Its reaction is：
Li2OAl2O3.4SiO2+ 8CaO=Li2O.Al2O3+4[2CaO.SiO2]
By roasting, the lithium in not tractable flyash is set to be converted into tractable lithium.
(2) by the Na of the ash concentration 5% of roasting2CO3Solution grinds to form pasty state, imports 150 DEG C of heating 1h in autoclave.
Its reaction is：
Li2O·Al2O3·4SiO2+nH2O+Na2CO3=Na2O·Al2O3·4SiO2·nH2O+Li2CO3
Sodium carbonate is with tractable lithium in the case of the presence of higher temperature, pressure and liquid phase water, and sodium and lithium displacement reaction make
Lithium is existed in solution in the form of lithium carbonate, and resulting solution is filtered, and it is powder that the liquid after filtering, which carries the solution obtained after aluminium,
Coal ash carries aluminium circulating mother liquor.Flyash used comes from Shanxi riding comfort model.
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
Prepare lithium ion sieve adsorbant：Weigh containing manganese compound and lithium-containing compound mass ratio 6:1, mix equal in crucible
It is even, it is placed in Muffle furnace and is calcined 180min at 400 DEG C, be down to room temperature, grinding obtains lithium type ion sieve, and (its chemical formula is
LiMn2O4), the salt acid soak lithium type ion sieve 18h for being 1.0mol/L with concentration is placed on magnetic stirrer 18h, during stirring
Temperature control is at 45-50 DEG C, mixing speed 500r/min, centrifuges, drying obtain form ion sieve, the i.e. lithium of the present invention from
Sub- sieve adsorbant.
Weigh the form ion sieve 0.1g prepared by the present embodiment, plus 160ml aluminum-extracted pulverized fuel ash circulating mother liquors, adsorption time
For 10min, centrifuge, isolated solid is eluted with 0.5mol/L hydrochloric acid, and elution time is 20min, is centrifuged,
Concentration before and after atomic absorption spectrometry absorption in aluminum-extracted pulverized fuel ash circulating mother liquor, determines the suction for the adsorbent that is applied
Attached concentration can reach more than 90% of concentration in former aluminum-extracted pulverized fuel ash circulating mother liquor.
Embodiment 2
Prepare lithium ion sieve adsorbant：Weigh and compare 8 containing manganese compound and the compound quality containing lithium:1, mixed in crucible
Uniformly, it is placed in Muffle furnace and is calcined 60min at 800 DEG C, be down to room temperature, grinding obtains lithium type ion sieve, is 0.5mol/ with concentration
L salt acid soak lithium type ion sieve 18h, is placed on magnetic stirrer 24h, and temperature control is at 45-50 DEG C during stirring, stirring speed
500r/min is spent, is centrifuged, drying obtains form ion sieve, i.e. lithium ion sieve adsorbant of the invention.
Weigh the form ion sieve 0.1g prepared by the present embodiment, plus 160ml aluminum-extracted pulverized fuel ash circulating mother liquors, adsorption time
For 40min, centrifuge, isolated solid is eluted with 1.5mol/L hydrochloric acid, and elution time is 40min, is centrifuged,
Concentration before and after atomic absorption spectrometry absorption in aluminum-extracted pulverized fuel ash circulating mother liquor, determines the suction for the adsorbent that is applied
Attached concentration can reach more than 90% of concentration in former aluminum-extracted pulverized fuel ash circulating mother liquor.
Embodiment 3
Prepare lithium ion sieve adsorbant：Weigh and compare 10 containing manganese compound and the compound quality containing lithium:1, mixed in crucible
Close uniform, be placed in Muffle furnace and be calcined 120min at 900 DEG C, be down to room temperature, grinding obtains lithium type ion sieve, is with concentration
1.5mol/L salt acid soak lithium type ion sieve 12h, is placed on magnetic stirrer 12h, temperature control is in 45-50 during stirring
DEG C, mixing speed 500r/min is centrifuged, and drying obtains form ion sieve, i.e. lithium ion sieve adsorbant of the invention.
Weigh the form ion sieve 0.1g prepared by the present embodiment, plus 160ml aluminum-extracted pulverized fuel ash circulating mother liquors, adsorption time
For 40min, centrifuge, isolated solid is eluted with 1.0mol/L hydrochloric acid, and elution time is 30min, is centrifuged,
Concentration before and after atomic absorption spectrometry absorption in aluminum-extracted pulverized fuel ash circulating mother liquor, determines the suction for the adsorbent that is applied
Attached concentration can reach 100% of concentration in former aluminum-extracted pulverized fuel ash circulating mother liquor.
Lithium type ion sieve obtained by being prepared to the present embodiment 3, carries out electronic microscope photos, and sample granularity has reunion than more uniform
Phenomenon, particle is presented irregular polyhedron-shaped, as a result sees Fig. 1, its chemical formula is LiMn with X-ray diffraction measure2O4, knot
Fruit sees Fig. 2, and the absorption principle of prepared lithium type ion sieve is shown in Fig. 3.
Embodiment 4
Prepare lithium ion sieve adsorbant：Weigh and compare 12 containing manganese compound and the compound quality containing lithium:1, mixed in crucible
Close uniform, be placed in Muffle furnace and be calcined 60min at 600 DEG C, be down to room temperature, grinding obtains lithium type ion sieve, is with concentration
1.5mol/L salt acid soak lithium type ion sieve 12h, is placed on magnetic stirrer 30h, temperature control is in 45-50 during stirring
DEG C, mixing speed 500r/min is centrifuged, and drying obtains form ion sieve, i.e. lithium ion sieve adsorbant of the invention.
Weigh the form ion sieve 0.1g prepared by the present embodiment, plus 160ml aluminum-extracted pulverized fuel ash circulating mother liquors, adsorption time
For 80min, centrifuge, isolated solid is eluted with 2.0mol/L hydrochloric acid, and elution time is 60min, is centrifuged,
Concentration before and after atomic absorption spectrometry absorption in aluminum-extracted pulverized fuel ash circulating mother liquor, determines the suction for the adsorbent that is applied
Attached concentration can reach more than 90% of concentration in former aluminum-extracted pulverized fuel ash circulating mother liquor.
Embodiment 5
Prepare lithium ion sieve adsorbant：Weigh containing manganese compound and lithium-containing compound mass ratio 14:1, mixed in crucible
Uniformly, it is placed in Muffle furnace and is calcined 300min at 1000 DEG C, be down to room temperature, grinding obtains lithium type ion sieve, is with concentration
3.0mol/L salt acid soak lithium type ion sieve 6h, is placed on magnetic stirrer 30h, during stirring temperature control at 45-50 DEG C,
Mixing speed 500r/min, is centrifuged, and drying obtains form ion sieve, i.e. lithium ion sieve adsorbant of the invention.
Weigh the form ion sieve 0.1g prepared by the present embodiment, plus 160ml aluminum-extracted pulverized fuel ash circulating mother liquors, adsorption time
For 80min, centrifuge, isolated solid is eluted with 3.0mol/L hydrochloric acid, and elution time is 60min, is centrifuged,
Concentration before and after atomic absorption spectrometry absorption in aluminum-extracted pulverized fuel ash circulating mother liquor, determines the suction for the adsorbent that is applied
Attached concentration can reach more than 90% of concentration in former aluminum-extracted pulverized fuel ash circulating mother liquor.
, but those skilled in the art once know basic creation although preferred embodiments of the present invention have been described
Property concept, then can make other change and modification to these embodiments.So, appended claims are intended to be construed to include excellent
Select embodiment and fall into having altered and changing for the scope of the invention.
Obviously, those skilled in the art can carry out the essence of various changes and modification without departing from the present invention to the present invention
God and scope.So, if these modifications and variations of the present invention belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising including these changes and modification.
Claims (9)
1. a kind of preparation method of lithium ion sieve adsorbant, it is characterised in that the method includes the steps of：
Step 1, weigh containing manganese compound and lithium-containing compound mass ratio 6:1~14:1, it is well mixed in crucible, is placed on Muffle
60~300min is calcined in stove at 400~1000 DEG C, room temperature is down to, grinding obtains lithium type ion sieve；
Step 2, with salt acid soak lithium type 6~18h of ion sieve that concentration is 0.5~3.0mol/L, it is placed on magnetic stirring apparatus rotation
Stir 12~30h, temperature control is at 45-50 DEG C during stirring, mixing speed 500r/min, centrifuge, drying obtain Hydrogen from
Son sieve, i.e. lithium ion sieve adsorbant.
2. a kind of preparation method of lithium ion sieve adsorbant as claimed in claim 1, it is characterised in that in step 1, weigh
The mass ratio containing manganese compound and lithium-containing compound be 10:1, it is well mixed in crucible, it is placed in Muffle furnace at 900 DEG C and is calcined
120min, is down to room temperature, and grinding obtains lithium type ion sieve；In step 2, with 1.5mol/L salt acid soak lithium type ion sieve
12h, is placed on magnetic stirrer 12h centrifugations, and drying obtains form ion sieve.
3. a kind of preparation method of lithium ion sieve adsorbant as claimed in claim 1, it is characterised in that containing described in step 1
Manganese compound is manganese dioxide, and lithium-containing compound is lithium hydroxide.
4. a kind of preparation method of lithium ion sieve adsorbant as claimed in claim 1, it is characterised in that the lithium described in step 1
The chemical formula of type ion sieve is LiMn2O4。
5. the method for lithium ion is adsorbed in a kind of circulating mother liquor from aluminum-extracted pulverized fuel ash, it is characterised in that appoint using claim 1-4
The lithium ion sieve adsorbant that one preparation method is prepared adsorbs lithium ion from aluminum-extracted pulverized fuel ash circulating mother liquor.
6. the method for lithium ion is adsorbed in a kind of circulating mother liquor from aluminum-extracted pulverized fuel ash as claimed in claim 5, it is characterised in that
Comprise the following steps：
Step 1, the appropriate lithium ion sieve adsorbant obtained by preparation added in aluminum-extracted pulverized fuel ash circulating mother liquor, adsorption time is
10~80min, is centrifuged, the solid after being separated；
Step 2, the solid being centrifugally separating to obtain in step 1 being eluted with 0.5~3.0mol/L hydrochloric acid, elution time is 20~
60min, centrifuges, takes supernatant, produces the solution of enrichment lithium ion.
7. the method for lithium ion is adsorbed in a kind of circulating mother liquor from aluminum-extracted pulverized fuel ash as claimed in claim 6, it is characterised in that
In step 1, the ratio of the lithium ion sieve adsorbant of addition and aluminum-extracted pulverized fuel ash circulating mother liquor is 1：1.6g/L.
8. the method for lithium ion is adsorbed in a kind of circulating mother liquor from aluminum-extracted pulverized fuel ash as claimed in claim 6, it is characterised in that
Adsorption time is 30~60min, it is highly preferred that adsorption time is 40min.
9. the method for lithium ion is adsorbed in a kind of circulating mother liquor from aluminum-extracted pulverized fuel ash as claimed in claim 6, it is characterised in that
The solid being centrifugally separating to obtain is eluted with 1.0mol/L hydrochloric acid, elution time is 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710585163.4A CN107138126A (en) | 2017-07-18 | 2017-07-18 | A kind of preparation method of lithium ion sieve adsorbant and the method for adsorbing lithium ion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710585163.4A CN107138126A (en) | 2017-07-18 | 2017-07-18 | A kind of preparation method of lithium ion sieve adsorbant and the method for adsorbing lithium ion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107138126A true CN107138126A (en) | 2017-09-08 |
Family
ID=59776041
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710585163.4A Pending CN107138126A (en) | 2017-07-18 | 2017-07-18 | A kind of preparation method of lithium ion sieve adsorbant and the method for adsorbing lithium ion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107138126A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439476A (en) * | 2018-04-23 | 2018-08-24 | 陕西省膜分离技术研究院有限公司 | A kind of preparation of low price Mn oxide, product and synthesizing lithium ion sieve presoma Li1.6Mn1.6O4Application |
| CN108461859A (en) * | 2018-06-11 | 2018-08-28 | 四会市恒星智能科技有限公司 | A method of from extraction lithium in waste liquid containing lithium |
| CN108682916A (en) * | 2018-06-11 | 2018-10-19 | 四会市恒星智能科技有限公司 | The recovery method of lithium in a kind of anode material for lithium-ion batteries |
| CN108745276A (en) * | 2018-04-18 | 2018-11-06 | 南京工业大学 | Preparation method of mixed forming lithium ion adsorbent |
| CN109761250A (en) * | 2019-04-11 | 2019-05-17 | 天齐锂业资源循环技术研发(江苏)有限公司 | A method of lithium ion sieve is prepared using waste and old lithium ion battery |
| CN110342554A (en) * | 2018-04-03 | 2019-10-18 | 国家能源投资集团有限责任公司 | The method of flyash extraction aluminum and coproducing lithium carbonate |
| CN110479228A (en) * | 2019-08-16 | 2019-11-22 | 黄冈师范学院 | A kind of regeneration method of the ion-sieve type manganese systems adsorbent of failure |
| CN110773112A (en) * | 2019-09-25 | 2020-02-11 | 中国科学院青海盐湖研究所 | Modified manganese-based lithium ion sieve and preparation method thereof |
| CN112717468A (en) * | 2020-12-09 | 2021-04-30 | 西安蓝晓科技新材料股份有限公司 | Method for recovering lithium in lithium precipitation mother liquor |
| CN116265080A (en) * | 2021-12-16 | 2023-06-20 | 中国科学院宁波材料技术与工程研究所 | Phosphate type lithium ion sieve and desorption method thereof |
| CN117358196A (en) * | 2023-09-20 | 2024-01-09 | 中国地质科学院矿产资源研究所 | Preparation method of bauxite-based aluminum lithium ion adsorbent and brine lithium extraction method |
| WO2024130975A1 (en) * | 2022-12-23 | 2024-06-27 | 重庆鑫景特种玻璃有限公司 | Ion sieve with high-temperature resistance and high stability, and preparation method therefor and use thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803273A (en) * | 2005-12-15 | 2006-07-19 | 北京矿冶研究总院 | Preparation method of lithium adsorbent |
| CN101157480A (en) * | 2007-09-18 | 2008-04-09 | 华东理工大学 | Manganese bioxide ionic sieve |
| CN101928042A (en) * | 2010-09-16 | 2010-12-29 | 中南大学 | Spinel-type lithium-ion sieve and method for preparing precursor LiMn2O4 thereof |
| CN103121724A (en) * | 2012-12-24 | 2013-05-29 | 华东理工大学 | Method for preparing lithium ion sieve MnO2.0.5H2O and precursor thereof Li1.6Mn1.6O4 |
| CN105692659A (en) * | 2016-01-26 | 2016-06-22 | 中国科学院过程工程研究所 | Method for extracting lithium from fly ash |
| CN106622116A (en) * | 2016-09-16 | 2017-05-10 | 北京工业大学 | Preparation method of spinel type lithium ion sieve |
-
2017
- 2017-07-18 CN CN201710585163.4A patent/CN107138126A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803273A (en) * | 2005-12-15 | 2006-07-19 | 北京矿冶研究总院 | Preparation method of lithium adsorbent |
| CN101157480A (en) * | 2007-09-18 | 2008-04-09 | 华东理工大学 | Manganese bioxide ionic sieve |
| CN101928042A (en) * | 2010-09-16 | 2010-12-29 | 中南大学 | Spinel-type lithium-ion sieve and method for preparing precursor LiMn2O4 thereof |
| CN103121724A (en) * | 2012-12-24 | 2013-05-29 | 华东理工大学 | Method for preparing lithium ion sieve MnO2.0.5H2O and precursor thereof Li1.6Mn1.6O4 |
| CN105692659A (en) * | 2016-01-26 | 2016-06-22 | 中国科学院过程工程研究所 | Method for extracting lithium from fly ash |
| CN106622116A (en) * | 2016-09-16 | 2017-05-10 | 北京工业大学 | Preparation method of spinel type lithium ion sieve |
Non-Patent Citations (1)
| Title |
|---|
| 侯永茹等: "用吸附法从粉煤灰碱性溶液里提取锂", 《粉煤灰综合利用》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110342554A (en) * | 2018-04-03 | 2019-10-18 | 国家能源投资集团有限责任公司 | The method of flyash extraction aluminum and coproducing lithium carbonate |
| CN108745276A (en) * | 2018-04-18 | 2018-11-06 | 南京工业大学 | Preparation method of mixed forming lithium ion adsorbent |
| CN108439476B (en) * | 2018-04-23 | 2020-07-28 | 陕西省膜分离技术研究院有限公司 | Preparation of low-valence manganese oxide, product and synthetic lithium ion sieve precursor L i1.6Mn1.6O4Application of |
| CN108439476A (en) * | 2018-04-23 | 2018-08-24 | 陕西省膜分离技术研究院有限公司 | A kind of preparation of low price Mn oxide, product and synthesizing lithium ion sieve presoma Li1.6Mn1.6O4Application |
| CN108461859A (en) * | 2018-06-11 | 2018-08-28 | 四会市恒星智能科技有限公司 | A method of from extraction lithium in waste liquid containing lithium |
| CN108682916A (en) * | 2018-06-11 | 2018-10-19 | 四会市恒星智能科技有限公司 | The recovery method of lithium in a kind of anode material for lithium-ion batteries |
| CN109761250A (en) * | 2019-04-11 | 2019-05-17 | 天齐锂业资源循环技术研发(江苏)有限公司 | A method of lithium ion sieve is prepared using waste and old lithium ion battery |
| CN110479228A (en) * | 2019-08-16 | 2019-11-22 | 黄冈师范学院 | A kind of regeneration method of the ion-sieve type manganese systems adsorbent of failure |
| CN110773112A (en) * | 2019-09-25 | 2020-02-11 | 中国科学院青海盐湖研究所 | Modified manganese-based lithium ion sieve and preparation method thereof |
| CN112717468A (en) * | 2020-12-09 | 2021-04-30 | 西安蓝晓科技新材料股份有限公司 | Method for recovering lithium in lithium precipitation mother liquor |
| CN116265080A (en) * | 2021-12-16 | 2023-06-20 | 中国科学院宁波材料技术与工程研究所 | Phosphate type lithium ion sieve and desorption method thereof |
| WO2024130975A1 (en) * | 2022-12-23 | 2024-06-27 | 重庆鑫景特种玻璃有限公司 | Ion sieve with high-temperature resistance and high stability, and preparation method therefor and use thereof |
| CN117358196A (en) * | 2023-09-20 | 2024-01-09 | 中国地质科学院矿产资源研究所 | Preparation method of bauxite-based aluminum lithium ion adsorbent and brine lithium extraction method |
| CN117358196B (en) * | 2023-09-20 | 2024-03-15 | 中国地质科学院矿产资源研究所 | Preparation method of bauxite-based aluminum lithium ion adsorbent and brine lithium extraction method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107138126A (en) | A kind of preparation method of lithium ion sieve adsorbant and the method for adsorbing lithium ion | |
| Yue et al. | Recovering valuable metals from spent lithium ion battery via a combination of reduction thermal treatment and facile acid leaching | |
| CN104525094B (en) | The preparation method of a kind of manganese system ion(ic)sieve sorbent material and presoma thereof | |
| CN101944600A (en) | Lithium-titanium oxide type lithium ion sieve absorbent and method for preparing precursor thereof | |
| CN103882234B (en) | A kind of method neodymium iron boron greasy filth being prepared into regeneration NdFeB magnetic powder | |
| CN110639467A (en) | Preparation method of magnetic aluminum salt lithium adsorbent | |
| WO2011003266A1 (en) | A preparation method for battery level lithium carbonate using lithium chloride solution | |
| WO2023226546A1 (en) | Method for recycling lithium from lithium clay | |
| CN106587116A (en) | Method for extracting lithium carbonate and aluminum hydroxide through lepidolite and fly ash | |
| CN101383442A (en) | Method for recovering and preparing lithium cobaltate from waste lithium ionic cell | |
| CN101928042A (en) | Spinel-type lithium-ion sieve and method for preparing precursor LiMn2O4 thereof | |
| CN109244588B (en) | Method for producing ternary precursor and high-purity lithium carbonate by using waste ternary lithium battery | |
| CN106636614B (en) | A method of leaching niobium, scandium and rare earth element from tailing | |
| CN103232065B (en) | Method for recycling before-kiln dehydration filtrate and method for producing titanium dioxide | |
| CN107857283B (en) | A method of isolation technics is consolidated based on selectivity and prepares battery-level lithium carbonate | |
| CN108584994A (en) | A kind of method of lepidolite calcined by rotary kiln lithium carbonate | |
| CN110510642A (en) | A kind of method that low-grade α spodumene economy mentions lithium | |
| CN103435080A (en) | Method for extracting and de-ironing aluminum chloride slurry | |
| CN103199319B (en) | Method for recycling lithium cobalt oxide from waste positive electrode of lithium cobalt oxide battery | |
| CN106319227A (en) | Comprehensive utilization method for acid leaching slag of neodymium iron boron waste | |
| CN104466293B (en) | The renovation process of lithium ion cell anode material lithium cobaltate waste material | |
| CN113548701A (en) | Preparation and application method of lithium ion sieve | |
| CN114804220B (en) | Porous spherical cobalt oxide particles and preparation method thereof | |
| Chen et al. | Hydrometallurgical processes for valuable metals recycling from spent lithium-ion batteries | |
| CN104485494B (en) | The renovation process of positive electrode active materials in cobalt acid lithium used Li ion cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170908 |
|
| RJ01 | Rejection of invention patent application after publication |