CN105771879A - Lithium adsorbent and preparation method and application thereof - Google Patents
Lithium adsorbent and preparation method and application thereof Download PDFInfo
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- CN105771879A CN105771879A CN201610129931.0A CN201610129931A CN105771879A CN 105771879 A CN105771879 A CN 105771879A CN 201610129931 A CN201610129931 A CN 201610129931A CN 105771879 A CN105771879 A CN 105771879A
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- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- 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
Abstract
The invention relates to lithium adsorbent and further relates to a preparation method of the lithium adsorbent.The preparation method sequentially includes the steps of selecting spodumene concentrate as the raw material, refining and purifying the spodumene concentrate, lithium removing, refining again and activating.The invention further relates to application of the lithium adsorbent to extraction of lithium from brine containing magnesium and lithium.The prepared lithium adsorbent has the advantages of being high in adsorption selectivity to lithium, high in lithium adsorption capacity and high in concentration of lithium removed out of a lithium solution.
Description
Technical field
The present invention relates to a kind of lithium adsorbent.
The invention still further relates to the preparation method of a kind of lithium adsorbent and in the application extracting lithium from the salt containing magnesium lithium.
Background technology
Along with socioeconomic development, the demand of lithium is increasing, the main source of lithium is derived from the salt in salt lake, China is the country that a lithium resource is abundant, but it is high that the feature of the saline lake lithium resource of China is the Mg/Li ratio containing lithium salt, lithium being separated technical difficulty from high Mg/Li ratio salt relatively larger, adopting lithium adsorbent separating Li from high Mg/Li ratio salt is considered as the most promising put forward lithium way.
The lithium adsorbent being used for adsorbing separation lithium at present is mainly two classes: aluminum system lithium adsorbent and manganese systems lithium adsorbent, this two classes adsorbent all exists very big deficiency.Aluminum system lithium adsorbent is very low to the adsorption capacity of lithium, and the lithium solution lithium concentration deviate from is only about 0.6g/L;Though manganese systems lithium adsorbent is relatively little higher to the adsorption capacity of lithium, but its lithium solution deviate from also can less than 2g/L containing lithium concentration.The lithium solution lithium concentration that this two classes lithium adsorbent is deviate from is all very low, and the follow-up concentration to lithium solution is brought significantly high cost.
Accordingly, it is desirable to provide a kind of new technical scheme solves the problems referred to above.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of can in the salt containing magnesium lithium the lithium adsorbent of adsorbing and extracting lithium.
The present invention also to solve the technical problem that the preparation method being to provide a kind of lithium adsorption capacity is big, deviate from lithium solution containing the high lithium adsorbent of lithium concentration.
The present invention also provides for a kind of lithium adsorbent in the application extracting lithium from the salt containing magnesium lithium.
For solving above-mentioned technical problem, the invention provides a kind of lithium adsorbent, this lithium adsorbent is prepared by following method: be transformed into after β-spodumene by the spodumene concentrate that lithium oxide weight/mass percentage composition is 4%-7.5% through high-temperature calcination, ball milling sieves, the purification refine material being collected by sieve mixes with concentrated sulphuric acid, it is warmed up to 200-300 DEG C after mix homogeneously and carries out heat preservation hot process 20-60 minute, it is subsequently cooled to not higher than 100 DEG C, again this sulfuric acid-treated good refining material is added to the water furnishing serosity sieving, then serosity it is filtered and washs, obtain filter cake and filtrate;The filter cake obtained joins after carrying out immersion activation in the subacidity water that pH is 4-5 1-10 hour, carries out filter cake after solid-liquid separation is activated, and filter cake is dried at 100-200 DEG C of temperature and just obtained lithium adsorbent product.
The preparation method that the invention provides a kind of lithium adsorbent, comprises the following steps:
(1) selecting spodumene concentrate is raw material stage: the spodumene concentrate selecting lithium oxide weight/mass percentage composition to be 4%-7.5% is the raw material preparing lithium adsorbent;
(2) to spodumene concentrate polishing purification step: the spodumene concentrate that lithium oxide weight/mass percentage composition is 4%-7.5% is transformed into after β-spodumene through high-temperature calcination, ball milling crosses 60 mesh sieves, remove the residue on sieve being mainly quartz, be collected by the purification refine material of 60 mesh sieves;
(3) de-lithium again purification step: the concentrated sulphuric acid of the purification refine material and mass concentration 98% that have passed through 60 mesh sieves that step (2) is collected mixes, the addition mole of concentrated sulphuric acid is in refining material 1~1.5 times of lithium oxide mole, it is warmed up to 200-300 DEG C after mix homogeneously and carries out heat preservation hot process 20-60 minute, it is subsequently cooled to not higher than 100 DEG C, be added to the water this sulfuric acid-treated good refining material furnishing serosity mistake 80 mesh sieves again, again remove residue on sieve, then the serosity having passed through 80 mesh sieves it is filtered and washs, obtain filter cake and filtrate, filtrate is that lithium sulfate solution can be used for preparing Lithium hydrate or lithium carbonate;
(4) activation step: the filter cake that step (3) is obtained joins after carrying out immersion activation in the subacidity water that pH is 4-5 1-10 hour, carries out filter cake after solid-liquid separation is activated, and filter cake is dried at 100-200 DEG C of temperature and just obtained lithium adsorbent product.
In step (4), pH is any in the mixed solution that subacidity water is dilute hydrochloric acid solution, dilution heat of sulfuric acid, dilute hydrochloric acid and sulphuric acid three kinds of 4-5.
The invention provides a kind of lithium adsorbent in the application extracting lithium from the salt containing magnesium lithium.
The present invention adopts spodumene concentrate to be raw material, calcining carries out ball milling after being converted into β type spodumene, because quartz is not easy to grind, so major part quartz can be got rid of by the mode sieved after ball milling, so that raw material obtains certain purification, process with sulphuric acid afterwards, it is slurred out de-lithium with water again with after sulfuric acid treatment, and the residue on sieves such as removal quartz that serosity sieved again, the serosity having passed through sieve carries out solid-liquid separation, filter cake is used weak acid activation processing, thus obtaining highly active lithium adsorbent, this lithium adsorbent not only lithium adsorption capacity is high, and the lithium solution lithium concentration deviate from may be up to about 25g/L.
Beneficial effects of the present invention: lithium adsorbent prepared by the present invention, for adsorbing and extracting lithium from the salt containing magnesium lithium, absorption lithium capacity is big, and the lithium solution lithium concentration deviate from is high.Prepare the low in raw material price that adsorbent adopts, and the lithium taken off in the step prepare adsorbent can be used for producing lithium carbonate, so that the adsorbent cost of preparation is non-normally low, be with a wide range of applications.
Detailed description of the invention
In order to deepen the understanding of the present invention, below the invention will be further described, this embodiment is only used for explaining the present invention, is not intended that the restriction to protection scope of the present invention.
Embodiment 1
nullTake and carry out ball milling after the spodumene concentrate high-temperature calcination that 1300 grams of lithium oxide content is 6% is transformed into β-spodumene concentrate and cross 60 mesh sieves,The refining material being collected by sieve is 1140 grams,The lithium oxide content recording this refining material is 6.8%,Take 1100 grams of these refining material concentrated sulphuric acids with 274 gram 98% to mix to add and be uniformly placed at 230 DEG C of temperature isothermal holding 40 minutes,It is subsequently cooled to 100 DEG C,Again this is joined in 2000mL water through the refining material that dense sulfuric acid treatment is good and be slurred,Serosity is crossed 80 mesh sieves,The serosity having passed through 80 mesh sieves is filtered washing and obtains filter cake,This filter cake is soaked activation 3 hours in joining the dilute sulfuric acid aqueous solution that pH value is 4,Carry out solid-liquid separation afterwards,Isolated filter cake obtains Novel lithium adsorbent product 1050 grams after drying at 200 DEG C of temperature.
Take this lithium adsorbent 1000 grams to join 8000mL content of magnesium to be 120g/L, lithium content be the high Mg/Li ratio aqueous salt brine of 4g/L is stirred under state absorption lithium, when absorption reach 2 little time after stop stirring carrying out solid-liquid separation, recording content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content is 0.1g/L, and isolated adsorbent filter cake sulphuric acid is deviate from lithium, obtaining the lithium solution 1200mL deviate from, the lithium concentration recording this lithium solution is 26g/L.
Above-mentioned deviate from lithium after adsorbent again put into 8000mL content of magnesium to be 120g/L, lithium content be the high Mg/Li ratio aqueous salt brine of 4g/L is stirred under state absorption lithium, when absorption reach 2 little time after stop stirring carrying out solid-liquid separation, recording content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content is 0.1g/L, and isolated adsorbent filter cake sulphuric acid is deviate from lithium, obtaining the lithium solution 1200mL deviate from, the lithium concentration recording this lithium solution is 26.1g/L.
Embodiment 2
nullTake and carry out ball milling after the spodumene concentrate high-temperature calcination that 1200 grams of lithium oxide content is 7.5% is transformed into β-spodumene concentrate and cross 60 mesh sieves,The refining material being collected by sieve is 1185 grams,The lithium oxide content recording this refining material is 7.5%,Take 1100 grams of these refining material concentrated sulphuric acids with 362.2 gram 98% to mix to add and be uniformly placed at 200 DEG C of temperature isothermal holding 20 minutes,It is subsequently cooled to 80 DEG C,Again this is joined in 2000mL water through the refining material that dense sulfuric acid treatment is good and be slurred,Serosity is crossed 80 mesh sieves,The serosity having passed through 80 mesh sieves is filtered washing and obtains filter cake,This filter cake is soaked activation 1 hour in joining the diluted hydrochloric acid aqueous solution that pH value is 4,Carry out solid-liquid separation afterwards,Isolated filter cake obtains Novel lithium adsorbent product 1050 grams after drying at 100 DEG C of temperature.
Take this lithium adsorbent 1000 grams to join 8800mL content of magnesium to be 120g/L, lithium content be the high Mg/Li ratio aqueous salt brine of 4g/L is stirred under state absorption lithium, when absorption reach 2 little time after stop stirring carrying out solid-liquid separation, recording content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content is 0.1g/L, and isolated adsorbent filter cake sulphuric acid is deviate from lithium, obtaining the lithium solution 1300mL deviate from, the lithium concentration recording this lithium solution is 26g/L.
Above-mentioned deviate from lithium after adsorbent again put into 8800mL content of magnesium to be 120g/L, lithium content be the high Mg/Li ratio aqueous salt brine of 4g/L is stirred under state absorption lithium, when absorption reach 2 little time after stop stirring carrying out solid-liquid separation, recording content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content is 0.1g/L, and isolated adsorbent filter cake sulphuric acid is deviate from lithium, obtaining the lithium solution 1300mL deviate from, the lithium concentration recording this lithium solution is 26.2g/L.
Embodiment 3
nullTake and carry out ball milling after the spodumene concentrate high-temperature calcination that 1500 grams of lithium oxide content is 4% is transformed into β-spodumene concentrate and cross 60 mesh sieves,The refining material being collected by sieve is 1150 grams,The lithium oxide content recording this refining material is 5.2%,Take 1100 grams of these refining material concentrated sulphuric acids with 190.7 gram 98% to mix to add and be uniformly placed at 300 DEG C of temperature isothermal holding 60 minutes,It is subsequently cooled to 60 DEG C,Again this is joined in 2000mL water through the refining material that concentrated sulphuric acid heat treatment is good and be slurred,Serosity is crossed 80 mesh sieves,The serosity having passed through 80 mesh sieves is filtered washing and obtains filter cake,This filter cake is soaked activation 10 hours in joining dilute sulfuric acid that pH value is 4 mixed aqueous solution with dilute hydrochloric acid,Carry out solid-liquid separation afterwards,Isolated filter cake is dried at 150 DEG C of temperature and is obtained Novel lithium adsorbent product 1040 grams.
Take this Novel lithium adsorbent 1000 grams to join 6000mL content of magnesium to be 120g/L, lithium content be the high Mg/Li ratio aqueous salt brine of 4g/L is stirred under state absorption lithium, when absorption reach 2 little time after stop stirring carrying out solid-liquid separation, recording content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content is 0.15g/L, and isolated adsorbent filter cake sulfuric acid solution is deviate from lithium, obtaining the lithium solution 1000mL deviate from, the lithium concentration recording this lithium solution is 23g/L.
Above-mentioned deviate from lithium after adsorbent again put into 6000mL content of magnesium to be 120g/L, lithium content be the high Mg/Li ratio aqueous salt brine of 4g/L is stirred under state absorption lithium, when absorption reach 2 little time after stop stirring carrying out solid-liquid separation, recording content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content is 0.14g/L, and isolated adsorbent filter cake sulphuric acid is deviate from lithium, obtaining the lithium solution 1000mL deviate from, the lithium concentration recording this lithium solution is 23g/L.
Embodiment 4
nullTake and carry out ball milling after the spodumene concentrate high-temperature calcination that 1400 grams of lithium oxide content is 5% is transformed into β-spodumene concentrate and cross 60 mesh sieves,The refining material being collected by sieve is 1150 grams,The lithium oxide content recording this refining material is 6%,Take 1100 grams of these refining material concentrated sulphuric acids with 330 gram 98% to mix to add and be uniformly placed at 260 DEG C of temperature isothermal holding 40 minutes,It is subsequently cooled to 40 DEG C,Again this is joined in 2000mL water through the refining material that concentrated sulphuric acid heat treatment is good and be slurred,Serosity is crossed 80 mesh sieves,The serosity having passed through 80 mesh sieves is filtered washing and obtains filter cake,This filter cake is soaked activation 8 hours in joining the dilute sulfuric acid aqueous solution that pH value is 4,Carry out solid-liquid separation afterwards,Isolated filter cake is dried at 180 DEG C of temperature and is obtained Novel lithium adsorbent product 1050 grams.
Take this Novel lithium adsorbent 1000 grams to join 7000mL content of magnesium to be 120g/L, lithium content be the high Mg/Li ratio aqueous salt brine of 4g/L is stirred under state absorption lithium, when absorption reach 2 little time after stop stirring carrying out solid-liquid separation, recording content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content is 0.1g/L, and isolated adsorbent filter cake sulfuric acid solution is deviate from lithium, obtaining the lithium solution 1100mL deviate from, the lithium concentration recording this lithium solution is 24.4g/L.
Above-mentioned deviate from lithium after adsorbent again put into 7000mL content of magnesium to be 120g/L, lithium content be the high Mg/Li ratio aqueous salt brine of 4g/L is stirred under state absorption lithium, when absorption reach 2 little time after stop stirring carrying out solid-liquid separation, recording content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content is 0.1g/L, and isolated adsorbent filter cake sulphuric acid is deviate from lithium, obtaining the lithium solution 1100mL deviate from, the lithium concentration recording this lithium solution is 24.3g/L.
Lithium adsorbent prepared by the inventive method is big to the adsorption capacity of lithium, the lithium solution lithium concentration deviate from can up to about 25g/L, and the lithium solution deviate from after the lithium adsorbent absorption lithium of the inventive method production is lithium sulfate solution, except can be directly used for reacting production lithium carbonate with sodium carbonate, also can be directly used for hydro-oxidation sodium adopts freezing method to produce Lithium hydrate product, has spodumene ore deposit method and produces the advantage that Lithium hydrate technique is the same.
Claims (4)
1. a lithium adsorbent, this lithium adsorbent is prepared by following method: being transformed into after β-spodumene through high-temperature calcination by the spodumene concentrate that lithium oxide weight/mass percentage composition is 4%-7.5%, ball milling sieves, and has been collected by the purification refine material of sieve;Purification refine material mixes with concentrated sulphuric acid, it is warmed up to 200-300 DEG C after mix homogeneously and carries out heat preservation hot process 20-60 minute, it is subsequently cooled to not higher than 100 DEG C, again this sulfuric acid-treated good refining material is added to the water furnishing serosity sieving, then serosity it is filtered and washs, obtaining filter cake and filtrate;The filter cake obtained joins after carrying out immersion activation in the subacidity water that pH is 4-5 1-10 hour, carries out filter cake after solid-liquid separation is activated, and filter cake is dried at 100-200 DEG C of temperature and just obtained lithium adsorbent product.
2. the preparation method of a lithium adsorbent, it is characterised in that comprise the following steps:
(1) selecting spodumene concentrate is raw material stage: the spodumene concentrate selecting lithium oxide weight/mass percentage composition to be 4%-7.5% is the raw material preparing lithium adsorbent;
(2) to spodumene concentrate polishing purification step: the spodumene concentrate that lithium oxide weight/mass percentage composition is 4%-7.5% is transformed into after β-spodumene through high-temperature calcination, ball milling crosses 60 mesh sieves, remove the residue on sieve being mainly quartz, be collected by the purification refine material of 60 mesh sieves;
(3) de-lithium again purification step: the concentrated sulphuric acid of the purification refine material and mass concentration 98% that have passed through 60 mesh sieves that step (2) is collected mixes, the addition mole of concentrated sulphuric acid is in refining material 1~1.5 times of lithium oxide mole, it is warmed up to 200-300 DEG C after mix homogeneously and carries out heat preservation hot process 20-60 minute, it is subsequently cooled to not higher than 100 DEG C, be added to the water this sulfuric acid-treated good refining material furnishing serosity mistake 80 mesh sieves again, again remove residue on sieve, then the serosity having passed through 80 mesh sieves it is filtered and washs, obtain filter cake and filtrate, filtrate is that lithium sulfate solution can be used for preparing Lithium hydrate or lithium carbonate;
(4) activation step: the filter cake that step (3) is obtained joins after carrying out immersion activation in the subacidity water that pH is 4-5 1-10 hour, carries out filter cake after solid-liquid separation is activated, and filter cake is dried at 100-200 DEG C of temperature and just obtained lithium adsorbent product.
3. the preparation method of a kind of lithium adsorbent according to claim 2, it is characterised in that: in step (4), pH is any in the mixed solution that subacidity water is dilute hydrochloric acid solution, dilution heat of sulfuric acid, dilute hydrochloric acid and sulphuric acid three kinds of 4-5.
4. a kind of lithium adsorbent described in claim 1 is extracting the application of lithium from the salt containing magnesium lithium.
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Cited By (2)
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KR20200023884A (en) * | 2018-08-27 | 2020-03-06 | 주식회사 엘지화학 | Lithium ion adsorbent and a method for recovering lithium ion using the same |
CN115814755A (en) * | 2022-12-20 | 2023-03-21 | 江苏容汇通用锂业股份有限公司 | Adsorbent for waste residue of phosphorus-lithium aluminum, preparation method and application thereof |
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Cited By (3)
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KR20200023884A (en) * | 2018-08-27 | 2020-03-06 | 주식회사 엘지화학 | Lithium ion adsorbent and a method for recovering lithium ion using the same |
KR102521570B1 (en) | 2018-08-27 | 2023-04-12 | 주식회사 엘지화학 | Lithium ion adsorbent and a method for recovering lithium ion using the same |
CN115814755A (en) * | 2022-12-20 | 2023-03-21 | 江苏容汇通用锂业股份有限公司 | Adsorbent for waste residue of phosphorus-lithium aluminum, preparation method and application thereof |
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Application publication date: 20160720 |