CN110508234A - A kind of aluminium salt type nano fibrous membrane lithium adsorbent and the preparation method and application thereof - Google Patents
A kind of aluminium salt type nano fibrous membrane lithium adsorbent and the preparation method and application thereof Download PDFInfo
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- CN110508234A CN110508234A CN201910725553.6A CN201910725553A CN110508234A CN 110508234 A CN110508234 A CN 110508234A CN 201910725553 A CN201910725553 A CN 201910725553A CN 110508234 A CN110508234 A CN 110508234A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J20/046—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 containing halogens, e.g. halides
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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
- B01J20/06—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
- B01J20/08—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 comprising aluminium oxide or hydroxide; comprising bauxite
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
- B01J20/28038—Membranes or mats made from fibers or filaments
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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Abstract
The invention discloses a kind of aluminium salt fiber type film lithium adsorbents and the preparation method and application thereof, comprising the following steps: S1, preparation aluminium salt type lithium ion adsorbent；S2, suspension of the preparation containing aluminium salt type lithium ion adsorbent and polymer: it takes polymer to be dissolved in organic solvent and is prepared into polymer solution, after stirring, aluminium salt type lithium ion adsorbent is added to continue to stir, obtains the suspension containing aluminium salt type lithium ion adsorbent and polymer；S3, the progress electrostatic spinning of suspension made from aforesaid operations is taken to obtain the aluminium salt type nano fibrous membrane lithium adsorbent.The present invention program by electrostatic spinning technique by the aluminium salt type lithium ion sorbent-loaded with good adsorption effect on nano fibrous membrane, more active sites can be exposed, nanofiber is staggered, it is easy to the intrusion of lithium liquid, it can sufficiently be contacted with adsorbent, good penetrability is conducive to pillar operation, but is not limited to pillar operation.
Description
Technical field
The present invention relates to lithium electro-technical fields, and in particular to a kind of aluminium salt type nano fibrous membrane lithium adsorbent and its preparation side
Method and application.
Background technique
Currently, salt lake mention lithium technique mainly use the precipitation method, solvent extraction, absorption method, calcining leaching method, carbonizatin method,
Pump suction method and electroosmose process etc..Wherein, since there are various inherent shortcomings (such as poor selectivity, complex process), precipitatings for method
Method, solvent extraction, calcining leaching method, carbonizatin method, pump suction method and electroosmose process etc. can not heavy industrialization application.Absorption
Method is as a kind of simple process, the good, rate of recovery of selectivity is high and it is environmentally protective propose lithium method, have with other methods ratio certain excellent
Gesture is suitble to large-scale industrial production.
Absorption method is that adsorbent is achieved the purpose that and other ion isolations by selective absorption lithium ion.Adsorb legal system lithium
Key be the excellent adsorbent of processability.Lithium adsorbent can be divided to organic adsorbent and two kinds of inorganic adsorbent.Organic adsorption
Agent typically refers to ion exchange organic resin, according to its charge differences, due to being that lithium ion is adsorbed on resin by library power
On, based on the limitation of this physicochemical properties so that it is selectively low to lithium ion, exchange velocity is slow, molten damage degree is big and
Utilization rate is low, and therefore, the application of organic adsorbent is by certain limitation.Inorganic adsorbent is high to lithium selectivity, it is alternatively that
Property mention lithium inorganic ions exchange and adsorbent, mainly include layered adsorbent, unformed hydroxide adsorbent, stibate inhale
Attached dose, aluminium salt lithium adsorbent and ion-sieve type adsorbent etc..Layered adsorbent structure during adsorption-desorption is easy to be broken
It is bad, lead to not realize that industrialized production, the excessively high problem of the unformed molten damage of hydroxide cannot solve always；The absorption of titanium system
Agent is with high costs.Aluminium salt type adsorbent material is cheap and easy to get, lithium ion selectivity is strong, is a research hotspot in recent years,
But aluminium salt type adsorbent in the prior art be it is powdered, lead to its mobility and poor permeability, be unfavorable for actual production, because
This, is granulated and film forming is to propose lithium technology industrialization urgent problem to be solved.
Summary of the invention
The first technical problem to be solved by the present invention is: providing the aluminium salt fiber type of a kind of mobility and good penetrability
The preparation method of film lithium adsorbent.
Second technical problem to be solved by this invention is: providing a kind of aluminium salt type nanometer as made from the above method
Tunica fibrosa lithium adsorbent.
Third technical problem to be solved by this invention is: providing answering for above-mentioned aluminium salt type nano fibrous membrane lithium adsorbent
With.
In order to solve above-mentioned first technical problem, the technical solution adopted by the present invention are as follows: a kind of aluminium salt fiber type film lithium
The preparation method of adsorbent, comprising the following steps:
S1, preparation aluminium salt type lithium ion adsorbent, the aluminium salt type lithium ion adsorbent are xLiCl2Al (OH)3·
nH2O, wherein the value of x and n meets the following conditions: 0 < x < 1,0.5≤n≤2 respectively；
S2, suspension of the preparation containing aluminium salt type lithium ion adsorbent and polymer: polymer is taken to be dissolved in organic solvent
It is prepared into polymer solution, at (40~60) DEG C, after stirring (1~3) h with the speed of (300~1000) r/min, aluminium is added
Salt form lithium ion adsorbent continues to stir (3~6) h, obtains the suspension containing aluminium salt type lithium ion adsorbent and polymer；
S3, the progress electrostatic spinning of suspension made from aforesaid operations is taken to obtain the aluminium salt type nano fibrous membrane lithium absorption
Agent.
Further, the operation of aluminium salt type lithium ion adsorbent is prepared in the step S1 are as follows: close using aluminium salt and lithiumation
Object is reacted under alkaline condition or in acid condition with lithium chloride using meta-aluminate the aluminium salt type lithium ion adsorbent is made.
Further, the operation of aluminium salt type lithium ion adsorbent is prepared in the rapid S1 specifically: utilize aluminium chloride and chlorine
Change lithium and prepares the aluminium salt type lithium ion adsorbent；Preferably, by AlCl3Contain alkalization with being added after LiCl mixing to addition
It closes and is reacted in the solution of object, be (30~600) r/min, (40~70) DEG C heating reaction (30~70) min in reaction revolving speed
Afterwards, it is separated by solid-liquid separation, collects solid up to the aluminium salt type lithium ion adsorbent.
Preferably, mole metering of the aluminium chloride and lithium chloride is than being (1.8~2.5): 1.
Further, aluminium element and hydroxy mole of metering ratio in alkali compounds are 1:(3~3.3 in aluminium chloride).
Preferably, the solution containing alkali compounds is ammonium hydroxide or sodium hydroxide solution；It is highly preferred that the ammonium hydroxide
Or the concentration of sodium hydroxide solution is (2~8) mol/L.
Further, mole metering of aluminium chloride and ammonium hydroxide or sodium hydroxide is than being 1:(3~3.3).
Preferably, after separation of solid and liquid, after solid washing, dry (8~12) h at (80~105) DEG C, after grinding
Sieving obtains the aluminium salt type lithium ion adsorbent.
Further, the mesh number of sieve used in the sieving operating process is 400 mesh.
Further, the organic solvent includes n,N-Dimethylformamide (N, N-Dimethylformamide, DMF)
Or at least one of dimethyl acetamide (Dimethylacetamide, DMAC).
Preferably, the organic solvent is DMF, and the polymer is polyacrylonitrile (polyacrylonitrile, PAN)
Or polylactic acid (polylactic acid, PLA)；Preferably, the molecular weight of the PAN is one in 8.5 ten thousand, 150,000 or 250,000
Kind；Preferably, the molecular weight of the PLA is 160,000.
Further, the mass fraction of polymer is 8%~12% in the polymer solution；Preferably 10%.
Further, the mass fraction of aluminium salt type lithium ion adsorbent is 15%~22% in the suspension；Preferably
18%.
It further, further include to the nano fibrous membrane obtained after electrostatic spinning in (65~105) DEG C in the step S3
The step of lower drying (12~24) h.
Further, in the step S3, voltage is (16~21) kV in electrostatic spinning operating process.
Further, in the step S3, the flow velocity of suspension is (1.0~2.5) ml/h during electrostatic spinning.
The beneficial effects of the present invention are: by electrostatic spinning technique by the aluminium salt type lithium ion with good adsorption effect
Sorbent-loaded can expose more active sites on nano fibrous membrane, and nanofiber is staggered, and be easy to lithium liquid
Intrusion, can sufficiently contact with adsorbent, good penetrability, be conducive to pillar operation, but be not limited to pillar operation.
In order to solve above-mentioned second technical problem, the technical solution adopted by the present invention are as follows: one kind passes through above method system
The aluminium salt fiber type film lithium adsorbent obtained.
In order to solve above-mentioned third technical problem, the technical solution adopted by the present invention are as follows: a kind of extraction work of lithium ion
Skill, comprising the following steps: elemental lithium is extracted from the solution containing elemental lithium using above-mentioned aluminium salt fiber type film lithium adsorbent.
Preferably, the solution containing elemental lithium is salt lake bittern.
The beneficial effects of the present invention are: lithium adsorbent made from the present invention program is applied to the solution containing elemental lithium
In, especially salt lake bittern has good application effect, and molten damage is low in absorption-resolving, and reusable rate is high, energy
It is enough effectively to solve the problems, such as the flowing of aluminium salt type lithium adsorbent, poor permeability in the prior art, there is good prospects for commercial application.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The embodiment of the present invention one are as follows: a kind of preparation method of aluminium salt type nano fibrous membrane lithium adsorbent, including following step
It is rapid:
(1) after 240.0g anhydrous aluminum chloride 42.4g lithium chloride being dissolved in 500mL, being added to 740mL concentration is 8mol/L
Sodium hydroxide solution in, be 600r/min in reaction revolving speed, be separated by solid-liquid separation after heating reaction 70min at 40 DEG C, solid is washed
8h is dried after washing at 105 DEG C, obtains 112.09 aluminium salt type lithium ion adsorbents after crossing 400 mesh screens after grinding.
(2) PAN that 34.78g molecular weight is 8.5 ten thousand is added into the DMF solution of 334.7g, is 40 DEG C in temperature,
3h is stirred under 300r/min stirring rate, then weighs 65.22g aluminium salt type lithium ion adsorbent into solution, is obtained after stirring 3h
The suspension of polymer and adsorbent.
(3) above-mentioned suspension 100mL is taken, is 21.0kV in operation voltage, suspension flow velocity is that 2.5mL/h carries out Static Spinning
Thread, nano fibrous membrane is removed after electrostatic spinning, is dried at 65 DEG C and obtains aluminium salt type nano fibrous membrane lithium adsorbent afterwards for 24 hours.
The embodiment of the present invention two are as follows: a kind of preparation method of aluminium salt type nano fibrous membrane lithium adsorbent, including following step
It is rapid:
(1) after 240.0g anhydrous aluminum chloride 30.6g lithium chloride being dissolved in 500mL, being added to 2.7L concentration is 2mol/L
Sodium hydroxide solution in, be 30r/min in reaction revolving speed, be separated by solid-liquid separation after heating reaction 30min at 70 DEG C, solid is washed
The dry 12h at 80 DEG C afterwards, obtains 119.0g aluminium salt type lithium ion adsorbent after crossing 400 mesh screens after grinding.
(2) PAN that 47.28g molecular weight is 150,000 is added into the DMF solution of 294.0g, is 60 DEG C in temperature,
1h is stirred under 1000r/min stirring rate, then weighs 86.68g aluminium salt type lithium ion adsorbent into solution, is obtained after stirring 6h
The suspension of polymer and adsorbent.
(3) above-mentioned suspension 100mL is taken, is 19.0kV in operation voltage, suspension flow velocity is that 1.0mL/h carries out Static Spinning
Thread, nano fibrous membrane is removed after electrostatic spinning, obtains aluminium salt type nano fibrous membrane lithium adsorbent after drying 12h at 105 DEG C.
The embodiment of the present invention three are as follows: a kind of preparation method of aluminium salt type nano fibrous membrane lithium adsorbent, including following step
It is rapid:
(1) after 240.0g anhydrous aluminum chloride 38.2g lithium chloride being dissolved in 600mL, being added to 1440ml concentration is 4mol/
In the ammonia spirit of L, it is 300r/min in reaction revolving speed, is separated by solid-liquid separation after heating reaction 60min at 50 DEG C, after solid is washed
Dry 10h, obtains 106.0g aluminium salt type lithium ion adsorbent after crossing 400 mesh screens after grinding at 90 DEG C.
(2) PAN that 35.74g molecular weight is 250,000 is added into the DMF solution of 257.4g, is 50 DEG C in temperature,
2h is stirred under 500r/min stirring rate, then weighs 64.30g aluminium salt type lithium ion adsorbent into solution, is obtained after stirring 5h
The suspension of polymer and adsorbent.
(3) above-mentioned suspension 100mL is taken, is 16.0kV in operation voltage, suspension flow velocity is that 1.5mL/h carries out Static Spinning
Thread, nano fibrous membrane is removed after electrostatic spinning, obtains aluminium salt type nano fibrous membrane lithium adsorbent after drying 18h at 95 DEG C.
The embodiment of the present invention four are as follows: a kind of preparation method of aluminium salt type nano fibrous membrane lithium adsorbent, including following step
It is rapid:
(1) after 240.0g anhydrous aluminum chloride 36.2g lithium chloride being dissolved in 1000mL, being added to 930ml concentration is 6mol/
In the sodium hydroxide solution of L, it is 800r/min in reaction revolving speed, is separated by solid-liquid separation after heating reaction 50min at 55 DEG C, solid is washed
10h is dried after washing at 105 DEG C, obtains 114.5g aluminium salt type lithium ion adsorbent after crossing 400 mesh screens after grinding.
(2) PLC that 30.1g molecular weight is 160,000 is added into the DMF solution of 233.4g, is 45 DEG C in temperature, 800r/
3h is stirred under min stirring rate, then weighs 49.9g aluminium salt type lithium ion adsorbent into solution, obtains polymer after stirring 4h
With the suspension of adsorbent.
(3) above-mentioned suspension 100mL is taken, is 20.0kV in operation voltage, suspension flow velocity is that 2.0mL/h carries out Static Spinning
Thread, nano fibrous membrane is removed after electrostatic spinning, obtains aluminium salt type nano fibrous membrane lithium adsorbent after drying 20h at 105 DEG C.
Physico-chemical analysis detection is carried out to aluminium salt type nano fibrous membrane lithium adsorbent obtained in Examples 1 to 4 and tension is strong
Degree test, test result is as follows shown in table 1 for analysis:
The lithium ion adsorbent physical and chemical index and tensile strength test result of 1 embodiment of the present invention 1~4 of table preparation
Aluminium salt type nano fibrous membrane lithium adsorbent obtained in Examples 1 to 4 proposes the acidification of certain salt lake and obtains after boron
Brine carries out Static Adsorption-parsing and proposes lithium experiment, tests brine composition used and physical property is as shown in table 2 below:
The acidification of certain salt lake of table 2 mentions brine main component and physical property table after boron
10ml brine is taken to be diluted to 200mL respectively, the absorption of aluminium salt type nano fibrous membrane lithium obtained in Example 1~4
Each 5.0g of agent, at normal temperature, magnetic agitation, adsorption time carry out adsorption experiment under the conditions of being 120min, after filtering, measurement absorption
Li in solution afterwards+Concentration.Then ionized water 200mL is removed, at normal temperature, magnetic agitation, under the conditions of the parsing time is 150min
It is parsed, measures the Li in desorbed solution+Concentration.By the aluminium salt type nano fibrous membrane lithium adsorbent weighing after absorption-parsing, survey
Determine the molten damage of adsorbent, it is molten in absorption-resolving of aluminium salt type nano fibrous membrane lithium adsorbent obtained in Examples 1 to 4
The results are shown in Table 3 for damage:
Absorption-parsing data of the aluminium salt type nano fibrous membrane lithium adsorbent of 3 embodiment of the present invention 1~4 of table preparation
As can be seen that the Li of the granular lithium ion adsorbent of the embodiment of the present invention preparation from upper table 3+Adsorption capacity
In 4.88g/mg or more, analytic capacity 3.19g/mg or more, resolution factor reaches 65% or more, while in absorption-resolving
Middle nano fibrous membrane is simultaneously not damaged, and the molten damage of absorption-resolving is low, reusable, efficiently solves existing powdery aluminium ion
The problem of adsorbent flowing, poor permeability, there is good industrial application value.
By AlCl in the embodiment of the present invention3The solution containing alkali compounds is added with the mode of cocurrent after LiCl mixing
In, reaction initial pH value is higher, generates meta-aluminate, and as mixed solution is further added, pH value is reduced, and meta-aluminate turns
It is melted into the stronger unformed aluminium hydroxide of adsorption activity, partial size is small, and adsorption area is big, and adsorption effect is good.Pass through electrostatic spinning skill
Aluminium salt type lithium ion sorbent-loaded on nano fibrous membrane, can be exposed more active sites by art, and nanofiber is handed over
Mistake arrangement, is easy to the intrusion of lithium liquid, can sufficiently contact with adsorbent, good penetrability, is conducive to pillar operation, but is not limited to
Pillar operation.The PAN and PLA used simultaneously is as fibre-forming polymer, and filming performance is good, and chemical stability is good, and cost of material is low,
Conducive to industrialized production.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (10)
1. a kind of preparation method of aluminium salt fiber type film lithium adsorbent, it is characterised in that: the following steps are included:
S1, preparation aluminium salt type lithium ion adsorbent, the aluminium salt type lithium ion adsorbent are xLiCl2Al (OH)3·nH2O,
In, the value of x and n meet the following conditions: 0 < x < 1,0.5≤n≤2 respectively；
S2, suspension of the preparation containing aluminium salt type lithium ion adsorbent and polymer: it takes polymer to be dissolved in organic solvent and prepares
At polymer solution, at (40~60) DEG C, after stirring (1~3) h with the speed of (300~1000) r/min, aluminium salt type is added
Lithium ion adsorbent continues to stir (3~6) h, obtains the suspension containing aluminium salt type lithium ion adsorbent and polymer；
S3, the progress electrostatic spinning of suspension made from aforesaid operations is taken to obtain the aluminium salt type nano fibrous membrane lithium adsorbent.
2. the preparation method of aluminium salt fiber type film lithium adsorbent according to claim 1, it is characterised in that: the step S1
The operation of middle preparation aluminium salt type lithium ion adsorbent specifically: by AlCl3Contain alkalization with being added after LiCl mixing to addition
It closes and is reacted in the solution of object, be (30~600) r/min, (40~70) DEG C heating reaction (30~70) min in reaction revolving speed
Afterwards, it is separated by solid-liquid separation, collects solid up to the aluminium salt type lithium ion adsorbent.
3. the preparation method of aluminium salt fiber type film lithium adsorbent according to claim 2, it is characterised in that: the aluminium chloride
Mole metering with lithium chloride is than being (1.8~2.5): 1.
4. the preparation method of aluminium salt fiber type film lithium adsorbent according to claim 2, it is characterised in that: aluminium in aluminium chloride
Hydroxy mole of metering is than being 1:(3~3.3 in element and alkali compounds).
5. the preparation method of aluminium salt fiber type film lithium adsorbent according to claim 1, it is characterised in that: described organic molten
Agent includes at least one of DMF or DMAC.
6. the preparation method of aluminium salt fiber type film lithium adsorbent according to claim 5, it is characterised in that: described organic molten
Agent is DMF, and the polymer is PAN or PLA；Preferably, the molecular weight of the PAN is one in 8.5 ten thousand, 150,000 or 250,000
Kind；Preferably, the molecular weight of the PLA is 160,000.
7. the preparation method of aluminium salt fiber type film lithium adsorbent according to claim 1, it is characterised in that: the polymer
The mass fraction of polymer is 8%~12% in solution；Preferably, in the suspension aluminium salt type lithium ion adsorbent quality
Score is 15%~22%；Preferably 18%.
8. the preparation method of aluminium salt fiber type film lithium adsorbent according to claim 1, it is characterised in that: the step S3
In, voltage is (16~21) kV in electrostatic spinning operating process；Preferably, the flow velocity of suspension is (1.0 during electrostatic spinning
~2.5) ml/h.
9. a kind of aluminium salt fiber type film lithium adsorbent as made from method as described in any one of claims 1 to 8.
10. a kind of extraction process of lithium ion, comprising the following steps: utilize aluminium salt fiber type film lithium as claimed in claim 9
Adsorbent extracts elemental lithium from the solution containing elemental lithium.
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