CN110090614A - A kind of preparation method of lithium ion sieve adsorbant and products thereof and application - Google Patents
A kind of preparation method of lithium ion sieve adsorbant and products thereof and application Download PDFInfo
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- CN110090614A CN110090614A CN201910451148.XA CN201910451148A CN110090614A CN 110090614 A CN110090614 A CN 110090614A CN 201910451148 A CN201910451148 A CN 201910451148A CN 110090614 A CN110090614 A CN 110090614A
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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Abstract
The invention discloses preparation methods of a kind of lithium ion sieve adsorbant and products thereof and application, the following steps are included: pore-foaming agent, lithium salts, assistant metal salt are placed in solvent, after being stirred, butyl titanate is added, it is uniform to solution mixing to continue stirring, obtains spinning solution；Spinning solution is placed in the solution storage device of electrostatic spinning machine, the technological parameter of electrostatic spinning is set, electrospinning is then carried out, obtains nanofiber；After nanofiber drying, is calcined in air atmosphere, after calcining, obtain lithium ion sieve presoma；Lithium ion sieve presoma is stirred to react in mineral acid, after completion of the reaction, obtains lithium ion sieve adsorbant.Porous nano-fibre shape lithium ion sieve adsorbant specific surface area prepared by the present invention is very big, increases the contact area of adsorbent and solution, its adsorption capacity to lithium ion can be improved.Porous fibrous lithium ion sieve generally ion sieve structure is high to lithium ion adsorptive selectivity.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of preparation method of lithium ion sieve adsorbant and products thereof with
Using.
Background technique
With the fast development of clean energy resource, the demand of lithium is increasing.The complex process that lithium is extracted from lithium mine, at
This height.Lake water containing lithium salts is important lithium source, however contains sodium at high concentration, magnesium, potassium plasma in salt lake saline.Conventional solvent extraction
It takes, the methods of ion exchange, precipitating and UF membrane are difficult highly selective separating Li.Lithium ion sieve can effectively high-selectivity adsorption divide
From lithium ion.The most commonly used is manganese base lithium ion sieves, but there are the molten damage phenomenons of manganese for manganese base lithium ion sieve, especially in acidic environment
The molten damage of middle manganese is more serious, and crystal structure is destroyed, and declines to the adsorptive selectivity of lithium ion, the stability of cycle applications compared with
Difference, the adsorption capacity decline of lithium ion.It is sieved compared to manganese base lithium ion, titanium-based lithium ion sieve chemical stability is higher.Using tradition
Solid phase synthesis process preparation titanium-based lithium ion sieve be fine particle, be easy to happen aggregation in water, substantially weaken its to lithium from
Sub- adsorption capacity.Come supported ionic sieve particle, but carrier although with some carriers (including carbon material, polymer nanofiber)
Use so that lithium ion diffusion hindered and partial adsorbates site are blanked, lithium ion adsorption efficiency is low.Before this, not yet
Report porous fibrous lithium ion sieve.Porous fibrous lithium ion sieve generally ion sieve structure of the invention, lithium ion
Diffusion rate is fast, adsorption capacity is high, selectivity is high.
Summary of the invention
The lithium ion sieve adsorbant that the object of the present invention is to provide a kind of adsorption capacities is high, selectivity is high, performance is stable
Preparation method and products thereof and application.
The preparation method of this lithium ion sieve adsorbant of the present invention, comprising the following steps:
1) pore-foaming agent, lithium salts, assistant metal salt are placed in the mixed solvent, after being stirred, butyl titanate is added, continues
Stirring is uniform to solution mixing, obtains spinning solution；
2) spinning solution in step 1) is placed in the solution storage device of electrostatic spinning machine, the technique for setting electrostatic spinning
Parameter then carries out electrospinning, obtains nanofiber；
3) by the nanofiber in step 2) it is dry after, calcined in air atmosphere, after calcining, obtain lithium from
Son sieve presoma (P-LXTO-NF)；
4) the lithium ion sieve presoma in step 3) is stirred to react in mineral acid, after completion of the reaction, obtains lithium
Ion sieve adsorbant (P-HXTO-NF).
P represents porous structure in the skeleton symbol P-LXTO-NF and P-HXTO-NF, and L represents lithium, and X represents assistant metal, T generation
Table titanium, O represent oxygen, and NF represents nanofiber.
Pore-foaming agent in the step 1) is polyvinylpyrrolidone (PVP), polyethylene oxide (PEO), polylactide
(PLA), one of polyacrylonitrile (PAN), polyvinyl alcohol (PVA)；Lithium salts is LiAc；Assistant metal salt is FeAc2、ZrOCl2
One of；Pore-foaming agent, lithium salts, assistant metal salt and butyl titanate mass ratio be 7:(2~10): (0~6): (20~
50)；Mixed solvent is made of EtOH, HAc, DMF, and the volume ratio of three is (50~100): (10~50): (15~60)；It is described
Pore-foaming agent and mixed solvent mass volume ratio be 7:(90~110) g/ml.
In the step 2), the technological parameter of electrospinning are as follows: 3~15kV of voltage.
In the step 3), calcination temperature is 550~750 DEG C, and calcination time is 3~5h.
In the step 4), being stirred to react the time is 0.5~1.5h.
Lithium ion sieve presoma (P-LXTO-NF) and lithium ion sieve adsorbant is prepared according to the preparation method
(P-HXTO-NF), X therein is F, Z or does not have that F represents Fe2O3, Z represents ZrO2。
The lithium ion sieve presoma and lithium ion sieve adsorbant have porous nano-fibre structure.
The method of the lithium ion sieve absorption lithium ion, comprising the following steps: the pH to 6~12 for adjusting lithium-containing solution connects
Adsorbent is added in lithium-containing solution, followed by absorption lithium ion is stirred to react, after absorption, be separated by filtration suction
Attached dose, after then impregnating desorption lithium ion in acid, regeneration lithium ion adsorbent is obtained, a sorption cycle is completed.
Beneficial effects of the present invention: 1) lithium ion sieve adsorbant prepared by the present invention is a kind of porous nano-fibre, originally
The structure of nanofiber has made adsorbent specific surface area bigger, also has microcellular structure on fiber in addition, so that this hair
Bright adsorbent specific surface area is very big, largely increases the contact area of adsorbent and solution, can be largely
Upper its suction-operated to lithium ion of raising.2) lithium ion sieve adsorbant of the invention is high to the adsorption capacity of lithium, thus its is right
Containing lithium, sodium, potassium, magnesium ion water in lithium have high-selectivity adsorption, by taking the P-HTO-NF in embodiment 1 as an example, to the heat of lithium
Mechanics adsorption capacity is up to 59.12mg/g；Even if potassium (928mg/L), sodium (753mg/L), magnesium (4288mg/L) ion are dense in water
Degree is much higher than lithium concentration (40mg/L), and the adsorption equilibrium distribution coefficient (360mL/g) of lithium ion is much larger than potassium ion
(1.6mL/g), sodium ion (0.66mL/g), magnesium ion (0.33mL/g) have very high selectivity to lithium ion absorption.3)
Adsorbent in the present invention can be recycled repeatedly, can effectively reduce cost.Also, the porous lithium ion of the invention sieves absorption
Agent has higher lithium ion adsorption capacity than the lithium ion sieve adsorbant that conventional solid synthesizes, and reusing is more excellent.4)
The present invention adulterates Fe in titanium-based lithium ion sieve2O3Be conducive to the Magnetic Isolation of adsorbent；ZrO is adulterated in titanium-based lithium ion sieve2
Be conducive to improve the chemical stability of molecular sieve.
Detailed description of the invention
Fig. 1 is the P-LTO-NF (a1) of Examples 1 to 3 preparation, the scanning electricity of P-LFTO-NF (b1), P-LZTO-NF (c1)
Mirror figure；P-LTO-NF (a2), P-LFTO-NF (b2), the transmission electron microscope picture of P-LZTO-NF (c2)；P-LTO-NF (a3), P-
LFTO-NF (b3), the high-resolution-ration transmission electric-lens figure of P-LZTO-NF (c3).
The XRD diagram of P-LTO-NF (a), P-LFTO-NF (b), P-LZTO-NF (c) prepared by Fig. 2 Examples 1 to 3.
P-HTO-NF prepared by Fig. 3 embodiment 1 is to lithium ion Adsorption thermodynamics figure.
Specific embodiment
Embodiment 1
(1) porous nano-fibre shape Li4Ti5O12(P-LTO-NF) it prepares
7g pore-foaming agent (PVP), 5g lithium salts (LiAc) and 105mL mixed solvent (80mL EtOH, 10mLHAc and 15mLDMF)
It is mixed, 1h is then stirred at room temperature；Followed by 25g butyl titanate (TBOT) is added, then proceedes to that 2h is stirred at room temperature, obtain
Spinning solution.Electrospinning liquid is put into the solution stowage device of electrostatic spinning machine, the voltage that electrospinning is arranged is 14kV, then carries out electricity
It spins, obtains nano fibrous membrane.
By nano fibrous membrane after drying at room temperature, 650 DEG C of calcining 3h, obtain porous nano-fibre shape titanium under air environment
Base lithium ion sieves presoma (P-LTO-NF).
(2) lithium ion sieve adsorbant H4Ti5O12(P-HTO-NF) it prepares
1g P-LTO-NF is put into the hydrochloric acid of 100mL 0.2M and stirs 1h, solid room temperature is dried to obtain H4Ti5O12
(P-HTO-NF) adsorbent.
P-LTO-NF manufactured in the present embodiment is subjected to SEM, TEM test, shown in a1, a2 and the a3 of result as shown in figure 1.
From a1 it is found that P-LTO-NF is at threadiness, and fiber surface is coarse, and the average diameter of fiber is about 400nm；It can from a2
Out, there are porous structures on P-LTO-NF fiber；It can be concluded that, duct 0.48nm just corresponds to spinelle from a3
Li4Ti5O12111 crystal faces.
The present embodiment preparation P-LTO-NF is subjected to XRD test, shown in result such as Fig. 2 (a): the spy of P-LTO-NF map
Levy the Li at peak and highly crystalline4Ti5O12Spinel structure is to comply fully with.
Embodiment 2
(1) porous nano-fibre shape Li4Ti5O12-Fe2O3(P-LFTO-NF) it prepares
7g pore-foaming agent (PVP), 5g lithium salts (LiAc), 5g molysite (FeAc2) and 105mL mixed solvent (80mL EtOH,
10mLHAc and 15mLDMF) it is mixed, 1h is then stirred at room temperature；Followed by be added 25g butyl titanate (TBOT), then after
It is continuous that 2h is stirred at room temperature, obtain spinning solution.Spinning solution is put into the solution stowage device of electrostatic spinning machine, the voltage of electrospinning is set
Then 14kV carries out electrospinning, obtains nanofiber.
By nanofiber after drying at room temperature, 650 DEG C of calcining 3h, obtain porous nano-fibre shape titanium-based under air environment
Lithium ion sieve presoma (P-LFTO-NF).
(2) lithium ion sieve adsorbant H4Ti5O12(P-HFTO-NF) it prepares
1g P-LFTO-NF is put into the hydrochloric acid of 100mL 0.2M and stirs 1h, solid room temperature is dried to obtain H4Ti5O12
(P-HFTO-NF) adsorbent.
P-LFTO-NF manufactured in the present embodiment is subjected to SEM, TEM test, b1, b2 and b3 institute of result as shown in figure 1
Show.From b1 it is found that P-LFTO-NF is at threadiness, and fiber surface is coarse, and the average diameter of fiber is about 300nm；It can from b2
To find out, there are porous structures on P-LFTO-NF fiber；It can be concluded that, duct 0.48nm, just corresponding point is brilliant from b3
Stone Li4Ti5O12111 crystal faces.
The present embodiment preparation P-LFTO-NF is subjected to XRD test, shown in result such as Fig. 2 (b): P-LFTO-NF map
Characteristic peak, not only containing the Li of highly crystalline4Ti5O12Spinel structure further includes having Fe2O3Maghemite crystalline character peak.
Fe is introduced in lithium ion sieve adsorbant2O3The Magnetic Isolation of adsorbent can be achieved.
Embodiment 3
(1) porous nano-fibre shape Li4Ti5O12-ZrO2(P-LZTO-NF) it prepares
7g pore-foaming agent (PVP), 5g lithium salts (LiAc), 5g zirconates (ZrOCl2) and 105mL mixed solvent (80mL EtOH,
10mL HAc and 15mL DMF) it is mixed, 1h is then stirred at room temperature；Followed by 25g butyl titanate is added, room is then proceeded to
Temperature stirring 2h, obtains spinning solution.Spinning solution is put into the solution stowage device of electrostatic spinning machine, the voltage of electrospinning is set
Then 14kV carries out electrospinning, obtains nanofiber.
By nanofiber after drying at room temperature, 650 DEG C of calcining 3h, obtain porous nano-fibre shape titanium-based under air environment
Lithium ion sieve presoma (P-LZTO-NF).
(2) lithium ion sieve adsorbant H4Ti5O12-ZrO2(P-HZTO-NF) it prepares
1g P-LFTO-NF is put into the hydrochloric acid of 100mL 0.2M and stirs 1h, solid room temperature is dried to obtain H4Ti5O12
(P-HFTO-NF) adsorbent.
P-LZTO-NF manufactured in the present embodiment is subjected to SEM, TEM test, c1, c2 and c3 institute of result as shown in figure 1
Show.From b1 it is found that P-LZTO-NF is at threadiness, and fiber surface is coarse, and the average diameter of fiber is about 250nm；It can from c2
To find out, there are porous structures on P-LZTO-NF fiber；It can be concluded that, duct 0.48nm is just corresponded to from c3
Li4Ti5O12111 crystal faces.
The present embodiment preparation P-LZTO-NF is subjected to XRD test, shown in result such as Fig. 2 (c): P-LZTO-NF map
Characteristic peak, not only containing the Li of highly crystalline4Ti5O12Spinel structure further includes having ZrO2Tetragonal crystal characteristic peak.
The test of 4 absorption property of embodiment
(1) lithium ion adsorption experiment
1g lithium ion sieve adsorbant (P-HTO-NF, P-HFTO-NF and P-HZTO-NF of Examples 1 to 3 preparation) is added
In the water for being 1L to volume, Li in water+Reaction 2h is stirred at room temperature in=25~1000mg/L, pH=10, and reaction is completed, filtering point
From adsorbent, each ion concentration in water is detected.Adsorption capacity Q of the adsorbent to lithium ione=(Co-Ce) V/m, QeBigger expression
Adsorbent is stronger to the adsorption capacity of the ion.
1 adsorbent P-HTO-NF of embodiment, according to Adsorption thermodynamics data fitting result, absorption more meets Langmuir mould
Type (as shown in Figure 3) has respectively reached 47.48,59.12 Hes in highest adsorption capacity of 288, the 298 and 308K to lithium ion
68.92mg/g。
P-HFTO-NF and P-HZTO-NF adsorbent prepared by embodiment 2 and 3 is in 298K (25 DEG C) to the highest of lithium ion
Adsorption capacity has respectively reached 53.27mg/g and 54.83mg/g.
(2) lithium ion selective absorption is tested
1g lithium ion sieve adsorbant (P-HTO-NF, P-HFTO-NF and P-HZTO-NF of Examples 1 to 3 preparation) is added
In the water for being 1L to volume, Li in water+=40mg/L, Na+=753mg/L, K+=928mg/L, Mg2+=4288mg/L, pH=
10, reaction 30min is stirred at room temperature, reaction is completed, and adsorbent is separated by filtration, and detects each ion concentration in water.With the absorption of ion
Equilibrium distribution coefficient (Kd=(Co-Ce)V/CeM) adsorbent is evaluated to the adsorption capacity of ion, KdBigger expression adsorbent is to this
The selective adsorption capacity of ion is stronger.
The lithium ion K of the adsorbent P-HTO-NF (preparation of embodiment 1)dFor 360mL/g, potassium ion KdFor 1.6mL/g,
The K of sodium iondFor 0.66mL/g, the K of magnesium iondFor 0.33mL/g.From adsorbent P-HTO-NF known to above data to lithium ion
KdValue is far longer than other ions, shows that P-HTO-NF adsorbent has very high selective absorption to lithium ion.
The lithium ion K of the adsorbent P-HFTO-NF (preparation of embodiment 2)dFor 351mL/g, potassium ion KdFor 1.9mL/g,
The K of sodium iondFor 0.82mL/g, the K of magnesium iondFor 0.69mL/g.Known to the above data adsorbent P-HFTO-NF to lithium from
Sub- KdValue is far longer than other ions, shows that P-HFTO-NF adsorbent has very high selective absorption to lithium ion.
The lithium ion K of the adsorbent P-HZTO-NF (preparation of embodiment 3)dFor 354mL/g, potassium ion KdFor 1.78mL/
G, the K of sodium iondFor 0.73mL/g, the K of magnesium iondFor 0.52mL/g.From adsorbent P-HZTO-NF known to above data to lithium
Ion KdValue is far longer than other ions, shows that P-HZTO-NF adsorbent has very high selective absorption to lithium ion
The test of 5 cycle performance of embodiment
P-HTO-NF adsorbent (preparation of embodiment 1) and synthesis in solid state titanium-based lithium ion adsorbent (HTO) inhale lithium ion
Attached recycling performance experiment
Using synthesis in solid state spinel-type Li4Ti5O12Nano particle (200nm or so), 1g Li4Ti5O12Use 200mL
0.2M hydrochloric acid vibrates immersion 5h at room temperature and obtains titanium-based lithium ion adsorbent (HTO).
1g adsorbent is added in the water that volume is 1L, Li in water+Reaction is stirred at room temperature in=1000mg/L, pH=10
30min, reaction are completed, and adsorbent is separated by filtration, and detect lithium concentration in water.Adsorbent is calculated to the adsorption capacity of lithium ion
=(Co-Ce)V/m.The adsorbent separated is placed in 100mL 0.2M hydrochloric acid, stirs 1h, is then separated by filtration washing and obtains again
Raw adsorbent.Regenerated adsorbent is reused for lithium ion absorption, and reaction condition and adsorbent reactivation condition are the same as the first time.It inhales
Attached experiment is repeated 6 times.
First time adsorption experiment, P-HTO-NF adsorbent are 59.12mg/g to the adsorption capacity of lithium；6th absorption is real
It tests, P-HTO-NF adsorbent is 54.26mg/g to the adsorption capacity of lithium, and compared to for the first time, adsorption capacity only declines 8.2%.
First time adsorption experiment, HTO adsorbent are 33.54mg/g to the adsorption capacity of lithium；6th adsorption experiment, HTO
Adsorbent is 26.07mg/g to the adsorption capacity of lithium, and compared to for the first time, adsorption capacity has dropped 22.3%.
Contrast and experiment shows: porous fibrous P-HTO-NF adsorbent synthesizes titanium-based lithium ion than conventional solid
(HTO) adsorbent, it is more preferable to lithium ion absorption Repeatability.It adsorbs for the first time, the former is higher by 70% than the latter adsorption capacity；The
Six absorption, the former is higher by 108% than the latter adsorption capacity.P-HTO-NF adsorbent is to the higher reason of lithium ion adsorption capacity
Be: P-HTO-NF is porous structure, and adsorption site exposure is more；P-HTO-NF adsorbent is better to lithium ion absorption repeatability
The reason is that: P-HTO-NF is porous structure, and lithium ion elution is more abundant in each hypo acid processing, and adsorption site recovery rate is higher.
Claims (9)
1. a kind of preparation method of lithium ion sieve adsorbant, comprising the following steps:
1) pore-foaming agent, lithium salts, assistant metal salt are placed in solvent, after being stirred, butyl titanate is added, continues stirring extremely
Solution mixing is uniform, obtains spinning solution；
2) spinning solution in step 1) is placed in the solution storage device of electrostatic spinning machine, sets the technique ginseng of electrostatic spinning
Number, then carries out electrospinning, obtains nanofiber；
3) it by after the nanofiber drying in step 2), is calcined in air atmosphere, after calcining, obtains lithium ion sieve
Presoma；
4) the lithium ion sieve presoma in step 3) is stirred to react in mineral acid, after completion of the reaction, obtains lithium ion
Sieve adsorbant.
2. a kind of preparation method of lithium ion sieve adsorbant according to claim 1, which is characterized in that the step 1)
In, pore-foaming agent is one of polyvinylpyrrolidone, polyethylene oxide, polylactide, polyacrylonitrile, polyvinyl alcohol；Lithium salts
For LiAc；Assistant metal salt is FeAc2、ZrOCl2One of；The matter of pore-foaming agent, lithium salts, assistant metal salt and butyl titanate
Amount is than being 7:(2~10): (0~6): (20~50).
3. a kind of preparation method of lithium ion sieve adsorbant according to claim 1 or 2, which is characterized in that the step
1) in, the volume ratio of the mixed solvent of mixed solvent EtOH, HAc, DMF composition, three is (50~100): (10~50):
(15~60)；The mass volume ratio of the pore-foaming agent and mixed solvent is 7:(90~110) g/mL.
4. a kind of preparation method of lithium ion sieve adsorbant according to claim 1, which is characterized in that the step 2)
In, the technological parameter of electrospinning are as follows: 3~15kV of voltage.
5. a kind of preparation method of lithium ion sieve adsorbant according to claim 1, which is characterized in that the step 3)
In, calcination temperature is 550~750 DEG C, and calcination time is 3~5h.
6. a kind of preparation method of lithium ion sieve adsorbant according to claim 1, which is characterized in that the step 4)
In, being stirred to react the time is 0.5~1.5h.
7. a kind of preparation method of lithium ion sieve adsorbant according to claim 1 be prepared lithium ion sieve presoma and
Lithium ion sieve adsorbant.
8. lithium ion sieve presoma according to claim 7 and lithium ion sieve adsorbant, which is characterized in that the lithium ion
Sieving presoma and lithium ion sieve adsorbant has porous nano-fibre structure.
9. the method for lithium ion sieve adsorbant absorption lithium ion according to claim 8 or claim 9, comprising the following steps: adjusting contains
Adsorbent, is then added in lithium-containing solution by the pH to 6~12 of lithium solution, followed by being stirred to react absorption lithium ion,
After absorption, it is separated by filtration adsorbent, after then impregnating desorption lithium ion in acid, obtains regeneration lithium ion sieve adsorbant,
Complete a sorption cycle.
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| CN112490410A (en) * | 2020-11-26 | 2021-03-12 | 宁波大学 | PEO-TiO for inhibiting growth of lithium dendrite2Composite film material and preparation method thereof |
| CN114288983A (en) * | 2021-11-29 | 2022-04-08 | 台州闪能科技有限公司 | Titanium-based lithium ion exchanger and preparation method thereof |
| WO2022134221A1 (en) * | 2020-12-22 | 2022-06-30 | 天津科技大学 | Preparation method for porous spinning composite material, and application thereof in lithium extraction |
| CN115069208A (en) * | 2022-06-07 | 2022-09-20 | 四川大学 | Porous fiber bundle-shaped titanium lithium adsorbent and preparation method thereof |
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| CN112490410A (en) * | 2020-11-26 | 2021-03-12 | 宁波大学 | PEO-TiO for inhibiting growth of lithium dendrite2Composite film material and preparation method thereof |
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| CN115069208A (en) * | 2022-06-07 | 2022-09-20 | 四川大学 | Porous fiber bundle-shaped titanium lithium adsorbent and preparation method thereof |
| CN115069208B (en) * | 2022-06-07 | 2023-11-17 | 四川大学 | Porous fiber bundle-shaped titanium-based lithium adsorbent and preparation method thereof |
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