CN110090614B - Preparation method of lithium ion sieve adsorbent, product and application thereof - Google Patents
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Abstract
The invention discloses a preparation method of a lithium ion sieve adsorbent, a product and an application thereof, wherein the preparation method comprises the following steps: placing a pore-foaming agent, a lithium salt and an auxiliary metal salt in a solvent, stirring and mixing, adding tetrabutyl titanate, and continuously stirring until the solution is uniformly mixed to obtain a spinning solution; placing the spinning solution in a solution storage device of an electrostatic spinning machine, setting technological parameters of electrostatic spinning, and then carrying out electrospinning to obtain nanofibers; drying the nano-fiber, calcining in an air atmosphere, and obtaining a lithium ion sieve precursor after calcining is finished; and (3) stirring the lithium ion sieve precursor in an inorganic acid for reaction, and obtaining the lithium ion sieve adsorbent after the reaction is finished. The porous nano fibrous lithium ion sieve adsorbent prepared by the invention has very large specific surface area, increases the contact area of the adsorbent and a solution, and can improve the adsorption capacity of the adsorbent to lithium ions. The porous fibrous lithium ion sieve has an ion sieve structure as a whole and has high adsorption selectivity to lithium ions.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a lithium ion sieve adsorbent, and a product and application thereof.
Background
With the rapid development of clean energy, the demand of lithium is increasing. The process for extracting lithium from lithium ore is complex and high in cost. Lithium-containing salt lake water is an important lithium source, however, the salt lake water contains high-concentration ions such as sodium, magnesium, potassium and the like. The traditional methods such as solvent extraction, ion exchange, precipitation, membrane separation and the like are difficult to separate lithium with high selectivity. The lithium ion sieve can effectively adsorb and separate lithium ions with high selectivity. The manganese-based lithium ion sieve is commonly used, but the manganese-based lithium ion sieve has the phenomenon of manganese dissolution loss, particularly the phenomenon that the manganese dissolution loss is more serious in an acid environment, the crystal structure is damaged, the adsorption selectivity of the lithium ion is reduced, the stability of cycle application is poor, and the adsorption capacity of the lithium ion is reduced. Compared with a manganese-based lithium ion sieve, the titanium-based lithium ion sieve has higher chemical stability. The titanium-based lithium ion sieve prepared by the traditional solid phase synthesis method is fine particles, and is easy to aggregate in water, so that the adsorption capacity of the titanium-based lithium ion sieve on lithium ions is greatly reduced. Although some carriers (including carbon materials and polymer nano fibers) are used for supporting the ion sieve particles, the use of the carriers enables diffusion of lithium ions to be hindered and partial adsorption sites to be covered, and the lithium ion adsorption efficiency is low. Heretofore, porous fibrous lithium ion sieves have not been reported. The porous fibrous lithium ion sieve has an ion sieve structure as a whole, and has the advantages of high lithium ion diffusion rate, high adsorption capacity and high selectivity.
Disclosure of Invention
The invention aims to provide a preparation method of a lithium ion sieve adsorbent with high adsorption capacity, high selectivity and stable performance, and a product and application thereof.
The preparation method of the lithium ion sieve adsorbent comprises the following steps:
1) placing a pore-foaming agent, a lithium salt and an auxiliary metal salt in a mixed solvent, stirring and mixing, adding butyl titanate, and continuously stirring until the solution is uniformly mixed to obtain a spinning solution;
2) placing the spinning solution obtained in the step 1) in a solution storage device of an electrostatic spinning machine, setting technological parameters of electrostatic spinning, and then carrying out electrospinning to obtain nanofibers;
3) drying the nanofibers obtained in the step 2), calcining the dried nanofibers in the air atmosphere, and obtaining a lithium ion sieve precursor (P-LXTO-NF) after the calcination is finished;
4) stirring the lithium ion sieve precursor in the step 3) in an inorganic acid for reaction to obtain a lithium ion sieve adsorbent (P-HXTO-NF).
P in the simple formulas P-LXTO-NF and P-HXTO-NF represents a porous structure, L represents lithium, X represents an auxiliary metal, T represents titanium, O represents oxygen, and NF represents nano-fibers.
The pore-foaming agent in the step 1) is one of polyvinylpyrrolidone (PVP), polyethylene oxide (PEO), Polylactide (PLA), Polyacrylonitrile (PAN) and polyvinyl alcohol (PVA); the lithium salt is LiAc; the auxiliary metal salt is FeAc2、ZrOCl2One of (1); the mass ratio of the pore-foaming agent to the lithium salt to the auxiliary metal salt to the tetrabutyl titanate is 7 (2-10) to (0-6) to (20-50); the mixed solvent consists of EtOH, HAc and DMF, and the volume ratio of the EtOH, the HAc and the DMF is (50-100): 10-50): 15-60); the mass volume ratio of the pore-foaming agent to the mixed solvent is 7 (90-110) g/ml.
In the step 2), the electrospinning process parameters are as follows: the voltage is 3-15 kV.
In the step 3), the calcining temperature is 550-750 ℃, and the calcining time is 3-5 h.
In the step 4), the stirring reaction time is 0.5-1.5 h.
The lithium ion sieve precursor (P-LXTO-NF) and the lithium ion sieve adsorbent (P-HXTO-NF) are prepared according to the preparation method, wherein X is F, Z or not, and F represents Fe2O3Z represents ZrO2。
The lithium ion sieve precursor and the lithium ion sieve adsorbent have porous nanofiber structures.
The method for adsorbing lithium ions by the lithium ion sieve comprises the following steps: adjusting the pH value of the lithium-containing solution to 6-12, adding an adsorbent into the lithium-containing solution, stirring for reaction to adsorb lithium ions, filtering and separating the adsorbent after adsorption is finished, soaking in acid to desorb the lithium ions to obtain a regenerated lithium ion adsorbent, and completing one adsorption cycle.
The invention has the beneficial effects that: 1) the lithium ion sieve adsorbent prepared by the invention is a porous nanofiber, the specific surface area of the adsorbent is larger due to the structure of the nanofiber, and the specific surface area of the adsorbent is very large due to the microporous structure on the fiber, so that the connection between the adsorbent and a solution is greatly increasedThe contact area can greatly improve the adsorption effect of the lithium ion adsorbent. 2) The lithium ion sieve adsorbent has high adsorption capacity to lithium, so that the lithium ion sieve adsorbent has high selective adsorption to lithium in water containing lithium, sodium, potassium and magnesium ions, and the thermodynamic adsorption capacity to lithium is as high as 59.12mg/g by taking P-HTO-NF in example 1 as an example; even if the concentrations of potassium (928mg/L), sodium (753mg/L) and magnesium (4288mg/L) ions in water are far higher than that of lithium ions (40mg/L), the adsorption equilibrium partition coefficient (360mL/g) of the lithium ions is far higher than that of the potassium ions (1.6mL/g), the sodium ions (0.66mL/g) and the magnesium ions (0.33mL/g), and the lithium ion adsorption selectivity is very high. 3) The adsorbent can be recycled for multiple times, and the cost can be effectively reduced. In addition, compared with the traditional lithium ion sieve adsorbent synthesized by a solid phase, the porous lithium ion sieve adsorbent has higher lithium ion adsorption capacity and more excellent reusability. 4) The invention dopes Fe in the titanium-based lithium ion sieve2O3Magnetic separation of the adsorbent is facilitated; doping ZrO in titanium-based lithium ion sieve2Is favorable for improving the chemical stability of the molecular sieve.
Drawings
FIG. 1 is a scanning electron micrograph of P-LTO-NF (a1), P-LFTO-NF (b1) and P-LZTO-NF (c1) prepared in examples 1 to 3; TEM images of P-LTO-NF (a2), P-LFTO-NF (b2), P-LZTO-NF (c 2); high resolution TEM images of P-LTO-NF (a3), P-LFTO-NF (b3), P-LZTO-NF (c 3).
FIG. 2 XRD patterns of P-LTO-NF (a), P-LFTO-NF (b), and P-LZTO-NF (c) prepared in examples 1 to 3.
FIG. 3 thermodynamic diagram of P-HTO-NF vs. Li-ion adsorption prepared in example 1.
Detailed Description
Example 1
(1) Porous nanofibrous Li4Ti5O12(P-LTO-NF) preparation
7g of a porogen (PVP), 5g of a lithium salt (LiAc) and 105mL of a mixed solvent (80mL of EtOH,10mLHAc and 15mLDMF) were mixed, followed by stirring at room temperature for 1 h; then, 25g of butyl titanate (TBOT) was added thereto, followed by further stirring at room temperature for 2 hours to obtain a spinning solution. And (3) putting the electrospinning solution into a solution loading device of an electrostatic spinning machine, setting the electrospinning voltage to be 14kV, and then carrying out electrospinning to obtain the nanofiber membrane.
And (3) drying the nanofiber membrane at room temperature, and calcining the nanofiber membrane for 3h at 650 ℃ in an air environment to obtain a porous nano fibrous titanium-based lithium ion sieve precursor (P-LTO-NF).
(2) Lithium ion sieve adsorbent H4Ti5O12(P-HTO-NF) preparation
Adding 1g P-LTO-NF into 100mL of 0.2M hydrochloric acid, stirring for 1H, and drying the solid at room temperature to obtain H4Ti5O12(P-HTO-NF) adsorbent.
The P-LTO-NF prepared in this example was subjected to SEM and TEM tests, and the results are shown as a1, a2 and a3 in FIG. 1. From a1, P-LTO-NF was fibrous and had rough fiber surface, and the average diameter of the fiber was about 400 nm; as can be seen from a2, a porous structure exists on the P-LTO-NF fiber; it can be derived from a3 that the channel has a diameter of 0.48nm, which corresponds exactly to the spinel Li4Ti5O12The 111 crystal plane of (1).
XRD testing was performed on P-LTO-NF prepared in this example, and the results are shown in FIG. 2 (a): characteristic peak of P-LTO-NF atlas and highly crystalline Li4Ti5O12The spinel structure is fully satisfactory.
Example 2
(1) Porous nanofibrous Li4Ti5O12-Fe2O3(P-LFTO-NF) production
7g porogen (PVP), 5g lithium salt (LiAc), 5g iron salt (FeAc)2) And 105mL of a mixed solvent (80mL of EtOH,10mLHAc, and 15mLDMF), followed by stirring at room temperature for 1 h; then, 25g of butyl titanate (TBOT) was added thereto, followed by further stirring at room temperature for 2 hours to obtain a spinning solution. And (3) putting the spinning solution into a solution loading device of an electrostatic spinning machine, setting the voltage of electrospinning to be 14kV, and then carrying out electrospinning to obtain the nanofiber.
And (3) drying the nano-fiber at room temperature, and calcining the nano-fiber at 650 ℃ for 3h in an air environment to obtain a porous nano-fibrous titanium-based lithium ion sieve precursor (P-LFTO-NF).
(2) Lithium ion sieve adsorbent H4Ti5O12(P-HFTO-NF) production
Adding 1g P-LFTO-NF into 100mL of 0.2M hydrochloric acid, stirring for 1H, and drying the solid at room temperature to obtain H4Ti5O12(P-HFTO-NF) adsorbent.
The P-LFTO-NF prepared in this example was tested by SEM and TEM, and the results are shown as b1, b2 and b3 in FIG. 1. From b1, P-LFTO-NF was fibrous and had rough fiber surface with an average fiber diameter of about 300 nm; as can be seen from b2, a porous structure exists on the P-LFTO-NF fiber; from b3, it can be seen that the channels are 0.48nm, which corresponds exactly to spinel Li4Ti5O12The 111 crystal plane of (1).
XRD testing was performed on P-LFTO-NF prepared in this example, and the results are shown in FIG. 2 (b): characteristic peak of P-LFTO-NF atlas not only contains highly crystalline Li4Ti5O12Spinel structure, also including Fe2O3And (4) a characteristic peak of the crystalline state of the maghemite.
Introduction of Fe into lithium ion sieve adsorbent2O3Magnetic separation of the adsorbent can be achieved.
Example 3
(1) Porous nanofibrous Li4Ti5O12-ZrO2(P-LZTO-NF) production
7g of porogen (PVP), 5g of lithium salt (LiAc), 5g of zirconium salt (ZrOCl)2) And 105mL of a mixed solvent (80mL of EtOH,10mL of HAc and 15mL of DMF), followed by stirring at room temperature for 1 h; then 25g of butyl titanate was added, and then stirring was continued at room temperature for 2 hours to obtain a spinning solution. And (3) putting the spinning solution into a solution loading device of an electrostatic spinning machine, setting the voltage of electrospinning to be 14kV, and then carrying out electrospinning to obtain the nanofiber.
And (3) drying the nano-fiber at room temperature, and calcining the nano-fiber at 650 ℃ for 3h in an air environment to obtain a porous nano-fibrous titanium-based lithium ion sieve precursor (P-LZTO-NF).
(2) Lithium ion sieve adsorbent H4Ti5O12-ZrO2(P-HZTO-NF) production
1g P-LFTO-NF was put into 100mL of 0.2M hydrochloric acid and stirred for 1h, and the solid was isolatedDrying at room temperature to obtain H4Ti5O12(P-HFTO-NF) adsorbent.
The P-LZTO-NF prepared in this example was subjected to SEM and TEM tests, and the results are shown as c1, c2 and c3 in FIG. 1. From b1, P-LZTO-NF was fibrous and had a rough fiber surface, and the average fiber diameter was about 250 nm; as can be seen from c2, a porous structure exists on the P-LZTO-NF fiber; from c3, it can be seen that the channel diameter is 0.48nm, which corresponds exactly to Li4Ti5O12The 111 crystal plane of (1).
XRD testing was performed on P-LZTO-NF prepared in this example, and the results are shown in FIG. 2 (c): characteristic peak of P-LZTO-NF atlas not only contains highly crystalline Li4Ti5O12Spinel structure, also including ZrO2Characteristic peak of tetragonal crystal.
Example 4 adsorption Performance testing
(1) Lithium ion adsorption experiment
1g of lithium ion sieve adsorbent (P-HTO-NF, P-HFTO-NF and P-HZTO-NF prepared in examples 1 to 3) was added to 1L of water containing Li+Stirring at room temperature for 2h under the conditions of 25-1000 mg/L and pH 10, completing the reaction, filtering and separating the adsorbent, and detecting the concentration of each ion in water. Adsorption capacity Q of the adsorbent to lithium ionse＝(Co-Ce)V/m，QeA larger size indicates a stronger adsorption capacity of the adsorbent for the ion.
The adsorbent P-HTO-NF in example 1 is matched with adsorption thermodynamic data, adsorption is more consistent with a Langmuir model (shown in figure 3), and the highest adsorption capacities of 288, 298 and 308K on lithium ions respectively reach 47.48, 59.12 and 68.92 mg/g.
The highest adsorption capacities of the P-HFTO-NF and P-HZTO-NF adsorbents prepared in examples 2 and 3 to lithium ions at 298K (25 ℃) were 53.27mg/g and 54.83mg/g, respectively.
(2) Selective adsorption experiment of lithium ion
1g of lithium ion sieve adsorbent (P-HTO-NF, P-HFTO-NF and P-HZTO-NF prepared in examples 1 to 3) was added to 1L of water containing Li+＝40mg/L,Na+＝753mg/L,K+＝928mg/L,Mg2+4288mg/L, pH 10, stirring at room temperature for 30min, filtering to separate the adsorbent, and detecting the ion concentration in water. Equilibrium partition coefficient (K) by adsorption of ionsd＝(Co-Ce)V/Cem) to evaluate the adsorption capacity of the adsorbent for ions, KdA larger size indicates a stronger selective adsorption capacity of the adsorbent for the ion.
Lithium ion K of the adsorbent P-HTO-NF (prepared in example 1)dIs 360mL/g, potassium ion Kd1.6mL/g, K of sodium iond0.66mL/g, K of magnesium iondIt was 0.33 mL/g. From the above data, the adsorbent P-HTO-NF can be used for the lithium ion KdThe value is far greater than that of other ions, and the P-HTO-NF adsorbent has high selective adsorption on lithium ions.
Lithium ion K of the adsorbent P-HFTO-NF (prepared in example 2)d351mL/g, potassium ion Kd1.9mL/g, K of sodium iond0.82mL/g, K of magnesium iondIt was 0.69 mL/g. From the above data, the P-HFTO-NF adsorbent was found to be responsible for the lithium ion KdThe value is far greater than other ions, and the P-HFTO-NF adsorbent has high selective adsorption on lithium ions.
Lithium ion K of the adsorbent P-HZTO-NF (prepared in example 3)d354mL/g, potassium ion Kd1.78mL/g, K of sodium iond0.73mL/g, K of magnesium iondIt was 0.52 mL/g. From the above data, it can be seen that the adsorbent P-HZTO-NF is responsible for the lithium ion KdThe value is far greater than that of other ions, and the P-HZTO-NF adsorbent has high selective adsorption on lithium ions
Example 5 cycle performance test
Lithium ion adsorption recycle performance experiment of P-HTO-NF adsorbent (prepared in example 1) and solid-phase synthesis titanium-based lithium ion adsorbent (HTO)
Synthesis of spinel type Li by solid phase4Ti5O12Nanoparticles (around 200 nm), 1g Li4Ti5O12The titanium-based lithium ion adsorbent (HTO) is obtained by shaking and soaking 200mL of 0.2M hydrochloric acid at room temperature for 5 h.
1g of the adsorbent was added to 1L of water, Li in water+Stirring at 1000mg/L and pH 10 for reaction at room temperature for 30min, filtering to separate the adsorbent, and detecting the lithium ion concentration in water. The adsorption capacity of the adsorbent for lithium ions was calculated as (C)o-Ce) V/m. The separated adsorbent is placed in 100mL of 0.2M hydrochloric acid, stirred for 1h, and then filtered, separated and washed with water to obtain the regenerated adsorbent. The regenerated adsorbent is reused for lithium ion adsorption, and the reaction conditions and the adsorbent regeneration conditions are the same as those of the first time. The adsorption experiment was repeated 6 times.
In the first adsorption experiment, the adsorption capacity of the P-HTO-NF adsorbent to lithium is 59.12 mg/g; in the sixth adsorption experiment, the adsorption capacity of the P-HTO-NF adsorbent to lithium is 54.26mg/g, which is only reduced by 8.2% compared with that of the first adsorption experiment.
In the first adsorption experiment, the adsorption capacity of the HTO adsorbent to lithium is 33.54 mg/g; in the sixth adsorption experiment, the adsorption capacity of the HTO adsorbent to lithium was 26.07mg/g, which was 22.3% lower than that in the first adsorption experiment.
The results of the comparative experiment show that: compared with the traditional solid-phase synthesis titanium-based lithium ion (HTO) adsorbent, the porous fibrous P-HTO-NF adsorbent has better repeated performance on lithium ion adsorption. The first adsorption, the former has 70% higher adsorption capacity than the latter; and in the sixth adsorption, the adsorption capacity of the former is 108 percent higher than that of the latter. The reason why the P-HTO-NF adsorbent has a higher adsorption capacity for lithium ions is that: the P-HTO-NF is of a porous structure, and adsorption sites are more exposed; the reason why the P-HTO-NF adsorbent has better repeatability on the adsorption of lithium ions is that: the P-HTO-NF is a porous structure, lithium ions are more sufficiently eluted in each acid treatment, and the recovery rate of adsorption sites is higher.
Claims (4)
1. A preparation method of a lithium ion sieve adsorbent comprises the following steps:
1) placing a pore-foaming agent, a lithium salt and an auxiliary metal salt in a solvent, stirring and mixing, adding tetrabutyl titanate, and continuously stirring until the solution is uniformly mixed to obtain a spinning solution;
2) placing the spinning solution obtained in the step 1) in a solution storage device of an electrostatic spinning machine, setting technological parameters of electrostatic spinning, and then carrying out electrospinning to obtain nanofibers;
3) drying the nanofibers obtained in the step 2), calcining the dried nanofibers in the air atmosphere, and obtaining a lithium ion sieve precursor after calcining is finished;
4) stirring the lithium ion sieve precursor in the step 3) in an inorganic acid for reaction to obtain a lithium ion sieve adsorbent after the reaction is finished;
in the step 1), the pore-foaming agent is one of polyvinylpyrrolidone, polyethylene oxide, polylactide, polyacrylonitrile and polyvinyl alcohol; the lithium salt is LiAc; the auxiliary metal salt is FeAc2、ZrOCl2One of (1); the mass ratio of the pore-foaming agent to the lithium salt to the auxiliary metal salt to the tetrabutyl titanate is 7 (2-10) to (0-6) to (20-50);
in the step 1), the solvent is a mixed solvent consisting of EtOH, HAc and DMF, and the volume ratio of the EtOH, HAc and DMF is (50-100): 10-50): 15-60; the mass-volume ratio of the pore-foaming agent to the mixed solvent is 7 (90-110) g/mL;
in the step 2), the electrospinning process parameters are as follows: the voltage is 3-15 kV;
in the step 3), the calcining temperature is 550-750 ℃, and the calcining time is 3-5 h.
2. The preparation method of the lithium ion sieve adsorbent according to claim 1, wherein in the step 4), the stirring reaction time is 0.5-1.5 h.
3. The lithium ion sieve adsorbent prepared by the preparation method of the lithium ion sieve adsorbent according to claim 1, wherein the lithium ion sieve adsorbent has a porous nanofiber structure.
4. The method for adsorbing lithium ions by using the lithium ion sieve adsorbent according to claim 3, comprising the steps of: adjusting the pH value of a lithium-containing solution to 6-12, adding the lithium ion sieve adsorbent into the lithium-containing solution, stirring to react to adsorb lithium ions, filtering and separating the lithium ion sieve adsorbent after adsorption is finished, soaking in acid to desorb the lithium ions to obtain a regenerated lithium ion sieve adsorbent, and finishing one adsorption cycle.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8765278B2 (en) * | 2009-09-10 | 2014-07-01 | Battelle Memorial Institute | High-energy metal air batteries |
| CN105375018A (en) * | 2015-10-23 | 2016-03-02 | 济南大学 | Preparation method of bead chain-shaped lithium titanate fiber and obtained product |
| CN108160023A (en) * | 2018-01-14 | 2018-06-15 | 天津市职业大学 | A kind of compound metantimonic acid lithium ion sieve filler and preparation method thereof |
| CN108212074A (en) * | 2016-12-12 | 2018-06-29 | 中国科学院过程工程研究所 | It is a kind of can the metatitanic acid type lithium ion sieve of Magnetic Isolation, preparation method and applications |
| CN109317087A (en) * | 2018-09-14 | 2019-02-12 | 成都理工大学 | A kind of doped titanic acid lithium adsorbent and preparation method thereof |
-
2019
- 2019-05-28 CN CN201910451148.XA patent/CN110090614B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8765278B2 (en) * | 2009-09-10 | 2014-07-01 | Battelle Memorial Institute | High-energy metal air batteries |
| CN105375018A (en) * | 2015-10-23 | 2016-03-02 | 济南大学 | Preparation method of bead chain-shaped lithium titanate fiber and obtained product |
| CN108212074A (en) * | 2016-12-12 | 2018-06-29 | 中国科学院过程工程研究所 | It is a kind of can the metatitanic acid type lithium ion sieve of Magnetic Isolation, preparation method and applications |
| CN108160023A (en) * | 2018-01-14 | 2018-06-15 | 天津市职业大学 | A kind of compound metantimonic acid lithium ion sieve filler and preparation method thereof |
| CN109317087A (en) * | 2018-09-14 | 2019-02-12 | 成都理工大学 | A kind of doped titanic acid lithium adsorbent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Continuous lithium mining from aqueous resources by an adsorbent filter with a 3D polymeric nanofiber network infused with ion sieves;Chung, Wook-Jin，et al;《CHEMICAL ENGINEERING JOURNAL》;20160929;第309卷;第49-62页 * |
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