CN114011386A - Preparation method of lithium adsorption particles - Google Patents
Preparation method of lithium adsorption particles Download PDFInfo
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- CN114011386A CN114011386A CN202111469475.1A CN202111469475A CN114011386A CN 114011386 A CN114011386 A CN 114011386A CN 202111469475 A CN202111469475 A CN 202111469475A CN 114011386 A CN114011386 A CN 114011386A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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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
- B01J20/04—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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- 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
- B01J20/28—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
- B01J20/28016—Particle form
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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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- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
The invention discloses a preparation method of lithium adsorption particles, which comprises the steps of mixing LiCl.2Al (OH)3·nH2Mixing and granulating O powder, dihydric alcohol, diisocyanate and the like, further mixing and granulating with an adhesive, and removing the solvent to obtain the lithium adsorption particles. The preparation method of some embodiments of the invention has simple operation, can obtain lithium adsorption particles, has more uniform particle distribution and more abundant pore channels, can quickly adsorb lithium ions in brine, and has relatively simple elution operation. In some embodiments of the invention, the diol and diisocyanate are reacted to form a mixture having a sparse monoThe polyurethane network with fixed hydrophilicity has more gaps in the middle, then the adhesive is further introduced to form an interpenetrating network, so that the brine is favorably introduced, and meanwhile, the double-interpenetrating network is easy to form a pore channel, so that the adsorption speed and the adsorption quantity of lithium are favorably improved.
Description
Technical Field
The invention relates to a new energy industry, in particular to a preparation method of lithium adsorption particles.
Background
To reduce CO2The emission, new energy and energy storage technologies are increasingly receiving attention and welcomed by people. Lithium is one of the key materials of new energy and energy storage technology, and is increasingly paid attention to by people in new energy materials.
Lithium carbonate is an important battery material, and statistical data shows that the expression consumption of lithium carbonate in 2020 of China exceeds 25 ten thousand tons, the self-supporting rate is about 30%, and as new energy is more and more valued, lithium becomes a strategic resource gradually. The main sources of lithium are lithium ore and salt lake brine. The extraction of lithium from lithium ore requires high-temperature calcination, which results in high energy consumption and high pollution, and thus the extraction of lithium from lithium ore is increasingly limited. The extraction of lithium from salt lake brine is relatively simple and has become the main route for producing lithium salt in the world.
The method for extracting lithium from salt lake brine mainly comprises an adsorption method, wherein Li in brine is adsorbed by ion exchange with high selectivity+And after elution, the lithium finished product is obtained through operations such as impurity removal and purification, and the method is simple in process, low in energy consumption and relatively environment-friendly. The aluminium-based adsorbent being relatively mature Li+An adsorbent. LiCl 2Al (OH)3·nH2O particles are a common lithium adsorbent, and the advantage of their performance directly determines their cost of use. LiCl 2Al (OH)3·nH2The O particles are generally prepared to obtain LiCl.2Al (OH)3·nH2And mixing the O powder with an organic polymer, and granulating. The organic polymer binder is a copolymer of vinylidene chloride, tetrachloroethylene and hexachloropropylene, or a polymer of vinyl chloride, polyvinyl chloride, vinylidene chloride and high vinyl chloride resins, or a copolymer of vinylidene chloride-vinyl chloride and vinyl chloride-vinyl acetate. The mixing granulation method comprises hot melt extrusion, binding with a binder and then removing the solvent for granulation. To obtain a better adsorption effect, LiCl 2Al (OH) in the particles is required3·nH2The O powder has sufficient contact area with the brine. However, in the existing preparation process, a thick glue layer is easily formed, so that partial pore channels are blocked or the resistance of the channels is high, which has adverse effect on the adsorption of lithium.
How to prepare lithium adsorption particles with high adsorption speed and high adsorption quantity is a very challenging task.
Disclosure of Invention
It is an object of the present invention to overcome at least one of the disadvantages of the prior art and to provide a method for preparing lithium-adsorbing particles.
The technical scheme adopted by the invention is as follows:
a method for preparing lithium-adsorbing particles, comprising the steps of:
mixing LiCl 2Al (OH)3·nH2Mixing O powder, dihydric alcohol, diisocyanate, a pore-foaming agent and a solvent uniformly, and granulating to obtain primary particles;
initiating the polymerization of dihydric alcohol and diisocyanate, and drying to obtain secondary particles;
and mixing the secondary particles with a polyethylene adhesive solution, performing secondary granulation, and removing the solvent and the pore-forming agent to obtain the lithium adsorption particles.
In some examples, LiCl 2Al (OH)3·nH2Molar amount of O powder calculated as Al, LiCl 2Al (OH)3·nH2The molar mixing ratio of the O powder, the dihydric alcohol and the diisocyanate is 100: (0.3-0.8): (0.2-0.4).
In some examples, the molar mixing ratio of the dihydric alcohol to the diisocyanate is (1.2-2.0): 1.
In some examples, the porogen is selected from at least one of sodium bicarbonate, ammonium bicarbonate.
In some examples, the solvent used to prepare the primary particles is water.
In some embodiments, the amount of water used does not exceed LiCl 2Al (OH)3·nH220% of the mass of the O powder.
In some examples, the mixing ratio of the secondary particles to the polyethylene-based binder is 100: (5-9).
In some examples, the polyvinyl binder is selected from at least one of a copolymer of vinylidene chloride with tetrachloroethylene, hexachloropropylene, or a polymer of vinyl chloride, polyvinyl chloride, vinylidene chloride, a high vinyl chloride resin, and a copolymer of vinylidene chloride-vinyl chloride, vinyl chloride-vinyl acetate.
In some examples, the primary particles have a particle size of 0.01 mm to 0.5 mm.
In some examples, the lithium-adsorbing particles have a particle size of 1mm to 10 mm.
The invention has the beneficial effects that:
the preparation method of some embodiments of the invention has simple operation, can obtain lithium adsorption particles, has more uniform particle distribution and more abundant pore channels, can quickly adsorb lithium ions in brine, and has relatively simple elution operation.
According to the preparation method of some embodiments of the invention, the dihydric alcohol and the diisocyanate react to form a sparse polyurethane network with certain hydrophilicity, a plurality of gaps are formed in the polyurethane network, then the adhesive is further introduced to form an interpenetrating network, so that the brine can be introduced conveniently, and meanwhile, the double-interpenetrating network is easy to form a pore channel, so that the adsorption speed and the adsorption quantity of lithium can be improved conveniently.
Detailed Description
A method for preparing lithium-adsorbing particles, comprising the steps of:
mixing LiCl 2Al (OH)3·nH2Mixing O powder, dihydric alcohol, diisocyanate, a pore-foaming agent and a solvent uniformly, and granulating to obtain primary particles;
initiating the polymerization of dihydric alcohol and diisocyanate, and drying to obtain secondary particles;
and mixing the secondary particles with a polyethylene adhesive solution, performing secondary granulation, and removing the solvent and the pore-forming agent to obtain the lithium adsorption particles.
The type of the dihydric alcohol is not particularly required, and the dihydric alcohol can be well dispersed in water or other solvents. The diol is preferably a C3-C6 chain diol, including but not limited to propylene glycol, butylene glycol, pentylene glycol, hexylene glycol, or a polymer thereof, such as PEG.
The polymerization of the diols and diisocyanates can be initiated according to the prior art. Such as heating, addition of initiators, etc.
The type of diisocyanate is not particularly limited, and it can be well dispersed in water or other solvents. Diisocyanates include, but are not limited to, Toluene Diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI), Hexamethylene Diisocyanate (HDI), Lysine Diisocyanate (LDI).
In some examples, LiCl 2Al (OH)3·nH2Molar amount of O powder calculated as Al, LiCl 2Al (OH)3·nH2The molar mixing ratio of the O powder, the dihydric alcohol and the diisocyanate is 100: 100: (0.3-0.8): (0.2-0.4).
In some examples, the molar mixing ratio of the dihydric alcohol to the diisocyanate is (1.2-2.0): 1. The excessive diol can well protect the isocyanate from completely reacting and simultaneously ensure that the formed network has certain hydrophilicity. Unreacted diol can be removed well by washing with water or the like without causing adverse effects.
In some examples, the porogen is selected from at least one of sodium bicarbonate, ammonium bicarbonate. These porogens can generate gas and fully form pores. Even if the amount of the lithium ion is excessive, water is easy to remove firstly, a corresponding pore channel is formed, and the specific surface area of the lithium adsorption particles is improved.
In some examples, the solvent used to prepare the primary particles is water. Thus, the cost is saved, and the use of organic solvent is avoided.
The amount of water is such that the raw materials are well dispersed and granulation is facilitated. In some embodiments, the amount of water used does not exceed LiCl 2Al (OH)3·nH220% of the mass of the O powder. In some cases, the amount can be further reduced to about LiCl 2Al (OH)3·nH215% or 10% or less of the mass of the O powder. The less water used, the more advantageous the drying.
In some examples, the mixing ratio of the secondary particles to the polyethylene-based binder is 100: (5-9).
In some examples, the polyvinyl binder is selected from at least one of a copolymer of vinylidene chloride with tetrachloroethylene, hexachloropropylene, or a polymer of vinyl chloride, polyvinyl chloride, vinylidene chloride, a high vinyl chloride resin, and a copolymer of vinylidene chloride-vinyl chloride, vinyl chloride-vinyl acetate.
In some examples, the primary particles have a particle size of 0.01 mm to 0.5 mm. The specific particle size can be adjusted accordingly as required.
In some examples, the lithium-adsorbing particles have a particle size of 1mm to 10 mm. The specific particle size can be adjusted accordingly as required.
The technical solution of the present invention is further illustrated below by referring to examples and experimental data.
For convenience of comparison, if not specifically stated, the diol used in the following examples is hexanediol, the diisocyanate is isophorone diisocyanate (IPDI), the porogen is ammonium bicarbonate, and the polyethylene binder is polyvinyl chloride. LiCl 2Al (OH)3·nH2The molar amount of the O powder is calculated by Al.
Example 1:
mixing LiCl 2Al (OH)3·nH2Uniformly mixing O powder, dihydric alcohol, diisocyanate, a pore-foaming agent and a proper amount of water, and granulating to obtain primary particles; wherein, LiCl 2Al (OH)3·nH2The molar mixing ratio of the O powder, the dihydric alcohol and the diisocyanate is 100: 0.3: 0.2 amount of pore-forming agent LiCl 2Al (OH)3·nH22% of the O powder by mass, the primary particles have a particle size of 0.01 mm-0.10 mm;
initiating the polymerization of dihydric alcohol and diisocyanate, and drying to obtain secondary particles;
mixing the secondary particles with a polyethylene adhesive solution, wherein the mass mixing ratio of the secondary particles to the polyethylene adhesive is 100: and 9, carrying out secondary granulation, and removing the solvent and the pore-foaming agent to obtain the lithium adsorption particles with the particle size of 1-3 mm.
Example 2:
mixing LiCl 2Al (OH)3·nH2Uniformly mixing O powder, dihydric alcohol, diisocyanate, a pore-foaming agent and a proper amount of water, and granulating to obtain primary particles; wherein, LiCl 2Al (OH)3·nH2O powderThe molar mixing ratio of the powder, the dihydric alcohol and the diisocyanate is 100: 0.8: 0.4 the amount of pore-forming agent LiCl 2Al (OH)3·nH24% of the O powder by mass, and the particle size of the primary particles is 0.10 mm-0.30 mm;
initiating the polymerization of dihydric alcohol and diisocyanate, and drying to obtain secondary particles;
mixing the secondary particles with a polyethylene adhesive solution, wherein the mass mixing ratio of the secondary particles to the polyethylene adhesive is 100: and 5, carrying out secondary granulation, and removing the solvent and the pore-foaming agent to obtain the lithium adsorption particles with the particle size of 4-7 mm.
Example 3:
mixing LiCl 2Al (OH)3·nH2Uniformly mixing O powder, dihydric alcohol, diisocyanate, a pore-foaming agent and a proper amount of water, and granulating to obtain primary particles; wherein, LiCl 2Al (OH)3·nH2The molar mixing ratio of the O powder, the dihydric alcohol and the diisocyanate is 100: 0.6: 0.4 the amount of pore-forming agent LiCl 2Al (OH)3·nH23.5 percent of the mass of the O powder, and the grain diameter of the primary particles is 0.30 mm-0.50 mm;
initiating the polymerization of dihydric alcohol and diisocyanate, and drying to obtain secondary particles;
mixing the secondary particles with a polyethylene adhesive solution, wherein the mass mixing ratio of the secondary particles to the polyethylene adhesive is 100: and 7, carrying out secondary granulation, and removing the solvent and the pore-foaming agent to obtain the lithium adsorption particles with the particle size of 5-10 mm.
Example 4:
mixing LiCl 2Al (OH)3·nH2Uniformly mixing O powder, dihydric alcohol, diisocyanate, a pore-foaming agent and a proper amount of water, and granulating to obtain primary particles; wherein, LiCl 2Al (OH)3·nH2The molar mixing ratio of the O powder, the dihydric alcohol and the diisocyanate is 100: 0.5: 0.3 the amount of pore-forming agent is LiCl 2Al (OH)3·nH24% of the O powder by mass, and the particle size of the primary particles is 0.10 mm-0.20 mm;
initiating the polymerization of dihydric alcohol and diisocyanate, and drying to obtain secondary particles;
mixing the secondary particles with a polyethylene adhesive solution, wherein the mass mixing ratio of the secondary particles to the polyethylene adhesive is 100: and 7, carrying out secondary granulation, and removing the solvent and the pore-foaming agent to obtain the lithium adsorption particles with the particle size of 3-6 mm.
Comparative example 1:
mixing LiCl 2Al (OH)3·nH2Mixing O powder with polyethylene binder solution, wherein the amount of polyethylene binder is LiCl 2Al (OH)3·nH2And (3) granulating 8% of the O powder by mass, and removing the solvent to obtain the lithium adsorption particles with the particle size of 1-3 mm.
And (3) performance detection:
the properties of the prepared lithium-adsorbing particulate material were examined, wherein the adsorption capacity of lithium was measured according to the method disclosed in CN106622103A, and the results are shown in table 1.
TABLE 1 lithium adsorption amounts of different lithium adsorbing particulate materials
| Numbering | Lithium adsorption amount/mg/g |
| Example 1 | 9.6±0.1 |
| Example 2 | 9.4±0.1 |
| Example 3 | 9.3±0.1 |
| Example 4 | 9.4±0.1 |
| Comparative example 1 | 8.6±0.1 |
After saturation adsorption, the adsorbed lithium ions were eluted, repeated several times, and the adsorption performance after several times of adsorption was tested, with the results shown in table 2.
TABLE 2 lithium adsorption capacity after multiple use of different lithium adsorbing particulate materials
As can be seen from the data in tables 1 and 2, the lithium adsorption particle material prepared by the method has good lithium adsorption capacity, and the loss of the adsorption performance after multiple use is small, and the performance is excellent.
Comparison of Water absorption:
100g of each of the dried lithium-adsorbing particulate materials was sufficiently soaked in purified water, and then the lithium-adsorbing particulate material was taken out, naturally drained, weighed, and the water absorption was calculated, and the results are shown in Table 3.
TABLE 3 Water uptake for different lithium-adsorbing particulate materials
| Numbering | Water absorption capacity/g/100 g |
| Example 1 | 14±0.3 |
| Example 2 | 18±0.4 |
| Example 3 | 16±0.3 |
| Example 4 | 16±0.4 |
| Comparative example 1 | 12±0.4 |
As can be seen from the data in table 3, the lithium-adsorbing particulate material of the embodiment of the present invention has better water absorption, which indicates that it has better hydrophilicity, and is more favorable for allowing brine to rapidly enter the interior of the particles, thereby reducing the time for saturated adsorption. Even a large lithium-adsorbing particulate material still has good lithium-adsorbing capacity.
The foregoing is a more detailed description of the invention and is not to be taken in a limiting sense. It will be apparent to those skilled in the art that simple deductions or substitutions without departing from the spirit of the invention are within the scope of the invention.
Claims (10)
1. A method for preparing lithium-adsorbing particles, comprising the steps of:
mixing LiCl 2Al (OH)3·nH2Mixing O powder, dihydric alcohol, diisocyanate, a pore-foaming agent and a solvent uniformly, and granulating to obtain primary particles;
initiating the polymerization of dihydric alcohol and diisocyanate, and drying to obtain secondary particles;
and mixing the secondary particles with a polyethylene adhesive solution, performing secondary granulation, and removing the solvent and the pore-forming agent to obtain the lithium adsorption particles.
2. The method of claim 1, wherein: LiCl 2Al (OH)3·nH2Molar amount of O powder calculated as Al, LiCl 2Al (OH)3·nH2The molar mixing ratio of the O powder, the dihydric alcohol and the diisocyanate is 100: (0.3-0.8): (0.2-0.4).
3. The method of claim 2, wherein: the molar mixing ratio of the dihydric alcohol to the diisocyanate is 1.2-2.0.
4. The method of claim 1, wherein: the pore-forming agent is selected from at least one of sodium bicarbonate and ammonium bicarbonate.
5. The method of claim 1, wherein: the solvent used to prepare the primary particles is water.
6. The method of claim 5, wherein: the amount of water is not more than LiCl 2Al (OH)3·nH220% of the mass of the O powder.
7. The production method according to any one of claims 1 to 6, characterized in that: the mixing ratio of the secondary particles to the polyethylene adhesive is 100: (5-9).
8. The production method according to any one of claims 1 to 6, characterized in that: the polyethylene adhesive is selected from at least one of a copolymer of vinylidene chloride, tetrachloroethylene and hexachloropropylene, or a polymer of vinyl chloride, polyvinyl chloride, vinylidene chloride and high vinyl chloride resin, and a copolymer of vinylidene chloride-vinyl chloride and vinyl chloride-vinyl acetate.
9. The production method according to any one of claims 1 to 6, characterized in that: the primary particles have a particle size of 0.01 mm to 0.5 mm.
10. The production method according to any one of claims 1 to 6, characterized in that: the particle size of the lithium adsorption particles is 1 mm-10 mm.
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