CN112808251A - Adsorbent for extracting lithium from salt lake and preparation method thereof - Google Patents

Adsorbent for extracting lithium from salt lake and preparation method thereof Download PDF

Info

Publication number
CN112808251A
CN112808251A CN202011620460.6A CN202011620460A CN112808251A CN 112808251 A CN112808251 A CN 112808251A CN 202011620460 A CN202011620460 A CN 202011620460A CN 112808251 A CN112808251 A CN 112808251A
Authority
CN
China
Prior art keywords
lithium
adsorbent
metatitanate
salt lake
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011620460.6A
Other languages
Chinese (zh)
Inventor
蔡建国
石洪雁
胡银龙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Helper Functional Materials Co ltd
Original Assignee
Jiangsu Helper Functional Materials Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Helper Functional Materials Co ltd filed Critical Jiangsu Helper Functional Materials Co ltd
Priority to CN202011620460.6A priority Critical patent/CN112808251A/en
Publication of CN112808251A publication Critical patent/CN112808251A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28095—Shape or type of pores, voids, channels, ducts
    • B01J20/28097—Shape or type of pores, voids, channels, ducts being coated, filled or plugged with specific compounds
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Materials Engineering (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

An adsorbent for extracting lithium from salt lake and a preparation method thereof, belonging to the technical field of raw material purification. The preparation method of the adsorbent for extracting lithium from the salt lake comprises the following steps: s1, adding lithium hydroxide into the titanium salt solution to prepare a lithium metatitanate precursor, and roasting the lithium metatitanate precursor to obtain lithium metatitanate powder; s2, mixing a polymer monomer, a cross-linking agent and a pore-foaming agent to obtain an oil phase solution, adding an initiator for reaction, and then adding lithium metatitanate powder to obtain a mixture; s3, adding a dispersing agent and NaCl into deionized water to prepare an aqueous phase solution; adding the water phase solution into the mixture prepared in the step S2, dispersing the oil phase into the water phase to form oil droplets, heating for reaction, and finally, cooling and washing to obtain the lithium metatitanate loaded adsorbent carrier; and S4, immersing the adsorbent carrier into an eluent to elute lithium ions, and then washing with deionized water to obtain the adsorbent for extracting lithium from the salt lake. The invention has good lithium ion adsorption selectivity and high adsorption capacity.

Description

Adsorbent for extracting lithium from salt lake and preparation method thereof
Technical Field
The invention relates to a technology in the field of raw material purification, in particular to an adsorbent for extracting lithium from a salt lake and a preparation method thereof.
Background
With the popularization of new energy electric vehicles, the demand for lithium ion batteries is continuously rising, and the price of lithium as a core material of the lithium ion battery is driven to rise. At present, the mainstream new energy electric automobile mainly uses a lithium ion battery as a driving battery. Lithium is an essential raw material (including a cathode material and an electrolyte) for producing a secondary lithium ion battery. Therefore, sufficient lithium resources are essential for the development of new energy electric automobile industry.
In view of the dispersibility of lithium resources, the change of the lithium resource structure and the cost advantage of lithium extraction from brine, the research and application of the lithium extraction technology at present are mainly applied to the aspect of lithium extraction from salt lake brine. The adsorption method can extract lithium from the salt lake brine with high magnesium-lithium ratio, thereby having good development prospect. The adsorbents can be classified into organic ion exchange adsorbents and inorganic ion exchange adsorbents according to their properties. The organic ion exchange resin has low selectivity to lithium, while the inorganic ion adsorbent has high selectivity to lithium, and can realize selective adsorption of lithium from dilute solution. Currently, the commonly used inorganic ion exchange adsorbents mainly include: amorphous hydroxide adsorbent, ion sieve type oxide adsorbent, layered adsorbent, composite antimonate adsorbent and aluminum salt adsorbent.
The Chinese invention patent application number 201410353274.9 discloses a method for extracting lithium from salt lake brine by an adsorption method, which comprises the following steps: adding an adsorbent into brine, and adsorbing lithium ions in the brine on the adsorbent; and (2) processing by a ceramic membrane, retaining the adsorbent in the concentrated solution, performing plate-and-frame filter pressing on the concentrated solution to obtain an adsorbent filter cake, removing most impurities and water in the brine, performing water washing and eluent desorption on the filter cake to obtain a desorption solution, removing magnesium in the desorption solution by the desorption solution through weak acid type cation exchange resin, and concentrating by a reverse osmosis membrane to obtain the refined lithium solution for preparing the lithium carbonate. The method has the advantages of simple process, easy operation, high utilization efficiency of the adsorbent, short lithium extraction process period and preparation of high-content refined lithium solution.
The Chinese invention patent application CN02145583.X discloses a method for extracting lithium from salt lake brine by an adsorption method, and the Chinese invention patent application CN201010290231.2 discloses a method for extracting lithium from salt lake brine by a resin adsorption method. However, in both of the above adsorption methods, the adsorbent is filled in the fixed bed adsorber, which results in a long adsorption period and a decrease in adsorption efficiency.
From the prior art, the currently synthesized lithium extraction adsorbent mainly has the problems of high production cost, high dissolution loss rate, low adsorption capacity, poor selectivity, long adsorption period and the like, and the large-scale application of the lithium extraction adsorbent in salt lake brine is also seriously influenced.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an adsorbent for extracting lithium from a salt lake and a preparation method thereof, and the adsorbent has good lithium ion adsorption selectivity and high adsorption capacity.
The invention relates to a preparation method of an adsorbent for extracting lithium from a salt lake, which comprises the following steps:
s1, adding lithium hydroxide into the titanium salt solution to enable the pH value of the solution to be 9-10, reacting for 2-3h at the temperature of 60-70 ℃, filtering, washing and drying to obtain a lithium metatitanate precursor; transferring the lithium metatitanate precursor to a muffle furnace, roasting for 2-3h under a certain temperature condition, and cooling to obtain lithium metatitanate powder;
s2, mixing a polymer monomer, a cross-linking agent and a pore-foaming agent according to a certain weight ratio to obtain an oil phase solution, then adding an initiator, stirring at room temperature until the initiator is completely dissolved, and then adding the lithium metatitanate powder prepared in the step S1 into the oil phase solution to obtain a mixture;
s3, adding a dispersing agent and a salting-out agent into deionized water, and stirring at room temperature until the dispersing agent and the salting-out agent are completely dissolved to obtain an aqueous phase solution; according to the weight ratio of the aqueous phase solution to the mixture of 1: 3-2: 3, adding the aqueous phase solution into the mixture prepared in the step S2, dispersing the oil phase into oil droplets with the particle size of 0.3-1.2mm in the aqueous phase by stirring, heating for reaction, and finally cooling and washing to obtain the adsorbent carrier loaded with lithium metatitanate;
s4, immersing the adsorbent carrier loaded with lithium metatitanate prepared in the step S3 into an eluent to enable lithium ions in the adsorbent carrier to be eluted out, and then cleaning the adsorbent carrier with deionized water to obtain the adsorbent for extracting lithium from the salt lake and the high-molecular-group titanium-based lithium ion sieve.
Preferably, in step S1, the feeding molar ratio of the titanium salt to the lithium hydroxide is controlled to be 1 (0.6-0.8); the titanium salt is at least one of titanium sulfate, titanyl sulfate, titanium tetrachloride and titanium nitrate; the concentration of titanium in the titanium salt solution is 1.0-2.5 mol/L.
Preferably, in step S1, the calcination temperature is 200-400 ℃, and the lithium metatitanate powder is Li4Ti5O12And/or Li2TiO3。
Preferably, in step S2, the polymer monomer is at least one of methyl acrylate, propyl acrylate, butyl acrylate, methyl methacrylate, propyl methacrylate, and butyl methacrylate; the cross-linking agent is at least one of divinylbenzene, allyl itaconate, diethylene glycol dimethacrylate, allyl methacrylate and allyl isocyanurate; the initiator is at least one of benzoyl peroxide and azobisisobutyronitrile; the pore-foaming agent is at least one of toluene, isooctane, aviation gasoline and n-heptane.
Further preferably, the weight ratio of the polymer monomer to the cross-linking agent is 1:3-3:1, the weight ratio of the polymer monomer to the cross-linking agent to the pore-forming agent is 2:1-1:2, and the addition amount of the initiator is 0.1% -2% of the weight of the oil phase solution.
Preferably, in step S3, the weight ratio of the dispersant is 0.5% -3.0%, and the weight ratio of NaCl is 5% -15%; the dispersant is at least one of polyvinyl alcohol, methylcellulose, hydroxyethyl cellulose and methyl hydroxypropyl cellulose.
In the step S3, the temperature-rising reaction comprises two stages, wherein the temperature rises to 50-70 ℃ in the first stage, and the reaction lasts for 2-6 h; in the second stage, the temperature is raised to 80-95 ℃ and the reaction lasts for 4-10 h.
Preferably, in step S4, the eluent is at least one of hydrochloric acid solution, sulfuric acid solution and nitric acid solution, the concentration of hydrogen ions in the eluent is 5-15 wt%, and the elution time is 1-10 h.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) hybridizing a titanium lithium ion sieve type oxide into a pore channel of a high polymer material by an in-situ polymerization method, and eluting lithium ions to prepare a lithium ion sieve for extracting lithium from salt lake brine for adsorption; the preparation process is simple and has no pollution to the environment;
2) when the method is applied to extracting lithium from salt lake brine, the lithium ion selectivity is good, the dissolution loss rate is low, the adsorption capacity is high, and the adsorption period is short.
Drawings
Fig. 1 is a process route diagram of an embodiment of the invention.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description. The experimental procedures, in which specific conditions are not specified in the examples, were carried out according to the conventional methods and conditions.
Example 1
As shown in FIG. 1, the procedure of this example for preparing the adsorbent for extracting lithium from salt lake is as follows:
firstly, preparing lithium metatitanate powder;
adding lithium hydroxide into 1mol/L titanyl sulfate solution to enable the pH value of the solution to be 9-10, reacting for 3 hours at 70 ℃, filtering, washing and drying to obtain a lithium metatitanate precursor; transferring the lithium metatitanate precursor to a muffle furnace, roasting for 2-3h at 300 ℃, and cooling to obtain lithium metatitanate powder;
secondly, preparing an adsorbent carrier loaded with lithium metatitanate;
1) adding 250ml of water, 10g of sodium chloride, 1.0g of dispersing agent gelatin and 0.2g of dispersing methyl hydroxypropyl cellulose into a 1L flask with a stirring and temperature control device, and stirring until the materials are completely dissolved to obtain an aqueous phase solution;
2) mixing 100g of polymer monomer butyl methacrylate, 200g of cross-linking agent divinylbenzene, 100g of cross-linking agent diethylene glycol dimethacrylate and 50g of pore-foaming agent toluene, and then adding 1g of initiator benzoyl peroxide and 1g of initiator azobisisobutyronitrile for reaction; then adding lithium metatitanate powder, and stirring until the lithium metatitanate powder is completely dissolved;
3) adding the aqueous phase solution into the solution obtained in the step 2), dispersing the oil phase into the aqueous phase by violent stirring to form oil droplets with the particle size of 0.3-1.2mm, and then carrying out heating reaction; firstly, controlling the reaction temperature to be 50-70 ℃ and reacting for 2-6 h; then, controlling the reaction temperature to be 80-95 ℃ and reacting for 4-10 h; finally, cooling and washing to obtain an adsorbent carrier loaded with lithium metatitanate;
thirdly, activating an adsorbent;
and (3) activating the adsorbent carrier by using hydrochloric acid with the concentration of 5 wt%, and completely eluting lithium ions in the adsorbent carrier to obtain a lithium extraction adsorbent A.
Example 2
As shown in FIG. 1, the procedure of this example for preparing the adsorbent for extracting lithium from salt lake is as follows:
firstly, preparing lithium metatitanate powder;
adding lithium hydroxide into a 1mol/L titanium nitrate solution to enable the pH value of the solution to be 9-10, reacting for 3 hours at 70 ℃, filtering, washing and drying to obtain a lithium metatitanate precursor; transferring the lithium metatitanate precursor to a muffle furnace, roasting for 2-3h at 300 ℃, and cooling to obtain lithium metatitanate powder;
secondly, preparing an adsorbent carrier loaded with lithium metatitanate;
1) adding 250ml of water, 10g of sodium chloride, 1.0g of dispersing agent gelatin and 0.2g of dispersing methyl hydroxypropyl cellulose into a 1L flask with a stirring and temperature control device, and stirring until the materials are completely dissolved to obtain an aqueous phase solution;
2) mixing 100g of polymer monomer butyl methacrylate, 200g of cross-linking agent divinylbenzene, 100g of cross-linking agent diethylene glycol dimethacrylate and 50g of pore-foaming agent toluene, and then adding 1g of initiator benzoyl peroxide and 1g of initiator azobisisobutyronitrile for reaction; then adding lithium metatitanate powder, and stirring until the lithium metatitanate powder is completely dissolved;
3) adding the aqueous phase solution into the solution obtained in the step 2), dispersing the oil phase into the aqueous phase by violent stirring to form oil droplets with the particle size of 0.3-1.2mm, and then carrying out heating reaction; firstly, controlling the reaction temperature to be 50-70 ℃ and reacting for 2-6 h; then, controlling the reaction temperature to be 80-95 ℃ and reacting for 4-10 h; finally, cooling and washing to obtain an adsorbent carrier loaded with lithium metatitanate;
thirdly, activating an adsorbent;
and (3) activating the adsorbent carrier by using hydrochloric acid with the concentration of 5 wt%, and completely eluting lithium ions in the adsorbent carrier to obtain a lithium extraction adsorbent B.
Example 3
As shown in FIG. 1, the procedure of this example for preparing the adsorbent for extracting lithium from salt lake is as follows:
firstly, preparing lithium metatitanate powder;
adding lithium hydroxide into a 1mol/L titanium nitrate solution to enable the pH value of the solution to be 9-10, reacting for 3 hours at 70 ℃, filtering, washing and drying to obtain a lithium metatitanate precursor; transferring the lithium metatitanate precursor to a muffle furnace, roasting for 2-3h at 300 ℃, and cooling to obtain lithium metatitanate powder;
secondly, preparing an adsorbent carrier loaded with lithium metatitanate;
1) adding 250ml of water, 10g of sodium chloride, 1.0g of dispersing agent gelatin and 0.2g of dispersing methyl hydroxypropyl cellulose into a 1L flask with a stirring and temperature control device;
2) mixing 100g of polymer monomer butyl methacrylate, 200g of cross-linking agent divinylbenzene, 100g of cross-linking agent diethylene glycol dimethacrylate and 50g of pore-foaming agent toluene, and then adding 1g of initiator benzoyl peroxide and 1g of initiator azobisisobutyronitrile for reaction; then adding lithium metatitanate powder, and stirring until the lithium metatitanate powder is completely dissolved;
3) adding the aqueous phase solution into the solution obtained in the step 2), dispersing the oil phase into the aqueous phase by violent stirring to form oil droplets with the particle size of 0.3-1.2mm, and then carrying out heating reaction; firstly, controlling the reaction temperature to be 50-70 ℃ and reacting for 2-6 h; then, controlling the reaction temperature to be 80-95 ℃ and reacting for 4-10 h; finally, cooling and washing to obtain an adsorbent carrier loaded with lithium metatitanate;
third, adsorbent activation
Activating the adsorbent carrier by using nitric acid with the concentration of 5 wt%, and completely eluting lithium ions in the adsorbent carrier to obtain a lithium extraction adsorbent C.
The performance tests of the lithium extraction adsorbents A, B and C prepared in examples 1-3 were carried out, and the brine raw material was taken from a salt lake, and the specific components are shown in Table 1.
TABLE 1 ingredient table of magnesium and lithium in salt lake brine
Figure BDA0002873955680000051
The evaluation conditions of the lithium extraction adsorbent are as follows:
1. filling 10mL of lithium extraction adsorbent into an adsorption column;
2. mixing 1BV bittern (Mg)2+：2134mg/L，Li+：562mg/L，Mg2+/Li+3.79) was added to the column and the bubbles were driven off;
3. and (3) adsorbing at the flow rate of 1BV/h, collecting effluent, measuring the concentrations of magnesium and lithium, and calculating the saturated adsorption capacity and the magnesium-lithium ratio of the effluent.
The results are shown in Table 2.
TABLE 2 variation of Mg/Li concentration and Mg/Li ratio before and after adsorption
Item Saturated adsorption Capacity (mg/1g adsorbent) Magnesium to lithium ratio of effluent
Lithium extraction adsorbent A 35.2 85
Lithium extraction adsorbent B 43.2 132
Lithium extraction adsorbent C 28.1 61
The data in table 2 show that the lithium extraction adsorbent prepared in the embodiment of the invention has higher saturated adsorption capacity and good selectivity to lithium; can fundamentally solve the defects of poor mechanical strength, high dissolution loss rate, difficult engineering and the like when the existing titanium-based lithium ion sieve powder is used as an adsorbent. In addition, the method provided by the embodiment of the invention is simple to operate, low in energy consumption, stable in water outlet and high in purity of the prepared adsorbent.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.

Claims (9)

1. A preparation method of an adsorbent for extracting lithium from a salt lake is characterized by comprising the following steps:
s1, adding lithium hydroxide into the titanium salt solution to enable the pH value of the solution to be 9-10, reacting for 2-3h at the temperature of 60-70 ℃, filtering, washing and drying to obtain a lithium metatitanate precursor; transferring the lithium metatitanate precursor to a muffle furnace, roasting for 2-3h under a certain temperature condition, and cooling to obtain lithium metatitanate powder;
s2, mixing a polymer monomer, a cross-linking agent and a pore-foaming agent according to a certain weight ratio to obtain an oil phase solution, then adding an initiator, stirring at room temperature until the initiator is completely dissolved, and then adding the lithium metatitanate powder prepared in the step S1 into the oil phase solution to obtain a mixture;
s3, adding a dispersing agent and a salting-out agent into deionized water, and stirring at room temperature until the dispersing agent and the salting-out agent are completely dissolved to obtain an aqueous phase solution; according to the weight ratio of the aqueous phase solution to the mixture of 1: 3-2: 3, adding the aqueous phase solution into the mixture prepared in the step S2, dispersing the oil phase into oil droplets with the particle size of 0.3-1.2mm in the aqueous phase by stirring, heating for reaction, and finally cooling and washing to obtain the adsorbent carrier loaded with lithium metatitanate;
s4, immersing the adsorbent carrier loaded with lithium metatitanate prepared in the step S3 into an eluent to enable lithium ions in the adsorbent carrier to be eluted out, and then cleaning the adsorbent carrier with deionized water to obtain the adsorbent for extracting lithium from the salt lake and the high-molecular-group titanium-based lithium ion sieve.
2. The method for preparing the adsorbent for extracting lithium from the salt lake according to claim 1, wherein in step S1, the feeding molar ratio of the titanium salt to the lithium hydroxide is controlled to be 1 (0.6-0.8); the titanium salt is at least one of titanium sulfate, titanyl sulfate, titanium tetrachloride and titanium nitrate; the concentration of titanium in the titanium salt solution is 1.0-2.5 mol/L.
3. The method as claimed in claim 1, wherein the calcining temperature is 200-400 ℃ and the lithium metatitanate powder is Li in step S14Ti5O12And/or Li2TiO3。
4. The method of claim 1, wherein in step S2, the polymer monomer is at least one of methyl acrylate, propyl acrylate, butyl acrylate, methyl methacrylate, propyl methacrylate, and butyl methacrylate; the cross-linking agent is at least one of divinylbenzene, allyl itaconate, diethylene glycol dimethacrylate, allyl methacrylate and allyl isocyanurate; the initiator is at least one of benzoyl peroxide and azobisisobutyronitrile; the pore-foaming agent is at least one of toluene, isooctane, aviation gasoline and n-heptane.
5. The method for preparing the adsorbent for extracting lithium from the salt lake according to claim 4, wherein the weight ratio of the polymer monomer to the cross-linking agent is 1:3-3:1, the weight ratio of the polymer monomer to the cross-linking agent to the pore-forming agent is 2:1-1:2, and the addition amount of the initiator is 0.1-2% of the weight of the oil phase solution.
6. The method for preparing the adsorbent for extracting lithium from the salt lake according to claim 1, wherein in the step S3, the weight ratio of the dispersing agent is 0.5-3.0%, and the weight ratio of the salting-out agent is 5-15%; the dispersant is at least one of polyvinyl alcohol, methylcellulose, hydroxyethyl cellulose and methyl hydroxypropyl cellulose.
7. The method for preparing the adsorbent for extracting lithium from the salt lake according to claim 1, wherein the temperature-raising reaction comprises two stages in step S3, wherein the temperature is raised to 50-70 ℃ in the first stage, and the reaction lasts for 2-6 h; in the second stage, the temperature is raised to 80-95 ℃ and the reaction lasts for 4-10 h.
8. The method of claim 1, wherein in step S4, the eluent is at least one of hydrochloric acid solution, sulfuric acid solution and nitric acid solution, the concentration of hydrogen ions in the eluent is 5-15 wt%, and the elution time is 1-10 h.
9. An adsorbent for extracting lithium from a salt lake, which is prepared by the preparation method of any one of claims 1 to 8.
CN202011620460.6A 2020-12-30 2020-12-30 Adsorbent for extracting lithium from salt lake and preparation method thereof Pending CN112808251A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011620460.6A CN112808251A (en) 2020-12-30 2020-12-30 Adsorbent for extracting lithium from salt lake and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011620460.6A CN112808251A (en) 2020-12-30 2020-12-30 Adsorbent for extracting lithium from salt lake and preparation method thereof

Publications (1)

Publication Number Publication Date
CN112808251A true CN112808251A (en) 2021-05-18

Family

ID=75855980

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011620460.6A Pending CN112808251A (en) 2020-12-30 2020-12-30 Adsorbent for extracting lithium from salt lake and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112808251A (en)

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114272914A (en) * 2022-01-24 2022-04-05 北京碧水源膜科技有限公司 Lithium adsorbent, membrane element, preparation method of membrane element, and lithium extraction method and device
CN114289000A (en) * 2021-12-25 2022-04-08 广东台泉环保科技有限公司 Salt lake lithium extraction adsorbent and preparation method thereof
CN114917862A (en) * 2022-06-10 2022-08-19 中国科学院青海盐湖研究所 Porous lithium adsorbent and preparation method and application thereof
CN115069208A (en) * 2022-06-07 2022-09-20 四川大学 Porous fiber bundle-shaped titanium lithium adsorbent and preparation method thereof
CN115212844A (en) * 2022-08-09 2022-10-21 杭州电子科技大学 Composite adsorbent for extracting lithium from salt lake brine and preparation method thereof
CN115432733A (en) * 2022-10-18 2022-12-06 攀枝花学院 Method for preparing metatitanic acid with narrow particle size distribution
CN115532219A (en) * 2022-08-30 2022-12-30 上海交通大学 Salt lake lithium extraction adsorbent based on garnet type solid electrolyte powder and preparation and application thereof
CN115558798A (en) * 2021-07-02 2023-01-03 浙江新化化工股份有限公司 Method for producing lithium compound
CN115945179A (en) * 2023-02-20 2023-04-11 江苏苏青水处理工程集团有限公司 Low-solution-loss high-adsorption-capacity salt lake lithium extraction and boron extraction adsorption material and preparation method thereof
CN115945161A (en) * 2022-11-25 2023-04-11 广东松泉环保设备有限公司 Lithium adsorbent, preparation method and lithium extraction process
CN115957727A (en) * 2022-11-25 2023-04-14 广东松泉环保设备有限公司 Composite lithium adsorbent and preparation process thereof
CN115970661A (en) * 2023-01-30 2023-04-18 江苏海普功能材料有限公司 Preparation method of high-adsorption-capacity lithium ion imprinted nano composite particles
CN116043255A (en) * 2022-12-29 2023-05-02 天津科技大学 Lithium extraction electrode preparation method and lithium extraction device
CN116173925A (en) * 2023-03-31 2023-05-30 江苏海普功能材料有限公司 High-adsorption-rate lithium extraction adsorbent and preparation method and application thereof
CN116371373A (en) * 2022-11-28 2023-07-04 江西赣锋锂业集团股份有限公司 Preparation method of titanium particle adsorbent with high adsorption stability

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101955210A (en) * 2010-09-14 2011-01-26 华东理工大学 Granular lithium ion sieve
CN104014308A (en) * 2014-02-25 2014-09-03 江苏海普功能材料有限公司 Method for preparing high-performance brine lithium-extraction adsorption agent and adsorption agent prepared by method
CN109173976A (en) * 2018-09-07 2019-01-11 成都理工大学 It is a kind of to efficiently separate the synthetic method for extracting the metatitanic acid type lithium adsorbent of lithium in brine

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101955210A (en) * 2010-09-14 2011-01-26 华东理工大学 Granular lithium ion sieve
CN104014308A (en) * 2014-02-25 2014-09-03 江苏海普功能材料有限公司 Method for preparing high-performance brine lithium-extraction adsorption agent and adsorption agent prepared by method
CN109173976A (en) * 2018-09-07 2019-01-11 成都理工大学 It is a kind of to efficiently separate the synthetic method for extracting the metatitanic acid type lithium adsorbent of lithium in brine

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115558798A (en) * 2021-07-02 2023-01-03 浙江新化化工股份有限公司 Method for producing lithium compound
CN115558798B (en) * 2021-07-02 2023-12-01 浙江新化化工股份有限公司 Method for producing lithium compound
CN114289000A (en) * 2021-12-25 2022-04-08 广东台泉环保科技有限公司 Salt lake lithium extraction adsorbent and preparation method thereof
CN114289000B (en) * 2021-12-25 2024-04-02 广东台泉科技股份有限公司 Salt lake lithium extraction adsorbent and preparation method thereof
CN114272914B (en) * 2022-01-24 2023-06-02 北京碧水源膜科技有限公司 Lithium adsorbent, membrane element, preparation method of membrane element, and lithium extraction method and device
CN114272914A (en) * 2022-01-24 2022-04-05 北京碧水源膜科技有限公司 Lithium adsorbent, membrane element, preparation method of membrane element, and lithium extraction method and device
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
CN114917862A (en) * 2022-06-10 2022-08-19 中国科学院青海盐湖研究所 Porous lithium adsorbent and preparation method and application thereof
CN114917862B (en) * 2022-06-10 2024-04-12 中国科学院青海盐湖研究所 Porous lithium adsorbent and preparation method and application thereof
CN115212844A (en) * 2022-08-09 2022-10-21 杭州电子科技大学 Composite adsorbent for extracting lithium from salt lake brine and preparation method thereof
CN115212844B (en) * 2022-08-09 2024-02-02 杭州电子科技大学 Composite adsorbent for extracting lithium from salt lake brine and preparation method thereof
CN115532219A (en) * 2022-08-30 2022-12-30 上海交通大学 Salt lake lithium extraction adsorbent based on garnet type solid electrolyte powder and preparation and application thereof
CN115532219B (en) * 2022-08-30 2024-03-22 上海交通大学 Salt lake lithium extraction adsorbent based on garnet type solid electrolyte powder and preparation and application thereof
CN115432733A (en) * 2022-10-18 2022-12-06 攀枝花学院 Method for preparing metatitanic acid with narrow particle size distribution
CN115432733B (en) * 2022-10-18 2024-04-30 攀枝花学院 Method for preparing metatitanic acid with narrow particle size distribution
CN115957727A (en) * 2022-11-25 2023-04-14 广东松泉环保设备有限公司 Composite lithium adsorbent and preparation process thereof
CN115945161A (en) * 2022-11-25 2023-04-11 广东松泉环保设备有限公司 Lithium adsorbent, preparation method and lithium extraction process
CN116371373A (en) * 2022-11-28 2023-07-04 江西赣锋锂业集团股份有限公司 Preparation method of titanium particle adsorbent with high adsorption stability
CN116043255A (en) * 2022-12-29 2023-05-02 天津科技大学 Lithium extraction electrode preparation method and lithium extraction device
CN115970661A (en) * 2023-01-30 2023-04-18 江苏海普功能材料有限公司 Preparation method of high-adsorption-capacity lithium ion imprinted nano composite particles
CN115945179B (en) * 2023-02-20 2023-08-29 江苏苏青水处理工程集团有限公司 Low-solution-loss high-adsorption capacity salt lake lithium-extracting boron-extracting adsorption material and preparation method thereof
CN115945179A (en) * 2023-02-20 2023-04-11 江苏苏青水处理工程集团有限公司 Low-solution-loss high-adsorption-capacity salt lake lithium extraction and boron extraction adsorption material and preparation method thereof
CN116173925A (en) * 2023-03-31 2023-05-30 江苏海普功能材料有限公司 High-adsorption-rate lithium extraction adsorbent and preparation method and application thereof
CN116173925B (en) * 2023-03-31 2024-05-17 江苏海普功能材料有限公司 High-adsorption-rate lithium extraction adsorbent and preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN112808251A (en) Adsorbent for extracting lithium from salt lake and preparation method thereof
CN112871127B (en) Preparation method of high-porosity lithium ion sieve particles
EP4306667A1 (en) Method for preparing granular titanium-based lithium ion sieve adsorbent having high adsorption capacity
CN109266851B (en) Method for extracting lithium through magnetic microporous lithium adsorbent
CN111250063B (en) Preparation of conductive manganese-titanium lithium ion sieve/graphene composite hydrogel and application of conductive manganese-titanium lithium ion sieve/graphene composite hydrogel in extraction of lithium from salt lake brine
CN107376827A (en) A kind of zirconia-coated manganese systems lithium ion sieve and its preparation method and application
CN114288983B (en) Titanium-based lithium ion exchanger and preparation method thereof
CN109078602B (en) Magnetic microporous lithium adsorbent and preparation method and application thereof
CN113731371A (en) Preparation method of lithium ion adsorption material
CN116920807B (en) Adsorbent for extracting lithium from salt lake and preparation method thereof
CN108046368B (en) Lithium ion sieve filler loaded by open-cell foam glass and preparation method thereof
CN111229177A (en) Poly- (styrene-divinylbenzene-vinyl imidazole) @ Fe3O4Water treatment agent and preparation method thereof
CN117427604A (en) Sand-like aluminum salt adsorbent, preparation method thereof and application of adsorbent in lithium extraction by adsorption method
CN110106356B (en) Method for separating lithium from salt lake brine by using powder type titanium ion exchanger
CN116899525A (en) Lithium extraction adsorbent and preparation method and application thereof
CN116173925B (en) High-adsorption-rate lithium extraction adsorbent and preparation method and application thereof
CN105664735A (en) PTFE blend flat sheet membrane and preparation method thereof
CN116159531A (en) Preparation method of hollow fiber membrane lithium ion adsorbent
CN116328713A (en) Method for preparing lithium ion sieve adsorbent particles and application thereof
CN111302326A (en) Nitrogen-doped hierarchical porous carbon material for lead-carbon battery and preparation method thereof
CN116966867A (en) Layered lithium adsorbent powder, preparation method, layered lithium adsorbent particles and application
CN116371373A (en) Preparation method of titanium particle adsorbent with high adsorption stability
CN116237026A (en) Nano lithium extraction adsorbent, preparation method thereof and electrochemical reactor using nano lithium extraction adsorbent
CN110711551A (en) Lithium adsorbent and preparation method thereof
CN115722195B (en) Preparation method of fluoride ion adsorbent

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210518