CN116571221A - Aluminum salt composite hydrogel adsorbent and preparation method and application thereof - Google Patents
Aluminum salt composite hydrogel adsorbent and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an aluminum salt composite hydrogel adsorbent, and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing the gel skeleton material with water, and adding an aluminum salt lithium adsorption material to obtain a mixed solution; the solid spherical aluminum salt composite hydrogel adsorbent with high specific surface area and three-dimensional network structure is prepared by taking boric acid and calcium chloride as receiving liquid, dripping the mixed liquid into the receiving liquid to form precipitate, and carrying out low-temperature freezing-thawing treatment on the precipitate.
Description
Technical Field
The invention belongs to the technical field of adsorbents, and particularly relates to an aluminum salt composite hydrogel adsorbent, and a preparation method and application thereof.
Background
Lithium is widely used in the industries of batteries, ceramics, glass, lubricants, refrigerating fluids, nuclear industry, photoelectricity and the like, and the demand of lithium is increasing year by year. The method has rich lithium resources in China, mainly comprises three brine types of carbonate brine, chloride brine and sulfate brine, and aims to realize efficient lithium extraction of salt lake brine, and the key is that the technical bottleneck of extracting lithium from brine with high magnesium-lithium ratio cannot be broken through.
The adsorption method is to prepare an adsorbent with high adsorption performance, and the aim of separating lithium ions from other impurity ions is fulfilled by selectively adsorbing the lithium ions and eluting the lithium ions. The method has the advantages of simple process, high recovery rate, good selectivity, simple preparation process, low cost, little environmental pollution and great superiority compared with other methods. At present, more adsorbents are researched mainly in three categories of aluminum salt adsorbents, manganese ion sieves and titanium ion sieves, wherein the manganese ion sieves have excellent lithium adsorption performance, but the manganese dissolution loss in the desorption process is a large short plate in the application process; the dissolution loss rate of the titanium ion sieve is lower than that of the manganese ion sieve, but the synthesis process is complex, and the adsorption and desorption rates are slower; the aluminum salt lithium adsorbent is simple to prepare, low in cost and capable of being desorbed under neutral conditions, and becomes the only lithium adsorbent which is put into industrial lithium extraction application at present, but the powdery aluminum salt adsorbent is poor in fluidity, high in dissolution loss in water and low in cycling stability. In practical application, a binder is generally adopted to granulate and form the powder aluminum salt adsorbent, but the granulated adsorbent has low porosity and few active sites, so that the lithium adsorption capacity of the aluminum salt adsorbent is obviously reduced to only about 2mg/g, and therefore, the aluminum salt adsorbent material with high specific surface area and network structure needs to be designed and developed, and the adsorption capacity and the cycle stability of the aluminum salt adsorbent are improved.
Disclosure of Invention
The invention aims to solve the technical problems that: provides an aluminum salt composite hydrogel adsorbent, a preparation method and application thereof, and aims to solve the technical problems of high dissolution loss rate, severely reduced adsorption capacity, difficult recovery and poor stability of the powdery aluminum salt adsorbent.
In order to achieve the above purpose, the invention adopts the following technical scheme: the preparation method of the aluminum salt composite hydrogel adsorbent comprises the following steps:
s1: mixing aluminum salt and lithium salt in 10-20:1 in mass ratio, uniformly stirring, regulating the pH value of the solution to be neutral, stirring at room temperature for reaction for 2-3h, filtering, washing filter residues with water for 3-5 times, and drying to obtain an aluminum salt adsorbent;
s2: adding the aluminum salt adsorbent into the hydrogel matrix solution for reaction, then adding the aluminum salt adsorbent into the mixed solution, stirring for 10-20min, then filtering, washing the filtrate with water for 3-5 times, and drying after 3-4 freeze-thawing cycles to obtain the aluminum salt composite hydrogel adsorbent; the proportioning relationship between the aluminum salt adsorbent and the hydrogel matrix solution is 1g:10-20mL, wherein the mixed solution comprises 1-5wt% of boric acid solution and 1-10wt% of calcium chloride solution according to the volume ratio of 1-6:1 are evenly mixed to prepare the composite material.
Based on the technical scheme, the invention can also be improved as follows:
further, the aluminum salt is polyaluminum chloride and AlCl 3 ·6H 2 O、Al(OH) 3 、Al 2 (SO 4 ) 3 And Al (NO) 3 ) 3 At least one of the lithium salts is LiCl.H 2 O、LiOH、Li 2 SO 4 And LiNO 3 At least one of them.
Further, in the step S1, the drying temperature is 50-70 ℃ and the drying time is 8-10h.
Further, the hydrogel matrix solution is at least one of a polyacrylonitrile solution of 1-15wt%, a polyvinyl alcohol solution of 1-15wt% and a sodium alginate solution of 0.5-10 wt%.
The beneficial effects of adopting the further technical scheme are as follows: the hydrogel is used as a polymer material for forming a three-dimensional network structure through crosslinking, has higher structural stability and solute diffusion rate, is favorable for the diffusion and adsorption of target ions, and has great potential in the aspect of ion adsorption and separation in water due to the advantages of simple preparation, convenient recovery and the like. Therefore, the three-dimensional network structure hydrogel adsorbent material with good mechanical strength and chemical property is prepared based on the high selectivity of the aluminum-based adsorbent to lithium.
Further, the reaction temperature in the step S2 is 40-70 ℃ and the reaction time is 1-2h.
Further, the freezing process is freezing for 4-5h at-6 to-4 ℃, the thawing process is thawing for 2-3h at room temperature, and the drying process is drying for 12-15h at-6 to-4 ℃.
The invention also discloses the aluminum salt composite hydrogel adsorbent prepared by the preparation method of the aluminum salt composite hydrogel adsorbent.
The invention also discloses application of the aluminum salt composite hydrogel adsorbent in adsorption of lithium in salt lake brine.
Based on the technical scheme, the invention can also be improved as follows:
further, the specific steps include:
s1: adsorption: adding the aluminum salt composite hydrogel adsorbent into salt lake brine with the lithium ion concentration of 0.05-10g/L, then adsorbing for 2-8h at 20-70 ℃, and centrifuging to obtain a load adsorbent; the proportioning relationship between the aluminum salt composite hydrogel adsorbent and brine is 0.5-20g:1L;
s2: and (3) desorption: desorbing the loaded adsorbent at 10-70 ℃ by using an eluent, and centrifuging to obtain a lithium solution containing LiCl; the eluent is water or hydrochloric acid with the concentration of 0.01-2mol/L, and the ratio relationship of the loaded adsorbent and the eluent is 10-30g:1L.
Further, the mass ratio of the magnesium salt to the lithium salt in the brine is 1-100:1.
the invention has the following beneficial effects:
1. the powder aluminum-based adsorbent is prepared into a solid spherical aluminum salt composite hydrogel adsorbent through crosslinking, so that the adsorption capacity is high, the selectivity is good, and the technical problems of high dissolution loss rate, serious reduction in adsorption capacity, difficult recovery and poor stability of the powder aluminum salt adsorbent are solved;
2. the three-dimensional network structure aluminum salt composite hydrogel adsorbent prepared by the invention does not need to adjust the pH value of brine when separating lithium ions from salt lake brine, has simple and convenient process, is easy to recycle after being used, and reduces the production cost.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing an aluminum salt composite hydrogel adsorbent;
FIG. 2 is a physical diagram of the aluminum salt composite hydrogel adsorbent prepared in example 1;
FIG. 3 is an internal scanning electron microscope image of the aluminum salt composite hydrogel adsorbent prepared in example 1;
FIG. 4 shows the pair of Li of the aluminum salt adsorbents prepared in examples 1 to 3 + A comparison graph of adsorption capacity as a function of temperature;
FIG. 5 shows the aluminum salt adsorbent pair Li prepared in examples 1-3 + Is a graph of adsorption capacity versus adsorption time.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
the preparation method of the aluminum salt composite hydrogel adsorbent, as shown in fig. 1, comprises the following steps:
s1: 48g AlCl 3 ·6H 2 O and 4g LiCl.H 2 Dissolving O in water, stirring uniformly, regulating the pH of the solution to be neutral by using 6mol/L NaOH, stirring at room temperature for reaction for 2 hours, filtering, washing filter residues with water for 3 times, and drying at 65 ℃ for 8 hours to obtain an aluminum salt adsorbent;
s2: weighing 8g of polyvinyl alcohol and 3g of sodium alginate, dissolving in 100mL of deionized water, uniformly stirring, adding 5g of aluminum salt lithium adsorbent, and stirring at 60 ℃ for reaction for 1h; then adding a boric acid solution with 5 weight percent and a calcium chloride solution with 3 weight percent into the mixture according to the volume ratio of 3:1, stirring for 15min, filtering, washing the filtrate with water for 3 times, and drying after 3 times of freezing-thawing cycles to obtain the spherical aluminum salt composite hydrogel adsorbent, wherein the freezing process is freezing at-4 ℃ for 5h, the thawing process is thawing at room temperature for 2h, and the drying process is drying at-4 ℃ for 12h.
The prepared spherical aluminum salt composite hydrogel adsorbent is shown in a real object in fig. 2, and an internal scanning electron microscope is shown in fig. 3.
The embodiment also comprises the application of the aluminum salt composite hydrogel adsorbent prepared by the preparation method of the aluminum salt composite hydrogel adsorbent, which comprises the following specific steps:
s1: adsorption: adding the aluminum salt composite hydrogel adsorbent into brine with the lithium ion concentration of 0.35g/L and the magnesium ion concentration of 90g/L, wherein the proportioning relationship between the aluminum salt composite hydrogel adsorbent and the brine is 10g:1L; then adsorbing for 8 hours at 50 ℃, and centrifuging to obtain a loaded adsorbent;
s2: and (3) desorption: carrying out desorption treatment on the loaded adsorbent by deionized water at 50 ℃, wherein the ratio relationship of the loaded adsorbent to the eluent is 20g:1L; and then centrifuging to obtain a lithium solution containing LiCl.
Example 2:
the preparation method of the aluminum salt composite hydrogel adsorbent comprises the following steps:
s1: 20g AlCl 3 ·6H 2 O and 1g LiCl.H 2 Dissolving O in water, uniformly stirring, regulating the pH of the solution to be neutral by using 6mol/L KOH, stirring at room temperature for reaction for 2 hours, filtering, washing filter residues with water for 3 times, and drying at 50 ℃ for 10 hours to obtain an aluminum salt adsorbent;
s2: weighing 8g of polyvinyl alcohol, dissolving in 100mL of deionized water, uniformly stirring, adding 5g of aluminum salt lithium adsorbent, and stirring at 60 ℃ for reaction for 2 hours; then adding a boric acid solution with the weight percent of 1 and a calcium chloride solution with the weight percent of 10 into the mixture according to the volume ratio of 6:1, stirring for 20min, filtering, washing the filtrate with water for 3 times, and drying after 4 times of freezing-thawing cycles to obtain the spherical aluminum salt composite hydrogel adsorbent, wherein the freezing process is freezing at-6 ℃ for 5h, the thawing process is thawing at room temperature for 3h, and the drying process is drying at-6 ℃ for 15h.
The embodiment also comprises the application of the aluminum salt composite hydrogel adsorbent prepared by the preparation method of the aluminum salt composite hydrogel adsorbent, which comprises the following specific steps:
s1: adsorption: adding the aluminum salt composite hydrogel adsorbent into brine with the lithium ion concentration of 0.35g/L and the magnesium ion concentration of 92.17g/L, wherein the proportioning relationship between the aluminum salt composite hydrogel adsorbent and the brine is 20g:1L; then adsorbing for 2 hours at 70 ℃, and centrifuging to obtain a loaded adsorbent;
s2: and (3) desorption: carrying out desorption treatment on the loaded adsorbent by using hydrochloric acid with the concentration of 0.01mol/L at the temperature of 10 ℃, wherein the proportioning relationship between the loaded adsorbent and the eluent is 30g:1L; and then centrifuging to obtain a lithium solution containing LiCl.
Example 3:
the preparation method of the aluminum salt composite hydrogel adsorbent comprises the following steps:
s1: 40g AlCl 3 ·6H 2 O and 4g LiCl.H 2 Dissolving O in water, stirring uniformly, regulating the pH of the solution to be neutral by using 6mol/L NaOH, stirring at room temperature for reaction for 3 hours, filtering, washing filter residues with water for 5 times, and drying at 70 ℃ for 8 hours to obtain an aluminum salt adsorbent;
s2: weighing 10g of sodium alginate, dissolving in 100mL of deionized water, uniformly stirring, adding 5g of aluminum salt lithium adsorbent, and stirring at 60 ℃ for reaction for 1h; then adding a boric acid solution with 5 weight percent and a calcium chloride solution with 1 weight percent into the mixture according to the volume ratio of 1:1, stirring for 10min, filtering, washing the filtrate with water for 5 times, and drying after 3 times of freezing-thawing cycles to obtain the spherical aluminum salt composite hydrogel adsorbent, wherein the freezing process is freezing at-4 ℃ for 5h, the thawing process is thawing at room temperature for 2h, and the drying process is drying at-4 ℃ for 12h.
The embodiment also comprises the application of the aluminum salt composite hydrogel adsorbent prepared by the preparation method of the aluminum salt composite hydrogel adsorbent, which comprises the following specific steps:
s1: adsorption: adding the aluminum salt composite hydrogel adsorbent into brine with the lithium ion concentration of 0.1g/L and the magnesium ion concentration of 100g/L, wherein the proportioning relationship between the aluminum salt composite hydrogel adsorbent and the brine is 30g:1L; then adsorbing for 6.5h at 70 ℃, and centrifuging to obtain a loaded adsorbent;
s2: and (3) desorption: carrying out desorption treatment on the loaded adsorbent by using hydrochloric acid with the concentration of 2mol/L at the temperature of 70 ℃, wherein the proportioning relationship between the loaded adsorbent and the eluent is 10g:1L; and then centrifuging to obtain a lithium solution containing LiCl.
Analysis of results:
(1) The concentration of lithium ions in the supernatants after adsorption of examples 1-3 was measured using an inductively coupled plasma atomic emission spectrometer (ICP-OES) and adsorption capacity data was calculated as shown in Table 1, with the following calculation formula:
wherein:
q-adsorption capacity of adsorbent mg/g;
C 0 li in aqueous solution containing Li before adsorption + Concentration of (2) mg/L;
C e li in the aqueous solution containing Li after adsorption + Concentration of (2) mg/L;
v-the volume of the aqueous lithium-containing solution, L;
m-mass of aluminum salt adsorbent, g.
TABLE 1 influence of hydrogel matrix on Li+ adsorption Capacity at optimal temperature and adsorption time
| Examples | Hydrogel matrix | Adsorption capacity/mg.g -1 |
| 1 | PVA+SA | 14.86 |
| 2 | PVA | 11.15 |
| 3 | SA | 13.49 |
It can be seen that the adsorption capacity of the prepared aluminum salt adsorbent for lithium ions is higher when polyvinyl alcohol (PVA) and Sodium Alginate (SA) are used as hydrogel matrixes.
(2) The adsorption capacities of the gel ball adsorbents prepared in examples 1-3 for Li+ at different temperatures and adsorption times are shown in fig. 4 and 5, and the adsorption conditions of the adsorbent prepared in example 1 at 50 ℃ for 5h are the optimal adsorption conditions, and the polyvinyl alcohol (PVA) and Sodium Alginate (SA) are selected as hydrogel matrixes, so that the defects of low adsorption capacity and poor stability of the aluminum salt adsorbent can be overcome, and the prepared adsorbent is solid spherical, is easy to recover and can realize efficient separation of lithium ions in solution.
(3) The concentration of lithium ions in the lithium solution obtained after desorption in examples 1-3 was measured, and desorption rate data of examples 1-3 were obtained by calculation, and the calculation formula was as follows:
wherein:
d-desorption rate of adsorbent,%;
c-concentration of Li+ in the solution after desorption, mg/L;
v-the volume of the aqueous lithium-containing solution, L;
m 0 -adsorbing the mass of saturated adsorbent, g;
Q 0 saturated adsorption capacity, mg/g.
The single-stage lithium ion desorption rate of example 1 was calculated to be 98.86%, the single-stage lithium ion desorption rate of example 2 was calculated to be 90.27%, and the single-stage lithium ion desorption rate of example 3 was calculated to be 99.21%. Therefore, the dilute hydrochloric acid solution and the deionized water are selected as the desorption solution, so that the desorption solution has a good desorption effect, but compared with the deionized water, the desorption solution is more environment-friendly, so that the deionized water can be generally selected, the desorption temperature is properly increased, and the efficient desorption of lithium ions can be realized.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The preparation method of the aluminum salt composite hydrogel adsorbent is characterized by comprising the following steps of:
s1: mixing aluminum salt and lithium salt in 10-20:1 in mass ratio, uniformly stirring, regulating the pH value of the solution to be neutral, stirring at room temperature for reaction for 2-3h, filtering, washing filter residues with water for 3-5 times, and drying to obtain an aluminum salt adsorbent;
s2: adding the aluminum salt adsorbent into a hydrogel matrix solution for reaction, then adding the hydrogel matrix solution into the mixed solution, stirring for 10-20min, then filtering, washing the filtrate with water for 3-5 times, and drying after 3-4 freeze-thawing cycles to obtain the aluminum salt composite hydrogel adsorbent; the proportioning relationship between the aluminum salt adsorbent and the hydrogel matrix solution is 1g:10-20mL, wherein the mixed solution comprises 1-5wt% of boric acid solution and 1-10wt% of calcium chloride solution according to the volume ratio of 1-6:1 are evenly mixed to prepare the composite material.
2. The method for preparing the aluminum salt composite hydrogel adsorbent of claim 1, wherein the method comprises the following steps: the aluminum salt is polyaluminum chloride and AlCl 3 ·6H 2 O、Al(OH) 3 、Al 2 (SO 4 ) 3 And Al (NO) 3 ) 3 At least one of the lithium salts is LiCl.H 2 O、LiOH、Li 2 SO 4 And LiNO 3 At least one of them.
3. The method for preparing the aluminum salt composite hydrogel adsorbent of claim 1, wherein the method comprises the following steps: and in the step S1, the drying temperature is 50-70 ℃ and the drying time is 8-10h.
4. The method for preparing the aluminum salt composite hydrogel adsorbent of claim 1, wherein the method comprises the following steps: the hydrogel matrix solution is at least one of a polyacrylonitrile solution with the weight percent of 1-15, a polyvinyl alcohol solution with the weight percent of 1-15 and a sodium alginate solution with the weight percent of 0.5-10.
5. The method for preparing the aluminum salt composite hydrogel adsorbent of claim 1, wherein the method comprises the following steps: the reaction temperature in the step S2 is 40-70 ℃ and the reaction time is 1-2h.
6. The method for preparing the aluminum salt composite hydrogel adsorbent of claim 1, wherein the method comprises the following steps: the freezing process is freezing for 4-5h at-6 to-4 ℃, the thawing process is thawing for 2-3h at room temperature, and the drying process is drying for 12-15h at-6 to-4 ℃.
7. The aluminum salt composite hydrogel adsorbent produced by the method for producing an aluminum salt composite hydrogel adsorbent of any one of claims 1 to 6.
8. The use of the aluminum salt composite hydrogel adsorbent of claim 7 in adsorption of lithium by salt lake brine.
9. The use of the aluminum salt composite hydrogel adsorbent of claim 8, wherein the specific steps include:
s1: adsorption: adding the aluminum salt composite hydrogel adsorbent into salt lake brine with the lithium ion concentration of 0.05-10g/L, then adsorbing for 2-8h at 20-70 ℃, and centrifuging to obtain a load adsorbent; the proportioning relationship between the aluminum salt composite hydrogel adsorbent and brine is 0.5-20g:1L;
s2: and (3) desorption: desorbing the loaded adsorbent at 10-70 ℃ by using an eluent, and centrifuging to obtain a lithium solution containing LiCl; the eluent is water or hydrochloric acid with the concentration of 0.01-2mol/L, and the ratio of the load adsorbent to the eluent is 10-30g:1L.
10. The use of the aluminum salt composite hydrogel adsorbent of claim 9, wherein: the mass ratio of the magnesium salt to the lithium salt in the brine is 1-100:1.
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| CN117380152A (en) * | 2023-09-20 | 2024-01-12 | 中国地质科学院矿产资源研究所 | Preparation method of composite mineral lithium ion adsorbent and brine lithium extraction method |
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| CN117380152A (en) * | 2023-09-20 | 2024-01-12 | 中国地质科学院矿产资源研究所 | Preparation method of composite mineral lithium ion adsorbent and brine lithium extraction method |
| CN117380152B (en) * | 2023-09-20 | 2024-03-19 | 中国地质科学院矿产资源研究所 | Preparation method of composite mineral lithium ion adsorbent and brine lithium extraction method |
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