A preparation method of a novel high specific surface area aluminum-based lithium adsorption precursor
A high specific surface area aluminum-based lithium adsorption precursor was prepared by doping with RSO3M and washing with organic solvents, which solved the problem of insufficient adsorption capacity in the prior art and achieved a significant improvement in specific surface area and adsorption performance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- TIBET JIUWU NEW MATERIAL TECH CO LTD
- Filing Date
- 2024-12-17
- Publication Date
- 2026-06-05
AI Technical Summary
Existing aluminum salt adsorbents have low adsorption capacity, and how to increase their specific surface area to improve adsorption performance is a hot research topic.
A high specific surface area aluminum-based lithium adsorbent precursor was prepared by doping with RSO3M and washing with an organic solvent. The specific steps included co-precipitation reaction, filtration of precipitate, drying and washing with organic solvent.
It significantly improved the specific surface area and adsorption capacity of the aluminum-based lithium adsorption precursor, increasing the adsorption performance by 21.8%.
Smart Images
Figure CN122141632A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of inorganic synthetic adsorption precursor technology, specifically relating to a method for preparing a novel high specific surface area aluminum-based lithium adsorption precursor. Background Technology
[0002] Aluminum salt adsorbents are characterized by simple preparation and good stability, but their adsorption capacity is relatively low. Therefore, how to efficiently improve adsorption capacity is a current research hotspot. Specific surface area, which is the surface area per unit mass or volume of a substance, is one of the important indicators for evaluating adsorbent performance. Preparing adsorbent powders with higher specific surface areas is key to improving the adsorption capacity of aluminum-based lithium adsorption precursors. Summary of the Invention
[0003] In view of the shortcomings of the existing technology, the present invention prepares aluminum-based powder by doping with RSO3M, and then washes off RSO3M with an organic solvent to obtain an aluminum-based lithium adsorption precursor with a high specific surface area.
[0004] A novel method for preparing a high specific surface area aluminum-based lithium adsorption precursor includes the following steps:
[0005] Step 1: Prepare a solution containing lithium source and aluminum source, add sulfonic acid surfactant, add alkali to adjust pH to carry out precipitation reaction, filter out the precipitate and dry it;
[0006] Step 2: Wash the dried powder with an organic solvent to remove excess sulfonic acid surfactant and obtain the aluminum-based lithium adsorbent precursor.
[0007] In step 1, the lithium source is selected from one or a mixture of several of lithium hydroxide, lithium chloride, lithium carbonate, lithium citrate, lithium acetate, and lithium formate.
[0008] In step 1, the aluminum source is selected from one or a mixture of several of the following: boehmite, aluminum chloride, aluminum hydroxide, sodium aluminate, aluminum hydroxyaluminate, and boehmite.
[0009] The selected surfactant includes one or a mixture of several of alkylbenzene sulfonates, alkylnaphthalene sulfonates, and succinate sulfonates, added in the solution in step 1 at an amount of 1%-5%.
[0010] In the lithium and aluminum sources, the molar ratio of aluminum to lithium is 2 to 2.2:1.
[0011] Organic solvents include one or a mixture of several of the following: trichloroethylene, dimethylacetamide, methanol, acetone, and acetonitrile.
[0012] The amount of organic solvent used is 20-100 times the mass of the powder. Attached Figure Description
[0013] Figure 1 This is a bar chart showing the specific surface area of the aluminum-based adsorption precursors prepared in Examples 1-2 and Comparative Examples 1-2 of this invention.
[0014] Figure 2 This is a bar chart showing the adsorption capacity of the aluminum-based adsorption precursors prepared in Examples 1-2 and Comparative Examples 1-2 of this invention.
[0015] Figure 3 These are XRD patterns of the aluminum-based adsorption precursors prepared in Examples 1-2 and Comparative Examples 1-2 of this invention.
[0016] Figure 4 This is a SEM image of the prepared adsorbent. Detailed Implementation
[0017] This invention discloses a novel method for preparing a high specific surface area aluminum-based lithium adsorbent precursor. The method involves co-precipitation, where a specific lithium source and an aluminum source are mixed and RSO3M is added. NaOH is then added to adjust the pH to 5.0-7.0. During co-precipitation, the hydrophilic SO3M groups of RSO3M are embedded into the crystal structure. After precipitation, the mixture is aged for a period of time, filtered, and dried. The filter cake is then washed with a specific organic solvent to remove RSO3M. After further filtration and drying, a novel aluminum-based lithium adsorbent precursor with a high specific surface area is obtained.
[0018] The lithium source is selected from one or a mixture of several of lithium hydroxide, lithium chloride, lithium carbonate, lithium citrate, lithium acetate, and lithium formate.
[0019] The aluminum source is selected from one or a mixture of several of the following: boehmite, aluminum chloride, aluminum hydroxide, sodium aluminate, aluminum hydroxyaluminate, and boehmite.
[0020] The selected surfactants include one or a mixture of several of alkylbenzene sulfonates, alkylnaphthalene sulfonates, and succinate sulfonates, added at a rate of 1%-5%.
[0021] After adding lithium and aluminum sources, the molar ratio of aluminum to lithium is ensured to be 2 to 2.2:1.
[0022] The specific organic solvents selected include one or a mixture of several of the following: trichloroethylene, dimethylacetamide, methanol, acetone, and acetonitrile. The amount added is 20-100 times the mass of the powder.
[0023] Example 1
[0024] Weigh 100.7g of aluminum chloride hexahydrate and 10.6g of lithium chloride solid into 100ml of aqueous solution, stir for 15min until completely dissolved, then add 4g of sodium dodecyl sulfonate, continue stirring for 15min, then add 50% NaOH solution to adjust the pH to 6.0. The mixture is then filtered, and the filter cake is washed twice with 300ml of pure water to remove the sodium chloride produced in the reaction. The filter cake is then placed in an 80°C oven and dried for 12 hours. After the filter cake is completely dry, it is crushed using a pulverizer. The resulting powder is placed in a 500ml beaker, and 300ml of dimethylacetamide is added. The mixture is stirred and washed twice, and the filter cake is dried again for 8 hours to obtain the aluminum-based lithium adsorption precursor.
[0025] Comparative Example 1
[0026] Weigh 100.7g of aluminum chloride hexahydrate and 10.6g of lithium chloride solid into 100ml of aqueous solution, stir for 15min until completely dissolved, then add 50% NaOH solution to adjust the pH to 6.0. The mixture is then filtered, and the filter cake is washed twice with 300ml of pure water to remove the sodium chloride produced in the reaction. The filter cake is then placed in an 80°C oven and dried for 12 hours. After the filter cake is completely dried, it is crushed using a pulverizer to obtain the aluminum-based lithium adsorption precursor.
[0027] Example 2
[0028] Weigh 503.5g of aluminum chloride hexahydrate and 53g of lithium chloride solid into 500ml of aqueous solution, stir for 15min until completely dissolved, add 20g of sodium alkylnaphthalene sulfonate, continue stirring for 15min, then add 50% NaOH solution to adjust the pH to 6.5. The mixture is then filtered, and the filter cake is washed twice with 1500ml of pure water to remove the sodium chloride produced in the reaction. The filter cake is then placed in an 80°C oven and dried for 12 hours. After the filter cake is completely dry, it is crushed using a pulverizer. The resulting powder is placed in a 3L beaker, and 1500ml of dimethylacetamide is added. The mixture is stirred and washed twice, and the filter cake is dried again for 8 hours to obtain the aluminum-based lithium adsorption precursor.
[0029] Comparative Example 2
[0030] Weigh 503.5 g of aluminum chloride hexahydrate and 53 g of lithium chloride solid into 500 ml of aqueous solution. Stir for 15 min until completely dissolved, then add 50% NaOH solution to adjust the pH to 6.5. The mixture is then filtered. The filter cake is washed twice with 1500 ml of pure water to remove the sodium chloride produced in the reaction. The filter cake is then placed in an 80°C oven and dried for 12 hours. After complete drying, the filter cake is broken up using a pulverizer and dried again for 8 hours to obtain the aluminum-based lithium adsorption precursor. Structural characterization: [The remaining text appears to be incomplete and requires further context.] Figure 3It can be seen that the peak values of both the examples and the comparative examples correspond to the peak values of the 31-0700-LiAlLDHs standard card, indicating that the powders prepared in both examples and the comparative examples are aluminum-based lithium adsorption precursors. Figure 1 It can be seen that the specific surface area of the embodiments is significantly improved compared with the comparative examples, with Example 1 showing a 240% increase compared to Comparative Example 1. Combined with scanning electron microscopy images, it is clearly observed that the surface of the aluminum-based adsorbent powder is relatively rough with numerous pores. This clearly demonstrates that the powder preparation method of this patent can effectively improve the specific surface area of the aluminum-based adsorbent powder compared to the general co-precipitation method.
[0031] Performance characterization: 5g of aluminum-based lithium adsorption precursor was activated twice in 200ml of pure water at room temperature for 30min. The activated powder was then subjected to adsorption experiments in 200ml of a standard solution with a lithium concentration of 340mg / kg. (See attached...) Figure 3 It can be seen that the adsorption capacity of the adsorbent powder in the examples is significantly higher than that in the comparative examples, with Example 1 showing a 21.8% improvement in adsorption performance compared to Comparative Example 1. This indicates that the aluminum-based lithium adsorbent precursor prepared by this method has better adsorption performance.
Claims
1. A novel method for preparing a high specific surface area aluminum-based lithium adsorption precursor, characterized in that, Includes the following steps: Step 1: Prepare a solution containing lithium source and aluminum source, add sulfonic acid surfactant, add alkali to adjust pH to carry out precipitation reaction, filter out the precipitate and dry it; Step 2: Wash the dried powder with an organic solvent to remove excess sulfonic acid surfactant and obtain the aluminum-based lithium adsorbent precursor.
2. The method for preparing the novel high specific surface area aluminum-based lithium adsorption precursor according to claim 1, characterized in that, In step 1, the lithium source is selected from one or a mixture of several of lithium hydroxide, lithium chloride, lithium carbonate, lithium citrate, lithium acetate, and lithium formate.
3. The method for preparing the novel high specific surface area aluminum-based lithium adsorption precursor according to claim 1, characterized in that, In step 1, the aluminum source is selected from one or a mixture of several of the following: boehmite, aluminum chloride, aluminum hydroxide, sodium aluminate, aluminum hydroxyaluminate, and boehmite.
4. The method for preparing the novel high specific surface area aluminum-based lithium adsorption precursor according to claim 1, characterized in that, The selected surfactant includes one or a mixture of several of alkylbenzene sulfonates, alkylnaphthalene sulfonates, and succinate sulfonates, added in the solution in step 1 at an amount of 1%-5%.
5. The method for preparing the novel high specific surface area aluminum-based lithium adsorption precursor according to claim 1, characterized in that, In the lithium and aluminum sources, the molar ratio of aluminum to lithium is 2 to 2.2:
1.
6. The method for preparing the novel high specific surface area aluminum-based lithium adsorption precursor according to claim 1, characterized in that, Organic solvents include one or a mixture of several of the following: trichloroethylene, dimethylacetamide, methanol, acetone, and acetonitrile.
7. The method for preparing the novel high specific surface area aluminum-based lithium adsorption precursor according to claim 1, characterized in that, The amount of organic solvent used is 20-100 times the mass of the powder.