LITHIUM ADSORBENT, PREPARATION METHOD, AND AN APPLICATION.

Abstract

This description outlines a lithium adsorbent preparation method and an application related to lithium extraction techniques. The method described involves obtaining a lithium adsorbent intermediate by mixing an oil phase with an aqueous phase; and obtaining a lithium adsorbent by mixing the lithium adsorbent intermediate with an organic auxiliary; where the oil phase contains a lithium source, an aluminum source, an oil phase matrix, and an oil phase auxiliary, and the oil phase matrix contains a high molecular weight polymer and vinylidene fluoride; mixing an oil phase with an aqueous phase involves performing gradient mixing on the oil phase and aqueous phase mixture. According to the description, a lithium adsorbent with high stability can be prepared by optimizing and screening a high-temperature resistant oil phase matrix and a specific preparation process.Compared to an existing lithium adsorbent, the lithium adsorbent prepared through the specification exhibits less degradation, better mechanical strength, and stronger corrosion resistance in high-temperature environments, thus providing a way to effectively extract lithium resources from high-temperature and high-salt brine.

Description

1 TARIFF LITHIUM ADSORBENT, PREPARATION METHOD, AND AN APPLICATION. Technical Scope of the Invention 5 This specification pertains to the technical field of lithium extraction, and specifically to a lithium extract. regarding the adsorbent, a preparation method and its application It has been arranged. Invention Foundation 10 Lithium resources are currently considered as key emerging resources. However, due to the persistent imbalance between supply and demand, this will remain the case for a long time in the future. A shortage in this area is also quite possible. Therefore, geothermal resources... Lithium extraction has become a new topic of discussion in this field. 15 for extracting the element lithium from high-temperature geothermal brine. Because the physical and chemical stability of adsorbents needs to be resolved, Extracting lithium from geothermal brine is a very difficult process. The physical characteristics of existing lithium adsorbents in a high-temperature environment are being evaluated. Damage, chemical attenuation, etc., are likely to occur, which makes lithium adsorbents... shortens the service life and industrial use of lithium adsorbents 20 This leads to very high costs. In high-temperature salt water an adsorbent that can be used stably and can efficiently remove lithium Its development is considered an urgent matter. This specification has been prepared taking into account the points mentioned above. Summary of the Invention The purpose of this specification is to describe a lithium adsorbent and a method for its preparation. and to provide an application of this. Specifications are provided as follows: In the examples in the specification, from the first point of view, a lithium adsorbent 30 is included in this scope. 2 The preparation method is provided. The method involves the following steps: mixing an oil phase with water. a lithium adsorbent intermediate is obtained by mixing it excessively and Mixing lithium adsorbent intermediate with an organic excipient Obtaining lithium adsorbent by means of; where the oil phase is a lithium source, and a lithium adsorbent is used. The aluminum source includes an oil-phase matrix and an oil-phase auxiliary agent. 5 It has an oil phase matrix containing high molecular weight polymer and vinylidene fluoride; an oil a phase mixing step with an aqueous phase, gradient on the oil phase and aqueous phase mixture It involves performing mixing, and the gradient mixing step is the initial stage of mixing. It involves mixing at a specific speed; where the initial mixing speed is 30 rpm. It is in the range of 190 rpm; 10 after mixing for the initial fixation time of the mixture. The mixing process is stopped for each second fixation period; each After stopping, the mixing speed is reduced to the 1st set rotation speed, then The mixture is continuously stirred until the stirring speed is equal to the second set rotation speed. or the mixing process is stopped until the mixture is less than this; here, 2. The adjustable rotation speed is between 10 rpm and 30 rpm; the adjustable rotation speed is 2 to 15. While being protected, it is stirred at 40°C to 120°C for periods ranging from 20 minutes to 600 minutes. Secondly, a lithium adsorbent is provided in the sample specifications. Lithium adsorbent prepared using the method described in the example above. It contains a lithium adsorbent. From a third perspective, according to the example above, the lithium adsorbent has 20% lithium. in the extraction or preparation of a product used in the extraction of lithium The implementation is being carried out. The specification has the following beneficial effects: According to the specifications, a new preparation process was developed, allowing for high temperatures. Screening of a durable organic matrix and a special preparation process with a high 25 Stable lithium adsorbents are being prepared within this scope. An existing lithium lithium adsorbent prepared via specification compared to adsorbent. less deformation, better mechanical strength, and suitability for high-temperature environments. It has stronger corrosion resistance and therefore can withstand high temperatures and high salt concentrations. One way to effectively extract lithium resources from saline water containing 30 3 has been provided. Figures that Aid in Explaining the Invention Examples of technical solutions included in the specification. In order to explain it more clearly, 5 examples are needed to illustrate the points. A brief description of the drawings will be given below. In this context, the following are given: the drawings only show some examples of the specification and therefore It should be understood that its scope should not be considered restrictive. This Individuals with average technical skills can achieve this without requiring creative effort. Besides the drawings provided, they can also create related drawings themselves. 10 Figure 1 shows an electron microscope image of a lithium adsorbent prepared in Example 1. It is an image. Disclosure of the Invention The purposes, technical solutions, and 15 examples within the scope of the specification In order to make the advantages more understandable, in the sample specifications Technical solutions will be explained clearly and completely below. The examples in question are: Unless specific conditions are stated, the usual conditions or those recommended by the manufacturer shall apply. This is carried out according to the requirements within the scope of the conditions in question. The manufacturer's Unless otherwise specified, the reagents or devices used are available on the market. These are conventional products. A new lithium adsorbent, prepared through specification, can withstand a high temperature of 80°C. 2000 or more adsorption and analysis cycles in salt water at high temperature It may not show any decrease afterwards. A conventional lithium adsorbent, at a high temperature of 80°C... After 100 or more adsorption and analysis cycles in saline solution at a certain temperature, 25 It shows a significant decrease. In one respect, preparing a lithium adsorbent in the examples covered by the specification. The method is provided. This method involves mixing an oil phase with an aqueous phase. This involves obtaining a lithium adsorbent intermediate by mixing them. lithium adsorbent, lithium adsorbent intermediate with an organic excipient 30 4 It is obtained by mixing; here oil phase, a lithium source, an aluminum source, an oil phase matrix and a It contains an oil phase excipient, and the oil phase matrix is ​​a high molecular weight matrix. It contains polymer and vinylidene fluoride; The step of mixing the oil phase with the aqueous phase has a 5-degree effect on the oil phase and aqueous phase mixture. This involves performing gradient mixing, and the gradient mixing step is: This involves mixing the mixture at the initial mixing speed; where the initial The mixing speed is between 30 rpm and 190 rpm; the mixing of the mixture, the initial mixing of the mixture After mixing for the fixation time, each time for the second fixation time The mixing speed is stopped; after each stop, the mixing speed is adjusted to the set rotation speed of 10. is reduced, then the mixture continues to be stirred and the stirring speed is set to setting 2. The mixing of the mixture is not stopped until the rotational speed is equal to or less than the rotational speed. Here, the second set rotation speed is between 10 rpm and 30 rpm, and the second set rotation speed... The speed is maintained and the mixture is kept between 40°C and 120°C for 20 minutes to 600 minutes. They are mixed. A polymerization process improves the lithium aluminum oxide crystallites. 15 can bind and polymerize vinylidene fluoride in oil droplets, A smoother texture is obtained by gradually reducing the mixing speed. The mixing speed is adjusted after vinylidene fluoride polymerization begins. This reduces the polymer content within the oil droplets. Their structures do not collapse significantly, and in this way, aluminum and 20 escape into the aqueous phase. The amount of lithium can be reduced. The lithium adsorbent prepared using the method described in the specification is essentially It exhibits high temperature resistance in two aspects: firstly, from vinylidene. fluoride, in a high-temperature environment by selecting a special organic matrix. It is unlikely to decompose. Lithium aluminum hydroxide (lithium aluminum oxide) 25 The crystals are a resin with a low probability of causing chemical degradation, like an oil-phase matrix. It bonds better by mixing the matrix with the high molecular weight polymer. Active The amount of desorption from the crystals is less due to the tighter bonding. High Adsorption and analysis at high temperatures, as well as a small skeleton in the organic matrix. a change occurs. Also, adsorption at high temperature and at low temperature 30 The analysis shows that the contraction and expansion of the organic skeleton are smaller. This happens. Accordingly, repeated exposure of lithium ions in a high-temperature environment Adsorption and desorption cause less structural damage. Second In this respect, a special preparation process is utilized. Lithium adsorbent intermediate In the process of preparing the material, mixing the oil phase with the aqueous phase is step 5. When gradient mixing is used in the process, lithium in the adsorbent particles In this case, aluminum oxide crystallites are more uniformly distributed. This Therefore, the binding force is stronger in the active inorganic regions. The escape of aluminum and lithium is reduced, and lithium chloride at high temperatures Adsorption and desorption become more stable in this environment. 10 In some examples, the initial mixing speed is 30 rpm, 40 rpm, 60 rpm, 80 rpm, 100 rpm. any of the following: 120 rpm, 140 rpm, 160 rpm, 170 rpm, 180 rpm, and 190 rpm Or it could be somewhere in between. In some cases, the initial setup time ranges from 20 minutes to 120 minutes. The initial setup time is specifically 20 minutes, 40 minutes, 60 minutes, 80 minutes, 100 minutes and 15 minutes. It can be within any one of the 120-minute intervals, or somewhere in between. In some cases, the second setting time is between 20 minutes and 120 minutes. It is within a range. The second setting time is specifically 20 minutes, 40 minutes, 60 minutes, 80 minutes, It can be between 100 minutes and 120 minutes, or anywhere in between. In some examples, the set rotation speed is a 20 between 10 rpm and 30 rpm. It is within the range. The adjustable rotation speed is 1, 10 rpm, 12 rpm, 14 rpm, 16 rpm, 18 rpm, 20 rpm, Any one or two of the following: 22 rpm, 24 rpm, 26 rpm, 28 rpm, and 30 rpm. It could be in December. In some examples, the set rotation speed is between 2, 10 rpm and 30 rpm. It is within the range. The adjustable rotation speed is 2, 10 rpm, 12 rpm, 14 rpm, 16 rpm, 18 rpm, 20 rpm, 25 rpm. Any one or two of the following: 22 rpm, 24 rpm, 26 rpm, 28 rpm, and 30 rpm. It could be in December. In some cases, the mixing temperature reaches 40°C before the set rotation speed is 2. The temperature range is 80°C. Mixing temperatures are particularly suitable at 40°C, 42°C, 44°C, 46°C, and 48°C. 50°C, 52°C, 54°C, 56°C, 58°C, 60°C, 62°C, 64°C, 66°C, 68°C, 70°C, 72°C, 74°C, 30 6 It can be in the range of 76°C, 78°C, and 80°C, or between any two of these. In some cases, mixing occurs after maintaining the set rotation speed of 2. The temperature is any value, or 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, Any of 75°C, 80°C, 85°C, 90°C, 95°C, 100°C, 105°C, 110°C, 115°C and 120°C It is in the range between the two. 5 In some examples, the high molecular weight polymer in the oil phase matrix is ​​vinylidene. The mass ratio of fluoride is 5:(1-10). The mass ratio can be any one or 5:1, In any two intervals between 5:2, 5:3, 5:4, 5:5, 5:6, 5:7, 5:8, 5:9 and 5:10 it could be. In some examples, the high molecular weight polymer polyacrylamide, polyacrylic acid, 10 polyacrylate, polyurethane, polyester, polyether, polystyrene, polyenol, phenolic resin, and epoxy It contains one or more of these resins. It is more resistant to vinylidene fluoride. Polystyrene or polyacrylate, which have a strong affinity, are preferred, so that the prepared The adsorbent's strength will be improved. In some examples, the sum of the lithium and aluminum sources is 15% of the oil. The mass ratio of the excipient in the phase is (3-18):10. The mass ratio is specifically It could be any of them, or 3:10, 4:10, 6:10, 8:10, 10:10, 12:10, 14:10, 16:10 and It could be somewhere in between 18:10 and any two points. In some examples, the oil phase excipient N-methylpyrrolidone and an organic Contains solvent. 20 In some examples, the mass ratio of N-methylpyrrolidone to organic solvent is (1-5):1. The mass ratio can be any one of the following: 1:1, 2:1, 3:1, 4:1, or 5:1. It could be somewhere in between the two. In some examples, the organic solvent in the oil phase excipient is methanol, ethanol, acetone, gasoline, N,N-dimethylformamide, ethyl acetate, dichloromethane, chloroform, 25 benzene, toluene, isopropanol, and diethyl ether, or any more of these. includes. In some examples, the volume ratio of the oil phase to the aqueous phase is 1:(1-3). Volume The ratio can be any one specifically, or any two of 1:1, 1:2, and 1:3. It could be within a range between 30. 7 In some examples, the molar ratio of lithium source to aluminum source is 5:(1-10). The molar ratio can be any one of the following: 5:1, 5:2, 5:3, 5:4, 5:5, 5:6, 5:7, 5:8, It could be somewhere between 5:9 and 5:10. In some examples, the lithium source contains a lithium salt. In some examples, lithium sources include lithium chloride, lithium nitrate, lithium carbonate, 5 lithium sulfate, lithium hydroxide, lithium acetate, and lithium oxide, or any of these. It includes several. In some examples, the aluminum source contains an aluminum salt. Some examples include aluminum source, aluminum chloride, aluminum nitrate, aluminum carbonate, aluminum sulfate, aluminum hydroxide, aluminum acetate and 10 It contains one or more types of aluminum oxide. In some instances, the oil phase also acts as an initiator and a pore former. It contains at least one of these substances. In some examples, the initiators are benzoyl peroxide, cumene hydroperoxide, and tert-butyl. It contains one or more of the hydroperoxides. 15 In some examples, pore-forming agents include white oil, liquid wax, gasoline, and It contains any one or more of the n-points. In some examples, the aqueous phase contains water and a dispersant. In some examples, the mass-to-volume fraction of the dispersant in the aqueous phase is between 0.1% and 2%. It varies within this scope. Mass-volume fraction, special 20 as 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 1.0%, 1.2%, 1.4%, 1.6%, It could be in a range between 1.8% and 2%, or both. More specifically... Mass-to-volume fraction = g / mL × 100%. In some examples, the dispersant is made from carboxymethyl cellulose and hydroxyethyl cellulose. Includes any one or more of these. 25 In some cases, after the oil phase is mixed with the aqueous phase, the resulting lithium is obtained. Before the step of mixing the adsorbent intermediate with the organic excipient, The method also involves mixing the oil phase with the aqueous phase to obtain a detergent product. This also includes removing the pore-forming substance by washing with water.1 Some examples include detergent 1, methanol, ethanol, acetone, gasoline, 30 8 N,N-dimethylformamide, ethyl acetate, dichloromethane, chloroform, benzene, toluene, It contains one or more of isopropanol and diethyl ether. In some examples, the organic excipients include polyvinyl alcohol, polylactic acid, and cellulose. acetate, ethyl cellulose, polyvinyl chloride, polycarbonate, vinyl alcohol-ethylene cellulose copolymer and any one or more of an ethylene-propylene polymer 5 includes. In some examples, the lithium adsorbent intermediate is combined with an organic auxiliary material. The mass ratio is 20:(1-8). The mass ratio can be any one or 20:1, 20:2, It could be anywhere between 20:3, 20:4, 20:5, 20:6, 20:7, and 20:8. In some examples, the lithium adsorbent intermediate is mixed with an organic excipient 10 The mixing condition is a temperature between 30°C and 80°C and an hour between 1 and 6 hours. It includes duration. The temperature is specifically 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, It can be between 75°C and 80°C, or in between both. The duration is especially 1 hours, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours and It could be any one or both of those six hours. 15 In some cases, the method also involves organic lithium adsorbent intermediates. During mixing with the excipient, a polar organic substance is added to the mixing system. It involves the addition of solvent. Some examples include the polar organic solvents ethanol, N,N-dimethylformamide, and acetonitrile. and contains one or more of isopropanol. 20 In some samples, the concentration of the polar organic solvent ranges from 15% to 35%. It varies between them. Concentration, specific as 15%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34% and 35% It could be in the range of either one or both. In some examples, the method also involves the organic 25 lithium adsorbent intermediate. After mixing with the excipient, the lithium adsorbent intermediate The product obtained after mixing with organic auxiliary substances is detergent 2. It includes washing with [the product / service]. In some examples, detergent 2 contains water and / or an organic solvent. Optional. as such, the organic solvent in detergent 2 is methanol, ethanol, acetone, gasoline, 30 9 N,N-dimethylformamide, ethyl acetate, dichloromethane, chloroform, benzene, toluene, isopropanol, N-methylpyrrolidone, and diethyl ether, or any more of these. includes. In some cases, the method also involves washing the product with detergent 2, The process involves washing the product with detergent 2, drying it, and obtaining the lithium adsorbent. 5 From another perspective, the samples covered by the specification also contain lithium. The adsorbent is provided. Lithium adsorbent, any of the above described. The sample contains lithium adsorbent prepared using the method described. Furthermore, compared to any of the examples described above, the lithium adsorbent 10 of a product used in the extraction of lithium or for the extraction of lithium The application in its preparation is further demonstrated in the examples provided in the explanation. In some cases, the extraction of lithium involves extracting lithium at high temperatures. It includes. In some examples, the high temperature is in the range of 50°C to 85°C and is specific. as any of 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C and 85°C or It could be somewhere in between. 15 In some cases, the lithium extraction process involves high-temperature geothermal salts. It also includes the process of extracting lithium from water. The specifications and performance details are further elaborated below, with examples. This is explained as follows. Example 1 20 The lithium adsorbent preparation method involves the following steps. (1) Oil phase First, add 100 mL of a mixed solution of N,N-dimethylformamide and N-methylpyrrolidone. (oil phase auxiliary agent) 50 g of aluminum chloride (an aluminum source) was added; Here, the mass ratio of N,N-dimethylformamide to N-methylpyrrolidone was 1:4. 25 Secondly, 70 mL of a 3 mol / L LiOH solution (a lithium source) is mixed in. added and then an oil phase matrix (30 g polystyrene + 30 g vinyl fluoride) It was added and mixed until dissolved, thus obtaining an oil phase. 2 by adding 40 gr benzoyl peroxide (initiator) and 40 gr liquid wax (pore-forming agent) The final oil phase was obtained by mixing for 30 minutes. (2) Aqueous phase First, 300 mL of water was poured into a 2000 mL reaction vessel, and 0.5 g was added to it. It was dissolved by mixing with the addition of carboxymethyl cellulose (a dispersant), so that The aqueous phase formed. (3) Lithium adsorbent intermediate 5 The oil phase liquid above was poured into the aqueous phase, and the oil phase liquid was formed into spheres. Gradient mixing was used to ensure rapid dispersion. Gradient mixing involves increasing the temperature. The temperature should be raised to 60°C, the initial stirring speed should be 180 rpm; the mixture... Stop stirring for 10 minutes every 2 hours, then restart the mixture. When mixing, the mixing speed should be reduced by 20 rpm (minimum rotation speed) and 10 Repeat the process until the mixing speed is less than or equal to 20 rpm; raising the temperature to 80°C and letting the reaction proceed at 20 rpm for 2 hours. after the containment and heat protection are completed, the spherical particles It includes filtering. (4) Lithium adsorbent 15 First, 200 grams of isopropanol (detergent 1) is added to the spherical particles to form a liquid. The wax (pore-forming substance) was washed away. Then 15 g of polylactic acid (organic (auxiliary substance) in 300 g of polar organic solvent containing water and ethanol (volume ratio 1:1) A mixed solution was obtained by dissolving it. 100 g of it was added to the reaction vessel. The spherical particles found and the mixed solutions weighing 300 grams were added. 20 The temperature was raised to 70°C for a 6-hour reaction. Finally, one product was mixed with acetone. (detergent 2) was washed and spherical adsorbents were obtained by removing acetone with water. Adsorbents with particle sizes of 0.6 mm–2.0 mm were eliminated as test products. The electron microscope image of the lithium adsorbent prepared in the example is shown in Figure. It is shown in 1. 25 Column chromatography adsorption experiment based on saline solution. This was carried out. See Table 1 for the components of the brine. 11 Table 1. Composition of salt water. Ion content (ppm) Lithium Cation m Magn ezyu m Calcium m Sodium Potassium egg Stronsi egg Baryu m Also mir Table of contents er 248.9 2512 6 31910 89201 1583 2 631 2.3 5.9 Borate Anion (B(OH) 4- ) Chloride ion Sulfate radical Bikar bonat radical Ali Bromine r ion Fluoride ion - Table of contents er 3235 22261 0 34 562 1902 15 - Salt water was heated for adsorption; here, the adsorption rate is 3 bed volumes. (BV) / hour, adsorption capacity of saltwater is 8 BV and 1-5 adsorptions. After the cycle, the average lithium loading capacity of the resin is 2.31 g / L. It was at that level. Then, on the resin, the salt water was 80°C and the water was 40°C. 5 300 cycles of saltwater-water impact test using a permeability testing device The test was carried out. After the test was completed, the mass loss of the adsorbent was 0.14%. It was at that level. Under the same conditions, the average lithium loading after 5 cycles. Its capacity was retested and found to be 2.27 g / L. Example 2 10 Lithium adsorbents, lithium adsorbent preparation method according to Example 1. It was prepared in 5 experimental groups determined by reference. 1st experimental group Sample The process was carried out as in Example 1, and groups 2-4 were carried out as in Example 1; the differences are as follows: This is shown in Table 2. After the lithium adsorbents were prepared, they were saline-based. Column chromatography adsorption experiments were conducted, and the components of the saline solution were 15. This is shown in Table 1. The salt water was heated for adsorption; where adsorption occurred. The rate is 3 BV / hour, the adsorption capacity of saltwater is 8 BV, and the adsorption rate is 1-5 BV. After the cycle, the average lithium loading capacity of the resin is 2.01 g / L. It was found. Then, saline solution was tested on the resin using a resin life cycle testing device. A saltwater impact test consisting of 300 cycles was conducted where the water temperature was 80°C and the surface temperature was 40°C. 20 The results in this context are shown in Table 2. Table 2. Experimental group 12 Group numa between Oil phase in step (1) auxiliary substance Step (1) oil phase matrix In step (3) gradient mixing done not done I, beginning to mix up speed and gradient mixing each of them reduction amount 300 cycle -most later adsorption direction amount decrease I 300 cycle -most later mass decrease I cycle -most later in hand done average a lithium loading capacity si and same conditions under again test 1 N,N-dimethylformamide din N-methyl mass of pyrrolidone rate :1:4 gr polystyrene + 30 gr vinylidene fluoride Yes 180 rpm, rpm / 1 s 1.7% 0.14% 2.27 g / L 2N,N-dimethylformamide din N-methyl mass of pyrrolidone rate :1:4 60g polystyrene Yes 180 rpm, rpm / 1 s 36.7% 9.34% 1.47g / L 3N,N-dimethylformamide din N-methyl mass of pyrrolidone rate :1:4 gr polystyrene + 30 gr vinylidene fluoride No 8.8% 3.25% 1.94 g / L 4N,N-dimethylformamide din N-methyl mass of pyrrolidone rate :1:1 40 grams of polystyrene + 20 gr vinylidene fluoride Yes 180 rpm, rpm / 1 s 4.1% 2.1% 1.87 g / L N,N-DIMETHYLFORM AMID gr polystyrene + 30 gr polyurethane No 23.8% 7.1% 1.32 g / L 6N,N-dimethylformamide din N-methyl mass of pyrrolidone rate :1:4 gr polystyrene + 30 gr vinylidene fluoride Yes 180 rpm, rpm / 1 s 7.6% 4.52% 1.96 g / L 7N,N-dimethylformamide din N-methyl mass of pyrrolidone rate :1:4 gr polystyrene + 30 gr vinylidene fluoride Yes 90 rpm, rpm / 1 s 5.7% 6.13% 1.88 g / L 13 No gradient mixing was performed in Group 3. Step (3) was specifically as follows: The oil phase liquid was poured into an aqueous phase and rapidly formed into spheres by adjusting the mixing speed. The mixture was dispersed; the temperature was raised to 60°C, and then the mixture was stirred. Here, the mixing speed was 180 rpm; the reaction lasted for 8 hours. This was carried out, then the temperature was increased to 80°C and stirred at a speed of 180 rpm for 2 5 minutes. The reaction was carried out for an hour; then, after the heat protection ended, global The particles were filtered. The above are only examples chosen within the scope of the specification, However, it is not intended to restrict the specification. Experts in the field, They may make various changes and variations to the description. The spirit of the specification and 10 Any changes, equivalent renewals, improvements, etc., made in accordance with its principles. The disclosure should be covered by protection.

Claims

14 REQUESTS 1. A method for preparing a lithium adsorbent that involves: mixing an oil phase with an aqueous phase. to obtain a lithium adsorbent intermediate by mixing excessively; and lithium adsorbent Lithium adsorbent is obtained by mixing the intermediate with an organic auxiliary substance. to do; here 5 oil phase, a lithium source, an aluminum source, an oil phase matrix and a It contains an oil phase auxiliary agent and the oil phase matrix is ​​a high molecular polymer and It contains vinylidene fluoride; The step of mixing an oil phase with an aqueous phase involves: the oil phase and the aqueous phase. Performing a gradient mixing process on the mixture and 10 The gradient mixing step involves: the mixture at the initial mixing speed. The mixing process here has an initial mixing speed between 30 rpm and 190 rpm; The mixing of the mixture must be stopped each time for the initial setting time; each After stopping, the mixing speed is reduced to the set rotation speed of 1, Then, continue stirring the mixture and adjust the stirring speed to 15. Interrupt the mixing of the mixture until the rotation speed is less than or equal to 2. not being given, the rotation speed set here is 2, which is between 10 rpm and 30 rpm; and maintaining the set rotation speed of 2 and 20 minutes at 40°C to 120°C with 600 Mixing between minutes.

2. A method for preparing a lithium adsorbent according to claim 1, with an initial setup time of 20°C. It is within a range of between 1 minute and 120 minutes; The second set duration is optional, between 20 and 120 minutes. It is changing; Optionally, the adjustable rotation speed can be between 1, 10 rpm and 30 rpm. is in December; and 25 Optionally, mixing before maintaining the set rotation speed of 2. Its temperature ranges from 40°C to 80°C.

3. A method for preparing a lithium adsorbent according to Claim 1, in an oil-phase matrix. The mass ratio of the high molecular polymer to vinylidene fluoride is 5:(1-10); Optionally, high molecular weight polymer polyacrylamide, polyacrylic acid, polyacrylate, polyurethane, polyester, polyether, polystyrene, polyenol, phenolic resin, and epoxy It contains one or more of the following resins; 5 Optionally, the sum of lithium and aluminum sources can be used for oil. The mass ratio of the excipient in the phase is (3-18):10; Optionally, the oil phase excipient includes: N-methylpyrrolidone and an organic solvent; Optionally, the mass ratio of N-methylpyrrolidone to organic solvent is (1-5):1; 10 Optionally, the organic solvent in the oil phase excipient is methanol. ethanol, acetone, gasoline, N,N-dimethylformamide, ethyl acetate, dichloromethane, chloroform, benzene, toluene, isopropanol, and diethyl ether, or any more of these. includes.

4. According to claims 1, 2 or 3, the volume ratio of the oil phase to the aqueous phase mixture is 1:(1-3) This is the method used; Optionally, the molar ratio of lithium source to aluminum source. 5:(1-10) Optionally, the lithium source includes a lithium salt; 20 Optionally, lithium sources include lithium chloride, lithium nitrate, and lithium carbonate. lithium sulfate, lithium hydroxide, lithium acetate, and lithium oxide, or any of these. It includes several; Optionally, the aluminum source includes an aluminum salt; and Optionally, aluminum source, aluminum chloride, aluminum nitrate, 25 aluminum carbonate, aluminum sulfate, aluminum hydroxide, aluminum acetate and It contains one or more types of aluminum oxide. 16 5. According to claims 1, 2 or 3, the oil phase also acts as an initiator and a pore. a method that contains at least one of the constituent substances; Optionally, the initiators are benzoyl peroxide, cumene hydroperoxide, and tert-butyl. contains one or more of the hydroperoxides; Optionally, pore-forming agents such as white oil, liquid wax, gasoline, and 5 can be used. It contains any one or more of the n-points; Optionally, the aqueous phase includes water and a dispersant; Optionally, the mass-to-volume fraction of the dispersant in the aqueous phase can be between 0.1% and 2%. It varies within this scope. Optionally, the dispersant can be 10% carboxymethyl cellulose and hydroxyethyl cellulose. includes any one or more of these; Optionally, after mixing the oil phase with the aqueous phase, the resulting lithium can be obtained. Before the step of mixing the adsorbent intermediate with the organic excipient, The method also involves mixing the oil phase with the aqueous phase to obtain a detergent product. This also includes removing the pore-forming substance by washing with water1 and; 15 Optionally, detergent 1, methanol, ethanol, acetone, gasoline, N,N-dimethylformamide, ethyl acetate, dichloromethane, chloroform, benzene, toluene, It contains one or more of isopropanol and diethyl ether.

6. According to claims 1, 2 or 3, the organic excipient is polyvinyl alcohol, polylactic acid, 20 cellulose acetate, ethyl cellulose, polyvinyl chloride, polycarbonate, vinyl alcohol-ethylene cellulose copolymer and either or more of an ethylene-propylene polymer the method it involves; Optionally, the lithium adsorbent intermediate can be combined with an organic auxiliary material. mass ratio is 20:(1-8) and 25 Optionally, the lithium adsorbent intermediate can be combined with an organic auxiliary substance. The mixing requirements include a temperature of 30°C to 80°C and a time period of 1 to 6 hours. 17 7. Method according to claim 1, 2 or 3, where the lithium adsorbent intermediate is organic. During mixing with the excipient, a polar organic substance is added to the mixing system. This also involves the addition of the solvent; Optionally, polar organic solvents ethanol, N,N-dimethylformamide, 5 It contains either or both of acetonitrile and isopropanol; Optionally, the method can also incorporate an organic lithium adsorbent intermediate. After mixing with the excipient, the lithium adsorbent intermediate The product obtained after mixing with organic auxiliary substances is detergent 2. It includes washing with [the cleaning agent]. 10 Optionally, detergent 2 contains water and / or an organic solvent; Optionally, the organic solvent in detergent 2 can be methanol, ethanol, or acetone. gasoline, N,N-dimethylformamide, ethyl acetate, dichloromethane, chloroform, benzene, toluene, isopropanol, N-methylpyrrolidone, and diethyl ether, or any more of these. includes and 15 Optionally, the method can also be followed by washing the product with detergent 2, The process involves washing the product with detergent 2, drying it, and obtaining the lithium adsorbent.

8. Containing lithium adsorbent prepared by method according to any of claims 1-7. It is a lithium adsorbent. 20 9. Lithium adsorbent according to claim 8, used for the removal of lithium or for the absorption of lithium. It is applied in the preparation of a product used in extraction.

10. According to claim 9, the extraction of lithium involves extracting lithium at a high temperature. 25 includes; and Optionally, in the samples, the lithium extraction process can be carried out at high temperature. 18 It also includes the process of extracting lithium from geothermal brine.

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