CN108525636B - Adsorbent for rapid adsorption and desorption, preparation and application in lithium/rubidium adsorption - Google Patents
Adsorbent for rapid adsorption and desorption, preparation and application in lithium/rubidium adsorption Download PDFInfo
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Abstract
The invention discloses an adsorbent for rapid adsorption and desorption, a preparation method and an application in lithium/rubidium adsorption, wherein a powder adsorbent is mixed with a hydrophilic polymer and water, heated and dissolved into a viscous liquid-solid mixture, and the viscous liquid-solid mixture is dripped into a phase conversion agent in a liquid drop form to form a spherical nascent state adsorbent through solution phase conversion; and drying the nascent adsorbent at low temperature under reduced pressure, and adding the nascent adsorbent into a solution containing a chemical cross-linking agent for cross-linking reaction to obtain the high-hydrophilicity adsorbent. The method provided by the invention has simple and convenient operation process and low price and easy obtainment of raw materials. The prepared high-hydrophilicity adsorbent has stable property, low dissolution loss rate and high adsorption and desorption rates.
Description
Technical Field
The invention belongs to the technical field of adsorbent preparation, and particularly relates to an adsorbent capable of rapidly adsorbing and resolving, preparation and application in lithium/rubidium adsorption.
Background
Lithium metal and compounds thereof play more and more important roles in national economy and national defense construction, and more than 80% of lithium resources are stored in salt lake brine and seawater, so that research on extracting lithium from the salt lake brine has great strategic significance on development and utilization of the lithium resources. The method for extracting lithium by the ion sieve adsorption method has the characteristics of stable circulation, high selectivity, high adsorption capacity and the like, low cost and the like, and becomes one of the most promising methods for extracting lithium from salt lake brine in China. However, most of the ion sieve adsorbent is powder, and the fluidity and permeability of the ion sieve adsorbent are poor, so that the direct application of the ion sieve adsorbent to a fixed bed for adsorbing and extracting lithium has certain difficulty, and therefore, the forming of the ion sieve powder is the key for realizing the industrialization of extracting lithium by using the ion sieve.
The forming agent in the current ion sieve adsorbent is a plurality of hydrophobic polymers such as PVC or PVDF, on one hand, the affinity between the hydrophobic polymers and inorganic adsorbent powder is small, and the powder is easy to fall off. On the other hand, because the polymer has strong hydrophobicity, water molecules are not easy to carry exchanged ions to enter the content of the adsorbent, so that an ion sieve or an ion exchanger in the adsorbent cannot be effectively contacted and exchanged with water, the adsorption quantity of the adsorbent is low, and the adsorption rate and the desorption rate are slow. The production efficiency is seriously affected. Therefore, how to maintain the performance of the powder ionic sieve in the forming process becomes a key problem for industrialization of lithium extraction placed in the ionic sieve.
The method for preparing the spherical lithium ion sieve adsorbent in the prior art is generally prepared by preparing the spheres and crosslinking, but the obtained adsorbent cannot be repeatedly used in the crosslinking process and the reaction process is long. For example, "CN 103212388A gel ball type rubidium/cesium ion adsorbent, its preparation method and application" provide a forming technique for preparing rubidium ion adsorbent by using hydrophilic polymer such as alginic acid as embedding agent, and the rubidium ion adsorbent is prepared by complexing sodium alginate with calcium ion in calcium chloride solution and precipitating. However, calcium alginate is decomplexed when meeting strong acid, carbonate or sulfate, so the adsorbent prepared by the method is decomposed when meeting acid, and therefore, the method cannot be applied to the preparation of the lithium ion adsorbent for resolving lithium by acid. Meanwhile, the rubidium ion adsorbent prepared by the method can not be applied to solutions containing carbonate radicals or sulfate radicals, such as lepidolite lithium extraction raffinate, lithium carbonate precipitation raffinate and the like, for extracting rubidium ions or lithium ions.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a rapid adsorbent, a preparation method and application for adsorbing rubidium ions or lithium ions, and solves the problems of low adsorption and desorption speed, low adsorption capacity, dissolution loss in repeated use of the conventional adsorbent and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a rapid adsorbent comprises mixing powder adsorbent with hydrophilic polymer and water, heating to dissolve into viscous liquid-solid mixture, dripping into phase inversion agent in the form of liquid drop, and performing solution phase inversion to form spherical nascent adsorbent; and drying the nascent adsorbent at low temperature under reduced pressure, and adding the nascent adsorbent into a solution containing a chemical cross-linking agent for cross-linking reaction to obtain the rapid adsorbent.
Optionally, the hydrophilic polymer is hydroxyethyl cellulose or sodium carboxymethyl cellulose;
the powder adsorbent is a lithium ion sieve or rubidium ion exchanger, wherein the mass ratio of the powder adsorbent to the hydrophilic polymer is 1-2/1, and the water-solid ratio is 100/20-50.
Optionally, the lithium ion sieve is LixMn3-xO4The manganese oxide lithium ion sieve of (1), wherein x is 1.6, 1.33, or 1; the rubidium ion exchanger is ammonium phosphomolybdate or ammonium tungstomolybdate.
Optionally, the phase inversion agent and the water-soluble organic solvent are mutually soluble; the pressure of the low-temperature reduced pressure drying is 0.1MPa, and the temperature is 30-60 ℃.
Optionally, the solution of the chemical crosslinking agent is a sodium hydroxide aqueous solution with the mass concentration of 5-10% of epoxy chloropropane being 10%, and the temperature of the crosslinking reaction is 30-60 ℃.
The adsorbent is prepared by the preparation method of the rapid adsorbent.
The adsorbent prepared by the preparation method of the rapid adsorbent is applied to adsorption extraction of lithium ions and/or rubidium ions in brine, seawater and rubidium-mica mineral powder acid leaching solution.
Optionally, the conditions for adsorbing and extracting lithium ions are a lithium-containing solution with a pH of 8-10, and the analysis conditions are a hydrochloric acid solution of 0.3-0.5 mol/L.
Optionally, the adsorption for adsorbing and extracting rubidium ions is performed in a neutral rubidium-containing solution, and the resolving condition is an ammonium chloride solution with a mass concentration of 20%.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a method for embedding a powdery lithium ion sieve or rubidium ion exchanger by using a hydrophilic polymer, which effectively solves the problem of dissolution loss of a powdery lithium ion or rubidium ion adsorption material in the process of adsorbing and extracting lithium or rubidium.
(2) The invention provides a product obtained by using a hydrophilic polymer to prepare a lithium/rubidium ion adsorbent, which effectively solves the problem that the adsorption performance of the adsorbent is influenced because an ion sieve cannot be effectively contacted with water to generate ion exchange because the ion sieve is coated by hydrophobic polymers such as PVC (polyvinyl chloride) or PVDF (polyvinylidene fluoride) in the prior art;
(3) the method for forming polyether crosslinking reaction by condensation reaction of the alkaline solution of epoxy chloropropane and hydroxyl in a hydrophilic polymer chain can stably exist in weakly acidic or weakly alkaline solution, can resist the solution environment containing sulfate radicals and carbonate radicals, can be widely applied to extraction of lithium/rubidium ions from seawater, brine, lepidolite and stone acid leaching raffinate and lithium carbonate precipitation raffinate, and has strong production applicability.
(4) The adsorbent prepared by the method can generate good hydrogen bond action with water, so that the lithium/rubidium-containing aqueous solution can effectively perform ion exchange with the adsorbent in the adsorbent, and therefore, the adsorption rate is high, and the resolution rate is high. Is a product for extracting lithium and rubidium with high performance.
(5) The invention has simple production process and mild operation condition; high production efficiency and low cost. For another example, CN103316623A, "a method for preparing spherical lithium ion sieve adsorbent", includes: heating, dissolving and mixing the polysaccharide and the solvent, adding the ionic sieve precursor into the solution, and uniformly stirring to obtain a viscous solution; dripping the viscous solution into an oil phase at 50-100 ℃ to obtain a solid spherical adsorbent with the particle size of 2-5 mm; placing the spherical adsorbent in a cross-linking agent, cross-linking for 10-30 h at 20-80 ℃, filtering and washing to obtain cross-linked spherical MnO2 adsorbent particles; and eluting the adsorbent particles in a lithium removal solvent to finally prepare the spherical lithium ion sieve adsorbent. The polysaccharide is selected in the preparation method, the reaction process is long (crosslinking is carried out for 10-30 h), the reaction temperature is high and the oil phase is dripped at 50-100 ℃, but the method disclosed by the invention is fast in reaction (30min), and the phase conversion process can be completed at normal temperature, so that the types of all the raw materials and the proportion relation among all the reaction conditions are creatives.
Also, in "a method for preparing a spherical granular lithium ion sieve" of CN106084102A, the method comprises the following steps: step (1): mixing and dissolving a dispersing agent and water to obtain a water phase; step (2): adding a powdery lithium ion sieve into the water phase obtained in the step (1), stirring and heating, and then adding an oil phase containing a monomer and an initiator to perform suspension polymerization reaction; the monomer comprises styrene; and (3): and (3) after the reaction in the step (2) is finished, continuously heating to harden the spherical particles prepared by the suspension polymerization reaction, and sequentially washing, drying, pickling, washing and drying the hardened particles to obtain the spherical lithium ion sieve. It can be seen that the forming agent in the existing forming ion sieve adsorbent is rich in hydrophobic polymers such as PVC, PVDF, styrene and the like, so that the ion sieve cannot effectively contact and exchange with water, the adsorption rate and the adsorption quantity of the adsorbent are reduced, and the embedded powder is easy to fall off. Therefore, how to maintain the performance of the powder ionic sieve in the forming process becomes a key problem for industrialization of lithium extraction placed in the ionic sieve; the adsorbent prepared by adjusting the factors such as raw materials, dosage, preparation parameters and the like has the function of repeated crosslinking and repeated use, ensures high-efficiency adsorption of the adsorbent, and has quick adsorption and desorption processes.
"CN 102671634A a modified cellulose adsorbent and its preparation method and application" provides a modified cellulose adsorbent and its preparation method and application, including the following steps: (1) pretreatment: cleaning cellulose raw materials, air drying, slicing and crushing; (2) pretreatment: carrying out alkali liquor-ultrasonic treatment on the cellulose powder; (3) reaction: adding epoxy chloropropane, reacting for 1h at the temperature of 100-; (4) and (3) finished product: and cooling the reacted feed liquid, then washing the solution with water until the solution is neutral, filtering and drying the solution to obtain the target adsorbent. The production method disclosed in this document is also different from the present invention, and the adsorbent produced using a fibrous material as a raw material is different from the technical problems to be solved by the present invention.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure without limiting the disclosure. In the drawings:
FIG. 1 is a graph of the morphology of the adsorbents prepared in example 1, (a)500 times, (b)1000 times;
FIG. 2 is a graph of the morphology of the adsorbents prepared in example 2, (a)500 times, (b)1000 times;
the invention is described in detail below with reference to the drawings and the detailed description.
Detailed Description
The invention discloses a preparation method of a rapid adsorbent, which specifically comprises the following steps: directly mixing powder adsorbent (such as powdered lithium ion adsorbent or rubidium ion adsorbent) with hydrophilic polymer and water, heating to dissolve to form uniform liquid-solid mixture, dripping into phase conversion agent in the form of liquid drop, and performing solution phase conversion to form spherical nascent adsorbent; and adding the nascent-state adsorbent into an alkaline solution of epoxy chloropropane for chemical crosslinking reaction to obtain the rapid adsorbent.
The rapid adsorbent prepared by the invention is mainly used for adsorbing and extracting rubidium ions or lithium ions from seawater, brine, lepidolite acid leaching lithium extraction raffinate, lithium carbonate precipitation lithium extraction raffinate and the like.
The following embodiments of the present invention are provided, and it should be noted that the present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention are within the protection scope of the present invention.
Example 1:
10g of hydroxyethyl cellulose and 10g of manganese-based lithium ion sieve adsorbent precursor Li1.6Mn1.6O4Mixing, heating with 50g water to 100 deg.C, stirring to obtain uniform viscous liquid-solid solution, manually extruding with a syringe, and dripping into tetrahydrofuran solution as phase inversion agent for phase inversion reaction for 3min to obtain ballForming solid particles to obtain the nascent state lithium ion spherical adsorbent.
Drying the nascent spherical adsorbent at 60 ℃ under the negative pressure of 0.1MPa, adding the nascent spherical adsorbent into a sodium hydroxide aqueous solution with the mass concentration of 5% of epichlorohydrin and the mass concentration of 10%, heating the mixture to react at 50 ℃ for 30min, and taking out the mixture to obtain the spherical high-hydrophilicity lithium ion adsorbent.
The morphology of the adsorbent is shown in fig. 1, fig. 1(a) is a 500-fold magnified surface morphology of the adsorbent, and fig. 1(b) is a 1000-fold magnified surface morphology of the adsorbent.
The prepared spherical lithium ion adsorbent is used for separating and recovering lithium ions in brine. The actual brine contains various ions: li+The concentration is 200Mg/L, Mg2+The concentration is 23g/L, K+The concentration is 15g/L, Na+The concentration is 110g/L, 3g (wet weight, powder adsorbent content is 0.615g) of spherical adsorbent is used for adsorption at the flow rate of 2mL/min, the lithium content in the effluent liquid after 60min is the same as that of the original liquid, indicating that the adsorption reaches the balance, and the average adsorption quantity of the adsorbent to lithium is 6.8mg/g (calculated according to the mass of the powder adsorbent) according to the materials in the mother liquid after adsorption. After 30min of desorption in 0.3mol/L hydrochloric acid solution at the same flow rate, no lithium ions were detected in the effluent, indicating that the desorption had reached equilibrium. The K/Li ratio in the resulting analysis liquid was 4/1, the Na/Li ratio was 17/1, and the Mg/Li ratio was 6/1. The resolution was 92%. The equilibrium adsorption quantity of lithium is still stabilized at 6.5mg/g when the adsorbent is repeatedly used for four times.
Example 2:
10g of sodium carboxymethylcellulose and 10g of manganese-based lithium ion sieve adsorbent precursor LiMn2O4Mixing, heating with 50g water to 80 deg.C, stirring to form uniform viscous liquid-solid solution, manually extruding with injector, dripping into phase inversion agent tetrahydrofuran solution, and performing phase inversion reaction for 3min to obtain spherical solid particles to obtain nascent state lithium ion spherical adsorbent.
Drying the nascent spherical adsorbent at 60 ℃ under the negative pressure of 0.1MPa, adding the nascent spherical adsorbent into a 10% sodium hydroxide aqueous solution of 5% epichlorohydrin by mass-volume ratio, heating the mixture to react for 60min at 50 ℃, and taking out the mixture to obtain the spherical high-hydrophilicity lithium ion adsorbent.
The morphology of the adsorbent is shown in fig. 2, where fig. 2(a) is a 500-fold magnified map of the surface of the adsorbent, and fig. 2(b) is a 1000-fold magnified map of the surface of the adsorbent.
The prepared spherical lithium ion adsorbent is used for separating and recovering lithium ions in brine. The actual brine composition was the same as in example 1, and 3g of the adsorbent (wet weight, 0.615g powder adsorbent content) was packed in the column and the flow rate was set at 2 mL/min. After 120min adsorption reaches equilibrium, the average adsorption quantity of the adsorbent to lithium is 4.6mg/g (calculated by the mass of the powder adsorbent) according to the material in the mother liquor after adsorption. The solution was analyzed at the same flow rate for 120min to reach equilibrium in a 0.5mol/L hydrochloric acid solution, and the analysis rate was found to be 90%. When the adsorbent is repeatedly used for four times, the equilibrium adsorption quantity of lithium is stabilized at 4.5 mg/g.
Example 3:
10g of hydroxyethyl cellulose and 12.3g of manganese lithium ion sieve adsorbent precursor Li4Mn5O12Mixing, heating to 100 ℃ by 50g of water, stirring to form uniform and viscous liquid-solid solution, manually extruding by using an injector, dripping into tetrahydrofuran solution as a phase conversion agent, drying spherical solid particles after the phase conversion reaction for 30min at 60 ℃ under the negative pressure of 0.1MPa, adding into 10 mass percent sodium hydroxide aqueous solution of 5 mass percent epichlorohydrin, heating to react for 30min at 40 ℃, and taking out to obtain the spherical high-hydrophilicity lithium ion adsorbent.
The prepared spherical lithium ion adsorbent was loaded into a column (65 g of loading amount, wet weight, 12.3g of powder adsorbent content), the flow rate was set to 2mL/min, the adsorption was performed with the same brine as in example 1, the adsorption was balanced after 4 hours, and the adsorption amount was measured to be 12mg/g (based on the mass of the powder adsorbent). The solution is analyzed for 3h at the flow rate of 3mL/min by 0.5M hydrochloric acid solution, the analysis rate reaches 92 percent, the solution is repeatedly used for four times, and the adsorption quantity is stabilized to be about 10 mg/g.
The preferred embodiments of the present disclosure are described in detail with reference to the accompanying drawings, however, the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present disclosure within the technical idea of the present disclosure, and these simple modifications all belong to the protection scope of the present disclosure.
It should be noted that, in the foregoing embodiments, various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various combinations that are possible in the present disclosure are not described again.
In addition, any combination of various embodiments of the present disclosure may be made, and the same should be considered as the disclosure of the present disclosure, as long as it does not depart from the spirit of the present disclosure.
Claims (5)
1. A preparation method of a rapid adsorbent is characterized in that a powder adsorbent is mixed with a hydrophilic polymer and water, heated and dissolved into a viscous liquid-solid mixture, and the viscous liquid-solid mixture is dripped into a phase conversion agent in a liquid drop form to form a spherical nascent adsorbent through solution phase conversion; drying the nascent adsorbent at low temperature under reduced pressure, and adding the nascent adsorbent into a solution containing a chemical cross-linking agent for cross-linking reaction to obtain a rapid adsorbent;
the hydrophilic polymer is hydroxyethyl cellulose or sodium carboxymethyl cellulose;
the powder adsorbent is a lithium ion sieve or rubidium ion exchanger, wherein the mass ratio of the powder adsorbent to the hydrophilic polymer is 1-2/1, and the water-solid ratio is 100/20-50;
the lithium ion sieve is LixMn3-xO4The manganese oxide lithium ion sieve of (1), wherein x is 1.6, 1.33, or 1; the rubidium ion exchanger is ammonium phosphomolybdate or ammonium tungstomolybdate;
the phase inversion agent and the organic solvent which can be mutually dissolved by water; the pressure of the low-temperature reduced pressure drying is 0.1MPa, and the temperature is 30-60 ℃;
the solution of the chemical crosslinking agent is a sodium hydroxide aqueous solution with the mass concentration of 5-10% of epoxy chloropropane being 10%, and the temperature of the crosslinking reaction is 30-60 ℃.
2. An adsorbent, characterized in that it is prepared by the method of claim 1.
3. The use of the adsorbent prepared by the method of claim 1 for adsorption extraction of lithium ions and/or rubidium ions from brine, seawater and acid leaching solution of rubidium mica ore powder.
4. The use according to claim 3, wherein the condition for adsorbing and extracting lithium ions is a lithium-containing solution with pH 8-10, and the desorption condition is 0.3-0.5 mol/L hydrochloric acid solution.
5. The use of claim 3, wherein the adsorption for the adsorptive extraction of rubidium ions is in a neutral rubidium-containing solution under conditions of 20% by mass ammonium chloride solution.
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| CN110804120B (en) * | 2019-11-15 | 2021-02-26 | 四川大学 | Gel microsphere with ultrahigh cleaning capability on positively charged toxins and preparation method thereof |
| CN113509918B (en) * | 2020-11-25 | 2022-06-10 | 中国科学院青海盐湖研究所 | Preparation method of heteropolyacid salt ion sieve adsorbent particles for extracting liquid rubidium and cesium resources |
| CN115738892B (en) * | 2022-11-30 | 2023-06-02 | 中国科学院青海盐湖研究所 | Spherical combined lithium adsorbent and granulating method thereof |
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Effective date of registration: 20211220 Address after: 710068 Room 301, Shaanxi Membrane Separation Technology Research Institute, No. 13, middle section of Yanta Road, Beilin District, Xi'an City, Shaanxi Province Patentee after: Xi'an jinzang membrane Environmental Protection Technology Co.,Ltd. Address before: Room S205, innovation building, No.25, Gaoxin 1st Road, high tech Zone, Xi'an, Shaanxi 710068 Patentee before: SHAANXI MEMBRANE SEPARATION TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. |