CN113663638A - Lithium ion adsorption caisson and preparation method and application thereof - Google Patents
Lithium ion adsorption caisson and preparation method and application thereof Download PDFInfo
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- CN113663638A CN113663638A CN202110881586.7A CN202110881586A CN113663638A CN 113663638 A CN113663638 A CN 113663638A CN 202110881586 A CN202110881586 A CN 202110881586A CN 113663638 A CN113663638 A CN 113663638A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/70—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/71—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being an organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
The invention discloses a lithium ion adsorption caisson and a preparation method and application thereof, and firstly proposes that a concrete surface coating applied to a marine environment is combined with a lithium adsorbent and is applied to a waste concrete material to obtain the lithium ion adsorption caisson which can be repeatedly used for a long time, so that the lithium ion adsorption caisson can adsorb lithium ions with low concentration and rich reserves in the sea while the waste concrete is reused; the preparation method of the lithium adsorbent is simple, and the steps are controllable; meanwhile, the adsorption caisson has excellent adsorption on low-concentration seawater lithium ions, and can be reused after simple acid leaching and washing treatment, thereby providing a new way for obtaining lithium resources by utilizing seawater resources.
Description
Technical Field
The invention belongs to the technical field of lithium ion adsorption, and particularly relates to a lithium ion adsorption caisson and a preparation method and application thereof.
Background
Lithium is an alkali metal with the smallest atomic radius and the lightest mass in nature, is silvery white, has special physical and chemical properties, and is widely applied to various fields of industry, agriculture, aerospace, medical treatment and the like. With the popularization of electronic products and the advocation of clean energy use, the usage amount of batteries is increasing day by day. The advantages of high energy density, high voltage, no pollution, no memory effect, long service life and the like of the lithium battery make the lithium battery become the most widely used battery at present. With the increase of the demand of each country for lithium batteries, the demand for lithium is directly and greatly improved, so that lithium becomes an important strategic resource.
The abundance of lithium in nature is low, and the total amount of the proven lithium resources in China is the fourth world and accounts for about 5.88 percent of the total amount of the globally proven lithium reserves. While global lithium resources are mainly present in lithium ores, salt lakes, and seawater. The mining and refining technology of lithium ore is not suitable for the development requirement of the current society due to the fact that energy consumption is too high and lithium ore resources are limited, so that the extraction of lithium in salt lake brine becomes a main way for obtaining lithium resources in recent years. However, with the increasing exhaustion of lithium resources in lithium ores and salt lakes, the abundant lithium resources in seawater become very important.
The method for extracting lithium from the aqueous solution mainly comprises a precipitation method, an evaporative crystallization method, a solvent extraction method, a calcination leaching method, a salting-out method, a carbonization method and an adsorbent method. The precipitation method uses chemical reagents such as carbonate and aluminate to perform precipitation reaction with each substance in the solution, so as to separate lithium from other impurities in the solution, but the method has complex process and difficult control of reaction conditions, and is not suitable for the solution with low lithium content. The solvent extraction method adopts various organic extracting agents with high lithium selectivity to obtain lithium in a solution, but the comprehensive benefit of obtaining lithium by the extraction method is not high due to the complicated extraction process, high cost of the extracting agents and environmental pollution. The calcination leaching method is to add soda ash to precipitate lithium after the solution is evaporated and concentrated, but the extraction cost is too high due to large evaporation energy consumption and complex process flow. The carbonization method is a method of precipitating impurities in a solution in addition to the precipitation method, but the conditions of the method are difficult to control, and the method cannot be used on a large scale. The adsorbent method is a method for extracting lithium from a solution by selecting a proper adsorbent, and the inorganic ion adsorbent has low cost, good adsorption effect and stable result, and is the most effective method for extracting lithium from a dilute solution. In the prior art, the preparation of the lithium adsorbent usually requires the synthesis of lithium-containing oxide, but the synthesis conditions are more delicate, which results in a complex synthesis process of the adsorbent.
Meanwhile, with the rapid development of economy in China, the number of infrastructure construction is continuously increased, and old buildings are dismantled and transformed in recent years, so that the use amount of concrete is continuously increased and a large amount of waste concrete is generated. From the perspective of green sustainable development, the reuse of waste concrete is particularly important. At present, the most common method for recycling waste concrete is to make the waste concrete become recycled aggregate by crushing or other means, and the recycled aggregate is used for producing concrete again, and no relevant report is found on the application of the concrete in absorbing lithium ions in seawater.
The invention provides the waste concrete lithium ion adsorption caisson which is simple in process and can be applied to the marine environment in a large scale, so that the waste concrete is recycled, and lithium ions with low concentration and rich reserves in the sea are adsorbed.
Disclosure of Invention
In view of the defects in the prior art, one of the purposes of the present invention is to provide a lithium ion adsorption caisson, wherein the adsorption caisson is prepared by coating a lithium adsorbent on a waste concrete test block, and is suitable for adsorption of lithium ions in seawater, and can realize reuse of waste concrete.
The invention also aims to provide the preparation method of the lithium ion adsorption caisson, which has the advantages of simple preparation process, controllable raw material consumption and convenient operation.
Another object of the present invention is to provide an application of the above lithium ion adsorption caisson for adsorbing lithium ions in seawater, which shows good adsorption performance both in indoor and practical engineering applications, is suitable for adsorbing lithium ions with low concentration but abundant reserves in the ocean, and has high application value.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a lithium ion adsorption caisson comprises the following steps:
(1) preparing a lithium adsorbent;
(2) uniformly brushing the coating on the surface of the waste concrete test block;
(3) uniformly coating the lithium adsorbent in the step (1) on the surface of the coating coated in the step (2);
(4) and (4) after the lithium-containing adsorbent coating is dried, placing the waste concrete test block obtained in the step (3) into a caisson to obtain the lithium ion adsorption caisson.
Preferably, the preparation of the lithium adsorbent in step (1) comprises the steps of:
s11, dissolving lithium acetate and manganese acetate in deionized water according to the Li/Mn molar ratio of 0.6-1, and then dropwise adding citric acid under the stirring condition to obtain transparent liquid;
s12, reacting the transparent liquid obtained in the step S11 at 60-100 ℃ for 0.5-4 h, drying at 120-180 ℃ for 8-16 h after the reaction is finished, and then grinding to obtain light yellow powder;
s13, heating and roasting the light yellow powder obtained in the step S12 in an air atmosphere at the temperature of 300-400 ℃ for 8-16 h, wherein the heating rate of the heating and roasting is 5 ℃/min, and grinding the roasted product to obtain black powder;
s14, soaking the black powder obtained in the step S13 in 0.5mol/L HCl solution, and then filtering to obtain dark red powder;
and S15, washing the dark red powder obtained in the step S14 with water until the dark red powder is neutral, and then drying the dark red powder to obtain the lithium adsorbent.
As a further preferable scheme of the invention, the molar ratio of the citric acid to the manganese acetate in the step S11 is 1.6-2.
Preferably, the coating in step (2) is a polyurea coating.
Preferably, 1g of lithium adsorbent is coated on every 500g of waste concrete test block in the step (3).
Preferably, the size of the caisson in the step (4) is 2 × 2 × 2m3。
The invention also claims the lithium ion adsorption caisson prepared by the method.
Meanwhile, the invention also claims the application of the lithium ion adsorption caisson prepared by the method in adsorption of lithium ions in seawater.
Preferably, the application comprises the steps of:
s21, placing the lithium ion adsorption caisson in seawater, and adsorbing for 30 days;
s22, taking out the waste concrete test block from the lithium ion adsorption caisson after adsorption in the step S21, performing acid leaching to obtain an acid solution containing lithium ions, and further extracting to obtain lithium;
s23, washing the waste concrete test block subjected to acid leaching in the step S22 with deionized water until the waste concrete test block is neutral, and then, adsorbing lithium ions again.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention firstly provides a new way for obtaining lithium resources by combining a concrete surface coating applied to a marine environment with a lithium ion adsorbent and applying the concrete surface coating to a waste concrete material to obtain a lithium ion adsorption caisson which can be repeatedly used for a long time.
(2) The adsorption caisson provides a new method for recycling the waste concrete and provides a new idea for green sustainable development.
(3) The adsorption caisson provided by the invention can adjust the concrete carrying capacity according to the concentration of lithium ions to be recovered, can select the size of a concrete test block, and is flexible to use.
(4) The preparation method of the lithium adsorbent provided by the invention is simple and controllable in steps.
(5) The lithium adsorbent provided by the invention has a good lithium adsorption effect, and the subsequent extraction process of lithium is simple and convenient, so that the lithium adsorbent can be applied to the engineering field in a large scale, and the cost advantage is outstanding.
Drawings
Fig. 1 is a graph showing phase characterization results of a lithium adsorbent according to the present invention.
FIG. 2 is a schematic diagram of the surface adsorption of lithium on the caisson of the present invention.
Fig. 3 is a schematic view of the caisson design of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly illustrated, the present invention will be further explained in detail with reference to the embodiments.
It should be noted that the experimental drugs according to the present invention were purchased commercially unless otherwise specified.
Example 1
A preparation method of a lithium adsorbent comprises the following steps:
(1) dissolving 0.5mol of lithium acetate and 0.8mol of manganese acetate in 1000ml of deionized water, and then dropwise adding 1.28mol of citric acid under the stirring condition to obtain transparent liquid;
(2) reacting the transparent liquid obtained in the step (1) at 80 ℃ for 2h, drying the transparent liquid at 150 ℃ for 12h after the reaction is finished, and then grinding the transparent liquid to obtain light yellow powder;
(3) placing the light yellow powder obtained in the step (2) in an air atmosphere, heating at a speed of 5 ℃/min, roasting at 350 ℃ for 12h, and then grinding to obtain black powder;
(4) soaking the black powder obtained in the step (3) in 0.5mol/L HCl solution for 24 hours, and then filtering to obtain dark red powder;
(5) and (4) washing the dark red powder obtained in the step (4) to be neutral, and then drying to obtain the lithium adsorbent.
Fig. 1 is a phase characterization result of the lithium adsorbent prepared in example 1.
Example 2
The lithium adsorbent prepared in example 1 was used for indoor lithium ion solution adsorption, and the adsorption test method was as follows:
s11, uniformly brushing the polyurea coating on the surface of a waste concrete test block, wherein the test block is a cylinder, the specification of the test block is 50 x 100mm, and the mass of the test block is about 500g, and then uniformly smearing 1g of the prepared lithium adsorbent on the surface of the polyurea coating; the polyurea coating is coated on the surface, so that the lithium adsorbent can be adsorbed more easily;
s12, after the lithium-containing adsorbent coating applied in the step S11 is dried, placing the waste concrete test block into a solution containing lithium ions;
and S13, taking out the waste concrete test block after the waste concrete test block is adsorbed for 7 days in the step S12, and measuring the lithium ion concentration of the solution again.
Experiments show that the concentration of the lithium ions before adsorption is 650.85mg/kg, the concentration of the lithium ions after 7 days of adsorption is 603.70mg/kg, and the adsorption efficiency is 7.24%.
Example 3
This example provides a method for preparing a lithium ion adsorption caisson by using the lithium adsorbent prepared in example 1, and as shown in fig. 2 and fig. 3, the lithium ion adsorption caisson is prepared by the following steps:
s21, uniformly brushing the polyurea coating on the surface of the waste concrete test block;
s22, uniformly applying the lithium adsorbent prepared in example 1 on the surface of the paint applied in step S21;
and S23, after the lithium-containing adsorbent coating is dried, placing the waste concrete test block obtained in the step S22 into a caisson to obtain the lithium ion adsorption caisson.
In this embodiment, specification and weight of abandonment concrete test block can be selected according to actual demand, and the homoenergetic realizes better adsorption effect.
In this embodiment, the amount of the lithium adsorbent is preferably 1g per 500g of the waste concrete block.
In this embodiment, the specification of the caisson is not particularly limited, and may preferably be 2 × 2 × 2m3Thus, a certain amount of concrete test blocks can be loaded, and the operation is relatively easy.
As a further preferable mode in this embodiment, there is no special requirement for the size and specification of the waste concrete test block, and it is sufficient that the waste concrete test block has a certain specific surface area.
As a further preferable scheme in the embodiment, the caisson has no special requirements, can bear a concrete test block with corresponding weight, has a certain anticorrosion function, and can be used for multiple times in a marine environment.
In this embodiment, there is no clear requirement for the loading capacity of the concrete test block, and flexible selection can be performed according to the specification and the adsorption requirement of the caisson, for example, 10t waste concrete test blocks can be loaded.
The lithium ion adsorption caisson prepared in the embodiment is used for adsorbing lithium ions in seawater, and comprises the following steps:
s31, placing the lithium ion adsorption caisson prepared in the embodiment in seawater, and adsorbing for 30 days to complete the adsorption of lithium ions;
s32, taking out the waste concrete test block from the lithium ion adsorption caisson after adsorption in the step S31, performing acid leaching to obtain an acid solution containing lithium ions, and further extracting to obtain lithium;
s33, washing the waste concrete test block subjected to acid leaching in the step S32 with deionized water until the waste concrete test block is neutral, and then, adsorbing lithium ions again.
It should be noted that, the further extraction of the lithium ion-containing acid solution in step S32 is the prior art, and the present invention does not limit the above extraction method, and can realize the enrichment extraction of lithium ions.
The above description describes the preferred embodiments of the present invention and should not be taken as limiting the scope of the invention as claimed. Any modification, equivalent replacement and improvement without departing from the principle and spirit of the present invention shall be considered to be within the protection scope of the present claims.
Claims (9)
1. A preparation method of a lithium ion adsorption caisson is characterized by comprising the following steps:
(1) preparing a lithium adsorbent;
(2) uniformly brushing the coating on the surface of the waste concrete test block;
(3) uniformly coating the lithium adsorbent prepared in the step (1) on the surface of the coating coated in the step (2);
(4) and (4) after the lithium-containing adsorbent coating is dried, placing the waste concrete test block obtained in the step (3) into a caisson to obtain the lithium ion adsorption caisson.
2. The method of claim 1, wherein the step (1) of preparing the lithium adsorbent comprises the steps of:
s11, dissolving lithium acetate and manganese acetate in deionized water according to the Li/Mn molar ratio of 0.6-1, and then dropwise adding citric acid under the stirring condition to obtain transparent liquid;
s12, reacting the transparent liquid obtained in the step S11 at 60-100 ℃ for 0.5-4 h, drying at 120-180 ℃ for 8-16 h after the reaction is finished, and then grinding to obtain light yellow powder;
s13, heating and roasting the light yellow powder obtained in the step S12 in an air atmosphere at the temperature of 300-400 ℃ for 8-16 h, wherein the heating rate of the heating and roasting is 5 ℃/min, and grinding the roasted product to obtain black powder;
s14, soaking the black powder obtained in the step S13 in 0.5mol/L HCl solution, and then filtering to obtain dark red powder;
and S15, washing the dark red powder obtained in the step S14 with water until the dark red powder is neutral, and then drying the dark red powder to obtain the lithium adsorbent.
3. The method according to claim 2, wherein the molar ratio of citric acid to manganese acetate in step S11 is 1.6-2.
4. The method of claim 1, wherein the coating in step (2) is a polyurea coating.
5. The method for preparing a lithium ion adsorption caisson according to claim 4, wherein 1g of lithium adsorbent is coated on every 500g of waste concrete sample in the step (3).
6. The method for preparing a lithium ion adsorption caisson according to claims 1 to 5, wherein the caisson in the step (4) has a specification of 2 x 2m3。
7. A lithium ion adsorption caisson prepared by the method of any one of claims 1 to 6.
8. Use of the lithium ion adsorption caisson of claim 7 for the adsorption of lithium ions in seawater.
9. Use according to claim 8, characterized in that it comprises the following steps:
s21, placing the lithium ion adsorption caisson in seawater, and adsorbing for 30 days;
s22, taking out the waste concrete test block from the lithium ion adsorption caisson after adsorption in the step S21, performing acid leaching to obtain an acid solution containing lithium ions, and further extracting to obtain lithium;
s23, washing the waste concrete test block subjected to acid leaching in the step S22 with deionized water until the waste concrete test block is neutral, and then, adsorbing lithium ions again.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985098A (en) * | 2010-09-16 | 2011-03-16 | 中南大学 | Method for preparing manganese series lithium-ion sieve adsorbent H4Mn5O12 and precursor thereof |
| US20140087071A1 (en) * | 2012-09-24 | 2014-03-27 | Korea Institute Of Geoscience And Mineral Resources | Ion-exchange manganese oxide lithium adsorbent using porous structure and method for preparing the same |
| CN105817195A (en) * | 2015-01-28 | 2016-08-03 | 韩国地质资源研究院 | Method manufacturing of lithium adsorbent with high surface area |
| CN108793203A (en) * | 2018-07-08 | 2018-11-13 | 南通四度化工贸易有限公司 | A kind of technique for extracting lithium from seawater |
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- 2021-08-02 CN CN202110881586.7A patent/CN113663638A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985098A (en) * | 2010-09-16 | 2011-03-16 | 中南大学 | Method for preparing manganese series lithium-ion sieve adsorbent H4Mn5O12 and precursor thereof |
| US20140087071A1 (en) * | 2012-09-24 | 2014-03-27 | Korea Institute Of Geoscience And Mineral Resources | Ion-exchange manganese oxide lithium adsorbent using porous structure and method for preparing the same |
| CN105817195A (en) * | 2015-01-28 | 2016-08-03 | 韩国地质资源研究院 | Method manufacturing of lithium adsorbent with high surface area |
| CN108793203A (en) * | 2018-07-08 | 2018-11-13 | 南通四度化工贸易有限公司 | A kind of technique for extracting lithium from seawater |
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| Title |
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| 祁鲁梁 等: "《水处理工艺与运行管理实用手册》", 31 May 2002, 北京：中国石化出版社 * |
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