CN116196882A - Preparation method of titanium lithium ion sieve - Google Patents
Preparation method of titanium lithium ion sieve Download PDFInfo
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- CN116196882A CN116196882A CN202310380471.9A CN202310380471A CN116196882A CN 116196882 A CN116196882 A CN 116196882A CN 202310380471 A CN202310380471 A CN 202310380471A CN 116196882 A CN116196882 A CN 116196882A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention provides a preparation method of a titanium lithium ion sieve, which belongs to the technical field of ion sieves, and adopts potassium acetate as a potassium source, and the potassium acetate and meta-titanic acid are pulped together, dried and roasted at high temperature to prepare a potassium meta-titanate precursor; adding hydrochloric acid eluent into a certain mass of potassium metatitanate precursor for eluting, and adding hydrochloric acid solution in the eluting process to keep the pH value of the slurry between 1.3 and 2.0; stopping adding acid after the pH of the slurry is kept stable; centrifuging and washing the obtained slurry, drying the obtained solid, and pulverizing to obtain H 2 TiO 3 . The potassium salt is used for replacing a lithium source, the selectivity of the synthesized lithium ion sieve to lithium ions is not reduced, the interlayer spacing is moderately widened under the condition of ensuring the selectivity not to be reduced, the adsorption capacity is large, the cycle performance is stable, the synthesis cost is reduced, and the method is suitable for industrial production; solves the problems of the preparation of titanium-series lithium adsorbentHigh cost, low adsorption capacity and slow adsorption rate.
Description
Technical Field
The invention relates to the technical field of ion sieves, in particular to a preparation method of a titanium lithium ion sieve with high adsorption capacity and low cost.
Background
Lithium is used as the lightest metal element in the nature, and has high utilization value and wide application field due to excellent physical and chemical properties. The lithium and the salt compound thereof are widely applied to the fields of chemical industry, glass, ceramics, aerospace, new energy sources and the like, so that the development and utilization of lithium resources become a great hot spot.
There are mainly two methods for synthesizing the ion sieve precursor, a solid phase method and a liquid phase method. The high temperature solid phase method is one of the most common methods for preparing the precursor of the ion sieve, and mainly comprises the steps of carrying out solid phase reaction on salt which is easy to melt and decompose at a high temperature to generate oxide, and respectively, melting and fusing the salt of two different ions at a high temperature to continuously react with each other to form powder with small particle size. The ion sieve is prepared by adopting an adsorption method after the needed powder is synthesized, and the adsorption method has the characteristics of high selectivity, capability of processing brine with low lithium content and realization of clean production, and is simple in process and high in recovery rate, thereby being very suitable for extracting lithium from salt lake water.
The titanium-based lithium ion sieve adsorbent is an adsorption material with high selectivity to lithium ions, and the synthesis of the titanium-based lithium ion sieve is generally carried out by adopting a lithium source (a lithium-containing compound) and a titanium source (a titanium-containing compound) as raw materials, but the lithium salt is expensive, so that the industrial production cost of the titanium-based lithium ion sieve is too high. Therefore, it is necessary to adjust the raw materials to prepare the adsorbent with low cost, high adsorption, low solvent loss and high cycle performance.
Disclosure of Invention
The invention aims to provide a preparation method of a titanium lithium ion sieve with high adsorption capacity and low cost, so as to solve at least one technical problem in the prior art.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a preparation method of a titanium lithium ion sieve, which comprises the following steps:
adopting potassium acetate as a potassium source, pulping with metatitanic acid, drying, and roasting at high temperature to prepare a potassium metatitanate precursor;
adding hydrochloric acid eluent into a certain mass of potassium metatitanate precursor for eluting, and adding hydrochloric acid solution in the eluting process to keep the pH value of the slurry between 1.3 and 2.0;
stopping adding acid after the pH of the slurry is kept stable;
centrifuging and washing the obtained slurry, drying the obtained solid, and pulverizing to obtain H 2 TiO 3 。
Preferably, the potassium acetate solution is added with the meta-titanic acid and anatase type TiO 2 Adding PEG200, mixing, performing ultrasonic treatment in water bath, oven drying, grinding, and calcining to obtain K 2 Ti 6 O 13 A precursor.
Preferably, 50-100g of potassium acetate is added into 200ml of deionized water, and stirred at normal temperature until the potassium acetate is dissolved to obtain a potassium acetate solution.
Preferably, 110-240g of meta-titanic acid and 45-50g of anatase type TiO are added into the potassium acetate solution 2 。
Preferably, the mass of PEG200 added is 4-10g.
Preferably, the water temperature of 50-60 ℃ is treated for 20-30min by ultrasonic, the oven is dried for 6-10 h at 110-130 ℃, and the sample is taken out after the full drying and is transferred into a crucible for grinding.
Preferably, grinding and then transferring into a muffle furnace, heating up to calcine, wherein the heating up rate is 2-10 ℃/min, heating up to 500-650 ℃, calcining for 4-8h, heating up to 700-900 ℃ and calcining for 4-8h, thus obtaining the catalyst with high specific surface area, large adsorption capacity and high selectivityK of (2) 2 Ti 6 O 13 A precursor.
Preferably, a certain mass of potassium metatitanate precursor is taken, 0.05-0.1mol/L hydrochloric acid eluent is added, the feeding ratio is kept at 10-20g/L, and the solution is subjected to oscillation elution for 1-2h at the temperature of 50-60 ℃.
Preferably, 0.5-2mol/L hydrochloric acid solution is used for supplementing and keeping the pH value of the slurry between 1.3 and 2.0 in the elution process, and the acid solution is exchanged for two times to prevent K + The suck-back occurs at too high a concentration.
Preferably, stopping adding acid after the pH of the slurry is kept stable, centrifuging the obtained slurry, washing for 4-5 times, drying the obtained solid in a 50-60 ℃ oven, and pulverizing to obtain H 2 TiO 3 。
The invention has the beneficial effects that: the potassium salt is used for replacing a lithium source, the selectivity of the synthesized lithium ion sieve to lithium ions is not reduced, the interlayer spacing is moderately widened under the condition of ensuring the selectivity not reduced, the adsorption capacity is large, the cycle performance is stable, the synthesis cost is reduced, and the method is suitable for industrial production; solves the problems of high preparation cost, low adsorption capacity and low adsorption rate of the titanium-based lithium adsorbent.
The advantages of additional aspects of the invention will be set forth in part in the description which follows, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a process for preparing a potassium meta-titanate precursor according to an embodiment of the present invention.
Figure 2 is an XRD pattern of the resulting precursor according to example 1 of the present invention.
Fig. 3 is a schematic diagram of electron microscope scanning of the obtained precursor according to example 1 of the present invention.
FIG. 4 is a schematic illustration of an embodiment of the present inventionLi as described in example 1 + Schematic of adsorption rate curve.
FIG. 5 is a graph showing the cycle number versus Li according to example 1 of the present invention + Schematic of the effect of adsorption.
Figure 6 is an XRD pattern of the resulting precursor according to example 2 of the present invention.
Fig. 7 is a schematic diagram of electron microscope scanning of the obtained precursor according to embodiment 2 of the present invention.
FIG. 8 is a diagram of Li according to example 2 of the present invention + Schematic of adsorption rate curve.
FIG. 9 is a graph showing the cycle number versus Li according to example 2 of the present invention + Schematic of the effect of adsorption.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements throughout or elements having like or similar functionality. The embodiments described below by way of the drawings are exemplary only and should not be construed as limiting the invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless expressly stated otherwise, as understood by those skilled in the art. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, and/or groups thereof.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
In order that the invention may be readily understood, a further description of the invention will be rendered by reference to specific embodiments that are illustrated in the appended drawings and are not to be construed as limiting embodiments of the invention.
It will be appreciated by those skilled in the art that the drawings are merely schematic representations of examples and that the elements of the drawings are not necessarily required to practice the invention.
As shown in fig. 1, in this embodiment, a low-cost, high-adsorption capacity, high-selectivity and high-adsorption rate preparation method for a titanium-based lithium ion sieve is provided as follows:
preparing a titanium lithium ion sieve precursor: and (3) taking potassium acetate as a potassium source, pulping with metatitanic acid, drying, and roasting at high temperature to prepare the potassium metatitanate precursor.
The preparation of the titanium lithium ion sieve precursor specifically comprises the following steps: adding 55-100g of potassium acetate into 200ml of deionized water, stirring at normal temperature until the potassium acetate is dissolved, slowly adding 111-238g of metatitanic acid and 45-50g of anatase TiO 2 Adding 4-10g of PEG200 into the solution, fully mixing, carrying out ultrasonic treatment at the water temperature of 50-60 ℃ for 20-30min, drying for 6-10 h at the temperature of 110-130 ℃ in an oven, taking out a sample after fully drying, transferring the sample into a crucible, fully grinding, transferring the sample into a muffle furnace, calcining by adopting programmed heating, wherein the heating rate is 2-10 ℃/min, firstly rising to 500-650 ℃, calcining for 4-8h, and then rising to 700-900 ℃ and calcining for 4-8h, thereby obtaining the high-specific surface area and high adsorption capacityHigh selectivity K 2 Ti 6 O 13 A precursor.
Adding a certain mass of precursor into a beaker, respectively adding 0.05-0.1mol/L hydrochloric acid eluent, keeping the feeding ratio at 10-20g/L, carrying out shake elution at 50-60 ℃ for 1-2h, adding 0.5-2mol/L hydrochloric acid solution in the process to keep the pH value of the slurry at 1.3-2.0, and replacing acid liquor twice in the middle to prevent K + The suck-back occurs at too high a concentration. Stopping adding acid after the pH of the slurry is kept stable. Centrifuging the obtained slurry, washing for 4-5 times, drying the obtained solid in a 50-60deg.C oven, and pulverizing to obtain H 2 TiO 3 Titanium-based lithium ion sieves of (2).
Example 1
55g of potassium acetate was added to 200ml of deionized water and stirred at room temperature until dissolved. 111g of meta-titanic acid and 45g of anatase TiO were added 2 To the above solution, 4g of PEG200 was added to a beaker containing the sample and thoroughly mixed, sonicated at 50℃for 20min, and oven dried at 110℃for 10h. Taking out the sample after being sufficiently dried, transferring the sample into a crucible, sufficiently grinding the sample, transferring the sample into a muffle furnace, calcining the sample by adopting programmed heating, wherein the heating rate is 4 ℃/min, the temperature is firstly increased to 500 ℃, the calcining is carried out for 4 hours, then the calcining is carried out for 8 hours at 700 ℃, and cooling and grinding are carried out, thus obtaining K with high specific surface area, large adsorption capacity and high selectivity 2 Ti 6 O 13 A precursor. The XRD pattern of the precursor obtained in this example is shown in FIG. 2, and compared with that of the standard card PDF#74-0275, the precursor obtained is K 2 Ti 6 O 13 . Precursor K 2 Ti 6 O 13 The microstructure of (2) is shown in fig. 3, and it can be seen that the obtained precursor is nano-sized particles with uniform particle size distribution.
Adding a certain mass of precursor into a beaker, respectively adding 0.05mol/L hydrochloric acid eluent, keeping the feeding ratio at 20g/L, performing shake elution at 50 ℃ for 1h, adding 2mol/L hydrochloric acid liquid in the process to keep the pH value of the slurry at 1.3-2.0, and changing the acid liquid twice in the middle to prevent K + The suck-back occurs at too high a concentration. Stopping adding acid after the pH of the slurry is kept stable. Centrifuging the slurry, washing for 4 times to obtain solidOven drying at 50deg.C, pulverizing to obtain H 2 TiO 3 。
Li + Adsorption performance test: the adsorption performance was tested using 1L of laboratory self-assembled brine (containing lithium chloride (4.45 g), sodium silicate nonahydrate (0.21 g), anhydrous sodium sulfate (84.92 g), anhydrous sodium carbonate (15.57 g), sodium chloride (28.39 g), calcium chloride (0.19 g), magnesium chloride (8.93 g), potassium chloride (12.78 g)). 20g of the titanium-series lithium ion sieve in the first embodiment is soaked in 1L of laboratory prepared brine and stirred continuously, water samples are taken every 20min, and Li in the water samples is tested by ICP + Content of Li in water sample + The adsorption balance is the case when the content is no longer changed. The adsorption rate curve is shown in FIG. 4, and when the adsorption is carried out for 140min, the adsorption reaches equilibrium, the equilibrium adsorption amount is 31mg/g, and the adsorption capacity of the titanium-based lithium ion sieve is high.
Taking 2g of the lithium adsorbent adsorbed in the first case, maintaining the feeding ratio of 20g/L, analyzing the adsorbed sample, taking a sample every half an hour by adopting 0.1mol/L hydrochloric acid solution as an analysis solution, and testing Li in the sample by ICP + ，K + ，Ca 2+ ，Na + ，Mg 2+ The content and selectivity data are shown in Table 1. From table 1, it can be concluded that the lithium adsorbent obtained still has a high selectivity by replacing the lithium source with potassium salt.
Table 1 experimental case-ion concentration of adsorption stock solution and analytical solution
TABLE 2 ion concentration ratio of analytical solution for experimental case
The recycling performance of the material has great influence on the running cost of industrial operation, so that the research experiment on the recycling adsorption performance of the lithium ion sieve is shown in fig. 5, the adsorption performance floats in the interval of 29.5-31mg/g for 9 times in a recycling way, the phenomenon of rapid attenuation of the adsorption capacity does not occur, and the titanium lithium ion sieve adsorbent obtained by the experiment method has good recycling performance, and the performance ensures that the titanium lithium ion sieve can realize stable running of a system in the actual use process.
Example 2
100g of potassium acetate was added to 200ml of deionized water and stirred at room temperature until dissolved. Slowly add 238g of meta-titanic acid and 50g of anatase TiO 2 Adding 10g of PEG200 into a beaker with a sample, fully mixing, carrying out ultrasonic treatment at 60 ℃ for 30min, drying at 130 ℃ for 6h in a baking oven, taking out the sample after fully drying, transferring into a crucible, fully grinding, transferring into a muffle furnace, adopting programmed heating and calcining, wherein the heating rate is 5 ℃/min, firstly heating to 650 ℃, calcining for 8h, then heating to 900 ℃ and calcining for 4h, cooling, crushing and grinding, thereby obtaining K with high specific surface area, large adsorption capacity and high selectivity 2 Ti 6 O 13 A precursor. The XRD pattern of the precursor obtained in this example II is shown in FIG. 6, and compared with that of the standard card PDF#74-0275, the precursor obtained is K 2 Ti 6 O 13 . Precursor K 2 Ti 6 O 13 The microstructure of (2) is shown in fig. 7, and it can be seen that the obtained precursor is nano-sized particles with uniform particle size distribution.
Adding a certain mass of precursor into a beaker, respectively adding 0.1mol/L hydrochloric acid eluent, keeping the feeding ratio at 10g/L, stirring and eluting at 60 ℃ for 2 hours, adding 0.5mol/L hydrochloric acid solution in the process to keep the pH value of the slurry between 1.3 and 2.0, and changing the acid liquor twice to prevent K + The suck-back occurs at too high a concentration. Stopping adding acid after the pH of the slurry is kept stable. Centrifuging the obtained slurry, washing for 5 times, drying the obtained solid in a 60 ℃ oven, and pulverizing to obtain H 2 TiO 3 。
Li + Adsorption performance test: the adsorption performance was tested using laboratory self-assembling brine, in which the components and amounts were the same as in example one. 10g of the lithium adsorbent in example I is soaked in 1L of laboratory prepared brine and stirred continuously, water samples are taken every 20min, and Li is tested by ICP + Content of when waterLi in sample + The adsorption balance is the case when the content is no longer changed. The adsorption curve is shown in FIG. 8, and when the adsorption is carried out for 120min, the adsorption reaches equilibrium, the equilibrium adsorption amount is 35mg/g, and the adsorption capacity of the titanium-based lithium ion sieve is high.
Taking 2g of the lithium adsorbent adsorbed in the second case, keeping the feeding ratio at 10g/L, analyzing the adsorbed sample, taking a sample every half an hour by adopting 0.1mol/L hydrochloric acid solution as an analysis solution, and testing Li by ICP + ，K + ，Ca 2+ ，Na + ，Mg 2+ The content and selectivity data are shown in Table 3. As can be seen from tables 3 and 4, the lithium adsorbent obtained by replacing the lithium source with potassium salt has high selectivity.
TABLE 3 ion concentration of adsorption stock solution and analytical solution for experimental case two
TABLE 4 ion concentration ratio of the two analytical solutions for experimental cases
The recycling performance of the material has great influence on the running cost of industrial operation, so that the research experiment on the recycling adsorption performance of the lithium ion sieve is shown in fig. 9, the adsorption performance floats within the interval of 34-35.2mg/g for 9 times, the phenomenon of rapid attenuation of the adsorption capacity does not occur, and the titanium lithium ion sieve adsorbent obtained by the experiment method has good recycling performance, and the performance ensures that the titanium lithium ion sieve can realize the stable running of the system in the actual use process.
While the foregoing description of the embodiments of the present invention has been presented in conjunction with the drawings, it should be understood that it is not intended to limit the scope of the invention, but rather, it should be understood that various changes and modifications could be made by one skilled in the art without the need for inventive faculty, which would fall within the scope of the invention.
Claims (10)
1. The preparation method of the titanium lithium ion sieve is characterized by comprising the following steps:
adopting potassium acetate as a potassium source, pulping with metatitanic acid, drying, and roasting at high temperature to prepare a potassium metatitanate precursor;
adding hydrochloric acid eluent into a certain mass of potassium metatitanate precursor for eluting, and adding hydrochloric acid solution in the eluting process to keep the pH value of the slurry between 1.3 and 2.0;
stopping adding acid after the pH of the slurry is kept stable;
centrifuging and washing the obtained slurry, drying the obtained solid, and pulverizing to obtain H 2 TiO 3 。
2. The method for preparing a titanium-based lithium ion sieve according to claim 1, wherein the potassium acetate solution is added with meta-titanic acid and anatase type TiO 2 Adding PEG200, mixing, performing ultrasonic treatment in water bath, oven drying, grinding, and calcining to obtain K 2 Ti 6 O 13 A precursor.
3. The method for preparing the titanium-based lithium ion sieve according to claim 2, wherein 50-100g of potassium acetate is added into 200ml of deionized water, and stirred at normal temperature until the potassium acetate is dissolved to obtain a methyl acetate solution.
4. The method for preparing a titanium-based lithium ion sieve according to claim 3, wherein 110-240g of meta-titanic acid and 45-50g of anatase TiO are added into the methyl acetate solution 2 。
5. The method for preparing a titanium-based lithium ion sieve according to claim 4, wherein the mass of the PEG200 added is 4-10g.
6. The method for preparing the titanium-based lithium ion sieve according to claim 5, wherein the titanium-based lithium ion sieve is subjected to water temperature ultrasonic treatment at 50-60 ℃ for 20-30min, and is dried for 6-10 h at 110-130 ℃ in an oven, and after the titanium-based lithium ion sieve is sufficiently dried, a sample is taken out and is transferred into a crucible for grinding.
7. The method for preparing the titanium-series lithium ion sieve according to claim 6, wherein the titanium-series lithium ion sieve is transferred into a muffle furnace after being ground, heated and calcined, the heating rate is 2-10 ℃/min, the temperature is firstly increased to 500-650 ℃, the calcination is carried out for 4-8 hours, and then the temperature is increased to 700-900 ℃ and the calcination is carried out for 4-8 hours, so that K with high specific surface area, high adsorption capacity and high selectivity is obtained 2 Ti 6 O 13 A precursor.
8. The preparation method of the titanium lithium ion sieve according to claim 1, wherein a certain mass of potassium metatitanate precursor is taken, 0.05-0.1mol/L hydrochloric acid eluent is added, the feeding ratio is kept at 10-20g/L, and the solution is subjected to vibration elution at 50-60 ℃ for 1-2h.
9. The method for preparing a titanium-based lithium ion sieve according to claim 8, wherein the pH value of the slurry is maintained between 1.3 and 2.0 by supplementing 0.5 to 2mol/L hydrochloric acid solution in the elution process, and the acid solution is exchanged twice to prevent K + The suck-back occurs at too high a concentration.
10. The method for preparing a titanium-based lithium ion sieve according to claim 9, wherein the acid addition is stopped after the pH of the slurry is kept stable, the obtained slurry is centrifuged and washed for 4 to 5 times, and the obtained solid is dried in an oven at 50 to 60 ℃ and crushed to obtain H 2 TiO 3 。
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