CN115924996A - One-step synthesis-stripping method of nickel-iron layered double hydroxide - Google Patents
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- 239000008139 complexing agent Substances 0.000 claims abstract description 26
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 17
- 150000002815 nickel Chemical class 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 13
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- 150000002505 iron Chemical class 0.000 claims description 11
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- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 4
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- 238000001556 precipitation Methods 0.000 claims description 4
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- -1 iron ions Chemical class 0.000 claims description 3
- 229910001453 nickel ion Inorganic materials 0.000 claims description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 3
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 2
- YHGPYBQVSJBGHH-UHFFFAOYSA-H iron(3+);trisulfate;pentahydrate Chemical compound O.O.O.O.O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O YHGPYBQVSJBGHH-UHFFFAOYSA-H 0.000 claims description 2
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims description 2
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims description 2
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
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- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a one-step synthesis-stripping method of a layered ferronickel bimetal hydroxide, which comprises the main preparation steps of respectively preparing a bimetal solution and a complexing agent solution with certain concentration; dropwise adding a complexing agent solution into the bimetallic solution to obtain a stable solution to be treated; and (3) carrying out ultrasonic treatment on the solution to be treated, centrifugally washing a precipitated product by using ultrapure water and ethanol after the treatment is finished, and finally carrying out vacuum drying to obtain the nickel-iron layered double hydroxide with large interlayer spacing. The one-step synthesis-stripping method for the nickel-iron layered double hydroxide has the advantages of mild reaction conditions, simple raw materials, simple and convenient operation, good stripping effect, high efficiency, no need of stripping solvent and atmosphere protection in the stripping process, environmental friendliness and no introduction of impurity ions.
Description
Technical Field
The invention belongs to the technical field of inorganic material preparation, and particularly relates to a one-step synthesis-stripping method of nickel-iron layered double hydroxide.
Background
Layered Double Hydroxides (LDHs) are Hydroxides with a brucite-like structure composed of two or more metal elements. The LDHs have a layered structure and are assembled by a main layer plate with positive electricity, interlayer anions and water molecules through non-covalent bond action. The LDHs have unique physical and chemical characteristics, flexible and changeable structural composition and low cost, and show wide application prospects in the fields of adsorption, catalysis, supercapacitors, drug loading, flame retardance and the like.
The conventional method for preparing LDHs sheets is prone to stacking and agglomeration, so that the active sites of the LDHs sheets cannot be fully exposed, and the overall performance and practical application of the LDHs are limited. The LDHs can be peeled off to expose more active sites, so that the utilization rate of the lamella of the LDHs can be effectively improved, and the performance is improved. However, efficient exfoliation of LDHs remains challenging due to the high charge density of the LDHs and the strong interaction between the metal hydroxide layer and the interlayer charge-balancing anions through chemical bonds. Ultrasonic-assisted liquid phase stripping is a commonly used method for effectively stripping LDHs, but organic solvents with certain toxicity such as N-methylpyrrolidone (NMP), N-Dimethylformamide (DMF), formamide and the like are required to be used, a multi-step ion exchange process is usually required to be carried out, and meanwhile, in order to prevent carbon dioxide adsorption and metal ion oxidation, a nitrogen atmosphere protection is usually required in the stripping process, so that the operation is complicated and the time is long. Therefore, it is of great significance to develop a simple, efficient, environmentally friendly and cost-effective method for exfoliating the layered double hydroxides.
Disclosure of Invention
The invention aims to solve the technical problem of providing a one-step synthesis-stripping method of nickel-iron layered double hydroxide, which has the advantages of mild reaction conditions, simple raw materials, simple and convenient operation, good stripping effect, high efficiency and environmental protection.
The technical scheme for solving the technical problems comprises the following steps:
a one-step synthesis-stripping method of nickel-iron layered double hydroxide comprises the following steps:
preparing a bimetallic solution, weighing 0.95-2.79 g of nickel salt and 0.29-1.62 g of iron salt, dissolving the nickel salt and the iron salt in 60-100 mL of ultrapure water, and stirring until the nickel salt and the iron salt are completely dissolved in the ultrapure water to obtain the bimetallic solution with the total concentration of bimetallic being 0.06-0.2 mol/L;
preparing a complexing agent solution, weighing 3.58-8.95 g of complexing agent, dissolving in 30-60 mL of ultrapure water, and preparing into the complexing agent solution with the concentration of 0.4-2 mol/L;
preparing a solution to be treated, taking a complexing agent solution and a bimetallic solution according to the volume ratio of 1-2 to 2-3, dropwise adding the complexing agent solution into the bimetallic solution, and then carrying out magnetic stirring for 1h to obtain a clear and transparent solution to be treated;
ultrasonic treatment, namely placing the solution to be treated into an ultrasonic pulverizer for ultrasonic treatment, and stripping LDHs while synthesizing the nickel-iron layered double hydroxide;
centrifuging, after the ultrasonic treatment is finished, centrifuging the treated liquid, and collecting a precipitate product precipitated after centrifuging;
cleaning, namely cleaning the precipitation product by using ultrapure water and absolute ethyl alcohol;
drying and collecting, carrying out vacuum drying on the washed precipitate product, and obtaining the nickel-iron layered double hydroxide after the drying is finished.
The invention has the following beneficial effects:
(1) The one-step synthesis-stripping method for the nickel-iron layered double hydroxide has the advantages of mild reaction conditions, simple raw materials, simple and convenient operation, good stripping effect, high efficiency, no need of stripping solvent and atmosphere protection in the stripping process, environmental friendliness and no introduction of impurity ions.
(2) The method adopts a one-step ultrasonic-assisted method to synthesize the layered double hydroxides of ferronickel and realize stripping, a stripping solvent and atmosphere protection are not needed in the stripping process, the dispersion process of LDHs in the stripping solvent and the complex anion exchange process are not needed, the raw materials are simple, the operation is simple and convenient, and the reaction time is only 1-3 h.
(3) The stripping nickel-iron layered double hydroxide prepared by the invention has good stripping effect and high efficiency, the obtained stripping product is stable and has good durability, and other impurity ions are not introduced into the product, so that the product can not be assembled and polymerized again due to drying.
Drawings
Fig. 1 is a height view (left) and a corresponding height cross-sectional view (right) of an AFM according to example 1 of the present invention.
Figure 2 is an XRD pattern of the articles obtained in example 1, example 2 and comparative example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Example 1:
the one-step synthesis-stripping method of the layered nickel-iron double hydroxide in embodiment 1 of the invention comprises the following steps:
preparing a bimetallic solution, weighing 1.43g of nickel salt and 0.54g of ferric salt, dissolving the nickel salt and the ferric salt in 60mL of ultrapure water, stirring, and magnetically stirring for 15min until the nickel salt and the ferric salt are completely dissolved in the ultrapure water to obtain the bimetallic solution with the total concentration of bimetallic being 0.13 mol/L; the nickel salt is formed by combining at least one of nickel sulfate hexahydrate, nickel chloride hexahydrate and nickel nitrate hexahydrate, in this embodiment, nickel chloride hexahydrate is adopted, the iron salt is formed by combining at least one of ferric sulfate pentahydrate, ferric chloride hexahydrate and ferric nitrate nonahydrate, in this embodiment, ferric chloride hexahydrate is adopted, and the molar ratio of nickel ions to iron ions in the bimetallic solution is 3.
Preparing a complexing agent solution, weighing 4.77g of complexing agent, dissolving in 40mL of ultrapure water, and preparing into the complexing agent solution with the concentration of 0.8 mol/L; the complexing agent is triethanolamine.
Preparing a solution to be treated, respectively taking 40mL of a complexing agent solution and 60mL of a bimetallic solution according to the volume ratio of 2; the solution to be treated is a stable metal complex solution. Because triethanolamine is alkaline, the solution undergoes the process from clarification to turbidity and then clarification in the process of dropwise adding and stirring the triethanolamine, the solution needs to be fully stirred to obtain clear and transparent solution, and the solution is in a turbid state due to insufficient stirring, so that impurities are generated. The triethanolamine is used as a complexing agent and a precipitator at the same time, and the concentration of the triethanolamine is closely related to the generation rate of the ferronickel layered double hydroxide and the component structure of the product. In the preferred concentration range of triethanolamine, the formation of impurities can be avoided and a layered double hydroxide of nickel-iron with a certain crystallinity is obtained.
Ultrasonic treatment, namely placing the solution to be treated into an ultrasonic pulverizer for ultrasonic treatment, and stripping LDHs while synthesizing the nickel-iron layered double hydroxide; in this embodiment, the power of the ultrasonic pulverizer is 500W, the ultrasonic frequency is 20 to 25kHz, the single ultrasonic time is 2s, the single intermittent time is 2s, and the processing time of the entire ultrasonic processing is 3 hours. The power and frequency of the ultrasonic wave can regulate and control the growth rate and the stripping efficiency of the nickel-iron layered double hydroxide. Obtaining large interlamellar spacing ferronickel layered double hydroxides with good exfoliation results requires matching growth rate and exfoliation rate. Ultrathin nickel-iron double-metal hydroxide nanosheets with large layer spacing can be effectively obtained within the preferred ultrasonic power and frequency ranges. When the ultrasonic power is lower than the lower limit or the frequency is higher than the upper limit, the stripping effect of the nickel-iron layered double hydroxide is weakened, and when the ultrasonic power is higher than the upper limit or the frequency is lower than the lower limit, the nickel-iron layered double hydroxide with a complete structure cannot be obtained.
Centrifuging, after the ultrasonic treatment is finished, centrifuging the treated liquid, and collecting a precipitate product precipitated after centrifuging; centrifugation is used to throw off excess solution, leaving only the precipitate as a semi-finished product.
Cleaning, namely cleaning the precipitation product by using ultrapure water and absolute ethyl alcohol; the cleaning may be repeated multiple times, with the intention of completely cleaning away the impurities.
Drying and collecting, and carrying out vacuum drying on the cleaned precipitate product at the drying temperature of 50 ℃, thus obtaining the layered nickel-iron double hydroxide with the thickness of 1-2.5 nm after the drying is finished.
In order to solve the problems that the operation is complicated and the time consumption is long when the conventional method for obtaining the layered double hydroxide with large interlayer spacing by adopting ultrasonic-assisted liquid phase stripping is adopted, the invention researches and discovers that the ultrasonic-assisted liquid phase stripping of the LDHs needs to select a proper solvent to disperse the LDHs and weaken the interaction between the metal hydroxide layer of the LDHs and interlayer anions through ion exchange so as to promote the stripping of the LDHs, and the stripping effect is related to the drying mode of the prepared LDHs and the like. Therefore, the process of dispersing LDHs and ion exchange by using a toxic organic solvent can be saved by peeling the LDHs during liquid phase synthesis, and the high crystallization and agglomeration caused by the long-time growth and drying process of the LDHs are avoided, so that the peeling difficulty is reduced. Under the assistance of triethanolamine serving as a complexing agent and a precipitator, ultrasonic treatment is carried out, the heat effect of ultrasonic waves is utilized to provide energy to promote the metal complex to be converted into the nickel-iron layered double hydroxide, and meanwhile, the cavitation effect of the ultrasonic waves is utilized to realize the stripping of the generated nickel-iron layered double hydroxide. The growth rate and the stripping rate of the nickel-iron layered double hydroxide are regulated and controlled by optimizing the concentration of the complexing agent and the ultrasonic treatment parameters, so that the ultrathin nickel-iron layered double hydroxide nanosheet with the large interlayer spacing is obtained.
The prepared ferronickel layered double hydroxide is subjected to AFM detection to obtain an AFM height diagram and a corresponding height profile diagram as shown in fig. 1, and it can be seen that the thickness of the ferronickel layered double hydroxide nanosheet prepared in the embodiment is 1-2.5 nm, and the number of the corresponding ferronickel layered double hydroxide layers is 1-3.
Example 2:
the one-step synthesis-stripping method of the layered nickel-iron double hydroxide in embodiment 2 of the invention comprises the following steps:
preparing a bimetal solution, weighing 2.62g of nickel salt and 1.21g of iron salt, dissolving the nickel salt and the iron salt in 80mL of ultrapure water, stirring, and magnetically stirring for 15min until the nickel salt and the iron salt are completely dissolved in the ultrapure water to obtain the bimetal solution with the total concentration of bimetal of 0.15 mol/L; in this example, nickel nitrate hexahydrate is used as the nickel salt, and iron nitrate nonahydrate is used as the iron salt, and the molar ratio of nickel ions to iron ions in the bimetallic solution is 3.
Preparing a complexing agent solution, weighing 7.16g of complexing agent, dissolving in 40mL of ultrapure water, and preparing into the complexing agent solution with the concentration of 1.2 mol/L; the complexing agent is triethanolamine.
Preparing a solution to be treated, respectively taking 40mL of complexing agent solution and 80mL of bimetallic solution according to the volume ratio of 1; the solution to be treated is a stable metal complex solution.
Ultrasonic treatment, namely placing the solution to be treated into an ultrasonic pulverizer for ultrasonic treatment, and stripping LDHs while synthesizing the nickel-iron layered double hydroxide; in this embodiment, the power of the ultrasonic pulverizer is 800W, the ultrasonic frequency is 20 to 25kHz, the single ultrasonic time is 2s, the single intermittent time is 2s, and the processing time of the entire ultrasonic processing is 1h.
Centrifuging, after the ultrasonic treatment is finished, centrifuging the treated liquid, and collecting a precipitate product precipitated after centrifuging; centrifugation is used to throw off excess solution, leaving only the precipitate as a semi-finished product.
Cleaning, namely cleaning the precipitation product by using ultrapure water and absolute ethyl alcohol; the cleaning may be repeated multiple times, with the intention of completely cleaning away the impurities.
Drying and collecting, and carrying out vacuum drying on the cleaned precipitate product at the drying temperature of 50 ℃, thus obtaining the layered nickel-iron double hydroxide with the thickness of 1-2.5 nm after the drying is finished.
Comparative example 1:
(1) 1.43g of nickel chloride hexahydrate and 0.54g of ferric chloride hexahydrate were weighed and dissolved in 60mL of ultrapure water, and the solution was sufficiently dissolved by magnetic stirring for 15 min.
(2) 4.77g of triethanolamine is weighed and dissolved in 40mL of ultrapure water to prepare a triethanolamine solution with the concentration of 0.8 mol/L.
(3) The triethanolamine solution was added dropwise to the metal salt solution, and after 1h of magnetic stirring a stable metal complex solution was obtained, the solution was transferred to a round bottom flask and subjected to a constant temperature oil bath at 120 ℃ for 6h.
(4) After the reaction is finished and the temperature is cooled to room temperature, the reaction product is collected through centrifugal separation, and the nickel-iron layered double hydroxide is prepared after being cleaned by using ultrapure water and absolute ethyl alcohol and being dried in vacuum at the temperature of 50 ℃.
XRD detection is carried out on the products of examples 1 and 2 and comparative example 1 to obtain an XRD pattern as shown in figure 2, and it can be seen that the phase structures of the samples prepared in example 1, example 2 and comparative example 1 are all NiFe LDH. The diffraction peaks corresponding to the (003) planes in the XRD patterns of the articles of examples 1 and 2 were significantly shifted to a small angle compared to comparative example 1, confirming the successful achievement of exfoliation of the nickel iron layered double hydroxide.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, numerous simple deductions or substitutions may be made without departing from the spirit of the invention, which shall be deemed to belong to the scope of the invention.
Claims (6)
1. A one-step synthesis-stripping method of nickel-iron layered double hydroxide is characterized by comprising the following steps:
preparing a bimetallic solution, weighing 0.95-2.79 g of nickel salt and 0.29-1.62 g of iron salt, dissolving the nickel salt and the iron salt in 60-100 mL of ultrapure water, and stirring until the nickel salt and the iron salt are completely dissolved in the ultrapure water to obtain the bimetallic solution with the total concentration of bimetallic being 0.06-0.2 mol/L;
preparing a complexing agent solution, weighing 3.58-8.95 g of complexing agent, dissolving in 30-60 mL of ultrapure water, and preparing into the complexing agent solution with the concentration of 0.4-2 mol/L;
preparing a solution to be treated, taking a complexing agent solution and a bimetallic solution according to the volume ratio of 1-2 to 2-3, dropwise adding the complexing agent solution into the bimetallic solution, and then carrying out magnetic stirring for 1h to obtain a clear and transparent solution to be treated;
ultrasonic treatment, namely placing the solution to be treated into an ultrasonic pulverizer for ultrasonic treatment, and stripping LDHs while synthesizing the nickel-iron layered double hydroxide;
centrifuging, after the ultrasonic treatment is finished, centrifuging the treated liquid, and collecting a precipitate product precipitated after centrifuging;
cleaning, namely cleaning the precipitation product by using ultrapure water and absolute ethyl alcohol;
drying and collecting, carrying out vacuum drying on the washed precipitate product, and obtaining the nickel-iron layered double hydroxide after the drying is finished.
2. The one-step synthesis-exfoliation method of nickel iron layered double hydroxide according to claim 1, characterized in that: the molar ratio of nickel ions to iron ions in the bimetallic solution is 2-4.
3. The one-step synthesis-exfoliation method of nickel iron layered double hydroxide according to claim 2, characterized in that: the nickel salt is formed by combining at least one of nickel sulfate hexahydrate, nickel chloride hexahydrate and nickel nitrate hexahydrate, the ferric salt is formed by combining at least one of ferric sulfate pentahydrate, ferric chloride hexahydrate and ferric nitrate nonahydrate, and the complexing agent is triethanolamine.
4. The one-step synthesis-exfoliation method of nickel-iron layered double hydroxide as claimed in claim 2, characterized in that: in the ultrasonic treatment step, the power of the ultrasonic crushing instrument is 400-800W, the ultrasonic frequency is 20-40 kHz, the single ultrasonic time is 2-5 s, and the single intermittent time is 2-5 s.
5. The one-step synthesis-exfoliation method of nickel-iron layered double hydroxide as claimed in claim 4, characterized in that: the processing time of the ultrasonic treatment is 1-3 h.
6. The one-step synthesis-exfoliation method of nickel iron layered double hydroxide according to any of claims 1-5, characterized in that: the thickness of the obtained ferronickel layered double hydroxide is 1-2.5 nm.
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