CN112436132A - Method for preparing in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus - Google Patents
Method for preparing in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus Download PDFInfo
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Abstract
The invention discloses a method for preparing an in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus, which comprises the following specific preparation processes: adding the dried sweet osmanthus into a NaOH solution, and carrying out stirring, suction filtration and drying processes to obtain the pretreated loose and porous sweet osmanthus. Adding pretreated flos Osmanthi Fragrantis into surfactant-containing Fe (NO)3)3Adding NH dropwise into the solution after fully stirring4H2PO4Adjusting the pH value of the solution by using ammonia water, and stirring the solution until the solution is milky white. Reacting the milky white solution in a microwave hydrothermal reaction kettle, and naturally cooling, filtering and drying to obtain the FeP0 adsorbed4OfDrying the sweet osmanthus. And grinding and sintering to obtain the in-situ carbon-coated porous iron phosphate material. According to the invention, the in-situ carbon-coated porous ferric phosphate material is prepared under the space confinement and structure guiding effects of the osmanthus by utilizing the super-hydrophilic characteristic of the osmanthus and the three-dimensional structure after the osmanthus is treated.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a method for preparing an in-situ carbon-coated porous ferric phosphate material by adopting osmanthus fragrans.
Background
A lithium ion battery is a type of secondary battery that mainly operates by movement of lithium ions between a positive electrode and a negative electrode. During charging and discharging, Li+Intercalation and desorption to and from the two electrodes: upon charging, Li+Desorbing from the positive electrode, and embedding the electrolyte into the negative electrode, wherein the negative electrode is in a lithium-rich state; the opposite is true during discharge. In recent years, lithium ion batteries have been rapidly developed by the global strong support of new energy vehicles.
At present, lithium iron phosphate as a lithium ion positive electrode material occupies a huge market share in power batteries. With the gradual decline of subsidy policies, the lithium iron phosphate battery has the advantages of low price, good cycle performance, safety, stability, environmental friendliness and the like, and is increasingly paid more attention to the market. The characteristics of the iron phosphate material serving as a precursor of the lithium iron phosphate, such as morphology, structure, tap density, conductivity, specific surface area and the like, have important influence on the electrochemical performance of the lithium iron phosphate cathode material. Thus, high quality FePO4The precursor is the technical key for preparing the high-performance lithium iron phosphate battery.
"nature of law" is an effective way for human beings to acquire experience and inspiration from ancient to present. In the evolution process of the nature, in order to adapt to the change of the natural environment, various natural plants continuously evolve physical sign structures thereof to form unique tissue structures and surface morphologies. The space limitation and structure orientation functions inherent in the natural plants play a unique role in preparing various functional materials with special appearance and controllable structure. With the rapid development of new energy industry, the lithium ion electrode material with ideal electrochemical performance needs to be developed simply, cheaply and efficiently. Therefore, the invention is based on the idea and rich natural sweet-scented osmanthus resources of Guangxi Guilin, and prepares the in-situ carbon-coated porous ferric phosphate material through the space limitation and the structure guidance of the sweet-scented osmanthus, which is also the specific practice of 'natural classic' essence. The successful development of the material is believed to play a great role in promoting the development of the lithium iron phosphate industry and provide effective technical support for preparing other various lithium ion electrode materials.
Disclosure of Invention
The invention aims to prepare the in-situ carbon-coated porous ferric phosphate material by utilizing the hydrophilic characteristic of the osmanthus and the unique three-dimensional structure of the pretreated osmanthus through the space confinement and structure-oriented action of the osmanthus. The ferric phosphate with a porous structure is beneficial to the infiltration of the lithium iron phosphate material in the electrolyte and the insertion and desorption of lithium ions, and meanwhile, the electronic conductivity of the ferric phosphate material can be effectively enhanced by the in-situ carbon-coated structure.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing an in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus is designed, and comprises the following steps:
(1) accurately weighing 1-2 g of dried osmanthus fragrans and 0.4-0.8 g of NaOH, adding the weighed NaOH and the osmanthus fragrans into 100-200 mL of deionized water, stirring, performing suction filtration, adjusting the pH value of the solution, and performing drying treatment to obtain pretreated loose and porous osmanthus fragrans;
(2) accurately weighing 4.04-6.06 g of Fe (NO)3)31.15-2.3 g of NH4H2PO4And 0.0404-0.606 g of surfactant, respectively dissolving in 100-150 mL of deionized water, and fully stirring and dissolving to obtain Fe (NO)3)3Solution, surfactant solution and NH4H2PO4A solution;
(3) weighing 0.3-0.5 g of the loose and porous osmanthus fragrans prepared in the step (1), and respectively weighing 80-150 mL of Fe (NO) obtained in the step (2)3)3Solution with NH4H2PO4A solution;firstly, adding the weighed sweet osmanthus into Fe (NO)3)3Dripping 20-50 mL of surfactant solution into the solution, and stirring for 12-18 h; immediately after dropwise addition of NH4H2PO4Adjusting the pH value of the solution to 2.05-3.15 by using 0.1-0.3 mol/L ammonia water, and stirring for 0.5-1.5 h until the solution is milky white;
(4) adding the white solution prepared in the step (3) into a microwave hydrothermal reaction kettle for reaction at the temperature of 90-160 ℃ for 30-120 min; after the reaction is finished and the reaction product is naturally cooled to room temperature, the dried FePO adsorbed can be obtained through the processes of suction filtration and drying4The osmanthus compound of (1);
(5) grinding the sweet osmanthus compound obtained in the step (4) for 30-120 min, and then sintering in a muffle furnace, wherein the sintering conditions are as follows: the heating rate is 2-10 ℃/min, the sintering temperature is 450-600 ℃, the sintering time is 10-16 h, and after the sintering is finished and the temperature is cooled to room temperature, the in-situ carbon-coated porous iron phosphate material prepared under the space confinement and structure guidance effects of the osmanthus fragrans can be obtained.
The sweet osmanthus has good hydrophilic property, becomes a loose and porous structure after alkali treatment, and when Fe is used3+And PO4 3-After entering a porous structure with the assistance of a surfactant, the iron phosphate material with good crystallization is formed through microwave hydrothermal and heat treatment processes. Herein, the space confinement effect means that iron phosphate particles are limited by the space of the pore channel structure of the osmanthus fragrans and the in-situ coated carbon on the surface in the heat treatment process, and the growth of the particles is inhibited. The structure directing action is Fe3+And PO4 3-The ferric phosphate is deposited in the pore canal and the flower wall of the osmanthus fragrans, and when the osmanthus fragrans are converted into carbon materials in situ in the heat treatment process, the osmanthus fragrans play a role in structure guiding on the appearance and the structure of the ferric phosphate, so that the appearance of the finally formed ferric phosphate particles is similar to that of the osmanthus fragrans.
Preferably, in the step (1), a DF-101S type heat collection type constant temperature magnetic stirrer is adopted to fully stir the solution for 0.5-1 h, and after suction filtration, absolute ethyl alcohol and deionized water are used for washing until the pH value is 7-8; and then drying for 12-48 h at the temperature of 60-120 ℃ to obtain the pretreated loose and porous osmanthus fragrans.
Preferably, the surfactant in step (2) is one or more of benzoic acid, oleic acid and sorbic acid.
Preferably, in the step (2), a DF-101S type heat collection type constant temperature magnetic stirrer is adopted to stir the three solutions at normal temperature until the three solutions are fully dissolved.
Preferably, the drying temperature in the step (4) is 60-120 ℃, and the drying time is 12-48 h.
The invention has the beneficial effects that:
the in-situ carbon-coated porous ferric phosphate material prepared by the invention has the advantages of small particle size, uniform appearance and good conductivity, and simultaneously fully utilizes the natural resources with local advantages and low price, thereby achieving the purposes of controlling cost and enabling a legal person to be natural. After the osmanthus fragrans coated with the iron phosphate is subjected to heat treatment, the osmanthus fragrans in situ becomes a carbon material with good electrical conductivity, so that the electronic conductivity of the iron phosphate material is enhanced, and therefore, compared with the existing iron phosphate material, the porous iron phosphate prepared by the method has the advantages of more uniform appearance, greatly improved electrical conductivity and obviously reduced cost.
The ferric phosphate with a porous structure is beneficial to the infiltration of the lithium iron phosphate material in the electrolyte and the insertion and desorption of lithium ions, and meanwhile, the electronic conductivity of the ferric phosphate precursor material can be effectively improved due to the in-situ carbon-coated structure. Thus, the high quality FePO was prepared4The precursor is a technical key for improving the electrochemical performance of the lithium iron phosphate battery. The method fully utilizes the rich natural biological resource-osmanthus fragrans of Guangxi Guilin, has low cost, is green and environment-friendly, prepares the iron phosphate precursor with unique structure and excellent performance under the space limitation and structure guide effect of the osmanthus fragrans, effectively promotes the electrochemical performance of the lithium iron phosphate anode material, and promotes the development of new energy industry.
Drawings
FIG. 1 is iron phosphate (FePO) prepared in example 14) Precursor ofXRD pattern of volume;
FIG. 2 is iron phosphate (FePO) prepared in example 14) SEM picture of the precursor;
FIG. 3 is a prior art iron phosphate (FePO) prepared by co-precipitation4) SEM image of (d).
Detailed Description
The following examples are given to illustrate specific embodiments of the present invention, but are not intended to limit the scope of the present invention in any way. The apparatus elements referred to in the following examples are, unless otherwise specified, conventional apparatus elements; the industrial raw materials are all conventional industrial raw materials which are sold on the market, if not specifically mentioned.
Example 1: a method for preparing an in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus comprises the following steps:
(1) accurately weighing 2g of dried sweet osmanthus and 0.8g of NaOH, adding the weighed NaOH and sweet osmanthus into 100mL of deionized water, fully stirring for 1h, fully filtering, and washing with absolute ethyl alcohol and deionized water until the pH value is 7. Drying for 12h at the temperature of 80 ℃ to obtain the pretreated porous and loose osmanthus.
(2) 4.04g of Fe (NO) was accurately weighed3)31.725g of NH4H2PO4And 0.0404g of benzoic acid are respectively dissolved in 100mL of deionized water, and stirred at constant temperature by using a DF-101S type heat collection constant temperature magnetic stirrer at normal temperature until the benzoic acid is uniformly dissolved to obtain Fe (NO)3)3Solution, benzoic acid solution and NH4H2PO4And (3) solution.
(3) Taking 0.3g of the loose and porous osmanthus fragrans prepared in the step (1), and then respectively taking 100mL of Fe (NO) obtained in the step (2)3)3Solution with NH4H2PO4And (3) solution. Adding flos Osmanthi Fragrantis into Fe (NO)3)3Adding 50mL of benzoic acid solution into the solution dropwise, continuously stirring for 12h, and then adding NH dropwise4H2PO4Adding 1.5 mol/L ammonia water into the solution, titrating the solution until the pH value is 2.05, and stirring the solution for 1 hour until the solution is milky white.
(4) And (4) adding the milky white solution prepared in the step (3) into a microwave hydrothermal reaction kettle, controlling the reaction to be 150 ℃, and preserving the heat for 90 min. Naturally cooling to room temperature, then carrying out suction filtration, and drying at 80 ℃ for 36h to obtain the product with FeP0 adsorbed4The dried sweet osmanthus.
(5) Adsorbing FeP0 prepared in the step (4)4After grinding the dried sweet osmanthus for 30min, placing the ground sweet osmanthus in a muffle furnace for sintering, wherein the temperature rise rate is set to be 5 ℃/min, the sintering temperature is set to be 600 ℃, and the sintering time is 10 h. And naturally cooling to room temperature to obtain the in-situ carbon-coated porous iron phosphate material.
Example 2: a method for preparing an in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus comprises the following steps:
(1) accurately weighing 1.5g of dried sweet osmanthus and 0.6g of NaOH, adding the weighed NaOH and sweet osmanthus into 100mL of deionized water, fully stirring for 0.6h, fully filtering, and washing with absolute ethyl alcohol and deionized water until the pH value is 7. Drying for 24 h at the temperature of 80 ℃ to obtain the pretreated porous and loose osmanthus.
(2) 2.02g of Fe (NO) was accurately weighed3)30.8625g NH4H2PO4And 0.0202g sorbic acid are respectively dissolved in 100mL deionized water, and stirred at constant temperature by using a DF-101S type heat collection type constant temperature magnetic stirrer at normal temperature until the sorbic acid and the sorbic acid are uniformly dissolved to obtain Fe (NO)3)3Solution, sorbic acid solution and NH4H2PO4And (3) solution.
(3) Taking 0.2g of the loose and porous osmanthus fragrans prepared in the step (1), and then respectively taking 100mL of Fe (NO) obtained in the step (2)3)3Solution with NH4H2PO4And (3) solution. Adding flos Osmanthi Fragrantis into Fe (NO)3)3Adding 50mL sorbic acid solution into the solution dropwise, stirring for 12h, and then adding NH dropwise4H2PO4Adding 2 mol/L ammonia water into the solution, titrating the solution until the pH value is 2.85, and stirring the solution for 1 hour until the solution is milky white.
(4) Adding the milky white solution prepared in the step (3) into a microwave hydrothermal reaction kettle, and controllingThe reaction is carried out at 160 ℃ and the temperature is kept for 90 min. Naturally cooling to room temperature, then carrying out suction filtration, and drying at 80 ℃ for 36h to obtain the product with FeP0 adsorbed4The dried sweet osmanthus.
(5) Adsorbing FeP0 prepared in the step (4)4After grinding the dried sweet osmanthus for 30min, placing the ground sweet osmanthus in a muffle furnace for sintering, wherein the heating rate is set to be 8 ℃/min, the sintering temperature is set to be 650 ℃, and the sintering time is set to be 10 h. And naturally cooling to room temperature to obtain the in-situ carbon-coated porous iron phosphate material.
The invention relates to a method for preparing an in-situ carbon-coated iron phosphate material by using osmanthus fragrans, and although iron phosphate is a very important precursor material of lithium iron phosphate, the shape, structure and the like of the precursor iron phosphate have very important influence on the electrochemical performance of the lithium iron phosphate. In order to highlight the advantages of the present invention in preparing iron phosphate materials, we compared the co-precipitation method and the iron phosphate prepared by the present patent technology in terms of morphology and electrical conductivity, fig. 1 is an XRD chart of the iron phosphate precursor prepared in example 1 of the present invention, fig. 2 is an SEM chart of the iron phosphate precursor prepared in example 1 of the present invention, and fig. 3 is an SEM chart of the iron phosphate prepared by the co-precipitation method in the prior art. From a comparison of fig. 2 and 3, it can be seen that the ferric phosphate prepared by the present invention is different from the ferric phosphate prepared by the co-precipitation method in terms of the morphological structure: the iron phosphate particles prepared by the method have the advantages of smaller agglomeration degree, more uniform size and better dispersibility, and bear the natural framework of the osmanthus fragrans. In terms of conductivity: the electric conductivity of the iron phosphate prepared by the method is greatly improved, and the electric conductivity of the iron phosphate prepared by coprecipitation is 2.54 multiplied by 10-5 S/m, the conductivity of the in-situ carbon-coated porous iron phosphate prepared by the method is 1.99 multiplied by 10-4 S/m。
While the present invention has been described in detail with reference to the embodiments, those skilled in the art will appreciate that various changes can be made in the specific parameters of the embodiments without departing from the spirit of the present invention, and that various specific embodiments can be made, which are common variations of the present invention and will not be described in detail herein.
Claims (5)
1. A method for preparing an in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus is characterized by comprising the following steps:
(1) accurately weighing 1-2 g of dried osmanthus fragrans and 0.4-0.8 g of NaOH, adding the weighed NaOH and the osmanthus fragrans into 100-200 mL of deionized water, stirring, performing suction filtration, adjusting the pH value of the solution, and performing drying treatment to obtain pretreated loose and porous osmanthus fragrans;
(2) accurately weighing 4.04-6.06 g of Fe (NO)3)31.15-2.3 g of NH4H2PO4And 0.0404-0.606 g of surfactant, respectively dissolving in 100-150 mL of deionized water, and fully stirring and dissolving to obtain Fe (NO)3)3Solution, surfactant solution and NH4H2PO4A solution;
(3) weighing 0.3-0.5 g of the loose and porous osmanthus fragrans prepared in the step (1), and respectively weighing 80-150 mL of Fe (NO) obtained in the step (2)3)3Solution with NH4H2PO4A solution; firstly, adding the weighed sweet osmanthus into Fe (NO)3)3Dripping 20-50 mL of surfactant solution into the solution, and stirring for 12-18 h; immediately after dropwise addition of NH4H2PO4Adjusting the pH value of the solution to 2.05-3.15 by using 0.1-0.3 mol/L ammonia water, and stirring for 0.5-1.5 h until the solution is milky white;
(4) adding the white solution prepared in the step (3) into a microwave hydrothermal reaction kettle for reaction at the temperature of 90-160 ℃ for 30-120 min; after the reaction is finished and the reaction product is naturally cooled to room temperature, the dried FePO adsorbed can be obtained through the processes of suction filtration and drying4The osmanthus compound of (1);
(5) grinding the sweet osmanthus compound obtained in the step (4) for 30-120 min, and then sintering in a muffle furnace, wherein the sintering conditions are as follows: the heating rate is 2-10 ℃/min, the sintering temperature is 450-600 ℃, the sintering time is 10-16 h, and after the sintering is finished and the temperature is cooled to room temperature, the in-situ carbon-coated porous iron phosphate material prepared under the space confinement and structure guidance effects of the osmanthus fragrans can be obtained.
2. The method for preparing the in-situ carbon-coated porous ferric phosphate material by adopting the sweet osmanthus according to claim 1, wherein in the step (1), a DF-101S type heat collection type constant temperature magnetic stirrer is adopted to fully stir the solution for 0.5-1 h, and after suction filtration, the solution is washed by absolute ethyl alcohol and deionized water until the pH value is 7-8; and then drying for 12-48 h at the temperature of 60-120 ℃ to obtain the pretreated loose and porous osmanthus fragrans.
3. The method for preparing the in-situ carbon-coated porous ferric phosphate material by adopting the sweet osmanthus according to claim 1, wherein the surfactant in the step (2) is one or more of benzoic acid, oleic acid and sorbic acid.
4. The method for preparing the in-situ carbon-coated porous ferric phosphate material by adopting the sweet osmanthus according to claim 1, wherein in the step (2), a DF-101S type heat collection type constant temperature magnetic stirrer is adopted to stir the three solutions to be fully dissolved at normal temperature.
5. The method for preparing the in-situ carbon-coated porous ferric phosphate material by adopting the sweet osmanthus according to claim 1, wherein the drying temperature in the step (4) is 60-120 ℃, and the drying time is 12-48 h.
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| CN113336210A (en) * | 2021-05-07 | 2021-09-03 | 桂林理工大学 | Preparation method of high-conductivity iron phosphate with carbon network coating and embedding structure |
| CN113460992A (en) * | 2021-06-20 | 2021-10-01 | 桂林理工大学 | Method for realizing in-situ mosaic construction of cellular porous carbon and iron phosphate precursor by using waste shaddock peel |
| CN113460988A (en) * | 2021-06-20 | 2021-10-01 | 桂林理工大学 | Method for in-situ synthesis of high-quality iron phosphate precursor by using waste banana peels |
| CN113511641A (en) * | 2021-07-04 | 2021-10-19 | 桂林理工大学 | Method for preparing three-dimensional porous carbon/iron phosphate compound by salt crystal foaming with glucose as carbon source |
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