CN108847479B - Preparation method of porous layered chemical structure modified lithium magnesium silicate for lithium battery cathode material - Google Patents
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Abstract
The invention discloses a preparation method of porous layered chemical structure modified magnesium lithium silicate for a lithium battery anode material, which is characterized by firstly modifying an organic quaternary ammonium salt modified magnesium lithium silicate lattice structure by utilizing rare earth oxide and then introducing Mn into a tetrahedral structure2+And Fe3+And then the porous layered chemical structure modified magnesium lithium silicate is prepared through solid phase reaction, and the preparation method of the porous layered chemical structure modified magnesium lithium silicate for the lithium battery cathode material has the advantages of small charge transfer impedance, large lithium ion diffusion coefficient and good electrochemical performance, and has extremely bright application prospect.
Description
Technical Field
The invention relates to the field of preparation of lithium battery anode materials, in particular to a preparation method of porous layered chemical structure modified magnesium silicate lithium for a lithium battery anode material, which has the advantages of small charge transfer impedance, large lithium ion diffusion coefficient and good electrochemical performance.
Background
The lithium ion battery is a lithium ion embedded battery developed on the basis of a lithium secondary battery, is used as an electrochemical concentration battery, and has the working principle based on lithium ion embedding-releasing reaction generated between positive and negative active substances. In general, a lithium battery uses a lithium-containing metal oxide as a positive electrode material and a carbon-based material such as graphite as a negative electrode material, and uses a nonaqueous electrolyte. Although the research history of lithium batteries is not very long, with the development of scientific technology, lithium batteries have become one of the mainstream battery products. In particular, in industries such as portable electronic devices including mobile phones, notebooks, and calculators, lithium batteries are widely used as new small energy storage devices having significant advantages such as high capacity and long life, and are gradually developed into other industries.
The positive electrode material is an important factor influencing the cost and performance of the lithium battery. Therefore, research on novel cathode materials becomes a current international research hotspot. Research reports show that when the specific capacities of the positive electrode material and the negative electrode material in the battery are respectively improved by 50%, the power density of the battery is respectively improved by 28% and 13%, which means that the key factor for improving the performance of the lithium ion battery lies in the development of the positive electrode material. Typical common lithium ion battery positive electrode materials at present mainly include lithium iron phosphate, spinel-series lithium manganese oxide, lithium cobaltate and LiNixCoyMnzO2Ternary materials, and the like. Despite the extensive use and extensive research currently available on these cathode materials, there are several serious shortcomings:
(1) although lithium iron phosphate is a very widely applied cathode material with the characteristics of low cost, high safety and good cycle performance, the lithium iron phosphate as the cathode material has poor theoretical capacity, poor conductivity and poor rate performance, and particularly the electronic conductivity is far lower than that of other cathode materials.
(2) The spinel lithium manganese oxide has high preparation process requirement and unstable crystal structure, and the crystal is transformed from cubic phase to tetragonal phase (Jahn-Teller distortion effect) in the using process, so that the structure is damaged and the capacity is rapidly reduced.
(3) Lithium cobaltate is high in price and has certain toxicity due to limited cobalt resources, and is not friendly to the environment.
(4) Although LiNi is presentxCoyMnzO2The ternary material has the advantages of high specific capacity, good cycle performance and the like due to good ternary synergistic effect, but the preparation process is complex (especially element proportion and crystal structure control), the solid phase reaction temperature is high, the production cost is high, and the price is expensive.
Meanwhile, in addition to the above serious disadvantages and shortcomings, the typical cathode materials used at present must additionally use expensive lithium-containing compounds, which greatly increases the production cost, and thus their application is again greatly limited.
Therefore, how to prepare the lithium ion battery cathode material with the advantages of high charge-discharge specific capacity, high conductivity, excellent rate performance, long service life, simple preparation process, low production cost, environmental protection, no pollution and the like is a technical problem which is urgently solved by the domestic industry at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a porous layered chemical structure for a lithium battery cathode material, which has the advantages of small charge transfer impedance, large lithium ion diffusion coefficient and good electrochemical performanceA preparation method of modified lithium magnesium silicate. The preparation method comprises the steps of firstly, carrying out chemical doping modification on Si-O tetrahedron in an organic quaternary ammonium salt modified magnesium silicate lithium lattice structure by utilizing rare earth oxide, and then introducing Mn into the tetrahedron structure2+And Fe3+And then the porous layered chemical structure modified magnesium lithium silicate is prepared through solid phase reaction, and the electrochemical properties of the porous layered chemical structure modified magnesium lithium silicate are excellent, such as high charge-discharge specific capacity, high conductivity and the like, so that the lithium battery anode material meets the actual use requirements of the lithium battery anode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of porous layered chemical structure modified lithium magnesium silicate for a lithium battery anode material is characterized by comprising the following steps: the preparation method comprises the following steps of:
(1) firstly, completely dissolving 100 parts of magnesium lithium silicate in 1000 parts of pure water, simultaneously completely dissolving 5-15 parts of quaternary ammonium salt in 100 parts of pure water, then adding a quaternary ammonium salt solution into the pure magnesium lithium silicate solution, heating to 30-50 ℃, preserving heat, stirring for 30-60 min, then filtering and fully washing, and collecting to obtain an organically modified magnesium lithium silicate filter cake;
(2) uniformly stirring the organic modified magnesium lithium silicate filter cake collected in the step (1) and 1-5 parts of rare earth oxide, and roasting at 150-250 ℃ for 5-15 min; then taking out and adding 1000 parts of pure water, and fully stirring until the pure water is completely dispersed to obtain a modified magnesium lithium silicate solution;
(3) then adding 20-50 parts of soluble manganese salt and 10-30 parts of soluble ferric salt to the modified magnesium lithium silicate solution obtained in the step (2), and fully stirring for 1-2 hours; and then filtering and fully washing, and fully drying the filter cake at 105-150 ℃ to obtain the porous layered chemical structure modified magnesium lithium silicate.
In the invention, the quaternary ammonium salt is one or any combination of dodecyl trimethyl ammonium bromide, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide and hexadecyl trimethyl ammonium chloride. The first step of the invention is to prepare organic magnesium lithium silicate by intercalation reaction of quaternary ammonium salt and magnesium lithium silicate, and the organic magnesium lithium silicate is used as the initial base material and basic skeleton of the subsequent solid phase reaction.During the reaction in the step, the hydrophilic/hydrophobic balance of the interlayer region of the organic magnesium lithium silicate needs to be controlled, so that the cations of the organic quaternary ammonium salt are always kept in the interlayer region, the integrity of the interlayer region is kept, and a quick channel is provided for lithium ion or electron transmission; at the same time, the amount of quaternary ammonium salt should not be too great, otherwise the excessively hydrophobic interlaminar regions of the microenvironment strongly repel Mn2+And Fe3+Directly greatly influences the subsequent impregnation effect. Therefore, the molecular weight of the quaternary ammonium salt used in the present invention is not too high, and the number of carbons in the hydrocarbon chain must be less than 18. However, if the carbon number is less than 12 (in an extreme case, inorganic magnesium lithium silicate is used as a reaction initiation base), the interlayer region is liable to collapse in the subsequent solid-phase reaction to be completely destroyed.
In the invention, the rare earth oxide is La2O3、Ce2O3、Ln2O3One or more of the above components can be combined randomly. In the roasting process of the organic modified magnesium lithium silicate and the rare earth oxide at the temperature of 150-250 ℃, La in the rare earth oxide3+The rare earth ions enter and distort the Si-O tetrahedra, leaving a certain number of holes behind. The firing temperature for this step is important: the distortion degree of the rare earth ions/Si-O tetrahedron is not enough below 150 ℃; above 250 deg.C, the interlayer region is very prone to collapse.
In the invention, the soluble manganese salt is one or any combination of manganese sulfate, manganese chloride, manganese nitrate and manganese acetate; the soluble manganese salt is one or a combination of iron sulfate, iron chloride and iron nitrate. And (3) adding soluble manganese salt and soluble iron salt into the modified magnesium lithium silicate solution obtained in the step (2), and fully drying a filter cake obtained after filtering and washing at 105-150 ℃. First soluble Mn in manganese salt2+And Fe in soluble manganese salt3+Adsorbing in micropores of magnesium lithium silicate, and then entering cavities of rare earth ions/Si-O tetrahedron when drying (namely solid phase reaction) at 105-150 ℃, and enabling the rare earth ions/Si-O tetrahedron to be in La3+The oxidation-reduction reaction is carried out under the induction of the rare earth ions: mn2+Is oxidized to Mn4+While being Fe3+Is reduced to Fe2+. Then Mn4+And Fe2+Each distributed in Si-O tetrahedrons and participating in the formation of the crystal lattice of the magnesium lithium silicate.
The porous layered chemical structure modified magnesium lithium silicate prepared by the invention is a crystal with a brand new chemical structure, and a layer of Mg-O trioctahedral body (a small amount of Mg in the trioctahedral body) is sandwiched between an upper layer of rare earth ions/Si-Mn-Fe-O tetrahedron and a lower layer of rare earth ions/Si-Mn-Fe-O tetrahedron2+Is covered with Li+Substituted). Compared with the prior art, the invention has the beneficial effects that:
(1) the porous layered chemical structure modified magnesium lithium silicate prepared by the invention exerts the synergistic effect of Li-Mn-Fe oxide crystals in a layered framework, and has the advantages of high conductivity, specific capacity and energy density, strong energy storage capacity, good rate capability and the like.
Meanwhile, the ternary synergistic effect is exerted in the layered framework, so that the porous layered chemical structure modified magnesium silicate lithium only utilizes original Li in the lattice structure of the magnesium silicate lithium, and an expensive lithium-containing compound is not required to be additionally used, so that the production cost is greatly reduced.
(2) On one hand, the layered framework of the magnesium lithium silicate is stable, so that the prepared porous layered chemical structure modified magnesium lithium silicate has long service life and good recycling performance. On the other hand, other impurity crystals (such as Mn) are limited by the size of the lattice structure of the layered skeleton3O4、Fe2O3Etc.), so that not only the crystal structure and the chemical property are stable, but also the corresponding preparation process is simple to operate, the stability of the product batch is good, and the qualification rate and the yield meet the requirements of industrial production. In addition, the layered silicate has the characteristics of high specific surface area and more microporous structures, and provides a rapid channel for lithium ion or electron transmission in an interlayer region, so that the specific capacity is obviously improved.
(3) The invention abandons expensive and toxic compounds such as Ni, Co and the like, and only uses soluble manganese salt and soluble iron salt which are rich in sources and cheap, thereby being environment-friendly and environment-friendly.
(4) The invention adopts low-temperature solid-phase reaction, so the production process is safe and has no risk.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A porous layered chemical structure modified magnesium lithium silicate for a lithium battery anode material is prepared from the following raw material components in parts by mass:
(1) firstly, completely dissolving 100 parts of magnesium lithium silicate (Laponite RD, produced by Elementis Specialties, USA; the same below) in 1000 parts of pure water, simultaneously completely dissolving 5 parts of quaternary ammonium salt dodecyl trimethyl ammonium bromide in 100 parts of pure water, then adding a quaternary ammonium salt solution into the pure water solution of the magnesium lithium silicate, heating to 30 ℃, preserving heat and stirring for 30min, then filtering and fully washing, and collecting to obtain an organic modified magnesium lithium silicate filter cake;
(2) then, the organically modified magnesium lithium silicate filter cake collected in the step (1) and 1 part of La are added2O3Stirring uniformly, and roasting at 150 deg.C for 5 min; then taking out and adding 1000 parts of pure water, and fully stirring until the pure water is completely dispersed to obtain a modified magnesium lithium silicate solution;
(3) then adding 20 parts of manganese sulfate and 10 parts of ferric chloride into the modified magnesium lithium silicate solution obtained in the step (2), and fully stirring for 1 h; then filtering and fully washing, and fully drying the filter cake at 105 ℃ to obtain the porous layered chemical structure modified magnesium lithium silicate a.
Example 2
A porous layered chemical structure modified magnesium lithium silicate for a lithium battery anode material is prepared from the following raw material components in parts by mass:
(1) firstly, completely dissolving 100 parts of magnesium lithium silicate in 1000 parts of pure water, simultaneously completely dissolving 10 parts of dodecyl trimethyl ammonium chloride and 5 parts of hexadecyl trimethyl ammonium bromide in 100 parts of pure water, then adding a quaternary ammonium salt solution into the pure water solution of the magnesium lithium silicate, heating to 50 ℃, keeping the temperature and stirring for 60min, then filtering and fully washing, and collecting to obtain an organic modified magnesium lithium silicate filter cake;
(2) then the organic modified magnesium lithium silicate filter cake obtained in the step (1) and 2 parts of Ce2O3And 3 parts of Ln2O3Stirring uniformly, and roasting at 250 deg.C for 15 min; then taking out and adding 1000 parts of pure water, and fully stirring until the pure water is completely dispersed to obtain a modified magnesium lithium silicate solution;
(3) then adding 30 parts of manganese nitrate, 20 parts of manganese chloride, 15 parts of ferric sulfate and 15 parts of ferric nitrate into the modified magnesium lithium silicate solution obtained in the step (2), and fully stirring for 2 hours; then filtering and fully washing, and fully drying the filter cake at 150 ℃ to obtain the porous layered chemical structure modified magnesium lithium silicate b.
Example 3
A porous layered chemical structure modified magnesium lithium silicate for a lithium battery anode material is prepared from the following raw material components in parts by mass:
(1) firstly, completely dissolving 100 parts of magnesium lithium silicate in 1000 parts of pure water, simultaneously completely dissolving 3 parts of dodecyl trimethyl ammonium chloride, 3 parts of hexadecyl trimethyl ammonium bromide and 4 parts of hexadecyl trimethyl ammonium chloride in 100 parts of pure water, then adding a quaternary ammonium salt solution into the pure magnesium lithium silicate solution, heating to 40 ℃, keeping the temperature and stirring for 40min, then filtering and fully washing, and collecting to obtain an organic modified magnesium lithium silicate filter cake;
(2) then, the organically modified magnesium lithium silicate filter cake collected in the step (1) and 1 part of La are added2O31.5 parts of Ce2O30.5 part of Ln2O3Stirring uniformly, and roasting at 190 deg.C for 8 min; then taking out and adding 1000 parts of pure water, and fully stirring until the pure water is completely dispersed to obtain a modified magnesium lithium silicate solution;
(3) then adding 8 parts of manganese sulfate, 10 parts of manganese chloride, 5 parts of manganese nitrate, 4 parts of ferric sulfate, 6 parts of ferric chloride and 3 parts of ferric nitrate into the modified magnesium lithium silicate solution obtained in the step (2), and fully stirring for 1.5 hours; then filtering and fully washing, and fully drying the filter cake at 120 ℃ to obtain the porous layered chemical structure modified magnesium lithium silicate c.
Example 4
A porous layered chemical structure modified magnesium lithium silicate for a lithium battery anode material is prepared from the following raw material components in parts by mass:
(1) firstly, completely dissolving 100 parts of magnesium lithium silicate in 1000 parts of pure water, simultaneously completely dissolving 3 parts of dodecyl trimethyl ammonium bromide, 2 parts of dodecyl trimethyl ammonium chloride, 2 parts of hexadecyl trimethyl ammonium bromide and 2 parts of hexadecyl trimethyl ammonium chloride in 100 parts of pure water, then adding a quaternary ammonium salt solution into a pure water solution of the magnesium lithium silicate, heating to 45 ℃, preserving heat, stirring for 50min, then filtering and fully washing, and collecting to obtain an organic modified magnesium lithium silicate filter cake;
(2) then the organic modified magnesium lithium silicate filter cake collected in the step (1) and 0.5 part of La are added2O30.5 part of Ce2O31 part of Ln2O3Stirring uniformly, and roasting at 200 deg.C for 10 min; then taking out and adding 1000 parts of pure water, and fully stirring until the pure water is completely dispersed to obtain a modified magnesium lithium silicate solution;
(3) then adding 7 parts of manganese sulfate, 8 parts of manganese chloride, 6 parts of manganese nitrate, 7 parts of manganese acetate, 5 parts of ferric sulfate, 4 parts of ferric chloride and 9 parts of ferric nitrate into the modified magnesium lithium silicate solution obtained in the step (2), and fully stirring for 1.6 hours; then filtering and fully washing, and fully drying the filter cake at 140 ℃ to obtain the porous layered chemical structure modified magnesium lithium silicate d.
The prepared lithium battery positive electrode material is prepared by using porous layered Chemical structure modified magnesium lithium silicate a-d and a foreign imported lithium battery positive electrode material commodity (model: LB-af6, manufactured by Sumitomo Chemical, Japan; model: AC-N2, manufactured by Korea Yulchon Noterram; model: LCM-xt, manufactured by Celgard, USA), a conductive agent and a binder according to the mass ratio of 70: 20: 10, dispersing in a mixed solvent of isopropanol and water, grinding into slurry, coating on a stainless steel current collector, tabletting under the pressure of 10MPa, and finally vacuum drying at 90 ℃ for 12 hours to prepare an electrode to be detected; then, constant current charge and discharge tests were performed by setting a charge and discharge voltage interval and a charge and discharge current using a Land CT2001A battery test apparatus, and the results are shown in the following table.
Table comparison test data
According to test data, the porous layered chemical structure modified magnesium lithium silicate prepared by the technical scheme of the invention is used as a lithium battery anode material, the lithium battery anode material has excellent electrochemical properties such as charge-discharge conductivity, specific capacity and energy density, and the like, and related performance indexes of the lithium battery anode material exceed those of similar commodities imported from abroad. The lithium battery anode material prepared by the technical scheme of the invention can replace the current products on the market at home and abroad by the porous layered chemical structure modified magnesium lithium silicate, and has wide application prospect.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (5)
1. A preparation method of porous layered chemical structure modified lithium magnesium silicate for a lithium battery anode material is characterized by comprising the following steps: the preparation method comprises the following steps of:
(1) firstly, completely dissolving 100 parts of magnesium lithium silicate in 1000 parts of pure water, simultaneously completely dissolving 5-15 parts of quaternary ammonium salt in 100 parts of pure water, then adding a quaternary ammonium salt solution into the pure magnesium lithium silicate solution, heating to 30-50 ℃, preserving heat, stirring for 30-60 min, then filtering and fully washing, and collecting to obtain an organically modified magnesium lithium silicate filter cake;
(2) uniformly stirring the organic modified magnesium lithium silicate filter cake collected in the step (1) and 1-5 parts of rare earth oxide, and roasting at 150-250 ℃ for 5-15 min; then taking out and adding 1000 parts of pure water, and fully stirring until the pure water is completely dispersed to obtain a modified magnesium lithium silicate solution;
(3) then adding 20-50 parts of soluble manganese salt and 10-30 parts of soluble ferric salt to the modified magnesium lithium silicate solution obtained in the step (2), and fully stirring for 1-2 hours; and then filtering and fully washing, and fully drying the filter cake at 105-150 ℃ to obtain the porous layered chemical structure modified magnesium lithium silicate.
2. The method for preparing the porous layered chemical structure-modified lithium magnesium silicate for a lithium battery positive electrode material according to claim 1, wherein the method comprises the following steps: the quaternary ammonium salt is one or any combination of dodecyl trimethyl ammonium bromide, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide and hexadecyl trimethyl ammonium chloride.
3. The method for preparing the porous layered chemical structure-modified lithium magnesium silicate for a lithium battery positive electrode material according to claim 1, wherein the method comprises the following steps: the rare earth oxide is La2O3、Ce2O3、Ln2O3One or more of the above components can be combined randomly.
4. The method for preparing the porous layered chemical structure-modified lithium magnesium silicate for a lithium battery positive electrode material according to claim 1, wherein the method comprises the following steps: the soluble manganese salt is one or any combination of manganese sulfate, manganese chloride, manganese nitrate and manganese acetate.
5. The method for preparing the porous layered chemical structure-modified lithium magnesium silicate for a lithium battery positive electrode material according to claim 1, wherein the method comprises the following steps: the soluble ferric salt is one or any combination of ferric sulfate, ferric chloride and ferric nitrate.
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| CN101475196B (en) * | 2009-01-23 | 2010-12-08 | 浙江工业大学 | Method for in-situ synthesizing silicon, magnesium, and lithium containing organic composite multilayer material |
| CN107010707A (en) * | 2017-04-19 | 2017-08-04 | 江苏海明斯新材料科技有限公司 | A kind of preparation method of the universal lithium magnesium silicate lacquer mist coagulant of high-efficiency environment friendly |
| CN107057118A (en) * | 2017-04-19 | 2017-08-18 | 江苏海明斯新材料科技有限公司 | A kind of preparation method of enhancing by polymer copolymer resins intercalation modifying nanoscale organic silicic acid magnesium lithium |
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| EP2497138B1 (en) * | 2009-11-03 | 2016-06-08 | ZPower, LLC | Novel electrodes and rechargeable batteries |
| WO2012050682A2 (en) * | 2010-09-30 | 2012-04-19 | Applied Materials, Inc. | Electrospinning for integrated separator for lithium-ion batteries |
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| CN101475196B (en) * | 2009-01-23 | 2010-12-08 | 浙江工业大学 | Method for in-situ synthesizing silicon, magnesium, and lithium containing organic composite multilayer material |
| CN107010707A (en) * | 2017-04-19 | 2017-08-04 | 江苏海明斯新材料科技有限公司 | A kind of preparation method of the universal lithium magnesium silicate lacquer mist coagulant of high-efficiency environment friendly |
| CN107057118A (en) * | 2017-04-19 | 2017-08-18 | 江苏海明斯新材料科技有限公司 | A kind of preparation method of enhancing by polymer copolymer resins intercalation modifying nanoscale organic silicic acid magnesium lithium |
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