CN106186008B - Boehmite for lithium battery diaphragm coating and hydrothermal preparation method thereof - Google Patents
Boehmite for lithium battery diaphragm coating and hydrothermal preparation method thereof Download PDFInfo
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Abstract
The invention provides boehmite for a lithium battery diaphragm ceramic coating and a hydrothermal preparation method thereof3+Hydrolyzing the salt solution, aging, and press filtering to obtain the final productAnd putting the shaped aluminum precursor into a reaction kettle for hydrothermal reaction to obtain monodisperse and high-purity boehmite powder. The synthesized boehmite particles have high dispersibility and narrow particle size distribution, and the specific surface area is 2-15 m2The average grain diameter is 500-800 nm, and the purity is up to 99.95%. The method of the invention adopts inorganic flame retardant, inorganic catalyst, sewage treatment material and the like, and the prepared boehmite has high purity, high dispersity, good crystallinity and narrow particle size distribution.
Description
Technical Field
The invention relates to the technical field of inorganic non-metallic materials, in particular to boehmite for a lithium battery diaphragm coating and a hydrothermal preparation method thereof.
Background
Boehmite (Boehmite), also known as Boehmite or Boehmite, has the molecular formula of γ -AlOOH, AlO (OH) (hydrated alumina), is an alumina hydrate which is incompletely crystallized and contains one crystal water, belongs to an orthorhombic system, and has a layered structure. In these lamellar structures, one aluminum ion (A1)3+) With 6 oxygen ions (O) surrounding2-) A deformed octahedron is formed, the common octahedron boundary of oxygen ions is formed by connecting double-layer zigzag hydrogen bonds, and the unique structure makes it in preparation of α -Al2O3The material has great application prospect in the fields of important precursor materials, inorganic flame retardants, inorganic catalysts, adsorbents, sewage treatment materials and the like.
Boehmite has been used in the coating material for battery separator, and even boehmite products specifically used in the coating material for battery separator are commercially available, which is effective in achieving a coating effect similar to α -Al2O3The function of (1): avoid short circuit between the electrode, improve the security of lithium cell use to can promote the imbibition liquid retaining property to electrolyte. Moreover, the synthesized boehmite is far cheaperAt α -Al2O3Using boehmite instead of α -Al2O3As a diaphragm coating ceramic material, the coating diaphragm can greatly reduce the production cost of the coating diaphragm, and reduce the abrasion of the alumina with high hardness to a micro-concave roller during coating and the abrasion to a blade during diaphragm slitting.
In recent years, the technology for preparing boehmite materials has been rapidly developed, and many new synthesis methods have appeared, such as a gas phase method, a solvent thermal synthesis method (hydrothermal synthesis method), a sol-gel method, a precipitation method, an ionic liquid method, a hard template method, and the like. The boehmite material prepared by the method disclosed in the Chinese patent publication No. CN 103663519A uses metaaluminate as an aluminum source and urea as a precipitator, and boehmite with a diameter of 2-5 microns and a micro-nano hierarchical structure is prepared under the conditions of reaction for 2-24 hours at 130-200 ℃ in a hydrothermal environment. The Chinese patent publication No. CN 103011215A uses sodium aluminate and urea as raw materials, and the raw materials are heated to 140-180 ℃ in a high-temperature high-pressure reaction kettle, and the temperature is kept for 8-15 hours, so as to obtain the boehmite micro-nano structure spherical powder material. Chinese patent publication No. CN 102815733 a adopts pseudo-boehmite, inorganic acid or inorganic base as raw materials, and performs hydrothermal reaction in a high-pressure reaction kettle to obtain nano-grade boehmite. The Chinese patent publication No. CN 102701244A is to mix an aluminum salt solution and a precipitant in a hydrothermal reaction kettle, and react for 6-24 hours under hydrothermal conditions at a temperature of 120-200 ℃ to obtain boehmite ultrafine powder.
The invention aims to provide a method for preparing rhombic platy boehmite with uniformly dispersed particles, high purity and narrow particle size distribution. The synthesized boehmite can solve the defects of the alumina used in the prior diaphragm coating process, greatly reduce the cost, and reduce the abrasion of the alumina on a micro-concave roller during coating and the abrasion of a blade during diaphragm slitting.
Disclosure of Invention
The invention aims to provide a method for preparing boehmite with high particle dispersibility, narrow particle size distribution and high purity, which can solve the defects of the existing industrial production process, simplify the process and reduce the cost, and the prepared boehmite has high purity, high dispersity, good crystallinity and narrow particle size distribution.
The invention provides a preparation method for synthesizing boehmite by a hydrothermal method, which comprises the following steps:
(a) heating the pure water solution to 30-100 ℃;
(b) dissolving Al salt in pure water, and stirring to obtain an Al salt solution;
(c) dripping the precipitant solution into the Al salt solution, stirring and hydrolyzing;
(d) rapidly adjusting the pH value of the solution to 3.5-5.5, and then aging the solution at constant temperature for 1-10 hours;
(e) after aging, removing water in the solid-liquid mixture;
(f) putting the obtained amorphous aluminum precursor and precipitator solution into a (large) high-temperature high-pressure reaction kettle for reaction, wherein the filling degree is 60-80%;
(g) heating the reaction kettle to 150-250 ℃ under a rapid stirring state, and naturally cooling to obtain gamma-AlOOH slurry;
(h) washing the obtained gamma-AlOOH slurry for 1-7 times, and then carrying out spray drying to obtain boehmite powder.
Preferably, the temperature during hydrolysis in the step (c) is 40-70 ℃, preferably 50-65 ℃, and the stirring speed is 200-1000 rpm.
Preferably, the pH value of the solution in the step (d) is adjusted for 0.01-6 min, the effect is better when the adjusting speed is 0.01-3 min, the pH value is controlled to be 3.5-5.5, and the reaction is more favorable when the pH value is 4.0-5.0; aging for 1-10 hours at constant temperature, and preferably aging for 3-7 hours at constant temperature.
Preferably, the heating rate in the step (g) is controlled to be 0.5-4.0 ℃/min, and the effect is better when the heating rate reaches 1.0-3.0 ℃/min; the stirring speed of the reaction kettle is 200-1000 rpm, preferably 400-800 rpm.
Preferably, in the step (g), after the temperature of the reaction kettle is raised to 150-250 ℃, preferably 160-220 ℃; the temperature is preserved for 2-10 hours, preferably 2-7 hours, and then the temperature is naturally reduced.
Preferably, the concentration of the aluminum precursor in the mixed liquid in the reaction kettle in the step (f) is 0.1-2.0 mol.L-1Further, 0.4 to 1.0 mol.L-1。
Preferably, the Al salt in step (b) is selected from Al (NO)3)3·9H2O or AlCl3·6H2O, preferably Al (NO)3)3·9H2O。
Preferably, the precipitant solution is selected from urea, or NH3·H2O, or urea and NH3·H2Mixture of O, preferably urea and NH3·H2And O, mixing the solution.
Preferably, the water removal means of the solid-liquid mixture in step (e) is selected from filtration, pressure filtration or dewatering with a dewatering machine.
According to the method, boehmite powder is synthesized and prepared, wherein the boehmite powder is rhombic platy monodisperse particles, the crystallinity is high, and the specific surface area is 2-15 m2(ii)/g, the average particle diameter is 500-800 nm, and the purity is more than 99.95%.
The method is characterized in that a hydrothermal method is adopted, and the morphology of boehmite synthesized is controlled by controlling experimental parameters (such as aluminum source, temperature, PH value, precipitant and the like) of the whole process. The synthesized boehmite particles have high dispersibility and narrow particle size distribution, and the specific surface area is 2-15 m2The average particle size is 500-800 nm, the purity is up to 99.95%, and the method can be applied to coating of a lithium battery diaphragm with a ceramic material and preparation of α -Al2O3Important precursor materials, inorganic flame retardants, inorganic catalysts, sewage treatment materials and the like. The invention aims to provide a method for preparing rhombic platy boehmite with uniformly dispersed particles, high purity and narrow particle size distribution. The synthesized boehmite can solve the defects of the alumina used in the prior diaphragm coating process, greatly reduce the cost, and reduce the abrasion of the alumina on a micro-concave roller during coating and the abrasion of a blade during diaphragm slitting. The prepared boehmite has high purity, high dispersity, good crystallinity and narrow particle size distribution.
Drawings
FIG. 1 is a process flow diagram of the present invention
FIG. 2 scanning electron micrographs of a synthesized boehmite product according to the invention
FIG. 3 scanning electron micrograph of a synthesized boehmite product according to the present invention coated on a surface of a lithium battery separator
Detailed Description
The invention will be further described with reference to specific examples and figures, but the scope of protection of the invention is not limited to the examples described.
Example 1
(1) Heating the pure water solution to 100 ℃;
(2) accurately weighing AlCl according to stoichiometric ratio3·6H2Dissolving the obtained product in pure water, and stirring at a stirring speed of 200rpm to obtain a salt solution;
(3) the stirring speed is increased to 350rpm, the temperature of the solution is controlled at 70 ℃, and then the precipitator urea is quickly dripped into the Al3+The salt solution is hydrolyzed;
(4) quickly titrating within 6min until the pH value of the solution is 5.5, then keeping the stirring speed of 350rpm, and aging for 1 hour at the constant temperature of 70 ℃;
(5) aging at constant temperature to obtain solid-liquid mixture containing precipitate, press filtering to remove water, adding the obtained amorphous aluminum precursor and precipitant urea into (large) high-temperature high-pressure reaction kettle to fill 80%, and controlling the concentration of aluminum precursor to be 2.0 mol.L-1；
(6) Heating the reaction kettle to 250 ℃ at the heating rate of 4.0 ℃/min under stirring at the stirring speed of 200rpm, controlling the heat preservation time to be 2 hours, and naturally cooling to obtain gamma-AlOOH slurry;
(7) the obtained gamma-AlOOH slurry was washed with ultrapure water 7 times and then spray-dried to obtain monodisperse, high-purity boehmite powder. The synthesized boehmite particles have high dispersibility, narrow particle size distribution and specific surface area of 2.2m2The average grain diameter is 530nm, and the purity is up to 99.95 percent.
Example 2
(1) Heating the pure water solution to 75 ℃;
(2) accurately weighing Al (NO) in stoichiometric ratio3)3·9H2O, dissolving it inStirring in pure water at a stirring speed of 400rpm to prepare a salt solution;
(3) the stirring speed is increased to 500rpm, the solution temperature is controlled at 60 ℃, and NH is added3·H2Quickly dripping O solution into Al3+The salt solution is hydrolyzed;
(4) quickly titrating within 4min until the pH value of the solution is 4.8, then keeping the stirring speed of 500rpm, and aging at the constant temperature of 60 ℃ for 3 hours;
(5) aging at constant temperature to obtain solid-liquid mixture containing precipitate, dewatering to remove water, and mixing the amorphous aluminum precursor with NH3·H2The O solution is put into a (large) high-temperature high-pressure reaction kettle, added to 80 percent of the filling degree, and the concentration of the aluminum precursor is controlled to be 1.2 mol.L-1；
(6) Heating the reaction kettle to 210 ℃ at the heating rate of 2.8 ℃/min under stirring at 450rpm, controlling the heat preservation time to be 3.5 hours, and naturally cooling to obtain gamma-AlOOH slurry;
(7) and washing the obtained gamma-AlOOH slurry for 5 times by using ultrapure water, and then carrying out spray drying to obtain monodisperse and high-purity boehmite powder. The synthesized boehmite particles have high dispersibility, narrow particle size distribution and specific surface area of 5.6m2The average grain diameter is 780nm, and the purity is up to 99.95 percent.
Example 3
(1) Heating the pure water solution to 50 ℃;
(2) accurately weighing Al (NO) in stoichiometric ratio3)3·9H2Dissolving the obtained product in pure water, and stirring at a stirring speed of 650rpm to obtain a salt solution;
(3) keeping the stirring speed at 650rpm, controlling the temperature of the solution at 50 ℃, and precipitating agents of urea and NH3·H2The mixture solution of O and Al is quickly dropped into Al3+The salt solution is hydrolyzed;
(4) quickly titrating within 2.0min until the pH value of the solution is 4.2, and then aging at the constant temperature of 50 ℃ for 6 hours at the stirring speed of 650 rpm;
(5) aging at constant temperature to obtain solid-liquid mixture containing precipitate, filtering to remove water,the obtained amorphous aluminum precursor, precipitating agents of urea and NH3·H2The mixture solution of the O and the O is put into a (large) high-temperature high-pressure reaction kettle, the mixture solution is added to 80 percent of the filling degree, and the concentration of the aluminum precursor is controlled to be 0.62 mol.L-1；
(6) Heating the reaction kettle to 185 ℃ at the heating rate of 1.6 ℃/min under the stirring speed of 750rpm, controlling the heat preservation time to be 6 hours, and naturally cooling to obtain gamma-AlOOH slurry;
(7) washing the obtained gamma-AlOOH slurry with ultrapure water for 4 times, and then carrying out spray drying to obtain monodisperse and high-purity boehmite powder. The synthesized boehmite particles have high dispersibility, narrow particle size distribution and specific surface area of 8.9m2Per gram, the average particle diameter is 680nm, and the purity is as high as 99.95 percent.
Example 4
(1) Heating the pure water solution to 30 ℃;
(2) accurately weighing Al (NO) in stoichiometric ratio3)3·9H2Dissolving the obtained product in pure water, and stirring at a stirring speed of 1000rpm to obtain a salt solution;
(3) controlling the temperature of the solution at 40 ℃ under the stirring state of 1000rpm, and precipitating agents of urea and NH3·H2The mixture solution of O and Al is quickly dropped into Al3+The salt solution is hydrolyzed;
(4) quickly titrating within 0.5min until the pH value of the solution is 3.5, and then aging at the constant temperature of 40 ℃ for 10 hours at the stirring speed of 1000 rpm;
(5) aging at constant temperature to obtain solid-liquid mixture containing precipitate, press filtering to remove water, and mixing the obtained amorphous aluminum precursor with precipitating agent urea and NH3·H2The mixture solution of the O and the O is put into a (large) high-temperature high-pressure reaction kettle, added to 80 percent of the filling degree, and the concentration of the aluminum precursor is controlled to be 0.1 mol.L-1；
(6) Heating the reaction kettle to 150 ℃ at the heating rate of 0.5 ℃/min under stirring at the stirring speed of 1000rpm, controlling the heat preservation time to be 10 hours, and naturally cooling to obtain gamma-AlOOH slurry;
(7) washing the obtained gamma-AlOOH slurry with ultrapure waterWashing for 3 times, and spray drying to obtain monodisperse high-purity boehmite powder. The synthesized boehmite particles have high dispersibility, narrow particle size distribution and specific surface area of 15m2The average grain diameter is 690nm, and the purity is up to 99.95%.
The present invention has been described in detail for the purpose of illustration and understanding, but the present invention is not limited to the embodiments, and any changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit of the present invention are intended to be equivalent replacements within the scope of the present invention.
Claims (13)
1. A hydrothermal preparation method of boehmite for a lithium battery diaphragm coating mainly comprises the following steps:
(a) heating the pure water solution to 30-100 ℃;
(b) dissolving Al salt in pure water, and stirring to obtain an Al salt solution;
(c) dripping the precipitant solution into the Al salt solution, stirring and hydrolyzing;
(d) rapidly adjusting the pH value of the solution to 3.5-5.5, and then aging the solution at constant temperature for 1-10 hours;
(e) after aging, removing water in the solid-liquid mixture;
(f) putting the obtained amorphous aluminum precursor and precipitator solution into a high-temperature high-pressure reaction kettle for reaction, wherein the filling degree is 60-80%;
(g) heating the reaction kettle to 150-250 ℃ under a stirring state, and naturally cooling to obtain gamma-AlOOH slurry;
(h) washing the obtained gamma-AlOOH slurry for 1-7 times, and then carrying out spray drying to obtain boehmite powder;
the Al salt in the step (b) is Al (NO)3)3·9H2O or AlCl3·6H2O；
The precipitant solution is urea or NH3·H2O or a mixture of the two;
the boehmite powder is rhombic platy monodisperse particles, and the specific surface area is 2-15 m2(ii) g, average particle diameter of 500 to 800nmThe purity is more than 99.95 percent.
2. The method according to claim 1, wherein the hydrolysis temperature in the step (c) is 40 to 70 ℃ and the stirring speed is 200 to 1000 rpm.
3. The method according to claim 2, wherein the hydrolysis temperature in the step (c) is 50 to 65 ℃.
4. The method according to claim 1, wherein the time for adjusting the pH of the solution in the step (d) is 0.01 to 6 min; the pH value is 4.0-5.0, and the constant-temperature aging is carried out for 3-7 hours.
5. The method according to claim 4, wherein the pH of the solution is adjusted in the step (d) for 0.01 to 3 min.
6. The method according to claim 1, wherein the temperature rise rate in the step (g) is controlled to be 0.5 to 4.0 ℃/min; the stirring speed of the reaction kettle is 200-1000 rpm.
7. The method according to claim 6, wherein the temperature rise rate in the step (g) is controlled to be 1.0 to 3.0 ℃/min; the stirring speed of the reaction kettle is 400-800 rpm.
8. The preparation method according to claim 1, 6 or 7, characterized in that in the step (g), after the temperature of the reaction kettle is raised to 150-250 ℃, the temperature is maintained for 2-10 hours, and then the temperature is lowered.
9. The preparation method according to claim 8, wherein in the step (g), the temperature of the reaction kettle is raised to 150-250 ℃, and then is maintained for 3-7 hours, and then is lowered.
10. The method according to claim 1, wherein the concentration of the aluminum precursor in the mixed solution in the reaction kettle in the step (f) is 0.1-2.0 mol-L-1。
11. The method according to claim 10, wherein the concentration of the aluminum precursor in the mixed solution in the reaction kettle in the step (f) is 0.5 to 1.3 mol-L-1。
12. The method according to claim 1, wherein the step (e) of removing water from the solid-liquid mixture is performed by filtration, pressure filtration or dehydration with a dehydrator.
13. Boehmite for lithium battery separator coating prepared by the method according to any one of claims 1 to 12, characterized in that boehmite powder is a plate-like monodisperse particle having a rhombohedral shape and a specific surface of 2 to 15m2(ii)/g, the average particle diameter is 500-800 nm, and the purity is more than 99.95%.
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| CN107946521A (en) * | 2017-11-29 | 2018-04-20 | 山东聊城瑞利金属材料有限公司 | A kind of lithium battery diaphragm aluminium oxide manufacture method of boehmite coating |
| CN110197886A (en) * | 2018-02-26 | 2019-09-03 | 宁德新能源科技有限公司 | A kind of isolation film and electrochemical appliance |
| CN109534376A (en) * | 2019-01-17 | 2019-03-29 | 滨州市金毅设备有限公司 | A kind of high purification preparation method of boehmite |
| CN110357135B (en) * | 2019-06-19 | 2020-11-24 | 苏州盛曼特新材料有限公司 | Preparation method of special alumina for high-purity lithium battery diaphragm |
| CN110451538A (en) * | 2019-08-20 | 2019-11-15 | 中铝山东有限公司 | A kind of preparation method of high-purity boehmite and high purity aluminium oxide |
| CN111341982B (en) * | 2020-03-18 | 2022-11-25 | 江苏厚生新能源科技有限公司 | Coated diaphragm, preparation method, doped boehmite, ceramic slurry and lithium battery |
| CN111792660A (en) * | 2020-07-15 | 2020-10-20 | 东北大学 | Method for producing boehmite micro-nano powder by using aluminum chloride |
| CN113860342B (en) * | 2021-11-05 | 2023-08-08 | 中化学科学技术研究有限公司 | Method for preparing high-purity parallelepiped boehmite and high-purity parallelepiped boehmite |
| CN114538488A (en) * | 2022-02-23 | 2022-05-27 | 山东诚祥新能源股份有限公司 | Preparation method of high-purity boehmite for lithium battery diaphragm |
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| JP3694627B2 (en) * | 1999-12-28 | 2005-09-14 | キンセイマテック株式会社 | Method for producing flaky boehmite particles |
| US8282897B2 (en) * | 2010-08-25 | 2012-10-09 | Kuwait Institute for Scientific Reaearch | Process for recovering boehmite and y-AI2O3 from spent hydroprocessing catalysts |
| CN103303951B (en) * | 2013-07-05 | 2015-08-19 | 泰山医学院 | A kind of hydrothermal synthesis method of boehmite superfine powder of core-shell structure |
| CN105417562B (en) * | 2015-12-28 | 2018-01-30 | 深圳市星源材质科技股份有限公司 | A kind of preparation method of hydro-thermal method synthesis alpha-aluminium oxide |
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