CN113233483A - Preparation method of nano boehmite material - Google Patents
Preparation method of nano boehmite material Download PDFInfo
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- CN113233483A CN113233483A CN202110561137.4A CN202110561137A CN113233483A CN 113233483 A CN113233483 A CN 113233483A CN 202110561137 A CN202110561137 A CN 202110561137A CN 113233483 A CN113233483 A CN 113233483A
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- sodium aluminate
- aluminate solution
- nano
- boehmite
- carbonation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
- C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a nano boehmite material, which comprises the following steps: preparing superfine aluminum hydroxide micropowder from a sodium aluminate solution by using a carbonation method, wherein the concentration of alumina in the sodium aluminate solution is 70-160g/L, the causticization coefficient ak of the sodium aluminate solution is 1.3-1.6, the initial temperature of the sodium aluminate solution before carbonation is 15-30 ℃, and the termination temperature of the sodium aluminate solution after carbonation is 60-80 ℃; baking the superfine aluminum hydroxide micro powder into transition intermediate phase alumina in a kiln, wherein the baking temperature is set to be 500-800 ℃; adding water into the transitional intermediate phase alumina for size mixing, wherein the water-material ratio is (5-10) to 1, and then placing the mixture into a high-pressure reaction kettle for heat preservation to obtain a reaction product; the reaction product is subjected to pressure filtration, washing and drying to obtain the nano-scale crystalline boehmite with the average particle size (D50) of between 100 and 3000 nanometers. The equipment facilities and raw materials involved in the preparation process of the nano boehmite material are conventional prior art, the industrial batch production is easy to realize, the process cost is low, the energy consumption is low, and the environment is friendly.
Description
Technical Field
The invention relates to the field of materials, in particular to a preparation method of a nano boehmite material.
Background
Boehmite (AlOOH) is a precursor of gamma-alumina, and is widely applied to the fields of ceramic materials, composite materials, surface protection layer materials, optical materials, catalysts, carrier materials, semiconductor materials, coatings and the like by virtue of unique chemical, optical and mechanical properties of the boehmite. The boehmite has the intrinsic advantages of low density, small hardness, less adsorbed water, a layered structure and the like, so that the boehmite becomes a high-quality isolating membrane coating material of a lithium ion battery. The national standards for the safety performance of power and 3C batteries are improved, and the coating of a pole piece of a power battery pack is inevitably selected as a ternary battery; compared with NCM, the NCA has higher energy density, and 200-500 nm boehmite is used as one of aluminum sources; the market demand for pole piece coating and anode material synthesis is promoted. With the acceleration of the progress of light weight of batteries, the demand for ultra-fine nano-sized boehmite is gradually increased.
In the fields of electronic PCB substrates and pouring sealant, boehmite can effectively improve the heat resistance and yield of products, and the flame retardant property of the material is also obviously improved. In the field of coating, the plate-like crystal particles of boehmite can inhibit the invasion of water flow into a product and improve the air tightness, moisture resistance, water resistance, aging resistance, flame retardancy and the like.
As the purity requirement of the industry on materials is higher and higher, the application of nano materials is mature. The large-scale and low-cost nano boehmite preparation technology becomes an industrial demand. At present, aluminum salts such as aluminum chloride hexahydrate and aluminum nitrate nonahydrate are mostly adopted for preparing the nano-boehmite for hydrolysis, and anions can corrode equipment in the hydrolysis process, so that the requirement on the equipment is very high. Meanwhile, the byproduct salt can pollute the environment, special treatment is needed, and the organic aluminum alkoxide method has the problems of high cost, difficult industrialization and the like. The method for realizing large-scale and batch industrialization at present is that aluminum hydroxide is used as a raw material, boehmite is prepared by a hydrothermal method, the particle size of the boehmite is large, the average particle size D50 is about 0.8-15 um, and ultrafine boehmite with the D50 below 0.5um cannot be prepared.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a preparation method of a nano-grade boehmite material, which adopts the key technology of gamma alumina reverse reaction, utilizes the gibbsite to generate micro-cracks in the processes of low-temperature roasting and dehydration, and boehmite lattices can grow from the micro-cracks during hydrothermal reverse reaction, thereby realizing the preparation of micro-nano and nano-grade boehmite.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a nano-scale boehmite material comprises the following steps:
s1: preparing superfine aluminum hydroxide micropowder from a sodium aluminate solution by using a carbonation method, wherein the concentration of alumina in the sodium aluminate solution is 70-160g/L, the causticization coefficient ak of the sodium aluminate solution is 1.3-1.6, the initial temperature of the sodium aluminate solution before carbonation is 15-30 ℃, the termination temperature of the sodium aluminate solution after carbonation is 60-80 ℃, and the decomposition rate is 80-95%;
s2: baking the superfine aluminum hydroxide micro powder into r-phase aluminum oxide in a kiln, wherein the baking temperature is set to be 500-800 ℃;
s3: adding water into transitional intermediate phase alumina for size mixing, wherein the water-material ratio is (5-10) to 1, then placing the mixture into a high-pressure reaction kettle for heat preservation, the temperature of the high-pressure reaction kettle is set to be 150-240 ℃, and the heat preservation time is 1-5 hours, so as to obtain a reaction product;
s4: the reaction product is subjected to pressure filtration, washing and drying to obtain the nano-scale crystalline boehmite with the average particle size (D50) of between 100 and 3000 nanometers.
The invention has the beneficial effects that:
(1) the equipment facilities and raw materials involved in the preparation process of the nano boehmite material are conventional prior art, so that the industrial batch production is easy to realize, the process cost is low, and the energy consumption is low; is beneficial to the popularization and the application of the nano boehmite material.
(2) A fine filtering device and ceramic lining equipment can be adopted in the filter pressing stage to avoid the introduction of foreign matters, so that the preparation of a high-purity product is realized;
(3) no harmful waste is discharged in the production process, and the method is environment-friendly;
(4) the prepared nano boehmite has the characteristics of narrow particle size distribution, uniform appearance, good dispersibility, high purity and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a nano-crystalline boehmite XRD pattern;
FIG. 2 is an electron micrograph of nano-crystalline boehmite.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment provides a preparation method of a nano-scale boehmite material, which comprises the following steps:
s1: preparing superfine aluminum hydroxide micropowder from a sodium aluminate solution by using a carbonation method, wherein the concentration of alumina in the sodium aluminate solution is 70-160g/L, the causticization coefficient ak of the sodium aluminate solution is 1.3-1.6, the initial temperature of the sodium aluminate solution before carbonation is 15-30 ℃, the termination temperature of the sodium aluminate solution after carbonation is 60-80 ℃, and the decomposition rate is 80-95%;
s2: baking the superfine aluminum hydroxide micro powder into transition intermediate phase alumina in a kiln, wherein the baking temperature is set to be 500-800 ℃;
s3: adding water into transitional intermediate phase alumina for size mixing, wherein the water-material ratio is (5-10) to 1, then placing the mixture into a high-pressure reaction kettle for heat preservation, the temperature of the high-pressure reaction kettle is set to be 150-240 ℃, and the heat preservation time is 1-5 hours, so as to obtain a reaction product;
s4: the reaction product is subjected to pressure filtration, washing and drying to obtain the nano-scale crystalline boehmite with the average particle size (D50) of between 100 and 3000 nanometers. Fig. 1 and 2 are an XRD chart and an electron micrograph of nano-crystalline boehmite, respectively.
The above embodiments and drawings are only for illustrating the technical solutions of the present invention and not for limiting the present invention, and the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that changes, modifications, additions or substitutions within the spirit and scope of the present invention may be made by those skilled in the art without departing from the spirit of the present invention, and shall also fall within the scope of the claims of the present invention.
Claims (1)
1. A preparation method of a nano-scale boehmite material is characterized by comprising the following steps:
s1: preparing superfine aluminum hydroxide micropowder from a sodium aluminate solution by using a carbonation method, wherein the concentration of alumina in the sodium aluminate solution is 70-160g/L, the causticization coefficient ak of the sodium aluminate solution is 1.3-1.6, the initial temperature of the sodium aluminate solution before carbonation is 15-30 ℃, the termination temperature of the sodium aluminate solution after carbonation is 60-80 ℃, and the decomposition rate is 80-95%;
s2: baking the superfine aluminum hydroxide micro powder into transition intermediate phase alumina in a kiln, wherein the baking temperature is set to be 500-800 ℃;
s3: adding water into transitional intermediate phase alumina for size mixing, wherein the water-material ratio is (5-10) to 1, then placing the mixture into a high-pressure reaction kettle for heat preservation, the temperature of the high-pressure reaction kettle is set to be 150-240 ℃, and the heat preservation time is 1-5 hours, so as to obtain a reaction product;
s4: the reaction product is subjected to pressure filtration, washing and drying to obtain the nano-scale crystalline boehmite with the average particle size (D50) of between 100 and 3000 nanometers.
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| CN202110561137.4A CN113233483A (en) | 2021-05-22 | 2021-05-22 | Preparation method of nano boehmite material |
| CN202210546353.6A CN114873618B (en) | 2021-05-22 | 2022-05-18 | Nanoscale boehmite and preparation method and application thereof |
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| CN202110561137.4A CN113233483A (en) | 2021-05-22 | 2021-05-22 | Preparation method of nano boehmite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2887023B2 (en) * | 1992-03-30 | 1999-04-26 | ワイケイケイ株式会社 | Fine plate-like boehmite particles and method for producing the same |
| DE69722596D1 (en) * | 1996-03-05 | 2003-07-10 | Goro Sato | ALUMINUM OXIDE SOL, METHOD FOR THE PRODUCTION THEREOF, METHOD FOR THE PRODUCTION OF AN ALUMINUM OXIDE PART USING THE SAME AND A CATALYST BASED ON IT FROM ITS ALUMINUM OXIDE |
| CN1149177C (en) * | 2000-11-09 | 2004-05-12 | 中国铝业股份有限公司 | Process for preparing aluminium hydroxide |
| CN1164494C (en) * | 2002-05-31 | 2004-09-01 | 中国石油化工集团公司 | Prepn of gamma-alumina |
| CN100339304C (en) * | 2004-05-21 | 2007-09-26 | 山东铝业股份有限公司 | Sand-like alumina producing method for removing periodic subdivision of species fracture |
| EP3230209A1 (en) * | 2014-12-11 | 2017-10-18 | Pacific Industrial Development Corporation | Process for producing nano-scale crystalline boehmite |
| CN104944454A (en) * | 2015-06-12 | 2015-09-30 | 安徽壹石通材料科技股份有限公司 | Granularity-controllable boehmite preparation method |
| CN110078104A (en) * | 2018-01-25 | 2019-08-02 | 齐鲁工业大学 | A kind of preparation method of boehmite nano powder |
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| CN114873618A (en) | 2022-08-09 |
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Application publication date: 20210810 |