CN113060748B - Submicron boehmite and preparation method - Google Patents
Submicron boehmite and preparation method Download PDFInfo
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- CN113060748B CN113060748B CN202110402841.5A CN202110402841A CN113060748B CN 113060748 B CN113060748 B CN 113060748B CN 202110402841 A CN202110402841 A CN 202110402841A CN 113060748 B CN113060748 B CN 113060748B
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- C—CHEMISTRY; METALLURGY
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- 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
- C01F7/447—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes
- C01F7/448—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes using superatmospheric pressure, e.g. hydrothermal conversion of gibbsite into boehmite
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention provides a method for preparing submicron boehmite from industrial aluminum hydroxide, and relates to the field of new materials. The method comprises the following steps: (1) grinding industrial hydroxide to a certain particle size distribution by a dry method, (2) placing the ground aluminum hydroxide into suspension, and adding grinding aid dispersant. (3) Wet grinding the slurry obtained in the step (2) by using a ball mill, further adjusting the particle size distribution of the slurry, and (4) transferring the ground aluminum hydroxide slurry into a high-pressure reaction kettle to perform hydrothermal reaction to obtain the submicron boehmite. The method has the advantages of easily available raw materials, low cost, short reaction time, low energy consumption, mild conditions and small corrosion to equipment, and can prepare the submicron boehmite with good dispersity, narrow particle size distribution and uniform appearance.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to preparation of an inorganic fine powder material.
Background
Boehmite is also called boehmite, the molecular formula is gamma-AlOOH, and with the attention of China and international society on environmental protection in recent years, boehmite is increasingly applied to the fields of copper-clad plates, lithium battery diaphragm coating, alumina precursors, flame-retardant fillers and the like due to excellent properties. Among them, in the application of copper-clad plates, lithium battery separators and other fields, boehmite with submicron particle size becomes a trend of future development. At present, a plurality of methods for preparing submicron boehmite can not directly use industrial-grade aluminum hydroxide, but deep-processed aluminum hydroxide with the grade of 10 mu m is required to be selected, and the characteristics of poor availability and selectivity of raw materials, high cost, poor morphology uniformity, wide particle size distribution and the like are provided.
CN104944454A discloses a method for preparing boehmite with controllable particle size, wherein the boehmite with 0.1-0.8 micron particle size prepared by the method needs to be treated under the condition of pH less than 5 for 24-40 hours to obtain the boehmite. CN101654269A discloses a method for producing boehmite particles and a method for producing alumina particles, which require hydrothermal reaction of aluminum hydroxide powder and a nucleating agent together, and have a slurry pH of 8 or less and a reaction time of 3 hours or more. The two methods are carried out in an acid environment, so that the corrosion to equipment is serious, or a nucleating agent is required to be added, the reaction time is long, the energy consumption is high, and the production cost is greatly increased.
CN108569713A discloses a method for preparing flake boehmite by an alkaline method and flake boehmite prepared by the method, wherein the median particle size of the boehmite prepared by the method is below 0.873 mu m, the median particle size of aluminum hydroxide is required to be ground to be below 1.083 microns, the solid content is 200g/L, the reaction time is 1-12h, and the pH is 11-14. The method needs to grind the aluminum hydroxide to an extremely small particle size and perform the grinding under a strong alkaline environment, so that the grinding difficulty is greatly improved, equipment is corroded, the solid content is low, the reaction time is long, and the production cost is greatly improved.
Therefore, how to realize the accessibility of raw materials and reduce the production cost, and the preparation of the submicron boehmite with small granularity, good dispersibility, narrow granularity distribution and uniform appearance has important practical significance.
Disclosure of Invention
The invention mainly aims to overcome the defects of the prior art and provide a method for preparing submicron boehmite from industrial aluminum hydroxide, which can prepare submicron boehmite with small granularity, good dispersibility, narrow granularity distribution and uniform appearance; in addition, the method has the advantages of easily available raw materials, low grinding difficulty, short reaction time, high solid content and greatly reduced production cost, the integral reaction is in a weak alkali environment, the corrosion to equipment is small, and the filtrate in the whole process can be recycled and is environment-friendly.
In order to achieve the above object, the first aspect of the present invention provides a method for preparing submicron boehmite from industrial aluminum hydroxide, characterized in that the method comprises the following steps:
(1) dry grinding industrial aluminum hydroxide to obtain a particle size distribution with D10 of 1.5-1.8 μm, D50 of 4-5 μm and D90 of 8-9 μm;
(2) adding water into the ground aluminum hydroxide to prepare a suspension, and adding a grinding-aid dispersing agent;
(3) performing wet ball milling on the slurry obtained in the step (2), and further adjusting the particle size distribution of the slurry to ensure that the slurry has the particle size distribution of D10 of 1.0-1.3 mu m, D50 of 2.6-3.2 mu m and D90 of 5.6-6.5 mu m, so as to obtain aluminum hydroxide slurry;
(4) transferring the aluminum hydroxide slurry obtained in the step (3) into a high-pressure reaction kettle for hydrothermal reaction;
(5) and post-treating the product after the hydrothermal reaction to obtain the submicron boehmite.
In the step (1), a vertical roller mill is adopted as the dry grinding, and the frequency of a powder concentrator (airflow classifier) is 38-42 Hz.
Further, in the step (2), the aluminum hydroxide is adjusted to be slurry with the solid content of 250-600 g/L.
Further, in the step (3), zirconia and/or alumina grinding balls of 2.0 to 2.2mm are used.
As a further preferred, in the step (3), the weight ratio of the grinding balls to the slurry is 5:1-8: 1.
As another preferred mode, in the step (3), a pot mill or a horizontal ball mill is used for ball milling, the rotating speed is 15-25r/min, and the time is 0.5-3 h.
In a typical embodiment, in the step (2), grinding aid selected from one or more of ammonium polyacrylate, polyacrylamide and sodium polyacrylate is introduced into the slurry, and the amount of the grinding aid is 1-8 per mill of the mass of aluminum hydroxide.
In a second aspect the invention provides a submicron boehmite wherein the boehmite has a D50 of 0.3-0.6 μm and a D90<1.3 μm, and a specific surface area of 7-12m 2/g.
The invention has the advantages that industrial aluminum hydroxide is directly used as a raw material, and the boehmite powder with submicron grade and suitable for use can be obtained only by simple grinding and short-time hydrothermal reaction. Strong acid and strong base are not introduced in the preparation process, so that the equipment is not corroded, and the environmental burden of waste liquid treatment is reduced. The invention has the outstanding advantages that the aluminum hydroxide is adjusted to a specific particle size distribution range by the twice grinding process, so that the submicron boehmite obtained after the hydrothermal reaction has the advantages of narrow particle size distribution, uniform appearance and good dispersibility. .
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
figure 1 is a boehmite XRD picture prepared according to the present invention.
Fig. 2 is a particle size distribution of boehmite prepared in example 1.
Fig. 3 is a SEM image of boehmite prepared in example 2.
Fig. 4 is a particle size distribution of boehmite prepared in example 3.
Fig. 5 is a SEM image of boehmite prepared by example 1.
Fig. 6 is a particle size distribution of boehmite prepared in example 2.
Fig. 7 is a SEM image of boehmite prepared in example 3.
Detailed Description
In a first aspect of the invention, the starting material used to produce the submicron boehmite is commercial grade aluminum hydroxide. In the present invention, the term "industrial aluminum hydroxide" means an industrial aluminum hydroxide powder supplied by a manufacturer not directed to a specific use, having a particle size generally in the range of 30 to 100 μm and a purity of not less than 99%, preferably not less than 99.8%, and produced by a method including a Bayer process, a soda lime sintering process, a Bayer-sintering process and an ammonium bicarbonate process. Detailed embodiments according to the present invention are described in detail below.
One-time grinding
It is a feature of the present invention that a process step is performed to obtain a selected distribution for different sources and specifications of industrial aluminum hydroxide. In the present invention, it is important to process the particle size distribution of the aluminum hydroxide raw material to have D10 in the range of 1.5 to 1.8. mu.m, D50 in the range of 4 to 5 μm, and D90 in the range of 8 to 9 μm. The particle size distribution is obtained by performing first-step adjustment on the primary particle distribution of the aluminum hydroxide, so that the primary particle distribution meeting the requirements can be obtained in subsequent wet grinding, the predetermined particle size distribution is shown, the subsequent grinding difficulty can be reduced, the required particle size of the reaction slurry is increased, and the solid content is increased. In one embodiment, the industrial aluminum hydroxide is processed using dry milling. The embodiment of the invention adopts a vertical mill which is a VSLM-1100H type vertical roller mill produced by five full mechanical Limited companies in Dongguan city to refine industrial aluminum hydroxide, and the model of a powder concentrator (airflow classifier) is ATP-NG-450/5, and the frequency is 38-42 Hz.
Secondary grinding
The once ground aluminum hydroxide powder is added with water to prepare a suspension, and the particle size distribution is adjusted by wet ball milling. In the present invention, the particle size distribution of the aluminum hydroxide powder is adjusted to the ranges of D10 of 1.0 to 1.3 μm, D50 of 2.6 to 3.2 μm and D90 of 5.6 to 6.5. mu.m. After hydrothermal reaction is carried out on the aluminum hydroxide slurry containing the particle size distribution, boehmite with ideal particle size and morphology characteristics can be obtained.
In a specific embodiment, the solid content of the suspension is selected from 250-600g/L, zirconia and/or alumina grinding balls with the size of 2mm-2.2mm are selected, the weight ratio of the grinding balls to the slurry is controlled within the range of 5:1-8:1, and the aluminum hydroxide slurry with the required specification can be obtained after ball milling for 0.5-3 h. In the invention, the selection of the grinding balls has great influence on the grinding quality, when the zirconium oxide or aluminum oxide grinding balls with the grain diameter of 2.0-2.2mm are selected, primary particles of the high-solid-content aluminum hydroxide slurry can be ground to a required distribution state in a short time within the range of 5:1-8:1 of the weight ratio of the grinding balls to the slurry, and the primary particles are externally expressed into a preset grain diameter distribution, so that the production efficiency is greatly improved. In the embodiment, the dosage of the grinding balls can be adjusted according to the solid content of the suspension, the higher the solid content is, the dosage of the grinding balls is correspondingly reduced, and the grinding time can be prolonged. The lower the solid content, the more the grinding ball consumption is increased and the grinding time is shortened. However, if the amount of the grinding balls is more than 8:1, the grinding effect is reduced.
As a more preferred approach, a grinding aid dispersant is introduced into the suspension. The grinding-aid dispersing agent is one or more of ammonium polyacrylate, polyacrylamide and sodium polyacrylate, and the dosage of the grinding-aid dispersing agent is 1-8 per mill of the mass of aluminum hydroxide. Through adding the grinding aid dispersant, the viscosity of the slurry can be reduced, the grinding speed and the solid content of the ground slurry are obviously improved, the problem of crust formation of a reaction kettle with high solid content can be solved, the production efficiency is effectively improved, the production cost is reduced, correspondingly, the addition amount of the grinding aid dispersant needs to be increased along with the increase of the solid content of the slurry to be reacted, but after the excessive addition amount exceeds 8 per mill, the reaction cannot be carried out.
Hydrothermal reaction
According to the invention, the hydrothermal reaction is carried out in an autoclave, the reaction temperature is controlled between 190 ℃ and 210 ℃, and the hydrothermal reaction can be completed within 0.5-1h due to the process conditions of the invention.
Post-treatment
In the present invention, the post-treatment operation includes filtering, washing, drying and dispersing the reactant after the hydrothermal reaction. These operations are prior art. Simple filtration achieves a solid-liquid separation, thereby removing a majority of the grinding aid. The trace grinding aid is removed by washing, and pure water washing or slurry washing can be adopted. The drying may be carried out in an oven or a spray dryer, and the dispersion treatment may be carried out using a high-speed pulverizer or a jet mill.
By the above process, D can be obtained500.3-0.6 μm and D90<1.3 μm, specific surface area of 7-12m2Boehmite per g. Fig. 1 is an X-ray diffraction test (XRD) pattern of boehmite obtained by an example of the present invention. All the characteristic peaks at 2 theta angles shown in the figure are characteristic peaks of gamma-AlOOH, and no other impurity peaks.
Thus, according to a second aspect of the present invention, there is provided a submicron boehmite having a primary particle size of 0.3 to 0.6 μm and D90<1.3 μm, specific surface area of 7-12m2/g。
In the following examples, the raw material of industrial aluminum hydroxide is commercially available from Luoyang Xiangjiang Wanji aluminum industries, Ltd.
In the following examples, the raw material of industrial aluminum hydroxide is commercially available from Luoyang Xiangjiang Wanji aluminum industries, Ltd.
Example 1
(1) Industrial aluminium hydroxide is reacted withGrinding by a vertical grinding dry method to obtain D10Is 1.526, D504.225 μm, D908.432 aluminum hydroxide powder.
(2) 400g of dry-ground aluminum hydroxide powder is added with water to prepare 1L of suspension containing 400g/L of solid, and grinding aid dispersant polyacrylamide is added by 6 per mill.
(3) Adding the prepared mixed slurry into a ball mill for grinding for 2 hours, wherein the ball-material ratio is 7:1, and the rotating speed is 25r/min, so as to obtain D10Is 1.235, D503.098 μm, D906.298 μm aluminum hydroxide slurry.
(4) Adding the ground aluminum hydroxide slurry into a high-pressure reaction kettle, sealing, heating with water at 195 ℃ for 0.5h, cooling to room temperature, filtering, washing, drying at 105 ℃ for 10h, and dispersing by using a high-speed pulverizer to finally obtain the monodisperse submicron boehmite. D of the boehmite50At 0.532 μm, the specific surface area is 8.5325m2/g。
Example 2
(1) The industrial aluminum hydroxide is ground by a vertical mill to obtain aluminum hydroxide powder with D10 of 1.658 μm, D50 of 4.432 μm and D90 of 8.591 μm.
(2) 600g of dry-ground aluminum hydroxide powder is added with water to prepare 1L of suspension containing 600g/L of solid, and grinding aid dispersant ammonium polyacrylate is added by 8 per mill.
(3) And adding the prepared mixed slurry into a ball mill for grinding for 3h, wherein the ball-to-material ratio is 5:1, and the rotating speed is 25r/min, so that the aluminum hydroxide slurry with the D10 of 1.093, the D50 of 2.832 microns and the D90 of 5.985 microns is obtained.
(4) Adding the ground aluminum hydroxide slurry into a high-pressure reaction kettle, sealing, heating with water at 195 ℃ for 1h, cooling to room temperature, filtering, washing, drying at 105 ℃ for 10h, and dispersing by using a high-speed pulverizer to finally obtain the monodisperse submicron boehmite. D of the boehmite50At 0.452 μm, the specific surface area is 9.4623m2/g。
Example 3
(1) The industrial aluminum hydroxide is ground by a vertical mill to obtain aluminum hydroxide powder with D10 of 1.812 mu m, D50 of 4.693 mu m and D90 of 8.791 mu m.
(2) 300g of dry-ground aluminum hydroxide powder is added with water to prepare 1L of suspension containing 300g/L of solid, and grinding aid dispersant sodium polyacrylate is added by 5 per mill.
(3) And adding the prepared mixed slurry into a ball mill, and grinding for 1.5h, wherein the ball-to-material ratio is 8:1, and the rotating speed is 20r/min, so that the aluminum hydroxide slurry with the D10 of 1.059, the D50 of 2.625 microns and the D90 of 5.641 microns is obtained.
(3) Adding the ground aluminum hydroxide slurry into a high-pressure reaction kettle, sealing, then carrying out hydrothermal treatment for 1h at the temperature of 200 ℃, cooling to room temperature, then filtering, washing, drying at the temperature of 105 ℃ for 10h, and carrying out dispersion treatment by using a high-speed pulverizer to finally obtain the monodisperse submicron boehmite. D of the boehmite50At 0.387 μm, the specific surface area is 10.3264m2/g。
Comparative example 1
Boehmite was prepared according to the same method as example 3, except that: the industrial aluminum hydroxide is directly ground by a ball mill for 4h until the aluminum hydroxide slurry D10 is 1.436 μm, D50 is 2.727 μm and D90 is 5.442 μm. The median particle size of the boehmite prepared was 0.798 μm.
Comparative example 2
Boehmite was prepared according to the same method as example 3, except that: the ball mill was replaced with a rapid mill, and the obtained aluminum hydroxide slurry had a D10 of 0.904. mu.m, a D50 of 2.635. mu.m, and a D90 of 5.435. mu.m. The median particle size of the boehmite prepared was 1.301. mu.m.
Comparative example 3
Boehmite was prepared according to the same method as example 3, except that: the grinding ball is replaced by a grinding ball with the diameter of about 3mm, the grinding time is 5h, and the obtained aluminum hydroxide slurry D10 is 1.462 μm, D50 is 2.782 μm, and D90 is 5.501 μm. The median particle size of the boehmite prepared was 1.022 μm.
Comparative example 4
Boehmite was prepared according to the same method as example 3, except that: the addition amount of the grinding aid dispersant is 9 per mill, and the XRD result of the reaction product shows that the reaction is not carried out.
The technical solution of the present invention is described in detail with reference to the specific embodiments. The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Claims (9)
1. A process for producing submicron boehmite with industrial aluminum hydroxide, the process comprising the steps of:
(1) dry grinding industrial aluminum hydroxide to obtain a particle size distribution with D10 of 1.5-1.8 μm, D50 of 4-5 μm and D90 of 8-9 μm;
(2) adding water into the ground aluminum hydroxide to prepare a suspension, and adding a grinding-aid dispersant, wherein the dosage of the grinding-aid dispersant is 1-8 per mill of the mass of the aluminum hydroxide;
(3) performing wet ball milling on the slurry obtained in the step (2), and further adjusting the particle size distribution of the slurry to ensure that the slurry has the particle size distribution of D10 of 1.0-1.3 mu m, D50 of 2.6-3.2 mu m and D90 of 5.6-6.5 mu m, so as to obtain aluminum hydroxide slurry;
(4) transferring the aluminum hydroxide slurry obtained in the step (3) into a high-pressure reaction kettle for hydrothermal reaction, wherein the hydrothermal temperature is 190-210 ℃, and the hydrothermal time is 0.5-1 h;
(5) and post-treating the product after the hydrothermal reaction to obtain the submicron boehmite.
2. The method according to claim 1, wherein the industrial aluminum hydroxide in step (1) is commercially available industrial aluminum hydroxide.
3. The method according to claim 1, wherein the dry grinding in the step (1) adopts a vertical roller grinder, and the frequency of an air classifier as a powder concentrator is 38-42 Hz.
4. The method as claimed in claim 1, wherein in the step (2), the aluminum hydroxide is prepared into a slurry with a solid content of 250-600 g/L.
5. The method of claim 1, wherein the grinding aid dispersant in step (2) is one or more of ammonium polyacrylate, polyacrylamide and sodium polyacrylate.
6. The method as claimed in claim 1, wherein in step (3), the ball milling is carried out by using a pot mill or a horizontal ball mill, the rotating speed is 15-25r/min, and the time is 0.5-3 h.
7. The method of claim 1, wherein in step (3) 2.0-2.2mm of zirconia and/or alumina milling balls are used.
8. The method of claim 1, wherein in step (3), the weight ratio of grinding balls to slurry is 5:1 to 8: 1.
9. The method of claim 1, wherein in step (5), the post-treatment comprises filtering, washing, drying and dispersing.
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