CN114436305A - Method for controlling thickness of plate-shaped boehmite - Google Patents
Method for controlling thickness of plate-shaped boehmite Download PDFInfo
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- CN114436305A CN114436305A CN202111656283.1A CN202111656283A CN114436305A CN 114436305 A CN114436305 A CN 114436305A CN 202111656283 A CN202111656283 A CN 202111656283A CN 114436305 A CN114436305 A CN 114436305A
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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
- C01F7/447—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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a plate-shaped boehmite thickness control method, which relates to the technical field of inorganic materials, and compared with the prior art, the plate-shaped boehmite obtained by the invention has more uniform thickness under the condition of uniform length and width; under the condition that the reaction temperature and the reaction time are kept unchanged, the thickness of the platy boehmite is adjusted by adjusting the dosage of the cationic surfactant; the platy boehmite obtained by the hydrothermal reaction has no notch and uniform appearance.
Description
The technical field is as follows:
the invention relates to the technical field of inorganic materials, in particular to a method for controlling the thickness of plate-shaped boehmite.
Background art:
boehmite is also called boehmite, the molecular formula is gamma-AlOOH, the boehmite has unique chemical, optical and mechanical properties, and is widely applied in the fields of catalysis, composite materials, lithium battery diaphragm coating materials and the like, wherein the plate-shaped boehmite lithium battery diaphragm material has more advantages in application.
Many methods for preparing platy boehmite have been reported, for example: solvothermal, microemulsion, hydrothermal methods. In recent years, boehmite with a special structure and morphology is more and more concerned and is synthesized by a hydrothermal method. For example, flower-like boehmite has been synthesized in ZANGANEH N, ZANGANEH S, RAJABI A, et al, flower-like bolt nano structure formation in two-steps [ J ]. Journal of coding Chemistry,2014,67(3): 555-62; hollow microspherical boehmites are synthesized in the literature ZHOU J, CAI W, YANG Z, et al.N, N-dimethyl used conventional synthesis of boehmite microspheres for high effective removal of logo red from water [ J ]. Journal of colloid and Interface Science,2021,583 (128-38).
Patent CN201810592975.6 discloses a method for preparing sheet boehmite by an alkaline process and sheet boehmite, which uses aluminum hydroxide as a raw material, and prepares suspension after ball milling, adds a morphology control agent, then adjusts pH with an inorganic base, and moves the suspension into a high-pressure reaction kettle for hydrothermal reaction, after the hydrothermal reaction is finished, the reactant is cooled to room temperature, and then is filtered, washed, dried and depolymerized to obtain diamond sheet boehmite, but as can be seen from an electron microscope image, the thickness of the sheet boehmite is not uniform.
The invention content is as follows:
the invention aims to provide a method for controlling the thickness of plate-shaped boehmite, and the plate-shaped boehmite with uniform thickness is prepared by the method.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a method for controlling the thickness of plate-shaped boehmite comprises the following steps:
(1) mixing aluminum hydroxide and water to form aluminum hydroxide slurry, and performing ultrasonic dispersion to obtain a suspension;
(2) mixing the suspension obtained in the step (1) with a cationic surfactant, and fully stirring;
(3) and (3) carrying out hydrothermal reaction on the mixture obtained in the step (2), and filtering, washing and drying to obtain the platy boehmite.
The mass ratio of the aluminum hydroxide to the water is 1: 2-1: 5.
The cationic surfactant is at least one of Dodecyl Dimethyl Benzyl Ammonium Chloride (DDBAC), Dodecyl Trimethyl Ammonium Chloride (DTAC) and hexadecyl trimethyl ammonium bromide (CTAB).
The dosage of the cationic surfactant is 0.125-7.5% of the mass of the aluminum hydroxide slurry. .
The reaction temperature of the hydrothermal reaction is 180-220 ℃, and the reaction time is 24-48 h.
The drying temperature is 80-110 ℃, and the drying time is 8-20 h.
The plate-shaped boehmite has a thickness of 50-800 nm, a purity of 99% or more, and a crystallinity of 95% or more.
The invention has the beneficial effects that:
1. compared with the prior art, the plate-shaped boehmite obtained by the invention has more uniform thickness under the condition of uniform length and width; under the condition that the reaction temperature and the reaction time are kept unchanged, the thickness of the platy boehmite is adjusted by adjusting the dosage of the cationic surfactant.
2. The platy boehmite obtained by the hydrothermal reaction has no notch and uniform appearance.
Description of the drawings:
FIG. 1 is an SEM photograph of plate-like boehmite obtained in example 1;
FIG. 2 is an SEM photograph of the plate-like boehmite obtained in example 2;
FIG. 3 is an SEM photograph of the plate-like boehmite obtained in example 3;
FIG. 4 is an SEM photograph of the plate-like boehmite obtained in example 4;
FIG. 5 is an SEM photograph of the plate-like boehmite obtained in example 5;
FIG. 6 is an SEM photograph of the plate-like boehmite obtained in example 6;
FIG. 7 is an SEM photograph of plate-like boehmite obtained in example 7;
FIG. 8 is an SEM photograph of plate-like boehmite obtained in example 8;
FIG. 9 is an SEM photograph of the plate-like boehmite obtained in comparative example 1;
FIG. 10 is an SEM photograph of the plate-like boehmite obtained in comparative example 2;
FIG. 11 is an SEM image of plate-like boehmite obtained in comparative example 3;
FIG. 12 is an XRD pattern of platy boehmites corresponding to examples 1-8
The specific implementation mode is as follows:
in order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easy to understand, the invention is further explained by combining the specific embodiments and the drawings.
The aluminum hydroxide used in the following examples was aluminum hydroxide having a particle size of 5 μm sold by Amano-Shitong cermet materials Co.
Example 1
Mixing 10g of aluminum hydroxide, 0.05g of DDBAC and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 200 ℃ for 24 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 80 ℃ for 8 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 1, the boehmite prepared has a plate-like structure, a length and width of about 1.2 μm, and a thickness of 300 to 500nm, and as can be seen from fig. 12, the boehmite purity is 99.86% and the crystallinity is 95.3%.
Example 2
Mixing 10g of aluminum hydroxide, 0.15g of DDBAC and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 200 ℃ for 24 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 80 ℃ for 8 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 2, the boehmite prepared has a plate-like structure, a length and width of about 1.2 μm, and a thickness of 400 to 600nm, and as can be seen from fig. 12, the boehmite purity was 99.92% and the crystallinity was 95.9%.
Example 3
Mixing 10g of aluminum hydroxide, 3g of DDBAC and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 200 ℃ for 24 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 80 ℃ for 8 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 3, the boehmite prepared has a plate-like structure, a length and width of about 1.2 μm, and a thickness of 500 to 800nm, and as can be seen from fig. 12, the boehmite purity was 99.98% and the crystallinity was 96.2%.
Example 4
Mixing 10g of aluminum hydroxide, 0.05g of DTAC and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 200 ℃ for 24 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 100 ℃ for 18 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 4, the boehmite prepared has a plate-like structure, a length and a width of about 1 μm, and a thickness of 200 to 300nm, and as can be seen from fig. 12, the boehmite purity is 99.96% and the crystallinity is 95.8%.
Example 5
Mixing 10g of aluminum hydroxide, 0.15g of DTAC and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 200 ℃ for 24 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 100 ℃ for 18 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 5, the boehmite prepared has a plate-like structure, a length and width of about 1 μm, and a thickness of 300 to 500nm, and as can be seen from fig. 12, the boehmite purity was 99.76% and the crystallinity was 96.4%.
Example 6
Mixing 10g of aluminum hydroxide, 3g of DTAC and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 200 ℃ for 24 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 100 ℃ for 18 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 6, the boehmite prepared has a plate-like structure, a length and width of about 1 μm, and a thickness of 500 to 600nm, and as can be seen from fig. 12, the boehmite purity was 99.89%, and the crystallinity was 95.6%.
Example 7
Mixing 10g of aluminum hydroxide, 0.05g of CTAB and 20g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 180 ℃ for 48 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 110 ℃ for 20 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 7, the boehmite prepared has a plate-like structure, a length and width of about 400nm, and a thickness of 150 to 250nm, and as can be seen from fig. 12, the boehmite purity is 99.73% and the crystallinity is 96.2%.
Example 8
Mixing 10g of aluminum hydroxide, 3g of CTAB and 50g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at 220 ℃ for 48 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 110 ℃ for 20 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 8, the boehmite prepared has a plate-like structure, a length and width of about 400nm, and a thickness of 50 to 150nm, and as can be seen from fig. 12, the boehmite purity is 99.81% and the crystallinity is 95.9%.
Comparative example 1 (no cationic surfactant added)
Mixing 10g of aluminum hydroxide and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 200 ℃ for 24 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 80 ℃ for 12 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 9, the boehmite prepared has non-uniform morphology and size, some of which grow into a plate-like structure, and some of which have more notches.
Comparative example 2 (addition of nonionic surfactant PVP)
Mixing 10g of aluminum hydroxide, 3g of PVP and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (2) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction for 24 hours at the temperature of 200 ℃. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 80 ℃ for 12 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from FIG. 10, the thickness of the boehmite obtained was not uniform and ranged from 100 to 1000 nm.
Comparative example 3 (addition of anionic surfactant SDS)
Mixing 10g of aluminum hydroxide, 3g of SDS and 30g of water to form aluminum hydroxide slurry, performing ultrasonic dispersion for 15min to obtain a suspension, and fully stirring the suspension until the suspension is uniformly mixed for 12 h; and (3) putting the mixture obtained in the step (A) into a high-pressure hydrothermal reaction kettle, sealing, and then carrying out hydrothermal reaction at the temperature of 200 ℃ for 24 hours. And (3) carrying out suction filtration on a product after the hydrothermal reaction, washing the product with distilled water for three times, washing the product with absolute ethyl alcohol for one time, drying the product in a vacuum drying oven at the temperature of 80 ℃ for 12 hours, and finally observing the size of the platy boehmite through an SEM (scanning electron microscope).
As can be seen from fig. 11, the boehmite prepared was produced in a large amount of small crushed particles and in a non-uniform size.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A method for controlling the thickness of plate-shaped boehmite is characterized in that: the method comprises the following steps:
(1) mixing aluminum hydroxide and water to form aluminum hydroxide slurry, and performing ultrasonic dispersion to obtain a suspension;
(2) mixing the suspension obtained in the step (1) with a cationic surfactant, and fully stirring;
(3) and (3) carrying out hydrothermal reaction on the mixture obtained in the step (2), and filtering, washing and drying to obtain the platy boehmite.
2. The method for controlling the thickness of plate-like boehmite according to claim 1, characterized in that: the mass ratio of the aluminum hydroxide to the water is 1: 2-1: 5.
3. The method for controlling the thickness of plate-like boehmite according to claim 1, characterized in that: the cationic surfactant is at least one of Dodecyl Dimethyl Benzyl Ammonium Chloride (DDBAC), Dodecyl Trimethyl Ammonium Chloride (DTAC) and hexadecyl trimethyl ammonium bromide (CTAB).
4. The method for controlling the thickness of plate-like boehmite according to claim 1, characterized in that: the dosage of the cationic surfactant is 0.125-7.5% of the mass of the aluminum hydroxide slurry.
5. The method for controlling the thickness of plate-like boehmite according to claim 1, characterized in that: the reaction temperature of the hydrothermal reaction is 180-220 ℃, and the reaction time is 24-48 h.
6. The method for controlling the thickness of plate-like boehmite according to claim 1, characterized in that: the drying temperature is 80-110 ℃, and the drying time is 8-20 h.
7. The method for controlling the thickness of plate-like boehmite according to claim 1, characterized in that: the plate-shaped boehmite has a thickness of 50-800 nm, a purity of 99% or more, and a crystallinity of 95% or more.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115304405A (en) * | 2022-07-29 | 2022-11-08 | 广东精英无机材料有限公司 | Boehmite digital glaze ink and preparation method thereof |
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US5306680A (en) * | 1992-03-30 | 1994-04-26 | Yoshida Kogyo K.K. | Fine flaky boehmite particles and process for the preparation of the same |
US20090104108A1 (en) * | 2005-03-23 | 2009-04-23 | Ki-Won Jun | Method of Preparing Boehmite and Gamma-Alumina With High Surface Area |
CN108569713A (en) * | 2018-06-11 | 2018-09-25 | 洛阳中超新材料股份有限公司 | Alkaline process prepares the method and sheet boehmite of sheet boehmite |
CN111924865A (en) * | 2020-08-05 | 2020-11-13 | 北京化工大学 | Crystal face selective growth boehmite and preparation method thereof |
CN112607759A (en) * | 2020-12-15 | 2021-04-06 | 安徽壹石通材料科技股份有限公司 | Boehmite morphology control method |
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US5306680A (en) * | 1992-03-30 | 1994-04-26 | Yoshida Kogyo K.K. | Fine flaky boehmite particles and process for the preparation of the same |
US20090104108A1 (en) * | 2005-03-23 | 2009-04-23 | Ki-Won Jun | Method of Preparing Boehmite and Gamma-Alumina With High Surface Area |
CN108569713A (en) * | 2018-06-11 | 2018-09-25 | 洛阳中超新材料股份有限公司 | Alkaline process prepares the method and sheet boehmite of sheet boehmite |
CN111924865A (en) * | 2020-08-05 | 2020-11-13 | 北京化工大学 | Crystal face selective growth boehmite and preparation method thereof |
CN112607759A (en) * | 2020-12-15 | 2021-04-06 | 安徽壹石通材料科技股份有限公司 | Boehmite morphology control method |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115304405A (en) * | 2022-07-29 | 2022-11-08 | 广东精英无机材料有限公司 | Boehmite digital glaze ink and preparation method thereof |
CN115304405B (en) * | 2022-07-29 | 2023-09-26 | 广东精英无机材料有限公司 | Boehmite digital glaze ink and preparation method thereof |
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