CN113666402A - Hydroxy aluminum oxide nano material and preparation method thereof - Google Patents

Hydroxy aluminum oxide nano material and preparation method thereof Download PDF

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CN113666402A
CN113666402A CN202110929692.8A CN202110929692A CN113666402A CN 113666402 A CN113666402 A CN 113666402A CN 202110929692 A CN202110929692 A CN 202110929692A CN 113666402 A CN113666402 A CN 113666402A
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anhydrous
aluminum
anhydrous ethanol
aluminum chloride
nano
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CN113666402B (en
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李艳伟
邢旭宏
崔航
罗亚肖
余红
吴佳怡
杨晓莹
李萌萌
王雪
张剑
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Jilin University
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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
    • C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • 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
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/45—Aggregated particles or particles with an intergrown morphology
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    • 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

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Abstract

The invention relates to a hydroxy aluminum oxide nano material and a preparation method thereof, belonging to the field of preparation of IIIA group hydroxy oxide nano materials. The aluminum oxyhydroxide nano material is composed of an aluminum oxyhydroxide nano cone and a nano flower formed by self-assembling the nano cone. The preparation method comprises the following steps: adding anhydrous aluminum chloride into anhydrous ethanol, and uniformly mixing by adopting a magnetic stirrer; then adding oleic acid into the mixed solution of anhydrous aluminum chloride and anhydrous ethanol, and continuously and uniformly mixing the oleic acid and the anhydrous aluminum chloride and the anhydrous ethanol by adopting a magnetic stirrer; then pouring the mixed solution into a reaction kettle, and sealing and preserving heat for 24-48 h at the temperature of 180-200 ℃; and after the reaction is finished, naturally cooling to room temperature, and cleaning, drying and grinding the product to obtain white hydroxy alumina powder. The method has the advantages of simple operation method, easy control, good repeatability, high sample purity and good crystallinity.

Description

Hydroxy aluminum oxide nano material and preparation method thereof
Technical Field
The invention belongs to the field of preparation of IIIA group oxyhydroxide nano materials, and particularly relates to a simple, novel and efficient method for preparing an aluminum oxyhydroxide nanocone and a nanoflower.
Background
Aluminum is an element contained in the earth crust at the highest content, and aluminum oxyhydroxide is one of the existing forms of aluminum, and is mostly present in minerals in nature. The aluminum oxyhydroxide has unique structural characteristics, can show excellent performance in many aspects, has wide application, has huge application prospect in many aspects, and also arouses the enthusiasm of researchers for extensive research.
The surface of the aluminum oxyhydroxide (gamma-AlOOH) has rich hydroxyl groups, is one of hydrogen bond type two-dimensional materials, and the nano-sized aluminum oxyhydroxide has the characteristics of large specific surface area and the like, and is widely applied to the aspects of treating industrial wastewater, protecting the environment and the like as an adsorbent. In biomedicine, aluminum salt has been used as vaccine adjuvant for decades, and aluminum oxyhydroxide adjuvant is one of the more used vaccine adjuvants due to its high adsorption capacity and good adsorption to certain antigens. The hydroxy aluminum oxide also has the characteristics of easy regulation and control of shape and size, better biocompatibility, wide surface binding capacity and the like, and has wide application prospect in the aspects of drug delivery and the like; some particularly morphologically specific aluminum oxyhydroxides are even promising as delivery systems for chemotherapeutic drugs.
Meanwhile, the hydroxy aluminum oxide is easy to decompose by heat, can absorb heat and generate water, and can be used as a flame retardant. The hydroxy alumina has good application prospect in the aspects of catalysts, microelectronic functional materials and the like.
The controllable morphology is an important reason that the nano-scale aluminum oxyhydroxide can have wide application. At present, the method for synthesizing the aluminum oxyhydroxide with different shapes by using a plurality of methods is a hydrothermal synthesis method. For example: fu et al synthesized a nanorod of gamma-AlOOH with a diameter of about 8nm and a length of over 300nm by a hydrothermal method, and the nanorod had good light absorption capacity. Zhu et al prepared flower-like gamma-AlOOH nanocrystals with good crystallinity by hydrothermal method, and were suitable for use as catalytic carriers. In addition to hydrothermal synthesis, sol-gel method and solvothermal method are also relatively common preparation methods. For example, Song et al prepared sea urchin-like alumina oxide microspheres by a solvent thermal synthesis method, and the sea urchin-like alumina oxide microspheres have the characteristics of porosity, large specific surface area and the like.
Researchers have invested much research enthusiasm in the research of different shapes of aluminum oxyhydroxide, and a large amount of aluminum oxyhydroxide products with different shapes are also harvested, but the research on the aluminum oxyhydroxide with the shape of a nanocone is less at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a novel method for preparing aluminum oxyhydroxide (gamma-AlOOH) nanocones and nanoflowers formed by self-assembling the nanocones, wherein the method is simple, easy to control, good in repeatability, high in sample purity and good in crystallinity.
The specific technical scheme is as follows:
an aluminum oxyhydroxide nano material is composed of aluminum oxyhydroxide nano cones and nano flowers formed by self-assembling the nano cones, is gamma-AlOOH formed by aluminum, oxygen and hydroxyl according to the proportion of 1:1:1 in stoichiometric number, belongs to an orthorhombic system, and has a diaspore structure.
The nano-cone has the length of 1-2 mu m, the diameter of the bottom of 100-200 nm, the diameter of the tip of 10-20 nm, a flat side surface and a smooth surface.
The nanometer flower is formed by self-assembling nanometer cones, the bottoms of the nanometer cones are mutually connected, the tips of the nanometer cones are separated to form petals, and the diameter of the nanometer flower is 3-6 microns.
A preparation method of a hydroxy aluminum oxide nano material takes anhydrous aluminum chloride, anhydrous ethanol and oleic acid as raw materials, and firstly, the anhydrous aluminum chloride and the anhydrous ethanol are uniformly mixed according to the proportion of 20mL of anhydrous ethanol corresponding to each gram of the anhydrous aluminum chloride; then adding oleic acid into the mixed solution of anhydrous aluminum chloride and anhydrous ethanol according to the volume ratio of the oleic acid to the anhydrous ethanol of 1:4, and uniformly mixing; then pouring the mixed solution into a reaction kettle, and sealing and preserving heat for 24-48 h at the temperature of 180-200 ℃; and after the reaction is finished, naturally cooling the product to room temperature, and cleaning, drying and grinding the product to obtain white hydroxy alumina powder.
In order to prepare the hydroxyl alumina nanocones with uniform size and complete crystal form and the nanoflowers self-assembled by the nanocones, the reaction temperature in a reaction kettle is preferably 200 ℃; the reaction time is preferably 48 hours.
The anhydrous aluminum chloride and the anhydrous ethanol are uniformly mixed, specifically, the mixture is stirred on a magnetic stirrer for 30 minutes, and a preservative film is used for sealing in the stirring process, so that the volatilization of the ethanol is reduced; the oleic acid is added into the mixed solution of the anhydrous aluminum chloride and the anhydrous ethanol and is uniformly mixed, and the mixture is stirred for 30 minutes on a magnetic stirrer.
And preferably, cyclohexane and absolute ethyl alcohol are used for centrifugal cleaning for 3-5 times.
The drying is preferably carried out at 60 ℃ for 3 hours.
Has the advantages that:
the method synthesizes the aluminum hydroxide oxide (gamma-AlOOH) nanocones and the nanoflower structure formed by self-assembly of the nanocones for the first time; the length of the nanocone is about 1-2 mu m, the diameter of the bottom is 100-200 nm, the diameter of the tip is 10-20 nm, the side surface is straight, and the surface is smooth; the nanometer flower is formed by self-assembling nanometer cones, the bottoms of the nanometer cones are mutually connected, the tips of the nanometer cones are separated to form petals, and the size of the nanometer flower is about several micrometers. The invention uses the solvent thermal synthesis method, has simple operation, good repeatability and low cost; the prepared gamma-AlOOH nano cone and nano flower has high yield and high purity, and lays a foundation for further research on application of oxyhydroxide.
Drawings
FIG. 1 is an SEM image of the gamma-AlOOH nanocone prepared in example 1.
Fig. 2 is a SEM image of the gamma-AlOOH nanoflower prepared in example 1.
FIG. 3 is a TEM image of the γ -AlOOH nanopyramids prepared in example 1.
FIG. 4 is XRD spectrum of γ -AlOOH nanocones and nanoflowers prepared in example 1.
FIG. 5 is an SEM image of the gamma-AlOOH nanocone prepared in example 2.
FIG. 6 is an XRD spectrum of the γ -AlOOH nanocones and nanoflowers prepared in example 2.
FIG. 7 is an XRD spectrum of the γ -AlOOH nanocones and nanoflowers prepared in example 3.
FIG. 8 is an SEM image of the gamma-AlOOH nanotubes prepared in example 4.
FIG. 9 is a TEM image of the γ -AlOOH nanotubes prepared in example 4.
Detailed Description
Example 1
Taking anhydrous aluminum chloride, anhydrous ethanol and oleic acid as raw materials, firstly adding 0.6g of anhydrous aluminum chloride into a beaker containing 12mL of anhydrous ethanol, sealing the beaker by using a preservative film, and stirring the beaker in a magnetic stirrer for 30 minutes to obtain a mixed solution; then adding 3mL of oleic acid into a beaker containing a mixed solution of anhydrous aluminum chloride and anhydrous ethanol, and stirring for 30 minutes by using a magnetic stirrer; pouring the mixed solution into a reaction kettle after stirring is finished, and sealing and preserving heat for 48 hours at 200 ℃; and naturally cooling to room temperature, washing the product with cyclohexane and absolute ethyl alcohol for three times, drying and grinding to obtain a white powdery aluminum oxyhydroxide sample, wherein the sample comprises aluminum oxyhydroxide gamma-AlOOH nanocones and nanoflowers formed by self-assembling the nanocones.
This embodiment is the most preferred embodiment.
FIG. 1 shows an SEM image of a gamma-AlOOH nanocone prepared under the above conditions, and it can be seen that the nanocone has a sharp tip; it can also be seen that the gamma-AlOOH nanocone has a length of about 1 μm, a bottom of about 164nm, and a tip portion of about 16nm in diameter. FIG. 2 shows SEM images of the gamma-AlOOH nanoflowers prepared under the above conditions, and it can be seen that the nanoflowers are assembled by connecting the bottoms of the nanocones, and the diameters of the nanoflowers are 3-6 microns; FIG. 3 shows a TEM image of a γ -AlOOH nanocone prepared under the above conditions, and the upper right corner is an electron diffraction pattern of the nanocone. Fig. 4 shows XRD patterns of the gamma-AlOOH nanopyramids and nanoflowers prepared under the above conditions. The synthesized aluminum oxyhydroxide sample is proved to have good crystallinity and high product purity.
Example 2
Taking anhydrous aluminum chloride, anhydrous ethanol and oleic acid as raw materials, firstly adding 0.6g of anhydrous aluminum chloride into a beaker containing 12mL of anhydrous ethanol, sealing the beaker by using a preservative film, and stirring the beaker in a magnetic stirrer for 30 minutes to obtain a mixed solution; then adding 3mL of oleic acid into a beaker containing a mixed solution of anhydrous aluminum chloride and anhydrous ethanol, and stirring for 30 minutes by using a magnetic stirrer; pouring the mixed solution into a reaction kettle after stirring is finished, and sealing and preserving heat for 24 hours at 200 ℃; and naturally cooling to room temperature, washing the product with cyclohexane and absolute ethyl alcohol for three times, drying and grinding to obtain a white powdery aluminum hydroxide sample.
Fig. 5 shows a scanning electron microscope of the prepared gamma-AlOOH nanocone crystal, which can show that the size of the gamma-AlOOH nanocone is large and the side wall is not smooth enough. FIG. 6 shows XRD patterns of prepared γ -AlOOH nanocones and nanoflower crystals, with a peak between (002) and (102), which is a peak of AlOOH colloid by comparison, indicating slightly poorer crystallinity than example 1.
Example 3
Taking anhydrous aluminum chloride, anhydrous ethanol and oleic acid as raw materials, firstly adding 0.6g of anhydrous aluminum chloride into a beaker containing 12mL of anhydrous ethanol, sealing the beaker by using a preservative film, and stirring the beaker in a magnetic stirrer for 30 minutes to obtain a mixed solution; then adding 3mL of oleic acid into a beaker containing a mixed solution of anhydrous aluminum chloride and anhydrous ethanol, and stirring for 30 minutes by using a magnetic stirrer; pouring the mixed solution into a reaction kettle after stirring is finished, and sealing and preserving heat for 48 hours at 180 ℃; and naturally cooling to room temperature, washing the product with cyclohexane and absolute ethyl alcohol for three times, drying and grinding to obtain a white powdery aluminum hydroxide sample.
Fig. 7 shows XRD patterns of prepared γ -AlOOH nanocones and nanoflower crystals with a small bulge between (002) and (102), which are peaks of AlOOH colloid by comparison, indicating slightly poor crystallinity.
Example 4
Taking anhydrous aluminum chloride and anhydrous ethanol as raw materials, adding 0.6g of anhydrous aluminum chloride into a beaker containing 15mL of anhydrous ethanol, sealing the beaker by using a preservative film, and stirring the beaker in a magnetic stirrer for 30 minutes to obtain a mixed solution; pouring the mixed solution into a reaction kettle, sealing and preserving heat for 48 hours at 200 ℃; and cooling to room temperature, drying and grinding to obtain a white powdery aluminum hydroxide sample.
FIG. 8 shows an SEM image of γ -AlOOH nanotubes prepared under the present conditions; FIG. 9 shows a TEM image of the γ -AlOOH nanotubes prepared under the present conditions, and it can be seen that the γ -AlOOH nanotubes prepared under the condition without adding oleic acid have a morphology of nanotubes.

Claims (7)

1. An aluminum oxyhydroxide nano material is composed of aluminum oxyhydroxide nano cones and nano flowers formed by self-assembling the nano cones, is gamma-AlOOH formed by aluminum, oxygen and hydroxyl according to the proportion of 1:1:1 in stoichiometric number, belongs to an orthorhombic system, and has a diaspore structure.
2. The aluminum oxyhydroxide nanomaterial according to claim 1, wherein the nanocone has a length of 1-2 μm, a bottom diameter of 100-200 nm, a tip diameter of 10-20 nm, a flat side surface and a smooth surface.
3. The aluminum oxyhydroxide nanomaterial according to claim 1, wherein the nanoflower is formed by self-assembly of nanocones, the bottoms of the nanocones are connected with each other, the tips of the nanocones are separated to form petals, and the diameter of the nanoflower is 3-6 microns.
4. A preparation method of the aluminum hydroxide nano material as claimed in claim 1, which takes anhydrous aluminum chloride, anhydrous ethanol and oleic acid as raw materials, and firstly, the anhydrous aluminum chloride and the anhydrous ethanol are uniformly mixed according to the proportion of 20mL of the anhydrous ethanol corresponding to each gram of the anhydrous aluminum chloride; then adding oleic acid into the mixed solution of anhydrous aluminum chloride and anhydrous ethanol according to the volume ratio of the oleic acid to the anhydrous ethanol of 1:4, and uniformly mixing; then pouring the mixed solution into a reaction kettle, and sealing and preserving heat for 24-48 h at the temperature of 180-200 ℃; and after the reaction is finished, naturally cooling to room temperature, and cleaning, drying and grinding the product to obtain white hydroxy alumina powder.
5. The method for preparing the aluminum oxyhydroxide nanomaterial according to claim 4, wherein the reaction temperature in the reaction kettle is 200 ℃; the reaction time was 48 hours.
6. The method for preparing the aluminum oxyhydroxide nanomaterial according to claim 4, wherein the step of uniformly mixing the anhydrous aluminum chloride and the anhydrous ethanol is carried out by stirring on a magnetic stirrer for 30 minutes, and a preservative film is used for sealing during the stirring process to reduce the volatilization of the ethanol; the oleic acid is added into the mixed solution of the anhydrous aluminum chloride and the anhydrous ethanol and is uniformly mixed, and the mixture is stirred on a magnetic stirrer for 30 minutes.
7. The preparation method of the aluminum oxyhydroxide nanomaterial according to claim 4, wherein the washing is performed by centrifuging and washing with cyclohexane and absolute ethyl alcohol for 3-5 times; the drying is carried out for 3 hours at 60 ℃.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5100641A (en) * 1988-02-11 1992-03-31 Vereinigte Aluminium-Werke Aktiengesellschaft Method for the production of fillers and flame retardants based on gibbsite and application in plastics
CN101792164A (en) * 2009-11-19 2010-08-04 国家纳米科学中心 Method for preparing nano aluminum oxide through vacuum freeze drying technology
CN101890371A (en) * 2009-05-19 2010-11-24 中国石油化工股份有限公司 Titanium dioxide-aluminum oxide composite carrier and preparation method thereof
CN103449470A (en) * 2012-06-01 2013-12-18 中国石油天然气股份有限公司 High-stability small-crystal-grain NaY molecular sieve
CN106745120A (en) * 2016-12-16 2017-05-31 东北大学 It is a kind of prepare three-dimensional flower-shaped boehmite without the hot method of template mixed solvent
CN110395756A (en) * 2019-06-20 2019-11-01 广西玉林市思达粉体技术有限公司 A method of preparing macropore appearance, multi-pore channel, wide distribution boehmite

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5100641A (en) * 1988-02-11 1992-03-31 Vereinigte Aluminium-Werke Aktiengesellschaft Method for the production of fillers and flame retardants based on gibbsite and application in plastics
CN101890371A (en) * 2009-05-19 2010-11-24 中国石油化工股份有限公司 Titanium dioxide-aluminum oxide composite carrier and preparation method thereof
CN101792164A (en) * 2009-11-19 2010-08-04 国家纳米科学中心 Method for preparing nano aluminum oxide through vacuum freeze drying technology
CN103449470A (en) * 2012-06-01 2013-12-18 中国石油天然气股份有限公司 High-stability small-crystal-grain NaY molecular sieve
CN106745120A (en) * 2016-12-16 2017-05-31 东北大学 It is a kind of prepare three-dimensional flower-shaped boehmite without the hot method of template mixed solvent
CN110395756A (en) * 2019-06-20 2019-11-01 广西玉林市思达粉体技术有限公司 A method of preparing macropore appearance, multi-pore channel, wide distribution boehmite

Non-Patent Citations (1)

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Title
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