CN108557850A - A kind of preparation method of γ-AlOOH nanometer sheets - Google Patents
A kind of preparation method of γ-AlOOH nanometer sheets Download PDFInfo
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- CN108557850A CN108557850A CN201810364503.5A CN201810364503A CN108557850A CN 108557850 A CN108557850 A CN 108557850A CN 201810364503 A CN201810364503 A CN 201810364503A CN 108557850 A CN108557850 A CN 108557850A
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- alooh
- nanometer sheets
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- Life Sciences & Earth Sciences (AREA)
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- Manufacturing & Machinery (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation method of γ AlOOH nanometer sheets, the preparation method of the γ AlOOH nanometer sheets mainly includes the following steps that：(1) it weighs a certain amount of aluminium salt and surface modifier is dissolved in a certain amount of deionized water, be configured to the aluminum salt solution of a concentration of 0.5 ~ 3mol/L；(2) compound concentration is the aqueous slkali of 0.1 ~ 3mol/L；(3) at 50 ~ 80 DEG C, above-mentioned aluminum salt solution is poured into rapidly in above-mentioned aqueous slkali, and stirs 1 3h；Sediment is filtered, removing foreign ion is cleaned and is scattered in again in a certain amount of deionized water under ultrasound condition；(4) above-mentioned dispersion liquid is transferred in autoclave and carries out solvent thermal reaction, 1 ~ 10h is reacted at 200 ~ 350 DEG C, γ AlOOH nano-film sols are obtained, are then evaporated the colloidal sol at 100 ~ 150 DEG C, obtain white solid powder shape γ AlOOH nanometer sheets.Hexagon subject to the nanometer sheet, length are 30 ~ 175nm, and width is 20 ~ 75nm, and thickness is 10 ~ 30nm.It can be applied to the fields such as flame-resistant high-temperature-resistant filler, lithium battery diaphragm coating, ceramic material, catalyst carrier, semi-conducting material.
Description
Technical field
The present invention relates to a kind of preparation methods of-AlOOH nanometer sheets of γ under hydrothermal conditions, belong to inorganic nano material system
Standby technology field.
Background technology
Boehmite is also known as boehmite, and molecular formula is γ-AlOOH.It is a kind of important basic raw material, is widely used as
Fire retardant, lithium battery diaphragm coating, the fields such as catalyst carrier and alumina precursor.
Lot of domestic and international document and patent report the boehmite preparation method of different-shape, US 4797139
The spherical shape boehmite for having prepared zero dimension is handled by seeding so that it is suitable for abrasive applications；Wu Yongxiang etc.
" normal pressure prepares acicular boehmite (γ-AlOOH) ultramicron " (Shanghai Normal University's journal (natural science edition), 1998
The fourth phase) disclose a kind of method preparing one-dimensional needle-shaped γ-AlOOH under normal pressure and lower temperature, length-width ratio about 30
nm: 4 nm.Chinese patent CN1546380 proposes a kind of hydro-thermal reaction-microwave radiation dehydration and drying method synthesizing one-dimensional
The preparation method of AlOOH nanotubes.Chinese patent CN101503206A proposes a kind of preparation side of 1-dimention nano γ-AlOOH
Method, a diameter of 10 ~ 30 nm, length are 0.8 ~ 3 μm.Two-dimensional sheet γ-AlOOH are to prepare sheet γ-Al2O3Presoma,
Sheet γ-Al2O3As a kind of important basic powder body material, not only there is common γ-Al2O3High rigidity, high-melting-point, height are led
Outside the good characteristics such as hot, corrosion-resistant, also there is two-dimensional structure, larger external surface area, good adhesive force and surface-active
Etc. properties, be widely used in terms of ceramic toughening.But for the preparation method of two-dimensional sheet γ-AlOOH
Research and few, being effectively synthesized the controllable sheet γ-AlOOH of size still has certain challenge.Relative to other
Method, hydro-thermal method have many advantages, such as that grain development is complete, granularity is small and is evenly distributed, and particle agglomeration is light.Especially after hydro-thermal not
It needs high-temperature calcination to handle, can avoid the shortcomings of impurity introduces, crystal grain is grown up and hard aggregation caused by calcination process.
Invention content
The object of the present invention is to provide a kind of preparation methods of γ-AlOOH nanometer sheets.It is yet another object of the invention to provide
A kind of γ-AlOOH nano-film sol preparation methods simple for process, yield is high.
Under thermal and hydric environment appropriate, γ-AlOOH can crystallize to form two-dimensional structure the present invention, and yield is high, be a kind of
Synthesis two dimension γ-AlOOH nanometer sheets are relatively simple and go to effective method.
In order to achieve the above objectives, the present invention uses following technical scheme：
A kind of preparation method of γ-AlOOH nanometer sheets of the present invention, including following procedure and step：
(a) it weighs a certain amount of aluminium salt and surface modifier is dissolved in suitable deionized water, be configured to a concentration of 0.5 ~ 3
The aluminum salt solution of mol/L；The surface modifier is polyvinyl alcohol polyacrylic acid, polyacrylamide, polyethylene glycol or citric acid
Any one of.The dosage of the surface modifier is 0.1 ~ 3 wt % of theory γ-AlOOH yield.
(b) aqueous slkali of a certain amount of a concentration of 0.1 ~ 3 mol/L is prepared；The alkali is any in sodium hydroxide or ammonium hydroxide
Kind.
(c) at 50 ~ 80 DEG C by aluminum salt solution pours into (b) rapidly in (a) aqueous slkali, and 1-3 h are stirred, will precipitated
Object is filtered, cleans removing foreign ion and in the ultrasonic cleaner that supersonic frequency is 20 ~ 100 kHz, power is 150 W
Upper ultrasound is scattered in again in a certain amount of deionized water, obtains the aqueous dispersions of presoma；The molar ratio of the aluminium salt and alkali
Example is 1: 3~10.
(d) dispersion liquid in above-mentioned (c) is transferred in autoclave and carries out solvent thermal reaction, at 200 ~ 350 DEG C
1 ~ 10 h is reacted, γ-AlOOH nano-film sols is obtained, colloidal sol is evaporated at 100 ~ 150 DEG C then, obtains white solid powder
Last shape γ-AlOOH nanometer sheets.
Aluminium salt in the step (a) is any one of aluminum nitrate, aluminum sulfate or alchlor.
The characteristics of the method for the present invention and advantage are as described below：
(1) γ-AlOOH nanometer sheet good dispersions obtained by, length be 30 ~ 175 nm, width be 20 ~ 75 nm, thickness be 10 ~
30 nm。
(2) γ-AlOOH nano-film sols storage obtained by is stablized, and it is more than half a year can to stablize storage at room temperature.
(3) the method for the present invention is simple for process, does not use organic formwork agent and organic solvent, environmental pollution is smaller, passes through
Reaction time and reaction temperature can regulate and control length, the width and thickness of nanometer sheet.
Description of the drawings
Fig. 1 is the XRD diagram of γ-AlOOH nanometer sheets prepared by the embodiment of the present invention 1；
Fig. 2 is the TEM figures of γ-AlOOH nanometer sheets prepared by the embodiment of the present invention 1；
Fig. 3 is the aqueous dispersions pictorial diagram (a) and Tyndall phenomenon figure of γ-AlOOH nanometer sheets prepared by the embodiment of the present invention 1
(b).（Tyndall phenomenon illustrates that the γ-AlOOH disperseed inside solvent are Nano grade）.
Specific implementation mode
The present invention will be described in more detail by following specific embodiment, but protection scope of the present invention not by
It is limited to these embodiments.
1 the present embodiment of embodiment includes the following steps：
(a) 200 mL of aluminum nitrate solution of 3 mol/L is measured；(b) 600 mL of sodium hydroxide solution of 3 mol/L is measured；(c)
In the sodium hydroxide solution that the aluminum nitrate solution of (a) is poured into (b) by 80 DEG C rapidly, and 1 h is stirred, sediment was carried out
Filter, cleaning remove foreign ion and the ultrasound weight on the ultrasonic cleaner that supersonic frequency is 20 ~ 100 kHz, power is 150 W
Newly it is scattered in the deionized water of 200 mL；(d) above-mentioned dispersion liquid is transferred in autoclave and carries out solvent thermal reaction,
2 h are reacted at 350 DEG C, obtain γ-AlOOH nano-film sols, and colloidal sol is evaporated at 120 DEG C then, obtains white solid
Powdered γ-AlOOH nanometer sheets, length are 50 ~ 175 nm, and width is 25 ~ 75 nm, and thickness is 25 ~ 30 nm.From XRD (Fig. 1)
It is found that having obtained γ-AlOOH pure phases.From TEM (Fig. 2), hexagon sheet subject to γ-AlOOH is obtained, is reunited now without apparent
As.
2 the present embodiment of embodiment includes the following steps：
(a) 200 mL of aluminum sulfate solution of 2 mol/L is measured；(b) 1200 mL of sodium hydroxide solution of 2 mol/L is measured；(c)
In the sodium hydroxide solution that the aluminum sulfate solution of (a) is poured into (b) by 80 DEG C rapidly, and 1 h is stirred, sediment was carried out
Filter, cleaning remove foreign ion and the ultrasound weight on the ultrasonic cleaner that supersonic frequency is 20 ~ 100 kHz, power is 150 W
Newly it is scattered in the deionized water of 200 mL；(d) above-mentioned dispersion liquid is transferred in autoclave and carries out solvent thermal reaction,
2 h are reacted at 300 DEG C, obtain γ-AlOOH nano-film sols, and colloidal sol is evaporated at 120 DEG C then, obtains white solid
Powdered γ-AlOOH nanometer sheets, length are 35 ~ 120 nm, and width is 20 ~ 50 nm, and thickness is 10 ~ 30 nm.
3 the present embodiment of embodiment includes the following steps：
(a) 200 mL of aluminum trichloride solution of 1 mol/L is measured；(b) 600 mL of ammonia spirit of 1 mol/L is measured；(c) exist
80 DEG C of aluminum trichloride solutions by (a) pour into the ammonia spirit of (b) rapidly, and stir 1 h, sediment are filtered, clearly
It removes decontamination ion and ultrasound is divided again on the ultrasonic cleaner that supersonic frequency is 20 ~ 100 kHz, power is 150 W
It dissipates in the deionized water of 200 mL；(d) above-mentioned dispersion liquid is transferred in autoclave and carries out solvent thermal reaction, 250
2 h are reacted at DEG C, obtain γ-AlOOH nano-film sols, and colloidal sol is evaporated at 120 DEG C then, obtains white solid powder
Shape γ-AlOOH nanometer sheets, length are 30 ~ 100 nm, and width is 20 ~ 40 nm, and thickness is 10 ~ 25 nm.
Claims (2)
1. a kind of preparation method of γ-AlOOH nanometer sheets, it is characterised in that this method includes mainly following procedure and step：
(a) it weighs a certain amount of aluminium salt and surface modifier is dissolved in suitable deionized water, be configured to a concentration of 0.5 ~ 3
The aluminum salt solution of mol/L；The surface modifier is polyvinyl alcohol polyacrylic acid, polyacrylamide, polyethylene glycol or citric acid
Any one of；The dosage of the surface modifier is 0.1 ~ 3 wt % of theory γ-AlOOH yield；
(b) aqueous slkali of a certain amount of a concentration of 0.1 ~ 3 mol/L is prepared；The alkali is any one of sodium hydroxide or ammonium hydroxide；
(c) at 50 ~ 80 DEG C by aluminum salt solution pours into (b) rapidly in (a) aqueous slkali, and 1-3 h are stirred, by sediment into
Row filtering, cleaning remove foreign ion and surpass on the ultrasonic cleaner that supersonic frequency is 20 ~ 100 kHz, power is 150 W
It is low voice speaking to be newly scattered in a certain amount of deionized water, obtain the aqueous dispersions of presoma；The molar ratio of the aluminium salt and alkali is
1: 3~10；
(d) dispersion liquid in above-mentioned (c) is transferred in autoclave and carries out solvent thermal reaction, reacted at 200 ~ 350 DEG C
1 ~ 10 h obtains γ-AlOOH nano-film sols, is then evaporated colloidal sol at 100 ~ 150 DEG C, obtains white solid powder shape
γ-AlOOH nanometer sheets.
2. a kind of preparation method of γ-AlOOH nanometer sheets according to claim 1, it is characterised in that：The step (a)
In aluminium salt be any one of aluminum nitrate, aluminum sulfate or alchlor.
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| CN201810364503.5A CN108557850A (en) | 2018-04-23 | 2018-04-23 | A kind of preparation method of γ-AlOOH nanometer sheets |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574051A (en) * | 2019-01-15 | 2019-04-05 | 吉林大学 | A kind of preparation method of γ-AlOOH nanotube |
| CN109694096A (en) * | 2019-01-15 | 2019-04-30 | 吉林大学 | A kind of γ-AlOOH platy-monocrystal and preparation method thereof |
| CN110137422A (en) * | 2019-05-30 | 2019-08-16 | 湖南电将军新能源有限公司 | A kind of lithium ion battery composite separation membrane and preparation method thereof |
| CN110652957A (en) * | 2019-11-14 | 2020-01-07 | 广州大学 | Preparation method and application of pseudo-boehmite microspheres |
| CN110656250A (en) * | 2019-11-11 | 2020-01-07 | 东北师范大学 | Method for recovering aluminum and heavy metals in electroplating sludge |
| CN110683568A (en) * | 2019-10-11 | 2020-01-14 | 湖北工业大学 | Preparation method of high-activity copper-loaded aluminum oxide nanosheet root-resisting agent |
| CN111470523A (en) * | 2020-05-07 | 2020-07-31 | 郑州中科新兴产业技术研究院 | Template-free graded growth preparation method of water-dispersible boehmite nanosheet |
| CN112809864A (en) * | 2021-01-12 | 2021-05-18 | 广州大学 | Flame-retardant wood and preparation method and application thereof |
| CN113371747A (en) * | 2021-06-11 | 2021-09-10 | 中铝郑州有色金属研究院有限公司 | Preparation method of boehmite with sheet structure and application of boehmite |
| CN117165106A (en) * | 2023-08-18 | 2023-12-05 | 浙江浙能技术研究院有限公司 | Preparation method of wear-resistant flame-retardant self-cleaning anti-reflection coating for photovoltaic |
-
2018
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109694096B (en) * | 2019-01-15 | 2021-06-01 | 吉林大学 | Gamma-AlOOH flaky monocrystal and preparation method thereof |
| CN109694096A (en) * | 2019-01-15 | 2019-04-30 | 吉林大学 | A kind of γ-AlOOH platy-monocrystal and preparation method thereof |
| CN109574051A (en) * | 2019-01-15 | 2019-04-05 | 吉林大学 | A kind of preparation method of γ-AlOOH nanotube |
| CN109574051B (en) * | 2019-01-15 | 2021-01-19 | 吉林大学 | Preparation method of gamma-AlOOH nanotube |
| CN110137422A (en) * | 2019-05-30 | 2019-08-16 | 湖南电将军新能源有限公司 | A kind of lithium ion battery composite separation membrane and preparation method thereof |
| CN110683568A (en) * | 2019-10-11 | 2020-01-14 | 湖北工业大学 | Preparation method of high-activity copper-loaded aluminum oxide nanosheet root-resisting agent |
| CN110656250A (en) * | 2019-11-11 | 2020-01-07 | 东北师范大学 | Method for recovering aluminum and heavy metals in electroplating sludge |
| CN110656250B (en) * | 2019-11-11 | 2021-04-16 | 东北师范大学 | Method for recovering aluminum and heavy metals in electroplating sludge |
| CN110652957A (en) * | 2019-11-14 | 2020-01-07 | 广州大学 | Preparation method and application of pseudo-boehmite microspheres |
| CN110652957B (en) * | 2019-11-14 | 2022-02-18 | 广州大学 | Preparation method and application of pseudo-boehmite microspheres |
| CN111470523A (en) * | 2020-05-07 | 2020-07-31 | 郑州中科新兴产业技术研究院 | Template-free graded growth preparation method of water-dispersible boehmite nanosheet |
| CN112809864A (en) * | 2021-01-12 | 2021-05-18 | 广州大学 | Flame-retardant wood and preparation method and application thereof |
| CN113371747A (en) * | 2021-06-11 | 2021-09-10 | 中铝郑州有色金属研究院有限公司 | Preparation method of boehmite with sheet structure and application of boehmite |
| CN117165106A (en) * | 2023-08-18 | 2023-12-05 | 浙江浙能技术研究院有限公司 | Preparation method of wear-resistant flame-retardant self-cleaning anti-reflection coating for photovoltaic |
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