CN109503888A - A kind of preparation method of boehmite/graphene composite material - Google Patents
A kind of preparation method of boehmite/graphene composite material Download PDFInfo
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- CN109503888A CN109503888A CN201811438823.7A CN201811438823A CN109503888A CN 109503888 A CN109503888 A CN 109503888A CN 201811438823 A CN201811438823 A CN 201811438823A CN 109503888 A CN109503888 A CN 109503888A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Abstract
A kind of preparation method of boehmite/graphene composite material, belongs to field of nanometer technology.Preparation method: 1, by boehmite/graphene composite material quality proportioning, graphene oxide dispersion, aluminum salt solution and aqueous slkali are configured；2, graphene oxide dispersion, aluminum salt solution and aqueous slkali are added sequentially in microwave reactor, reaction obtains composite material crude product；3, composite material crude product is filtered, washed, dried, obtain boehmite/graphene composite material.Boehmite in boehmite/graphene composite material of the present invention is flake, and one-dimensional size 10nm~3 μm are evenly distributed on the surface of graphene and are closely adhered on the surface of graphene.Compared with the prior art, preparation method of the present invention quickly, simply, efficiently, is suitable for large-scale industrial production.Composite material of the present invention is with a wide range of applications in fields such as fire-retardant, water process.
Description
Technical field
The invention belongs to field of nanocomposite materials, and in particular to a kind of preparation side of boehmite/graphene composite material
Method.
Background technique
Halogen containing flame-retardant is current plastics, the most flame retardant products of rubber flame-retarded middle application, is primarily due to organic resistance
The chemical property for firing agent is inert, low with the compatibility of plastics or rubber product is relatively good, good flame retardation effect, use cost.But
It is that, when fire occurs, halogen fire proofing can generate a large amount of smog and toxic corrosive hydrogen halides gas, cause secondary
Harm.Therefore, halogen-free flame retardants has obtained extensive concern in recent years.Currently, common halogen-free flame retardants mainly has hydroxide
Aluminium, boehmite, magnesium hydroxide, phosphorus flame retardant, expansion type flame retardant etc..But for aluminium hydroxide, magnesium hydroxide and Bo Mu
Competence exertion antiflaming effect when needing to add relatively large for stone often has an impact the performance of matrix, especially influences
The mechanical property of material；Poor heat resistance, the poor compatibility of volatility greatly, with matrix of phosphorus flame retardant, and in combustion process
In have molten drop phenomenon；Expansion type flame retardant then has the shortcomings that the carbon-coating compactness of generation is poor, thermal stability is poor.
A kind of novel carbon simple substance with hexagonal honeycomb structure that graphene is made of carbon atom, the conduction with superelevation
Property thermal conductivity, is similar to transparent transparent and excellent gas barrier property at the specific surface area of super large.However, it is single with
Graphene as fire retardant, economically consider that cost is excessively high, is not particularly suited for applying on a large scale.By the inorganic resistance of tradition
Combustion agent is a kind of novel fire retardant with fire-retardant dose of graphene-based composite material that graphene is combined.This kind of composite material
Flame retardant property is better than one-component under inorganic fire retardants and the synergistic effect of graphene.The present invention uses microwave-assisted synthesis system
Standby boehmite/graphene composite material, as new flame retardant.
Microwave-assisted synthesis is to generate billions of times using the rapid electromagnetic wave absorption of polar molecule in microwave field
Dipole oscillation and collision and reaction is heated, and the polar substances molecule in the microwave field is generated in vibration, collision
Also intermolecular warm-up movement is accelerated while thermal energy, improves the transmission speed of substance significantly.Therefore, microwave-assisted synthesis
Efficient mass transfer can be realized while realizing quick, efficient, uniform heat production, greatly improve microcosmic mixed heat transfer and pass
Matter efficiency highly shortened the uniformly mixedization characteristic time, uniform environment required for particulate nucleation be met, in certain journey
Product cut size can be improved on degree to be unevenly distributed and less reproducible situation.Polarity of the simultaneous reactions process because of different substances
It is different and show excellent selection polarity, reaction efficiency is significantly improved, the quality of reactor product is improved, and improves heat energy utilization
Rate.
Summary of the invention
The present invention provide it is a kind of prepare boehmite/graphene composite material preparation method, using microwave-assisted synthesis, with
Graphene oxide dispersion, aluminum salt solution and aqueous slkali are that raw material prepares boehmite/graphene composite material.
A kind of preparation method of boehmite/graphene composite material, comprising the following steps:
(1) boehmite/graphene composite material quality proportioning, graphene oxide: aluminium salt: alkali=1:(10~500 are pressed):
(10~500), configuration concentration are the graphene oxide dispersion of 0.01~5mg/ml, and concentration is that the aluminium salt of 0.5~50wt% is molten
The aqueous slkali that liquid and concentration are 0.5~50wt%；
(2) graphene oxide dispersion, aluminum salt solution and aqueous slkali are sequentially added in microwave reactor, reaction temperature is
20~200 DEG C, the time is 5s~for 24 hours, obtains boehmite/graphene composite material crude product；
(3) boehmite/graphene composite material crude product is filtered, washed, dried, it is multiple to obtain boehmite/graphene
Condensation material.
In the step (1), the solvent of the graphene oxide dispersion is water, methanol, ethyl alcohol, ethylene glycol, third
Triol, normal propyl alcohol, isopropanol, n-butanol, n-amyl alcohol, n-hexyl alcohol, acetone, n-hexane, hexamethylene, 1-Methyl-2-Pyrrolidone,
One of N-METHYLFORMAMIDE, ethyl acetate, butyl acetate are a variety of.
In the step (1), the aluminium salt be selected from aluminium chloride, aluminium acetate, aluminum sulfate, aluminum nitrate, aluminum aluminum sulfate and
One of hydrate of above-mentioned aluminium salt is a variety of, and the solvent is selected from water, methanol, ethyl alcohol, ethylene glycol, glycerine, positive third
Alcohol, isopropanol, n-butanol, n-amyl alcohol, n-hexyl alcohol, acetone, n-hexane, hexamethylene, 1-Methyl-2-Pyrrolidone, N- methyl first
One of amide, ethyl acetate, butyl acetate are a variety of.
In the step (1), the aqueous slkali in sodium hydroxide solution, potassium hydroxide solution, ammonium hydroxide one
Kind is a variety of；The solvent of the sodium hydroxide solution is water or organic solvent；The solvent of the potassium hydroxide solution is water
Or organic solvent；The organic solvent is selected from methanol, ethyl alcohol, ethylene glycol, glycerine, normal propyl alcohol, isopropanol, n-butanol, just
Amylalcohol, n-hexyl alcohol, acetone, n-hexane, hexamethylene, 1-Methyl-2-Pyrrolidone, N-METHYLFORMAMIDE, ethyl acetate, acetic acid fourth
One of ester is a variety of.
In the step (3), the drying mode be heat drying, vacuum drying or freeze-drying one of or
It is a variety of.
Beneficial effects of the present invention are as follows:
1, the present invention prepares boehmite/graphene composite material using microwave irradiation technology, can be in efficient microcosmic mixing
Under by raw material of graphene oxide dispersion, aluminum salt solution and aqueous slkali prepare boehmite/graphene composite material, it is prepared
Boehmite/graphene composite material in boehmite pattern be flake, it is one-dimensional having a size of 10nm~3 μm, boehmite is in stone
Black alkene surface is evenly distributed and is closely attached to the surface of graphene；
2, preparation method of the present invention is quickly, simple, efficient, repeatability is strong, and is suitable for large-scale industrial
Metaplasia produces；
3, heretofore described boehmite/graphene composite material can be used for fire-retardant and water treatment field.
Detailed description of the invention
Fig. 1 is the boehmite/graphene composite material TEM figure prepared in the embodiment of the present invention 1；
Fig. 2 is the boehmite/graphene composite material XRD diagram prepared in the embodiment of the present invention 1.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
Embodiment 1
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:200:24 is matched
100ml0.5mg/ml graphene oxide aqueous dispersions processed；Prepare the aluminum nitrate aqueous solution of 50g 20wt%；Prepare 50g
The sodium hydrate aqueous solution of 2.4wt%；
(2) that graphene oxide aqueous dispersions, aluminum nitrate aqueous solution and sodium hydrate aqueous solution are added sequentially to microwave is anti-
It answers in device, at 180 DEG C, reaction 10min obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is freeze-dried i.e.
Obtain boehmite/graphene composite material.
Boehmite/graphene composite material TEM the figure prepared in embodiment 1, as shown in Figure 1；Boehmite/graphene is multiple
The XRD diagram of condensation material, as shown in Figure 2.
Embodiment 2
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:250:30 is matched
100ml0.1mg/ml graphene oxide aqueous dispersions processed；Prepare the aluminum nitrate aqueous solution of 50g 5wt%；Prepare 50g 0.6wt%
Sodium hydrate aqueous solution；
(2) that graphene oxide aqueous dispersions, aluminum nitrate aqueous solution and sodium hydrate aqueous solution are added sequentially to microwave is anti-
It answers in device, at 180 DEG C, reaction 10min obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is dried in vacuo i.e.
Obtain boehmite/graphene composite material.
Embodiment 3
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:150:18 is matched
100ml1mg/ml graphene oxide aqueous dispersions processed；Prepare the aluminum sulfate aqueous solution of 50g 30wt%；Prepare 50g 3.6wt%
Sodium hydrate aqueous solution；
(2) graphene oxide aqueous dispersions, aluminum sulfate aqueous solution and sodium hydrate aqueous solution are added to microwave reactor
In, at 150 DEG C, reaction 30min obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is freeze-dried i.e.
Obtain boehmite/graphene composite material.
Embodiment 4
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:200:24 is matched
100ml0.5mg/ml graphene oxide alcohol dispersion liquid processed；Prepare the aluminum nitrate aqueous solution of 50g 20wt%；Prepare 50g
The sodium hydrate aqueous solution of 2.4wt%；
(2) graphene oxide alcohol dispersion liquid, aluminum nitrate aqueous solution and sodium hydrate aqueous solution are added sequentially to microwave
In reactor, at 120 DEG C, reaction 2h obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, heat drying i.e.
Obtain boehmite/graphene composite material.
Embodiment 5
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:500:100 is matched
100ml5mg/ml graphene oxide alcohol dispersion liquid processed；Prepare the aluminum nitrate aqueous solution of 50g 50wt%；Prepare 50g 10wt%
Potassium hydroxide aqueous solution；
(2) graphene oxide alcohol dispersion liquid, aluminum nitrate aqueous solution and potassium hydroxide aqueous solution are added sequentially to microwave
In reactor, at 200 DEG C, reaction 1min obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is dried in vacuo i.e.
Obtain boehmite/graphene composite material.
Embodiment 6
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:200:200 is matched
100ml0.5mg/ml graphene oxide aqueous dispersions processed；Prepare the aluminum nitrate aqueous solution of 50g 20wt%；Prepare 50g 20wt%
Sodium hydrate aqueous solution；
(2) that graphene oxide aqueous dispersions, aluminum nitrate aqueous solution and sodium hydrate aqueous solution are added sequentially to microwave is anti-
It answers in device, at 200 DEG C, reaction 10s obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is freeze-dried i.e.
Obtain boehmite/graphene composite material.
Embodiment 7
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:200:24 is matched
100ml0.5mg/ml graphene oxide alcohol dispersion liquid processed；Prepare the conjunction aluminum nitrate ethanol solution of 50g 20wt%；Prepare 50g
The sodium hydroxide ethanol solution of 2.4wt%；
(2) graphene oxide alcohol dispersion liquid, aluminum nitrate ethanol solution and sodium hydroxide ethanol solution are added sequentially to
In microwave reactor, at 180 DEG C, reaction 10h obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is freeze-dried i.e.
Obtain boehmite/graphene composite material.
Embodiment 8
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:100:25 is matched
100ml2mg/ml graphene oxide aqueous dispersions processed；Prepare the aluminum nitrate aqueous solution of 50g 40wt%；Prepare 50g 10wt%'s
Ammonia spirit；
(2) graphene oxide aqueous dispersions, aluminum nitrate aqueous solution and ammonia spirit are added sequentially in microwave reactor,
At 180 DEG C, reaction 10h obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is dried in vacuo i.e.
Obtain boehmite/graphene composite material.
Embodiment 9
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:200:50 is matched
100ml0.5mg/ml graphene oxide aqueous dispersions processed；Prepare the aluminum sulfate aqueous solution of 50g 20wt%；Prepare 50g 5wt%
Potassium hydroxide aqueous solution；
(2) that graphene oxide aqueous dispersions, aluminum sulfate aqueous solution and potassium hydroxide aqueous solution are added sequentially to microwave is anti-
It answers in device, at 150 DEG C, reaction 5h obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is freeze-dried i.e.
Obtain boehmite/graphene composite material.
Embodiment 10
A kind of boehmite/graphene composite material is prepared, steps are as follows:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=1:500:500 is matched
100ml5mg/ml graphene oxide aqueous dispersions processed；Prepare the aluminum nitrate aqueous solution of 50g 50wt%；Prepare 50g 50wt%'s
Sodium hydrate aqueous solution；
(2) that graphene oxide aqueous dispersions, aluminum nitrate aqueous solution and sodium hydrate aqueous solution are added sequentially to microwave is anti-
It answers in device, at 200 DEG C, reaction 2h obtains boehmite/graphene composite material crude product；
(3) boehmite obtained in step (2)/graphene composite material crude product is filtered, washed, is dried in vacuo i.e.
Obtain boehmite/graphene composite material.
Table 1: corresponding embodiment experimental result
Obviously, the above embodiment of the present invention is only intended to clearly illustrate examples made by the present invention, and is not to this
The restriction of the embodiment of invention for those of ordinary skill in the art on the basis of the above description can be with
It makes other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to the present invention
Technical solution changes and variations that derived from still in the scope of protection of the present invention.
Claims (5)
1. a kind of preparation method of boehmite/graphene composite material, which comprises the following steps:
(1) boehmite/graphene composite material quality proportioning is pressed, graphene oxide: aluminium salt: alkali=graphene oxide: aluminium salt:
Alkali=1:(10~500): (10~500), configuration concentration are the graphene oxide dispersion of 0.01~5mg/ml, concentration 0.5
The aluminum salt solution and concentration of~50wt% is the aqueous slkali of 0.5~50wt%；
(2) graphene oxide dispersion, aluminum salt solution and aqueous slkali are sequentially added in microwave reactor, reaction temperature be 20~
200 DEG C, the time is 5s~for 24 hours, obtains boehmite/graphene composite material crude product；
(3) boehmite/graphene composite material crude product is filtered, washed, dried, obtain boehmite/graphene composite wood
Material.
2. preparation method according to claim 1, which is characterized in that in the step (1), the graphene oxide
The solvent of dispersion liquid be water, methanol, ethyl alcohol, ethylene glycol, glycerine, normal propyl alcohol, isopropanol, n-butanol, n-amyl alcohol, n-hexyl alcohol,
One of acetone, n-hexane, hexamethylene, 1-Methyl-2-Pyrrolidone, N-METHYLFORMAMIDE, ethyl acetate, butyl acetate or
It is a variety of.
3. preparation method according to claim 1, which is characterized in that in the step (1), the aluminium salt is selected from chlorine
Change one of hydrate of aluminium, aluminium acetate, aluminum sulfate, aluminum nitrate, aluminum aluminum sulfate and above-mentioned aluminium salt or a variety of, described solvents
Selected from water, methanol, ethyl alcohol, ethylene glycol, glycerine, normal propyl alcohol, isopropanol, n-butanol, n-amyl alcohol, n-hexyl alcohol, acetone, just oneself
One of alkane, hexamethylene, 1-Methyl-2-Pyrrolidone, N-METHYLFORMAMIDE, ethyl acetate, butyl acetate are a variety of.
4. preparation method according to claim 1, which is characterized in that in the step (1), the aqueous slkali is selected from
One of sodium hydroxide solution, potassium hydroxide solution, ammonium hydroxide are a variety of；The solvent of the sodium hydroxide solution is water or has
Solvent；The solvent of the potassium hydroxide solution is water or organic solvent；The organic solvent is selected from methanol, ethyl alcohol, second
Glycol, glycerine, normal propyl alcohol, isopropanol, n-butanol, n-amyl alcohol, n-hexyl alcohol, acetone, n-hexane, hexamethylene, 1- methyl -2- pyrrole
One of pyrrolidone, N-METHYLFORMAMIDE, ethyl acetate, butyl acetate are a variety of.
5. preparation method according to claim 1, which is characterized in that in the step (3), the drying mode is
Heat drying, one of vacuum drying or freeze-drying or a variety of.
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| CN110862573B (en) * | 2019-11-29 | 2022-04-15 | 山东师范大学 | Iron oxide red composite flame-retardant material, preparation method and application thereof in pigment |
| CN111019123A (en) * | 2019-12-31 | 2020-04-17 | 郑州中科新兴产业技术研究院 | Method for flame-retardant modification of polyamide 56 by biomimetic modification of Lehm stone/graphene oxide nano composite material |
| CN111019123B (en) * | 2019-12-31 | 2022-05-13 | 郑州中科新兴产业技术研究院 | Method for flame-retardant modification of polyamide 56 by biomimetic modification of Lehm stone/graphene oxide nano composite material |
| CN112645373A (en) * | 2020-12-17 | 2021-04-13 | 安徽理工大学 | Gamma-AlOOH/RGO composite wave-absorbing material and preparation method thereof |
| CN112645373B (en) * | 2020-12-17 | 2023-05-02 | 安徽理工大学 | Gamma-AlOOH/RGO composite wave-absorbing material and preparation method thereof |
| CN117181188A (en) * | 2023-08-17 | 2023-12-08 | 天津大学 | Three-dimensional graphene oxide composite material and preparation method and application thereof |
| CN117181188B (en) * | 2023-08-17 | 2024-04-09 | 天津大学 | Three-dimensional graphene oxide composite material and preparation method and application thereof |
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