CN109503888B - Preparation method of boehmite/graphene composite material - Google Patents
Preparation method of boehmite/graphene composite material Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/04—Carbon
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- 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
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Abstract
A preparation method of a boehmite/graphene composite material belongs to the field of nanotechnology. The preparation method comprises the following steps: 1. preparing a graphene oxide dispersion liquid, an aluminum salt solution and an alkali solution according to the mass ratio of the boehmite/graphene composite material; 2. sequentially adding the graphene oxide dispersion liquid, the aluminum salt solution and the alkali solution into a microwave reactor, and reacting to obtain a crude composite material; 3. and filtering, washing and drying the crude product of the composite material to obtain the boehmite/graphene composite material. Boehmite in the boehmite/graphene composite material is flaky, has a one-dimensional size of 10 nm-3 mu m, and is uniformly distributed on the surface of graphene and tightly attached to the surface of the graphene. Compared with the prior art, the preparation method is quick, simple and efficient, and is suitable for large-scale industrial production. The composite material has wide application prospect in the fields of flame retardance, water treatment and the like.
Description
Technical Field
The invention belongs to the field of nano composite materials, and particularly relates to a preparation method of a boehmite/graphene composite material.
Background
The halogen-containing flame retardant is a flame retardant product which is most applied to the flame retardance of plastics and rubber at present, and mainly has the advantages of inert chemical property, good compatibility with plastics or rubber products, good flame retardant effect and low use cost. However, in the event of a fire, the halogen-containing flame retardant material generates a large amount of smoke and toxic corrosive hydrogen halide gas, causing secondary damage. Therefore, halogen-free flame retardants have gained wide attention in recent years. At present, the common halogen-free flame retardant mainly comprises aluminum hydroxide, boehmite, magnesium hydroxide, phosphorus flame retardant, intumescent flame retardant and the like. However, aluminum hydroxide, magnesium hydroxide and boehmite need to be added in a relatively large amount to exert flame retardant effect, which often affects the properties of the matrix, especially the mechanical properties of the material; the phosphorus flame retardant has poor heat resistance, high volatility and poor compatibility with a matrix, and has a dripping phenomenon in the combustion process; the intumescent flame retardant has the defects of poor compactness of a generated carbon layer, poor thermal stability and the like.
The graphene is a novel carbon simple substance with a hexagonal honeycomb structure and composed of carbon atoms, and has ultrahigh electrical conductivity and thermal conductivity, an ultrahigh specific surface area, transparency similar to transparency and excellent gas barrier property. However, graphene alone is too expensive as a flame retardant from the economical point of view, and is not suitable for large-scale application. The graphene-based composite material flame retardant compounded by the traditional inorganic flame retardant and the graphene is a novel flame retardant. The flame retardant property of the composite material is superior to that of a single component under the synergistic effect of the inorganic flame retardant and the graphene. According to the invention, a microwave synthesis technology is adopted to prepare the boehmite/graphene composite material as a novel flame retardant.
The microwave synthesis technology is that polar molecules in a microwave field rapidly absorb electromagnetic waves to generate billions of dipole vibration and collision to heat the reaction, and polar substance molecules in the microwave field vibrate and collide to generate heat energy and accelerate the thermal motion among the molecules, so that the transmission speed of the substance is obviously improved. Therefore, the microwave synthesis technology can realize rapid, efficient and uniform heat generation and simultaneously realize efficient mass transfer, greatly improve the heat and mass transfer efficiency of micro mixing, greatly shorten the mixing homogenization characteristic time, meet the uniform environment required by particle nucleation, and improve the conditions of uneven particle size distribution and poorer repeatability of products to a certain extent. Meanwhile, the reaction process shows excellent selective polarity due to different polarities of different substances, so that the reaction efficiency is obviously improved, the quality of a reaction product is improved, and the heat energy utilization rate is improved.
Disclosure of Invention
The invention provides a preparation method for preparing a boehmite/graphene composite material, which adopts a microwave synthesis technology and takes graphene oxide dispersion liquid, aluminum salt solution and alkali solution as raw materials to prepare the boehmite/graphene composite material.
A preparation method of a boehmite/graphene composite material comprises the following steps:
(1) preparing graphene oxide, namely aluminum salt and alkali, wherein the alkali comprises (10-500) and (10-500) according to the mass ratio of the boehmite/graphene composite material, and preparing a graphene oxide dispersion liquid with the concentration of 0.01-5 mg/ml, an aluminum salt solution with the concentration of 0.5-50 wt% and an alkali solution with the concentration of 0.5-50 wt%;
(2) sequentially adding the graphene oxide dispersion liquid, the aluminum salt solution and the alkali solution into a microwave reactor, wherein the reaction temperature is 20-200 ℃, and the reaction time is 5 s-24 h, so as to obtain a boehmite/graphene composite crude product;
(3) and filtering, washing and drying the boehmite/graphene composite material crude product to obtain the boehmite/graphene composite material.
In the step (1), the solvent of the graphene oxide dispersion liquid is one or more of water, methanol, ethanol, ethylene glycol, glycerol, N-propanol, isopropanol, N-butanol, N-pentanol, N-hexanol, acetone, N-hexane, cyclohexane, 1-methyl-2-pyrrolidone, N-methylformamide, ethyl acetate and butyl acetate.
In the step (1), the aluminum salt is selected from one or more of aluminum chloride, aluminum acetate, aluminum sulfate, aluminum nitrate, aluminum potassium sulfate and hydrates of the aluminum salt, and the solvent is selected from one or more of water, methanol, ethanol, ethylene glycol, glycerol, N-propanol, isopropanol, N-butanol, N-pentanol, N-hexanol, acetone, N-hexane, cyclohexane, 1-methyl-2-pyrrolidone, N-methylformamide, ethyl acetate and butyl acetate.
In the step (1), the alkali solution is one or more selected from sodium hydroxide solution, potassium hydroxide solution and ammonia water; the solvent of the sodium hydroxide solution is water or an organic solvent; the solvent of the potassium hydroxide solution is water or an organic solvent; the organic solvent is selected from one or more of methanol, ethanol, ethylene glycol, glycerol, N-propanol, isopropanol, N-butanol, N-pentanol, N-hexanol, acetone, N-hexane, cyclohexane, 1-methyl-2-pyrrolidone, N-methylformamide, ethyl acetate and butyl acetate.
In the step (3), the drying mode is one or more of heating drying, vacuum drying or freeze drying.
The invention has the following beneficial effects:
1. according to the invention, a microwave radiation technology is adopted to prepare the boehmite/graphene composite material, the graphene oxide dispersion liquid, the aluminum salt solution and the alkali solution are used as raw materials to prepare the boehmite/graphene composite material under the condition of efficient micro-mixing, the morphology of boehmite in the prepared boehmite/graphene composite material is flaky, the one-dimensional size is 10 nm-3 mu m, and boehmite is uniformly distributed on the surface of graphene and is tightly attached to the surface of the graphene;
2. the preparation method is rapid, simple, efficient and high in repeatability, and is suitable for large-scale industrial production;
3. the boehmite/graphene composite material disclosed by the invention can be applied to the fields of flame retardance and water treatment.
Drawings
Fig. 1 is a TEM image of a boehmite/graphene composite prepared in example 1 of the present invention;
fig. 2 is an XRD pattern of the boehmite/graphene composite material prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 0.5mg/ml graphene oxide aqueous dispersion according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, aluminum salt and alkali, wherein the ratio is 1:200: 24; preparing 50g of 20 wt% aluminum nitrate aqueous solution; preparing 50g of 2.4 wt% sodium hydroxide aqueous solution;
(2) sequentially adding the graphene oxide aqueous dispersion, an aluminum nitrate aqueous solution and a sodium hydroxide aqueous solution into a microwave reactor, and reacting at 180 ℃ for 10min to obtain a boehmite/graphene composite crude product;
(3) and (3) filtering, washing and freeze-drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
TEM images of boehmite/graphene composites prepared in example 1, as shown in figure 1; the XRD pattern of the boehmite/graphene composite material is shown in fig. 2.
Example 2
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 0.1mg/ml graphene oxide aqueous dispersion according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, namely aluminum salt and alkali, namely 1:250: 30; preparing 50g of 5 wt% aluminum nitrate aqueous solution; preparing 50g of 0.6 wt% sodium hydroxide aqueous solution;
(2) sequentially adding the graphene oxide aqueous dispersion, an aluminum nitrate aqueous solution and a sodium hydroxide aqueous solution into a microwave reactor, and reacting at 180 ℃ for 10min to obtain a boehmite/graphene composite crude product;
(3) and (3) filtering, washing and vacuum drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Example 3
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 1mg/ml graphene oxide aqueous dispersion according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, namely aluminum salt and alkali, namely 1:150: 18; preparing 50g of 30 wt% aluminum sulfate aqueous solution; preparing 50g of 3.6 wt% sodium hydroxide aqueous solution;
(2) adding the graphene oxide aqueous dispersion, an aluminum sulfate aqueous solution and a sodium hydroxide aqueous solution into a microwave reactor, and reacting for 30min at 150 ℃ to obtain a boehmite/graphene composite crude product;
(3) and (3) filtering, washing and freeze-drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Example 4
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 0.5mg/ml graphene oxide ethanol dispersion liquid according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, aluminum salt and alkali, wherein the ratio is 1:200: 24; preparing 50g of 20 wt% aluminum nitrate aqueous solution; preparing 50g of 2.4 wt% sodium hydroxide aqueous solution;
(2) sequentially adding the graphene oxide ethanol dispersion liquid, an aluminum nitrate aqueous solution and a sodium hydroxide aqueous solution into a microwave reactor, and reacting for 2 hours at 120 ℃ to obtain a boehmite/graphene composite material crude product;
(3) and (3) filtering, washing, heating and drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Example 5
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 5mg/ml graphene oxide ethanol dispersion liquid according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, namely aluminum salt and alkali, namely 1:500: 100; preparing 50g of 50 wt% aluminum nitrate aqueous solution; preparing 50g of 10 wt% potassium hydroxide aqueous solution;
(2) sequentially adding the graphene oxide ethanol dispersion liquid, an aluminum nitrate aqueous solution and a potassium hydroxide aqueous solution into a microwave reactor, and reacting at 200 ℃ for 1min to obtain a boehmite/graphene composite material crude product;
(3) and (3) filtering, washing and vacuum drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Example 6
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 0.5mg/ml graphene oxide aqueous dispersion according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, aluminum salt and alkali, wherein the ratio is 1:200: 200; preparing 50g of 20 wt% aluminum nitrate aqueous solution; preparing 50g of 20 wt% sodium hydroxide aqueous solution;
(2) sequentially adding the graphene oxide aqueous dispersion, an aluminum nitrate aqueous solution and a sodium hydroxide aqueous solution into a microwave reactor, and reacting for 10s at 200 ℃ to obtain a boehmite/graphene composite crude product;
(3) and (3) filtering, washing and freeze-drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Example 7
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 0.5mg/ml graphene oxide ethanol dispersion liquid according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, aluminum salt and alkali, wherein the ratio is 1:200: 24; preparing 50g of 20 wt% aluminum nitrate mixed ethanol solution; preparing 50g of 2.4 wt% sodium hydroxide ethanol solution;
(2) sequentially adding the graphene oxide ethanol dispersion liquid, an aluminum nitrate ethanol solution and a sodium hydroxide ethanol solution into a microwave reactor, and reacting at 180 ℃ for 10 hours to obtain a boehmite/graphene composite crude product;
(3) and (3) filtering, washing and freeze-drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Example 8
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 2mg/ml graphene oxide aqueous dispersion according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, namely aluminum salt and alkali, namely 1:100: 25; preparing 50g of 40 wt% aluminum nitrate aqueous solution; preparing 50g of 10 wt% ammonia water solution;
(2) sequentially adding the graphene oxide aqueous dispersion, an aluminum nitrate aqueous solution and an ammonia water solution into a microwave reactor, and reacting for 10 hours at 180 ℃ to obtain a boehmite/graphene composite crude product;
(3) and (3) filtering, washing and vacuum drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Example 9
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 0.5mg/ml graphene oxide aqueous dispersion according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, aluminum salt and alkali, wherein the ratio is 1:200: 50; preparing 50g of 20 wt% aluminum sulfate aqueous solution; preparing 50g of 5 wt% potassium hydroxide aqueous solution;
(2) sequentially adding the graphene oxide aqueous dispersion, an aluminum sulfate aqueous solution and a potassium hydroxide aqueous solution into a microwave reactor, and reacting for 5 hours at 150 ℃ to obtain a boehmite/graphene composite material crude product;
(3) and (3) filtering, washing and freeze-drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Example 10
Preparing a boehmite/graphene composite material, comprising the following steps:
(1) preparing 100ml of 5mg/ml graphene oxide aqueous dispersion according to the mass ratio of the boehmite/graphene composite material to the graphene oxide, namely aluminum salt and alkali, namely 1:500: 500; preparing 50g of 50 wt% aluminum nitrate aqueous solution; preparing 50g of 50 wt% sodium hydroxide aqueous solution;
(2) sequentially adding the graphene oxide aqueous dispersion, an aluminum nitrate aqueous solution and a sodium hydroxide aqueous solution into a microwave reactor, and reacting for 2 hours at 200 ℃ to obtain a boehmite/graphene composite material crude product;
(3) and (3) filtering, washing and vacuum drying the boehmite/graphene composite crude product obtained in the step (2) to obtain the boehmite/graphene composite.
Table 1: experimental results of corresponding examples
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be made within the scope of the present invention.
Claims (5)
1. A preparation method of a boehmite/graphene composite material is characterized by comprising the following steps:
(1) preparing graphene oxide dispersion liquid with the concentration of 0.1-5 mg/ml, aluminum salt solution with the concentration of 5-50 wt% and alkali solution with the concentration of 0.6-50 wt% according to the mass ratio of boehmite/graphene composite material, wherein the graphene oxide is aluminum salt and alkali (1) (100-500) (18-500);
(2) sequentially adding the graphene oxide dispersion liquid, the aluminum salt solution and the alkali solution into a microwave reactor, wherein the reaction temperature is 120-200 ℃, and the reaction time is 10 s-10 h, so as to obtain a boehmite/graphene composite crude product;
(3) and filtering, washing and drying the boehmite/graphene composite crude product to obtain the boehmite/graphene composite, wherein boehmite in the boehmite/graphene composite is flaky in shape and 200-2500 nm in size.
2. The method according to claim 1, wherein in the step (1), the solvent of the graphene oxide dispersion is one or more selected from water, methanol, ethanol, ethylene glycol, glycerol, N-propanol, isopropanol, N-butanol, N-pentanol, N-hexanol, acetone, N-hexane, cyclohexane, 1-methyl-2-pyrrolidone, N-methylformamide, ethyl acetate and butyl acetate.
3. The method according to claim 1, wherein in the step (1), the aluminum salt is selected from one or more of aluminum chloride, aluminum acetate, aluminum sulfate, aluminum nitrate, aluminum potassium sulfate and hydrates of the aluminum salt, and the solvent is selected from one or more of water, methanol, ethanol, ethylene glycol, glycerol, N-propanol, isopropanol, N-butanol, N-pentanol, N-hexanol, acetone, N-hexane, cyclohexane, 1-methyl-2-pyrrolidone, N-methylformamide, ethyl acetate and butyl acetate.
4. The method according to claim 1, wherein in the step (1), the alkali solution is selected from one or more of sodium hydroxide solution, potassium hydroxide solution and ammonia water; the solvent of the sodium hydroxide solution is water or an organic solvent; the solvent of the potassium hydroxide solution is water or an organic solvent; the organic solvent is selected from one or more of methanol, ethanol, ethylene glycol, glycerol, N-propanol, isopropanol, N-butanol, N-pentanol, N-hexanol, acetone, N-hexane, cyclohexane, 1-methyl-2-pyrrolidone, N-methylformamide, ethyl acetate and butyl acetate.
5. The method according to claim 1, wherein in the step (3), the drying manner is one or more of heat drying, vacuum drying or freeze drying.
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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 |
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