CN113213819A - High-oil-absorption boron nitride-based aerogel composite material and preparation method and application thereof - Google Patents
High-oil-absorption boron nitride-based aerogel composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of boron nitride-based aerogel composite materials, and discloses a high oil absorption boron nitride-based aerogel composite material, and a preparation method and application thereof. The method comprises the following steps: 1) performing ball milling treatment on hexagonal boron nitride and a modifier sodium cholate to obtain hydroxylated hexagonal boron nitride; 2) preparing cellulose derivatives into cellulose derivative sol by adopting water; dispersing hydroxylated hexagonal boron nitride in water to obtain a boron nitride dispersion liquid; 3) and uniformly mixing the cellulose derivative sol and the hydroxylated hexagonal boron nitride dispersion liquid, adding a cross-linking agent, standing, freeze-drying, and thermally drying to obtain the boron nitride-based aerogel composite material. The method disclosed by the invention is simple, low in energy consumption, low in carbon and environment-friendly, and the prepared aerogel composite material has high oil absorption capacity and recycling performance, and is green and nontoxic. The aerogel composite material is used in the field of oil absorption.
Description
Technical Field
The invention belongs to the technical field of boron nitride-based aerogel composite materials, and particularly relates to a high-oil-absorption boron nitride-based aerogel composite material, a preparation method thereof and application of the composite material in oil absorption and other pollutants.
Background
The oil absorption material can effectively absorb pollutant oil in water, and has an environment restoration effect. The oil absorption materials widely used in the oil absorption field at present are activated carbon, kaolin and some high polymers. Boron nitride is used as a substance with high biocompatibility, strong temperature resistance, corrosion resistance and strong chemical inertness, and the porous form of the boron nitride is an ideal oil absorption material.
However, the three-dimensional boron nitride aerogel is agglomerated due to the strong attraction of the boron nitride lamella, and the surface inertia causes the loss of the surface active functional groups of the boron nitride, which leads to the collapse of the skeleton of the boron nitride aerogel and influences the formation of the boron nitride. In order to improve the forming performance, a large number of researchers use a high-temperature reducing atmosphere sintering method to improve the forming performance of the boron nitride aerogel. Through sintering, the strength of the boron nitride is improved, and the use experience after molding is improved. However, the sintering in high-temperature reducing atmosphere can not control the structural difference between the surface and the interior, and consumes huge energy; the use of reducing atmospheres such as ammonia increases the safety risk of the preparation process. Researchers have noted this, using a form that is compounded with a polymer, to improve the plasticity, elasticity and recyclability of the material. However, most of these polymers are difficult to degrade and toxic, and use of toxic reagents is not favorable for the green concept. For example, patent application CN110938297A discloses "a polymer composite material containing boron nitride aerogel, a preparation method and applications thereof" and CN110938297A discloses "a preparation method of boron nitride/epoxy resin composite material, a product and applications thereof" use a large amount of toxic reagents such as isopropyl alcohol, etc., which are harmful to the safety of the preparation process. And the oil absorption performance of the existing boron nitride composite aerogel also needs to be improved.
The invention adopts a simple and convenient freezing casting method to synthesize the high oil absorption boron nitride-based aerogel composite material. The method disclosed by the invention is simple and efficient, low in energy consumption and low in risk coefficient, the cellulose derivative is environment-friendly, non-toxic and degradable, and the prepared boron nitride-based aerogel composite material has high oil absorption performance.
Disclosure of Invention
In view of the defects of the existing boron nitride composite aerogel material and the preparation method thereof, the invention aims to provide a boron nitride-based aerogel composite material with high oil absorption performance and a preparation method thereof.
Another object of the present invention is to provide the use of the above-described boron nitride-based aerogel composite. The boron nitride-based aerogel composite material is applied to the field of oil absorption.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high oil absorption boron nitride-based aerogel composite material comprises the following steps:
1) performing ball milling treatment on hexagonal boron nitride and a modifier sodium cholate to obtain hydroxylated hexagonal boron nitride;
2) preparing cellulose derivatives into cellulose derivative sol by adopting water; dispersing hydroxylated hexagonal boron nitride in water to obtain a boron nitride dispersion liquid;
3) and uniformly mixing the cellulose derivative sol and the hydroxylated hexagonal boron nitride dispersion liquid, adding a cross-linking agent, standing, freeze-drying, and thermally drying to obtain the boron nitride-based aerogel composite material.
The mass ratio of the hexagonal boron nitride to the modifier in the step 1) is 100: 1-10: 1.
The rotation speed of the ball milling in the step 1) is 200-500 rpm, preferably 300-500 rpm; the ball milling time is 5-30h, preferably 15-20 h.
The ball milling treatment in the step 1) is ball milling treatment in a solvent; the solvent is water; the mass ratio of the water to the boron nitride is 20: 1-100: 1, and the preferred mass ratio is 70: 1-30: 1.
After the ball milling treatment in the step 1), filtering, washing and drying; the filtering, washing and drying refer to filtering the ball-milled product for 3-5 times by using a filter membrane with the diameter of 450 mu m, and drying for 2-5 hours at the temperature of 70-80 ℃.
The cellulose derivative in the step 2) is sodium carboxymethyl cellulose or hydroxypropyl methyl cellulose; the concentration of the cellulose derivative sol is 1 to 3 wt%.
And 2) heating, stirring and dissolving the cellulose derivative in the step 2) when preparing the sol, wherein the temperature is 90-95 ℃.
And (3) preparing the hexagonal boron nitride dispersion liquid in the step (2) at the temperature of 25-40 ℃.
The mass ratio of the hydroxylated boron nitride in the dispersion liquid in the step 3) to the cellulose derivative in the sol is 10: 1-2: 1.
The uniformly mixing in the step 3) refers to homogenizing and stirring: stirring for 1-2 h at room temperature.
In the step 3), the cross-linking agent is epichlorohydrin. The mass concentration of the cross-linking agent in the system is 0.1-1%, preferably 0.3-0.9%. The system comprises cellulose derivative sol, hexagonal boron nitride dispersion liquid and a cross-linking agent; the energy consumption of the cross-linking agent is 0.1-1% of the total mass of the system; preferably 0.3 to 0.9%.
In the step (3), the freeze drying is divided into freezing and vacuum drying; the freezing temperature is-198 to-15 ℃, and the freezing time is 2 to 24 hours.
The vacuum drying conditions are as follows: and drying for 24-72 h under the air pressure of less than 20 Pa.
The thermal drying condition in the step 3) is drying for 1-2 hours at 70-80 ℃.
The standing time in the step 3) is 30-120 min.
The high oil absorption boron nitride-based aerogel composite material is prepared by the method.
The high oil absorption boron nitride based aerogel composite material is applied to the field of oil absorption and is used as an oil absorption material.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention prepares a high oil absorption boron nitride-based aerogel composite material, and the density of the material (namely hexagonal boron nitride/cellulose composite aerogel) is 24-154 mg/cm-3. And controllable pore size distribution (38-86 μm) is realized. Has high oil absorption capacity and cyclic use performance.
2. The invention adopts a freeze drying method, omits the sintering and blocking process of boron nitride, greatly reduces energy consumption compared with high-temperature sintering preparation, and is low-carbon and environment-friendly.
3. The main product of the invention is green, nontoxic, natural and harmless, and can be recycled after use.
Drawings
FIG. 1 is a surface water wetting angle image of a boron nitride aerogel composite prepared in example 1;
FIG. 2 is a surface water wetting angle image of the boron nitride aerogel composite prepared in comparative example 1;
FIG. 3 is an SEM image of the boron nitride aerogel composite prepared in example 1;
fig. 4 is an SEM image of the boron nitride aerogel composite prepared in comparative example 1;
FIG. 5 is a pore size distribution of the boron nitride aerogel composite prepared in example 1;
FIG. 6 is a graph comparing the absorption capacities of the boron nitride aerogel composite prepared in example 1(S2) and the boron nitride aerogel composite prepared in comparative example 1(S1) for peanut oil, engine oil, and dimethicone.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Adding hexagonal boron nitride and a modifier (the mass ratio is 20: 1) into 100mL of water, performing ball milling treatment, wherein the water-material ratio is 70: 1 (the mass ratio of water to hexagonal boron nitride is 70: 1), the ball milling rotation speed is 400rpm, the ball milling time is 15h, filtering and washing the mixture by a 450-micron water-based filter membrane for 3 times, and drying the mixture at 70 ℃ to obtain hydroxylated hexagonal boron nitride;
(2) stirring and uniformly mixing sodium carboxymethylcellulose in water to prepare 3 wt% sodium carboxymethylcellulose sol; dispersing the hydroxylated hexagonal boron nitride prepared in the step (1) in water to prepare a 3 wt% boron nitride dispersion liquid;
(3) and (3) homogenizing and stirring 3g of the cellulose derivative sol prepared in the step (2) and 12g of the hydroxylated hexagonal boron nitride dispersion liquid (1h, 200rpm), adding 90mg of a cross-linking agent, standing for 1h, freezing at-35 ℃ for 2h, vacuum drying at 20Pa for 48h, and thermally drying at 70 ℃ for 2h to obtain the boron nitride-based composite aerogel.
The average pore diameter of the boron nitride-based composite aerogel prepared in the embodiment is 38 μm, and the capacities of absorbing peanut oil, simethicone and engine oil reach about 26.2g/g, 29.3g/g and 27.9g/g respectively. The density of the boron nitride-based composite aerogel prepared by the embodiment is 42.2mg/cm-3。
Fig. 1 shows the pore size distribution of the boron nitride-based composite aerogel prepared in this example, measured by mercury intrusion method.
Example 2
(1) Adding hexagonal boron nitride and a modifier (the mass ratio is 50: 1) into 100mL of water, performing ball milling treatment, wherein the water-material ratio is 70: 1, the ball milling rotation speed is 400rpm, the ball milling time is 15h, filtering and washing the mixture by a 450-micron aqueous filter membrane for 3 times, and drying the mixture at 70 ℃ to obtain the hydroxylated hexagonal boron nitride.
(2) Uniformly stirring sodium carboxymethylcellulose in water to prepare 3 wt% sodium carboxymethylcellulose sol, and dispersing the hydroxylated hexagonal boron nitride prepared in the step (1) in water to prepare 3 wt% boron nitride dispersion liquid;
(3) and (3) homogenizing and stirring 5g of the cellulose derivative sol prepared in the step (2) and 10g of the prepared hydroxylated hexagonal boron nitride dispersion liquid for 1h, adding 90mg of a cross-linking agent, standing for 1h, freezing at-35 ℃ for 2h, vacuum drying at 20Pa for 48h, and thermally drying at 70 ℃ for 2h to obtain the boron nitride-based composite aerogel.
The composite aerogel prepared by the embodiment has capacities of absorbing peanut oil, dimethyl silicone oil and engine oil of about 25.3g/g, 27.1g/g and 25.9g/g respectively.
Example 3
(1) Adding hexagonal boron nitride and a modifier (the mass ratio is 20: 1) into 100mL of water, performing ball milling treatment, wherein the water-material ratio is 70: 1, the ball milling rotation speed is 400rpm, the ball milling time is 15h, filtering and washing the mixture by a 450-micron aqueous filter membrane for 3 times, and drying the mixture at 70 ℃ to obtain hydroxylated hexagonal boron nitride;
(2) stirring and uniformly mixing sodium carboxymethylcellulose in water to prepare 3 wt% sodium carboxymethylcellulose sol, and dispersing the hydroxylated hexagonal boron nitride prepared in the step (1) to prepare 3 wt% boron nitride dispersion;
(3) and (3) homogenizing and stirring 1.5g of the cellulose derivative sol prepared in the step (2) and 13.5g of the prepared hydroxylated hexagonal boron nitride dispersion liquid, adding 45mg of a cross-linking agent, standing for 1h, freezing at-35 ℃ for 2h, drying under 20Pa for 48h in vacuum, and drying at 70 ℃ for 2h to obtain the boron nitride-based composite aerogel.
The composite aerogel prepared by the embodiment has capacities of absorbing peanut oil, dimethyl silicon oil and engine oil of about 25.9g/g, 28.0g/g and 26.4g/g respectively.
Example 4
(1) Adding hexagonal boron nitride and a modifier (the mass ratio is 50: 1) into 100mL of water, performing ball milling treatment, wherein the water-material ratio is 70: 1, the ball milling rotation speed is 300rpm, the ball milling time is 15h, filtering and washing the mixture by a 450-micron aqueous filter membrane for 3 times, and drying the mixture at 70 ℃ to obtain hydroxylated hexagonal boron nitride;
(2) stirring and uniformly mixing sodium carboxymethylcellulose in water to prepare 3 wt% sodium carboxymethylcellulose sol, and dispersing the hydroxylated hexagonal boron nitride prepared in the step (1) to prepare 3 wt% boron nitride dispersion;
(3) and (3) homogenizing and stirring 3g of the cellulose derivative sol prepared in the step (2) and 12g of the hydroxylated hexagonal boron nitride dispersion liquid, adding 90mg of a cross-linking agent, standing for 1h, freezing for 2h at-35 ℃, vacuum-drying for 60h at 20Pa, and heat-drying for 2h at 70 ℃ to obtain the boron nitride-based composite aerogel. The aerogel prepared in the example has the capacity of absorbing the dimethicone, and the capacity of the aerogel reaches 31.5 g/g.
Comparative example 1
(1) Adding hexagonal boron nitride and a modifier (the mass ratio is 20: 1) into 100mL of water, performing ball milling treatment, wherein the water-material ratio is 70: 1, the ball milling rotation speed is 200rpm, the ball milling time is 10h, filtering and washing the mixture by a 450-micron aqueous filter membrane for 3 times, and drying the mixture at 70 ℃ to obtain the hydroxylated hexagonal boron nitride.
(2) Stirring and dissolving sodium carboxymethylcellulose to prepare 3 wt% sodium carboxymethylcellulose sol, and dispersing the hydroxylated hexagonal boron nitride prepared in the step (1) to prepare 3 wt% boron nitride dispersion.
(3) And (3) homogenizing and stirring 10g of the cellulose derivative sol prepared in the step (2) and 5g of the prepared hydroxylated hexagonal boron nitride dispersion liquid, adding 90mg of a cross-linking agent, standing for 1h, freezing for 2h at-35 ℃, vacuum drying for 48h at 20Pa, and heat drying for 2h at 70 ℃ to obtain the boron nitride-based composite aerogel.
The capacities of the composite aerogel prepared by the comparative example for absorbing peanut oil, dimethyl silicone oil and engine oil reach about 24.7g/g, 26.0g/g and 25.4g/g respectively.
Comparative example 2
(1) Adding hexagonal boron nitride and a modifier (in a mass ratio of 50: 1) into 100mL of water, and performing ball milling treatment, wherein the water-material ratio is 100: 1, ball milling at the rotation speed of 400rpm for 20h, filtering and washing the mixture for 3 times by a 450-micron water-based filter membrane, and drying the mixture at 70 ℃ to obtain hydroxylated hexagonal boron nitride;
(2) stirring and uniformly mixing sodium carboxymethylcellulose in water to obtain 3 wt% sodium carboxymethylcellulose sol; dispersing the hydroxylated hexagonal boron nitride prepared in the step (1) in water to prepare a 3 wt% boron nitride dispersion liquid;
(3) and (3) homogenizing and stirring 3g of the cellulose derivative sol prepared in the step (2) and 12g of the hydroxylated hexagonal boron nitride dispersion liquid, adding 90mg of a cross-linking agent, standing for 1h, freezing for 2h at-35 ℃, vacuum drying for 48h at 20Pa, and heat drying for 1h at 70 ℃ to obtain the boron nitride-based composite aerogel.
The aerogel prepared by the comparative example has low mechanical strength and is not suitable for oil absorption.
Structural characterization and performance testing:
fig. 2 is a surface water wetting angle diagram of the boron nitride aerogel composite prepared in example 1, and fig. 3 is a surface water wetting angle diagram of the boron nitride aerogel composite prepared in comparative example 1. It can be seen that the surface water wetting angles of the boron nitride aerogel composites prepared in example 1 and comparative example 1 were 120 ° and 63 °, respectively. The boron nitride aerogel composite material with the preparation parameters in the optimal range has stronger hydrophobic property, and can effectively resist the interference of water in the oil absorption application.
Fig. 4 is an SEM image of the boron nitride aerogel composite prepared in example 1, and fig. 5 is an SEM image of the boron nitride aerogel composite prepared in comparative example 1. It can be seen that the boron nitride aerogel composite material prepared by adding the cellulose derivative with high specific gravity causes the smoothness and densification of the microscopic interface, which is not beneficial to the surface hydrophobicity and oil absorption.
FIG. 6 is a comparison of peanut oil, dimethicone and engine oil absorption for boron nitride based aerogel composites prepared in example 1(S2) and comparative example 1 (S1). Therefore, the boron nitride aerogel composite material with the optimal preparation parameter range has higher oil absorption capacity and is suitable for the absorption of various oils.
Although the above-described embodiments have been disclosed as above, they are not limited to the above examples and are not to be construed as limiting the embodiments. It is easily modified by workers in the same field of research, and thus the present invention is not exhaustive. Any similar design considerations and obvious changes or modifications are within the scope of the invention as created by the present application.
Claims (10)
1. A preparation method of a high oil absorption boron nitride-based aerogel composite material is characterized by comprising the following steps: the method comprises the following steps:
1) performing ball milling treatment on hexagonal boron nitride and a modifier sodium cholate to obtain hydroxylated hexagonal boron nitride;
2) preparing cellulose derivatives into cellulose derivative sol by adopting water; dispersing hydroxylated hexagonal boron nitride in water to obtain a boron nitride dispersion liquid;
3) uniformly mixing the cellulose derivative sol and the hydroxylated hexagonal boron nitride dispersion liquid, adding a cross-linking agent, standing, freeze-drying, and thermally drying to obtain a boron nitride-based aerogel composite material;
the cross-linking agent in the step 3) is epichlorohydrin; the mass concentration of the cross-linking agent in the system is 0.1-1%, and the system comprises cellulose derivative sol, hexagonal boron nitride dispersion liquid and the cross-linking agent;
the ball milling treatment in the step 1) is ball milling treatment in a solvent; the solvent is water; the mass ratio of the water to the boron nitride is 20: 1-100: 1.
2. The method for preparing the high oil absorption boron nitride-based aerogel composite material according to claim 1, wherein the method comprises the following steps: in the step 3), the mass concentration of the cross-linking agent in the system is 0.3-0.9%;
the mass ratio of the water to the boron nitride in the step 1) is 70: 1-30: 1;
the mass ratio of the hydroxylated hexagonal boron nitride in the dispersion liquid in the step 3) to the cellulose derivative in the sol is 10: 1-2: 1.
3. The method for preparing the high oil absorption boron nitride-based aerogel composite material according to claim 1, wherein the method comprises the following steps: the mass ratio of the hexagonal boron nitride to the modifier in the step 1) is 100: 1-10: 1;
the rotating speed of the ball milling in the step 1) is 200-500 rpm; the ball milling time is 5-30 h;
the cellulose derivative in the step 2) is more than one of sodium carboxymethyl cellulose or hydroxypropyl methyl cellulose.
4. The method for preparing the high oil absorption boron nitride-based aerogel composite material according to claim 3, wherein the method comprises the following steps: the rotating speed of the ball milling in the step 1) is 300-500 rpm; the ball milling time is 15-20 h.
5. The method for preparing the high oil absorption boron nitride-based aerogel composite material according to claim 1, wherein the method comprises the following steps: in the step (3), the freeze drying is divided into freezing and vacuum drying; the freezing temperature is-198 to-15 ℃, and the freezing time is 2 to 24 hours;
the vacuum drying conditions are as follows: and drying for 24-72 h under the air pressure of less than 20 Pa.
6. The method for preparing the high oil absorption boron nitride-based aerogel composite material according to claim 1, wherein the method comprises the following steps: the thermal drying condition in the step 3) is drying for 1-2 h at 70-80 ℃;
the standing time in the step 3) is 30-120 min;
the concentration of the cellulose derivative sol in the step 2) is 1-3 wt%; the concentration of the boron nitride dispersion is 1-3 wt%.
7. The method for preparing the high oil absorption boron nitride-based aerogel composite material according to claim 1, wherein the method comprises the following steps: after the ball milling treatment in the step 1), filtering, washing and drying; the filtering, washing and drying refer to filtering the ball-milled product for 3-5 times by using a filter membrane with the diameter of 450 mu m, and drying for 2-5 hours at the temperature of 70-80 ℃.
8. A high oil absorption boron nitride-based aerogel composite material obtained by the preparation method of any one of claims 1 to 7.
9. The application of the high oil absorption boron nitride-based aerogel composite material in the oil absorption field according to claim 8.
10. Use according to claim 8, characterized in that: the oil comprises more than one of peanut oil, dimethyl silicone oil and engine oil.
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CN116254699A (en) * | 2023-02-28 | 2023-06-13 | 四川轻化工大学 | Anti-bacterial textile based on difunctional boron nitride and preparation method thereof |
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