CN108455576B - Super-hydrophobic octyl graphene foam and preparation method and application thereof - Google Patents
Super-hydrophobic octyl graphene foam and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the field of composite foam, and particularly relates to super-hydrophobic octyl graphene foam and a preparation method thereof. The preparation method comprises the following steps: taking foamed nickel as a substrate, and attaching octyl graphene on the surface of the foamed nickel to obtain the graphene-based composite material; the octyl graphene is obtained by reacting graphene oxide with octyl-triethoxysilane to obtain octyl graphene oxide and then carrying out reduction reaction on the octyl graphene oxide. According to the invention, octyl-triethoxysilane is grafted to the surface of graphene to prepare graphene with octyl groups on the surface, and the octyl groups enhance the interaction force between foamed nickel and graphene, improve the compatibility between nano graphene and a matrix, so that the prepared super-hydrophobic foam has more stable hydrophobic performance in the use process. It can be seen that the obtained superhydrophobic octyl graphene foam is a promising and commercially available high-performance material.
Description
Technical Field
The invention relates to the field of composite foam, and particularly relates to super-hydrophobic octyl graphene foam and a preparation method thereof.
Background
The environmental problems caused by the leakage of oil and liquid organic substances are not of small magnitude, and the carcinogenic substances in the oil continuously damage the health of human beings, thereby providing a new challenge for corresponding quick response and treatment. Therefore, research and development of high-performance environment-friendly materials are receiving much attention.
In the face of oil leakage problems, typical remedies include mechanical harvesting, chemical dispersants, bioremediation and in situ combustion. However, these techniques suffer from the disadvantages of time consumption, environmental unfriendliness, poor repeatability, etc. With the development of nanomaterials, a number of nanosorbent materials have emerged. But the preparation process is complex and has poor stability, and the method is not completely suitable for real enterprises.
Therefore, it is urgently required to find an ideal adsorbing material to solve these problems. The metal foam material is developed rapidly in the late 20 th century 80 s internationally, and is a novel functional material with an internal structure containing a plurality of pores. Has excellent physical properties and good mechanical properties, and can be widely applied to the fields of aviation, electronics, medical use and biochemistry. The foamed nickel has large specific surface area, rough surface characteristic, temperature resistance and corrosion resistance.
Disclosure of Invention
Aiming at the defects of long time consumption, complicated steps, poor repeatability and the like in the existing technology for treating leaked oil products and liquid organic matters, the invention aims to provide novel super-hydrophobic octyl graphene foam and a preparation method thereof.
An octyl graphene foam is prepared by the following steps:
taking foamed nickel as a substrate, and attaching octyl graphene on the surface of the foamed nickel to obtain the graphene-based composite material;
the octyl graphene is obtained by reacting graphene oxide with octyl-triethoxysilane to obtain octyl graphene oxide and then carrying out reduction reaction on the octyl graphene oxide.
The raw materials are selected and prepared according to the method, and the octyl graphene foam can be prepared simply. The method also has the advantages of low cost, simple process, easy operation, good material hydrophobicity and strong recycling property.
Preferably, in the reduction reaction, the reducing agent is ascorbic acid. The ascorbic acid has the advantages of high reducing capability, environmental friendliness and the like. The ascorbic acid can effectively convert the graphene oxide aqueous solution into the stable monodisperse graphene suspension under the mild condition, and compared with other reducing agents, the ascorbic acid is adopted to reduce the graphene oxide at room temperature, so that the control on the reduction degree of the graphene oxide is easy to realize, and the subsequent application of octyl graphene foam is facilitated.
Further, the mass ratio of the ascorbic acid to the octyl graphene oxide is (1-2): 1; according to the above ratio, the reaction can be efficiently carried out without wasting the raw material.
Specifically, the method comprises the following steps:
1) octyl-triethoxysilane-modified graphene oxide: ultrasonically dispersing graphene oxide into an organic solvent, adding octyl-triethoxysilane, heating and stirring in an oil bath to obtain octyl graphene oxide; the mass-to-volume ratio of the graphene oxide to the octyl-triethoxysilane is (1-3) to 10 (g/mL);
2) preparing octyl graphene: dispersing the octyl graphene oxide in an organic solvent, adding ascorbic acid, and carrying out reduction reaction to obtain octyl graphene;
3) preparing octyl graphene foam: and fully dispersing the octyl graphene by using an organic solvent, so that the octyl graphene is fully and stably attached to the surface of the foamed nickel.
In the preparation method of the invention, in the step 1), in the octyl-triethoxysilane modified graphene oxide, the graphene oxide may be prepared by using a commercially available product or any method known in the art, and is not particularly limited herein, but only provides a preferred method, and the graphene oxide is prepared by the following method:
adding concentrated sulfuric acid into graphite powder and KNO at the temperature of less than or equal to 0 DEG C3To the mixture of (1), KMnO is added4Stirring the mixture, heating to room temperature, stirring to homogeneity, diluting the mixture with water, and adding H2O2And continuously stirring to obtain the graphene oxide. The mass-volume ratio of the graphite powder to the concentrated sulfuric acid is 1.5 g: (60-75) ml, wherein the graphite powder: KNO3：KMnO4The mass ratio of (A) to (B) is 1.5: (1-1.5): (5 to 6), H2O2The amount of (b) added is 1% to 1.5% of the total volume of the mixture obtained after diluting the mixture with water. Said H2O2The mass concentration of (A) is 25-30%.
The preparation of the graphene oxide also comprises the steps of washing and drying, and the obtained graphene oxide is washed by repeatedly washing with dilute hydrochloric acid solution until SO does not exist in washing liquor4 2-And repeatedly washing with ultrapure water until the solution is neutral, and drying according to the conventional operation in the field.
The method comprises the following steps of 1) modifying graphene oxide by octyl-triethoxysilane:
when the mass-volume ratio of the graphene oxide to the octyl-triethoxysilane is (1-3):10(g/mL), the prepared octyl-triethoxysilane modified graphene oxide can be ensured, and the advantages of huge specific surface area and more adsorption sites of the graphene can be fully exerted. With a 2:10 ratio being optimal.
Preferably, the temperature of the oil bath heating is 100-120 ℃ (110 ℃ being the most preferred); this temperature is favorable for the reaction. The stirring is controlled at a rotation speed of 200-300 rpm.
The organic solvent is selected from one of Dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and Tetrahydrofuran (THF). Preferably dimethylformamide;
further, the mass-to-volume ratio of the graphene oxide to the organic solvent is (1-5):100 (g/mL). The excessive or insufficient amount of the organic solvent can influence the reaction, and the solvent can fully disperse the graphene and is beneficial to post-treatment under the control of the proportion.
The purpose of the ultrasonic treatment is to uniformly disperse the graphene oxide into the organic solvent, preferably 1 hour.
The method comprises the following steps of 2) preparing octyl graphene:
the organic solvent is selected from one of Dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and Tetrahydrofuran (THF). Preferably dimethylformamide; the mass-volume ratio of the octyl graphene oxide to the organic solvent is (1-3) to 100 (g/mL);
the temperature of the reduction reaction is 70-80 deg.C (preferably 80 deg.C), and ultrasonic treatment is preferably carried out for 30-70min, preferably 40 min. The ultrasonic heating at the temperature can complete the reaction with high efficiency, and the raw materials are saved as much as possible.
The method comprises the following steps of 3) preparing octyl graphene foam:
the organic solvent is selected from one of Dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and Tetrahydrofuran (THF).
Preferably, the sufficient dispersion is at least two dispersions and centrifugation. The specific operation is as follows: dispersing and centrifuging for the first time, dispersing and centrifuging again, and then carrying out ultrasonic treatment on the suspension. And then adding foamed nickel, uniformly dispersing by ultrasonic, and taking out the foamed nickel to obtain the superhydrophobic octyl graphene foam. The purpose of the multiple dispersion is to ensure that octyl graphene is fully and stably attached to the surface of the nickel foam.
The dispersion and centrifugation means ultrasonic treatment for 30min at normal temperature and centrifugation for 10min at 10000 rpm. Dispersing again, centrifuging, and subjecting the obtained suspension to ultrasound for 20-30 min.
The attachment is carried out at 70-80 ℃, specifically, the foam nickel is slowly put into the suspension, and after uniform ultrasonic dispersion (ultrasonic treatment is carried out for 40min at 70-80 ℃), the foam nickel is taken out and dried to obtain octyl graphene foam; the purpose of ultrasonic dispersion is to enable the turbid liquid to be uniformly adsorbed on the foamed nickel as far as possible, and the temperature is adopted because the speed is moderate at the temperature, the graphene cannot be damaged, and the adhesion rate is high.
The foamed nickel is completely immersed in the suspension. Preferably, the nickel foam has a size of 10 x 200 x 300mm, which can be varied up to and down to 10% on this basis.
Preferably, repeating the steps (namely, the step of slowly putting the foamed nickel into the suspension, uniformly dispersing by ultrasonic waves and then taking out the foamed nickel) for 3-5 times to obtain the octyl graphene foam.
Among them, the prepared octyl graphene foam is preferably washed with absolute ethyl alcohol.
The drying may be carried out by conventional means in the art, but provides a preferred means of rapid drying at 180 ℃ in a forced air drying cabinet.
The invention also provides the superhydrophobic octyl graphene foam prepared by any one of the preparation methods.
The invention creatively discovers that the active reaction sites of graphene oxide are subjected to hydrophobic treatment by octyl groups by virtue of the unique property difference of graphene-graphene oxide. After the graphene is reduced, the excellent characteristics of the graphene can be further obtained. Octyl-triethoxysilane is grafted to the surface of graphene to prepare graphene with octyl groups on the surface, and octyl enhances the interaction force between foamed nickel and graphene, improves the compatibility between nano graphene and a matrix, so that the prepared super-hydrophobic foam has more stable hydrophobic performance in the use process. It can be seen that the obtained superhydrophobic octyl graphene foam is a promising and commercially available high-performance material.
Compared with organic foam and porous sponge, the foam nickel has high mechanical strength and strong pressure resistance, can still maintain good strength at a very thin thickness, and is not easy to become brittle and pulverize.
The performances of all aspects of the modified octyl graphene foam nickel are enhanced, the ductility is stronger, and the requirements can be met in different shapes according to specific scenes; the original shape is kept in the process of recycling for multiple times. In addition, the nickel foam has high heat resistance level, large temperature range for treating wastewater, low toxicity and low pollution.
The invention provides application of the octyl graphene foam in medical analysis, food detection and sewage treatment.
Specifically, the invention provides an application of the octyl graphene foam in sewage treatment to adsorb liquid organic matters (such as diesel oil, engine oil, toluene and the like).
Drawings
FIG. 1 is a graph comparing a conventional foam and an octyl graphene foam in example 1 of the present invention. (a is plain foam from Peveri silk manufacturing, Anping, prefecture, b is octyl graphene foam prepared as in example 1)
Fig. 2 is a contact angle graph of octyl graphene foam and water in example 1 of the present invention.
FIG. 3 is a graph showing the comparison of the hydrophobicity of octyl graphene foam to different substances in test example 1 of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the following examples, the graphene oxide used was prepared by the following method: at the temperature of less than or equal to 0 ℃, 75mL of concentrated sulfuric acid is added into 1.5g of graphite powder and 1.5g of KNO3To the mixture was added 6.0g of KMnO4Obtaining a mixture 1, continuously stirring the mixture 1 for 20min, raising the temperature to room temperature, continuously stirring for 1.5h, adding 200mL of water to dilute the mixture 1, and adding 15mL of 30% by mass of the mixtureH2O2Stirring was continued for 3 h. Repeatedly washing with 5% by mass HCl solution until 1% BaCl is used2The solution does not detect the presence of SO in the wash solution4 2-And repeatedly washing with ultrapure water till the graphene oxide is neutral, and drying to obtain the solid graphene oxide.
Example 1
The embodiment provides octyl graphene foam and a preparation method thereof, and the preparation method comprises the following steps:
(1) modified graphene oxide: 2.0g of graphene oxide and 200mL of Dimethylformamide (DMF) are added into a round bottom flask and ultrasonically mixed for 1h at normal temperature, then 10mL of octyl-triethoxysilane is added into the flask, placed on a magnetic stirrer and stirred, heated and stirred in an oil bath at 110 ℃ at the rotating speed of 270 rpm.
(2) Preparing octyl graphene: 0.6g ascorbic acid and 0.5g octyl graphene oxide were added to 50mL Dimethylformamide (DMF) and ultrasonically mixed at 80 ℃ for 40 min.
(3) Preparing octyl graphene foam: dispersing the obtained octyl graphene with dimethyl formamide (DMF), centrifuging, dispersing again, performing ultrasonic treatment on the suspension for 20min, putting the foamed nickel into the suspension, performing ultrasonic treatment at 80 ℃ for 40min, standing, taking out, and drying to obtain the superhydrophobic octyl graphene foam (shown in figure 1 b).
The contact angle with water is 147.1 degrees as shown in figure 2, which shows that the material has good super-hydrophobic property.
Example 2
The embodiment provides octyl graphene foam and a preparation method thereof, and the preparation method comprises the following steps:
(1) modified graphene oxide: 2.0g of graphene oxide and 200mL of Dimethylformamide (DMF) were added to a round bottom flask and ultrasonically mixed at room temperature for 50min, after which 10mL of octyl-triethoxysilane was added to the flask, stirred on a magnetic stirrer and oil-bathed at 110 ℃ with a rotation speed of 270 rpm.
(2) Preparing octyl graphene: 0.6g ascorbic acid and 0.5g octyl graphene oxide were added to 50mL Dimethylformamide (DMF) and ultrasonically mixed at 80 ℃ for 85 min.
(3) Preparing octyl graphene foam: dispersing the obtained octyl graphene with dimethyl formamide (DMF), centrifuging, dispersing again, performing ultrasonic treatment on the suspension for 20min, putting the foamed nickel into the suspension, performing ultrasonic treatment at 80 ℃ for 1h, standing, taking out and drying. Thereby preparing octyl graphene foam.
Example 3
The embodiment provides octyl graphene foam and a preparation method thereof, and the preparation method comprises the following steps:
(1) modified graphene oxide: 2.0g of graphene oxide and 200mL of Dimethylformamide (DMF) were added to a round bottom flask and ultrasonically mixed at room temperature for 40min, then 10mL of octyl-triethoxysilane was added to the flask containing the graphene solution, stirred on a magnetic stirrer and subjected to an oil bath at 110 ℃ and a rotational speed of 270 rpm.
(2) Preparing octyl graphene: 0.6g ascorbic acid and 0.5g octyl graphene oxide were added to 50mL Dimethylformamide (DMF) and ultrasonically mixed at 50 ℃ for 90 min.
(3) Preparing octyl graphene foam: dispersing the obtained octyl graphene with dimethyl formamide (DMF), centrifuging, dispersing again, performing ultrasonic treatment on the turbid liquid for 20min, putting the foamed nickel into the turbid liquid, performing ultrasonic treatment at normal temperature for 90min, standing, taking out, and drying to obtain octyl graphene foam.
Example 4
The embodiment provides octyl graphene foam and a preparation method thereof, and the preparation method comprises the following steps:
(1) modified graphene oxide: 1.0g of graphene oxide and 200mL of Dimethylformamide (DMF) are added into a round bottom flask and ultrasonically mixed for 1h at normal temperature, then 10mL of octyl-triethoxysilane is added into the flask, placed on a magnetic stirrer and stirred, heated and stirred in an oil bath at 110 ℃ at the rotating speed of 270 rpm.
(2) Preparing octyl graphene: 1.0g ascorbic acid and 0.5g octyl graphene oxide were added to 50mL Dimethylformamide (DMF) and ultrasonically mixed at 70 ℃ for 60 min.
(3) Preparing octyl graphene foam: dispersing the obtained octyl graphene with dimethyl formamide (DMF), centrifuging, dispersing again, performing ultrasonic treatment on the turbid liquid for 20min, putting the foamed nickel into the turbid liquid, performing ultrasonic treatment at 80 ℃ for 40min, standing, taking out, and drying to obtain the superhydrophobic octyl graphene foam.
Example 5
The embodiment provides octyl graphene foam and a preparation method thereof, and the preparation method comprises the following steps:
(1) modified graphene oxide: 2.0g of graphene oxide and 200mL of Dimethylformamide (DMF) are added into a round bottom flask and ultrasonically mixed for 1h at normal temperature, then 10mL of octyl-triethoxysilane is added into the flask, placed on a magnetic stirrer and stirred, heated and stirred in an oil bath at 110 ℃ at the rotating speed of 270 rpm.
(2) Preparing octyl graphene: 0.5g ascorbic acid and 0.5g octyl graphene oxide were added to 50mL Dimethylformamide (DMF) and ultrasonically mixed at 70 ℃ for 60 min.
(3) Preparing octyl graphene foam: dispersing the obtained octyl graphene with dimethyl formamide (DMF), centrifuging, dispersing again, performing ultrasonic treatment on the turbid liquid for 20min, putting the foamed nickel into the turbid liquid, performing ultrasonic treatment at 80 ℃ for 40min, standing, taking out, and drying to obtain the superhydrophobic octyl graphene foam.
Example 6
The embodiment provides octyl graphene foam and a preparation method thereof, and the preparation method comprises the following steps:
(1) preparing Graphene Oxide (GO): at the temperature of less than or equal to 0 ℃, 75mL of concentrated sulfuric acid is added into 1.5g of graphite powder and 1.5g of KNO3To the mixture was added 6.0g of KMnO4Obtaining a mixture 1, continuously stirring the mixture 1 for 20min, raising the temperature to room temperature, continuously stirring for 1.5H, adding 200mL of water to dilute the mixture 1, and adding 15mL of H with the mass ratio of 30%2O2Stirring was continued for 3 h. Repeatedly washing with 5% by mass HCl solution until 1% BaCl is used2The solution does not detect the presence of SO in the wash solution4 2-And repeatedly washing with ultrapure water till the graphene oxide is neutral, and drying to obtain the solid graphene oxide.
(2) Modified graphene oxide: 2.0g of graphene oxide and 200mL of Dimethylformamide (DMF) are added into a round bottom flask and ultrasonically mixed for 1h at normal temperature, then 10mL of octyl-triethoxysilane is added into the flask, placed on a magnetic stirrer and stirred, heated and stirred in an oil bath at 110 ℃ and the rotating speed is 270 rpm.
(3) Preparing octyl graphene: 0.6g ascorbic acid and 0.5g octyl graphene oxide were added to 50mL Dimethylformamide (DMF) and ultrasonically mixed at 80 ℃ for 40 min.
(4) Preparing octyl graphene foam: dispersing the obtained octyl graphene with dimethyl formamide (DMF), centrifuging, dispersing again, performing ultrasonic treatment on the turbid liquid for 20min, putting the foamed nickel into the turbid liquid, performing ultrasonic treatment at 80 ℃ for 40min, standing, taking out, and drying to obtain the superhydrophobic octyl graphene foam.
Test example 1
This experimental example provides a hydrophobic adsorption test of octyl graphene foam.
Test subjects: hydrochloric acid (concentration of 1mol/L), sodium hydroxide (mass concentration of 1mol/L), sodium chloride (mass concentration of 1mol/L) and water which are respectively marked by methyl orange.
The test method comprises the following steps: the solutions were dropped on the surface of the prepared octyl graphene foam (prepared in example 1) to perform a hydrophobic property test.
And (3) test results: as shown in fig. 3, the results show that the octyl graphene foam has a strong hydrophobic ability for the above four solutions.
The above four solutions can represent most solutions (such as acid solution, alkali solution, salt solution and water), so that the octyl graphene foam provided by the invention has strong hydrophobic capability.
The above experimental procedure was repeated with the octyl graphene foams prepared in examples 2-6, and the results were the same.
Test example 2
This experimental example provides an adsorption capacity test of octyl graphene foam.
Test subjects: octyl graphene foam provided in example 1.
The test method comprises the following steps: and respectively measuring the adsorption quantity of the foam to toluene and diesel oil by adopting a static adsorption method.
40mL of toluene and diesel oil were respectively placed in a 200mL conical flask, and two 4cm by 3cm pieces of the octyl graphene foam prepared in example 1 were weighed in sequence and recorded as m0Respectively placing the mixture into two conical flasks, sealing the conical flasks at room temperature, keeping the temperature for 10min, taking out the octyl graphene foam, weighing again and recording as m1. By the formula Q ═ m1-m0)/m0The adsorption capacity of the adsorbent was calculated, and the average was obtained by repeating 5 times.
The experimental results show that: by calculation, the adsorption capacities Q of the octyl graphene foam to toluene and diesel oil are respectively 2.8 and 3.24(g/g) on average, which shows that the product prepared by the method has better adsorption capacity to different organic solvents.
Test example 3
This test example provides the oil-water separation ability of octyl graphene foam.
Test subjects: octyl graphene foam provided in example 1.
The test method comprises the following steps:
mixing diesel oil (0.38g) and appropriate amount of distilled water to 30mL in a 50mL dry round bottom flask to obtain an oil-water mixture, performing ultrasonic treatment for 15min, putting 4cm x 3cm octyl graphene foam into 30mL of distilled water, taking out, and weighing the foam with the mass qw(ii) a Drying, placing in the above diesel oil-water mixture, sealing the round bottom flask, adsorbing at room constant temperature for 30min, slowly taking out octyl graphene foam, and weighing (q)f) The weight of the adsorbed diesel oil is (q)f-qw) Therefore, diesel removal efficiency η (%) - (q)f-qw) 0.38, repeat 5 times to get the average.
The experimental results show that: the removal efficiency of the diesel reaches 96 percent, which shows that the product prepared by the invention has stronger hydrophobicity and lipophilicity and shows good oil-water separation capability.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. A preparation method of superhydrophobic octyl graphene foam is characterized by comprising the following steps:
1) octyl-triethoxysilane-modified graphene oxide: ultrasonically dispersing graphene oxide into an organic solvent, adding octyl-triethoxysilane, heating and stirring in an oil bath to obtain octyl graphene oxide;
the mass-volume ratio of the graphene oxide to the octyl-triethoxysilane is 2: 10;
2) preparing octyl graphene: dispersing the octyl graphene oxide in an organic solvent, adding ascorbic acid, and carrying out reduction reaction to obtain octyl graphene; the mass ratio of the ascorbic acid to the octyl graphene oxide is (1-2): 1;
3) preparing octyl graphene foam: fully dispersing the octyl graphene by using an organic solvent to ensure that the octyl graphene is fully and stably attached to the surface of the foamed nickel;
in the step 1) and the step 2), the organic solvent is dimethylformamide; in the step 1), the mass-to-volume ratio of the graphene to the dimethylformamide is (1-5) to 100; in the step 2), the mass-to-volume ratio of the octyl graphene oxide to the dimethylformamide is (1-3) to 100;
in the step 3), the attaching operation is carried out at 70-80 ℃.
2. The method according to claim 1, wherein the temperature of the reduction reaction is 70 ℃ to 80 ℃.
3. The preparation method according to claim 2, wherein the reduction reaction is performed by ultrasonication for 30-60 min.
4. The method as claimed in claim 1, wherein the temperature for heating the oil bath in step 1) is 100-120 ℃.
5. The method as claimed in claim 4, wherein the stirring in step 1) is controlled at a rotation speed of 200-300 rpm.
6. The production method according to claim 4 or 5,
in the step 3), fully ultrasonically dispersing a turbid liquid formed by octyl graphene and an organic solvent, putting foamed nickel into the turbid liquid at the temperature of 70-80 ℃, and taking out the foamed nickel; and repeating the ultrasonic dispersion at the same temperature at least once and taking out the foamed nickel to obtain the octyl graphene foam.
7. A superhydrophobic octyl graphene foam prepared by the preparation method of any one of claims 1-6.
8. The use of the superhydrophobic octyl graphene foam of claim 7 in medical analysis, food testing, and wastewater treatment.
9. The superhydrophobic octyl graphene foam of claim 8, being used to adsorb liquid organics in sewage treatment.
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