CN109331780B - Preparation method of activated carbon fiber/graphene tube composite material - Google Patents
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Abstract
The invention provides a preparation method of an activated carbon fiber/graphene tube composite material. Then dipping the activated carbon fiber in concentrated nitric acid and carrying out ultrasound to obtain pretreated activated carbon fiber, dipping the pretreated activated carbon fiber in graphene oxide solution and carrying out ultrasound or oscillation, self-assembling graphene oxide on the surface of the activated carbon fiber to form a graphene tube, and finally drying to obtain the activated carbon fiber/graphene tube composite material, wherein the tube diameter of the graphene tube is 10-50 nm, and the specific surface area of the activated carbon fiber/graphene tube composite material reaches 1200-1500m2(ii) in terms of/g. The activated carbon fiber/graphene tube composite material has excellent adsorption performance on persistent organic pollutants. The method is simple and easy to implement, safe and environment-friendly, and has great application value.
Description
Technical Field
The invention relates to the technical field of nano composite materials, in particular to an activated carbon fiber/graphene tube composite material and a preparation method thereof.
Background
The persistent organic pollutant is toxic refractory organic matter, has high chemical stability, and has carcinogenic, teratogenic and mutagenic effects. It is directly harmful to human health, and also seriously damages water, soil and ecological environment, causing unthinkable consequences. The adsorption method has the advantages of low cost, simple operation and high speed, and is considered to be an effective method for treating the persistent organic pollutants in the water body. The performance of the adsorbent in the adsorption method is the most critical. Thus, the development of high efficiency adsorbents has been the focus of research in this field.
The activated carbon fiber has high specific surface area and is a high-efficiency active adsorption material. But its pore structure is basically composed of micropores (pore diameter <2nm), and therefore, its adsorption efficiency to macromolecular persistent organic pollutants is low. Graphene oxide has a large specific Surface area and rich functional groups, and has an aromatic-like ring structure in itself, and thus graphene oxide and its composites have received much attention in the field of persistent organic contaminant adsorption since its discovery, such as documents z.wu, et al, water Research,2014,67: 330-.
It is reported that the graphene tube has a stronger adsorption effect on organic pollutants. Publication No. CN102586869 discloses a preparation method of a three-dimensional graphene tube, but the method needs a high-temperature chemical vapor deposition method for preparation, and finally needs strong acid for etching, and the method has harsh experimental conditions and higher cost. Therefore, the activated carbon fiber with high specific surface area and the graphene tube with the aromatic-like ring structure are combined to prepare the activated carbon fiber/graphene tube composite material which can be used as an excellent adsorbent for organic pollutants in water. However, no relevant research report for preparing the activated carbon fiber/graphene tube under the low-temperature condition exists at present.
Disclosure of Invention
The invention aims to provide a preparation method of an activated carbon fiber/graphene tube composite material. The high specific surface area of the activated carbon fiber and the structure of the graphene tube aromatic ring are combined, graphene is oxidized by strong ultrasonic waves and then self-assembled on the surface of the activated carbon fiber, and the activated carbon fiber/graphene tube composite material with high adsorption performance on organic pollutants is formed.
The technical scheme of the active carbon fiber/graphene tube composite material is as follows:
(1) the graphene oxide is prepared by a modified Hummers method. Namely: adding H2SO4/H3PO4(360mL:40mL)9:1 mixture to 3.0g graphite and 18.0g KMnO4In the mixture of (3), a small amount of heat is generated to raise the temperature to 35-40 ℃. Then heated to 50 ℃ and stirred for reaction for 12 h. The reaction solution was cooled to room temperature, and a certain amount of ice water and 30% H were added2O2The solution was bright yellow. Then, it was washed with 5% HCl solution and deionized water until no sulfate was detected in the filtrate.
(2) And (3) centrifugally separating the dispersion liquid obtained in the step (1), removing unoxidized graphite at the lower part, and keeping a supernatant. And obtaining the graphene oxide solution.
(3) Diluting the graphene oxide solution prepared in the step (2) with deionized water and performing strong ultrasonic treatment to obtain the required graphene oxide solution.
(4) Dipping the activated carbon fiber in concentrated nitric acid for ultrasonic treatment, then pouring the concentrated nitric acid, washing with deionized water and drying. Wherein the amount of the activated carbon fiber is 5-10g, the activated carbon fiber is immersed in 1000mL concentrated nitric acid and is subjected to ultrasonic treatment for 3-6h, the ultrasonic frequency is 40KHz, and the power is 400W. Washing the activated carbon fiber treated by concentrated nitric acid with deionized water until the pH value is 6-7, and drying at 60-80 ℃.
(5) And (3) dipping the activated carbon fiber treated in the step (4) in the graphene oxide solution prepared in the step (3), taking out the activated carbon fiber after ultrasonic treatment or oscillation, and drying the activated carbon fiber/graphene tube composite material to obtain the activated carbon fiber/graphene tube composite material. Wherein, ultrasonic treatment or oscillation is carried out for 3-6h at 35-45 ℃, when ultrasonic treatment is selected, the wave frequency is 30-60KHz, and the power is 400W; and selecting oscillation with the oscillation speed of 60-100 r/min.
The concentration of the graphene oxide solution required in the step (3) is 3-8 mg/mL.
And (3) the graphene oxide ultrasonic frequency is 100KHz, and the power is 800W.
And (4) carrying out ultrasonic treatment on the graphene oxide solution in the step (3) for 4-8 h.
According to the method, graphene oxide is subjected to ultrasonic treatment, then graphene oxide is self-assembled on the surface of the activated carbon fiber at a low temperature to form a graphene tube, the activated carbon fiber/graphene tube composite material is prepared, the tube diameter of the graphene tube is 10-50 nm, and the specific surface area of the activated carbon fiber/graphene tube composite material reaches 1200-1500 m-2The activated carbon fiber/graphene tube composite material has excellent adsorption performance on persistent organic pollutants.
Drawings
Fig. 1 SEM of activated carbon fiber/graphene tube composite.
Detailed Description
Example 1
(1) The graphene oxide is prepared by a modified Hummers method. Namely: adding H2SO4/H3PO4(360mL:40mL)9:1 mixture to 3.0g graphite and 18.0g KMnO4In the mixture of (3), a small amount of heat is generated to raise the temperature to 35-40 ℃. Then heated to 50 ℃ and stirred for reaction for 12 h. The reaction solution was cooled to room temperature, and a certain amount of ice water and 30% H were added2O2The solution was bright yellow. Then, it was washed with 5% HCl solution and deionized water until no sulfate was detected in the filtrate.
(2) And (3) centrifugally separating the dispersion liquid obtained in the step (1), removing unoxidized graphite at the lower part, and keeping a supernatant. And obtaining the graphene oxide solution.
(3) Diluting the graphene oxide solution prepared in the step (2) with deionized water to the concentration of 5mg/mL, and performing ultrasonic treatment for 6 hours at the ultrasonic frequency of 100KHz and the power of 800W to obtain the required graphene oxide solution.
(4) 6g of activated carbon fiber is soaked in 1000mL of concentrated nitric acid for ultrasonic treatment for 4h, the ultrasonic frequency is 40KHz, and the power is 400W. The concentrated nitric acid was then decanted, washed with deionized water to a pH of 6-7, and dried at 70 ℃.
(5) And (3) dipping the activated carbon fiber treated in the step (4) in the graphene oxide solution of 5mg/mL prepared in the step (3), performing ultrasonic treatment at 40 ℃ for 4 hours, taking out and drying, wherein the ultrasonic frequency is 40KHz, and the power is 400W, so as to prepare the activated carbon fiber/graphene tube composite material.
Example 2:
(1) the graphene oxide is prepared by a modified Hummers method. Namely: adding H2SO4/H3PO4(360mL:40mL)9:1 mixture to 3.0g graphite and 18.0g KMnO4In the mixture of (3), a small amount of heat is generated to raise the temperature to 35-40 ℃. Then heated to 50 ℃ and stirred for reaction for 12 h. The reaction solution was cooled to room temperature, and a certain amount of ice water and 30% H were added2O2The solution was bright yellow. Then, it was washed with 5% HCl solution and deionized water until no sulfate was detected in the filtrate.
(2) And (3) centrifugally separating the dispersion liquid obtained in the step (1), removing unoxidized graphite at the lower part, and keeping a supernatant. And obtaining the graphene oxide solution.
(3) Diluting the graphene oxide solution prepared in the step (2) with deionized water to the concentration of 3mg/mL, and performing ultrasonic treatment for 4 hours at the ultrasonic frequency of 100KHz and the power of 800W to obtain the required graphene oxide solution.
(4) 5g of activated carbon fiber is soaked in 1000mL of concentrated nitric acid for ultrasonic treatment for 3h, the ultrasonic frequency is 40KHz, and the power is 400W. The concentrated nitric acid was then decanted, washed with deionized water to a pH of 6-7 and dried at 60 ℃.
(5) And (3) dipping the activated carbon fiber treated in the step (4) in the graphene oxide solution of 3mg/mL prepared in the step (3), performing ultrasonic treatment at 35 ℃ for 3 hours, taking out and drying, wherein the ultrasonic frequency is 30KHz, and the power is 400W, so as to prepare the activated carbon fiber/graphene tube composite material.
Example 3
(1) The graphene oxide is prepared by a modified Hummers method. Namely: adding H2SO4/H3PO4(360mL:40mL)9:1 mixture to 3.0g graphite and 18.0g KMnO4In the mixture of (3), a small amount of heat is generated to raise the temperature to 35-40 ℃. Then heated to 50 ℃ and stirred for reaction for 12 h. Inverse directionCooling the reaction solution to room temperature, adding a certain amount of ice water and 30% of H2O2The solution was bright yellow. Then, it was washed with 5% HCl solution and deionized water until no sulfate was detected in the filtrate.
(2) And (3) centrifugally separating the dispersion liquid obtained in the step (1), removing unoxidized graphite at the lower part, and keeping a supernatant. And obtaining the graphene oxide solution.
(3) Diluting the graphene oxide solution prepared in the step (2) with deionized water to the concentration of 8mg/mL, and performing ultrasonic treatment for 8 hours at the ultrasonic frequency of 100KHz and the power of 800W to obtain the required graphene oxide solution.
(4) 10g of activated carbon fiber is soaked in 1000mL of concentrated nitric acid for 6 hours of ultrasonic treatment, the ultrasonic frequency is 40KHz, and the power is 400W. The concentrated nitric acid was then decanted, washed with deionized water to a pH of 6-7, and dried at 80 ℃.
(5) And (3) dipping the activated carbon fiber treated in the step (4) in the graphene oxide solution of 8mg/mL prepared in the step (3), performing ultrasonic treatment at 45 ℃ for 6 hours, taking out and drying, wherein the ultrasonic frequency is 60KHz, and the power is 400W, so as to prepare the activated carbon fiber/graphene tube composite material.
Example 4
(1) The graphene oxide is prepared by a modified Hummers method. Namely: adding H2SO4/H3PO4(360mL:40mL)9:1 mixture to 3.0g graphite and 18.0g KMnO4In the mixture of (3), a small amount of heat is generated to raise the temperature to 35-40 ℃. Then heated to 50 ℃ and stirred for reaction for 12 h. The reaction solution was cooled to room temperature, and a certain amount of ice water and 30% H were added2O2The solution was bright yellow. Then, it was washed with 5% HCl solution and deionized water until no sulfate was detected in the filtrate.
(2) And (3) centrifugally separating the dispersion liquid obtained in the step (1), removing unoxidized graphite at the lower part, and keeping a supernatant. And obtaining the graphene oxide solution.
(3) Diluting the graphene oxide solution prepared in the step (2) with deionized water to the concentration of 5mg/mL, and performing ultrasonic treatment for 6 hours at the ultrasonic frequency of 100KHz and the power of 800W to obtain the required graphene oxide solution.
(4) 6g of activated carbon fiber is soaked in 1000mL of concentrated nitric acid for ultrasonic treatment for 4h, the ultrasonic frequency is 40KHz, and the power is 400W. The concentrated nitric acid was then decanted, washed with deionized water to a pH of 6-7, and dried at 70 ℃.
(5) And (3) soaking the activated carbon fiber treated in the step (4) in the graphene oxide solution of 5mg/mL prepared in the step (3), oscillating at 40 ℃ for 4h, taking out and drying, and oscillating at the speed of 80r/min to obtain the activated carbon fiber/graphene tube composite material.
Example 5
(1) The graphene oxide is prepared by a modified Hummers method. Namely: adding H2SO4/H3PO4(360mL:40mL)9:1 mixture to 3.0g graphite and 18.0g KMnO4In the mixture of (3), a small amount of heat is generated to raise the temperature to 35-40 ℃. Then heated to 50 ℃ and stirred for reaction for 12 h. The reaction solution was cooled to room temperature, and a certain amount of ice water and 30% H were added2O2The solution was bright yellow. Then, it was washed with 5% HCl solution and deionized water until no sulfate was detected in the filtrate.
(2) And (3) centrifugally separating the dispersion liquid obtained in the step (1), removing unoxidized graphite at the lower part, and keeping a supernatant. And obtaining the graphene oxide solution.
(3) Diluting the graphene oxide solution prepared in the step (2) with deionized water to the concentration of 3mg/mL, and performing ultrasonic treatment for 4 hours at the ultrasonic frequency of 100KHz and the power of 800W to obtain the required graphene oxide solution.
(4) 5g of activated carbon fiber is soaked in 1000mL of concentrated nitric acid for ultrasonic treatment for 3h, the ultrasonic frequency is 40KHz, and the power is 400W. The concentrated nitric acid was then decanted, washed with deionized water to a pH of 6-7 and dried at 60 ℃.
(5) And (3) soaking the activated carbon fiber treated in the step (4) in the graphene oxide solution of 3mg/mL prepared in the step (3), oscillating at 35 ℃ for 3h, taking out and drying, and oscillating at the speed of 60r/min to obtain the activated carbon fiber/graphene tube composite material.
Example 6
(1) The graphene oxide is prepared by a modified Hummers method. Namely: adding H2SO4/H3PO4(360mL:40mL)9:1 mixture to 3.0g graphite and 18.0g KMnO4In the mixture of (3), a small amount of heat is generated to raise the temperature to 35-40 ℃. Then heated to 50 ℃ and stirred for reaction for 12 h. The reaction solution was cooled to room temperature, and a certain amount of ice water and 30% H were added2O2The solution was bright yellow. Then, it was washed with 5% HCl solution and deionized water until no sulfate was detected in the filtrate.
(2) And (3) centrifugally separating the dispersion liquid obtained in the step (1), removing unoxidized graphite at the lower part, and keeping a supernatant. And obtaining the graphene oxide solution.
(3) Diluting the graphene oxide solution prepared in the step (2) with deionized water to the concentration of 8mg/mL, and performing ultrasonic treatment for 8 hours at the ultrasonic frequency of 100KHz and the power of 800W to obtain the required graphene oxide solution.
(4) 10g of activated carbon fiber is soaked in 1000mL of concentrated nitric acid for 6 hours of ultrasonic treatment, the ultrasonic frequency is 40KHz, and the power is 400W. The concentrated nitric acid was then decanted, washed with deionized water to a pH of 6-7, and dried at 80 ℃.
(5) And (3) dipping the activated carbon fiber treated in the step (4) in the graphene oxide solution of 8mg/mL prepared in the step (3), oscillating at 45 ℃ for 6h, taking out and drying, and oscillating at the speed of 100r/min to obtain the activated carbon fiber/graphene tube composite material.
Claims (6)
1. The preparation method of the activated carbon fiber/graphene tube composite material is characterized by comprising the following steps:
step 1, preparing a graphene oxide solution by an improved Hummers method: 360mL of H2SO4And 40mL H3PO4I.e. H2SO4And H3PO4After mixing at a volume ratio of 9:1, the mixture was added to 3.0g of graphite and 18.0g of KMnO4I.e. graphite and KMnO4The mass ratio is 1: 6, the heat generated raises the temperature to 35-40 ℃; then heating to 50 ℃, and stirring for reaction for 12 hours; the reaction solution was cooled to room temperature, and ice water and 30% H were added2O2Until the solution is bright yellow; then, 5% HCl solution and deionized water were usedWashing until no sulfate radical is detected in the filtrate; centrifuging the obtained dispersion liquid, removing the graphite which is not oxidized at the lower part, and reserving the supernatant liquid to obtain a graphene oxide solution; diluting the prepared graphene oxide solution with deionized water and performing ultrasonic treatment to obtain the required graphene oxide solution;
step 2, dipping 5-10g of activated carbon fiber in 1000mL of concentrated nitric acid for ultrasonic treatment, taking out, washing with deionized water until the pH value is 6-7, and drying at 60-80 ℃ for pretreatment; then dipping the pretreated activated carbon fiber in the required graphene oxide solution prepared in the step 1, carrying out ultrasonic treatment or oscillation for 3-6h at 35-45 ℃, wherein the ultrasonic frequency is 30-60KHz, the power is 400W, and the oscillation speed is 60-100r/min, taking out the activated carbon fiber after oscillation is finished, and drying the activated carbon fiber at 60-80 ℃ to prepare the activated carbon fiber/graphene tube composite material; the pipe diameter of the graphene pipe is 10nm-50nm, and the specific surface area of the activated carbon fiber/graphene pipe composite material reaches 1200-1500m2/g。
2. The preparation method of the activated carbon fiber/graphene tube composite material according to claim 1, wherein: the diluted graphene oxide solution obtained in the step 1 has the concentration of 3-8mg/mL, the ultrasonic frequency of 100KHz and the power of 800W, and the ultrasonic time of the graphene oxide solution is 4-8 h.
3. The preparation method of the activated carbon fiber/graphene tube composite material according to claim 1, wherein: the amount of the activated carbon fiber is 5-8g, the activated carbon fiber is soaked in concentrated nitric acid for ultrasonic treatment for 3-5h, the ultrasonic frequency is 40KHz, the power is 400W, and the activated carbon fiber treated by the concentrated nitric acid is washed by deionized water until the pH value is 6-6.5.
4. The preparation method of the activated carbon fiber/graphene tube composite material according to claim 1, wherein: and dipping the activated carbon fiber obtained by pretreatment in a graphene oxide solution, and performing ultrasonic treatment or oscillation for 4-5h at 35-40 ℃.
5. The preparation method of the activated carbon fiber/graphene tube composite material according to claim 1, wherein: and dipping the activated carbon fiber obtained by the pretreatment in a graphene oxide solution and carrying out ultrasonic treatment, wherein the ultrasonic frequency is 40-50KHz, and the power is 400W.
6. The preparation method of the activated carbon fiber/graphene tube composite material according to claim 1, wherein: and the activated carbon fiber obtained by pretreatment is immersed in the graphene oxide solution and oscillated at the oscillation speed of 70-80 r/min.
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