CN110330091B - Magnetic biomass functional carbon fiber based on photo-Fenton catalysis and preparation method and application thereof - Google Patents

Magnetic biomass functional carbon fiber based on photo-Fenton catalysis and preparation method and application thereof Download PDF

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CN110330091B
CN110330091B CN201910446269.5A CN201910446269A CN110330091B CN 110330091 B CN110330091 B CN 110330091B CN 201910446269 A CN201910446269 A CN 201910446269A CN 110330091 B CN110330091 B CN 110330091B
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fiber
polydopamine
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CN110330091A (en
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胡进波
卢斌达
刘贡钢
薛志成
李婷
苌姗姗
李贤军
刘元
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Central South University of Forestry and Technology
Hunan Taohuajiang Bamboo Science and Technology Co Ltd
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Hunan Taohuajiang Bamboo Science and Technology Co Ltd
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Abstract

The invention discloses a method for preparing magnetic biomass functional carbon fibers based on photo-Fenton catalysis. The magnetic biomass functional carbon fiber prepared by the invention comprises carbon fiber, and ferroferric oxide nano particles and titanium dioxide nano particles loaded on the carbon fiber in situ, can be applied to photo-Fenton treatment of wastewater, and has the advantages of low raw material cost, simple preparation method, magnetic recovery in the wastewater treatment process, good treatment effect and the like.

Description

Magnetic biomass functional carbon fiber based on photo-Fenton catalysis and preparation method and application thereof
Technical Field
The invention relates to the field of carbon fiber materials, in particular to magnetic biomass functional carbon fiber based on photo-Fenton catalysis, and a preparation method and application thereof.
Background
The activated carbon fiber has the advantages of large contact area, high specific surface area, large adsorption capacity, high adsorption and desorption rate, heat resistance, acid and alkali resistance and the like, and is widely applied to the aspects of environmental purification, catalyst carriers, electrode materials and the like as a novel adsorption functional material. Carbon fiber as nano titanium dioxide photocatalystThe carrier is used for treating organic wastewater, so that the efficient adsorption synergistic effect of carbon fibers can be exerted, the photocatalytic degradation performance of titanium dioxide on organic pollutants is effectively improved, the problems of immobilization and loss of nano-scale titanium dioxide can be solved, and the carrier is widely applied to treating organic pollutant wastewater. However, the photocatalytic effect of the carbon fiber photocatalyst is limited by light source and catalytic efficiency, and the organic pollutant wastewater is difficult to be treated efficiently in a large scale. The photo-Fenton catalytic degradation technology combining photocatalysis and Fenton reaction has no secondary pollution and H in the treatment process2O2The dosage is reduced, the cost is reduced, and the toxic/difficultly degraded waste water can be efficiently degraded, so that the deep research is carried out. Therefore, designing the carbon fiber photo-Fenton catalyst with excellent catalytic degradation performance is very important for efficiently treating organic pollutants in wastewater. However, the preparation of the micron-sized activated carbon fiber photo-Fenton catalyst and the application of the micron-sized activated carbon fiber photo-Fenton catalyst in water treatment environment purification still have cost problems, and in the practical application process, the recovery operation of the micron-sized photo-Fenton catalyst can further increase the water treatment cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides the magnetic biomass functional carbon fiber prepared by taking the biomass material as the fiber raw material, has the advantages of low cost, simple preparation method and the like, has the functions of magnetic recovery and photo-Fenton catalysis, and can be applied to the treatment of wastewater.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of magnetic biomass functional carbon fibers based on photo-Fenton catalysis comprises the following steps:
s1, placing the biomass material in a strong alkaline solution for hydrothermal treatment to extract plant fibers, filtering and drying to obtain pretreated fibers;
s2, carbonizing the pretreated fiber to obtain carbonized fiber;
s3, placing the carbonized fiber in a dopamine solution, stirring for reaction, and drying to obtain a polydopamine-modified carbon fiber;
s4, polydopamine modified carbon fiber, Fe-containing3+The ferric salt, the pH regulator and the reducing agent are placed in water to be dispersed uniformly, then hydrothermal reaction is carried out, so that ferroferric oxide nano particles are loaded on the polydopamine modified carbon fiber in situ, and the magnetic carbon fiber is obtained after filtration and drying;
s5, placing the magnetic carbon fiber and titanium dioxide in a strong alkaline solution, mixing, carrying out hydrothermal reaction, loading titanium dioxide nanoparticles on the magnetic carbon fiber in situ, carrying out magnetic separation, washing and drying to obtain the magnetic biomass functional carbon fiber loaded with titanium dioxide.
As a further improvement to the above technical solution:
the step S4 specifically includes: the carbon fiber modified by polydopamine is placed in water to be dispersed evenly, and then Fe is added3+Uniformly dispersing the ferric salt, finally adding a pH regulator and a reducing agent, carrying out hydrothermal reaction at the temperature of 100-180 ℃ to enable the ferroferric oxide nanoparticles to be loaded on the carbon fiber in situ, and filtering and drying to obtain the magnetic carbon fiber.
In the step S4, the mass ratio of the polydopamine-modified carbon fiber to the iron salt is 1: 0.1-5, the pH regulator is sodium carbonate, and the reducing agent is ascorbic acid.
In the step S1, the biomass material is a fiber-containing plant-based biomass material and/or waste paper.
In the step S1, the concentration of the strong alkaline solution is 0.1-10 mol/L, and the temperature of the hydrothermal treatment is 160 ℃.
In the step S2, the carbonization temperature is 300-900 ℃ and the carbonization time is 1-3 h.
In the step S3, the concentration of the dopamine solution is 0.01-2 mg/mL, the pH value of the dopamine solution is 8-11, and the stirring reaction time is 0.5-12 h.
In the step S3, the drying temperature is 60 ℃.
In the step S5, the temperature of the hydrothermal reaction is 100-160 ℃, and the concentration of the strong alkaline solution is 5-12 mol/L.
As a general inventive concept, the invention also provides a magnetic biomass functional carbon fiber which is prepared according to the preparation method and comprises the carbon fiber, ferroferric oxide nanoparticles and titanium dioxide nanoparticles, wherein the ferroferric oxide nanoparticles and the titanium dioxide nanoparticles are loaded on the carbon fiber in situ.
The ferroferric oxide nanoparticles have the double functions of magnetic recovery and Fenton catalysis, and the titanium dioxide nanoparticles have the photocatalysis function.
As a general inventive concept, the invention also provides the application of the magnetic biomass functional carbon fiber prepared by the preparation method or the magnetic biomass functional carbon fiber in the photo-Fenton catalytic treatment of wastewater.
The application comprises the following steps: and (2) placing the magnetic biomass functional carbon fiber into a solution of wastewater and hydrogen peroxide, stirring under a dark condition until the solution reaches adsorption-desorption balance, and then placing under a light condition for photocatalytic degradation reaction.
Compared with the prior art, the invention has the advantages that:
according to the magnetic biomass functional carbon fiber based on photo-Fenton catalysis and the preparation method thereof, cheap biomass resources (especially waste biomass resources such as waste paper and plant-based waste biomass materials in the wood and bamboo processing industry are used as carbon fiber preparation raw materials) are used for preparing the magnetic biomass functional carbon fiber and are used as a photo-Fenton catalyst, so that the preparation cost is greatly reduced; the bionic material polydopamine is used for modifying carbon fibers, the surface chemical activity of the carbon fibers is improved by virtue of amino and phenolic hydroxyl high-activity functional groups of the polydopamine, ferroferric oxide nanoparticles and titanium dioxide nanoparticles are efficiently loaded, the magnetic ferroferric oxide nanoparticles are loaded, so that the recovery of a powder catalytic material can be realized by an external magnetic field, the purposes of recycling and simple recovery of the magnetic biomass functional carbon fibers are achieved, the manufacturing and using costs of the magnetic biomass functional carbon fibers are further reduced, and meanwhile, the ferroferric oxide nanoparticles are used as a Fenton catalyst to catalyze hydrogen peroxide to degrade to generate strong oxidizing radicals to degrade organic pollutants; and the load of the nano titanium dioxide endows the carbon fiber with photocatalytic degradation capability. Therefore, in the process of photocatalytic degradation of organic pollutants, the magnetic biomass functional carbon fiber can not only exert the synergistic effect of efficient adsorption-photocatalysis-Fenton catalysis of the carbon fiber photo-Fenton catalyst, effectively improve the degradation performance of the photo-Fenton catalyst on the organic pollutants, but also solve the problems of immobilization and loss of catalyst nanoparticles and recovery and reuse of micron carbon fibers.
Drawings
FIG. 1 is a process flow diagram of example 1 of the present invention.
FIG. 2 shows the catalytic degradation performance of the functional carbon fiber in example 1 of the present invention on methylene blue under different process conditions.
FIG. 3 is a photograph showing samples of waste paper, waste paper fibers and functional carbon fibers in example 1 of the present invention.
FIG. 4 is a scanning electron micrograph (a) and a mapping analysis of C, O, N, Fe, Ti elements (b, C, d, e, f) of the functional carbon fiber in example 1 of the present invention.
FIG. 5 is a scanning electron micrograph (a) and an EDS energy spectrum analysis chart (b) of the functional carbon fiber in example 1 of the present invention.
Detailed Description
The invention will be described in further detail below with reference to the drawings and specific examples. Unless otherwise specified, all materials and equipment used in the present application are commercially available.
Example 1
As shown in fig. 1, the preparation method of the magnetic biomass functional carbon fiber based on photo-fenton catalysis in the embodiment includes the following steps:
1. mechanically and ultrasonically crushing waste paper, putting the crushed paper into a sodium hydroxide solution with the concentration of 5 mol/L for hydrothermal treatment at 160 ℃ to extract plant fibers, wherein the hydrothermal time is 24 hours, and filtering, washing and drying the obtained fibrous solid matters to obtain the waste paper fibers. In the step, in other embodiments, the sodium hydroxide solution may be other strongly alkaline solutions, and the concentration of the sodium hydroxide solution is 0.1-10 mol/L, which can achieve the same or similar technical effects.
2. And putting the obtained pretreated waste paper fiber into a muffle furnace for high-temperature carbonization at the temperature rise rate of 5 ℃/min, the carbonization temperature of 500 ℃ and the carbonization time of 2h to obtain carbonized fiber. In other embodiments, the carbonization temperature is 300-900 ℃ and the carbonization time is 1-3 hours, which can achieve the same or similar technical effects.
3. Preparing 2mg/mL dopamine solution, taking 200mL dopamine solution, adding trihydroxymethyl aminomethane buffer solution or sodium hydroxide solution to adjust the pH value to about 8.5, placing 2g carbonized fiber in the buffer solution, stirring at normal temperature for 8h, and after the reaction is finished, drying at 60 ℃ to obtain the polydopamine modified carbon fiber. In other embodiments, the concentration of the dopamine solution is 0.01-2 mg/mL, the pH value is 8-11, and the stirring time is 0.5-12 h.
4. Adding 0.5g of polydopamine-modified carbon fiber into 35mL of distilled water, performing ultrasonic dispersion for 2min to obtain a mixed solution A, adding 1g of ferric chloride, performing ultrasonic dispersion for 30min to obtain a mixed solution B, adding 25mL of 0.6mol/L sodium carbonate, adjusting the pH value to 9, adding 0.18g of ascorbic acid as a reducing agent, performing hydrothermal reaction for 24h at 160 ℃, loading ferroferric oxide nanoparticles on the carbon fiber in situ, filtering and drying to obtain the magnetic carbon fiber. In other embodiments, the hydrothermal reaction temperature is 100-180 ℃, the mass ratio of the polydopamine modified carbon fiber to the ferric chloride is 1: 0.1-5, and the same or similar technical effects can be obtained.
5. 0.5g P25 type titanium dioxide and 1g of magnetic carbon fiber are placed in 60 mL of 10mol/L concentrated alkali solution (in the embodiment, the concentrated alkali solution is sodium hydroxide solution) to be mixed, hydrothermal reaction is carried out for 24h at 160 ℃, the in-situ loading of titanium dioxide nanoparticles on the surface of the carbon fiber is realized by utilizing the crystal structure dissociation and recombination processes of the P25 type titanium dioxide in the concentrated alkali solution, the magnetic biomass functional carbon fiber loaded with the titanium dioxide is separated by magnetic separation, and the magnetic biomass functional carbon fiber which can be applied to photo-Fenton catalytic treatment of wastewater is finally obtained after washing and drying. In other embodiments, the concentrated alkali solution may be other strong alkali solution, the concentration is 5-12 mol/L, the temperature of the hydrothermal reaction is 100-160 ℃, and the same or similar technical effects can be obtained.
The catalytic degradation performance of the prepared magnetic biomass functional carbon fiber is inspected by adopting three different process conditions, namely a conventional photocatalytic process, a Fenton catalytic process and a photocatalytic and Fenton combined catalytic process. The photocatalysis combined Fenton reaction process comprises the following specific steps: 0.1g of the prepared magnetic biomass functional carbon fiber is poured into a beaker containing 200mL of mixed solution of 10mg/L Methylene Blue (MB) and 0.1 mol/L hydrogen peroxide. The beaker was left to stir in the dark for 30min to bring the MB solution to equilibrium of adsorption-desorption. 5mL of the solution was placed in a sampling tube for magnetic separation, and the supernatant was tested for absorbance (Abs) and poured back into the beaker after completion of the test. And (3) turning on a xenon lamp source to start a photocatalytic degradation reaction, keeping the room temperature in the dark box at 25 ℃ in the reaction process, and keeping the magnetic stirrer in a stirring state. Taking 5mL of degradation liquid from the degradation pool every 20min of illumination, taking supernate after magnetic separation to test absorbance (Abs), and pouring the supernate back into the beaker after the test is complete.
By contrast, the same sampling and testing method was used to test the individual photocatalytic performance (no hydrogen peroxide, only light irradiation, i.e., photocatalytic process) and fenton catalytic performance (no light irradiation, only hydrogen peroxide, i.e., fenton catalytic process) of the magnetic biomass functional carbon fiber. FIG. 2 shows the performance of the prepared magnetic biomass functional carbon fiber in catalytic degradation of methylene blue under different process conditions. As can be seen from the figure, under the photo-Fenton process, the magnetic biomass functional carbon fiber has excellent catalytic degradation performance on methylene blue, and is far superior to a single photo-catalysis and Fenton catalysis process.
As shown in fig. 3, the waste paper is pretreated to obtain fibrous waste paper fibers, and after the processes of carbonization, polydopamine modification, ferroferric oxide and titanium dioxide nanoparticle loading and the like, the magnetic biomass functional carbon fibers with strong magnetism are obtained, the magnetic field recovery function can be realized, the waste paper fibers are white, and the magnetic biomass functional carbon fibers after carbonization and nanoparticle loading are black.
Fig. 4 is a scanning electron micrograph (a) of the functional carbon fiber and a mapping analysis chart of elements (b, C, d, e, f) of C, O, N, Fe, and Ti in example 1, and it can be seen from fig. 4 that the magnetic biomass functional carbon fiber retains a fibrous structure of the paper fiber, elements such as nitrogen, iron, and titanium are uniformly distributed on the surface of the carbon fiber, and nitrogen is derived from an amino group on the modified polydopamine, which indicates that the polydopamine successfully modifies the carbon fiber, and provides favorable conditions for uniform and firm loading of ferroferric oxide and titanium dioxide nanoparticles on the surface of the carbon fiber.
Fig. 5 is a scanning electron micrograph (a) and an EDS (EDS) energy spectrum analysis chart (b) of the magnetic biomass functional carbon fiber in example 1, which shows that the weight percentage of the iron element supported on the surface of the carbon fiber is 36.57% and the weight percentage of the titanium element is 0.65%. From the above, it can be concluded that the high loading of iron element on the surface of the carbon fiber benefits from the polydopamine high-activity functional group, while the loading of the magnetic ferroferric oxide nanoparticles is higher than that of the nano titanium dioxide photocatalyst, which may cause the loading of titanium dioxide to be smaller than that of the ferroferric oxide nanoparticles because the ferroferric oxide load occupies part of the active sites loaded on the surface of the carbon fiber.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments to equivalent variations, without departing from the scope of the invention, using the teachings disclosed above. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.

Claims (10)

1. A preparation method of magnetic biomass functional carbon fiber based on photo-Fenton catalysis is characterized by comprising the following steps: the method comprises the following steps:
s1, placing the biomass material in a strong alkaline solution for hydrothermal treatment to extract plant fibers, filtering and drying to obtain pretreated fibers;
s2, carbonizing the pretreated fiber to obtain carbonized fiber;
s3, placing the carbonized fiber in a dopamine solution, improving the surface chemical activity of the carbonized fiber by virtue of the high-activity functional groups of amino and phenolic hydroxyl of polydopamine, stirring for reaction, and drying to obtain the polydopamine-modified carbon fiber;
s4, polydopamine modified carbon fiber, Fe-containing3+The ferric salt, the pH regulator and the reducing agent are placed in water to be dispersed uniformly, then hydrothermal reaction is carried out, so that ferroferric oxide nano particles are loaded on the polydopamine modified carbon fiber in situ, and the magnetic carbon fiber is obtained after filtration and drying;
s5, placing the magnetic carbon fiber and titanium dioxide in a strong alkaline solution, mixing, carrying out hydrothermal reaction, loading titanium dioxide nanoparticles on the magnetic carbon fiber in situ, carrying out magnetic separation, washing and drying to obtain the magnetic biomass functional carbon fiber loaded with titanium dioxide.
2. The method of claim 1, wherein: the step S4 specifically includes: the carbon fiber modified by polydopamine is placed in water to be dispersed evenly, and then Fe is added3+Uniformly dispersing the ferric salt, finally adding a pH regulator and a reducing agent, carrying out hydrothermal reaction at the temperature of 100-180 ℃ to enable the ferroferric oxide nanoparticles to be loaded on the carbon fiber in situ, and filtering and drying to obtain the magnetic carbon fiber.
3. The method of claim 2, wherein: in the step S4, the mass ratio of the polydopamine-modified carbon fiber to the iron salt is 1: 0.1-5, the pH regulator is sodium carbonate, and the reducing agent is ascorbic acid.
4. The production method according to any one of claims 1 to 3, characterized in that: in the step S1, the biomass material is a fiber-containing plant-based biomass material and/or waste paper.
5. The method of claim 4, wherein: in the step S1, the concentration of the strong alkaline solution is 0.1-10 mol/L, and the temperature of the hydrothermal treatment is 160 ℃.
6. The production method according to any one of claims 1 to 3, characterized in that: in the step S2, the carbonization temperature is 300-900 ℃ and the carbonization time is 1-3 h.
7. The production method according to any one of claims 1 to 3, characterized in that: in the step S3, the concentration of the dopamine solution is 0.01-2 mg/mL, the pH value of the dopamine solution is 8-11, and the stirring reaction time is 0.5-12 h; in the step S3, the drying temperature is 60 ℃.
8. The production method according to any one of claims 1 to 3, characterized in that: in the step S5, the temperature of the hydrothermal reaction is 100-160 ℃, and the concentration of the strong alkaline solution is 5-12 mol/L.
9. A magnetic biomass functional carbon fiber based on photo-Fenton catalysis is characterized in that: the magnetic biomass functional carbon fiber is prepared according to the preparation method of any one of claims 1 to 8 and comprises a carbon fiber, ferroferric oxide nanoparticles and titanium dioxide nanoparticles, wherein the ferroferric oxide nanoparticles and the titanium dioxide nanoparticles are both loaded on the carbon fiber in situ.
10. Use of the magnetic biomass functional carbon fiber prepared according to the preparation method of any one of claims 1 to 8 or the magnetic biomass functional carbon fiber according to claim 9 for photo-fenton catalytic treatment of wastewater.
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