CN116622368B - Blue fluorescent carbon dot with waste wind power blade fiber powder as carbon source, and preparation method and application thereof - Google Patents

Blue fluorescent carbon dot with waste wind power blade fiber powder as carbon source, and preparation method and application thereof Download PDF

Info

Publication number
CN116622368B
CN116622368B CN202310480387.4A CN202310480387A CN116622368B CN 116622368 B CN116622368 B CN 116622368B CN 202310480387 A CN202310480387 A CN 202310480387A CN 116622368 B CN116622368 B CN 116622368B
Authority
CN
China
Prior art keywords
wind power
waste
fiber powder
power blade
waste wind
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202310480387.4A
Other languages
Chinese (zh)
Other versions
CN116622368A (en
Inventor
王冬至
王聪伶
杨立琳
徐郡
王道备
赵蔚琳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Jinan
Original Assignee
University of Jinan
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Jinan filed Critical University of Jinan
Priority to CN202310480387.4A priority Critical patent/CN116622368B/en
Publication of CN116622368A publication Critical patent/CN116622368A/en
Application granted granted Critical
Publication of CN116622368B publication Critical patent/CN116622368B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • B01J35/39—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/40—Organic compounds containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

Abstract

The invention relates to the technical field of solid waste material recycling, in particular to a blue fluorescent carbon dot taking waste wind power blade fiber powder as a carbon source, a preparation method and application thereof. Screening and washing the waste wind power blades to prepare waste fibers, drying and further crushing to prepare waste wind power blade fiber powder; (2) Adding waste wind power blade fiber powder into a solvent which is one or more mixed solutions in DMAC, DEAC, DEF, DEP, DMF, uniformly mixing, putting into a reactor, heating, naturally cooling, and centrifuging to remove agglomerated precipitate; filtering the supernatant, and dialyzing with a dialysis bag; freeze drying to obtain carbon dot powder. The method for synthesizing the blue carbon dots by adopting the hydrothermal method is simple to operate, the waste wind power blade regenerated fiber powder is used as a carbon source, the waste is recycled, the carbon source is provided, the self doping of N and Si elements can be realized, and the fluorescence performance and the yield of the carbon dots are improved; and carbon dots can realize dye degradation.

Description

Blue fluorescent carbon dot with waste wind power blade fiber powder as carbon source, and preparation method and application thereof
Technical Field
The invention relates to the technical field of solid waste material recycling, in particular to a blue fluorescent carbon dot taking waste wind power blade fiber powder as a carbon source, a preparation method and application thereof.
Background
The wind energy is used as clean, safe and renewable green clean energy, greatly contributes to the development of energy industry in China, and promotes the sustainable development of human society. However, wind turbine blades, which are the most important core components in wind turbines, age gradually as they operate for a long period of time. The service life of the wind power blade is generally 20 years, and when the service life of the blade reaches the service life, the blade is retired and becomes waste for treatment. The common treatment methods are landfill, incineration and recycling. Because landfill and incineration methods are easy to cause environmental and pollution and are unfavorable for popularization and application, recycling becomes a main discussion method for scientists.
The carbon dots are spherical fluorescent nanoclusters with a diameter of less than 10nm and composed of carbon as a skeleton. The outstanding advantages of the carbon dots include good biocompatibility, low toxicity, unique photoinduced electron transfer characteristic, tunable fluorescence characteristic and the like, and the carbon dots are widely applied to the fields of chemical/fluorescence sensing, biological imaging, biomedicine, super capacitors, photocatalysis and the like.
At present, carbon point research has been advanced to some extent, but there is still a great room for improvement: (1) The manufacturing cost of raw materials is high, particularly in the selection of carbon sources, carbon is a main source of carbon points, and the higher the content of the carbon points in the carbon sources is, the stronger the fluorescence performance is; (2) Doping of heteroatoms such as nitrogen and silicon is also beneficial to improving the fluorescence performance of carbon dots, and how to realize doping efficiently is a problem to be solved; (3) The existing carbon dot preparation process is complex, and the yield of carbon dot products is low; the carbon dot obtained in (4) is unstable in performance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the blue fluorescent carbon dots (B-CDs) taking the waste wind power blade fiber powder as the carbon source and the preparation method thereof, the blue carbon dots are synthesized by adopting a hydrothermal method, the operation is simple, the waste is recycled by taking the waste wind power blade regenerated fiber powder as the carbon source, the carbon source is provided, the self doping of N and Si elements can be realized, the fluorescent performance and the yield of the carbon dots are improved, and the performance is good.
On the one hand, the invention provides a blue fluorescent carbon dot taking waste wind power blade fiber powder as a carbon source and a preparation method thereof, and the blue fluorescent carbon dot comprises the following steps:
(1) The preparation process of the waste wind power blade fiber powder comprises the following steps: screening and washing the waste wind power blades to prepare waste fibers, drying, and further crushing to prepare waste wind power blade fiber powder;
(2) The preparation process of the blue fluorescent carbon dots comprises the following steps: adding waste wind power blade fiber powder into a solvent, wherein the solvent is one, two, three, four or five mixed solutions of DMAC (dimethylacetamide), DEAC (diethylene glycol diethyl ether acetate), DEF (N, N-diethyl formamide), DEP (diethyl phthalate) and DMF (N, N-dimethyl formamide), uniformly mixing by ultrasonic, putting into a reactor, heating, naturally cooling, and centrifuging to remove agglomerated precipitate; filtering the supernatant, and dialyzing the obtained liquid by a dialysis bag; freeze drying to obtain carbon dot powder.
According to the scheme, the preparation process of the waste wind power blade fiber powder is as follows: cutting, crushing, screening and washing the waste wind power blades to obtain waste fibers with the diameter of 7-12 mu m and the length of 0.5-5 cm, drying the waste fibers in an oven at the temperature of 80-100 ℃, and crushing the waste fibers by a universal crusher to obtain regenerated fiber powder with the granularity of 80+/-10 mu m.
According to the scheme, the consumption of the waste wind power blade fiber powder in the step (2) is 0.3 g-0.5 g, and the solvent is 20 ml-34 ml.
According to a further improvement of the scheme, the ultrasonic condition in the step (2) is that ultrasonic vibration is carried out for 30-40 min at 20+/-2 ℃; the heating condition is that the oven is heated for 7 to 8 hours at 180 to 200 ℃.
In a further development of the solution, in step (2), the supernatant is filtered with a filter paper, the filter paper being a 0.22 μm filter paper; the dialysis conditions of the dialysis bag are 1000Da MWCO dialysis bag for dialysis for 20-24 hours; the freeze drying time is 20-24 hours.
According to a further improvement of the scheme, the blue fluorescent carbon dot size obtained in the step (2) is 2-7nm.
Further improvement of the scheme, the preparation technology of the blue fluorescent carbon dots comprises the following steps: adopting a one-step hydrothermal method to synthesize, adding 0.3 g-0.5 g of waste wind power blade fiber powder into 20 ml-34 ml of solution, uniformly mixing one, two, three, four or five of DMAC, DEAC, DEF, DEP, DMF solvent solutions by ultrasonic vibration at 20+/-2 ℃ for 30-40 min, then placing into a reactor with 50ml of PTFE lining, and heating for 7-8 h at 180-200 ℃ in an oven; naturally cooling the sample to 25+/-5 ℃, and centrifuging at a speed of 8000 revolutions per minute for 10-15 minutes to remove agglomerated sediment; filtering the supernatant with 0.22 μm filter to remove larger insoluble substances; dialyzing the obtained liquid for 20-24 hours by using a 1000Da MWCO dialysis bag to remove tiny particles for further purification; after freeze drying for 20-24 hours, the carbon dots are blue fluorescence, and the fluorescence quantum yield is 29-35%.
Preferably, the blue fluorescent carbon dot preparation process comprises the following steps of adopting a one-step hydrothermal method to synthesize, adding 0.3g of waste wind power blade fiber powder into 20ml of DMF solution, carrying out ultrasonic vibration at 20+/-2 ℃ for 30min to uniformly mix, then placing into a 50ml reactor with a PTFE lining, and heating for 8h in a 180 oven; naturally cooling the sample to 25+/-5 ℃, and centrifuging at 8000 rpm for 10 minutes to remove agglomerated sediment; then filtering the supernatant with 0.22 μm filter paper to remove larger insoluble substances; the obtained liquid is dialyzed for 24 hours by a 1000Da MWCO dialysis bag to remove tiny particles for further purification; after 24 hours of lyophilization, approximately 0.12g of carbon dot powder was obtained, which was blue fluorescent.
The invention provides a blue fluorescent carbon dot obtained by a preparation method of the blue fluorescent carbon dot with the waste wind power blade fiber powder as a carbon source.
On the other hand, the invention provides an application of the blue fluorescent carbon dots obtained by the preparation method of the blue fluorescent carbon dots with the waste wind power blade fiber powder as a carbon source in photocatalytic degradation.
The invention has the beneficial effects that:
(1) The waste wind power blade regenerated fiber powder is used as a carbon source, so that the waste is recycled, the environment is protected, and the cost is reduced. The waste wind power blade mainly comprises a metal structure wrapped by epoxy resin and glass fiber, the chemical components of the waste wind power blade contain C, O, N, si, ca and other metal elements, and the chemical structure of the waste wind power blade contains O-H, N-H, C-N, C-O, si-O and other functional groups, so that the waste wind power blade is used as a precursor, a carbon source is provided, N and Si element self-doping can be realized, carbon is a main source of carbon points, and the higher the carbon point content in the carbon source is, the stronger the fluorescence performance is; the doping of hetero atoms such as nitrogen and silicon is also beneficial to improving the fluorescence performance of carbon dots. The method for preparing the carbon dots by utilizing the waste wind power blades can solve the recycling problem of the waste wind power blades, is beneficial to the application of solid waste and environmental protection, has low-cost and easily-obtained raw materials, reduces the production cost and has important value for recycling the waste wind power blades.
(2) The blue fluorescent carbon dots are synthesized by adopting a one-step hydrothermal method, the operation is simple, the reaction conditions are mild, the environment is friendly, the large-scale popularization and conversion are easy, the fluorescent quantum yield is high and can reach 29-35%, and the problems of low fluorescent quantum yield and complex preparation in the prior art are solved.
(3) The prepared carbon dot fluorescent property has high stability, small size and uniformity, and can effectively degrade dye by photocatalysis, and the degradation efficiency of MB in 40min reaches 64%.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 shows a Transmission Electron Microscope (TEM) image of blue carbon dots (B-CDs) at (a) 20nm and (B) 10nm and (c) diameter distribution in example 10 (1) of the present invention.
FIG. 2 is an infrared spectrum (FT-IR) of B-CDs and waste wind blade fiber powder (WFs) in example 10 (2) of the present invention.
FIG. 3 shows the ultraviolet-visible absorption spectrum (a) and the fluorescence emission spectrum (B) of B-CDs in example 10 (3) of the present invention.
FIG. 4 is a digital photograph (c) of the catalytic degradation of MB dye by B-CDs (a), pseudo first order kinetic rate curve (B), and the catalytic degradation of MB dye in example 10 (4) of the present invention.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the above.
The waste wind power blade fiber powder is from Tianjin Longbao energy-saving technology Co. The organic dye Methylene Blue (MB) was from the Tianjin metallocene chemical reagent plant. N, N-Dimethylformamide (DMF), edetate disodium (Na 2 EDTA), benzoquinone (PBQ) and dimethyl sulfoxide (DMSO), dimethylacetamide (DMAC), diethylene glycol Diethyl Ether Acetate (DEAC), N-Diethylformamide (DEF), diethyl phthalate (DEP), dialysis bags (1000 Da) were purchased from Shanghai Ala Biochemical technologies Co., ltd.
Example 1:
a preparation method of blue fluorescent carbon dots by taking waste wind power blade fiber powder as a carbon source comprises the following steps:
the preparation process of the waste wind power blade fiber powder comprises the following steps: cutting, crushing, screening and washing the waste wind power blades to obtain waste fibers with the diameter of 7-12 mu m and the length of 0.5-5 cm, drying the waste fibers in an oven at the temperature of 80-100 ℃, and crushing the waste fibers by a universal crusher to obtain regenerated fiber powder with the granularity of 80+/-10 mu m.
The preparation process of the blue fluorescent carbon dots comprises the following steps: adopting a one-step hydrothermal method to synthesize, adding 0.3g of waste wind power blade fiber powder into 20ml of DMF solution, carrying out ultrasonic vibration at 20+/-2 ℃ for 30min to uniformly mix, then putting into a 50ml reactor with PTFE lining, and heating for 8h in a 180 oven; naturally cooling the sample to 25+/-5 ℃, and centrifuging at 8000 rpm for 10 minutes to remove agglomerated sediment; then filtering the supernatant with 0.22 μm filter paper to remove larger insoluble substances; the obtained liquid is dialyzed for 24 hours by a 1000Da MWCO dialysis bag to remove tiny particles for further purification; after 24 hours of lyophilization, approximately 0.12g of carbon dot powder was obtained, which was blue fluorescent. The fluorescence quantum yield was 29.9%.
Example 2
The difference from example 1 is that the waste wind blade fiber powder preparation process is as follows: cutting, crushing, screening and washing the waste wind power blades to obtain waste fibers with the diameter of 7-12 mu m and the length of 0.5-5 cm, drying the waste fibers in an oven at the temperature of 80-100 ℃, and crushing the waste fibers by a universal crusher to obtain regenerated fiber powder with the granularity of 80+/-10 mu m.
The preparation process of the blue fluorescent carbon dots comprises the following steps: adopting a one-step hydrothermal method to synthesize, adding 0.5g of waste wind power blade fiber powder into 34ml of DMF solution, carrying out ultrasonic vibration at 20+/-2 ℃ for 40min to uniformly mix, then putting into a 50ml reactor with a PTFE lining, and heating for 8h in a 200 oven; naturally cooling the sample to 25+/-5 ℃, and centrifuging at 8000 rpm for 10 minutes to remove agglomerated sediment; then filtering the supernatant with 0.22 μm filter paper to remove larger insoluble substances; the obtained liquid is dialyzed for 24 hours by a 1000Da MWCO dialysis bag to remove tiny particles for further purification; after 24 hours of freeze drying, blue fluorescence of the carbon dots was obtained. The fluorescence quantum yield was 27.1%.
Example 3
The difference from example 1 is that the waste wind blade fiber powder preparation process is as follows: cutting, crushing, screening and washing the waste wind power blades to obtain waste fibers with the diameter of 7-12 mu m and the length of 0.5-5 cm, drying the waste fibers in a baking oven at the temperature of 90 ℃, and crushing the waste fibers by a universal crusher to obtain regenerated fiber powder with the granularity of 80+/-10 mu m.
The preparation process of the blue fluorescent carbon dots comprises the following steps: adopting a one-step hydrothermal method to synthesize, adding 0.4g of waste wind power blade fiber powder into 30ml of DMF solution, carrying out ultrasonic vibration at 20+/-2 ℃ for 35min to uniformly mix, then putting into a 50ml reactor with PTFE lining, and heating for 7.5h in a 190 oven; naturally cooling the sample to 25+/-5 ℃, and centrifuging at 8000 rpm for 10 minutes to remove agglomerated sediment; then filtering the supernatant with 0.22 μm filter paper to remove larger insoluble substances; the obtained liquid is dialyzed for 22 hours by a 1000Da MWCO dialysis bag to remove tiny particles for further purification; after freeze-drying for 22 hours, blue fluorescence of the carbon dots was obtained. The fluorescence quantum yield was 30.8%.
Example 4
The difference from example 1 is that the solvent is DMAC. The fluorescence quantum yield was 35%.
Example 5
The difference from example 1 is that the solvent is DEAC. The fluorescence quantum yield was 32.2%.
Example 6
The difference from example 1 is that the solvent is DEF. The fluorescence quantum yield was 25.1%.
Example 7
The difference from example 1 is that the solvent is DEP. The fluorescence quantum yield was 28.1%.
Example 8
The difference from example 1 is that the solvent is 20ml of DMAC, DEAC, DEF, DEP, DMF five mixed solutions and the volume ratio is 1:1:1:1:1. The fluorescence quantum yield was 33.1%.
Example 9
The difference from example 1 is that the solvent is 34ml of DMAC, DEAC, DEF, DEP, DMF five mixed solutions and the volume ratio is 1:1:1:1:1. The fluorescence quantum yield was 32.7%.
Example 10: performance testing
The test was performed with the blue fluorescent carbon dots obtained in example 1.
(1) Morphological characterization
The morphology and size of the blue fluorescent carbon dots were observed by transmission electron microscopy, and as shown in fig. 1 (a, b), the shape of the blue fluorescent carbon dots was nearly spherical. FIG. 1 (c) shows a size distribution of B-CDs diameters, which shows that the average diameter of B-CDs is 5.2nm by Gaussian fitting. Meanwhile, the distribution of B-CDs is relatively uniform, and no aggregation phenomenon is observed.
(2) Chemical characterization
The functional groups of the waste wind blade fiber powder (WFs, lower curve) and blue carbon dots (B-CDs, upper curve) as measured by FT-IR spectroscopy are shown in FIG. 2. As is evident from FT-IR spectra of WFs, WFs have C-O, C =O, -CH 3 And N-H bonds. This suggests that WFs can not only provide a carbon source for the preparation of B-CDs, but can also enhance the fluorescent properties of B-CDs by providing N elements. As can be seen from the spectral curve of B-CDs, the O-H and N-H groups with rich surfaces are positioned at 3500cm -1 Left and right regions having a broad absorption peak; the carbon groups may also be via CH 3 (2930cm -1 )、C＝O(1740cm -1 )、-CH 2 (1450cm -1 )、C-N(1280cm -1 ) And C-O (1130 cm) -1 ) Is observed. These indicate that B-CDs contain hydrophilic groups that are more hydrophilic. Furthermore, 963cm -1 The peak at which corresponds to the presence of Si-O bonds indicates that Si atoms have been co-present in the B-CDs.
(3) B-CDs optical characterization
The optical properties of B-CDs are understood primarily by analysis of the UV-vis absorption spectrum, excitation wavelength dependence. The uv-vis absorption spectrum is shown in fig. 3 (a), where B-CDs have significant light absorption in the uv region (230-285 nm) with some shoulders, achieved by pi-pi transitions of c=c bonds or c=o bonds.
The inset in FIG. 3 (a) shows a photograph of B-CDs under daylight and ultraviolet light, which appear brown under daylight (left) and fluoresce blue under illumination by 365nm ultraviolet light (right). Notably, the quantum yield of B-CDs calculated according to equation (1) was 29.9%. The B-CDs have relatively high quantum yields, which are mainly caused by the high C content of WF and N/Si self-doping.
1. Mu.g/mL quinine sulfate solution (dissolved in 0.1mol/L sulfuric acid) was selected as a reference solution, and the light absorption and fluorescence intensity of the solution at 360nm were measured, and the fluorescence quantum yield of B-CDs was calculated from the following formula (1):
wherein Q is the quantum yield (Q S =0.54), where ζ is the integrated area of the emission peak, a is the ultraviolet absorption, η represents the refractive index (both are 1.33), and subscript S represents the reference solution. To reduce the errors, the UV absorption at 360nm should be less than 0.05.
The dependence of the fluorescence emission spectrum of B-CDs on the excitation wavelength can be explained by the curve in FIG. 3 (B). The maximum position of the emission wavelength gradually shifts red with the increase of the excitation wavelength and the corresponding fluorescence intensity, and the intensity tends to be increased and then decreased. The optimal emission wavelength is 463nm, with a corresponding excitation wavelength of 380nm.
(4) Photocatalytic degradation characterization
The photocatalytic performance of B-CDs catalysts was tested for degradation of detrimental MB dyes under dark and sunlight conditions. The specific process is to add 0.1mg of B-CDs catalyst to 3ml of 30mg/L model pollutant water solution. The mixed solution was stirred in the dark for 10min, and adsorption-desorption equilibrium was established. In the next step, the samples were exposed to direct sunlight and 3ml samples were extracted every 5min for detection to determine degradation efficiency.
The photocatalytic properties of B-CDs as assessed by MB dyes are shown in FIG. 4, wherein C 0 And C is the dye concentration for the initial reaction time and for a time, C/C 0 The concentration ratio of the reaction time t to the reaction time 0 represents the degradation efficiency. C/C 0 The smaller the ratio, the lower the MB dye concentration, the higher the degradation efficiency. In fig. 4 (a), the upper curve shows the results of degradation of blank MB over time under sustainable sunlight. It can be seen that MB did not degrade after 40 minutes of continuous irradiation, indicating that MB has strong photostability. B-CDs were added as catalyst to the MB dye solution to give the middle and bottom curves in fig. 4. The middle and bottom curves are the degradation effects of MB solutions in darkness and sunlight, respectively. Can be used forAs can be seen, the middle curve C/C 0 The degradation rate of (2) was changed by only 4.8% in 40 minutes, so that B-CDs had little effect on MB degradation in the dark. And the sunlight irradiation causes remarkable effect, and the synchronous degradation efficiency reaches 64%.
Based on the degradation data in FIG. 4 (a), according to the pseudo first order kinetic equation ln (C 0 Per C) =kt, plotting ln (C 0 The graph of the reaction time versus the reaction time is shown in FIG. 4 (b). Here, k is the extinction coefficient constant, R 2 Is the degree of fit. R is R 2 The closer to 1, the better the fit, indicating ln (C 0 and/C) has a good linear relationship with the reaction time. In order to verify the reliability and accuracy of the experiment, the experiment was repeated three times, consistent results were obtained, and good stability of the B-CDs as a photocatalyst was verified. In addition, FIG. 4 (c) is a digital photograph showing the degradation process of MB dye solution by B-CDs in darkness and sunlight, recording the effect of sunlight on MB dye solution. It was found that the color of the solution did not change significantly in the dark (left panel) and became progressively lighter in the sun (right panel) until reaching almost transparent after 40 minutes, indicating a progressive decrease in the concentration of MB.
Although the present invention has been described in detail by way of preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications and substitutions may be made in the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and it is intended that all such modifications and substitutions be within the scope of the present invention/be within the scope of the present invention as defined by the appended claims. Therefore, the protection scope of the invention is subject to the protection scope of the claims.

Claims (10)

1. The preparation method of the blue fluorescent carbon dots by taking waste wind power blade fiber powder as a carbon source is characterized by comprising the following steps of:
(1) The preparation process of the waste wind power blade fiber powder comprises the following steps: cutting, crushing, pulverizing, screening and washing the waste wind power blades to prepare waste fibers, and further pulverizing the dried waste wind power blades to prepare waste wind power blade fiber powder;
(2) The preparation process of the blue fluorescent carbon dots comprises the following steps: the method comprises the steps of adopting a one-step solvothermal method to synthesize, adding waste wind power blade fiber powder into a solvent, wherein the solvent is one or more mixed solutions of dimethylacetamide, diethylene glycol diethyl ether acetate, N-diethyl formamide, diethyl phthalate and N, N-dimethyl formamide, putting the mixed solutions into a reactor after ultrasonic uniform mixing, heating, naturally cooling, and centrifuging to remove agglomerated precipitates; filtering the supernatant, and dialyzing the obtained liquid by a dialysis bag; freeze drying to obtain carbon dot powder;
the waste wind power blade mainly comprises a metal structure wrapped by epoxy resin and glass fiber, and the chemical components of the waste wind power blade comprise C, O, N, si and Ca elements;
the heating condition is that the heating is carried out for 7-8 hours at 180-200 ℃.
2. The method for preparing blue fluorescent carbon dots by taking waste wind power blade fiber powder as a carbon source, which is characterized by comprising the following steps of: cutting, crushing, screening and washing the waste wind power blades to prepare waste fibers with the diameter of 7-12 mu m and the length of 0.5-5 cm, drying the waste fibers in an oven at the temperature of 80-100 ℃, and crushing the waste fibers by a universal crusher to prepare waste wind power blade regenerated fiber powder with the granularity of 80+/-10 mu m.
3. The method for preparing blue fluorescent carbon dots by taking waste wind power blade fiber powder as a carbon source, which is characterized by comprising the following steps of: in the step (2), the consumption of the waste wind power blade fiber powder is 0.3-g-0.5 g, and the solvent is 20-34 ml.
4. The method for preparing blue fluorescent carbon dots by taking waste wind power blade fiber powder as a carbon source, which is characterized by comprising the following steps of: the ultrasonic condition in the step (2) is that ultrasonic vibration is carried out for 30-40 min at 20+/-2 ℃; the heating condition is that the oven is heated for 7-8 hours at 180-200 ℃.
5. The method for preparing blue fluorescent carbon dots by taking waste wind power blade fiber powder as a carbon source, which is characterized by comprising the following steps of: filtering the supernatant with a filter paper in the step (2), wherein the filter paper is 0.22 mu m filter paper; the dialysis conditions of the dialysis bag are 1000Da MWCO dialysis bag for dialysis for 20-24 hours; the freeze drying time is 20-24 hours.
6. The method for preparing blue fluorescent carbon dots by taking waste wind power blade fiber powder as a carbon source, which is characterized by comprising the following steps of: and (3) obtaining the blue fluorescent carbon dot size of 2-7nm in the step (2).
7. The method for preparing the blue fluorescent carbon dots by taking the waste wind power blade fiber powder as a carbon source, which is characterized by comprising the following steps of: adopting a one-step solvothermal method to synthesize, adding 20 ml-34 ml of solution into 0.3-g-0.5 g of waste wind power blade fiber powder, wherein the solvent is one or more mixed solutions of dimethylacetamide, diethylene glycol diethyl ether acetate, N-diethyl formamide, diethyl phthalate and N, N-dimethylformamide, carrying out ultrasonic vibration for 30-40 min at 20+/-2 ℃ to uniformly mix, then placing into a reactor with 50ml of PTFE lining, and heating for 7-8 h in an oven at 180-200 ℃; naturally cooling the sample to 25+/-5 ℃, and centrifuging at a speed of 8000 revolutions per minute for 10-15 minutes to remove agglomerated sediment; filtering the supernatant with 0.22 μm filter to remove larger insoluble substances; dialyzing the obtained liquid for 20-24 hours by using a 1000Da MWCO dialysis bag to remove tiny particles for further purification; after freeze drying for 20-24 hours, the carbon dots are blue fluorescence, and the fluorescence quantum yield is 29-35%.
8. The method for preparing the blue fluorescent carbon dots by taking the waste wind power blade fiber powder as a carbon source, which is characterized by comprising the following steps of: synthesizing by adopting a one-step solvothermal method, adding 20ml of N, N-dimethylformamide solution into 0.3-g waste wind power blade fiber powder, uniformly mixing the mixture by ultrasonic vibration for 30min at 20+/-2 ℃, then placing the mixture into a 50ml reactor with a PTFE lining, and heating the mixture for 8h in a 180 oven; naturally cooling the sample to 25+/-5 ℃, and centrifuging at a speed of 8000 revolutions per minute for 10 minutes to remove agglomerated sediment; then filtering the supernatant with 0.22 μm filter paper to remove larger insoluble substances; the obtained liquid is dialyzed for 24 hours by a 1000Da MWCO dialysis bag to remove tiny particles for further purification; after 24 hours of freeze-drying, a carbon dot powder was obtained, which was blue fluorescent.
9. A blue fluorescent carbon dot obtainable by the method according to any one of claims 1 to 8.
10. Use of a blue fluorescent carbon dot obtained according to the method of any one of claims 1-8 in photocatalytic degradation of methylene blue dye.
CN202310480387.4A 2023-04-28 2023-04-28 Blue fluorescent carbon dot with waste wind power blade fiber powder as carbon source, and preparation method and application thereof Active CN116622368B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310480387.4A CN116622368B (en) 2023-04-28 2023-04-28 Blue fluorescent carbon dot with waste wind power blade fiber powder as carbon source, and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310480387.4A CN116622368B (en) 2023-04-28 2023-04-28 Blue fluorescent carbon dot with waste wind power blade fiber powder as carbon source, and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN116622368A CN116622368A (en) 2023-08-22
CN116622368B true CN116622368B (en) 2024-04-16

Family

ID=87640874

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310480387.4A Active CN116622368B (en) 2023-04-28 2023-04-28 Blue fluorescent carbon dot with waste wind power blade fiber powder as carbon source, and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN116622368B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108659836A (en) * 2018-07-23 2018-10-16 辽宁大学 A kind of high quantum production rate nitrogen sulphur codope fluorescent carbon point and its preparation method and application
CN110938430A (en) * 2019-07-01 2020-03-31 北部湾大学 Silicon and nitrogen co-doped carbon quantum dot and preparation method and application thereof
CN115465867A (en) * 2022-11-14 2022-12-13 国能龙源环保有限公司 Method for preparing white carbon black by utilizing waste wind power blades
CN115780467A (en) * 2022-10-26 2023-03-14 华能阜新风力发电有限责任公司 Method for recovering glass fiber and carbon powder from waste wind power blades

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108659836A (en) * 2018-07-23 2018-10-16 辽宁大学 A kind of high quantum production rate nitrogen sulphur codope fluorescent carbon point and its preparation method and application
CN110938430A (en) * 2019-07-01 2020-03-31 北部湾大学 Silicon and nitrogen co-doped carbon quantum dot and preparation method and application thereof
CN115780467A (en) * 2022-10-26 2023-03-14 华能阜新风力发电有限责任公司 Method for recovering glass fiber and carbon powder from waste wind power blades
CN115465867A (en) * 2022-11-14 2022-12-13 国能龙源环保有限公司 Method for preparing white carbon black by utilizing waste wind power blades

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Sustainable production of nitrogen-doped carbon quantum dots for photocatalytic degradation of methylene blue and malachite green;Umairah Abd Rani et al.;Journal of Water Process Engineering;20201206;第40卷;第101816页 *
玉米秸秆粉水热炭化制备碳量子点及其光催化性能研究;刘彩云等;四川化工;20191231;第22卷(第4期);第1-5页 *

Also Published As

Publication number Publication date
CN116622368A (en) 2023-08-22

Similar Documents

Publication Publication Date Title
CN113908872B (en) Double-vacancy graphite-phase carbon nitride photocatalyst and preparation method thereof
CN113148979B (en) Method for preparing carbon dots with different colors under same wavelength by using tobacco waste and application
CN103342347A (en) Preparation method of carbon quantum dots with high fluorescence property
CN109266340A (en) A kind of preparation method and applications of nitrogen-doped carbon quantum dot
CN102911664A (en) Fluorescent polymer dot, hydrothermal synthesis method through linear non-conjugated polymers and application thereof
CN112871195B (en) Multi-morphology carbon nitride synthesized by salt assistance, and preparation method and application thereof
CN101654397B (en) Method for catalyzing and reducing ethanol with carbon dioxide under visible light
CN111822055A (en) Preparation method and application of BiOBr/COF composite photocatalyst
CN111167501B (en) Visible light response photocatalytic material, preparation thereof and application thereof in micro-polluted water treatment
CN116622368B (en) Blue fluorescent carbon dot with waste wind power blade fiber powder as carbon source, and preparation method and application thereof
CN107722974B (en) Preparation method of biomass tar derived carbon quantum dots
CN115851271B (en) Preparation method of nitrogen-doped fluorescent carbon dots
CN109647510B (en) Polyion liquid modified cerium-doped nano-zinc oxide photocatalyst and preparation method and application thereof
CN111573763A (en) Black porous carbon loaded TiO2Nano-particles and preparation method and application thereof
CN111073638A (en) Method for preparing controllable photoluminescence carbon dots by changing temperature
CN106390991A (en) Preparation method and application of ultra-fine WO3 nanowire
CN113713798B (en) Preparation method of graphene quantum dot modified zinc oxide and application of degradation dye
Long et al. Synthesis of high-performance carbon dots from laurel leaves and their application in anti-counterfeit ink
CN111762774A (en) Method for preparing solid-phase carbon quantum dots by adopting biological collagen waste and application
CN110142055B (en) Microwave irradiation method for enhancing photocatalytic performance of graphite-phase carbon nitride
CN114849758B (en) Tin oxide/carbon quantum dot composite photocatalyst and preparation method and application thereof
CN106111115B (en) A kind of BiVO4Nanobelt high efficiency photocatalyst and its preparation method and application
CN116622365B (en) N/S co-doped quantum dot based on microcystis aeruginosa and application thereof in fluorescence quantitative detection of Cu < 2+ >
CN115845902B (en) Graphite-phase carbon nitride photocatalytic material and preparation method thereof
CN113265248B (en) Orange red fluorescent carbon dot and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant