Electrospun PAN Nanofibers Research Articles

Electrospun polyacrylonitrile nanofiber composites integrated with Al-MOF/mesoporous carbon for superior CO2 capture and VOC removal

Electrospun PAN nanofiber composites with integrated Metal-Organic Frameworks (MOFs) and mesoporous carbon (MPC) offer an efficient solution for CO2 capture and hydrocarbon removal. In this study, we synthesized a series of NH2-MIL-101(Al)@MPC composites using a solvothermal method and incorporated them into PAN nanofibers via electrospinning. The composites were characterized by FTIR, XRD, FESEM, XPS, mechanical properties and TGA, showing enhanced surface area and pore structure. NH2-MIL-101(Al) exhibited a BET surface area of 933.14 m2/g, crucial for selective absorption. The PAN/MOF@MPC nanofibers demonstrated improved mechanical properties and achieved a CO2 uptake of 6.35 mmol g−1 at 298 K and 0.55 bar. Additionally, the modified nanofibers demonstrated excellent static and dynamic adsorption capacities for volatile organic compounds (VOCs) like acetone and benzene. This study highlights the synergistic effects of combining MOFs and MPCs within electrospun nanofibers, resulting in materials with enhanced adsorption efficiency and mechanical stability. The work presents a novel approach by integrating MOF@MPCs into electrospun PAN nanofibers, significantly enhancing CO2 capture and VOC removal. This innovative combination not only improves the adsorption performance but also advances the mechanical properties of the nanofibers, showcasing a new strategy for developing high-performance materials for environmental remediation. The results offer strong potential for real-world applications in air purification and carbon sequestration.

Electrospun Polyacrylonitrile (PAN) Derived One Dimensional Carbon Nanofibers for Na-Ion Batteries

The desire for high performance storage devices is driven by energy demand, security and sustainability. Metal oxide based nanomaterials have limitations of high cost, poor cycle life, low yeild and structural stability. In comparison, carbon materials exhibit porous structure, work well in a wide potential window, and are highly conductive. Hence, they show enhanced rate capability and cycle life. In this work, one dimensional (1D) carbon nanofibers are synthesized with the help of electrospun PAN nanofibers as precursors. These electrospun carbonaceous nanostructures can be employed as electrodes as well as substrates, leading to structural stability after cycling and increased electrode conductivity. The morphologies and structures of as-spun nanofibers were investigated in order to develop a fundamental understanding of the nucleation and growth mechanism of carbon nanofibers. These high surface area carbon nanofibers were used as anode material for sodium (Na)-ion batteries. The electrochemical performance was first optimized in a half cell configuration. These batteries can deliver a capacity of 300 mAh g-1 at 0.1 A g-1, with cycling stability of 82% for more than >500 cycles. Thus, these electrodes can become useful in batteries beyond lithium.

In Situ Synthesis of NH2-MIL-53-Al/PAN Nanofibers for Removal Co(II) through an Electrospinning Process.

In this study, researchers developed a novel composite material called NH2-MIL-53-Al/PAN, which consists of metal-organic frameworks (MOFs) grown on electrospun PAN nanofibers (NFs). The successful formation of the composite was confirmed by X-ray diffraction (XRD) and Fourier transform infrared (FTIR), and the hydrophilicity of NH2-MIL-53-Al/PAN was demonstrated by the water contact angle (WCA). Batch experiments were conducted to investigate the adsorption performance of Co(II) under different conditions. The maximum adsorption capacity reached 58.72 mg/g, and almost 95% of the adsorption was achieved within the first 6 h. The adsorption process was found to be spontaneous and endothermic and followed the pseudo-second-order kinetics and Langmuir models. Chemisorption and molecular layer adsorption are the main mechanisms of adsorption, and X-ray photoelectron spectroscopy (XPS) analysis further reveals that the interaction between the adsorbent and cobalt is a coordination interaction. In this study, NH2-MIL-53-Al was grown in situ on PAN to ensure effective loading of MOFs and prevent agglomeration during the NF mixing process. This approach successfully addressed the challenge of exposing active sites within the embedded MOF crystals. Additionally, it overcame the difficulty of recycling traditional MOF adsorbents. As a result, the exceptional performance of MOF NFs offers a promising solution for the efficient removal of cobalt-containing wastewater.

Growth of bimetallic Ni-Co MOFs on a skeleton of electrospun PAN nanofibers and coating on a thin film for SPME of amitriptyline and nortriptyline in urine and plasma samples

In this research, composited bimetallic organic framework-polyacrylonitrile (Ni-Co MOFs-PAN) was applied for thin-film solid phase microextraction (TF-SPME) of tricyclic antidepressant (TCA) drugs from biological samples. The separation and quantification of the analytes were accomplished by HPLC-UV. First, seeded nanofibers with organic ligands were electrospun on a sheet of foil. Then, with the uniform in-situ solvothermal growth of Ni-Co MOFs on the skeletal surface of nanofibers, the nanoparticles were successfully attached to the surfaces without effective bonds and produced a thin layer with a high flexibility, large active surface and abundant functional groups for adsorption. The characteristics of the produced nanocomposite were investigated by Fourier-transform infrared spectroscopy, field emission-scanning electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy and Brunauer-Emmett-Teller analysis. The stirring rate, pH, ionic strength, adsorption and desorption time along with type and volume of desorption solvents as influential factors on extraction efficiencies of the analytes, were optimized by one variable at a time method. Under optimized conditions, wide linear range for analytes in water and plasma matrices were obtained from 0.2 to 1000.0 μg L−1 and 1.0–1000.0 μg L−1, respectively, with R2 ≥ 0.9925. The limits of detection were in the range of 0.06–0.3 μg L−1 in different media. Good repeatability and reproducibility were attained within intra-day, inter-day and film-to-film RSDs% (n = 3) below 3.3 %, 3.9 % and 4.7 %, respectively. Since desirable relative recoveries were calculated between 91.4 % and 100.4 %. The method can be used for the successful extraction and measurement of amitriptyline and nortriptyline as its metabolite in different sampling time from urine and plasma matrices.

A green hydrothermal synthesis of polyacrylonitrile@carbon/MIL-101(Fe) composite nanofiber membrane for efficient selective removal of tetracycline

Developing highly efficient, low-cost and reusable adsorbents toward antibiotics is a great challenge for the treatment of wastewater. Here, a polyacrylonitrile@carbon/MIL-101(Fe) composite nanofiber membrane (PAN@C/MIL-101(Fe)) has been prepared for the first time via the combination of electrospinning technique and green hydrothermal method and showed a high adsorption performance toward tetracycline (TC). The MIL-101(Fe) nanocrystals were uniformly grown in-situ on the surface of activated hydrothermal carbon coated electrospun PAN nanofiber membrane. The incorporation of hydrothermal carbon and MIL-101(Fe) in nanofiber membrane obviously enhanced its adsorption ability. The adsorption process followed pseudo-second-order kinetic model and Freundlich isotherm model, with an adsorption capacity of 392.64 mg/g for TC. Moreover, the PAN@C/MIL-101(Fe) exhibited high selectivity and good regenerability, and the removal efficiency remained above 94% after five cycles. After the real wastewater filtration experiment, chemical oxygen demand (COD) concentration of TC significantly decreased from 155.55 mg/L to 51.84 mg/L, which is below the standard of wastewater discharge (GB 21904-2008). This study provides a promising green strategy for uniform MOFs modified carbon coating nanofiber membrane adsorbent, which has potential application in practical antibiotic wastewater treatment.

Electrospinning organic solvent resistant preoxidized poly(acrylonitrile) nanofiber membrane and its properties

A high performance O-PAN nanofiber with excellent solvent resistance, thermal stability and flexibility was fabricated. • O-PAN nanofiber membrane with excellent thermal stability and also flexibility was fabricated by the preoxidation of electrospun PAN nanofiber membrane. • In SiO 2 particle and DMAc suspension, O-PAN nanofiber membrane showed excellent organic solvent resistance and separation performance. • The O-PAN membrane after hydrophobic treatment showed excellent hydrophobicity and good oil/water separation performance. A high performance preoxidized poly(acrylonitrile) (O-PAN) nanofiber membrane with excellent solvent resistance, thermal stability and flexibility was fabricated by the preoxidation of electrospun PAN nanofiber membrane. The performance of resultant O-PAN nanofiber membrane was optimized by altering the PAN concentration and preoxidation temperature. The results showed that the O-PAN nanofiber membrane which made from PAN concentration of 14% (mass) and preoxidation temperature of 250.0 ℃ have a more optimal comprehensive performance. In the long-term separation test of SiO 2 particle (1 μm) in DMAc suspension, the permeate flux of O-PAN nanofiber membrane stabilized at 227.91 L·m −2 ·h −1 (25 ℃, 0.05 MPa) while the SiO 2 rejection above 99.6%, which showed excellent solvent resistance and separation performance. In order to further explore the application of the O-PAN nanofiber membrane, the O-PAN nanofiber membrane was treated with fluoride and used in oil/water separation process. The O-PAN nanofiber membrane after hydrophobic treatment showed excellent hydrophobicity and good oil/water separation performance with the permeate flux about 969.59 L·m −2 ·h −1 while the separation efficiency above 96.1%. The O-PAN nanofiber membrane exhibited a potential application prospect in harsh environment separation.

Novel F-doped carbon nanotube@(N,F)-co-doped TiO2-δ nanocomposite: Highly active visible-light-driven photocatalysts for water decontamination

The development of a facile strategy to prepared titanium oxide with reduced band gap, high electrical conductivity together with good chemical and structural stability that can be widely applied for photocatalysis under visible light holds great appeal. Herein, we reported a novel F-doped carbon nanotube@(N,F)-co-doped TiO2-δ nanocomposite, which was prepared simply by depositing titanium oxide onto electrospun PAN nanofibers containing NH4F via solvothermal synthesis, and the following thermal treatment process. The optimally synthesized nanocomposite shows outstanding photocatalytic performance by removing 77.2% of RhB, 84.1% of MB and 66.2% of Cr(VI) under visible light from a 5 W LED lamp within 60 min, which are approximately 33.6, 6.5 and 6.0 times those over the commercially available pure TiO2 powders, respectively. The greatly improved photocatalytic activity could be attributed to the facts that the co-doping of N and F together with oxygen deficiency enhanced the visible light absorption, and the F-doped carbon nanotube facilitated the exposure of active sites and the separation of photogenerated electrons and holes. This work provides a simple, feasible method for designing and fabricating high-performance titanium oxide photocatalysts.

Synthesis of carbon nanofibers from electrospun polyvinylidene fluoride nanofibers for cathode electrodes in Li-O2 batteries

PVDF nanofibers were fabricated by the electrospinning method from polyvinylidene fluoride (PVDF) solutions in mixture of DMF and acetone solvents. PVDF fibers were then converted to CNF fibers through the low-temperature chemical stabilization ("dehydrofluorination") before carbonization at 800°C. The free-standing, perforated features of the CNF-based PVDF enabled the CNF to be directly applied as an air cathode in a LOB just after drying, without requiring additional conducting additives or polymeric binders. The interconnected pores between the individual CNFs were estimated to be 2‒4 µm. This could prevent the electrode from clogging when the discharge product was formed. With the interstitial voids and a large surface area, the CNF electrode synthesized from polymer PVDF had a capacity of 2,600 mAh/g with a current density of 200 mA/g. Moreover, CNF fibers, synthesized from electrospun PVDF nanofibers containing C‒F bonds, could improve the electrode conductivity, forming Li2O2 discharge products with less crystalline properties, leading to overpotential reduction during a discharge. This contributed to the longer cycle life of Li-O2 batteries using the CNF synthesized from electrospun PVDF nanofibers electrode (97 cycles) compared to the one synthesized from electrospun PAN nanofibers electrode (73 cycles) at a limited capacity of 1,000 mA/h and a current density of 200 mA/g. Their structure and morphology were evaluated by Scanning Electron Microscopy, Fourier-transform infrared Spectroscopy, Energy Dispersive X-ray Spectroscopy, X-ray diffraction, and Raman Spectroscopy.

Residual solvent-assisted facile deposition of honeycomb-like silver nanoflakes on the surface of electrospun PAN nanofibers

Nobel metal nanoparticles-decorated electrospun nanofibers (ENFs) have attracted great attention for different applications. In the present work, solvent-assisted mild UV treatment was introduced as a unique, efficient and versatile technique for the fabrication of honeycomb-like Ag nanoflakes-decorated electrospun PAN nanofibers. Freshly prepared electrospun PAN nanofibrous membrane from its DMF solution (without vacuum drying) was treated with AgNO3 solution under mild UV irradiation. Microscopic images showed that honeycomb-like Ag-nanoflakes were well decorated on ENFs. XRD showed the formation of amorphous silver materials on the surface of PAN fibers. The Ag nanoflakes-decorated nanofibers showed promising antibacterial properties. Therefore, this facile technique with proposed mechanism can open a new platform for the fabrication of noble metal nanospecies-decorated ENFs for different applications.

Electrospun PAN-HNTs composite nanofiber membranes for efficient electrostatic capture of particulate matters

The fine particulate matter (PM) pollution has become a serious concern to public health. As the core part of PM air filters, high-performance electrostatic nanofiber membranes are urgently needed. However, the existing air filters remain challenging to further decrease the pressure drop to improve the wearer comfort. On the other hand, the rapidly disappearing static electricity of the existing electrostatic nanofiber inevitably gives rise to a relatively short service life. Here, we demonstrate a novel and enhanced electrostatic nanofiber membrane by introducing the halloysite nanotubes (HNTs) to the traditional electrospun PAN nanofiber membrane. The optimal PAN-HNTs nanofiber membrane shows a high removal efficiency of 99.54%, a low pressure drop of 39 Pa, and a high quality factor of 0.89 Pa−1. This greatly improved filtration performance can be attributed to the increased surface area and diameter of nanofiber after introducing the HNTs as additives with suitable doping concentrations. More importantly, compared with the pure PAN nanofiber membrane, the electrostatic capacity of the PAN-HNTs nanofiber membrane is significantly enhanced, which is confirmed by the leaf electroscope. After introducing the HNTs as additives, the surface of the PAN-HNTs nanofiber membrane becomes hydrophilic, which benefits for preventing foulants from attaching to the surface. We anticipate that the PAN-HNTs nanofibers as high-performance membrane air filters will bring great benefits to public health.

Rose bengal-integrated electrospun polyacrylonitrile nanofibers for photodynamic inactivation of bacteria

Rose bengal-integrated electrospun PAN nanofibers displayed high antimicrobial efficacy against both Gram-negative Escherichia coli and Gram-positive Bacillus subtilis bacteria under white light irradiation. This methodology offers a feasible strategy for water disinfection.

Synthesis of free-standing N-doping Si/SiC/C composite nanofiber film as superior lithium-ion batteries anode

This work shows a facile way of fabrication of high-performance anode material for lithium-ion batteries (LIBs). Electro-spun PAN nanofibers were firstly wrapped with mesoporous SiO2 via templating method to form a PAN@SiO2 composite nanofiber film. After magnesiothermic reduction and removal of unreacted SiO2 and byproduct, a free-standing N-doping Si/SiC/C composite nanofiber film was achieved. It can be directly applied as electrode material in LIBs without conductive additives, binders, and current collectors, and it exhibited high specific discharge capacity and good cycling stability, which was ascribed to its special composite composition and porous structure.

Free radical evolution and decay of PAN nano-fibers formed by irradiation and thermal stabilization

Radiation technique was found to accelerate the stabilization process of PAN nano-fibers in the production of carbon nano-fibers. The evolution and decay of the free radicals of electrospun PAN nano-fibers induced by gamma-rays irradiation were investigated using electron spin resonance. Mainly alkyl and polyimine radicals were formed and the total free radical concentration reached saturation of 1.3×1019spins/g at the dose of 200 kGy in vacuum. The free radicals were very stable with a half-life period longer than 40 days in vacuum but rapidly decayed in air. PAN nano-fibers were subject to radiation oxidation due to their small diameter when irradiated in air. The polyimine radicals were found to be more stable than alkyl radicals at room and elevated temperatures. Mainly polyene radicals were formed resulting from dehydrogenation during the stabilization process and the irradiated sample always contained higher radical concentration. The radiation oxidation facilitated the dehydrogenation to drive the thermal stabilization process.

Synthesis and characterization of electrospun PAN-based activated carbon nanofibers reinforced with cellulose nanocrystals for adsorption of VOCs

Electrospun Polyacrylonitrile/Cellulose nanocrystal (PAN-CNC) nanofibers with uniform diameter and smooth morphology were prepared. The nanofibers were stabilized, then activated to produce activated carbon nanofibers (ACnFs) and their physical and chemical properties were characterized. Last, the adsorption properties of ACnFs were tested for adsorption of methyl ethyl ketone (MEK) and cyclohexane. Scanning electron microscopy revealed that the addition of CNCs improves fiber uniformity and decreases fiber diameter due to enhanced electrical conductivity of electrospinning solutions. The addition of CNCs had minimal effect on fibers thermal stability; however, it brought large improvement in tensile strength. The pore size distribution indicated large volumes of micropores and mesopores in all samples. The maximum surface area and total pore volume were respectively 3497 m2/g and 2.62 cm3/g for 25%PAN-75%CNC nanofibers. The adsorption capacity for MEK and cyclohexane correlated well with the surface area of ACnF, reaching a maximum value of 1.7 and 1.8 gadsorbate/gadsorbent for MEK and cyclohexane, respectively. Compared to commercial activated carbons fiber and beads, the prepared ACnF exhibited higher capacities and faster adsorption kinetics due to larger surface area, higher mesoporosity, and better mass transfer. These results indicate that using CNC improves the mechanical and adsorption properties of electrospun PAN nanofibers. This article, for the first time, puts forward CNC reinforced activated carbon nanofibers as suitable adsorbents for environmental remediation applications.

Preparation and Structures of Carbon-Copper Oxide Nanofibers from Electrospun Polyacrylonitrile Composite

Carbon-copper oxide nanofibers have been prepared by heat treatment of polyacrylonitrile-copper salt nanofibers. In this study, fabrication of PAN-copper salt using two different methods - firstly, synthesis of PAN-copper salt solution using electrospinning (PAN-CuAc NF), and secondly, immersion of electrospun PAN nanofiber in the copper salt solution (PAN-c-CuAc NF). Those ways had a distinct effect on the structure of carbon-copper oxide nanofibers. The morphologies and structures of carbon-copper oxide nanofibers were observed by scanning electron microscopy-energy dispersive x-ray spectroscopy (SEM-EDX), infrared spectroscopy (IR), X-ray diffraction (XRD), and Raman spectroscopy. The SEM image showed a randomly oriented nanofiber structure without bead formation, which average diameter of the nanofiber decreased with increasing process temperature. IR spectra and XRD patterns confirmed the formation of aromatic structures and graphite-like structures on carbon-copper oxide nanofiber. The Raman spectrum revealed that the intensity ratio (ID/IG) of carbonized nanofibers showed different values when the electrospun PAN composite nanofibers were synthesized using a different method, 1.59 for electrospun PAN nanofibers (CNF), 1.92 for carbonized PAN- CuAc nanofibers (C-copper oxide NF), and 0.60 for carbonized PAN-c-CuAc nanofibers (C-c-copper oxide NF).The presence of Cu element has been successfully detected in carbon-copper oxide nanofibers using EDX analysis.

Zwitterionic nanogels modified nanofibrous membrane for efficient oil/water separation

Membrane fouling caused by surfactant-stabilized oil-in-water emulsions is a great challenge for oily water treatment. In this work, we fabricated a sulfobetaine-based zwitterionic nanogels modified polyacrylonitrile (ZPAN) nanofibrous membrane with superwetting surfaces. The zwitterionic nanogels were grafted on the surface of electrospun PAN nanofibers to construct hierarchical structure which can enhance surface roughness and antifouling performance of the membrane. The ZPAN membrane possesses superhydrophilic and underwater superoleophobic properties under a wide range of salt concentrations and pH values. Driven solely by gravity (applied pressure = 1 kPa), the ZPAN membrane can successfully separate oil and water emulsions. The oil content in the collected filtrates was below 20 ppm with a high separation efficiency of >99.6%, meanwhile, the permeation fluxes can reach 32800 L m−2 h−1 bar−1. Moreover, the ZPAN membrane exhibit strong mechanical property and stable reusability, indicating a great potential for efficient low-pressure-driven separation of oil-in-water emulsions.

Needleless electrospinning of PAN/SBA-15 for the preparation of nanofibers membranes

Polyacrylonitrile is one of the few waterproof polymers that can be spun from relatively safe solvents, facilitating the use of PAN nanofibers membranes in medical, filtration and biological applications. In this study PAN nanofiber membranes containing SBA-15 nanoparticles were prepared by the process of electrospinning in needless electrospinning machine and DMSO was used as solvent. A small amount of dispersing agent BYK W-9010 was added for a better deagglomerating of SBA-15 nanoparticles in the PAN/DMSO solution. The influence of rod like SBA-15 type ordered mesoporous silica particles as filler on the morphology and textural parameters of electrospun PAN nanofibers was studied. The effect of concentration, applied voltage, distance and feed rate on nanofibers diameter was investigated. The results obtained demonstrated that by increasing the concentration, applied voltage and feed rate, the number of nanofibers was increased and thicker nanofibers were obtained. Viscosity increased by increasing the concentration of polymer and it increased further by imparting small amount of silica nanoparticles. The SEM images of nanofibers were taken and their morphology explains that presence of silica nanoparticles in the nanofibers increases the specific surface area and makes the surface rough.

Production of polyacrylonitrile/boehmite nanofibrous composite tubular structures by opposite‐charge electrospinning with enhanced properties from a low‐concentration polymer solution

AbstractPolyacrylonitrile (PAN)/boehmite nanofibrous composite tubular structures were fabricated from dilute polymer solutions using an opposite‐charge electrospinning method. The samples were characterized by X‐ray diffraction, Differential scanning calorimetry, scanning electron microscopy, Fourier‐transform infrared spectroscopy, fast Fourier transform, and tensile tests. The presence of boehmite nanoparticles in the electrospun PAN nanofibers prevented bead formation, resulting in uniform fibers with smaller diameters, and improved alignment from low‐concentration PAN polymer solutions. 1 wt% boehmite‐loaded nanofibrous composite tubular structure was selected as the optimal formulation to proceed with the crystallinity and tensile tests, which showed enhanced crystalline properties as well as an abrupt shift in tensile performance. The tensile properties of the nanofiber strongly depended on their crystalline properties. The strong intermolecular forces (hydrogen bonds) between the AlOH groups formed at the surface of boehmite nanoparticles and the polar CN groups along the polymer chains. In addition, the high electrical force between the two tips of the needles in the opposite charge set‐up can contribute to the control of electrical jet deposition instability when using a low‐concentration electrospinning solution, leading to enhanced properties.

Preparation of non-woven nanofiber webs for detoxification of nerve gases

Non-woven nanofiber web with high surface areas and abundant functional groups were fabricated through electrospinning and chemical vapor deposition (CVD) in order to develop functional non-woven nanofiber webs for detoxifying simulant of chemical warfare agents. Functional groups that can hydrolysis diisopropyl fluorophosphate (simulant of G-series agents) were selectively modified onto the electrospun PAN nanofibers without causing deterioration of the fiber morphology. In order to achieve the most suitable conditions for functionalization, the CVD reaction temperature was adjusted and various functional groups were introduced. Here, CVD of ethylene diamine at 120 °C of reaction temperature shows the best detoxifying efficiency against diisopropyl fluorophosphates (DFP), which is simulant of G-series chemical warfare agent (complete removal of DFP within 24 h under humid condition). Density functional theory (DFT) calculations clarified the optimized functional groups for effectively detoxifying nerve gas agent (G types). Both of simulation and experimental results prove that the co-existence of hydroxyl and amine groups will be beneficial in detoxifying reaction (over 80% decomposition within 4 h).

Application of activated carbon-decorated polyacrylonitrile nanofibers as an adsorbent in dispersive solid-phase extraction of fluoroquinolones from wastewater

A cheap and simple sample preparation method, consisting of a dispersive solid-phase method and an adsorbent, activated carbon decorated PAN nanofibers, was employed and used for the extraction of antibiotics (ciprofloxacin, danofloxacin, and enrofloxacin) in wastewater. Electrospun PAN nanofibers that were decorated with activated carbon produced from waste tires were used as the solid phase and the antibiotics analyzed by using high-performance liquid chromatography. Parameters such as pH, mass of adsorbent (MA), extraction volume (EV), and extraction time (ET) were optimized owing to their potential effect on the extraction of antibiotics from water. The recovery of all antibiotics was satisfactory, in the range of 90%–99%. The limits of detection and quantification were 0.05, 0.11, 0.20, and 0.53, 1.21, 2.17 µg/L, respectively. The precision was determined from the repeatability and reproducibility and expressed as the intra-day (n = 20) and inter-day (n = 5) precision. The intra-day and inter-day precision was reported in terms of the percentage relative standard deviation, which was 3% and 4%, respectively. The adsorption capacity of the activated carbon-decorated PAN nanofibers was satisfactory, and the reusability of the adsorbent was impressive when reused ten times. The accuracy of the dispersive solid phase extraction (DSPE) was validated by spike recovery tests; the results proved the reliability and efficiency of adsorbing antibiotics from wastewater. Finally, the proposed method was applied to wastewater samples collected from a wastewater treatment plant, which included influent, secondary, and effluent wastewater.