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New generation washable PES membrane face mask for virus filtration

New generation washable PES membrane face mask for virus filtration NANOCOMPOSITES 2022, VOL. 8, NO. 1, 13–23 https://doi.org/10.1080/20550324.2021.2008209 RESEARCH ARTICLE a,b,c,d e f c d Md Eman Talukder , Fariya Alam , Md. Nahid Pervez , Wang Jiangming , Fahim Hassan , George K. g f c Stylios , Vincenzo Naddeo and Hongchen Song a b Shenzhen Institute of Advanced Technology, Chinese Academy of Sciences, Shenzhen, China; University of Chinese Academy of Sciences, Beijing, China; Water Science center, Guangzhou Institute of Advanced Technology, Chinese Academy of Sciences, d e Guangzhou, China; Department in Textile Engineering, Southeast University, Tejgaon, Bangladesh; Department of fashion Design & Technology (FDT), BGMEA University of Fashion & Technology, Turag, Bangladesh; Sanitary Environmental Engineering Division (SEED), Department of Civil Engineering, University of Salerno, Fisciano, Italy; Research Institute for Flexible Materials, School of Textiles and Design, Heriot-Watt University, Galashiels, UK ABSTRACT ARTICLE HISTORY Received 27 July 2021 Membrane materials might be used for face protection because they can decontaminate the Accepted 15 November 2021 inhaled air from particle pollution and viruses like the SARS-Cov0-2 which damages our res- piration system. In this study, plyethersulfone membranes (PES) were synthesized with green KEYWORDS solvent at room temperature and its filtration effectiveness was investigated against nano- Membrane filtration; PES bacteria (size 0.05 to 0.2 mm) by measuring their Bacterial Filtration Efficiency (BFE) and micro membrane; Corona-virus; aerosol size (0.3 mm), and Particulate Filtration Efficiency (PFE). The average SARS-CoV-2 microfiltration; nanofiltra- diameters are between 50 nm to 160 nm. A series of experiments were performed to accom- tion; air filtration; high plish between 0.03 to 0.21 mm PES sponge like diameters so that can be used for SARS-CoV- efficiency; fresh breathe 2 filtration. Results showed that nanofiltration/ultrafiltration could filter 99.9% of bacteria and aerosol from contaminated air the size of the Covid-19 molecule. GRAPHICAL ABSTRACT Highlights Covid-19 is still a pandemic and continues to spread A washable innovative PES membrane face mask and mutate becoming a major threat to public has been developed. health, infecting more than 219 M people worldwide The virus removal efficiency of the PES mem- with over 4.55 M deaths as reported on Oct 2021 brane face mask reaches 99.9%. [1,2]. Covid-19 might be transmitted from spit The PES membrane face mask is washable and droplets, airborne, fomite, fecal-oral, blood borne, reusable retaining its efficiency. and animal-to-human contact. Covid-19 may cause acute myocardial injury, severe pneumonia, and chronic damage, resulting in a mortality rate 1. Introduction between 1.5 to 2.5% [3,4]. Researchers examined the SARS-CoV-2 (the 2019 coronavirus pandemic size and content features of the SARS-CoV-2 par- (Covid-19)) is responsible for causing acute respira- ticles in addition to the mechanism of transmission. tory symptom, high contamination and death. Different studies have produced various findings CONTACT Md Eman Talukder eman-talukder@giat.ac.cn, 2654410096@mails.ucas.ac.cn Shenzhen Institute of Advanced Technology, Chinese Academy of Sciences, Shenzhen 518000, China; Hongchen Song hc.song@giat.ac.cn Water Science center, Guangzhou Institute of Advanced Technology, Chinese Academy of Sciences, Guangzhou 514480, China Supplemental data for this article is available online at https://doi.org/10.1080/20550324.2021.2008209. 2022 The Author(s). Published by Informa UK Limited, trading as Taylor & Francis Group. This is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. 14 M. E. TALUKDER ET AL. Figure 1. The filtration performance comparison among PES membrane, electrospun nanofiber membrane mask, N95 mask, and surgical facemask. when using electron microscopy to examine nega- exacerbated by very high demand, as a result of this, tive-stained SARS-CoV-2 particles, and reported while face coverings or homemade masks can help that the virus’s diameter ranges between 50 nm to to protect from bacteria, there is no scientific evi- 140 nm [5]. dence that they are effective against Covid-19 virus, Covid-19 virus primarily causes respiratory sick- mainly because most of them will have much bigger ness, ranging from moderate to severe, affecting the pore size than the Covid-19 virus. Pore size is one lungs and their function which might be lethal. of the most important parameters in the fabrication Whilst some people who are infected never show of masks for Covid-19, so that, the next generation any symptoms, they can infect others which is diffi- reusable and anti-virus nano pore filtration size cult to detect, but dangerous for spreading transmis- masks may be necessary [13]. However, reusable sion. Spit droplets and aerosols are mostly masks should prolong the use of the mask, not at important for the rapid spreading of Covid-19 [6,7]. the expense of filtration effectiveness. Anti-virus An infected person can release the virus via coughs masks can promptly shield as well as destroying the and sneezes [8]. According to recent studies, aero- virus in the filter of the mask, preventing virus sols and respiratory droplets ejected during sneeze/ retention [13–15]. The invention of such a novel cough can travel up to 12 to 26 feet [9,10], which is mask would aid us in dealing with epidemics such substantially further than the (CDC)- 6-feets social as COVID-19. distancing guideline [9,11]. In addition, droplets can Many researchers have reported on the fabrica- be stable in the air for an extended period of time tion of face masks by electrospinning and producing due to their micro-meter/nano-meter size and negli- nanofiber membranes. Zhang et al. employed melt- gible gravitational effect, posing a threat of airborne blown Polypropylene(PP) non-woven fabrics with a transmission, especially in enclosed spaces with fiber diameter of 0.5–10 mm[13,16]. Cheng et al. inadequate filtration systems. It was confirmed by reported on an electrospun polyetherimide non- the World Health Organization (WHO) that Covid- woven bi-functional material for an innovative face 19 is characterized as airborne and can remain 8 h mask [17]. Ultrafiltration or nanofiltration membranes, in the air, so people are asked to wear face masks to protect themselves and others from contamination whose width is measured in micro or nano-meters, in public places. are highly regarded for air filtration applications Before a significant percentage of the world’s due to the high surface area and sponge-like inter- population is vaccinated, wearing a mask in public membrane pore sizes less than 0.1 mm. These ultra- places might be the most effective weapon to reduce filtration or nanofiltration membranes supported the spread of the virus. Because of this reason, with a non-woven fabric might be a good candidate masks have become a necessity in every day’s life. for mask effectiveness, because it can possess high Commercial surgical face masks, and N95 masks level of air permeability promoting user comfort typically use melt blown non-woven tissue paper as and as well reuse [18,19]. Polyether sulfone (PES) is a virus filter sheet. PET (Polyethylene terephthalate) a soluble polymer, and the PES-based ultrafiltration melt blown nonwoven used mask can be worn only or nanofiltration membranes have shown high a few fours and then get disposed. [12], as shown in chemical resistance, thermal and mechanical stability Figure 1. Worldwide face mask shortages were and hydrophobicity, making them suitable for air NANOCOMPOSITES 15 filtration due to their nano sponge-like pore size bath, and the PES has successfully solubilized into distribution, while virus protection performance by the solvent at 60 C temperature. The 2 wt % PVP the pure PES membrane can be adjusted by the add- additives were used by continuous magnetic stirring ition of a catalytic process [20]. at 60 C temperature for 1 h or until a completely PES-based membrane products have an excellent clear and uniform solution was obtained. The homogeneous sponge-like pore size membrane hydrophobicity, surface charge, and roughness of structure. The sponge-like membrane pore size dis- the membrane are dependent on the blending ratio tribution mechanism is explored to improve virus of PES and PVP. Using a casting knife, the polymer filtration. The filtration performance of separation solution was then cast onto a glass plate, and the membranes with additional gradient structural cast film’s solvent was allowed to gently evaporate at change has been previously reported [21]. room temperature overnight. To complete precipita- Furthermore, because these virus particles are resist- tion and membrane development, the glass plate ant to inactivation procedures such as low pH, as in containing the cast film was gently submerged into the case of the reported parvovirus elimination a water bath for 6 h. Then, pure water is used as the [22,23]. When these membrane materials are washed coagulation bath, and the non-solvent induced phase and reused several times, and potentially the total separation method is used to obtain the PES flat membrane virus particle attachment maybe high to membrane by scraping. Prior to UF operation, the null, divergent flow filtering is preferable [22]. membranes were maintained in deionized water. This novel research introduces a washable and The PES membranes exhibit better antifouling abil- reusable innovative sponge-like structure with a ity and have a more sponge-like pore size structure non-woven supporting PES membrane for face because of the increase in positive polar charge mask use. The non-woven support PES membrane when the PES and PVP blend get in contact with face mask can effectively prevent the aerosol and the solvent. nano-bacteria/virus sized particles during the inhal- ing process. This novel material shows the following 2.3. Characterization advantages: (1) uniform pore size, sponge-like pore size distribution, and virus filtration by the non- The solution viscosity of the embrane sample was woven support PES membrane by phase inversion measured using a Rotational Viscometer (NDJ-8S via immersion precipitation method; (2) the filtra- Digital Viscosity Meter, Novel Scientific Instrument tion efficiency of particles (size of between 0.01 to Co., Ltd, China) at ambient temperature. Membrane 0.2 lm) and (3) the durability of the PES-based face sample contact angles were assessed using a TM TM mask with excellent working efficiency, which can dropmeter (dropmeter -A-300-main st vision, continuously protect from the virus more than 72 h. Kudos precision Instruments, USA). The mem- This novel work reports on a new efficient, wash- branes morphology was examined using scanning able, and reusable PES membrane for face mask electron microscopy (SEM) (Phenom XL, Phenom end uses. world, Thermo Scientific, Japan) at an accelerating voltage of 5 kV. Fourier transform infrared spectrum (FTIR) was recorded from 400 to 4000 cm-1 by 2. Experimental using (IR, Interspectrum, low noise DLATGS, FTIR- 2.1. Materials 920, Estonia). The thermal decomposition behavior of the membrane was studied using thermal gravi- This research was carried out using polyethersulfone metric analysis (TGA) (TG 209 F1 LibraV Netzsch (PES), ultrason E6020P (average M : 6 58 kDa,) company, United Kingdom), under a nitro- from BASF, Germany. PolarcleanV was purchased gen atmosphere. from Solvay Fine Chemical Additives (Qingdao) The prepared membrane pore size was deter- Co., Ltd., China. polyvinylpyrrolidone, (PVP)-K30, mined using prostate-specific membrane antigen-10 was purchased from Chemical Reagents Co., Ltd, (PSMA-10, Nanjing GAO Qian functional Materials China. The non-woven PET fabric was supplied by Technology Co., Ltd., and China). The pore volume Guocheng CO. (Wuxi, China). Sodium hydroxide (mL/g) at specific pore sizes (m) ranging from 0 to (NaOH) was obtained from Sinopharm Chemical 0.30 mm was measured for membrane air perme- Reagent Co., Ltd. (Shanghai, China). All chemicals ability and selectivity characteristics. Membrane and reagents were used without further purification. pore sizes were calculated from the smallest to the largest, with the mean flow pore diameter represent- 2.2. Membrane preparation ing the primary pore size. The thickness of the The membrane solution was prepared by dissolving membrane was measured with a digital micrometer a certain amount of PES in a PolarcleanV solvent Shanghai Liuling Hand-Type Qianfen Thickness 16 M. E. TALUKDER ET AL. Figure 2. (a) SEM image of PES membrane, (b) equal pore size distribution (sponge-like). CuCd Gauge CH-1-S Plastic Film Sheet Hand-Type Filtration efficiency ðFEÞ¼ (1) Thickness Gauge, which has a precision Cd of 0.001 mm. 2.5.1. Bacterial filtration efficiency (BFE) experiments The ASTMF 2101 standard Test Method was used 2.4. Tensile strength to evaluate the Bacteria Filtration Efficiency (BFE) Talukder et al. reported a procedure of tensile of the material. Here, biological nano-bacteria were strength for membranes [20]. The tensile strength used and, the virus filtration efficiency was tested by and elongation of five samples from each membrane obtaining the filtration percentage by comparing measuring 50 mm in length were measured at a con- between the nano-bacterial control counts and the stant elongation rate of 20 mm/min up to the break- test article effluent counts. The challenging part in ing points of the PES membrane using a tensile this test are the nano-bacteria (size 0.05 to 0.2 mm). strength tester KD-jjj model BA-100m by Transcell A nano-bacteria mixer liquid solution was passed Technology, China. throw to the filtration medium at a 28.3 liters per minute (LPM) flow rate [28] for 4 h at a 21 ± 5 C 2.5. Filtration efficiency (FE) temperature and relative humidity of 85 ± 5%. The Food and Drug Administration (FDA) issues 2.5.2. Particulate filtration efficiency (PFE) ASTM standards as the recognized standard in the According to the FDA guideline paper, the PFE of United States. ASTM F2100-11 (2011) is a funda- the various devices was tested with unneutralized mental standard that sets the performance require- 0.1 m PSL particles [29,30]. PFE testing was carried ments for respirators and face mask (3 Tips for out using the whole PES membrane mask material. Choosing the Right Face Mask) [24]. The ASTM According to the ASTM 2299 procedure, the test F2100-11 standard outlines the required characteris- velocity was between 1 and 25 cm/sec [27,31]. Prior tics and testing methods for the materials used in to testing, the test samples were preconditioned at the manufacture of face mask for use in hospitals, 30–50 percent relative humidity (RH) at 21 3 C health care, and patient care. In the 42 CFR Part 84 [31]. An automatic Particulate Filter Efficiency PFE certification process, there are several techniques for Tester GT-RA09 from GESTER INTERNATIONAL measuring filtration efficiency, including particle fil- CO. LTD. (China) was used to investigate the filtra- tration efficiency (PFE), bacterial filtration efficiency tion efficiency. Concentrations upstream and down- (BFE), virus filtration efficiency (VFE), and NIOSH stream of the respirator were monitored at a flow [25]. Material efficiency is linked to the PFE and rate of 80 L/min, with 2% accuracy. The user simply BFE techniques, which are employed as a barrier to needs to insert the filter paper in the fixture and protect the user from aqueous viral aerosols. The fil- push the button to change the test flow; the system tering efficiency test is carried out according to the will test the resistance and efficiency automatically ASTM F2100-19E1 methodology, which uses a via the controller. The PFE is calculated by equation nano-size salt aerosol/bacteria [26]. Eq. (1) is used (2). For each test material, the upstream count was to calculate the filtration efficiency of mask and res- measured before and after the downstream count. pirators, where Cu and Cd are the average particle Both upstream and downstream counts were meas- concentrations per each upstream and downstream test specimen [27]. ured three times for one minute each. NANOCOMPOSITES 17 Figure 3. Contact angle of PES membrane for the face mask (respectively 120.1 and 121.5 ). CuCd 3.3. Sponge-like structures adjustment control Particulate filtration efficiency ðPFEÞ¼  100 Cd As an excellent porogen, PVP can effectively (2) increase the porosity of the filter membrane and at the same time increase the hydrophilicity of the The PFE findings range from 1 to 99.99 percent, membrane. It is widely used in the preparation and where Cu and Cd are the averages of upstream and modification of membrane materials. The addition downstream counts. The greater the percentage, the of non-solvent additives, such as small inorganic better the mask filtration. For the PFE test, particle molecules and small organic molecules, has become sizes ranging from size 0.05 to 0.2 mm can be meas- an important method for adjusting the structure of ured. When comparing the test results, the particle membrane materials [20,32]. Additives can effect- size (e.g. size 0.05 to 0.2 mm) must be taken into ively affect the mass transfer rate of solvents and account, since using a particle with a greater size non-solvents, thereby forming different pore struc- might lead to a deceptive PFE evaluation. tures. This experiment uses PVP as an additive to control the structure of the polyethersulfone mem- brane material. 3. Results 3.1. Membrane characterization 3.4. Adjustment of membrane pore size and its The viscosity and electric conductivity of the solu- performance tions were 2465 mPa/S, and 1.4 mS/cm, respectively. The pore size and its distribution are important The morphology of the PES membrane was ana- indicators for the application of membrane materi- lyzed using SEM, as shown in Figure 2a. The PES als, which determine the filtration performance and membranes have a uniform structure with an aver- application fields of membrane materials. In this age membrane thickness at approximately 0.5 mm experiment, the effects of the solid content of PES and 0.3 mm, as shown in Figure 2a. The SEM image and the content of solvent in the casting liquid on shows the surface roughness of the PES membrane. the structure and pore size of the membrane were As shown in Figure 3, the PES membrane was investigated. Under the condition of ensuring cer- shown to exhibit hydrophilic behavior, with contact tain content of solvents and additives in the casting angles of 120.1 and 121.5 , as shown in Figure 3a liquid, the effect of solid content (PES mass frac- and b. tion) on the pure water flux of the PES membrane was investigated. The results are shown in Figure 2. It can be seen from the figure that as the solid con- 3.2. Pore size tent increases, the viscosity of the casting liquid Sponge-like pore size distribution of PES membrane increases, the force between the polymer molecules is depended on membrane diameter and on mem- becomes larger, the movement space between the brane fabrication environment such as temperature, polymer molecules becomes smaller, the double dif- humidity, coagulation bath temperature. The with- fusion speed between the solvent and the non-solv- drawing air pressure through the PES membrane ent becomes slower, the liquid phase separation rate was 145 to 200 kPa and shown a pore size distribu- becomes slower, and the structure of the prepared tion range of 0.03 to 0.21 lm. The pore size distri- PES separation membrane tends to be more dense bution experiment was reported 10 times and [33], which leads to a decrease in the pure water repeated an average pore size of 0.122 mm, as shown flux. And as the solid content of PES increases fur- in Figure 2b. ther, the viscosity of the material liquid becomes too 18 M. E. TALUKDER ET AL. Figure 4. (a) FTIR spectra of PES membrane, (b) TGA results of PES membrane. Figure 5. (a) XRD results of PES membrane, and (b) Tensile strength of PES membrane. large and the uniformity of the film formation membrane which is connected to PVP residue. PVP becomes worse. Therefore, the solid content is stretching vibration increased with increasing of maintained at 16% to 18%, which can ensure that PVP ratio from 1 wt% to 10 wt%, as illustrated in the PES membrane has good film-forming proper- Figure 4a. ties and pure water flux. Using Polarclean as a According to the TGA curves, the thermal solvent for membrane material preparation, and decomposition behavior temperature for the PES under the premise of ensuring the consistency of membrane was relatively stable up to 420 C (5% solid content and porogen, using acetone as the weight loss) [36]. As shown in Figure 4b, its thermal pore size regulator, the effect of PolarcleanV content degradation was demonstrated a one stage weight on the cross-sectional structure, pure water flux and loss. The PES membrane was stable up to 420 C rejection rate, pore size and pore size of the PES without significant weight loss, as compared to membrane was investigated. The results of the influ- 450 C for the pure PES membrane, concluding that ence of porosity are shown in Figure 2. adding PVP influences thermal degradation on the The FTIR spectra of the PES membrane is shown PES membrane [37,38]. in Figure 4a, and its functional group was analyzed The crystallinity of the PES membrane was ana- on different spectra. Four major peaks may be seen lyzed by WAXD, which shows the crystallinity prop- in the functionalized self-made membrane. Repeated erties of the PES membrane. As shown in Figure 5a, ether and sulfone linkages alternate between aro- the membrane was characterized as a typical matic rings in the PES. As a result, the stretching amorphous structure with peaks at 2h a.u. values vibrations of S ¼ O symmetric and S ¼ O asymmet- of 16–19 . ric may be ascribed to the bands at 1145 and 1261 cm , respectively [34]. And, the bands at 3.5. Tensile strength 1665 cm represent PVP’s amide group (OH). The spectrum of the PES/PVP membrane, on the other The tensile strength of the PES membrane is anes- hand, reveals that PVP was maintained in the mem- sential fact for face mask application, with its stress- strain properties shown in Figure 5b. The tensile brane structure. Another unique absorption peak at 1 1 1305 cm and 1663 cm is present in the C ¼ O properties and breaking elongation rate are functional group vibration stretching [35]. These enhanced because of the specific intermolecular peaks indicate the presence of PVP in the PES interactions by the additives in the PES membrane. NANOCOMPOSITES 19 The elongation at breaking point and tensile the number of viable nano-bacteria generated, the strength values are summarized in Table 1, with positive control system was employed without a PES 6.4 MPa tensile strength, and 77% elongation at membrane. On the triple side, the test system was break, [39] being higher than the ENM mask [40]. performed, and the negative control system was com- pleted without the nano-bacteria. And then, the nega- This rise could be attributed to the increase in PES membrane surface area. tive system was done by air sample in aerosol chamber on the triple part [45]. The average nano- bacteria size was 0.10 mm, which is the average size of 3.6. Virus filtration test Covid-19 virus droplets produced by coughing. The BFE method was modified, and Staphylococcus Bacteria filtration efficiency (BFE) was calculated by aureus (S. aureus) was replaced by nano-bacteria comparing the average positive hole number corrected (the hypothesized nano-bacteria are mostly 0.05 to of nano-bacteria captured after the PES membrane 0.2 mm in size) as the test specimen [41], which is mask, compared with the positive control. The BFE roughly similar to the SARS-CoV-2 diameter [42]. for each PES membrane mask was also calculated This precautionary change was applied to this without the largest size nano-bacteria, yielding an experiment, so that the chosen nano-bacteria can average nano-bacteria size of 0.1 mm[24]. This more represent SAR-CoV-2 [21]. 100 L of 8 10 PFU/mL accurately portrays the amount of inhaled aerosol nano-bacteria is used in sterile water at a flow rate reaching the lower respiratory system and alveolar of 28 L/min through the membrane (shown in region of 0.3 mm. Figure 6) under normal respiration range and cas- cade impact or constraints [43]. The filtration pres- 3.7. Particulate filtration efficiency (PFE) sure was kept at 35 kPa throughout the suspension. The particulate filtration efficiency was tested by Nacl Nano-bacteria was passed through the membrane testing methods with adjusting the rotary flow rate face mask on E. coli (Escherichia Coli) plates within 20 mg/m . When the upstream concentration is stabi- the 6 stage cascade impactor. The E. coli plates were lized, it automatically changes into the downstream incubated overnight at 37 C. The control plaques concentration test, and the curve is observed. When could enhance the performance of the PES mem- the downstream concentration is stable, the experi- brane, and the positive hole correction of multiple-jet ment starts counting until the end. The results reveal impactor was counted and recorded [44]. The positive an upstream concentration of 20.900 mg/m and hole was calculated for each of the 6 stages and added downstream concentration 0.243 mg/m ,producing together. The average number was counted. To assess 99% filtration efficiency, as shown in Figure S1. Table 1. Tensile strength and elongation (%) of PES membrane. 3.8. Hepa PES membrane mechanism Membrane type Tensile strength (MPa) Elongation (%) PES membrane 6.4 77 A HEPA filter is designed to collect very small par- ENM mask [40] 4.1 38 ticles and does not operate like a normal membrane Figure 6. Bacteria filtration efficiency process and apparatus according to ASTM. 20 M. E. TALUKDER ET AL. five cycles. After five recovery cycles, the Filtration Efficiency of the PES membrane decreased by 50%, showing that the PES membrane can be used after washing. 4. Discussion Handling, appearance and skin comfort of the PES membrane are good because it is soft, smooth, dust free and not irritating to the nose and face. Fabricated PES membranes show hydrophobic behavior, which could be used for face masks. The average coronavirus diameter ranges between 50 to 160 nm and those sizes could be filtered via the sponge-like pore size (0.03. ton 0.21 mm) of this PES Figure 7. PES membrane virus filtration efficiency against membrane. Moreover, its tensile strength is two or washing cycles. three times higher than any ENM [40,48]. After weighing, the membrane was found to provide filter, which captures particles bigger than the filter’s enough virus protection. More importantly PES pore size. Instead, HEPA filters capture particles membrane is capable of filtering aerosol and bac- using a mixture of three methods. Interception is teria with 99.9% efficiency, by its ability to filter the first process, in which particles are transported particles from air streams. They could be essential in the airflow around the filter fibers attached to the component in respirator and face mask fil- filter. To be collected, particles must be within one ter materials. radius of the filter fiber. The second process, impac- tion, is frequently used to collect larger particles. 5. Conclusion Because of their size, these particles are unable to respond to abrupt variations in airflow around the With the Covid-19 epidemic, face masks and respi- filter, and instead rush towards and embed them- rators ware becoming an everyday necessity poten- selves in the fibers of the filter. Diffusion is the last tially for years to come. PPE is subjected to a range process, which happens as a result of how tiny par- of tests to assess its performance and suitability ticles travel and interact with surrounding mole- under various conditions. The PES membrane has cules. Brownian motion describes how molecules soft handle and smoothness and does not irritate move in a random, zig-zag manner as they clash the skin around the face. This study has demon- strated the high filtration efficiency of the PES with neighboring molecules. membrane. The PES membrane was used in a direct flow configuration. The filtering surface of asym- 3.9. Washable and reusable metric membranes served as the downstream mem- Ethanol is an extensively used disinfectant, and has brane surface. To achieve optimum rejection of viral been shown to lower coronavirus infectivity by a particles and passage of product species, the mem- factor of four or more [46]. Although masks cleaned branes must have a very narrow pore-size distribu- by soaking in 70% ethanol for 2 h had no effect on tion. When constructing viral filters to exclude DP, they did exhibit a significant drop in BFE [47]. small parvovirus particles, this is very crucial. This The filter efficiency distribution across particle sizes PES membrane can be used for face masks and has appeared to be affected by ethanol treatment, with the potential of being certified for use to protect the MPPS changing from 0.03-0.21 mm to 0.05- against contamination. 0.23 mm pre- and post-treatment [47]. The reusing conduct of the PES membrane was Disclosure statement researched during five progressive reuse cycles to No potential conflict of interest was reported by explore PES membrane execution. The used PES the authors. membrane was recuperated by shaking in 1.0 mol/L NaOH arrangement at 50 rpm for 0.5 h, followed by centrifugation. The recovered adsorption limit of Authors’ contributions the PES membrane has appeared in Figure 7. The MET has conceived the idea, conducted the experiments, reused PES membrane capacity stayed flawless for and written the initial draft. MET, FA, MNP, WJ, FH, the initial two cycles and somewhat dropped after GKS, VN analyzed the data and prepared the final draft. NANOCOMPOSITES 21 HS has administered the project. All authors have read (Bangladesh) under the supervision of Prof Syed Fakhrul and approved the manuscript. Hassan. After that, he secured Color Root (Hubei) Scholarship to pursue his MSc studies in Textile Engineering at the Wuhan Textile University (China) in Funding 2016. During his MSc studies, he worked on dye waste- water treatment by Fenton catalytic system in the group This work was supported by the Guangzhou Institute of of Prof. Felix Y. Telegin (Russia). Afterwards, he worked Advanced Technology, Shenzhen Institute of Advanced as a visiting researcher at the Heriot-Watt University Technology, CAS, and China. The authors are also grate- (UK, 2016-2017), Vilnius University (Lithuania, 2018). ful to the Shenzhen Institute of Advanced Technology, Currently, he is a doctoral candidate at the University of the Chinese Academy of Sciences, Shenzhen, China, for Salerno (Italy) under the supervision of Prof. Vincenzo supporting this research. This research work was funded Naddeo, and he spent one year research period at the by the Shenzhen Science and Technology program (grant University of Boras (Sweden, 2020). His current research number: KCXFZ 2021221173402006). In addition, we focuses on the development of sustainable materials for would like to express our sincere gratitude to the support environmental applications. from the Sanitary Environmental Engineering Division (SEED) and grants (FARB projects) from the University Jianming Wang received the B.S. degree in Polymer of Salerno, Italy, coordinated by prof. V. Naddeo. The material and Engineering from Yaitai University, Yaitai, PhD School in “Risk and Sustainability in Civil China in 2009 and the M.S. degree in Materials Science Engineering, Environmental and Construction” is also and Engineering from Tiangong University, Tianjin, acknowledged for the scholarships (cycle-XXXIV) of China in 2012. In 2012, he joined Guangzhou Institute of M.N. Pervez. Advanced Technology and engaged in scientific research. He research interests include preparation and application of separation membrane, material modifica- Notes on contributors tion technology. MD Eman Takukder: During my undergraduate study, Fahim Hassan: For as long as I can remember I’ve known my major was in textile Engineering. Although my grades what I wanted to do with my life. Dedicating my life to were among the highest top 10, CGPA 3.81 out of 4.00 improving the lives of others is very appealing to me. Scale, I received a merit scholarship every semester. I had This is Fahim Hassan. I hold a [four year] Bachelor’s completed my undergraduate research project on the tex- Degree in Textile Engineering from Southeast University; tile dyeing section. This sector is also related to waste- Dhaka, Bangladesh, with a CGPA of 3.12 out of 4.00. I water treatment plant ETP (Effluent Treatment Plant). was amongst the top 50 students of my class of 120 stu- However, besides some cognition, what I gained from my dents. I have been, in the past, amongst the top rankers school education was a significant self-discovery. My in the entrance tests conducted by the academic institu- under-graduation and post-graduation study of medium tion of my education. Our university is considered to be of instruction and examination is English. In June 2015, I the one of the best university in my country for “Textile got Wuhan Textile University President Scholarship. Now Education” as a cradle for making the excellence of I am doing a research-based master’s degree within the Textile leaders. major of Textile Chemistry with the department of the Prof. George K. Stylios: I come from a textile business College of Chemistry and Chemical Engineering at background in Greece and studied in the UK. I completed Wuhan Textile University, China. My master thesis my postgraduate studies in Leeds and then went onto my research was done under the famous Chinese professor MSc and PhD, which were funded by M&S and their sup- Dr. Jinbo Yao Dean of College of Chemistry and pliers. I completed my PhD in 1986 and became a lec- Chemical Engineering, the preparation of layer by layer turer in clothing at Bradford, and then became a fellow of electrospun membrane-based wound dressing for skin the Science and Technology Agency in Japan in 1991 injuries treatment and stem cell tissue regeneration engin- before returning to Bradford in 1992. I obtained my per- eering by electrospinning process. I also had done one sonal chair in industrial engineering systems at Bradford project in my first year with my friend by using of mem- in 1994 whilst continuing research in textile objective brane bioreactor to remove the antibiotics micropollutants measurement applied at the textile and clothing interface. from wastewater. I have completed my master degree by In 1999 I joined the School of Textiles and Design at securing 2nd position in among all international students Heriot-Watt University as Professor of Textiles and I’m (CGPA 3.89 out of 4.00 Scale). Approximately in Oct currently Director of TechniTex and the Faraday 2021, my Ph.D. graduation will be completed from Partnership in Technical Textiles. Shenzhen Institute of Advanced Technology, Chinese Academy of Sciences with the project of Fabrication and Prof. Vincenzo Naddeo is Director of the Sanitary improving the membrane performance for wastewater fil- Environmental Engineering Division (SEED) at the tration and purification by using the Computational Fluid Department of Civil Engineering of the University of Dynamics (CFD) module. Salerno (Italy), where he drives research and academic activities in the Environmental Engineering fields. He FariyaAlam: I am doing my BSc degree in Textile serves as an affiliate professor at both the Department of Engineering at the BGMEA University of Fashion & Civil and Environmental Engineering of the University of Technology (Bangladesh). My current research focuses on Washington (Seattle, WA, USA) and at the Department the development of textile fashion and design sustainable of Water Resources and Environmental Engineering of textile product for environmental applications the Tamkang University (New Taipei City, Taiwan). His Md. Nahid Pervez received his BSc degree in Textile research focuses on advanced water/wastewater treatment, Engineering (2014) at the Southeast University characterization and control of environmental odours and 22 M. E. TALUKDER ET AL. environmental impact assessment (EIA). He developed 13. Zhang Z, Ji D, He H, et al. Electrospun ultrafine advanced biological processes for wastewater treatment fibers for advanced face masks. Mater Sci Eng: R: Rep. 2021;143:100594. and control of emerging contaminants, novel ultrasound- 14. Zhang Z, He H, Fu W, et al. Electro-hydrodynamic based technological processes for treating environmental direct-writing technology toward patterned ultra- matrices (solid, liquid and gaseous) and biotechnologies thin fibers: advances, materials and applications. for wastewater re-use with simultaneous energy produc- Nano Today. 2020;35:100942. tion within the framework of the circular economy. 15. Talukder ME, Hasan KMF, Wang J, et al. Novel Hongchen Song, Ph.D. Supervisor, Shenzhen Institute of fibrin functionalized multilayered electrospun nano- Advanced Technology, Chinese Academy of Sciences. fiber membrane for burn wound treatment. J Mater RESEARCH AREAS: (1) Preparation and Modification of Sci. 2021;56(22):12814–12834. Polymer Membranes. (2) Membrane Application in 16. Gahan R, Zguris GC. A review of the melt blown Water Treatment. (3) Continuous Bioseparation and process. In: 15th Annual Battery Conference on Purification Process System. (4) Design and Fabrication Applications and Advances (Cat. No. 00TH8490), of Flat Membrane Casting Equipment for IEEE, 2000. p. 145–149. Scientific Research. 17. Cheng Y, Wang C, Zhong J, et al. Electrospun poly- etherimide electret nonwoven for bi-functional smart face mask. Nano Energy. 2017;34:562–569. References 18. Bowen WR, Welfoot JS. Modelling of membrane nanofiltration—pore size distribution effects. Chem 1. Rothan HA, Byrareddy SN. The epidemiology and Eng Sci. 2002;57(8):1393–1407. pathogenesis of coronavirus disease (COVID-19) 19. Pervez M, Stylios GK. Investigating the synthesis outbreak. J Autoimmun. 2020;109:102433. and characterization of a novel “green” H2O2- 2. 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Wickramasinghe SR, Han B, Carlson JO, et al. water research community respond? Environ Sci: Clearance of minute virus of mice by flocculation Water Res Technol. 2020;6(7):1939–1939. and microfiltration. Biotechnol Bioeng. 2004;86(6): 5. Abu Ali H, Yaniv K, Bar-Zeev E, et al. Tracking 612–621. SARS-CoV-2 RNA through the wastewater treat- 23. Wickramasinghe SR, Stump ED, Grzenia DL, et al. ment process. ACS ES&T Water. 2021;1(5): Understanding virus filtration membrane perform- ance. J Membr Sci. 2010;365(1–2):160–169. 1161–1167. 24. Forouzandeh P, O’Dowd K, Pillai SC. Face masks 6. Buonanno G, Stabile L, Morawska L. Estimation of and respirators in the fight against the COVID-19 airborne viral emission: quanta emission rate of pandemic: An overview of the standards and testing SARS-CoV-2 for infection risk assessment. Environ methods. Safety Sci. 2021;133:104995. Int. 2020;141:105794. 25. Rengasamy S, Shaffer R, Williams B, et al. A com- 7. Tang S, Mao Y, Jones RM, et al. Aerosol transmis- parison of facemask and respirator filtration test sion of SARS-CoV-2? Evidence, prevention and methods. J Occup Environ Hyg. 2017;14(2):92–103. control. Environ Int. 2020;144:106039. 26. Using P, Spheres L. Standard specification for per- 8. Fennelly KP. Particle sizes of infectious aerosols: formance of materials used in medical face masks 1. implications for infection control. Lancet Respir Test. 2005;11(2018):19–21. Med. 2020;8(9):914–924. 27. Konda A, Prakash A, Moss GA, et al. Aerosol filtra- 9. Wu X, Nethery RC, Sabath MB, et al. Air pollution tion efficiency of common fabrics used in respira- and COVID-19 mortality in the United States: tory cloth masks. ACS Nano. 2020;14(5):6339–6347. strengths and limitations of an ecological regression 28. ASTM International. F21019. Standard test method analysis. Sci Adv. 2020;6(45):eabd4049. for evaluating the bacterial filtration efficiency 10. Bourouiba L. Turbulent gas clouds and respiratory (BFE) of medical face mask materials, using a bio- pathogen emissions: potential implications for logical aerosol of Staphylococcus aureus. American reducing transmission of COVID-19. JAMA. 2020; Society for Testing and Materials; 2019. 323(18):1837–1838. 29. Pourdeyhimi B. Surgical mask particle filtration effi- 11. Liang D, Shi L, Zhao J, et al. Urban air pollution ciency (PFE). J Sci Med. 2020;2(3):1–11. may enhance COVID-19 case-fatality and mortality 30. Staff., F.G.f.I.a.F., Surgical Masks - Premarket rates in the United States. Innovation (N Y)). 2020; Notification [510(K)] Submissions; Guidance for 1(3):100047. Industry and FDA; 2004. 12. Cowling BJ, Zhou Y, Ip DKM, et al. Face masks to 31. ASTM F2299. Standard test method for determining prevent transmission of influenza virus: a systematic the initial efficiency of materials used in medical review. Epidemiol Infect. 2010;138(4):449–456. face masks to penetration by particulates using latex NANOCOMPOSITES 23 spheres. West Conshohocken, PA: ASTM 40. Ullah S, Hashmi M, Kharaghani D, et al. International, 2003. Antibacterial properties of in situ and surface func- 32. Wang D, Li K, Teo WK. Relationship between mass tionalized impregnation of silver sulfadiazine in pol- yacrylonitrile nanofiber mats. Int J Nanomedicine. ratio of nonsolvent-additive to solvent in membrane 2019;14:2693–2703. casting solution and its coagulation value. J Membr 41. Kajander EO, et al. Nanobacteria from blood: the Sci. 1995;98(3):233–240. smallest culturable autonomously replicating agent 33. Shu Z, Song Z, Zhi W. Sponge structure supporting on earth. InInstruments, methods, and missions for membrane for reverse osmosis composite mem- the investigation of extraterrestrial microorganisms. brane preparation research. J Chem Ind Eng. 2015; Int Soc Opt Photonics. 1997;311:420–428. 66(10):31991–33999. 42. Park WB, Kwon NJ, Choi SJ, et al. Virus isolation 34. Moarefian A, Golestani HA, Bahmanpour H. from the first patient with sars-cov-2 in korea. J Removal of amoxicillin from wastewater by self- Korean Med Sci. 2020;35(7):e84, made polyethersulfone membrane using nanofiltra- 43. Rengasamy S, Miller A, Eimer BC, et al. Filtration tion. J Environ Health Sci Eng. 2014;12(1):127–110. performance of FDA-cleared surgical masks. J Int 35. Moradihamedani P, Ibrahim NA, Yunus WMZW, Soc Respir Prot. 2009;26(3):54. et al. Separation of CO2 from CH4 by pure PSF 44. Macher JM. Positive-hole correction of multiple-jet and PSF/PVP blend membranes: Effects of type of impactors for collecting viable microorganisms. Am nonsolvent, solvent, and PVP concentration. J Appl Ind Hyg Assoc J. 1989;50(11):561–568. Polym Sci. 2013;130(2):1139–1147. 45. Yang S, Lee GWM, Chen C-M, et al. The size and 36. Li J-F, Xu Z-L, Yang H, et al. Effect of TiO2 nano- concentration of droplets generated by coughing in particles on the surface morphology and perform- human subjects. J Aerosol Med. 2007;20(4):484–494. ance of microporous PES membrane. Appl Surf Sci. 46. Saini V, Sikri K, Batra SD, et al. Development of a 2009;255(9):4725–4732. highly effective low-cost vaporized hydrogen perox- 37. Farnam M, Mukhtar H, Shariff A. Investigation of ide-based method for disinfection of personal pro- optimum drying conditions for pure PES mem- tective equipment for their selective reuse during branes for gas separation. Adv Environ Biol. 2015; pandemics. Gut Pathog. 2020;12(1):1–11. 9(27):326–331. 47. Grinshpun SA, Yermakov M, Khodoun M. 38. Ahmad MS, et al. Effect of solvents on the morph- Autoclave sterilization and ethanol treatment of re- ology and performance of polyethersulfone (PES) used surgical masks and N95 respirators during polymeric membranes material for CO2/CH4 separ- COVID-19: impact on their performance and integ- ation. In: IOP Conference Series: Materials Science rity. J Hosp Infect. 2020;105(4):608–614. and Engineering. Vol. 290; 2018. p. 0120734. 48. Cao J, Cheng Z, Kang L, et al. Patterned nanofiber 39. Arahman N, Maimun T, Bilad MR. Fabrication of air filters with high optical transparency, robust polyethersulfone membranes using nanocarbon as mechanical strength, and effective PM 2.5 capture additive. GEOMATE. 2018;15(50):51–57. capability. RSC Adv. 2020;10(34):20155–20161. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Nanocomposites Taylor & Francis

New generation washable PES membrane face mask for virus filtration

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NANOCOMPOSITES 2022, VOL. 8, NO. 1, 13–23 https://doi.org/10.1080/20550324.2021.2008209 RESEARCH ARTICLE a,b,c,d e f c d Md Eman Talukder , Fariya Alam , Md. Nahid Pervez , Wang Jiangming , Fahim Hassan , George K. g f c Stylios , Vincenzo Naddeo and Hongchen Song a b Shenzhen Institute of Advanced Technology, Chinese Academy of Sciences, Shenzhen, China; University of Chinese Academy of Sciences, Beijing, China; Water Science center, Guangzhou Institute of Advanced Technology, Chinese Academy of Sciences, d e Guangzhou, China; Department in Textile Engineering, Southeast University, Tejgaon, Bangladesh; Department of fashion Design & Technology (FDT), BGMEA University of Fashion & Technology, Turag, Bangladesh; Sanitary Environmental Engineering Division (SEED), Department of Civil Engineering, University of Salerno, Fisciano, Italy; Research Institute for Flexible Materials, School of Textiles and Design, Heriot-Watt University, Galashiels, UK ABSTRACT ARTICLE HISTORY Received 27 July 2021 Membrane materials might be used for face protection because they can decontaminate the Accepted 15 November 2021 inhaled air from particle pollution and viruses like the SARS-Cov0-2 which damages our res- piration system. In this study, plyethersulfone membranes (PES) were synthesized with green KEYWORDS solvent at room temperature and its filtration effectiveness was investigated against nano- Membrane filtration; PES bacteria (size 0.05 to 0.2 mm) by measuring their Bacterial Filtration Efficiency (BFE) and micro membrane; Corona-virus; aerosol size (0.3 mm), and Particulate Filtration Efficiency (PFE). The average SARS-CoV-2 microfiltration; nanofiltra- diameters are between 50 nm to 160 nm. A series of experiments were performed to accom- tion; air filtration; high plish between 0.03 to 0.21 mm PES sponge like diameters so that can be used for SARS-CoV- efficiency; fresh breathe 2 filtration. Results showed that nanofiltration/ultrafiltration could filter 99.9% of bacteria and aerosol from contaminated air the size of the Covid-19 molecule. GRAPHICAL ABSTRACT Highlights Covid-19 is still a pandemic and continues to spread A washable innovative PES membrane face mask and mutate becoming a major threat to public has been developed. health, infecting more than 219 M people worldwide The virus removal efficiency of the PES mem- with over 4.55 M deaths as reported on Oct 2021 brane face mask reaches 99.9%. [1,2]. Covid-19 might be transmitted from spit The PES membrane face mask is washable and droplets, airborne, fomite, fecal-oral, blood borne, reusable retaining its efficiency. and animal-to-human contact. Covid-19 may cause acute myocardial injury, severe pneumonia, and chronic damage, resulting in a mortality rate 1. Introduction between 1.5 to 2.5% [3,4]. Researchers examined the SARS-CoV-2 (the 2019 coronavirus pandemic size and content features of the SARS-CoV-2 par- (Covid-19)) is responsible for causing acute respira- ticles in addition to the mechanism of transmission. tory symptom, high contamination and death. Different studies have produced various findings CONTACT Md Eman Talukder eman-talukder@giat.ac.cn, 2654410096@mails.ucas.ac.cn Shenzhen Institute of Advanced Technology, Chinese Academy of Sciences, Shenzhen 518000, China; Hongchen Song hc.song@giat.ac.cn Water Science center, Guangzhou Institute of Advanced Technology, Chinese Academy of Sciences, Guangzhou 514480, China Supplemental data for this article is available online at https://doi.org/10.1080/20550324.2021.2008209. 2022 The Author(s). Published by Informa UK Limited, trading as Taylor & Francis Group. This is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. 14 M. E. TALUKDER ET AL. Figure 1. The filtration performance comparison among PES membrane, electrospun nanofiber membrane mask, N95 mask, and surgical facemask. when using electron microscopy to examine nega- exacerbated by very high demand, as a result of this, tive-stained SARS-CoV-2 particles, and reported while face coverings or homemade masks can help that the virus’s diameter ranges between 50 nm to to protect from bacteria, there is no scientific evi- 140 nm [5]. dence that they are effective against Covid-19 virus, Covid-19 virus primarily causes respiratory sick- mainly because most of them will have much bigger ness, ranging from moderate to severe, affecting the pore size than the Covid-19 virus. Pore size is one lungs and their function which might be lethal. of the most important parameters in the fabrication Whilst some people who are infected never show of masks for Covid-19, so that, the next generation any symptoms, they can infect others which is diffi- reusable and anti-virus nano pore filtration size cult to detect, but dangerous for spreading transmis- masks may be necessary [13]. However, reusable sion. Spit droplets and aerosols are mostly masks should prolong the use of the mask, not at important for the rapid spreading of Covid-19 [6,7]. the expense of filtration effectiveness. Anti-virus An infected person can release the virus via coughs masks can promptly shield as well as destroying the and sneezes [8]. According to recent studies, aero- virus in the filter of the mask, preventing virus sols and respiratory droplets ejected during sneeze/ retention [13–15]. The invention of such a novel cough can travel up to 12 to 26 feet [9,10], which is mask would aid us in dealing with epidemics such substantially further than the (CDC)- 6-feets social as COVID-19. distancing guideline [9,11]. In addition, droplets can Many researchers have reported on the fabrica- be stable in the air for an extended period of time tion of face masks by electrospinning and producing due to their micro-meter/nano-meter size and negli- nanofiber membranes. Zhang et al. employed melt- gible gravitational effect, posing a threat of airborne blown Polypropylene(PP) non-woven fabrics with a transmission, especially in enclosed spaces with fiber diameter of 0.5–10 mm[13,16]. Cheng et al. inadequate filtration systems. It was confirmed by reported on an electrospun polyetherimide non- the World Health Organization (WHO) that Covid- woven bi-functional material for an innovative face 19 is characterized as airborne and can remain 8 h mask [17]. Ultrafiltration or nanofiltration membranes, in the air, so people are asked to wear face masks to protect themselves and others from contamination whose width is measured in micro or nano-meters, in public places. are highly regarded for air filtration applications Before a significant percentage of the world’s due to the high surface area and sponge-like inter- population is vaccinated, wearing a mask in public membrane pore sizes less than 0.1 mm. These ultra- places might be the most effective weapon to reduce filtration or nanofiltration membranes supported the spread of the virus. Because of this reason, with a non-woven fabric might be a good candidate masks have become a necessity in every day’s life. for mask effectiveness, because it can possess high Commercial surgical face masks, and N95 masks level of air permeability promoting user comfort typically use melt blown non-woven tissue paper as and as well reuse [18,19]. Polyether sulfone (PES) is a virus filter sheet. PET (Polyethylene terephthalate) a soluble polymer, and the PES-based ultrafiltration melt blown nonwoven used mask can be worn only or nanofiltration membranes have shown high a few fours and then get disposed. [12], as shown in chemical resistance, thermal and mechanical stability Figure 1. Worldwide face mask shortages were and hydrophobicity, making them suitable for air NANOCOMPOSITES 15 filtration due to their nano sponge-like pore size bath, and the PES has successfully solubilized into distribution, while virus protection performance by the solvent at 60 C temperature. The 2 wt % PVP the pure PES membrane can be adjusted by the add- additives were used by continuous magnetic stirring ition of a catalytic process [20]. at 60 C temperature for 1 h or until a completely PES-based membrane products have an excellent clear and uniform solution was obtained. The homogeneous sponge-like pore size membrane hydrophobicity, surface charge, and roughness of structure. The sponge-like membrane pore size dis- the membrane are dependent on the blending ratio tribution mechanism is explored to improve virus of PES and PVP. Using a casting knife, the polymer filtration. The filtration performance of separation solution was then cast onto a glass plate, and the membranes with additional gradient structural cast film’s solvent was allowed to gently evaporate at change has been previously reported [21]. room temperature overnight. To complete precipita- Furthermore, because these virus particles are resist- tion and membrane development, the glass plate ant to inactivation procedures such as low pH, as in containing the cast film was gently submerged into the case of the reported parvovirus elimination a water bath for 6 h. Then, pure water is used as the [22,23]. When these membrane materials are washed coagulation bath, and the non-solvent induced phase and reused several times, and potentially the total separation method is used to obtain the PES flat membrane virus particle attachment maybe high to membrane by scraping. Prior to UF operation, the null, divergent flow filtering is preferable [22]. membranes were maintained in deionized water. This novel research introduces a washable and The PES membranes exhibit better antifouling abil- reusable innovative sponge-like structure with a ity and have a more sponge-like pore size structure non-woven supporting PES membrane for face because of the increase in positive polar charge mask use. The non-woven support PES membrane when the PES and PVP blend get in contact with face mask can effectively prevent the aerosol and the solvent. nano-bacteria/virus sized particles during the inhal- ing process. This novel material shows the following 2.3. Characterization advantages: (1) uniform pore size, sponge-like pore size distribution, and virus filtration by the non- The solution viscosity of the embrane sample was woven support PES membrane by phase inversion measured using a Rotational Viscometer (NDJ-8S via immersion precipitation method; (2) the filtra- Digital Viscosity Meter, Novel Scientific Instrument tion efficiency of particles (size of between 0.01 to Co., Ltd, China) at ambient temperature. Membrane 0.2 lm) and (3) the durability of the PES-based face sample contact angles were assessed using a TM TM mask with excellent working efficiency, which can dropmeter (dropmeter -A-300-main st vision, continuously protect from the virus more than 72 h. Kudos precision Instruments, USA). The mem- This novel work reports on a new efficient, wash- branes morphology was examined using scanning able, and reusable PES membrane for face mask electron microscopy (SEM) (Phenom XL, Phenom end uses. world, Thermo Scientific, Japan) at an accelerating voltage of 5 kV. Fourier transform infrared spectrum (FTIR) was recorded from 400 to 4000 cm-1 by 2. Experimental using (IR, Interspectrum, low noise DLATGS, FTIR- 2.1. Materials 920, Estonia). The thermal decomposition behavior of the membrane was studied using thermal gravi- This research was carried out using polyethersulfone metric analysis (TGA) (TG 209 F1 LibraV Netzsch (PES), ultrason E6020P (average M : 6 58 kDa,) company, United Kingdom), under a nitro- from BASF, Germany. PolarcleanV was purchased gen atmosphere. from Solvay Fine Chemical Additives (Qingdao) The prepared membrane pore size was deter- Co., Ltd., China. polyvinylpyrrolidone, (PVP)-K30, mined using prostate-specific membrane antigen-10 was purchased from Chemical Reagents Co., Ltd, (PSMA-10, Nanjing GAO Qian functional Materials China. The non-woven PET fabric was supplied by Technology Co., Ltd., and China). The pore volume Guocheng CO. (Wuxi, China). Sodium hydroxide (mL/g) at specific pore sizes (m) ranging from 0 to (NaOH) was obtained from Sinopharm Chemical 0.30 mm was measured for membrane air perme- Reagent Co., Ltd. (Shanghai, China). All chemicals ability and selectivity characteristics. Membrane and reagents were used without further purification. pore sizes were calculated from the smallest to the largest, with the mean flow pore diameter represent- 2.2. Membrane preparation ing the primary pore size. The thickness of the The membrane solution was prepared by dissolving membrane was measured with a digital micrometer a certain amount of PES in a PolarcleanV solvent Shanghai Liuling Hand-Type Qianfen Thickness 16 M. E. TALUKDER ET AL. Figure 2. (a) SEM image of PES membrane, (b) equal pore size distribution (sponge-like). CuCd Gauge CH-1-S Plastic Film Sheet Hand-Type Filtration efficiency ðFEÞ¼ (1) Thickness Gauge, which has a precision Cd of 0.001 mm. 2.5.1. Bacterial filtration efficiency (BFE) experiments The ASTMF 2101 standard Test Method was used 2.4. Tensile strength to evaluate the Bacteria Filtration Efficiency (BFE) Talukder et al. reported a procedure of tensile of the material. Here, biological nano-bacteria were strength for membranes [20]. The tensile strength used and, the virus filtration efficiency was tested by and elongation of five samples from each membrane obtaining the filtration percentage by comparing measuring 50 mm in length were measured at a con- between the nano-bacterial control counts and the stant elongation rate of 20 mm/min up to the break- test article effluent counts. The challenging part in ing points of the PES membrane using a tensile this test are the nano-bacteria (size 0.05 to 0.2 mm). strength tester KD-jjj model BA-100m by Transcell A nano-bacteria mixer liquid solution was passed Technology, China. throw to the filtration medium at a 28.3 liters per minute (LPM) flow rate [28] for 4 h at a 21 ± 5 C 2.5. Filtration efficiency (FE) temperature and relative humidity of 85 ± 5%. The Food and Drug Administration (FDA) issues 2.5.2. Particulate filtration efficiency (PFE) ASTM standards as the recognized standard in the According to the FDA guideline paper, the PFE of United States. ASTM F2100-11 (2011) is a funda- the various devices was tested with unneutralized mental standard that sets the performance require- 0.1 m PSL particles [29,30]. PFE testing was carried ments for respirators and face mask (3 Tips for out using the whole PES membrane mask material. Choosing the Right Face Mask) [24]. The ASTM According to the ASTM 2299 procedure, the test F2100-11 standard outlines the required characteris- velocity was between 1 and 25 cm/sec [27,31]. Prior tics and testing methods for the materials used in to testing, the test samples were preconditioned at the manufacture of face mask for use in hospitals, 30–50 percent relative humidity (RH) at 21 3 C health care, and patient care. In the 42 CFR Part 84 [31]. An automatic Particulate Filter Efficiency PFE certification process, there are several techniques for Tester GT-RA09 from GESTER INTERNATIONAL measuring filtration efficiency, including particle fil- CO. LTD. (China) was used to investigate the filtra- tration efficiency (PFE), bacterial filtration efficiency tion efficiency. Concentrations upstream and down- (BFE), virus filtration efficiency (VFE), and NIOSH stream of the respirator were monitored at a flow [25]. Material efficiency is linked to the PFE and rate of 80 L/min, with 2% accuracy. The user simply BFE techniques, which are employed as a barrier to needs to insert the filter paper in the fixture and protect the user from aqueous viral aerosols. The fil- push the button to change the test flow; the system tering efficiency test is carried out according to the will test the resistance and efficiency automatically ASTM F2100-19E1 methodology, which uses a via the controller. The PFE is calculated by equation nano-size salt aerosol/bacteria [26]. Eq. (1) is used (2). For each test material, the upstream count was to calculate the filtration efficiency of mask and res- measured before and after the downstream count. pirators, where Cu and Cd are the average particle Both upstream and downstream counts were meas- concentrations per each upstream and downstream test specimen [27]. ured three times for one minute each. NANOCOMPOSITES 17 Figure 3. Contact angle of PES membrane for the face mask (respectively 120.1 and 121.5 ). CuCd 3.3. Sponge-like structures adjustment control Particulate filtration efficiency ðPFEÞ¼  100 Cd As an excellent porogen, PVP can effectively (2) increase the porosity of the filter membrane and at the same time increase the hydrophilicity of the The PFE findings range from 1 to 99.99 percent, membrane. It is widely used in the preparation and where Cu and Cd are the averages of upstream and modification of membrane materials. The addition downstream counts. The greater the percentage, the of non-solvent additives, such as small inorganic better the mask filtration. For the PFE test, particle molecules and small organic molecules, has become sizes ranging from size 0.05 to 0.2 mm can be meas- an important method for adjusting the structure of ured. When comparing the test results, the particle membrane materials [20,32]. Additives can effect- size (e.g. size 0.05 to 0.2 mm) must be taken into ively affect the mass transfer rate of solvents and account, since using a particle with a greater size non-solvents, thereby forming different pore struc- might lead to a deceptive PFE evaluation. tures. This experiment uses PVP as an additive to control the structure of the polyethersulfone mem- brane material. 3. Results 3.1. Membrane characterization 3.4. Adjustment of membrane pore size and its The viscosity and electric conductivity of the solu- performance tions were 2465 mPa/S, and 1.4 mS/cm, respectively. The pore size and its distribution are important The morphology of the PES membrane was ana- indicators for the application of membrane materi- lyzed using SEM, as shown in Figure 2a. The PES als, which determine the filtration performance and membranes have a uniform structure with an aver- application fields of membrane materials. In this age membrane thickness at approximately 0.5 mm experiment, the effects of the solid content of PES and 0.3 mm, as shown in Figure 2a. The SEM image and the content of solvent in the casting liquid on shows the surface roughness of the PES membrane. the structure and pore size of the membrane were As shown in Figure 3, the PES membrane was investigated. Under the condition of ensuring cer- shown to exhibit hydrophilic behavior, with contact tain content of solvents and additives in the casting angles of 120.1 and 121.5 , as shown in Figure 3a liquid, the effect of solid content (PES mass frac- and b. tion) on the pure water flux of the PES membrane was investigated. The results are shown in Figure 2. It can be seen from the figure that as the solid con- 3.2. Pore size tent increases, the viscosity of the casting liquid Sponge-like pore size distribution of PES membrane increases, the force between the polymer molecules is depended on membrane diameter and on mem- becomes larger, the movement space between the brane fabrication environment such as temperature, polymer molecules becomes smaller, the double dif- humidity, coagulation bath temperature. The with- fusion speed between the solvent and the non-solv- drawing air pressure through the PES membrane ent becomes slower, the liquid phase separation rate was 145 to 200 kPa and shown a pore size distribu- becomes slower, and the structure of the prepared tion range of 0.03 to 0.21 lm. The pore size distri- PES separation membrane tends to be more dense bution experiment was reported 10 times and [33], which leads to a decrease in the pure water repeated an average pore size of 0.122 mm, as shown flux. And as the solid content of PES increases fur- in Figure 2b. ther, the viscosity of the material liquid becomes too 18 M. E. TALUKDER ET AL. Figure 4. (a) FTIR spectra of PES membrane, (b) TGA results of PES membrane. Figure 5. (a) XRD results of PES membrane, and (b) Tensile strength of PES membrane. large and the uniformity of the film formation membrane which is connected to PVP residue. PVP becomes worse. Therefore, the solid content is stretching vibration increased with increasing of maintained at 16% to 18%, which can ensure that PVP ratio from 1 wt% to 10 wt%, as illustrated in the PES membrane has good film-forming proper- Figure 4a. ties and pure water flux. Using Polarclean as a According to the TGA curves, the thermal solvent for membrane material preparation, and decomposition behavior temperature for the PES under the premise of ensuring the consistency of membrane was relatively stable up to 420 C (5% solid content and porogen, using acetone as the weight loss) [36]. As shown in Figure 4b, its thermal pore size regulator, the effect of PolarcleanV content degradation was demonstrated a one stage weight on the cross-sectional structure, pure water flux and loss. The PES membrane was stable up to 420 C rejection rate, pore size and pore size of the PES without significant weight loss, as compared to membrane was investigated. The results of the influ- 450 C for the pure PES membrane, concluding that ence of porosity are shown in Figure 2. adding PVP influences thermal degradation on the The FTIR spectra of the PES membrane is shown PES membrane [37,38]. in Figure 4a, and its functional group was analyzed The crystallinity of the PES membrane was ana- on different spectra. Four major peaks may be seen lyzed by WAXD, which shows the crystallinity prop- in the functionalized self-made membrane. Repeated erties of the PES membrane. As shown in Figure 5a, ether and sulfone linkages alternate between aro- the membrane was characterized as a typical matic rings in the PES. As a result, the stretching amorphous structure with peaks at 2h a.u. values vibrations of S ¼ O symmetric and S ¼ O asymmet- of 16–19 . ric may be ascribed to the bands at 1145 and 1261 cm , respectively [34]. And, the bands at 3.5. Tensile strength 1665 cm represent PVP’s amide group (OH). The spectrum of the PES/PVP membrane, on the other The tensile strength of the PES membrane is anes- hand, reveals that PVP was maintained in the mem- sential fact for face mask application, with its stress- strain properties shown in Figure 5b. The tensile brane structure. Another unique absorption peak at 1 1 1305 cm and 1663 cm is present in the C ¼ O properties and breaking elongation rate are functional group vibration stretching [35]. These enhanced because of the specific intermolecular peaks indicate the presence of PVP in the PES interactions by the additives in the PES membrane. NANOCOMPOSITES 19 The elongation at breaking point and tensile the number of viable nano-bacteria generated, the strength values are summarized in Table 1, with positive control system was employed without a PES 6.4 MPa tensile strength, and 77% elongation at membrane. On the triple side, the test system was break, [39] being higher than the ENM mask [40]. performed, and the negative control system was com- pleted without the nano-bacteria. And then, the nega- This rise could be attributed to the increase in PES membrane surface area. tive system was done by air sample in aerosol chamber on the triple part [45]. The average nano- bacteria size was 0.10 mm, which is the average size of 3.6. Virus filtration test Covid-19 virus droplets produced by coughing. The BFE method was modified, and Staphylococcus Bacteria filtration efficiency (BFE) was calculated by aureus (S. aureus) was replaced by nano-bacteria comparing the average positive hole number corrected (the hypothesized nano-bacteria are mostly 0.05 to of nano-bacteria captured after the PES membrane 0.2 mm in size) as the test specimen [41], which is mask, compared with the positive control. The BFE roughly similar to the SARS-CoV-2 diameter [42]. for each PES membrane mask was also calculated This precautionary change was applied to this without the largest size nano-bacteria, yielding an experiment, so that the chosen nano-bacteria can average nano-bacteria size of 0.1 mm[24]. This more represent SAR-CoV-2 [21]. 100 L of 8 10 PFU/mL accurately portrays the amount of inhaled aerosol nano-bacteria is used in sterile water at a flow rate reaching the lower respiratory system and alveolar of 28 L/min through the membrane (shown in region of 0.3 mm. Figure 6) under normal respiration range and cas- cade impact or constraints [43]. The filtration pres- 3.7. Particulate filtration efficiency (PFE) sure was kept at 35 kPa throughout the suspension. The particulate filtration efficiency was tested by Nacl Nano-bacteria was passed through the membrane testing methods with adjusting the rotary flow rate face mask on E. coli (Escherichia Coli) plates within 20 mg/m . When the upstream concentration is stabi- the 6 stage cascade impactor. The E. coli plates were lized, it automatically changes into the downstream incubated overnight at 37 C. The control plaques concentration test, and the curve is observed. When could enhance the performance of the PES mem- the downstream concentration is stable, the experi- brane, and the positive hole correction of multiple-jet ment starts counting until the end. The results reveal impactor was counted and recorded [44]. The positive an upstream concentration of 20.900 mg/m and hole was calculated for each of the 6 stages and added downstream concentration 0.243 mg/m ,producing together. The average number was counted. To assess 99% filtration efficiency, as shown in Figure S1. Table 1. Tensile strength and elongation (%) of PES membrane. 3.8. Hepa PES membrane mechanism Membrane type Tensile strength (MPa) Elongation (%) PES membrane 6.4 77 A HEPA filter is designed to collect very small par- ENM mask [40] 4.1 38 ticles and does not operate like a normal membrane Figure 6. Bacteria filtration efficiency process and apparatus according to ASTM. 20 M. E. TALUKDER ET AL. five cycles. After five recovery cycles, the Filtration Efficiency of the PES membrane decreased by 50%, showing that the PES membrane can be used after washing. 4. Discussion Handling, appearance and skin comfort of the PES membrane are good because it is soft, smooth, dust free and not irritating to the nose and face. Fabricated PES membranes show hydrophobic behavior, which could be used for face masks. The average coronavirus diameter ranges between 50 to 160 nm and those sizes could be filtered via the sponge-like pore size (0.03. ton 0.21 mm) of this PES Figure 7. PES membrane virus filtration efficiency against membrane. Moreover, its tensile strength is two or washing cycles. three times higher than any ENM [40,48]. After weighing, the membrane was found to provide filter, which captures particles bigger than the filter’s enough virus protection. More importantly PES pore size. Instead, HEPA filters capture particles membrane is capable of filtering aerosol and bac- using a mixture of three methods. Interception is teria with 99.9% efficiency, by its ability to filter the first process, in which particles are transported particles from air streams. They could be essential in the airflow around the filter fibers attached to the component in respirator and face mask fil- filter. To be collected, particles must be within one ter materials. radius of the filter fiber. The second process, impac- tion, is frequently used to collect larger particles. 5. Conclusion Because of their size, these particles are unable to respond to abrupt variations in airflow around the With the Covid-19 epidemic, face masks and respi- filter, and instead rush towards and embed them- rators ware becoming an everyday necessity poten- selves in the fibers of the filter. Diffusion is the last tially for years to come. PPE is subjected to a range process, which happens as a result of how tiny par- of tests to assess its performance and suitability ticles travel and interact with surrounding mole- under various conditions. The PES membrane has cules. Brownian motion describes how molecules soft handle and smoothness and does not irritate move in a random, zig-zag manner as they clash the skin around the face. This study has demon- strated the high filtration efficiency of the PES with neighboring molecules. membrane. The PES membrane was used in a direct flow configuration. The filtering surface of asym- 3.9. Washable and reusable metric membranes served as the downstream mem- Ethanol is an extensively used disinfectant, and has brane surface. To achieve optimum rejection of viral been shown to lower coronavirus infectivity by a particles and passage of product species, the mem- factor of four or more [46]. Although masks cleaned branes must have a very narrow pore-size distribu- by soaking in 70% ethanol for 2 h had no effect on tion. When constructing viral filters to exclude DP, they did exhibit a significant drop in BFE [47]. small parvovirus particles, this is very crucial. This The filter efficiency distribution across particle sizes PES membrane can be used for face masks and has appeared to be affected by ethanol treatment, with the potential of being certified for use to protect the MPPS changing from 0.03-0.21 mm to 0.05- against contamination. 0.23 mm pre- and post-treatment [47]. The reusing conduct of the PES membrane was Disclosure statement researched during five progressive reuse cycles to No potential conflict of interest was reported by explore PES membrane execution. The used PES the authors. membrane was recuperated by shaking in 1.0 mol/L NaOH arrangement at 50 rpm for 0.5 h, followed by centrifugation. The recovered adsorption limit of Authors’ contributions the PES membrane has appeared in Figure 7. The MET has conceived the idea, conducted the experiments, reused PES membrane capacity stayed flawless for and written the initial draft. MET, FA, MNP, WJ, FH, the initial two cycles and somewhat dropped after GKS, VN analyzed the data and prepared the final draft. NANOCOMPOSITES 21 HS has administered the project. All authors have read (Bangladesh) under the supervision of Prof Syed Fakhrul and approved the manuscript. Hassan. After that, he secured Color Root (Hubei) Scholarship to pursue his MSc studies in Textile Engineering at the Wuhan Textile University (China) in Funding 2016. During his MSc studies, he worked on dye waste- water treatment by Fenton catalytic system in the group This work was supported by the Guangzhou Institute of of Prof. Felix Y. Telegin (Russia). Afterwards, he worked Advanced Technology, Shenzhen Institute of Advanced as a visiting researcher at the Heriot-Watt University Technology, CAS, and China. The authors are also grate- (UK, 2016-2017), Vilnius University (Lithuania, 2018). ful to the Shenzhen Institute of Advanced Technology, Currently, he is a doctoral candidate at the University of the Chinese Academy of Sciences, Shenzhen, China, for Salerno (Italy) under the supervision of Prof. Vincenzo supporting this research. This research work was funded Naddeo, and he spent one year research period at the by the Shenzhen Science and Technology program (grant University of Boras (Sweden, 2020). His current research number: KCXFZ 2021221173402006). In addition, we focuses on the development of sustainable materials for would like to express our sincere gratitude to the support environmental applications. from the Sanitary Environmental Engineering Division (SEED) and grants (FARB projects) from the University Jianming Wang received the B.S. degree in Polymer of Salerno, Italy, coordinated by prof. V. Naddeo. The material and Engineering from Yaitai University, Yaitai, PhD School in “Risk and Sustainability in Civil China in 2009 and the M.S. degree in Materials Science Engineering, Environmental and Construction” is also and Engineering from Tiangong University, Tianjin, acknowledged for the scholarships (cycle-XXXIV) of China in 2012. In 2012, he joined Guangzhou Institute of M.N. Pervez. Advanced Technology and engaged in scientific research. He research interests include preparation and application of separation membrane, material modifica- Notes on contributors tion technology. MD Eman Takukder: During my undergraduate study, Fahim Hassan: For as long as I can remember I’ve known my major was in textile Engineering. Although my grades what I wanted to do with my life. Dedicating my life to were among the highest top 10, CGPA 3.81 out of 4.00 improving the lives of others is very appealing to me. Scale, I received a merit scholarship every semester. I had This is Fahim Hassan. I hold a [four year] Bachelor’s completed my undergraduate research project on the tex- Degree in Textile Engineering from Southeast University; tile dyeing section. This sector is also related to waste- Dhaka, Bangladesh, with a CGPA of 3.12 out of 4.00. I water treatment plant ETP (Effluent Treatment Plant). was amongst the top 50 students of my class of 120 stu- However, besides some cognition, what I gained from my dents. I have been, in the past, amongst the top rankers school education was a significant self-discovery. My in the entrance tests conducted by the academic institu- under-graduation and post-graduation study of medium tion of my education. Our university is considered to be of instruction and examination is English. In June 2015, I the one of the best university in my country for “Textile got Wuhan Textile University President Scholarship. Now Education” as a cradle for making the excellence of I am doing a research-based master’s degree within the Textile leaders. major of Textile Chemistry with the department of the Prof. George K. Stylios: I come from a textile business College of Chemistry and Chemical Engineering at background in Greece and studied in the UK. I completed Wuhan Textile University, China. My master thesis my postgraduate studies in Leeds and then went onto my research was done under the famous Chinese professor MSc and PhD, which were funded by M&S and their sup- Dr. Jinbo Yao Dean of College of Chemistry and pliers. I completed my PhD in 1986 and became a lec- Chemical Engineering, the preparation of layer by layer turer in clothing at Bradford, and then became a fellow of electrospun membrane-based wound dressing for skin the Science and Technology Agency in Japan in 1991 injuries treatment and stem cell tissue regeneration engin- before returning to Bradford in 1992. I obtained my per- eering by electrospinning process. I also had done one sonal chair in industrial engineering systems at Bradford project in my first year with my friend by using of mem- in 1994 whilst continuing research in textile objective brane bioreactor to remove the antibiotics micropollutants measurement applied at the textile and clothing interface. from wastewater. I have completed my master degree by In 1999 I joined the School of Textiles and Design at securing 2nd position in among all international students Heriot-Watt University as Professor of Textiles and I’m (CGPA 3.89 out of 4.00 Scale). Approximately in Oct currently Director of TechniTex and the Faraday 2021, my Ph.D. graduation will be completed from Partnership in Technical Textiles. Shenzhen Institute of Advanced Technology, Chinese Academy of Sciences with the project of Fabrication and Prof. Vincenzo Naddeo is Director of the Sanitary improving the membrane performance for wastewater fil- Environmental Engineering Division (SEED) at the tration and purification by using the Computational Fluid Department of Civil Engineering of the University of Dynamics (CFD) module. Salerno (Italy), where he drives research and academic activities in the Environmental Engineering fields. He FariyaAlam: I am doing my BSc degree in Textile serves as an affiliate professor at both the Department of Engineering at the BGMEA University of Fashion & Civil and Environmental Engineering of the University of Technology (Bangladesh). My current research focuses on Washington (Seattle, WA, USA) and at the Department the development of textile fashion and design sustainable of Water Resources and Environmental Engineering of textile product for environmental applications the Tamkang University (New Taipei City, Taiwan). His Md. Nahid Pervez received his BSc degree in Textile research focuses on advanced water/wastewater treatment, Engineering (2014) at the Southeast University characterization and control of environmental odours and 22 M. E. TALUKDER ET AL. environmental impact assessment (EIA). He developed 13. Zhang Z, Ji D, He H, et al. Electrospun ultrafine advanced biological processes for wastewater treatment fibers for advanced face masks. 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Journal

Nanocomposites – Taylor & Francis

Published: Dec 31, 2022

Keywords: Membrane filtration; PES membrane; Corona-virus; microfiltration; nanofiltration; air filtration; high efficiency; fresh breathe

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