INTERNATIONAL JOURNAL OF OCCUPATIONAL SAFETY AND ERGONOMICS 1997, VOL. 3, NO. 3-4, 141-149 Investigation of Blended Fibre Filtering Materials Izabella Kruciriska Stawomir Zakrzewski1 Irena Kowalczyk Jadwiga Wisniewska-Konecka Technical University of Lodz, Poland 1 Central Institute for Labour Protection, Poland Five variants of mixtures of different synthetic fibres at different area ratios were manufactured into needled nonwovens intended to be used as a filtering material for respiratory protection. Two variants were produced according to an earlier patent, and the contents of the other three was completely new. Samples of the nonwovens were tested for sodium chloride particles penetration and for breathing resistance. The results showed that one variant of a nonwoven, designated PP/PPFM, had very valuable filtering properties and that those properties were stable in time. filtering material respiratory protection nonwoven triboelectrical exchange aerosol penetration breathing resistance 1. INTRODUCTION Electrically charged filter m aterial has had a history of several decades, since the Hansen filter had been invented (Brown, 1993; Gradori, 1984; Hansen, 1931; W arych, 1994). The advantage o f this type of m aterial results from the fact that the charge on the fibres considerably augments the filtration efficiency w ithout increasing the resistance to air flow. These features, that is, high filtration efficiency and low resist ance to air flow play a key role in the designing of filtering m aterial m anufacturing process. Various types of electrically charged m aterials are available (Brown, 1993; W arych, 1994) on the m arket at present. They can be classified into the following groups: materials charged by corona - split-flbre m aterial, - m aterial charged as a whole, materials charged by induction - fine-fibre m aterial provided from a solution, - fine-fibre m aterial provided from a melt, Correspondence and request for reprints should be sent to Slawomir Zakrzewski, Central Institute for Labour Protection, ul. Wierzbowa 48, 90-143 Lodz, Poland. 142 I. KRUCINSKA, S. ZAKRZEWSKI, I. KOWALCZYK, AND J. WISNIEWSKA-KONECKA materials charged by triboelectrical exchange - resin wool m aterial, - mixed-fibre m aterial. A corona discharge is a common means of applying electric charges to polymers (Ando, T akahashi, Togashi, & Okum ara, 1990). The first type of m aterial from this group is m ade from a corona-charged sheet of polypropylene shredded into fibres. This m aterial was described in detail by van T urnhout, van Bochove, and van Veldhuizen (1976). The second type of electret material is also made from polypropylene fibres but is charged by a corona discharge in felted form (Baumgartner, Loeffler, & U m hauer, 1985). Induction o f charge is the second form of an electric charging mechanism used in filtering m aterial technology. Fine-fibre m aterials provided from a solution or a melt belong to the group of m aterials that are charged during electrostatic extrusion. M ore inform ation concerning the fine-fibre filtering m aterial produced by electro static extrusion of a solution of polycarbonate is presented in the literature (Brown, 1993; Schmidt, 1980). A description of m aterials produced by electrostatic extrusion of a m elt of polypropylene has also been published (Trouilhet, 1981). The last group consists of a m aterial charged by triboelectrical effect. The oldest filter m aterial, charged by triboelectrical charge exchange, was m ade from a m ixture o f wool noils and particles of natural resin. This m aterial is called H ansen’s filter (Hansen, 1931) and has been described in detail (Felthman, 1979). D uring carding, wool fibres develop a positive charge and resin particles develop a negative one. In the 1980s, Brown and coworkers in the United Kingdom and G radon in Poland elaborated a new class of filtering m aterials called blended fibre filter m aterials (Brown, 1984; Brown, 1986; G radon, 1984; Smith, East, Brown, & W ake, 1988), which are related to the concept of the Hansen filter. These m aterials consist of a m ixture of two synthetic fibres charged by triboelectrical charge exchange during carding. One com ponent of the m ixture develops a positive charge and the other develops a negative one. The m ixture invented by Brown (Brown, 1986) comprises a blend of clean fibres of a substituted addition polymer containing chloride and cyanide groups. A nother m ixture developed by Carl Freudenberg Com pany (Brown, 1993) consists of bicom ponent polypropylene-polyethylene and polyacrylonitryle fibres (PP-PE/PAN ). In Poland, research on blended fibre mixtures, initiated by the Central Institute for L abour Protection, has been carried out for the last 2 years. The first positive results of the experiments on blended fibre filtering m aterial were obtained and published 2 years ago (Krucinska, Zakrzewski, K ot, & Brochocka, 1995). According to those results, the best efficiency of filtration was achieved for the filtering m aterial composed of polyvinyl chloride fibres and polypropylene fibres blended together in a 50/50 area ratio. On the basis of those results the following research was undertaken to clarify the influence of fibre m ixture content on the efficiency o f filtration. The second series of investigations showed that there was a problem with the repeatability of aerosol penetration results characterizing the investigated filtering materials. Therefore, this research was aimed at finding the best type of m ixture of fibres, which would guarantee the stabilization o f charge on m aterials m anufactured at various ambient conditions and preserve the same level of charge after a certain period o f time. BLENDED FIBRE FILTERING MATERIALS 143 2. MATERIALS M aterials consisted o f two variants of filtering m aterial produced from fibrous m ixtures, according to Brown and Carl Freudeberg Com pany’s patent specification. Additionally, three new blends of fibres were used for filtering m aterial preparation. The characteristics of the fibres used are presented in Table 1 and the characteristics of nonwovens m anufactured according to the procedure described further are listed in Table 2. TABLE 1. Characteristics of Fibres Symbol of Fibres Type of Fibres Polypropylene Shape of Cross-Section Linear Density (dtex) Length (mm) 40 PP round 2 .8 Polyvinyl chloride PVC bilobal 4.2 60 Polyacrylonitryle PAN round 3.3 60 5.0 60 Polypropylene/ Polyethylene PP/PE round Component PPFM PPFM round Note. PPFM— polycondensational polymeric fibrous material. 3. MANUFACTURING PROCESS Commercially produced synthetic fibres are normally covered with “spin finish,” which is a m ixture of a lubricant and an antistatic agent. To produce triboelectrical effect, this spin finish should be removed before carding. This can be done before or after the opening process. Any of the usual processes of textile scouring could be used, for example, detergent, alkali, or solvent scouring. In our research, all fibres were scoured using a non-ionic detergent and they were well-rinsed afterwards. A fter washing, fibre flocks were opened by a rag machine. The prepared m ixtures of fibres were carded into fleeces and then the fleeces were needled into felts. As a result of the m anufacturing process, a set of blended fibre filtering m aterials were obtained. TABLE 2. Characteristics of Blended Filtering M aterials Type of Mixture Area Content of Fibres Number Mass Density (g/m2) PP/PVC PP/PVC 30/70 series I 494 30/70 PP/PPFM PP/PPFM 30/70 series II series I 477 533 30/70 50/50 series II series I PP/PPFM 523 PP/PPFM 50/50 series II 534 554 PP-PE/PAN 30/70 series I 546 Note. PP— polypropylene, PVC— polyvinyl chloride, PP-PE/PAN— polypropylene polyethylene polyacrylonitryle, PPFM— polycondensational polymeric fibrous material. 144 I. KRUCINSKA, S. ZAKRZEWSKI, I. KOWALCZYK, AND J. WISNIEWSKA-KONECKA 4. EXPERIMENTS AND RESULTS The m ain requirem ent for the new type of particle filter m aterial to be approved as a raw m aterial for antidust respiratory protection, is that it should not exceed the defined value of standard aerosol particles penetration. The filtering m aterial should satisfy the requirements in the EN 143 standard (Comite Europeen de N orm alisation [CEN], 1990). This standard describes the methods of evaluating the initial penetration of standard aerosols, breathing resistance as well as other properties im portant for the user. Values o f penetration and breathing resistance are used as a basis for filter classification. According to the EN 143 standard, one of the standard aerosols is the sodium chloride aerosol, which is produced as a polydisperse aerosol with a mass m edian particle diam eter of about 0.6 pxn. Tests are carried out at the specified volume air rate of 1.6 dm 3/s or 0.8 dm 3/s for filters intended to be used with a twin-filter facepiece, taking care that the whole working surface of the filter takes part in the filtration process. Penetration is calculated according to the form ula p = — x 100% Ci where, Ci is the sodium chloride concentration before the filter, C2 is the sodium chloride concentration after the filter. To assess the m anufactured filtering m aterial, samples were tested for sodium chloride particles penetration and for resistance to air flow. In each case, three m easurem ents were m ade and the results were averaged. To com pare different variants o f the m anufactured m aterial, tests of penetration were carried out at the air linear velocity of the aerosol passing through the sample equal to 0.1 m /s. The diagram of the rig for testing penetration is presented in Figure 1. Sodium chloride w ater solution dispersion was produced in a Collisson atomiser at conditions 8 Figure 1. Diagram of measuring rig for sodium chloride particles penetration. Note. 1— co m p re sse d air, 2— filter, 3— ae roso l g e n e ra to r, 4— m e a s u rin g ch a m b e r, 5 sam p le , 6— m a n o m e te r, 7— valve, 8 — flow m eters, 9— flam e p h o to m e te r. tested BLENDED FIBRE FILTERING MATERIALS 145 allowing to obtain an aerosol of a mass m edian of particle diam eter 0.6 /an, after w ater evaporation. The geometrical average value of the particle diam eter was equal to dg = 0.18 /an, with natural logarithm o f standard deviation In <Sg = 0.65. The tested samples— circles— of 0.1 m in diam eter allowed to obtain a volume air rate equal to 0.8 dm 3/s, the same as for twin filters according to CEN (1990). The m easurem ents of resistance to air flow were carried out at the same linear velocity of air flow 0.1 m /s. To investigate the influence of preconditioning on filter efficiency, before testing, the samples were exposed for 24 hrs to atmospheres of three relative humidities: 20, 65, and 100%. To investigate the stabilization of the filtering m aterial effectiveness in time, all tests were repeated after 5 m onths. D uring the period of storage, ambient room conditions were m aintained. The results of aerosol penetration and resistance to air flow of the tested filtering m aterials obtained in both series of measurements are shown in Table 3. Table 4 presents the results of sodium chloride penetration and resistance to air flow for filtering materials m anufactured according to Brown and Carl Freudenberg Com pany’s invention, as well as for other tested blended nonwovens. TABLE 3. Sodium Chloride Penetration, Breathing Resistance, Mass Density, and Humidity of Fleeces for Two Variants of Fibre Blends Manufactured at Specified Ambient Conditions Type of mixture PP/PVC Penetration at 0.1 m/s (%) 4.87 Breathing resistance at 0.1 m/s (Pa) Mass density (g/m2) Humidity of fleeces (%) Ambient conditions temperature and relative humidity 30.0 494 5.66 21 °C 30/70 series 25% 1 PP/PVC 1 1 .2 0 43.0 477 6.23 30/70 25 °C 23% series II PP/PPFM 1 .2 0 37.7 523 1.28 30/70 series 21 °C 17% 1 PP/PPFM 30/70 1.90 35.0 533 2.23 23.5 °C 17% series II Note. PP— polypropylene, PVC— polyvinyl chloride, PPFM— polycondensational polymeric fibrous material. 146 I. KRUCINSKA, S. ZAKRZEWSKI, I. KOWALCZYK, AND J. WISNIEWSKA-KONECKA TABLE 4. Sodium Chloride Penetration and Breathing Resistance of Tested Filtering M aterials Breathing resistance at 0.1 m/s (Pa) Penetration at 0.1 m/s (%) Type of mixture dry 65% after 5 months new after 5 months new wet dry 65% wet dry 65% wet dry 65% wet PP/PVC 30/70 5.18 4.87 6.24 4.16 4.49 5.60 32 30 28 33 34 30 1.19 1 .2 0 1.67 0.79 0.81 1.90 38 38 34 38 39 35 1.81 2.04 2 .2 2 1.87 1.48 2.35 45 42 47 48 51 43 32.80 29.50 36.70 — — — 36 40 39 — — — 494 g/m 2 PP/PPFM 30/70 523 g/m 2 PP/PPFM 50/50 554 g/m 2 PP-PE/PAN 30/70 546 g/m 2 Note. PP— polypropylene, PVC— polyvinyl chloride, PP-PE/PAN— polypropylene polyethylene polyacrylonitryle, PPFM— polycondensational polymeric fibrous material. 6. DISCUSSION The results presented in Table 3 point to the lack of m easurem ent repeatability of sodium chloride penetration, particularly in the case of a m ixture of polyvinyl chloride and polypropylene fibres. To find the reason, further investigations were undertaken and the relative air humidity during production and the hum idity of fleeces were controlled. It turned out that the penetration of filtering m aterials composed o f PP/PV C fibres, m anufactured at similar ambient conditions but from fleeces of different humidity, changes. This might be a consequence of the greater discharging caused by the great am ount of m oisture in fleece. This would m ean that the final result is very sensitive to the humidity of raw m aterial and the whole process of m anufacturing should be carried out in conditions of very low relative air hum idity. Therefore, further investigations were undertaken to find out another m ixture, which would give better results of penetration, less dependent on the hum idity of fibres. The new m ixture composed of polycondensational polymeric fibres (PPFM ) and polypropylene fibres (PP) was m anufactured to produce filtering m aterial and was tested for sodium chloride penetration and breathing resistance. The results of the tests of this m ixture are presented in Table 3 and illustrated in Figure 2. The new m aterial is characterized by better filtration efficiency, which is m uch less sensitive to the changes of m oisture content in it. BLENDED FIBRE FILTERING MATERIALS 147 s? 10- c --------------------1------ — ...... 1-28 — i------ r — 2.23 ,------------------------------------ 5.66 6.23 Humidity of fleeces (%) □ PP/PPFM-series I □ PP/PPFM-series II ■ PP/PVC-series I □ PP/PVC-series II Figure 2. Influence of humidity of fleeces composed of various mixtures of fibres on aerosol penetration. A nother param eter characterizing the stability of the filtering m aterial properties is the penetration of aerosol measured after a certain time. The results presented in Table 4 and in Figure 3 indicate that in the case of two mixtures, that is, PP/PVC and PP/PPFM , sodium chloride penetration does not increase after 5 months. On the contrary, a slight decrease of sodium chloride penetration, especially for samples exposed, before testing, to atmosphere of relative humidity of 65%, was observed. New After 5 months ■ PP/PPFM-50/50 □ PP/PPFM-30/70 Figure 3. Sodium chloride particles penetration of blended fibre filtering m aterials measured directly after fabrication and after five months later. 148 I. KRUCINSKA, S. ZAKRZEWSKI, I. KOWALCZYK, AND J. WISNIEWSKA-KONECKA The com parative analysis o f penetration of sodium chloride particles through the filter m aterials composed of various type of mixtures indicates that the best results were obtained for filtering m aterials m ade of a mixture of PPFM and PP fibres, as illustrated in Figure 4. The good filtering properties developed during the carding of this m ixture are probably less sensitive to the humidity of the m aterial than the filtering properties of the PP/PVC mixture. However, the relative air hum idity during the production of this m ixture was lower than the relative air humidity during the production of the PP/PV C m ixture and this fact, as well as some variability of mass density, m ight also contribute to the final result. Penetration of the filtering m aterial m ade of the PP/PPFM m ixture depends on the content of the m ore conductive fibres in the m ixture. The higher the content of the m ore conductive fibres (PPFM ), the lower the value of aerosol penetration. In the case of the m ixture of PPFM and PP blended in a 70/30 ratio, penetration of aerosol takes the relatively low value of 1.20% for samples exposed to atmosphere of relative humidity equal to 65% before testing. Decrease of content of the m ore conductive PPFM fibres in a m ixture to the value of 50% , causes an increase of sodium chloride penetration to 2.04%. i PP/PVC 30/70 i ------- PP/PPFM 30/70 PP-PE/PAN 30/70 Figure 4. Comparison of aerosol penetration of various blended fibres filtering m aterials. The aim of the last part of the research was to find out if the relative hum idity of atm osphere to which the samples are exposed before testing, influences the filtering properties of the m aterial. In all cases, an increase of sodium chloride penetration for the samples exposed to saturated air (100% r.h.) was observed. This increase depended on the type of m ixture and changed from 8.8% for a m ixture of PP/PPFM blended in a 50/50 ratio to 39.1% for a m ixture of PP/PPFM blended in a 30/70 ratio. Despite the fact th at the change of penetration for samples exposed to saturated air was so distinctive, the filtering m aterial composed of PP/PPFM fibres was still relatively low. This could not be said about the samples constituted of biocom ponent polypropylene-polyethylene and polyacrylonitryle (PP-PE/PAN) fibres and samples m ade from the m ixture of PP/PVC fibres exposed before examination to saturated air. The change of resistance was negligible in every case. BLENDED FIBRE FILTERING MATERIALS 149 7. CONCLUSIONS M anufacturing nonwovens using certain fibre blends considerably augments the filtration efficiency w ithout changing the resistance to air flow of investigated m aterials in comparison to the filtration properties of one-component nonwovens or other blends of fibres. The improvement of particle capture efficiency results from the charge development on the surface of fibres by triboelectrical effect. 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