EP0695383B1 - Nachbehandlung von vliesstoffe. - Google Patents

Nachbehandlung von vliesstoffe. Download PDF

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Publication number
EP0695383B1
EP0695383B1 EP93910564A EP93910564A EP0695383B1 EP 0695383 B1 EP0695383 B1 EP 0695383B1 EP 93910564 A EP93910564 A EP 93910564A EP 93910564 A EP93910564 A EP 93910564A EP 0695383 B1 EP0695383 B1 EP 0695383B1
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EP
European Patent Office
Prior art keywords
web
precursor
fibers
pore size
nonwoven
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French (fr)
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EP0695383A4 (de
EP0695383A1 (de
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Charles B. Hassenboehler, Jr.
Larry C. Wadsworth
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University of Tennessee Research Foundation
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University of Tennessee Research Foundation
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Priority claimed from PCT/US1993/003090 external-priority patent/WO1994023109A1/en
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C3/00—Stretching, tentering or spreading textile fabrics; Producing elasticity in textile fabrics

Definitions

  • the invention refers to a method for lateral consolidation of and reducinq pore size of a web.
  • Meltblowing is a process for manufacturing nonwoven products by extruding molten thermoplastic resins through fine capillary holes (orifices) and blowing hot air on each side of the extruded filaments to attenuate and draw down the filaments.
  • the filaments are collected on a screen or other suitable collection device as a random entangled nonwoven web.
  • the web may be withdrawn and further processed into consumer goods such as mats, fabrics, webbing, filters, battery separators, and the like. Also, the consumer goods may be produced in line with the meltblowing line.
  • the present invention relates to the post-treatment of nonwoven webs to alter the filament spacing and structure of the webs.
  • filaments or “fibers” are used interchangeably herein, although “fibers” in nonwovens generally refers to discontinuous strands and “filaments” as continuous strands.
  • the present invention contemplate webs with continuous filaments and/or discontinuous fibers.
  • meltblown webs have a relatively broad distribution of fiber diameters.
  • Typical nonwoven webs produced by meltblowing have fiber diameters of 0.5 to 20 microns, preferably 0.5 to 8 microns, making them suitable for filtering out 5 micron particles at 80 percent efficiency or greater. It is known that filtration can be improved by practicing the web formation process to produce smaller and smaller diameter fibers while controlling other formation parameters such as porosity and thickness.
  • the fiber size can be produced in the order of 0.1 to 5 microns.
  • the process has the following disadvantages: low production rates, high energy usage.
  • efforts have been made to post-treat the webs by a variety of processes. Such efforts have included post calendering the web to improve, the tensile strength of the web, post electrification as disclosed in U.S. Patent 4,592,815 to improve filtration performance of the web, to name but two of such efforts. It is significant to note that none of these prior art techniques have been directed specifically at planar consolidation to reduce the size of the pores in the web.
  • U.S. Patent 4,048,364 discloses a process for drawing the meltblown web in the machine direction (MD) to produce a ten-fold increase in the tensile strength of the post-drawn web. It is significant to note, however, that the precursor web required in this invention contains relatively course fibers (10 to about 40 microns average fiber diameter) and polymer of low crystallinity. Low crystallinity generally means about 22% or less.
  • the extensive drawing of the web reduces the diameter of the fibers in the machine direction to an average diameter of 1 to 8 microns at draw ratios ranging from 2:1 to 10:1 and preferably 5:1 to 7:1.
  • the main purpose of the process is to increase the molecular orientation to enhance the strength of the greatly drawn fibers.
  • Precursor webs of very high post processing draw ratio capability are required in order to prevent rupture of fibers in the web drawing process.
  • U.S. 4,048,364 discloses a nonwoven web made from a precursor nonwoven web, said precursor web comprising randomly collected nonelastomeric fibers having and being uniaxially drawn and heat set, wherein the uniaxial heating and drawing are carried out continuously by passing the precursor web into an oven at a first linear velocity and withdrawing the precursor web from the oven at a second linear velocity and wherein the ratio of the second velocity to the first velocity includes the ranges from about 1.1:1 to 2:1, whereby a majority of the fibers are consolidated and aligned generally in the direction of draw and a minority of segments of fibers are disposed crosswise or transversely to the direction of draw and a method for forming such a web.
  • US 5,053,066 shows the use of a meltblown web for subjecting it to drawing under heat and to form randomly bundled pleats for a cigarette filter.
  • US 4,965,122 shows a reversably necked multilayer web material which has been necked by drawing at ambient temperature before being transported by heated rollers.
  • the invention provides a method for lateral consolidation of and reducing pore size of a web according to claim 1 and a nonwoven web made from a precursor nonwoven web according to claim 15.
  • a nonwoven web with certain properties and post-drawing the web under certain conditions, the fibers making up the web are restructured to provide the web with reduced pore sizes, and a narrower pore size distribution.
  • Such post-treated webs have unique measures of pore size, directional absorption and elastic recovery properties which make them ideally suited for a variety of end use applications such as filters, vacuum cleaner bags, protective apparel, face masks, diapers or sanitary napkin parts, wound dressings, respirators, wipes, chemical reservoirs, wicks, and surgical drapes.
  • the method of the present invention involves subjecting a bonded thermoplastic nonwoven web having a relatively low tensile extensibility during post processing (as reflected by a low draw ratio at break) to primary drawing under an elevated temperature.
  • This uni-directional drawing in the MD laterally consolidates the web to a great extent thereby reducing both the average pore size of the web and narrowing the pore size distribution.
  • the resultant web exhibits improved uniformity in pore size and high lateral elasticity characteristic of "stretch fabric" having approximately 120% elongation to break.
  • the nonwoven webs are firstly drawn under thermal conditions and secondly mechanically compacted to efficiently alter the geometric arrangement of the fibers making up the web resulting in web having reduced measures of pore size.
  • the web being drawn may be passed into supplemental mechanical compacting means to induce and/or refine the primary web consolidation.
  • meltblown and spunbond webs Although the present invention is described and exemplified in connection with meltblown and spunbond webs, it is to be understood that it has application with other nonwovens such as hydro-entangled, needled webs, and laminated combinations of these and with other web forms such as air laid, etc.
  • the present invention relates to the post-treatment of a precursor nonwoven web to reconstitute or restructure the fibers of the web and reduce the measures of pore size.
  • nonwoven as used herein means randomly laid fibers or filaments to form a web wherein some of the fibers are bonded by fiber-to-fiber fusion or fiber entanglement, or thermal bonds as by point bonding.
  • pore size means a quantification of the physical dimensions of channels oriented in a generally normal direction to the plane of the web. The pore size values recited herein are based on standard test method ASTM F 316-86. Embodiments and values not falling into the scope of the claims are comparative.
  • the present invention described with specific reference to the preferred webs will be meltblown webs; it is to be emphasized, however, that the method and product produced thereby includes other nonwoven webs, specifically spunbond, hydro-entangled, needled webs and laminated combinations of these. Also the web produced according to the present invention used in combination with other webs or substrates such as webs from elastomeric polymers, microporous films or stretch limiting materials post laminated to limit the CD extensibility to less than 100% provide additional performance properties for added utility.
  • Meltblowing is a well known process which generally utilizes equipment depicted in the schematic of Figure 1.
  • the process is carried out by introducing a thermoplastic resin into a extruder 10 where the polymer it is heated, melted, and extruded through a die 11 to form a plurality of side-by-side filaments 12 while converging layers of hot air (discharging from slots 13 on each side of the row of filaments) contact the filaments and through drag forces stretch and attenuate the filaments 12 to a micron-size.
  • the fibers 12 are collected onto a collector such as a rotating screen 15 forming a nonwoven web 17 which may be withdrawn on a take-up roller for later processing.
  • the collector 15 may include a vacuum screen wherein a vacuum, through line 18, is drawn by a vacuum pump 19.
  • the hot air (primary jet air) is introduced into opposite sides of the die through line 14.
  • secondary air which is aspirated into the primary air/fibrous stream serves to cool the filaments discharging from the die 11.
  • the process in one embodiment of the present invention comprises the steps of (a) selecting a thermoplastic nonwoven precursor web with substantial fiber bonding and having relatively low processing extensibility and (b) passing the nonwoven web through a heated zone to increase the temperature of the web to its softening temperature while drawing the web in the machine direction (MD) thereby greatly plastically bending the cross direction (CD) fibers in the web which consolidates the web in the CD reducing the maximum pore size of the precursor web by at least 20 percent, and, more significantly, reducing the pore size distribution by at least 20%.
  • the precursor web must have certain properties to enhance consolidation.
  • Apparatus for carrying out a preferred process is illustrated schematically in Figure 2 wherein the precursor web 17 is unwound from roll 20 and fed through the nip of counter-rotating feed rollers 22, through oven 23, and finally through the nip of counter-rotating rollers 24.
  • the oven 23 is maintained at a temperature to heat the precursor web 17 to a temperature between its softening point and the melting point of the polymers in the web.
  • the web is heated to a temperature within 8,3°C (15°F) of its melting point.
  • the rotating rollers 24 are driven at a speed in excess of the rotating feed rollers 22 so that the output velocity (V2) of the web is in excess of the feed velocity (V1) for the draw ratio which is a function of the velocity ratio V2/V1.
  • the initial drawing of the web 17 under thermal conditions causes web to contract within the oven 23 from its feed width 17a as illustrated by web section 17b in Figure 2.
  • This contraction is due primarily to the plastic bending deformation by planar compression of generally CD fibers of the web thereby reducing the measures of pore size of the web.
  • the high MD tensile forces developed at low MD strain during drawing together with the network nature of the fiber-fiber bonds in the web augments the generation of enough compressive stress to easily bend most CD fiber segments 27 and compact the web in the CD as shown in Figure 6. Since fiber bending rigidity is related to the fourth power of the fiber diameter, only webs having small average fiber diameters can be consolidated by the available stresses with the associated reduction in pore size measures.
  • Average fiber diameter for meltblown webs are preferably less than about 9 microns, and less than about 50 microns for spunbonded webs.
  • the lateral contraction which results in pore size reduction is not accompanied by significant average fiber diameter reduction of MD fibers. Continued web stretching beyond that necessary for web pore size reduction may cause fiber diameter reductions.
  • the web is contracted to a minimum width 17c as the web 17 exits the oven 23 or as the web 17 passes the nip of rollers 24. It is preferred but not essential to cool or permit the web to cool between the exit of the oven 23 and the nip of the rollers 24 thereby controlling the heat set or annealing in the restructured fibers under stress.
  • the web 17 As the web 17 cools to between 130 and 90°C (for PP), the web can be electrostatically charged to impart durable enhanced filtration efficiency to the web products.
  • the nip of the rollers 24 and that of rollers 22 preferably are parallel so that the tensile force applied by rollers 24 and the resistance applied by rollers 22 are uni-directional [e.g., uniaxial]).
  • FIG. 3 shows one alternate web processing embodiment in which the web passes into a supplementary or alternative web compacting device consisting of a (tilted) section of a torus 25.
  • the consolidation interval of the web 17 and the torus bar 25 are heated in an oven or heated to provide the proper temperatures for drawing and consolidating the web.
  • the web enters the outboard surface (of diameter D) of the torus at width dimension 17d and exits near the inboard surface of the torus which has a lesser width dimension 17e.
  • the converging surface of the path around the torus applies transverse compressive forces in the plane of the web of entry width 17d.
  • the added compressive forces overcome the bending resistance of inefficiently deformed large CD fiber segments or shot imperfections remaining in the web 17 following primary consolidation (if used). This improves the uniformity in pore sizes.
  • the heating and stretching of the apparatus in Figure 2 (gross drawing) and Figure 3 (secondary drawing) can be carried out in series.
  • the primary heating-drawing step imparts gross consolidation while the secondary torus consolidator refines the processing.
  • the maximum compressive strain imparted to the web by traversing about 180° around the torus surface is given by (D-d)/D, where D is the outboard or entry perimeter related to the entry width 17d and d is the inboard or web exit perimeter of the torus 25.
  • the torus surface can be fixed or can be a rotatable curved flexible bar. A fixed torus 25 with an air bearing between the surface and the web allows high lateral compressive strain and low friction for additional MD draw. It should be noted that revolving "Bowed rolls" are only used in textile applications to remove wrinkles from a moving textile fabric by laterally stretching the fabric as the textile proceeds around a surface of diverging width.
  • Precursor Web A nonelastomeric nonwoven precursor web is selected based on its dimensions, and its hot processing tensile properties (VIZ., elongation-at-break). In general, the breaking draw ratio of the web during hot processing should be less than about 4.0 and greater than about 1.4 evaluated while hot drawing at a strain rate greater than 2500 %/min and temperature greater than the softening point but at least 5,6°C (10 °F) less than the polymer melting temperature. This is an important indicator of precursor molecular orientation state for achieving sufficient stresses for CD fiber buckling and bending to cause reduction of the measures of pore size distribution of the web by the process of the present invention.
  • the room temperature elongation (strain) at break should be between 2 and 40 percent, preferably between 5 and 20 percent, based on test method ASTM D 1117-77 using the Instron tensile testing machine.
  • the precursor webs disclosed in U.S. Patent 4,048,364 are totally unsatisfactory for use in the present invention because such precursor webs are characterized as having at least 50%, preferably at least 70%, standardized elongation before break, preferable max processing draw ratio greater than 5. Webs made up of low modulus, low crystalline (less than 22%), exhibit too much elongation at low tension in the heating and drawing step to permit development of the necessary stresses.
  • the webs useful in the process of U.S. Patent 4,048,364 have far greater maximum draw ratio than 4 under the hot draw condition described above. It is estimated that these draw ratios are greater than 5.
  • the precursor nonwoven web may be made from many of the thermoplastics capable of being melt blown, provided the polymer selected develops filaments of sufficiently high tensile processing modulus to permit the development of high lateral compression forces on the web.
  • the thermoplastic resins useable in the production of nonwovens includes the nonelastomeric polyolefins such as polyethylene, polypropylene including high density polyethylene, ethylene copolymers (including EVA and EMA copolymers with high tensile moduli), nylon, polyamides, polyesters, polystyrene, poly-4-methylpentene-1, polymethylmethacrylate, polytrifluorochlorethylene, polyurethanes, polycarbonates, silicones, polyphenelene sulfide.
  • the crystallinity of the precursor web preferably should be sufficiently high to provide a room temperature breaking elongation less than 40%.
  • Meltblown webs useable in the present invention should break at a strain of less than 40 percent in accordance with ASTM test method D 5035-90.
  • the crystallinity in the range of 30 to 70 percent is preferred.
  • the proper high modulus and state of molecular orientation of the precursor is best reflected by a maximum or breaking draw ratio of the web during post treating of less than about 4.0.
  • the thickness of the web should preferably be at least 50,8 ⁇ m (2 mils) and up to about 5,08 mm (200 mils).
  • the width of the web can vary within wide limits, with 127mm (5) to 3,81 m 150 inches being preferred.
  • the average fiber diameter of the precursor meltblown web will preferably range from .5 to 8 microns, with 2 to 6 microns being preferred in order to provide the proper range of processing tensile stiffness for PP web.
  • the porosity of the precursor web will normally be in the range of 50 to 95 percent. Calendered precursor webs approach 50%.
  • the precursor web includes at least some fiber-to-fiber bonding which is typical in meltblown webs.
  • the bonding can be achieved by inherent fiber-to-fiber fusion, or by point bonding, calendering, or by fiber entanglement.
  • the properties of the selected polymer can be controlled to a degree by operation of the meltblowing process.
  • the primary purpose of the process of the present invention is to consolidate the web in the cross direction to reduce the average pore size and the pore size distribution in the web. Consolidation of the web in the cross-direction is to be distinguished from consolidation resulting from calendering since consolidation to reduce thickness as in calendering flattens the fibers and closes flow channels, thus decreasing the permeability of the web to a greater extent compared to web draw consolidation.
  • this planar disposition may be represented by representative cells illustrated in Figure 5.
  • the fibers 26, 27, and 28 are shown interconnected or bonded as a loose network at junctions 29 of the fibers. Again, it is to be emphasized that the bonds are fuse bonded during the meltblown process, or by fiber entanglement, or by thermal point calendering techniques.
  • the intermediate fibers 28 are easily aligned in the MD thus reducing pore dimensions whereas the CD fibers 27 tend to resist compression of the cell in which it is associated and may buckle and bend as illustrated in Figure 6.
  • the lateral consolidation of the precursor web in accordance with the present invention leaves pore space throughout the web layer which depends on the extent to which CD fibers are buckled. Fiber having a high slenderness ratio of length by diameter buckle easier.
  • the compressive force on element 27 in Figure 6 is 2Tsin(theta) where T is the tensile force in elements 28 and ⁇ is the angle between element 28 and the MD. Without the bonding at junctions 29, the webs would easily rupture without generating lateral (CD) compression as in a carded web.
  • actual webs do not include only the idealized structure as depicted in Figures 4 and 5, there is sufficient bonding and stresses developed in the select precursor web to provide the reduced porosity following the thermal drawing process as in Figure 6 and 7.
  • buckled CD fibers 27 act as spacers limiting the residual porosity and pore dimensions developed by the resultant compression forces due to the MD tensile drawing force.
  • external mechanical means can be incorporated to further compress the hot drawn web near 17c in order to augment the CD fiber bending and buckling beyond that obtained by hot drawing alone.
  • Figure 3 One such apparatus embodiment is illustrated in Figure 3 described above in which the mostly drawn web is subjected to transverse compression forces because the web is tracking the converging surface of the torus.
  • the post-drawn web withdrawn from the oven and preferably heat set exhibits two surprising and highly useful properties: (1) the pore space and all measures of pore size distribution have been reduced, and (2) the web exhibits remarkable elasticity in the CD. These two properties will be discussed in detail later.
  • the post-drawing process conditions and precursor properties for achieving the web with the improved properties described above are as follows: BROAD RANGE PREFERRED RANGE BEST MODE Draw ratio, V2/V1 1.05 - 3.00 1.10 - 2.00 1.2 -1.80 Temperature, °F 165 - 425 250 - 350 275 - 300 (PP) °C 73.9 - 218.3 121.1 - 176.7 135 - 148.9 V1, Feed Speed, F/M 10 - 400 25 - 200 35 - 60 MAX pore size, ⁇ M 5 - 250 10 -150 20 - 50 Crystallinity, % 30 - 95 30 - 80 35 - 60 Thickness, mils 2 - 200 2 - 100 6 - 20 ⁇ m 50.8 - 5080 50.8 - 2540 152.4 - 508 Avg.
  • the precursor webs made up of any of the thermoplastic polymers used in meltblowing may be used, the following polypropylene precursor meltblown web has produced excellent results in experiments carried out at the University of Tennessee.
  • PP Grade Exxon Grade
  • the precursor web 17 in a generally flat disposition is processed according to the present invention by passing the flat web 17 in an oven 23 at a temperature between the softening and melting temperature of the polymer (e.g., for PP, about 154°C (130 degrees F.)).
  • the line speed and draw ratio are selected to impart the desired lateral consolidation of the web expressed as a ratio of the web width entering to web 17 width exiting the oven (c/a in Figure 2).
  • the c/a values should be from 1.3 to 4, preferably from 1.5 to 3, and most preferably 2 to 2.5.
  • Web thickness entering the oven may range from 50,8 ⁇ m (2 mils) to 2,54 mm (100 mils) and those exiting may range from between 50,8 ⁇ m and 3,81 mm (2 and 150 mils), indicating that the thickness may under certain conditions increase.
  • Draw ratios of 1.05 to 3.00, preferably from 1.10 to 2.00, and most preferably 1.2 to 1.8 may be used to achieve satisfactory consolidation.
  • Line speeds (V2) can range from 3,048 to 121,92 m/min (10 to 400 fpm). As mentioned above, webs capable of hot processing breaking draw ratios greater than about 4 are unsuitable.
  • the consolidated and annealed web leaving the oven be cooled, either by ambient temperature or supplemental air to impart a set to the fibers in the deformed condition.
  • the consolidated heat set web can be rolled up for later conversion to end use. products.
  • the web consolidation restructures the fibers of the web by aligning more of the fibers in the MD.
  • the fiber bonding transforms tensile stress into CD consolidation in the manner described above, thereby reducing all of the web's measures of pore size distribution.
  • measures of pore size distribution of the web are the maximum pore size (MAX), the mean flow pore size (MFP), and the minimum pore size (MIN) as measured by a Coulter Porometer, described below in connection with Experiments.
  • the Coulter Porometer produces a characteristic distribution - size plot for each web where pore size plotted against percent differential flow through the web.
  • Figure 7 compares the characteristic curve for a precursor web (Plot 31), and the characteristic plot for the consolidated web (Plot 32).
  • Plot 31 precursor web
  • Plot 32 consolidated web
  • pore size distribution ranged from 6 to 17.5 microns (a spread of only 11.5 microns), with the mean flow pore size of 9.4 microns.
  • the web consolidation according to the present invention thus reduced the spread of the pore size distribution from 25 to 11.5 microns and the average pore size from about 20 (Plot 31) to about 9 (Plot 32).
  • the maximum pore size (BP) was reduced from 38.7 to 17.5 microns.
  • the consolidated web exhibited excellent "stretch fabric" elasticity in the CD and tested extremely well as a filter.
  • Coulter Porometer - a semiautomated instrument using a liquid displacement technique to measure the pore size measures and distributions of a sample according to ASTM F 316-86
  • Web Pore Size Distribution the distribution of pore sizes between the maximum and the minimum pore size as determined by ASTM F 316-86 on the Coulter II Porometer. (The maximum pore size [or bubble point] measure is distinguished in that it strongly relates to permeability, pressure drop, and filtration efficiency performance properties for the entire family of meltblown webs we studied.)
  • ASTM 316 - 86 Measures of Pore Size Distribution - MAX is the standardized measure of the diameter of the largest pore channels in the distribution of pore sizes supporting flow through the web.
  • MFP is the measure of the median (or mean) pore channel diameter for the pores supporting the total flow.
  • MIN is the minimum pore size measured for the web.
  • Crystallinity the relative fraction of highly ordered molecular structure regions compared to the poorly ordered amorphous regions. Crystallinity is determined by X-ray or DSC analysis.
  • Polymer Birefringence - is a property which is usually observed in optical microscopes when a material is anisotropic, that is when its refractive index is directional. Fibers having molecular chains of higher axial directionality have higher birefringence and relatively low tensile elongation at break.
  • Softening Temperature - is a thermal property of a polymer characterized by a temperature at which the material becomes sticky, viscus, or elastic (soft) prior to melting and looses its room temperature modulus (and can undergo plastic elongation) leading to maximum molecular orientation and breakage.
  • Average Fiber Diameter - a measure of the mean fiber diameter of the fibers in the web obtained from individual measures of the fibers diameters in focus on a scanning electron micrograph of the subject fibrous web--about 100 fibers are measured. Finer fibers generally arise from greater draw-down in meltblowing and have higher birefringence.
  • Web Elongation at Break - for a crystalline polymer is strain rate and temperature dependent.
  • the elongation at break primarily measures the extent of a plastic deformation process beginning at the initial state and terminating at the final well ordered state of molecular orientation (MO) of the polymer.
  • Precursor webs having fibers of high crystallinity and order have low elongation to break (from R.J. Samuels, Structured Polymer Properties, John Whiley & Sons, 1973).
  • evaluating the precursor MO state by breaking elongation is best accomplished at high temperatures instead of at standardized ASTM D 5035-90 room temperature test because of the wide range in fiber diameters, MO state and bonding in meltblown webs.
  • meltblown precursor webs were characterized by the magnitude of the breaking draw ratio attained while hot drawing at a strain rate at least 25 min-1 (or 2500 %/min) and temperature at least 10 F below the melting temperature of the precursor thermoplastic polymer (Hot breaking draw ratio).
  • Web Tensile Modulus - is the measure of the force required to produce a small extension (or compression). A highly inextensible material will usually have a large modulus.
  • the slenderness ratio of fiber segments subjected to compression as well as the magnitude the bending forces developed by drawing are ultimately related to the above.
  • the post-drawing on the precursor web was done in experimental apparatus similar to that illustrated in Figure 2 and 3.
  • the rollers were provided with speed controls.
  • the polymer used in all of the tests was polypropylene (PP).
  • PP polypropylene
  • the PP precursor web samples used in the tests are described in TABLE I. Pore Sz. Measures, ⁇ m Sample % Air Packing Density Ave. Fiber Diam. ⁇ m Break Elong. Max MFP Min Break D.R.
  • the filtration efficiency was based on dry particulate capture efficiency test using nominal 1.0 micrometer mono dispersed latex particles at an aerosol flow rate of 10 centimeters per second (ASTM 1215).
  • Fiber diameters were measured by SEM photographs of the specimens.
  • Pore Space Measurements were based on weights of dry specimens and the weight of the specimen wetted out with a liquid of known density. Planar densification is evidenced by the increase in packing density (PD) measure of the web given by the ratio of dry web weight to the weight of the void-free web. Porosity of the web or pore space is given by one minus the packing density.
  • PD packing density
  • the tests for measuring elasticity of the consolidated web were as follows: Measured the percentage to which specimen recovered its original (CD) length immediately following a given % (CD) elongation, for example, sample A recovered 92 % of its original length following a 100% CD elongation.
  • Another test on the consolidated webs included directional absorption of liquids. Surfactants for improving the water wettability of the fibers were applied to PP webs prior to aqueous absorption tests. The surfactants were nonionic and other types such as nonionic polyoxyethylenated tert-octylphenol, anionic ammonium lauryl sulfate, and cationic sulfobetaines.
  • the maximum hot draw ratio is the magnitude of the breaking draw ratio during hot processing and solely defines the molecular orientation present in the filaments of the precursor melt blown webs.
  • Web of PP having a maximum DR greater than about 3.5 are not consolidated according to the present invention.
  • the data on Figure 9 indicates that filtration efficiencies improve significantly for fiber diameters less than 8 microns, particularly less than 6 microns, the preferred and most preferred fiber sizes.
  • Figure 8 is a plot of packing density (PD) versus average fiber diameter for the precursor and processed webs.
  • Figure 8 indicates that web densification or consolidation initiates in meltblown precursor webs having average fiber diameters less than about 8 ⁇ m for meltblown polypropylene webs.
  • MB webs from precursors having fiber diameters greater than about 8 microns experience little to no alteration in packing density (or other performance properties) according to the method of the present invention.
  • Other measures of web performance such as filtration efficiency, air permeability, and maximum pore size (see Table I, II and Table III) show similar response to web average fiber diameter as shown in Figure 9 for filtration efficiency. In the experiments, these properties were generally maximized by post treating at draw ratio between about 1.5 and 2.0 for the precursors.
  • Spunbond Webs As indicated above, the principles embodied in the present invention have application with nonwoven webs others than meltblown webs. For example, for spunbond webs which are characterized as having an average filament diameters of 7 to 50 microns and elongation to break less than about 200% according to ASTM Test D 5035-90.
  • the spunbond webs are prepared by melt spinning a multiplicity of filaments molecularly oriented by plastic deformation draw-down and depositing the same on a moving collector to form a random collection of uniform filaments arranged similar to that depicted in Figure 4. The deposited filaments are then bonded by mechanical entangling, needling, hot calendering or otherwise thermal bonding at a plurality of points to impart integrity and strength to the spunbond material.
  • bonding such as thermal or mechanical bonding is normally necessary since the filaments are not typically fused or sufficiently entangled upon being laid or deposited on the collector.
  • the bonding must be strong (such as high temperature point bonding) in order to locally elongate, buckle, and bend the filament segments without spoiling the web integrity (see Figure 5 and 6) because the drawn filaments have relatively high tenacity and modulus.
  • point bonding the bond points and bonding pattern generally are as follows: The area of heated bonding points are 5 to 25% of the roll area and the shape of the raised points can be diamond shaped or a number of other shapes and point distribution.
  • the consolidation of the spunbond (SB) web in accordance with the present invention occurs as follows: Hot drawing the SB web creates reduction in the measures of pore size and creates CD elasticity because the tensile forces generate sufficient compressive forces to plastically buckle and bend CD segments of the filaments for inve itive reduction of pore measures.
  • the elasticity in the CD direction is a result of elastic recovery from bending of the well bonded network of strong filaments arranged similar to that idealized in Figure 6.
  • Spunbonded web was 1 meter wide, 33,9 g/m 2 (1 oz/sq. yd.) produced from 35 MFR PP on a Reicofil machine bonded between 90 and 140°C at the University of Tennessee. Oven temperature 157,2 °C (315°F), draw ratio 1.20 output velocity (V2) 50 FPM (15,24 m/min).
  • Electrostatic Charged Webs Another variation contemplated by the present invention is to apply an electrostatic charge to the consolidated web to improve its filtration performance.
  • the charging in the production of electrets can be applied by a variety of techniques described in the patent literature. See for example U.S. Patent 4,592,815. It is anticipated that the higher packing density of fiber in the hot consolidated webs results in an unusually high effectiveness of electron implantation in the web.
  • meltblown webs and spunbonded webs are relatively isotropic
  • the invention process can also be carried out by hot drawing in the CD as a continuous process (such as on a tenter frame at negative or minimal MD tension) or on a "by piece” process.
  • the precursor web comprises a composite of the following combinations: meltblown web/meltblown web (different webs), meltblown web/other nonwoven web (e.g., spunbond, hydroentangled, etc.) also, webs of thermoplastic/ nonthermoplastics combinations make useful precursors.
  • meltblown web/meltblown web different webs
  • meltblown web/other nonwoven web e.g., spunbond, hydroentangled, etc.
  • thermoplastic/ nonthermoplastics combinations make useful precursors.
  • These composite precursors can be made by techniques well known in the art.
  • the composite may also include more than two layers.
  • the meltblown web of the composite will have the properties described above.
  • One particularly useful composite precursor is the spunbond/meltblown/spunbond (SMS) structure.
  • the meltblown web should have the properties described above for meltblown webs.
  • the spunbond webs may be the same or different but should have the properties described above for spunbond webs.
  • the SMS composite precursor may be made by conventional methods, well known in the art.
  • the spunbond webs add strength and abrasion resistance to the structure thus increasing the application of the webs consolidated by the process of the present invention, particularly in the areas of surgical gowns, drapes, health care packaging, etc.
  • the consolidated composite is characterized by:
  • Hot or cold CD stretching following consolidation by MD stretching produces an open reticulated fabric having exceptional web uniformity and high porosity for an open structure.
  • Hot stretching in the CD at large draw ratios e.g., about 1.4
  • the following experiments demonstrate the effect of drawing an SMS precursor web in accordance with the process of the present invention.
  • the SMS web was thermally point bonded and had the following composition: Web Composition Thickness, Mils / ⁇ m Basis Wt, oz/yd 2 / g/m 2 S Spunbond PP 3 / 76,2 0.3 / 10,17 M Meltblown PP 9 / 228,6 1.7 / 57,63 S Spunbond PP 3 / 76,2 0.3 / 10,17
  • the precursor web was processed at a draw ratio of 1.9 through a 157 °C (315 degree Fahrenheit) oven at 6,4 m/min (21 fpm).
  • the drawn web was permitted to cool to room temperature while under the applied MD tension.
  • the elasticity of the drawn SMS fabric makes the fabric particularly useful in surgical gowns requiring relatively high strength, stretchability and barrier properties.
  • the same consolidated SMS fabric was tested for filtration efficiency.
  • the filtration tests were carried out on the SMS fabric without consolidation and the SMS fabric after consolidation.
  • the drawn or consolidated SMS web exhibited a filtration efficiency of 80.8% whereas the precursor SMS web exhibited a filtration efficiency of only 67.7%.
  • the method of the present invention produces a nonwoven fabric that posses unique and useful properties that lends the fabric to application in a variety of fields.
  • the properties of reduced pore size and pore size distribution makes the web ideally suited for filtration and absorption.
  • the property of CD elasticity increases the web utility in filtration (e.g., surgical masks where conformance to the face contours is important) and other uses such as flexible gowns or diapers and hygiene products.

Claims (28)

  1. Verfahren zur seitlichen Kondolidierung und Verkleinerung der Porengröße eines Stoffs, welches umfasst:
    (a) Erhitzen eines Vorläufervliesstoffes (17) aus zufällig vereinigten nicht-elastomeren thermoplastischen Fasern, worin die Fasern des Vorläuferstoffs eine Kristallinität von zumindest 30 % aufweisen und worin der Vorläuferstoff (17) aus einem Laminat aus zumindest zwei unterschiedlichen Vliesstofflagen hergestellt ist, worin jede Stofflage durchgehend verteilte Faser-Faser-Bindungen (29) aufweist, worin die Stofflagen an voneinander beabstandeten Stellen thermisch miteinander verbunden werden, wobei das Erhitzen bei einer Temperatur zwischen der Weichtemperatur und der Schmelztemperatur der thermoplastischen Fasern erfolgt,
    (b) Strecken des erhitzten Stoffs (17) unter Spannung im Wesentlichen in der Längsrichtung (MD), um den Stoff seitlich zu konsolidieren, ohne die planare Integrität des Stoffs zu unterbrechen und hierdurch das maximale Porengrößenmaß des Stoffs um zumindest 20 % zu reduzieren, wobei der konsolidierte Stoff (17) ein loses Netzwerk aus miteinander verbundenen Fasern (26 - 28) bildet und ein maximales Prozess-Bruchstreckverhältnis von weniger als 4 bei einer Temperatur von zumindest 5,6 °C (10 °F) unter dem Schmelzpunkt des Vorläuferthermoplasts und bei einer Reckrate von zumindest 2500 %/min sowie ein maximales Porengrößenmaß von 4 bis 250 Mikron auf der Basis von ASTM F 316-86 aufweist,
    worin die Erhitzungs- und Streckschritte kontinuierlich durchgeführt werden, indem der Vorläuferstoff (17) in einen Ofen (23) mit einer ersten linearen Geschwindigkeit (V1) eintritt und der Vorläuferstoff aus dem Ofen mit einer zweiten linearen Geschwindigkeit (V2) abgezogen wird, wobei das Verhältnis der zweiten Geschwindigkeit zur ersten Geschwindigkeit von etwa 1,1 : 1 bis 2 : 1 reicht,
    (c) Kühlen des Stoffs oder Abkühlenlassen des Stoffs,
    worin der Stoff auf ein maximales Porengrößenmaß von weniger als 80 % das des Vorläuferstoffs und auf eine Elastizität in Querrichtung, definiert durch zumindest 70 %ige Erholung aus einer 50 %igen Dehnung in der Querrichtung, und auf eine Bruchdehnung in der Längsrichtung von weniger als 30 % auf der Basis von ASTM D 5035-90 gestreckt und gekühlt wird.
  2. Verfahren nach Anspruch 1, worin der Streckschritt ausreicht, um dem Stoff ein mittleres Durchflussporengrößenmaß von zumindest 20 % kleiner als der mittleren Durchflussporengröße des Vorläuferstoffs zu geben.
  3. Verfahren nach Anspruch 1, worin der Streckschritt ausreicht, um dem Stoff eine Packungsdichte von zumindest 20 % größer als jener des Vorläuferstoffs zu geben.
  4. Verfahren nach Anspruch 1, worin der Kühlschritt vor dem Lösen der Streckspannung durchgeführt wird und den Stoff (17) auf eine Temperatur unter der Weichtemperatur des Thermoplasts abkühlt.
  5. Verfahren nach Anspruch 1, worin der Vorläufervliesstoff (17) ein schmelzgeblasener Stoff mit einem durchschnittlichen Faserdurchmesser von 0,5 bis 8 Mikron ist.
  6. Verfahren nach Anspruch 1, worin das Thermoplast ein Polyolefin ist, ausgewählt aus der Gruppe, die aus Polypropylen, Polyethylen und Copolymeren davon besteht, und der Heizschritt bei einer Temperatur von zwischen 87,8 bis 176,7 °C (190 bis 350 °F) durchgeführt wird.
  7. Verfahren nach Anspruch 1, worin das Thermoplast aus Polyestern, Polyamiden, Cellulosetriacetat, Cellulosediacetat, Poly-4-methylpenten-1, Polyphenelensulfid, Flüssigkristallpolymeren und Fluorpolymeren ausgewählt ist.
  8. Verfahren nach Anspruch 6, worin der schmelzgeblasene Vorläuferstoff durchgehende, zufällig verteilte Faser-Faser-Bindungen (29) aufweist.
  9. Verfahren nach Anspruch 1, worin der Vorläufervliesstoff (17) ein spinngebundener Stoff mit Fasern (26 - 28) mit einem durchschnittlichen Durchmesser von 7 bis 50 Mikron und mit voneinander beabstandeten über den Stoff verteilten Bindungen (29) ist.
  10. Verfahren nach Anspruch 1, das ferner den Schritt aufweist, den gestreckten Stoff (17a) über eine Stange (25) oder Rolle zu leiten, die eine Oberfläche aufweist, um innerhalb der Breite des Stoffs Querkompressionskräfte auszuüben.
  11. Verfahren nach Anspruch 5, worin der Vorläufervliesstoff eine Bruchdehnung von weniger als 40 % auf der Basis von ASTM D 5035-90 aufweist.
  12. Verfahren nach Anspruch 1, worin die erste Geschwindigkeit (V1) gesteuert/geregelt wird, indem der Vorläuferstoff (17) vor dem Heizschritt durch den Klemmspalt erster gegenläufiger Walzen (22) geleitet wird, und die zweite Geschwindigkeit (V2) gesteuert/geregelt wird, indem der konsolidierte Stoff nach dem Heizschritt durch den Klemmspalt zweiter gegenläufiger Walzen (24) geleitet wird, und worin der konsolidierte Stoff auf eine Temperatur unter dem Weichpunkt des Thermoplasts abkühlen gelassen wird, bevor er durch den Klemmspalt der zweiten gegenläufigen Walze (24) hindurchtritt.
  13. Verfahren nach Anspruch 1, worin der Vorläuferstoff (17) ein Komposit ist, in dem eine spinngebundene Lage, eine schmelzgeblasene Lage und eine spinngebundene Lage komprimiert sind.
  14. Verfahren nach Anspruch 1, worin der Vorläuferstoff eine Breite von 152 bis 4064 mm (6 bis 160 Zoll) sowie eine Dicke von 50,8 µm bis 2,54 mm (2 bis 100 mil) aufweist und worin der gestreckte Stoff eine Breite von weniger als 80 % des Vorläuferstoffs und eine Dicke von 50,8 µm bis 3,81 mm (2 bis 150 mil) aufweist, und worin das Dickenverhältnis des gestreckten Stoffs und des Vorläuferstoffs von 1 : 1 bis 1,5 : 1 reicht.
  15. Aus einem Vorläufervliesstoff hergestellter Vliesstoff, wobei der Vorläuferstoff zufällig vereinigte nicht-elastomere thermoplastische Fasern (26 - 28) aufweist, die eine Kristallinität von zumindest 30 % aufweisen und uniaxial gestreckt und heißfixiert sind, wobei der Vorläuferstoff (17) aus einem Laminat aus zumindest zwei unterschiedlichen Vlieslagen hergestellt ist, wobei jede Lage aus zufällig vereinigten nicht-elastomeren thermoplastischen Fasern (26 - 28) hergestellt ist und jede Stofflage durchgehend verteilte Faser-Faser-Bindungen (29) aufweist, worin die Stofflagen an voneinander beabstandeten Stellen thermisch miteinander verbunden sind, worin das uniaxiale Heizen und Strecken kontinuierlich durchgeführt wird, in dem der Vorläuferstoff (17) mit einer ersten linearen Geschwindigkeit (V1) in einen Ofen (23) geleitet wird und der Vorläuferstoff aus dem Ofen mit einer zweiten linearen Geschwindigkeit (V2) abgezogen wird, und worin das Verhältnis der zweiten Geschwindigkeit zur ersten Geschwindigkeit von etwa 1,1 : 1 bis 2 : 1 reicht, wodurch ein Großteil (26, 28) der Fasern allgemein in der Streckrichtung (MD) konsolidiert und ausgerichtet wird und ein kleinerer Anteil (27) von Faserabschnitten kreuzweise oder quer zur Streckrichtung angeordnet ist,
    worin der konsolidierte Stoff ein loses Netzwerk aus miteinander verbundenen Fasern bildet und ein maximales Prozess-Bruchstreckverhältnis von weniger als 4 bei einer Temperatur von zumindest 5,6 °C (10 °F) unter dem Schmelzpunkt des Vorläuferthermoplasts und bei einer Reckrate von zumindest 2500 %/min sowie ein maximales Porengrößenmaß von 4 bis 250 Mikron auf der Basis von ASTM F 316-86 aufweist,
    worin der konsolidierte Stoff eine maximale Porengröße von weniger als 80 % jener des Vorläuferstoffs aufweist und eine Elastizität in der Querrichtung, definiert durch zumindest 70 %ige Erholung aus einer 50 %igen Dehnung in der Querrichtung, aufweist und eine Bruchdehnung in der Längsrichtung von weniger als 30 % auf der Basis von ASTM D 5035-90 aufweist.
  16. Vliesstoff nach Anspruch 15, worin die Fasern (26 - 28) nicht-elastomere thermoplastische schmelzgeblasene Fasern sind, die zufällig gebunden sind und einen durchschnittlichen Durchmesser von 0,5 bis 8 Mikron aufweisen.
  17. Vliesstoff nach Anspruch 16, worin die Fasern (26 - 28) zumindest teilweise mit einem Tensid beschichtet sind, um die Wasserbenetzbarkeit des Stoffs zu erhöhen.
  18. Vliesstoff nach Anspruch 17, worin der Stoff (17) eine mittlere Durchflussporengröße von zwischen 3 bis 40 Mikron aufweist.
  19. Laminat, umfassend:
    (a) den Stoff von Anspruch 16; und
    (b) ein mit dem Stoff verbundenes polymeres Substrat.
  20. Laminat nach Anspruch 19, worin das Substrat ein elastomerer Stoff ist.
  21. Laminat nach Anspruch 19, worin das Substrat eine Folie ist.
  22. Laminat nach Anspruch 19, worin das Substrat ein Textil ist, das die Dehnbarkeit des Laminats in Querrichtung auf weniger als 100 Reckung begrenzt.
  23. Vliesstoff nach Anspruch 15, worin ein Teil der Fasern (27), der sich quer zur Längsrichtung erstreckt, mit den Längsfasern (26, 28) verbunden ist, ohne die planare Integrität des Stoffs zu unterbrechen.
  24. Filter aus einem Vliesstoff, der seitlich konsolidiert ist und eine reduzierte Porengröße aufweist, aufgebaut aus einem Vliesstoff nach Anspruch 15.
  25. Filter nach Anspruch 24, worin der Filter, der ein Basisgewicht von weniger als 50,85 g/m2 (1,5 Unzen/yd2) aufweist, in der Lage ist, zumindest 50 % von Partikeln, die größer oder gleich 1 Mikron sind, abzufangen, gemessen bei einer Aerosolgeschwindigkeit von 10 cm/Sekunde.
  26. Gesichtsmaske mit dem Filter von Anspruch 25.
  27. Filter nach Anspruch 25, worin die Fasern eine elektrostatische Ladung enthalten.
  28. Filter nach Anspruch 25, worin der Stoff eine ihm hinzugefügte elektrostatische Ladung aufweist.
EP93910564A 1993-03-26 1993-03-26 Nachbehandlung von vliesstoffe. Expired - Lifetime EP0695383B1 (de)

Applications Claiming Priority (1)

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PCT/US1993/003090 WO1994023109A1 (en) 1992-03-26 1993-03-26 Post-treatment of nonwoven webs

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EP0695383A1 EP0695383A1 (de) 1996-02-07
EP0695383A4 EP0695383A4 (de) 1997-12-17
EP0695383B1 true EP0695383B1 (de) 2001-10-31

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JP (1) JPH08508789A (de)
KR (1) KR100273483B1 (de)
DE (1) DE69331065T2 (de)
DK (1) DK0695383T3 (de)
HK (1) HK1014564A1 (de)

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WO2015128777A1 (en) * 2014-02-28 2015-09-03 Kimberly-Clark Worldwide, Inc. Hydrophilic electret media
US10273611B2 (en) 2006-03-28 2019-04-30 Irema-Filter Gmbh Pleatable nonwoven material and method and apparatus for production thereof

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ATE455886T1 (de) * 2003-12-05 2010-02-15 Phoenix Intellectuals And Tech Verfahren zum herstellen eines elastischen vliesstoffs
JP5013810B2 (ja) 2005-12-01 2012-08-29 花王株式会社 シートの加工装置及びシートの製造方法
KR100811328B1 (ko) 2007-02-23 2008-03-07 심재원 부직포 후가공장치 및 그 후가공방법, 이에 의해 제조된부직포
DE102010052155A1 (de) 2010-11-22 2012-05-24 Irema-Filter Gmbh Luftfiltermedium mit zwei Wirkmechanismen
CA2817897C (en) * 2010-12-08 2019-04-02 E. I. Du Pont De Nemours And Company Improved media for hot gas filtration
DE102011014202A1 (de) * 2011-03-16 2012-09-20 Sandler Ag Filtermedium für die Herstellung plissierter Filter
WO2013185874A2 (de) * 2012-06-14 2013-12-19 Irema-Filter Gmbh Filtermedium aus synthetischem polymer
DE102013008402A1 (de) 2013-05-16 2014-11-20 Irema-Filter Gmbh Faservlies und Verfahren zur Herstellung desselben
DE102014117506A1 (de) 2014-11-28 2016-06-02 Filta Co., Ltd Filtermedium mit großem Faltenabstand
WO2023106231A1 (ja) * 2021-12-06 2023-06-15 株式会社カネカ メルトブローン不織布及びその製造方法
CN115888250B (zh) * 2022-10-24 2023-09-29 连云港连泰滤材有限公司 一种车用空调活性炭过滤布及其生产装置

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US4088731A (en) * 1976-07-28 1978-05-09 Clupak, Inc. Method of softening nonwoven fabrics
US4965122A (en) * 1988-09-23 1990-10-23 Kimberly-Clark Corporation Reversibly necked material
US5053066A (en) * 1990-05-04 1991-10-01 Hassenboehler Charles B Nonwoven filter and method of manufacture
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US10273611B2 (en) 2006-03-28 2019-04-30 Irema-Filter Gmbh Pleatable nonwoven material and method and apparatus for production thereof
WO2015128777A1 (en) * 2014-02-28 2015-09-03 Kimberly-Clark Worldwide, Inc. Hydrophilic electret media

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EP0695383A4 (de) 1997-12-17
DE69331065T2 (de) 2002-03-21
EP0695383A1 (de) 1996-02-07
DE69331065D1 (de) 2001-12-06
JPH08508789A (ja) 1996-09-17
DK0695383T3 (da) 2002-02-25
KR100273483B1 (ko) 2000-12-15
KR950701022A (ko) 1995-02-20
HK1014564A1 (en) 1999-09-30

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