filter element and method of making a filter element

专利摘要:
UNPLIED TUBULAR DEPTH FILTER HAVING FINE FIBER FILTER MEANS, a depth filter element is provided. not applied in the form of a tubular half-depth filter ring. Multiple sheet wraps, some including fine fibers, are employed. The depth filter element has specific applications in liquid filtration applications.
公开号:BR112012021535B1
申请号:R112012021535-3
申请日:2011-02-24
公开日:2021-04-20
发明作者:Lei Li；John A. Krogue；Thomas B. Green
申请人:Parker-Hannifin Corporation；
IPC主号:

专利说明:

FIELD OF THE INVENTION
[001] The present invention relates generally to depth filters, and more particularly relates to unplied tube rings of depth medium and the filtration means employed in such depth filters. BACKGROUND OF THE INVENTION
[002] Fluid flows such as liquid flows and gaseous flows (eg air flows) often carry solid particulate materials and unwanted liquid droplets which are often unwanted contaminants trapped in the fluid flow. Filters are commonly used to remove some or all of the particulate materials from the fluid flow. Filters are often characterized as depth filters in which particulate materials filter through the entire depth of the filter media, or as surface filters, whereby particulate materials are retained along the surface of the filter media.
[003] Filter media including fine fibers formed using an electrostatic spinning process is also known. Such prior art includes Filter Material Construction and Method, US Patent No. 5,672,399; Cellulosic/Polyamide Composite, US Patent Publication No. 2007/0163217; Filtration Medias, Fine Fibers Under 100 Nanometers, And Methods, US Patent Publication No. 2009/0199717; Integrated Nanofiber Filter Media, US Patent Publication No. 2009/0266759; Filter Media Having Bi-Component Nanofiber Layer, US Provisional Patent Application No. 61,047,455; Expanded Composite Filter Media Including Nanofiber Matrix and Method, US Provisional Patent Application No. 61/308,488; and Compressed Nanofiber Composite Media, Provisional US Patent Application No. 61/330,462, the entire disclosures of which are incorporated herein by reference.
[004] Often, such fine fibers have been employed in surface charge applications. There is a publication proposing the use of gradient depth media in the form of a single applied sheet of filter media comprising alternative layers of strong fabric and nanofibers, as in US patent no. 6,521,321 to Kahlbaugh et al. Although Kahlbaugh's '321 patent suggests the possibility of an application to liquid filtration, it recognizes through examples and description that it is primarily focused on gas or air filtration (eg, cabin air, engine air, smoke from tobacco). Furthermore, depth filtration appears to be limited to the depth of the leaf itself as is often discussed in connection with a applied configuration. Furthermore, it is believed that previously fine fibers (and particularly electrotrophied fibers) were not generally applied to liquid applications because liquid momentum and viscosity tend to pull particulate materials through such a layer of fine fiber. Rather, it is believed that such fine fibers have typically been employed in air filtration applications. SUMMARY OF THE INVENTION
[005] The invention provides improvements referring to unplied depth filters, in which fine fibers can be configured in a tubular ring of medium depth. With techniques discussed here relating to the arrangement and covering of fine fibers, certain modalities although not exclusively limited thereto, have specific application to liquid filtration.
[006] According to an inventive aspect, a filter element comprises an unplied tubular ring of a medium depth having a medium thickness of at least approximately % of centimeter. The depth medium comprises carrier fibers and fine fibers. Carrier fibers having an average size greater than approximately 600 nanometers; and fine fibers having an average size of less than 800 nanometers carried by the carrier fibers. A certain ratio of carrier to fine fibers is provided in which the fine fibers have a size that is at least 4 times smaller than that of the carrier fibers.
[007] For example, electro-blown or electro-spun fibers can provide the fine fibers. However, the smaller the fine fibers are, the more preferred they are and have benefits, and it is an inventive aspect with the use of electrotrophied fine fibers that may have diameters smaller than 500 nanometers and more preferably smaller than 250 nanometers (and more preferably smaller than 100 nanometers).
[008] In many embodiments and in accordance with another inventive aspect, multiple wraps at least partially overlapping a sheet employing fine fibers are used. For example, the filter element may comprise a first sheet of filter media, wherein the first sheet of filter media comprises at least one substrate and at least one layer of the fine fibers deposited thereon. The sheet is at least partially rolled over itself to create multiple layers of the first sheet of filter media throughout the depth of the depth media.
[009] A specific sheet useful in winding modes is a multilayer composite. The first sheet of filter media may comprise a composite medium of a plurality of woven layers and a plurality of fine fiber layers of fine fiber laminated together in the first sheet of filter media. Selected fine fiber layers are separated on the first sheet of filter media by the strong fabric. The sheet of filter media itself may have a high level of coverage of electrotrophied fine fibers having an average size of less than 500 nanometers of at least approximately 5,000 km/n2, and preferably higher in accordance with various embodiments.
[0010] Based on testing, the first filter media has a filtration efficiency substantially comparable to, or better than, micro-glass filtration media for a pre-selected filtration application. Thereby, it can serve as a substitute for micro-glass filter media and totally eliminate micro-glass from a filtration structure while at the same time providing high efficiency with appropriate application life/flow requirements.
[0011] Another preferred aspect is the provision of a high linear coverage of nanofibers in terms of kilometers per square meter can be realized either in an individual wrap or sheet or collectively across the entire depth of the element (with square meters being measured in average diameter ). For example, the depth medium may have a full depth loaded fine fiber coverage of at least 0.1 gram/m2, and at least approximately 10,000 km/m2, more preferably a full depth loaded fine fiber coverage. of at least 0.5 grams/m2, and at least approximately 50,000 km/m2, and more preferably a blanket of fine fibers loaded over the entire depth of at least 1.0 gram/m2, and at least approximately 100,000 km/m2 .
[0012] According to another inventive aspect which may incorporate the above aspects, a filter element comprises an unplied tubular ring of a half depth having a half thickness of at least approximately % of centimeter. The depth medium comprises carrier fibers and fine fibers, the carrier fibers having an average size of at least approximately 3 microns; and fine fibers having an average size of less than 800 nanometers carried by the carrier fibers.
[0013] Other inventive aspects are directed to methods. For example, a method of making a filter element may comprise electrospinning fine fibers having an average size less than 800 nanometers from a solution comprising a polymer and a solvent under the effect of a potential difference; depositing the fine fibers onto a carrier fiber substrate, the carrier fibers having an average size of at least 3 microns; and winding the carrier fiber substrate and the fine fibers into a depth medium having a thickness of at least % centimeter. The method may alternatively employ smaller carrier fibers as discussed above with a size ratio of 4:1 or higher between fine and carrier fibers.
[0014] Other aspects, objectives and advantages of the invention will become more apparent from the following detailed description when taken in combination with the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The accompanying drawings incorporated in and forming a part of the descriptive report illustrate various aspects of the present invention and, together with the description, serve to explain the principles of the invention. In the drawings: Figure 1 is a perspective view in partial section of the preferred embodiment of the invention illustrating a multi-overlapped filter element made on a four-station wrapping machine using four rolls of selected non-woven cloth, and in which by at least one of the rolls employs a filter medium having fine fibers; Figure 1A is a perspective view of a filter element employing the filter media of Figure 1 with an optional support core and end caps employed for a filtration application; Figure 2 is a cross-sectional view illustrating the multi-overlapped coreless filter element of Figure 1 being formed in a hollow mandrel; Figure 3 is a schematic top view of the three stations of the machine used to manufacture the filter element of Figure 1; Figure 4 is a partially schematic cross-section of the multi-overlapped filter element schematically showing that the inner wrapper employs a sheet having multiple layers of successive fine fiber and substrate on the sheet; Figure 4A is an enlarged view of a section of Figure 4 taken around the dashed circle in Figure 4 further illustrating the sheet having on the sheet multiple layers of successive fine fiber and substrate, the relative thicknesses and arrangement being schematic for demonstration purposes only. as opposed to being scaled and with the proximity of strips being exaggerated to show gaps between strips (although in practice the adjacent strips and wraps touch each other); Fig. 5 illustrating an embodiment of a multi-overlay filter element similar to Fig. 1 also not to scale, but additionally employing an interlayer along the innermost shell; Figure 6 is a schematic illustration showing how the interleaving layers of Figure 5 can be wrapped; Figure 7 is an alternative embodiment of a depth filter element employing fine fibers shown in perspective view and cross section employing a spiral (not helical) wrap with a sheet of filter media and a sheet of full length filter media (width equal to the axial length of the filter element); Figure 8 is a still further alternative embodiment of a manufacturing process/system shown in schematic form for forming a depth filter element employing fine fibers; Figure 8A is a cross-section in partially schematic form of the depth filter element made by the manufacturing process/system of Figure 8; Figure 9 is a schematic cross-sectional view (e.g., relative thickness shown not to scale) of a filter medium including multiple tightly packed scrim layers carrying fine fibers in accordance with an embodiment of the present invention; Figure 10 is a schematic cross-sectional view of the filter medium of Figure 9 in a pre-compressed state being compressed to a compressed state by a set of rollers; Figure 11 is a schematic illustration of a system for making filter media in accordance with an embodiment of the present invention; Figure 12(A) is a Scanning Electron Microscopic image showing bicomponent fibers and fine fibers of a composite medium produced using the system of Figure 11 taken at a magnification level x300; Figure 12(B) is a Scanning Electron Microscopic image showing bicomponent fibers and fine fibers of a composite medium produced using the system of Figure 11 taken at a magnification level x1,000; Figure 12(C) is a Scanning Electron Microscopic image showing bonding between bicomponent fibers and the fine fibers of a composite medium produced using the system of Figure 11 taken at a magnification level x2,000; Figure 12(D) is a Scanning Electron Microscopic image showing bonding between bicomponent fibers and fine fibers of a composite medium produced using the system of Figure 11 at a magnification level x10,000; Figure 13 is a schematic illustration of a system for making a filter medium according to a different embodiment of the present invention; Figure 14 is a schematic illustration of a system for making filter media in accordance with yet another embodiment of the present invention; Figure 15 is a schematic cross-sectional view of a filter medium including multiple layers of tightly compressed strong fabric and fine fibers in accordance with an embodiment of the present invention; Figure 16 is efficiency test results of the first multilayer filter media test samples; Fig. 17 is efficiency test results of second multilayer filter media test samples; Fig. 18 is efficiency test results of third multilayer filter media test samples; Figure 19 is a schematic cross-sectional view of a filter means according to a different embodiment of the present invention; Figure 20 is efficiency test results of fourth multilayer filter media test samples; Figure 21 is a schematic cross-sectional view of a filter means in accordance with yet another embodiment of the present invention; Figure 22 is efficiency test results of fifth multilayer filter media test samples; Figures 23(A)-(H) are schematic illustrations of bicomponent fibers of a substrate in accordance with various embodiments of the present invention; Fig. 24 is efficiency test results of standard tubular depth filter test samples; and Figures 25-26 are efficiency test results of a tubular depth filter including fine fiber multilayer intersheet test samples.
[0016] While the invention is described with respect to certain preferred embodiments, it is not intended to limit the invention to those embodiments. Rather, the invention is to cover all alternatives, modifications and equivalents as included within the spirit and scope of the invention as defined by the appended claims. DETAILED DESCRIPTION OF THE INVENTION
[0017] In the sections below, different modalities of depth means will first be described. Later, sheets containing fine fibers that are useful in many of the embodiments will be described, with examples provided. Later, some examples of specific unapplied tubular depth media will be discussed. TUBULAR DEPTH FILTER NOT APPLIED
[0018] Referring to Figure 1 of the drawings, a multi-overlapping coreless filter element 10 is illustrated and constructed in accordance with an embodiment of the invention. As will be described herein, the filter element 10 has integrated therein a combination of fibers including carrier fibers having an average size greater than approximately 3 microns, and otherwise fine fibers having a size less than approximately 800 nanometers (most preferably less than 500 nanometers, even more preferably less than 250 nanometers and more preferably less than 100 nanometers).
[0019] The filter element 10 includes a first multi-overlapping non-woven cloth strip 12, a second multi-overlapping non-woven cloth strip 13, a third multi-overlapping non-woven cloth strip 14 and a fourth multi-overlay non-woven cloth strip 15. As used herein, a strip will sometimes be referred to as a sheet and vice versa. In that case, a strip of partial width is provided (partial width in relation to the axial length of the filter element) so that each strip can be helically wound in this mode. Each strip of cloth 12-15 is spirally or helically wound into overlapping layers to form overlapping strips 16, 17, 18, 19, respectively. Collectively, these strips form an unplied tubular ring 20 of one half depth having a total thickness of half T of at least approximately % of a centimeter.
[0020] The radially inner surface of the innermost strip 16 forms the periphery of an axially extended annular space (which can be used to collect clean fluid and facilitate axial flow of clean fluid). This hollow interior space extends from one end of the filter element to the oppositely facing end of the filter element 10. In the drawings the thickness of the cloth (as well as the fine fiber layers where illustrated) is exaggerated for demonstration purposes. However, the tubular depth media ring is typically at least % cm thick (radial thickness) and more typically between % cm and 5 cm (more typically between 1 cm and 3 cm) thick as a result of the wraps. It can be seen that each strip 12-15 at least partially overlaps itself as it thickens the given strip to a strip generally between 2-8 thick wraps for one of the given strips of cloth. Additionally similar embodiments of filter element 10 employ at least 1 thick cloth strip and more typically between 2-6 cloth strips. As such, filter elements can be made employing the helical wrap technique between 2 and 48 strips thick (more typically between 6 and 32 layers thick).
[0021] In this first embodiment of Figure 1, and with further reference to Figures 4, 4A and 9, a sheet of preformed, laminated multi-layer filter media 100 is selected and employed for use as the innermost cloth strip 13. In another embodiment, the sheet of multilayer filter media 100 is selected and employed for use as the second innermost cloth strip 14 as well as the innermost cloth strip 13. In contrast, the upstream cloth strips 15, 16 may not employ fine fibers but a more open structure to create a gradient medium across the entire thickness T.
[0022] For example, the upstream non-woven cloth strips 15, 16 can be composed of selected polymeric fibers such as polyester and polypropylene which serve as both base fibers and binder fibers. Base fibers have higher melting points than binder fibers, which is also referred to here as a bicomponent medium or multicomponent medium. The role of base fibers is to produce small pore structures in the coreless filter element 11. The role of fiber binder or binder material is to bind the base fibers into a rigid filter element that does not require a separate core. The binder fibers can consist of a pure fiber or one having a lower melting outer shell and a higher melting inner core. If the binder fiber is a pure type, then it will completely liquefy in the presence of sufficient heat. If the binder fiber has an outer shell and an inner core, then it is subjected to temperatures that liquefy only the outer shell in the presence of heat, leaving the inner core to assist the base fiber in producing small pore structures. The role of the binder fiber is therefore to liquefy all or part in the presence of heat, the liquid fraction thereof to twist on the base fibers to form a bonding point between the base fibers, thereby binding the base fibers together. after cooling. The binding material may be in a form other than fibrous.
[0023] Although a gradient depth medium is incorporated in Figure 1 with the multilayer filter medium sheet 100, it is envisioned that the multilayer filter medium sheet 100 can be employed at different locations in upstream locations or downstream and can be selected for use for any one or more of strips 12-15.
[0024] One embodiment of a method and apparatus for making such a filter element 10 can be seen with reference to Figures 2-3 of the patent application and may be in accordance with the disclosures of US patents nos. 5,827,430 to Perry Jr. et al; and/or US 2008/0128364 to Cloud et al., the entire disclosures of which are hereby incorporated by reference in their entirety. In Figure 2 of the drawings, numeral 22 designates a hollow cylindrical mandrel with an annular outer surface and an annular inner surface, the annular inner surface forming the periphery of a cylindrical channel 23, through which a gas heat exchange medium flows. or liquid (not shown). Band 16 of multi-overlapping non-woven cloth strip 12 is shown overlaid by band 17 of multi-overlapping non-woven cloth strip 13, which in turn is overlaid by band 18 of multi-overlapping non-woven cloth strip -overlay 14, which is then overlaid by the strip 19 of the multi-overlay non-woven cloth strip 15.
[0025] As shown in figure 3 of the drawings, only three stages are shown of the multistage winding machine shown in greater detail in the aforementioned referenced patents. In Figure 3, a first compression belt 25 is shown wrapping, in a multi-laid mode, the first strip of non-woven cloth 12 around the hollow mandrel 22. A second compression belt 26 is shown wrapping, in a way of multi-lapping, the second strip of non-woven cloth 13 around the strip of multi-lapping non-woven cloth 12. A third compression strap 27 is shown surrounding, in a multi-lapping mode, the third strip of cloth. non-woven fabric 14 around the multi-overlay non-woven cloth strip 13. A first set of preferably infrared heater heaters 28 is shown in a position to apply heat, simultaneously with compression of the compression belt 25, to the cloth strip non-woven mutli-overlay 12. A second set of infrared heater heaters 29 is shown in a position to apply heat, simultaneously with compression belt 26, the cloth strip does not multi-overlay fabric 13. A third set of infrared heater heaters 30 is shown in a position to apply heat, simultaneously with compression belt 27 compression, to the multi-overlay non-woven cloth strip 14.
[0026] After the filter element 10 is formed into a medium depth tubular ring 20, from there it can be cut into axial length segments and then configured with opposite open and closed end caps 32, 34 sealably attached to ends faces of the tubular ring as shown in Figure 1A. The open end cap 32 has an opening 35 to serve as an outlet for clean fluid. One or more seals such as O-ring gaskets 36 may be disposed on the end cap 32 for sealing with a fluid system mounting head. Additionally, a perforated core 38 may be employed along the interior of the medium.
[0027] Turning now to figure 4 and 4A, it can be seen that the resulting arrangement of the helical wrap presents a unique structure and arrangement by virtue of the multilayer lamination of the multilayer filter sheet 100. Although additional details of such sheet 100 are discussed later, it will be recognized that the multilayer filter sheet 100 provides flow structure in the individual strip 12 employing the filter sheet 100. In particular, with the helical wrap arrangement, the strips are slanted with respect to the longitudinal axis 40 of the filter element 10. As a consequence, the individual fine fiber layers 42 (eg corresponding to 124, 126, 128, 130, 132, 134, 136, 138, 140, 142 in figure 9) are arranged in a slanted alignment and not parallel to axis 40 such that fluid can flow through sheet 12 along individual fine fiber layers. In particular, the porous and more open substrate 44 (e.g. corresponding to 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 in Fig. 9) is also disposed in an inclined alignment and not parallel to the geometric axis 40; and thereby can act as a drainage layer or fluid flow layer on the strip 12.
[0028] Therefore, there may be slanted microflow paths through the strip 12 through the more open and porous substrate layers 44. Particulate materials can be retained during this process by the more efficient fine fiber layers 42. Additionally, between adjacent wraps of the strip 12, there may also be flow through and between the strips, which may be referred to as macroflow paths between strips, although in practice adjacent sheaths of a strip are in contact and touching. In addition to the potential for flow along sloped microflow or macroflow paths, a significant amount of flow is also radially through the material of the strip itself passing through successive substrate and fine fiber layers 44, 42 where particulate materials can be retained . However, it should be recognized that should the fine fiber layer 42 clog with particulate material there is an open inclined flow path through the strip along the porous substrate layers 44. As a consequence and while many filters tend to improve efficiency with over time, it may be that the present arrangement may eventually decrease in efficiency over time as particulate material loading causes more flow along the slanted flow paths through the substrate layers 44 as opposed to radially through the medium. (and fine fiber layers 42).
[0029] Turning now to figure 5-6, a filter element 50 in yet another embodiment is illustrated schematically in cross section. Filter element 50 is a similarly helically wrapped filter element to the first embodiment and as such similar reference numerals are used, but additionally employs an interleaving strip 52 covering strip 12 employing multilayer filter sheet 100 (see figure 9) with fine fiber layers 42. The arrangement and variations of an intercalation can also be in accordance with any of the examples of US patent publication no. 2008/0128364 from Cloud and others, which was previously incorporated by way of reference. Although a single track in this mode is shown as having an interleave, multiple tracks 16-19 (as in the first mode shown in Figure 1) may employ an interleave. One or more of these bands may include at least one of the strips as having fine fibers (the interleaving may also optionally include fine fibers).
[0030] In this embodiment, a lower efficiency interleaving strip 52 is wrapped together with strip 12 employing the multilayer filter sheet 100. Typically in this arrangement, one of the strips will have a greater flow porosity and the other strip a greater efficiency and less porous structure resulting in greater flow horizontally/diagonally. As a result, more flow in this mode can be along the inclined path through the interleaving strip 52 compared to the efficiency strip 12 employing the multilayer filter sheet 100.
[0031] Turning to Figure 7, another embodiment of a filter element 60 is illustrated employing a spiral wrap employing at least one full-length sheet that is spirally wrapped around the geometric axis and in that embodiment two sheets 62, 64 (more sheets can also be co-wrapped). At least one of the sheets and in that case sheet 62 has fine fibers integrated therein (for example sheet 62 may be formed from sheet 100 of Figure 9). Also illustrated is that the other sheet 64 may not have any fine fibers but may serve as a spacer layer. Each of the sheets extends parallel to the filter axis 66, unlike the previous embodiments. Generally in this modality, fluid may be able to flow along a spiral path, but more typically (especially if many sheaths are employed) fluid is forced to travel radially inward through the filter means of the strips 62, 64. In any event , this forms a medium of depth as multiple layers are employed. In addition, a lower efficiency strip may have more wraps and be longer so as to continue to spirally wrap around the element even after the higher efficiency sheet 62 is finished.
[0032] Returning to Figures 8-8A, yet another embodiment is illustrated schematically showing the creation of a mid-depth element 70 employing fine fibers. In this modality, multiple fusion blown head stations 72 and electro-spinning modules are arranged. Melt blown heads 72 pump molten polymer through a die having holes and are blown at a given speed and distance to create fibers having a selected diameter. Fusion blown heads will often produce fibers larger than 1 micron, but can also create fine fibers below 1 micron and down to approximately 600-700 nanometers if subjected to electric fields. As such, fine as well as coarse fibers can be created by melt blowing, which can be used in any of the embodiments of the present invention. Typically, fine fibers in one modality are characterized as being at least 4 times smaller than melt blown fibers. Each of the electrospinning and melt blowing module stations 72a-c and 74A-c can produce different fiber sizes as may be desired. For purposes of differentiation, melt-blown fibers and electrospinned fibers are thus meant to be more specific terms than fine fibers, which is meant to be generic.
[0033] In this embodiment a perforated core 76 is moved along an axis 78 rotationally and axially to deposit layers of melt blown fibers 80a-c and electrospinned fibers 82a-c into the core 76. To facilitate an electrical voltage potential, bars of 84 electrostatic wiring are employed to maintain a charge and differential. Electrospinning equipment such as the endless chains as revealed in US provisional order no. 60/989,218 entitled “Filtration medias, fine fibers under 100 nanometers, and methods” can be employed but with the endless leg extending under and parallel to support axis 78 for the process. From this process, a filter element is created having successive layers of melt blown fibers 80a-80c and electrospinned fibers 82a-82c as illustrated in Figure 8A. MULTILAYER COMPOSITE FILTER MEDIA
[0034] Turning now to Figures 9-10, the multilayer filter sheet 100 employing multiple layers of fine fibers as used in many of the above embodiments is illustrated along with alternative modes for making such a multilayer sheet. It should be recognized that embodiments using strips of sheet 100 may have fewer (or more) layers of fine fibers deposited thereon. In some embodiments some strips (as for Figure 1) may have a single layer of fine fiber, while in others, and more preferably, multiple layers of fine fiber are deposited and contained in one strip. In any case, it can be referred to as a “composite medium”. In some embodiments, a plurality of layers of strong fabric and a plurality of layers of fine fiber fine fibers are laminated together into a single sheet of filter media, with selected fine fiber layers being separated in the first sheet of filter media by the strong fabric. Preferably in wrapping situations, the fine fibers will be protected and sandwiched between substrate layers of carrier fibers.
[0035] Before turning to the details of the multilayer filter medium 100, some lexicography will be developed to aid in understanding the present invention. As used herein, the term "substrate" is intended to be broad in nature and is intended to include any structure onto which fine fibers are loaded or deposited. "Substrate" can include conventional formed filter media such as strong fabrics and the like that can be unrolled from rolls of media. Such filter means have a tangle of fibers that are typically bonded or secured together mechanically, chemically, adhesively and/or otherwise and thereby have strength such that they cannot be easily torn by hand (e.g., a sheet of 0 .09 square meter typically withstands the application of tension force of 2 kilograms and 200 grams) and has filtering properties. “Substrate” can also include looser fiber tangles that may not be bonded together or bonded together (for example, a 0.09 square meter sheet may come apart after applying tension forces of 2 kilograms and 200 grams). A "strong fabric" used herein refers to woven or non-woven fiber tangles, in which the fibers are bonded and compressed into a flat formed medium.
[0036] There are a few ways in which nanofiber coverage can be characterized. A first way to characterize nanofiber coating is basis weight. However, basis weight is dependent in part on the specific gravity of the nanofiber material, as well as the selected size (eg, also mentioned interchangeably as fiber diameter and/or thickness) of the nanofiber. Another useful measure to characterize nanofiber coverage is the calculated linear distance of nanofiber coverage which can be expressed in terms of kilometers per square meter (km/m2) which is useful as this coverage average eliminates variability due to fine fiber diameter and variability due to specific gravity differences between different materials that may be employed.
[0037] In many exemplary embodiments discussed here, fine fibers having an average fiber diameter of 0.08 microns (80 nanometers) have been employed. However, it will be recognized that a double sized fiber (eg a 160 nanometer sized fine fiber) based on a simple area calculation (II*R2) will be 4 times the weight, and a quad sized fiber will have, thus 16 times the weight. An over application of fine fibers can lead to a plastic film that is not very permeable or porous, thus not suitable for a filter medium. The use of smaller fine fibers is desirable as a higher level of linear coverage can be obtained. Considering that larger diameter fine fibers will tend to take up greater void space, generally or as a rule of thumb, it is desirable for the application rate of fine fibers on a kilometer basis to be lower as the fine fiber diameter increases. However, coverage on a basis weight may nevertheless increase as the fine fiber diameter increases, due to quadruple the mass for diameter doubling. As a rule of thumb, basis weight can increase 2-2.5 times for doubling in fiber diameter (approximately 4-6 times for quadruple fiber diameter); and for ease purposes a duplication will be employed. Thus, if 0.15 g/m2 is employed for an average diameter of 80 nm, then for a 160 nm fiber a 0.30 g/m2 sheath would be used, and a 320 nm fiber a sheath of 0.6 g/m2. Embodiments of the present invention are usable for a range of fine fibers smaller than 1 micron, typically smaller than 500 nm, and more preferably smaller fibers below 150 nm. However, coverage adjustments can be made in accordance with the above principles for embodiments of the present invention.
[0038] Here, the terms "first", "second" or "third" in reference to a composite of filter media or layers are not intended to refer to a specific location. “First tier” is not intended to mean the first tier, nor is it intended to be indicative of where upstream or downstream in relation to another tier (“upstream” or “downstream”) may be used for this purpose. Instead, such terms as “first” and “second are used for background purposes.
[0039] Figure 9 is a schematic cross-sectional view of a filter medium 100 according to an embodiment of the present invention. It is schematic in the sense that in reality the fine fiber layer has virtually no thickness, but for illustration and understanding, thickness is illustrated in Figure 9 and other schematic illustrations. In preferred embodiments, filter media 100 includes at least two different fibers, e.g., electrospinned nanofibers and a coarser fiber substrate carrying the nanofibers. As such, filter media 100 is also referred to as a composite filter media, a composite media, or other similar terms in that application. While filter media 100 is particularly well suited for liquid particulate material filtration applications with examples/modalities having a significant particulate material filtration impact now for liquid applications, filter media 100 can be used in other fluid filtration applications.
[0040] In the embodiment shown in Figure 9, the filter medium 100 comprises 10 substrate layers 102, 104, 106, 108, 110, 112, 114, 116, 118, 120, each of which carries fine fibers 124, 126 , 128, 130, 132, 134, 136, 138, 140, 142, and a means 122 on top of the fine fibers 142. The substrate is 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 and means 122 are formed from fibers having an average fiber diameter typically greater than that of fine fibers. The substrate layers 102, 104, 106, 108, 110, 112, 114, 116, 118, 120, the fine fibers 124, 126, 128, 130, 132, 134, 136, 138, 140, 142 and the medium 122 they are laminated and tightly compressed together to increase fiber surface area by volume. While such an embodiment is shown with media layer 122, such media layer is optional, and thus, filter media 100 in accordance with other embodiments may not include such media layer 122.
[0041] The filter media of Figure 9 can be formed using the process shown in Figure 10. Figure 10 illustrates the filter media 100 in a pre-compressed state 144 and a compressed state 146. As shown, the filter media 100 in the pre-compressed state 144 has an initial thickness t' (also referred to herein as an original thickness.) The filter medium 100 in the pre-compressed state 144 is compressed in the compressed state 146 using an array of rollers 148, 150, at that the initial thickness t' is reduced to a final thickness t.
[0042] In some embodiments, the filter medium 100 in the pre-compressed state 144 is heated prior to compression. In certain preferred embodiments, substrate fibers relax and reorient to increase an average distance between the fibers during heating (such as a scrim that has been at least partially compressed during the scrim production process). As such, the substrate layers expand and elevate, whereby the thickness of each of the substrate layer increases. Furthermore, as fibers close to the substrate surface relax and reorient, the fine fibers that are carried by these fibers move and reorient with the fibers. In this way, fine fibers are extended, pushed and pulled with the larger fibers. It is believed that this can create a three-dimensional matrix for fine fibers as opposed to being merely flat or flat (such a three-dimensional matrix of fine fibers can still be considered to be and may be referred to here as a "layer" even if integrated into the surface of the substrate.)
[0043] In such embodiments, the initial thickness t’ of the pre-compressed state 144 may increase by at least 1.5 times, 2 times, 3 times or even more via heating. In such embodiments, the final thickness t of the filter medium 100 after subsequent compression of the elevated filter medium 100 may be less than or equal to or greater than the initial thickness t', depending on the amount of expansion during heating and the amount of reduction during compression. In other embodiments, filter media 100 in the pre-compressed state 144 can be heated and compressed simultaneously through a set of heated calender rolls. In such embodiments, there may be no expansion or a very slight increase in the initial thickness t’ before the reduction in thickness to the final thickness t. in still different embodiments, the compressed filter medium 100 having the final thickness t can be heated post-compression, whereby the thickness t can be increased. In some embodiments, filter media 100 may be heated more than once. For example, filter media 100 can be compressed by a set of rollers arranged in an oven such that filter media 100 is heated just before being compressed, while being compressed, and immediately after being compressed. In any event, it was found that processing the medium after depositing the fine fibers to rearrange fine fibers in more than one three-dimensional matrix is advantageous. Expansion and/or compression are examples of such processing. Such processing can provide greater porosity and can be used for better flow and/or facilitate greater coverage of the fine fiber deposit.
[0044] In one embodiment, the final thickness t may be between approximately 50% and 300% of the initial thickness t', preferably between 70% and 200% of the initial thickness t', and more preferably between 80% and 150% of the thickness initial t'. As the filter medium 100 in the pre-compressed state 144 is pressed down to the final compressed state 144, the fine fibers 124, 126, 128, 130, 132, 134, 136, 138, 140, 142 become thinner. integrated with the coarse fibers of adjacent substrate layers 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 and form a three-dimensional fine fiber matrix in the filter medium 100. Although the filter medium 100 in this embodiment include 10 layers of substrate carrying fine fibers, other embodiments may include more or less layers of substrate carrying fine fibers. For example, a filter medium can include a single substrate layer carrying a sufficiently intense coverage of fine fibers (e.g., at least approximately 0.3g/m 2 ).
The substrate layers 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 may be formed from any suitable porous material. Each of the substrate layer can be formed from the same type of porous material or different types of porous material. In one embodiment, each layer of substrate 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 comprises a formed filter medium. The formed filter medium comprises fibers which are bonded together. For example, the fibers of the formed filter medium can be bonded together by solvent bonding, thermal bonding and/or pressure bonding. The formed filter medium can carry fine fibers and provide structural support. The formed filter media is also referred to as a substrate filter media, a filter media substrate, a substrate, a filter media or other similar terms in the present application.
[0046] Alternatively, the substrate may comprise one or more webs of fibers which are loosely entangled together in a thick, highly fuzzy state and may not be bonded together as in the case of a formed filter media. Thereby, the coarse fiber web can be easily separated with very little manual effort and has little structural integrity such that it is not considered a formed filter medium in the conventional sense. Fiber web fibers typically have an average fiber diameter greater than an average fiber diameter of fine fibers. As such, fiber web is also referred to as coarse fiber web or other similar terms in that application. A composite filter media including fine fibers integrated with such a coarse fiber web is described in Integrated Nanofiber filter media, US patent application publication no. 2009/0266759, which is assigned to the assignee of this application, the entire disclosures of which are incorporated herein by reference thereto.
[0047] Preferably, the substrate is formed from a multi-component filter medium. As used herein, the term "multi-component filter media", "multi-component media", "multi-component filter media" and other similar terms may be used interchangeably to refer to filter media including at least two different materials . For example, a multi-component filter medium can comprise fibers formed from a first material and fibers formed from a second material, wherein the first material and the second material are different materials. Alternatively, a multi-component filter media may be formed from fibers including at least two different materials, such as fibers including a core formed from the first material and a coating formed from the second material, as described in detail below. A multi-component filter media including two different materials is referred to here as "bicomponent filter media", "bicomponent media" and similar terms.
[0048] In a preferred embodiment, each of the substrate layers 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 comprises a strong fabric formed from bicomponent fibers including two different materials having different melting points. A composite filter media comprising fine fibers and a substrate formed from such multi-component fibers are described in Multi-component filter media with nanofiber attachment, PCT patent application no. PCT/US09/50392, which is assigned to the assignee of the present application, the entire disclosure of which is incorporated herein by reference thereto.
[0049] In this modality, one component of the bicomponent fibers of the strong fabric has a lower melting point than the other component. The low melting point component can be any suitable polymer such as polypropylene, polyethylene or polyester. The other component can be a polymer having a higher melting point than the low melting point component, or other suitable fiber materials such as vibro and/or cellulose. The bicomponent fibers are bonded together and/or compressed together to form a strong fabric or substrate filter medium having a certain thickness.
[0050] The bicomponent fibers of the strong fabric used as the substrate 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 may include a polymer component with a high melting point and a polymer component with a low melting point. fusion point. For example, the bicomponent may comprise a high melting polyester and a low melting polyester, in which one has a higher melting temperature than the other. Figures 23(A)-(H) schematically illustrate bicomponent fibers according to various embodiments. For example, Figure 23(A) shows a coating/concentric core type bicomponent, wherein a number is formed from a high melting point polymeric component and a coating is formed from a low melting point polymeric component.
[0051] The high melting polymer component is formed of a polymer having a higher melting temperature than the low melting polymer component. Suitable high melting polymers include, but are not limited to, polyester and polyamide. Suitable low melting polymers include polypropylene, polyethylene, copolyester, or any other suitable polymers having a lower melting temperature than the selected high melting polymer. For example, bicomponent fibers can be formed from a polyester core and a polypropylene coating. In this embodiment, the bicomponent fibers are formed from two different types of polyesters, one having a higher melting point than the other.
[0052] Now referring again to Figure 9, the fibers of the substrates are formed to have an average fiber diameter greater than that of the fine fibers. In one embodiment, the substrate fibers have an average fiber diameter that is at least 4 times that of fine fibers. In another embodiment, the substrate fibers may have an average fiber diameter greater than approximately 0.6 microns, preferably greater than approximately 3 microns, and more preferably greater than 5 microns. In one embodiment, an average diameter of the bicomponent substrate fibers is between approximately 1 micron and approximately 40 microns, and more typically between approximately 10-40 microns.
[0053] The coarse fibers are compressed and/or heated, for example via a set of calender rollers and/or an oven, to form the substrate 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 wherein any of the substrate layers are between approximately 0.05 and 1.0 mm thick, preferably between approximately 0.1 and 0.5 mm. Such a substrate can provide a necessary structural support for the fine fibers. Bicomponent strong fabrics of various thicknesses suitable for use as any of the substrate layers are commercially available from various suppliers such as HDK Industries, Inc. of Rogersville, TN, or other filter media suppliers. Thereby, the substrate can be selected from such two-component free sell media.
[0054] In one embodiment, each layer of substrate 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 and the middle 122 comprise a strong fabric formed from bicomponent textile fibers having a polyester core with high melting point and a polyester coating with a low melting point. Bicomponent textile fibers are compressed together to form strong fabric, wherein the bicomponent textile fibers are chemically, mechanically and/or thermally bonded together. For example, bicomponent textile fibers are heated to or near the melting temperature of low melting polyester and compressed together, where the coating formed from the low melting polyester melts or softens and acts as a binding agent for bind fibers together.
[0055] The fine fibers 124, 126, 128, 130, 132, 134, 136, 138, 140, 142 can be deposited directly on the corresponding substrate 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 as they are formed. Alternatively, the fine fibers can be separately prepared as a fine fiber web, then laminated to the substrate. Although the fine fibers may comprise fibers having various fiber diameters, preferably the fines are nanofibers having very fine fiber diameter. Such fine fibers can be formed by electrospinning or other suitable processes. In one embodiment, the fine fibers are electrospinned nanofibers having an average fiber diameter less than about 1 micron, preferably less than 0.5 micron, and more preferably between 0.01 and 0.3 micron. Examples of the present invention employed a diameter less than 0.08 micron (80 nm). Such small diameter fine fibers can provide the ability to pack more fibers together in a given volume to provide increased fiber surface area, which can increase filtration efficiency while decreasing the pressure drop of a filter medium.
[0056] The fine fibers can be formed from various suitable polymeric materials. To avoid destruction of the fine fibers during heating and/or compression of the filter medium 100, the fine fibers are typically formed from a material having a higher melting temperature than at least the low melting point component of the bicomponent fibers of the substrate. . In preferred embodiments, the fine fibers are formed from a polyamide. Other suitable polymers include, but are not limited to, polyvinyl chloride (PVC), polyolefin, polyacetal, polyester, cellulose ether, polyalkylene sulfide, polyarylene oxide, polysulfone, modified polysulfone polymers and polyvinyl alcohol, polyamide, polystyrene, polyacrylonitrile , polyvinylidene chloride, polymethyl methacrylate, polyvinylidene fluoride. Solvents for making polymeric solutions for electrostatic spinning may include acetic acid, formic acid, m-cresol, trifluoro ethanol, hexafluoro isopropanol chlorinated solvents, alcohols, water, ethanol, isopropanol, acetone, and N-methyl pyrrolidone and methanol.
[0057] In one embodiment the fine fibers are formed from nylon-6 (polyamide-6, also referred to as "PA-6" here) through electrospinning, in which the electrospinned fine fibers are deposited directly onto the substrate. In this embodiment, fine fibers 124 are electrostatically generated from a solution containing nylon-6 and deposited onto a surface of substrate 102. Fine fibers 126 can be similarly generated and deposited on substrate layer 104, and so on. Substrate layers 102, 104, 106, 108, 110, 112, 114, 116, 118, 120 coated with electrospinned nanofibers 124, 126, 128, 130, 132, 134, 136, 138, 140, 142 are then laminated together with means 122 such that each layer of the fine fibers is sandwiched between the adjacent substrate and/or means 122 to create filter means 100 in the pre-compressed state 144 as shown in Figure 10. As discussed above, the filter media 100 in pre-compressed state 144 is then compressed to form filter media 100 in its final compressed state 146 as shown in Figures 1 and 2. In preferred embodiments, filter media 100 is heated before, during, and/ or after compression. For example, filter media 100 in the pre-compressed state 144 is heated prior to passing through roller assembly 148, 150. In addition, roller assembly 148.150 can be heated to further heat filter media 100 during compression.
[0058] Bonding between the fine fibers and adjacent coarse fibers of the substrates and/or medium 122 may involve solvent bonding, pressure bonding and/or thermal bonding. For example, since fine fibers are electrostatically generated from a polymer solution containing a solvent, the solvent remaining on the surface of the fine fibers can effect a solvent bond as the fine fibers come into contact with the thick fibers of the substrate. In addition, the low melting point component of the bicomponent substrate fibers can be used to increase the bond between the fine fibers and adjacent coarse fibers of the substrate. In such an embodiment, the filter medium 100 is heated to or near the melting point of the low melting point component and compressed, wherein the low melting point component of the bicomponent coarse fibers melts or softens, which allows the adjacent fine fibers incorporate into the low melting point component as they are compressed together, thereby increasing the bond between the thick fibers and the fine fibers (via pressure bonding and thermal bonding.) in a preferred embodiment, adhesion between the fine fibers and the substrate on which the fine fibers have been deposited is larger than that between the fine fibers and the other adjacent substrate. For example, the adhesion between fine fibers 124 and substrate 102 is greater than the adhesion between fine fibers 124 and substrate 104. As such, when a delamination is forced, the fine fibers 124 will delaminate from substrate 104 and remain on the substrate 102. Thus when forced, the filter medium 100 of such an embodiment can be separated into ten layers of substrates carrying fine fibers (102/124, 104/126, 106/128, 108/130, 110/132, 112/ 134, 114/136, 116/138, 118/140, 120/142) and the medium 122.
[0059] In one embodiment, each of the substrate layers is formed of a strong bicomponent fiber fabric having an average fiber diameter between approximately 1 and 40 microns and a basis weight between approximately 0.01 and 0.46 kg/yard2. The bicomponent fibers comprise a high melting polyester core and a low melting polyester coating. Thin ones are electrotrophied nanofibers formed from nylon-6. The fine fibers have an average fiber diameter between approximately 0.01 and 0.5 microns, wherein each layer of the fine fibers 124, 126, 128, 130, 132, 134, 136, 138, 140, 142 has a basis weight between approximately 0.03 g/m2 and 0.5 g/m2, providing total fine fiber base coverage between 0.3 g/m2 and 5 g/m2. The fine fiber coverage of filter media 100 for liquid particulate material filtration applications is significantly greater than the fine fiber coverage of air or gas filter media. A target basis weight of fine fibers in each substrate layer is selected in accordance with an average fine fiber diameter and a desired efficiency and capacity of the filter media. A desired efficiency and capacity of the filter medium 100 can be obtained by adjusting fine fiber diameter, fine fiber coverage on each substrate, number of fine fiber layers, amount of lift and compression.
[0060] Although fine fiber coating can be characterized in terms of a basis weight, the basis weight depends on a specific weight of a polymer(s) and a diameter of the fine fibers. Thus, it is more useful to characterize thin fiber coverage in terms of linear coverage per area (km/m2) as this takes away the variability associated with specific weight and thin diameter. In this way, the linear covering truly measures how much fiber is laid out as how much fiber. In that regard, preferred fine fiber linear coverage ranges are greater than 5,000 km/m2 for the higher coverage fine fibers, more preferably greater than 10,000 km/m2, and more preferably between 20,000 km/m2 and 60,000 km/m m2. Fine fiber coatings in various terms including basis weight and linear coating for fine fibers having an average fiber diameter of approximately 0.08 microns (80 nm) in accordance with embodiments of the present invention are shown below in Table 1. fine fibers of these modalities are formed from PA-6 having a density of 1.084 g/cm3 through an electrospinning process. As shown, table 1 includes 0.03 - 0.225 g/m2 fine fiber mass topping form. Table 1: Nanofiber Coverage


[0061] Although coverage of fine fibers may vary based on fiber diameter, based on examples using 80 nm fibers and other calculations, typically modalities employing fine fibers having an average diameter less than 500 nm will have similar coverage ranges for broad characterization and claim purposes. METHOD OF MAKING MULTILAYER COMPOSITE FILTER MEDIA
[0062] Figure 11 schematically illustrates a representative process of making a filter medium according to a processing modality of the present invention. While this embodiment includes process steps for making filter media 100 of Figure 9, the process can produce filter media in accordance with other embodiments of the present invention with minor modifications. A system 200 shown in Figure 11 includes an upstream system 201 for making a composite media including a substrate and fine fibers deposited thereon, and a downstream system 203 for laminating, elevating, and compressing multiple layers of composite media to make a media. of multi-layer composite filter for liquid particulate material filtration applications.
[0063] The upstream system 201 includes an unwind station 202, an electrospinning station 204, an optional oven 206, an optional roll set 207, and a rewind station 208. which is used here as a substrate layer, is unwound from the unwinding station 202. The strong fabric 212 unwound from the stiff fabric roll 210 travels in a machine direction 214 towards the electrospinning station 204. In the electrospinning station 204 , fine fibers 216 are formed and deposited onto a surface of the scrim 212 to form a composite medium 218 comprising the scrim carrying the fine fibers 216. The composite medium 218 can be heated and compressed in the optional oven 206 and the optional set of rolls 207 before being wound onto a roll of composite media 230 at rewind station 208 for improved adhesion between the fine fibers and the substrate.
[0064] The strong fabric can be formed in an upstream process of system 200 (part of a continuous line process or broken line process) or it can be purchased in a roll form from a supplier such as HDK or another medium supplier. suitable as H&V or Ahlstrom or similar. The strong fabric can be formed from various suitable materials, such as the bicomponent fibers of Figures 3-10 as discussed above. For example, the strong fabric can be formed from bicomponent textile fibers of low melting polyester/high melting core polyester coating, which are compressed and/or heated to form strong fabric roll 210 having a thickness and desired strength. Alternatively, the substrate layer can be another one-component medium that can be compressed and held in place through a solvent bond, heat bond or the like.
[0065] In the case of bicomponent fibers, for example, bicomponent fibers of the concentric core/cladding type can be co-extruded using a high melting polyester as the core and a low melting polyester as the coating. Such bicomponent fibers can then be used to form a strong fabric or filter medium. In one embodiment, bicomponent fibers are used as textile fibers to form a multicomponent filter medium or a strong fabric via the conventional air laying or dry laying process. The textile fibers used in this process are relatively short and discontinuous but long enough to be handled by conventional equipment. Bicomponent fiber bales can be fed through a trough feed and separated into individual fibers in a carding device, which are then air-laid onto a fiber web (which itself for the purposes of the present disclosure can be used as a substrate .) the fiber web is then compressed using a set of calender rolls to form the scrim roll 210 (which can also be used as a substrate). The fiber web can optionally be heated prior to entering the calender roll assembly. Since the scrim 210 of this embodiment comprises bicomponent fibers including a high melting point component and a low melting point component, it is also referred to as a bicomponent filter media. In some embodiments, the fiber web is folded before being calendered to form a coarser bicomponent filter media.
[0066] In a different embodiment, a web comprising polymer fibers with high melting point as polyester fibers and a web comprising polymer fibers with low melting point as polypropylene fibers can be formed, separated and laminated together to form the roll of bicomponent filter media or strong fabric. In such an embodiment, the fine fibers 216 are deposited on the low melting point side of the strong fabric 212. In that embodiment, the low melting weft is substantially thinner than the high melting weft, such that the low melting point component does not clog the high melting point web surface when heated and melted.
[0067] In another embodiment, the strong bicomponent fiber fabric can be formed through a melt blowing process. For example, cast polyester and cast polypropylene can be extruded and drawn with heated, high velocity air to form coarse fibers. Fibers can be collected as a weft on a movable screen to form a strong bicomponent fabric 210.
[0068] The multi-component fiber filter media or strong fabric can also be spunbonded using at least two different polymeric materials. In a typical spin bonding process, a molten polymeric material is passed through a plurality of extrusion holes to form a multifilament melt line. The multifilament fusion line is stretched to increase its tenacity and passed through a sudden cooling zone where solidification occurs which is collected on a support such as a moving screen. The spin bonding process is similar to the melt blowing process, however melt blown fibers are typically thinner than spin bonded fibers.
[0069] In yet another modality, the multicomponent filter media is wet seated. In a wet laying process, high-melt fibers and low-melt fibers are dispersed on a conveyor belt, and the fibers are spread into a uniform weft while still wet. Wet laying operations typically use fibers that are 0.63 cm to 1.90 cm in length, but sometimes longer if the fiber is stiff or thick. The fibers discussed above, in accordance with various embodiments, are compressed to form a strong fabric 210 or filter medium having a desired thickness.
[0070] Referring again to Figure 11, the strong tissue 212 enters the electrospinning station 204, wherein the fine fibers 216 are formed and deposited on a surface of the strong tissue 212. In the electrospinning station 204, the fine fibers 216 are electrospinned from electrospinning cells 222 and deposited in strong tissue web 212. The electrospinning process of System 200 may be substantially similar to the electrospinning process disclosed in Fine fibers under 100 nanometers and methods, publication of US patent application no. US 2009/0199717, assigned to the assignee of the present application, the entire disclosure of which is incorporated herein by reference thereto. Alternatively, groups of nozzles or other electrospinning or reorientation equipment from chain electrodes of cells 222 can allow fibers to be deposited in any desired orientation (e.g., up is shown although fibers can also be spun down, horizontally, or diagonally over a conveyor carrying thicker fibers).
[0071] The electrospinning process produces small diameter synthetic fibers, which are also known as nanofibers. The basic electrostatic wiring process involves introducing electrostatic charge into a running stream or polymer solution in the presence of a strong electric field, such as a high voltage gradient. The introduction of electrostatic charge into polymeric fluid in electrospinning cells 222 results in the formation of a jet of charged fluid. The charged jet accelerates and thins in the electrostatic field, drawn towards a base collector. In such a process, viscoelastic forces of polymeric fluids stabilize the jet, forming small diameter filaments. An average fiber diameter can be controlled by designing electrospinning cells 222 and formulating polymer solutions.
[0072] The polymeric solutions used to form the fine fibers can comprise various polymeric materials and solvents. Examples of polymeric materials include polyvinyl chloride (PVC), polyolefin, polyacetal, polyester, cellulose ether, polyalkylene sulfide, polyarylene oxide, polysulfone, modified polysulfone polymers and polyvinyl alcohol, polyamide, polystyrene, polyacrylonitrile, polyvinylidene chloride , polymethyl methacrylate, polyvinylidene fluoride. Solvents for making polymeric solutions for electrostatic spinning may include acetic acid, formic acid, m-cresol, trifluoro ethanol, hexafluoro isopropanol chlorinated solvents, alcohols, water, ethanol, isopropanol, acetone, and N-methyl pyrrolidone, and methanol. Solvent and polymer may be matched for proper use based on sufficient solubility of the polymer in a given solvent and/or solvent mixture (which may both be referred to as "solvent"). For example, formic acid can be chosen for nylon-6. Reference can be made to the aforementioned patents for further details on fine fiber electrospinning.
[0073] In electrospinning station 204, an electrostatic field is generated between electrodes in electrospinning cells 222 and a vacuum collecting conveyor 224, provided by a high voltage supply that generates a high potential difference. As shown in Figure 11, there may be multiple electrospinning cells 222 in which fibers 216 are formed. The fine fibers 216 formed in the electrodes of the electrospinning cells 222 are stretched towards the vacuum collecting conveyor 224 by the force provided by the electrostatic field. The vacuum collecting conveyor 224 also retains and transfers the strong tissue 212 in the machine direction 214. As configured, the strong tissue 212 is positioned between the electrospinning cells 222 and the vacuum collecting conveyor 224 such that the fine fibers 216 are deposited on the strong fabric 212. In embodiments, where the strong fabric 212 is a multi-component filter medium including a component with a low melting point on one surface and a component with a high melting point on the other surface, the strong fabric of multicomponent 212 is positioned between electrospinning cells 222 and vacuum collecting conveyor 224 such that the low melting point component surface of the multicomponent strong tissue faces electrospinning cells 222.
[0074] In a preferred embodiment, the electrospinning cells 222 contain a polymeric solution comprising polyamide-6 (PA-6) and an appropriate solvent consisting of 2/3 acetic acid and 1/3 formic acid. In such a solvent, both acetic acid and formic acid act as a dissolving agent to dissolve PA-6, and acetic acid controls the conductivity and surface tension of the polymer solution. Electrospin cells 222 generate fine fibers formed from PA-6, which are deposited on a surface of strong tissue 212. As fine fibers 216 are deposited on the surface of strong tissue 212, some fine fibers 216 entangle with thick fibers of the tissue. strong tissue near the surface facing the electrospinning cells 222. When some fine fibers 216 tangle with some thick fibers, solvent remaining in the fine fibers 216 from the electrospinning process can make a solvent bond between the fine fibers 216 and the thick fibers of strong fabric 212.
[0075] In other embodiments, the fine fibers can be formed by other suitable processes such as melt blowing process. For example, fine fibers having an average fiber diameter of approximately 0.6 - 0.7 microns can be formed by melt blowing under the influence of electric fields. In such embodiments, coarse fibers for a substrate are prepared to have an average fiber diameter at least 4 times larger than fine fibers. For differentiation purposes, fusion-blown fibers and electrospinned nanofibers are thus intended to be more specific terms than fine fibers, which are intended to be generic.
[0076] The bond between bicomponent fibers of the strong fabric 212 and the fine fibers 216 can be increased through thermal bonding and pressure bonding by the optional kiln 206 and the optional set of calender rolls 207. As the composite medium 218 is heated in oven 206, the low melting polymer component of the bicomponent fibers softens or melts and allows the fine fibers 216 to incorporate into the low melting polymer component. Thus, during the heat treatment, composite filter media 218 is heated to at least above the glass transition temperature of the low melting point component, and more preferably at or near the melting temperature of the low melting point component. For example, composite media 2318 is heated at or near the melting point of low melting polyester such that the outer low melting polyester layer of the bicomponent fibers melts and bonds with the formed fine fibers 216 of PA-6. In such embodiments, fine fibers of PA-6 216 and the high melting polyester core of the bicomponent fibers do not fuse, as PA-6 and the high melting polyester have a significantly higher melting temperature than than that of polyester with a low melting point. Low melting polyester, which has the lowest melting temperature, melts or softens, and adjacent PA-6 fine fibers 216 are incorporated into the softened or melted low melting polyester, thereby bonding the fine fibers 216 and 212 strong fabric together. Thereby, the low melting polyester acts as a bonding agent between the bicomponent fiber strong fabric 212 and the fine fibers 216. The bond between the fine fibers 216 and the strong fabric 212 can be further enhanced through bonding by pressure via the roller assembly 207. As the composite media passes through the rollers 207, the fine fibers 216 and the stiff fabric 212 are compressed together, wherein the fine fibers are further incorporated into the fibers of the stiff fabric 212. , compression reduces void spaces in the composite medium to form a composite medium 220 with increased strength.
[0077] Figures 12(A)-12(D) are Scanning Electron Microscopic (SEM) images of bicomponent fibers of tissue 212 and fine fibers 216 near the surface of tissue 212 taken at various levels of magnification. As shown in the SEM images taken at the x200 and x1000 magnification levels of Figures 12(A) and 12(B), the fine fibers 216 deposited in the strong woven web 212 form a spider net-like fiber structure between the bicomponent fibers thicker ones that are located close to the surface of the strong tissue 212. SEM images taken at higher magnifications (figure 12(C) at x2,000 and figure 12(D) at x10,000) show the bond between the fine fibers 216 and bicomponent fibers. As clearly shown in Figure 12(D), the fine fibers 216 are incorporated into the low melting polyester surface of the bicomponent fibers.
[0078] The composite media roll 230 including the bicomponent strong fabric 212 and the fine fibers 216 is laminated with other composite media 232, 234, 236, 238, 240, 242, 244, 246, 248, and a media 250 in the system downstream 203. Each of composite media rolls 230, 232, 234, 236, 238, 240, 242, 244, 246, 248, and a middle roll 250 are each unwound from unwind stations 252, 254, 256, 258, 260, 262, 264, 266, 268, 270, 272, and laminated together by a set of rollers 274. The set of rollers may be calendering rollers to apply significant pressure to laminate and significantly reduce a thickness of the composite media layers . Alternatively, roller assembly 274 may apply slight pressure to laminate and reduce the thickness of the laminated layers just enough to fit through an oven 276. In such an embodiment, the laminated layers 280 are heated in the oven 276 and compressed through an oven. calender roll assembly 282, wherein the laminated layers 280 are pressed together in a compressed state having a desired thickness and strength.
[0079] In this embodiment, each composite media roll 232, 234, 236, 238, 240, 242, 244, 246, 248 is prepared similarly as composite media roll 230. Therefore, each composite media roll 232, 234 , 236, 238, 240, 242, 244, 246, 248 includes a substrate formed from a strong woven bicomponent fiber 284, 286, 288, 290, 292, 294, 296, 298, 300, and electrospun nanofibers 302, 304, 306, 308, 310, 312, 314, 316, 318, loaded by the bicomponent fiber scrim 284, 286, 288, 290, 292, 294, 296, 298, 300.
[0080] In one embodiment, each of the substrates 212, 284, 286, 288, 290, 292, 294, 296, 298, 300 and the medium 250 are formed from the same strong bicomponent fiber fabric having a thickness between approximately 0. 05 mm and 1.0 mm. Each layer of fine fibers 216, 302, 304, 306, 308, 310, 312, 314, 316, 318 is formed by electrospinning PA-6 polymer solution to produce a fine fiber covering between approximately 0.03 g/m2 and 0.5 g/m2. In other embodiments, substrates may be formed from different types of filter media or strong fabric, and each of the fine fiber layer may have different fine fiber coverage.
[0081] Composite medium 280 is heated in oven 276 to or near a melting temperature of the low melting point polyester component of the bicomponent fiber strong fabric. During heating the substrates may relax and expand in thickness. Thus, the elevated composite medium 281 may have a thickness that is at least 1.5 times, 2 times, 3 times or even greater than the thickness of the composite medium 280 before being heated in oven 276. The elevated composite medium 281 is then compressed through the calendering roller assembly 282 in the compressed state 320. The composite medium is compressed such that the thickness of the composite medium 280 is reduced by between approximately 50% and 300%, preferably between approximately 70% and 200% and more preferably between approximately 50% and 300%, preferably between approximately 70% and 200%, and more preferably between approximately 80% and 150% of the original thickness of the composite medium 280 before heating ((total thickness of 10 layers of strong fabric) carrying 10 layers of fine fibers + thickness of medium - thickness of composite medium in compressed state 320)/(total thickness of 10 layers of strong fabric carrying 10 layers of fine fibers + thickness of medium).) to re Thickness reduction may depend on the amount of lift during heating. Thus, when the heating rise is large, the final thickness of the composite medium after compression may be greater than the initial thickness of the composite medium before heating. Composite media in the compressed state 320 is then wound onto a roll of filter media 324.
[0082] In this embodiment, the composite medium rollers 230, 232, 234, 236, 238, 240, 242, 244, 246, 248. And the medium 250 are laminated together such that each of the fine fiber layers 216 , 302, 304, 306, 308, 310, 312, 314, 316, 318 is sandwiched between adjacent substrate layer and/or media. However, in other embodiments, the composite media layers may be laminated such that some of the fine fiber layers face each other to form fine fiber-to-fine fiber or substrate-to-substrate bond in the final composite medium 320. For example, system 200 can be used to make filter media 500 of Figure 15. In this embodiment, each of the first five unwind stations 252, 254, 256, 258, 260 unwinds a roll of composite media such that the nanofibers are facing upwards as shown in Figure 11. Meanwhile, the unwind station 262 unwinds a composite medium such that the nanofibers are facing downwards. As such, the fine fibers in the first four substrate layers 514, 516, 518, 520 are sandwiched between substrates 502, 504, 506, 508, 510 as shown in Figure 15. Meanwhile, the fine fibers 522 in substrate 510 and the fine fibers 524 of substrate 512 are turned together forming the fine fiber-fine fiber.
[0083] Figure 13 schematically illustrates a system and a method of making a filter medium according to a different embodiment of the present invention. A system 400 generally includes an unwind station 402, an electrospinning station 404, a folding station 406, a roller assembly 408, an oven 410, and a calendering roller assembly 412 and a rewind station 414.
[0084] In this modality a roll of substrate 416 is unwound from unwind station 402 and transferred to electrospinning station 404, where fine fibers are formed and deposited on a surface of substrate 416. Electrospin station 404 and the process are similar to electrospinning station 204 and the process described above. In this embodiment, substrate 416 is a strong fabric formed from bicomponent fibers including a high melting polyester core and a low melting polyester coating. Fine fibers 418 are formed from PA-6.
[0085] Composite medium 420 comprising substrate 416 and fine fibers 418 is folded at folding station 406. Composite medium 420 can be folded into 2-20 folds in thickness depending on the desired characteristics of the final medium. As shown, folding creates both fine-fiber-to-fine-fiber laminated surfaces and substrate-to-substrate laminated surfaces. Folding station 406 in this embodiment is shown as folding composite media 420 in a line direction such that the folds are pointing toward roller assembly 408. However, in other embodiments, composite media 402 may be folded such that the folds are pointing towards electrospinning station 404, or folded in cross-line directions. The folded composite media 422 is then compressed to an appropriate thickness to pass through an oven 410. As the composite media 424 is heated, the low melting polyester coating melts or softens to effect thermal bonding between layers. Upon exiting the furnace 410, the composite medium 424 passes through the set of calender rolls 412. The calender rolls 412 are separated from each other according to a desired final thickness of the medium. The composite medium 424 is pressed down to a compressed state having a desired thickness as it passes through the set of calender rolls 412.
[0086] In addition, layers of media 426, 428 are laminated to each surface of media 430 and rolled into a roll at rewind station 414. An expanded cross-sectional view of a filter media 432 including media 430, as layers of media 426, 428 is shown in Figure 13. As shown, media 430 includes multiple layers of substrate 416 and multiple layers of fine fibers 418 in an orientation inclined from the folding process. Media layers 426, 428 can be formed from any suitable medium, but in this embodiment, media layers 426, 428 are formed from the same bicomponent fiber scrim used for substrate 416.
[0087] Figure 14 still shows a different modality of a system and a process of making a medium. A 600 system is similar to a 400 system but the fine fibers in this modality are not deposited onto a substrate. Instead, fine fibers are formed and deposited onto a loosely tangled thick fiber web. System 600 generally includes a chute 602, a carding device 603, an electrospinning station 604, a folding station 606, a roller set 608, an oven 610, and a calendering roller set 612 and a winding station again 614.
[0088] In system 600, the coarse fiber web 616 is formed from textile fibers using a dry laying or air laying process. The textile fibers of this embodiment are bicomponent fibers comprising a high melting polyester core and a low melting polyester coating. Bicomponent textile fibers are relatively short and discontinuous, but long enough to be handled by conventional equipment. Textile fiber bales are separated into individual fibers and air laid to form coarse fiber web 616. At this point, coarse fiber web 616 can be tangled together in a thick, highly fuzzy state and cannot be bonded together. Coarse fiber web 616 can be easily separated with very little manual effort and has little structural integrity at that point such that it is not considered a filter media or substrate in the conventional sense.
[0089] The coarse fiber web 616 is transferred through a conveyor belt 617 towards the electrospinning station 604, where the fine fibers 618 are formed and deposited onto a surface of the coarse fiber web 616. As the fibers fines 618 are deposited in coarse fiber web 616, fibers 618 are integrated with coarse fibers of coarse fiber web 616 much more than in the previous embodiment with substrate 416, as coarse fiber web 616 is much more porous and less dense to allow deeper integration of fine fibers 616.
[0090] The coarse fiber web 616 integrated into the fine fibers 618 is then folded into 10-30 plies at the folding station 606 and compressed through the roller set 608, which is heated in the oven 610 and compressed again through the roller set of calendering 612 as it was with system 400. The medium 630 is then laminated with a layer of medium 626 and a porous layer 628 for a filter medium 632. The coarse bicomponent fibers and the fine fibers of the medium 630 of this embodiment are very more integrated. Thus, a cross-sectional view of medium 630 does not show multiple layers, but instead looks more like a single integrated medium 630. Medium 630 has sufficient fine fiber coating and structural integrity to capture particulate matter from a stream. liquid, such as a hydrocarbon fuel stream. EXAMPLES OF MULTILAYER FILTER MEDIA AND TEST RESULTS
[0091] Figure 15 is a schematic cross-sectional view of a filter medium 500 according to a different embodiment of the present invention. Filter media 500 is similarly constructed as filter media 100, but includes six layers of substrates 502, 504, 506, 508, 510, 512, each of which carries fine fibers 514, 516, 518, 520, 522, 524, instead of ten layers of substrate carrying fine fibers. In addition, the most upstream composite media layer comprising substrate layer 512 and fine fibers 524 is inverted such that fine fibers 524 face fine fibers 522 forming a fine fiber-fine fiber interface. As shown, substrate 512 provides an upstream surface 526 of filter media 500, thereby fine fibers are not exposed and protected.
[0092] Test samples of filter medium 500 were prepared in a laboratory. Test samples of all modalities described here are prepared to have a sample area of 0.009 m2. A strong bicomponent fiber fabric comprising a high melting polyester core and a low melting polyester coating having a basis weight of 35.0 GSY was used for each of the substrate layers 502, 504, 506, 508, 510 , 512. The fine fibers were formed through an electrospinning process from a polymer solution comprising PA-6 and deposited on each of the substrate layers. On substrate 512, approximately 0.05 g/m2 of the PA-6 524 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 9176 km/m2 (5.702 mi/m2.) On substrate 510, approximately 0.15 g/m2 of the PA-6 522 nanofibers having a fiber diameter average of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately t 27,530 km/m2 (17.106 miles/m2.) in each of the substrate layers 502, 504, 506, 508, approximately 0.225 g/m2 of the nanofibers PA-6 514, 516, 518, 520 having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 41,290 km/m2 (25,659 miles/m2) on each substrate. Thus, filter media 500 includes a total fine fiber basis weight of approximately 1.1 g/m2, which provides approximately 201,866 km/m2 (125,444 miles/m2) of linear fiber coverage.
[0093] The six layers of substrate carrying the fine fibers were arranged as shown in Figure 15 such that the substrate layer 512 forms the upstream surface 526 and the substrate layer 502 forms the downstream surface 528. The six layers of composite media were heated and compressed through a calender roll as described in the above embodiments to form composite filter media 500.
[0094] Test samples of filter media 500 were prepared and tested for efficiency and dust holding capacity in accordance with the international standard ISO 16889 for multi-pass method to evaluate filtration performance. All tests were carried out using a Mil-H-5606 hydraulic fluid having a viscosity at the test temperature of 15 mm2/s and loaded with ISOMTD test powder.
[0095] In the first test, the test fluid having a base amount contaminant concentration of 5.00 mg/L was used at a flow rate of 0.26 GPM. Figure 16 shows particle counts per mL and filtration ratio at 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, and 100% time intervals during the 6-hour trial period. When the test results have been converted to a fluid cleanliness rating in accordance with ISO code 4406:99 (R4/R6/R14), the cleanliness rating at 10% time interval is 7/5/0, at 100% it is 13/11/7, and the average is 6/4/0.
[0096] In the second test, the test fluid having a background contaminant concentration of 15.00 mg/L was used at a flow rate of 0.26 GPM. Figure 17 shows particle counts per ml and filtration ratio test results. The clean rating at 10% time interval is 7/6/0, at 100% it is 19/18/14, and the average is 12/11/7.
[0097] Test samples of filter media 500 for the third test were prepared in a laboratory similarly to the test samples for the first test and second test. However, the fine fiber basis weight of each substrate layer has changed. On each of substrates 510 and 512, approximately 0.05 g/m2 of PA-6 nanofibers 522, 524 having an average fiber diameter of 0.08 microns was formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 9176 km/m2 (5.702 miles/m2) on each substrate. On substrate 508, approximately 0.075 g/m2 of the PA-6 520 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 13,760 km/m2 (8.553 miles/m2.) On substrate 506, approximately 0.09 g/m2 of PA-6 518 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 16,520 km/m2 (10.263 miles/m2.) on substrate 504, approximately 0.15 g/m2 of PA-6 516 nanofibers having an average diameter of 0.08 micron fiber were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 27,530 km/m2 (17,106 miles/m2.) on substrate 502, approximately 0.225 g/m2 of the PA-6 514 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a fine fiber linear coverage of approximately 41,290 km/m2 (25.659 miles/m2.) therefore, filter media 500 includes a total fine fiber basis weight of approximately 0.64 g /m2, which provides approximately 117,452 km/m2 (72,985 miles/m2) of linear fiber coverage.
[0098] In the third test, the test fluid having a background contaminant concentration of 15.00 mg/L was used at a flow rate of 0.26 GPM. Figure 18 shows particle counts per ml and filtration ratio test results. The clean rating at 10% time interval is 9/11/4, at 100% it is 17/16/11, and the average is 16/15/10.
[0099] Figure 19 is a schematic cross-sectional view of a filter media 600 according to a different embodiment of the present invention. Filter media 600 is similarly constructed as filter media 500 of Figure 15, however, filter media 600 includes five layers of substrate 602, 604, 606, 608, 610 and five layers of fine fiber 612, 614, 616 , 618, 620. Test samples of filter media 600 for the fourth test were prepared in a laboratory similarly to the previous test samples. For these test samples, approximately 0.15 g/m2 of the PA-6 nanofibers 612, 614, 616, 618, 620 having an average fiber diameter of 0.08 microns were formed and deposited on each of the 602 substrate layers, 604, 606, 608, 610. This fine fiber basis weight level provides a fine fiber linear coverage of approximately 27,530 km/m2 (17,106 miles/m2) on each substrate. Thus, filter media 600 includes a total final fiber basis weight of approximately 0.75 g/m2, which provides approximately 137,650 km/m2 (85,530 miles/m2) of linear fiber coverage.
[00100] In the fourth test, the test fluid having a base amount contaminant concentration of 15.00 mg/L was used at a flow rate of 0.26 GPM. Figure 20 shows particle counts per ml and filtration ratio test results. The clean rating at 10% time interval is 10/8/0, at 100% it is 16/13/11, and the average is 12/14/8.
[00101] Figure 21 is a schematic cross-sectional view of a filter media 700 according to yet another embodiment of the present invention. Filter media 700 is similarly constructed as filter media 500 of Figure 15, however filter media 700 includes three layers of substrate 702, 704, 706 and three layers of fine fiber 708, 710, 712. 700 filter media for the fifth test were prepared in a laboratory similarly to the previous test samples. For these test samples, approximately 0.075 g/m2 of PA-6 712 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited onto substrate 706. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 13,760 km/m 2 (8.553 mi/m 2 ) on substrate 704, approximately 0.09 g/m 2 of the PA-6 710 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 16,520 km/m2 (10.263 miles/m2.) . on substrate 702, approximately 0.15 g/m2 of the PA-6 708 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 27,530 km/m2 (17,106 miles/m2.) therefore, filter media 700 includes a total fine fiber basis weight of approximately 0.315 g/m2. , which provides approximately 57,810 km/m2 (35,922 miles/m2) of linear fiber coverage.
[00102] In the fifth test, the test fluid having a base amount contaminant concentration of 5.00 mg/L was used at a flow rate of 0.26 GPM. The figure. 22 shows particle counts per mL and filtration ratio test results. The cleaning rating at 10% time interval is 11/10/5, at 100% it is 11/9/4, and the average is 9/8/0. TUBULAR DEPTH FILTER TEST EXAMPLES AND RESULTS
[00103] Tubular depth filters such as those shown in figures 1-1(A) including sheets of fine fiber multilayer filter media such as those shown in figures 15, 19, 21 have been prepared and tested for efficiency and dust retention in accordance with international standard ISO 16889 for multiple pass method to evaluate filtration performance. All tests were carried out using a Mil-H-5606 hydraulic fluid having a viscosity at the test temperature of 15 mm2/s and loaded with ISOMTD test powder. Tubular depth filters including fine fiber multilayer filter media sheets in accordance with embodiments of the present invention had superior efficiency test results than the standard tubular depth filter (benchmark).
[00104] The standard tubular depth filter was prepared similarly to the method described and shown in figures 3 and 6 using a 4-station winding machine. Station 2 fed an intercalation of glass microfiber sheet onto a polyester sheet to form the standard tubular depth filter. Test fluid having a base upstream contaminant concentration of 5.00 mg/L was used at a flow rate of 2.4 GPM. Figure 24 shows particle counts per ml and filtration ratio test results. The cleaning rating at 10% time interval is 15/14/9, at 100% it is 16/14/10, and the average is 16/15/9.
[00105] A tubular depth filter media including fine fiber multilayer media was prepared using the 4-station roll-up machine similarly as the standard tubular depth media. In this embodiment, a fine fiber multilayer filter media of Figure 19 was used as a replacement for station 2 in place of the glass microfiber sheet and a fine fiber multilayer filter media of Figure 21 was used as the interleaf for station 3 instead of the PEM sheet.
[00106] For station 2 fine fiber replacement medium, approximately 0.225 g/m2 of PA-6 nanofibers 612, 614 having an average fiber diameter of 0.08 microns were formed and deposited on each of the 602 substrate layers , 604. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 41,290 km/m2 on each substrate. On substrate 606, approximately 0.015 g/m2 of the PA-6 616 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 27,530 km/m2. In each of the substrate layers 608, 610, approximately 0.075 g/m 2 of the PA-6 nanofibers 618, 620 having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 13,760 km/m2 on each substrate. Thus, filter media 600 includes a total fine fiber basis weight of approximately 0.75 g/m2 which provides approximately 137,630 km/m2 of linear fiber coverage.
[00107] For station 3 fine fiber replacement medium, approximately 0.09 g/m2 of PA-6 708 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited on substrate layer 702. fine fiber basis weight provides a linear fine fiber coverage of approximately 16,520 km/m2. On substrate 704, approximately 0.075 g/m2 of the PA-6 710 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 13,760 km/m2. On substrate 706, approximately 0.05 g/m2 of the PA-6 712 nanofibers having an average fiber diameter of 0.08 microns were formed and deposited. This fine fiber basis weight level provides a linear fine fiber coverage of approximately 9,176 km/m2. Thus, filter media 600 includes a total fine fiber basis weight of approximately 0.215 g/m2 which provides approximately 39,456 km/m2 of linear fiber coverage.
[00108] First test samples of the tubular depth filter including the fine fiber multilayer intersheets of this modality were tested using the test fluid having a base amount contaminant concentration of 5.00 mg/L was used at a rate 3.0 GPM stream. Figure 25 shows particle counts per ml and filtration ratio test results. The cleaning rating at 10% time interval is 10/7/0, at 100% is 16/15/7, and the average is 12/14/4.
[00109] Second test samples of the tubular depth filter including the fine fiber multilayer intersheets of this modality were tested using the test fluid having a base amount contaminant concentration of 5.00 mg/L was used at a rate 1.0 GPM stream. Figure 26 shows particle counts per ml and filtration ratio test results. The cleaning rating at 10% of time interval is 8/6/0, at 100% is 16/14/5, and the average is 13/11/0.
[00110] All references, including publications, patent applications, and patents cited herein are hereby incorporated by reference to the same extent as if each reference were individually and specifically indicated to be incorporated by reference and have been set forth in the full here.
[00111] The use of the terms "a" and "an" and "o, a" and similar referents in the context of describing the invention (especially in the context of the following claims) shall be interpreted as covering both the singular and the plural, a unless otherwise indicated here or clearly contradicted by context. The terms "comprising", "having", "including" and "containing" are to be interpreted as unlimited terms (ie meaning "including, but not limited to,") unless otherwise noted. The recitation of ranges of values here is merely intended to serve as an abbreviated method of referring individually to each separate value comprised in the range, unless otherwise indicated herein, and each separate value is incorporated into the descriptive report as if it were individually mentioned here. All methods described herein may be performed in any appropriate order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (eg, “how”) provided herein is merely intended to further illuminate the invention and does not pose a limitation on the scope of the invention unless otherwise claimed. No language in the descriptive report should be interpreted as indicating any element not claimed to be essential to the practice of the invention.
[00112] Preferred embodiments of the present invention are described herein, including the best mode known to the inventors for carrying out the invention. Variations in preferred modalities may become evident to those of ordinary skill in the art upon reading the above description. The inventors expect that skilled artisans will employ such variations as appropriate, and the inventors intend that the invention be practiced other than as specifically described herein. Accordingly, the present invention includes all modifications and equivalents of subject matter recited in the claims appended hereto as permitted by applicable law. Furthermore, any combination of the above-described elements in all possible variations thereof is encompassed by the invention unless otherwise indicated herein or otherwise clearly contradicted by the context.

权利要求:
Claims (17)
[0001]
1. Filter element CHARACTERIZED in that it comprises: an unplied tubular ring of a medium depth having a medium thickness of at least % of centimeter; the depth medium comprising carrier fibers and fine electro-spun fibers, the carrier fibers having an average size greater than 600 nanometers; and fine fibers having an average size of less than 800 nanometers carried by the carrier fibers; wherein the fine fibers have a size that is at least 4 times as small as the carrier fibers, and wherein said depth means comprises multiple layers of carrier fiber substrate wound with fine fibers throughout the depth of the depth means, the depth medium having a full depth carrier fine fiber coverage of at least 0.1 g/m2 and at least 10,000 km/m2.
[0002]
2. The filter element according to claim 1, CHARACTERIZED by the fact that the depth means of the filter element comprises a first sheet of filter media, wherein the first sheet of filter media comprises at least one substrate comprising carrier fibers and at least one layer of the fine fibers deposited thereon, the first filter means of the sheet being at least partially wrapped around itself to create at least some of said multiple layers throughout the depth of the depth means.
[0003]
3. Filter element according to claim 2, CHARACTERIZED by the fact that the first sheet of filter medium comprises a composite medium of a plurality of layers of strong fabric, forming a plurality of substrate layers and a plurality of layers of fine fiber, said plurality of layers of scrim and said plurality of layers of fine fiber being laminated together in the first sheet of filter media, with selected fine fiber layers being spaced apart and separated in the first sheet of filter media by the strong fabric.
[0004]
4. Filter element according to claim 2, CHARACTERIZED by the fact that the first sheet of filter media has a fine fiber coverage level having an average size less than 500 nanometers of at least 5,000 km/m2.
[0005]
5. Filter element, according to claim 2, CHARACTERIZED by the fact that the filtration structure is free of micro-glass.
[0006]
6. Filter element according to claim 2, CHARACTERIZED by the fact that the depth medium of the filter element further comprises a second sheet of filter medium, the second sheet of filter medium comprising fibers of a larger average size than 1 micron, the second sheet of filter media being at least partially rolled over itself to further create one of said multiple layers over the entire depth of the depth means.
[0007]
7. Filter element according to claim 6, CHARACTERIZED by the fact that the first sheet of filter media is arranged downstream and radially into the second sheet of filter media.
[0008]
8. The filter element according to claim 7, CHARACTERIZED by the fact that the medium depth of the filter element comprises a third sheet of filter medium, wherein the third sheet of filter medium comprises at least one substrate comprising carrier fibers and at least one layer of the fine fibers deposited thereon, the third sheet filter means being at least partially rolled over itself to further create one of said multiple layers throughout the depth of the depth means, wherein the third sheet of filter media is disposed downstream and radially into the second sheet of filter media.
[0009]
9. Filter element according to claim 2, CHARACTERIZED by the fact that the first sheet of filter media includes an upstream face and a downstream face, wherein the sheet of filter media has a heavier concentration of fine fibers near the downstream face compared to the upstream face.
[0010]
10. Filter element according to claim 9, CHARACTERIZED by the fact that the first sheet of filter media comprises multiple depositions of fine fibers across the entire depth of the first sheet of filter media from the upstream face to the downstream face, the depositions being heavier closer to the downstream face to create an increasing gradient of fine fibers from the upstream face to the downstream face.
[0011]
11. Filter element according to claim 2, CHARACTERIZED by the fact that the first sheet of filter media is a strip of partial length that extends substantially shorter than a total axial length of the filter element, the strip of partial length being helically wound around a central geometric axis defined by the filter element with the partial length strip partially overlapping itself between 1-8 times, whereby a cross-sectional width of the strip is aligned diagonally with respect to the central geometric axis.
[0012]
12. Filter element according to claim 2, CHARACTERIZED by the fact that the first sheet of filter media is a full length strip that extends approximately for the full axial length of the filter element, the full length strip being spirally wound around a central geometric axis defined by the filter element.
[0013]
13. Filter element according to claim 1, CHARACTERIZED by the fact that the depth medium comprises alternating layers of melt-blown fibers and fine fibers deposited on the melt-blown fibers, wherein the melt-blown fibers serve as the carrier fibers.
[0014]
14. Filter element, according to claim 1, CHARACTERIZED by the fact that the fine fibers are electro-spun and have an average size smaller than 500 nanometers; wherein the depth medium has a loaded fine fiber coverage over the entire depth of at least 0.5 g/m2 and at least 50000 km/m2.
[0015]
15. Method of making a filter element, CHARACTERIZED in that it comprises: electrospinning fine fibers having an average size less than 800 nanometers from a solution comprising a polymer and a solvent under the effect of a potential difference; depositing the fine fibers on a carrier fiber substrate, the carrier fibers having an average size of at least 3 micrometers; fine fibers having a size that is at least 4 times as small as the carrier fibers; and winding the carrier fiber substrate and fine fibers into a depth medium having a thickness of at least 1/2 centimeter and comprising multiple layers of substrate and fine fibers over the entire depth of the depth medium, the depth medium having a full depth carrier fine fiber coverage of at least 0.1 g/m2 and at least 10000 km/m2.
[0016]
16. Method according to claim 15, CHARACTERIZED in that it further comprises: employing a multicomponent substrate having a higher melting component and a lower melting component, further comprising rearranging the fine fibers deposited on the substrate by applying heat to relax the multicomponent substrate.
[0017]
17. Method according to claim 15, CHARACTERIZED by the fact that it further comprises sandwiching at least one layer of fine fiber between protective layers upstream and downstream of the substrate to protect the fine fibers during winding, in which the winding is subsequent to deposition.

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法律状态:
2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|

---

2019-10-01| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|

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2020-11-03| B25A| Requested transfer of rights approved|Owner name: PARKER-HANNIFIN CORPORATION (US) |

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2020-12-08| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application [chapter 6.1 patent gazette]|

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2021-03-23| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2021-04-20| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 10 (DEZ) ANOS CONTADOS A PARTIR DE 20/04/2021, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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US30848810P| true| 2010-02-26|2010-02-26|

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US61308488|2010-02-26|

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US33046210P| true| 2010-05-03|2010-05-03|

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US61330462|2010-05-03|

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US38356910P| true| 2010-09-16|2010-09-16|

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US38348710P| true| 2010-09-16|2010-09-16|

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US61383.569|2010-09-16|

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US61383487|2010-09-16|

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