EP0842310A1 - Method and apparatus for the production of artificial fibers, non-woven webs and sorbency non-woven fabrics - Google Patents
Method and apparatus for the production of artificial fibers, non-woven webs and sorbency non-woven fabricsInfo
- Publication number
- EP0842310A1 EP0842310A1 EP96926103A EP96926103A EP0842310A1 EP 0842310 A1 EP0842310 A1 EP 0842310A1 EP 96926103 A EP96926103 A EP 96926103A EP 96926103 A EP96926103 A EP 96926103A EP 0842310 A1 EP0842310 A1 EP 0842310A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fluid
- plenum
- perturbation
- die
- fluid flow
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D4/00—Spinnerette packs; Cleaning thereof
- D01D4/02—Spinnerettes
- D01D4/025—Melt-blowing or solution-blowing dies
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
- D01D5/0985—Melt spinning methods with simultaneous stretching by means of a flowing gas (e.g. melt-blowing)
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
- D04H3/03—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random
Definitions
- This invention relates generally to the production of man-made fibers, and particularly, to the field of production of man-made fibers using melt-blown, coform and spunbond techniques.
- Figures la-lc illustrate a typical approach for producing melt-blown fibers.
- a hopper 10 contains pellets of resin.
- Extruder 12 melts the resin pellets by a conventional heating arrangement to form a molten extrudable composition which is extruded through a melt-blowing die 14 by the action of a turning extruder screw (not shown) located within the extruder 12.
- a turning extruder screw not shown
- Figure lc the extrudable composition is fed to the orifice 18 through extrusion slot 28.
- the die 14 and the gas supply fed therethrough are heated by a conventional arrangement (not shown) .
- Figure lb illustrates the die 14 in greater detail.
- the orifices 18 which are arranged in a linear array across the face 16.
- inlets 20 and 21 feed heated gas to the plenum chambers 22 and 23.
- the gas then exits respectively through the passages 24 and 25 to converge and form a gas stream which captures and attenuates the polymer or resin threads extruded from orifice 18 to form a gas borne stream of fibers 26 as is seen in Figure la.
- the melt-blowing die 14 includes a die member 36 having a base portion 38 and a protruding central portion 39 within which an extrusion slot 28 extends in fluid communication with the plurality of orifices 18, the outer ends of which terminate at the die tip.
- the gas borne stream of fibers 26 is projected onto a collecting device which in the embodiment illustrated in Figure la includes a foraminous endless belt 30 carried on rollers 31 and which may be fitted with one or more stationary vacuum chambers (not shown) located beneath the collecting surface on which a non-woven web 34 of fibers is formed.
- the collected entangled fibers form a coherent web 34, a segment of which is shown in plan view in Figure 2.
- the web 34 may be removed from the belt 30 by a pair of pinch rollers 33 (shown in Fig.
- FIG. 1 illustrates a prior art apparatus 44 for producing spunbond fibers.
- the spunbond apparatus typically contains a fiber draw unit 46 positioned above an endless belt 78 which is supported on rollers 76.
- Figure 3b illustrates the fiber draw unit in greater detail.
- Fiber draw unit 46 includes upper air regions 48 and 50 and a longitudinal air chamber which contains an upper portion 52, a mid-portion 54, and a lower portion or tail pipe 56.
- the fiber draw unit also includes a first air plenum 58 and an air inlet 60 leading from the first air plenum 58 to mid ⁇ portion 54 of the fiber draw unit. Additionally, a second air plenum 62 also communicates with mid-portion 54 of the fiber draw unit via air inlet 64.
- the spunbond apparatus 44 also includes standard equipment for melting an extruding resin through dies to create fibers 68. Typically, this equipment feeds resin fed from a supply to a hopper extruder, through a filter, and finally through a die to create the fibers 68.
- High velocity air is admitted into the fiber draw unit through plenums 58 and 62 via inlets 72 and 74, respectively.
- the addition of air to the fiber draw unit through inlet 60 and 64 aspirates air through inlets 50 and 48.
- the air and fibers then exit through tail pipe 56 into exit area 70.
- air admitted into the fiber draw unit through inlets 50 and 48 draws fibers 68 as they pass through the fiber draw unit.
- the drawn fibers are then laid down on endless belt 78 to form a non-woven web 80 as is seen in Figure 3a. Rollers 82 may then remove the non-woven web from the endless belt 78 and further press the entangled fibers H together to assist in forming the web.
- the web 80 is then bonded, such as by embossing by calender and anvil, ultrasonic embossing, or other known technique, to form the finished material. It is well known in the art to vary a number of processing parameters in both melt-blown and spunbond fiber forming processes to obtain fibers of desired properties in order to form fabrics with desired characteristics. However, the majority of prior art techniques for varying fiber characteristics required more time consuming changes in machinery or process, such as changing dies or changing the resins. Therefore, those techniques required that the production line be halted while the necessary changes were made, which resulted in inefficiency when a new material was to be run.
- the present invention relates to an apparatus for forming artificial fibers from a liquefied resin and for forming a non-woven web.
- the apparatus may include means for generating a substantially continuous airstream for entraining fibers along a primary axis, at least a first extrusion die located next to the airstream for extruding the liquefied resin, and perturbation means for selectively perturbing the air stream by varying the air pressure on either side or both sides of the primary axis.
- the apparatus may also include a substrate disposed below the first die, substrate translation means for moving the substrate relative to the die, wherein the entrained fibers are deposited on the substrate to form a non-woven web.
- the apparatus may include a first supply of air connected to first and second air plenum chambers located on opposite sides of the axis, wherein plenum chambers outlets provide a substantially continuous air stream for fiber attenuation.
- the perturbation means may include a valve for selectively varying the airflow rate to the first and second plenums, thereby providing airflow perturbation to the entrained fibers. Additionally, airstream perturbation may be achieved by superimposing a perturbed secondary air supply on the first air supply within the plenum chambers.
- the perturbation means may include first and second pressure transducers adjacent or attached to the first and second plenum chambers, and means for selective activation of the first and second pressure transducers for selectively varying the pressure in the first and second plenum chambers.
- the perturbation means varies a steady state pressure in the first and second plenum chambers at a perturbation frequency of approximately less than 1000 Hertz, and varies an average plenum pressure in the first and second plenum chamber up to about 100% of the total average plenum pressure in the absence of activation of the perturbation means.
- the apparatus may also include a fiber draw unit disposed below the first die and adapted to channel the primary air flow therethrough.
- the fiber draw unit may include a fiber inlet at a top portion thereof for receiving fluid flow and fibers entrained therein, an outlet for dispensing the air entrained fibers onto the substrate.
- the apparatus may also include a multiple die arrangement for extruding several types of resin simultaneously, as well as means for adding other fibers or particulates (coform) .
- the apparatus may also include first and second secondary perturbing air supplies disposed on opposite sides of said axis and near the die or fiber draw unit for alternatingly perturbing the substantially continuous flow of air.
- the present invention also relates to a method for forming artificial fibers from a liquefied resin and forming a non-woven web thereby, comprising the steps of generating a substantially continuous air stream along a primary axis, extruding the liquefied resin through a first die located adjacent to the air stream, entraining the liquefied resin in the air, stream to form fibers, selectively perturbing the flow of air in the airstream by varying the air pressure on either side of the primary axis.
- Figures la-lc illustrate schematic representations of a prior art apparatus for producing melt-blown fibers.
- Figure 2 is a surface representation of a non-woven web made in accordance with prior art methods.
- % Figures 3a and 3b illustrate schematic representations of a prior art apparatus for producing spunbond fibers.
- Figure 4 is a photograph of a surface of a non-woven web manufactured without airstream perturbation.
- Figure 5 is a photograph of a surface of a non-woven web manufactured in accordance with the present invention.
- Figures 6a-6d illustrate schematic representations of apparati for producing melt-blown fibers according to the present invention.
- Figures 7a-7e illustrate schematic representations of three-way valve embodiments which may be utilized in accordance with the present invention.
- Figures 8a and 8d illustrate plenum pressure as a function of time for a prior art apparatus for producing melt-blown fibers.
- Figures 8b-8c illustrate plenum pressure as a function of time for an apparatus for producing melt-blown fibers in accordance with the present invention.
- Figure 9 illustrates fiber diameter distribution for melt-blown fibers manufactured in accordance with the prior art.
- Figure 10 illustrates fiber diameter distribution for melt-blown fibers manufactured in accordance with the present invention.
- Figure 11 illustrates Frazier porosity as a function of perturbation frequency for a melt-blown non-woven web manufactured in accordance with the present invention.
- Figure 12 illustrates hydrohead as a function of perturbation frequency for a melt-blown non-woven web manufactured in accordance with the present invention.
- Figure 13 is a photograph of the surface of a non-woven web manufactured in the absence of airstream perturbation.
- Figure 14 is a photograph of the surface of a non-woven web manufactured in accordance with the present invention.
- Figure 15 illustrates peak load as a function of perturbation frequency of a non-woven web of spunbond fibers.
- Figure 16 is a schematic representation of a coform apparatus configured in accordance with the present invention.
- Figures 17a-17d and 19 illustrate various apparatus configurations for manufacturing a non-woven web of spunbond fibers in accordance with the present invention.
- Figures 18a-18f, 20a and 20b, and 21a-21d illustrate various configurations of secondary jets for use with the present invention.
- Figures 22 and 23 are X-Ray Diffraction Scans of a prior art meltblown fiber and a fiber made in accordance with the present invention.
- Figure 24 is a DSC (Differential Scanning Calorimetry) comparing the calorimetric characteristics of a prior art meltblown fiber and a fiber made in accordance with the present invention.
- “perturbation” means a small to moderate change from the steady flow of fluid, or the like, for example up to 50% of the steady flow, and not having a discontinuous flow to one side.
- the term fluid shall mean any liquid or gaseous medium; however, in general the preferred fluid is a gas and more particularly air.
- the term resin refers to any type of liquid or material which may be liquefied to form fibers or non-woven webs, including without limitation, polymers, copolymers, thermoplastic resins, waxes and emulsions.
- the preferred embodiments of the present invention provide for a much greater range of variation in fiber characteristics and provide for a greater range of control for forming various non-woven web materials from such fibers, these techniques allow one to "tune in” the characteristics of the non-woven web formed thereby with little or no interruption of the production process.
- the U basic technique involves perturbing the air used to draw the fiber from the die.
- the airflow in which the fiber travels is alternately perturbed on opposite sides of an axis parallel to the direction of travel of the fiber.
- the airstream carrying the forming fiber is perturbed, resulting in perturbation of the fiber during formation.
- Airstream perturbation according to the methods and apparati of the present invention may be implemented in melt-blown and spunbond manufacturing, but is not limited to those processes.
- the airflow may be perturbed in a variety of ways; however, regardless of the method used to perturb the airflow, the perturbations have two basic characteristics, frequency and amplitude.
- the perturbation frequency may be defined as the number of pulses provided per unit time to either side. As is common the frequency will be described in Hertz (number of cycles per second) throughout the specification.
- the amplitude may also be described by the percentage increase or difference in air pressure ( ⁇ P/P) X 100 in the perturbed stream as compared to the steady state. Additionally, the perturbation amplitude may be described as the percentage increase or difference in the air flow rate during perturbation as compared to the steady state.
- the primary variables which may be controlled by the new fiber forming techniques are perturbation frequency and perturbation amplitude.
- a final variable which may be changed is the phase of the perturbation.
- a 180° phase differential in perturbation is described ⁇ 7- below (that is, a portion of the airflow on one side of an axis parallel to the direction of flow is perturbed and then the other side is alternately perturbed) ; however, the phase differential could be adjusted between 0° to 180° to achieve any desired result.
- Tests have been conducted with the perturbation being symmetric (in phase) and with varying phase relationships. This variation allows for still more control over the fibers made thereby and the resulting web or material.
- the perturbation of the air stream and fibers during formation has several positive effects on the fiber formed thereby.
- the particular characteristics of the fiber such as strength and crimp may be adjusted by variation of the perturbation.
- increased bulk and tensile strength may be obtained by selecting the proper perturbation frequency and amplitude.
- Increased crimp in the fiber contributes to increased bulk in the non-woven web, since crimped fibers tend to take up more space.
- preliminary investigation of the characteristics of meltblown fibers made in accordance with the present invention, as compared to those made with prior art techniques, appear to indicate that fibers made in accordance with the present invention exhibit different crystalline and heat transfer characteristics. It is believed that such differences are due to heat transfer effects (including quenching) which result from the movement of fibers in a turbulent airflow.
- the present invention does not preclude the use of conventional process control techniques to adjust the fiber characteristics.
- FIGs 4 and 5 magnified photographs of melt-blown webs made in accordance with prior art techniques (Fig. 4) and according to the present invention (Fig. 5) may be compared.
- the individual fibers of the web are relatively linear.
- the fibers in the web made in accordance with the perturbation techniques of the present invention are much more crimped and are not predominantly aligned in the same direction.
- webs made in accordance with the present invention tend to exhibit greater bulk for a given •4 weight and frequently have greater machine and cross direction strengths (the machine direction is the direction of movement, relative to the forming die, of the substrate on which the web is formed; the cross direction is perpendicular to the machine direction) . It is believed that the increase crimp will provide many more points of contact for the fibers of the web which will enhance web strength. As a note, at first glance it would appear that many more and larger voids are present in the web of Figure 5 as compared to that of Figure 4; however, in fact, the web of Figure 5 does not contain more or larger voids than that of Figure 4.
- FIGS. 6a through 6d illustrate various embodiments of the present invention which utilize alternating air pulses to perturb air flow in the vicinity of the exit of a melt-blown die 59.
- Each melt-blown embodiment of the present invention includes diametrically opposed plenum/manifolds 22 and 23 and air passages 24 and 25 which lead to a tip of the melt die 59 to create a stream of fibers in a jet stream 26.
- the function of the present invention is to maintain a steady flow and to superimpose an alternating pressure perturbation on that steady flow near the tip of melt die 59 by alternatingly increasing or reducing the pressure of the manifolds 22 and 23. This technique assures controlled modifications in the gas borne stream of fibers 26 and therefore facilitates regularity of pressure fluctuations in the gas borne stream of fibers.
- the relatively high steady state air flow with respect to perturbation air flow amplitude also serves to prevent the airborne stream of fibers from becoming tangled on air plates 40 and 42.
- the jet structure air entrainment rate (and therefore quenching rate) and fiber entanglement are thus modified favorably.
- FIGs 7a through 7d illustrate a few examples of valves that alternatingly augment the pressure in plenum chambers 22 and 23 shown in Figs. 6a-6d.
- perturbation valve 86 is essentially comprised of a bifurcation of main air line 84 into inlet air lines 20 and 21.
- a pliant flapper 98 alternatingly traverses the full or partial width of the bifurcation. This provides a means for alternatingly restricting air flow to one of air inlet lines 20 and 21 thereby superimposing a fluctuation in air pressure in manifolds 22 and 23.
- an activator may mechanically oscillate the flapper across the bifurcation to produce the appropriate fluctuation in air pressure in llf plenums 22 and 23.
- Flapper valve 98 may traverse the bifurcation of mainline 84 in an alternating manner simply by the turbulence of air in mainline 84 using the natural frequency of the flapper.
- Oscillation frequency of valve 86 as disclosed in Figure 7a may be varied mechanically by an activator which reciprocates the flapper, or by simply adjusting the length of the flapper 98 to change its natural frequency.
- Figure 7b illustrates a second embodiment of the perturbation valve 86.
- This embodiment may include a motor
- the shaft 102 may be fixed to a rotation plate 109 which has a plurality of apertures 108 disposed thereon.
- Behind rotation plate 109 is a stationary plate 104 containing a plurality of apertures 106. Both disks may be mounted so that flow is realized through fixed disk openings only when apertures from the rotation plate 109 are aligned with apertures in the stationary plate 104.
- the apertures on each plate may be arranged such that a steady flow may be periodically augmented when apertures on each plate are aligned. The frequency of the augmented flow may be controlled through a speed control of motor 100.
- Figure 7c illustrates yet another embodiment of perturbation valve 84.
- a motor 100 is rotatingly coupled to a shaft 112 which supports a butterfly valve 110 having essentially a slightly smaller cross-section than main air line 84. Turbulence created downstream from rotating butterfly 110 may then provide an alternatingly augmented air pressure in air inlet lines 20 and 21 and also in air plenums 22 and 23 to achieve the flow conditions in accordance with the present invention.
- FIG. 7d represents yet another embodiment of a perturbation valve 86 in accordance with the present invention.
- a motor 100 is coupled to a shaft 112 and butterflies 110 and 114 within inlet air lines 20 and 21 respectively.
- butterflies 110 and 114 are mounted on shaft 112 approximately 90° to each other.
- each of the butterflies 110 and 114 may include apertures 111 so as to provide a constant air flow to each of the plenums while alternatingly augmenting pressure in each of the plenums 22 and 23 when the appropriate butterfly is in an open position.
- Figure 7e represents still another embodiment of the perturbation valve 86.
- an actuator 124 is coupled to a shaft 122 which in turn is mounted to a spool 123.
- Spool 123 includes channels 118 and 120 which communicate with air inlet lines 20 and 21 respectively, depending on the longitudinal position of the spool 123.
- Each of the channels 118 and 120 is fluidly connected to main channel 116 which is fluidly connected to main air line 84.
- perturbation valve 86 may achieve alternatingly augmented air pressures in each of the plenums by reciprocation of rod 122 from actuator 124.
- channels 118 and 120 may simultaneously be connected to main air line 84 while activator 124 reciprocates spool 123 to vary an amount of overlap, and thus air flow restriction, between channels 118 and 120 with lines 20 and 21, respectively, to achieve alternating augmented pressures in 1ST the plenum chambers 22 and 23, respectively.
- Actuator 124 may include any known means for achieving such reciprocation. This may include but is not limited to pneumatic, hydraulic or solenoid means.
- Figures 8a-8d illustrate, respectively, plenum air pressures in both the prior art melt-blown apparatus and in the melt-blown apparatus according to the present invention.
- a prior art air pressure in the plenum chambers is essentially constant over time whereas in Figures 8b and 8c the air pressure in the plenum chambers is essentially augmented in an oscillatory manner.
- the point at which the mean pressure intersects the ordinate can be about 7 psig.
- Fig. 8d illustrates a prior art air pressure in the vicinity of a prior art extrusion die where air is turned on and off. In this case, the mean pressure meets the ordinate at about 0.5 psig, for example.
- the on/off control of prior art air flow as illustrated in Fig. 8d is conducive to die clogging due to the intermittent flow, as explained above. Additionally, the prior art on/off air flow control illustrated in Fig.
- Perturbation valve 86 may be placed in a multitude of arrangements to achieve the alternatingly augmented flow in plenum chambers 22 and 23 of the melt-blown apparatus according to the present invention.
- Figure 6b shows another embodiment according to the present invention.
- main air line 84 bifurcates constant air flow to inlet air lines 20 and 21 while bleeding an appropriate flow of air to perturbation valve 86 via bleeder valve 90.
- plenum chambers 23 and 22 each include two inlets.
- the first inlet introduces essentially constant flow from air inlet lines 20 and 21.
- the second inlet of each plenum chamber introduces the alternating flow to the chamber, thereby superimposing oscillatory flow on the constant flow from lines 20 and 21.
- the amount of air bled from bleeder valve 88 will control the amplitude of the pressure augmentation for precise adjustment of fiber characterization, as explained in greater detail below, while perturbation valve 86 controls frequency.
- Figure 6c represents yet another embodiment of the present invention.
- main air line 84 bifurcates into air lines 21 and 22 to supply air pressure to plenum chambers 22 and 23.
- an auxiliary air line 92 bifurcates at perturbation valve 86.
- the perturbation valve 86 then superimposes an alternatingly augmented air pressure onto plenum chambers 22 and 23 to achieve the oscillatory flow conditions in accordance with the present invention.
- pressure on the air line 92 controls the amplitude of air pressure perturbation, while perturbation valve 86 controls perturbation frequency, as explained above.
- Figure 6d represents yet another embodiment of the present invention.
- main air line 84 bifurcates into inlet air lines 20 and 21 which lead to plenum chambers 22 and 23 respectively.
- the alternatingly augmented pressure in plenum chambers 22 and 23 may be provided by transducers 94 and 96 respectively.
- Transducers 94 and 96 are actuated by means of an electrical signal.
- the transducers may actually be large speakers which receive an electrical signal to pulsate 180° out of phase in order to provide the alternating augmented pressures in plenum chambers 22 and 23.
- any type of appropriate transducer may create an augmented air flow by using any means of actuation. This may include but is not limited to electromagnetic means, hydraulic means, pneumatic means or mechanical means.
- the material is preferably made of small diameter fibers.
- larger diameter fibers may be desired for other materials.
- disposable diapers generally consist of a wicking layer designed to move moisture away from contact with the skin of an infant and to keep such moisture away.
- a middle, absorbent layer is used to retain the moisture.
- an outer, barrier layer is desired to prevent the absorbed moisture from seeping out of the diaper.
- the fiber characteristics for each layer of the diaper are different in order to achieve the specific functions of each type of material.
- various portions of the web can be formed by varying the perturbation parameters with respect to time so that each layer of the diaper is formed sequentially in one non-woven web. Then the single web may be folded to provide the layered finished material.
- Sorbent structures for oil are described, for example, in U.S. Patent No. 5,364,680 to Cotton which is incorporated herein in its entirety by reference.
- a microfiber web that is oleophilic and characterized by a bulk in terms of density of no more than about O.lg/cc, preferably no more than about 0.06g/cc.
- lower densities are preferred but densities below O.Olg/cc are difficult to handle.
- Such webs have the ability to soak up and retain oil in an amount of at least about 10 times the web weight, preferably at least about 20 times the web weight.
- Figures 9 and 10 illustrate fiber diameter distribution for samples taken from prior art melt-blown techniques and the melt-blown fiber producing technique according to the melt-blown apparatus embodiment of Figure 6c.
- Figure 9 shows a diameter distribution in accordance with the prior art.
- Figure 10 represents a fiber diameter distribution chart for melt-blown fibers made in accordance with the inventive technique.
- the fiber distribution in Figure 10 illustrates a fiber diameter sample which has a distribution that is centered on a peak between about 1 and 2 microns.
- the narrow band of fiber distribution achieved by the perturbation method and apparatus illustrates the great extent to which fiber diameter may be controlled by only varying perturbation frequency or amplitude.
- Figure 11 represents the Frazier porosity of a non-woven melt-blown web made in accordance with the present invention as a function of perturbation frequency in the plenum chambers 22 and 23.
- the Frazier Porosity is a standard measure in the non-woven web art of the rate of airflow per square foot through the material and is thus a measure of the permeability of the material (units are cubic feet per square foot per minute) .
- the procedure used to determine Frazier air permeability was conducted in accordance with the specifications of method 5450, Federal Test Methods Stand No. 191 A, except that the specimen sizes were 8 inches by 8 inches rather than 7 inches by 7 inches. The larger size made it possible to ensure that all sides of the specimen extended well beyond the retaining ring and facilitated clamping of the specimen securely and evenly across the orifice.
- the Frazier porosity generally falls first to a minimum and then increases with perturbation frequency from a steady state to approximately 500 hertz.
- the oscillation frequency and/or the amplitude
- changes in porosity often required changes to the die or starting materials or the duplication of machinery.
- the present techniques it is possible to easily change the porosity of a material once a run is completed; it is only necessary to adjust the perturbation frequency (or amplitude) , which can easily be done with simple controls and without stopping production. Therefore, the melt-blowing apparati according to the present invention may quickly and easily manufacture filtering materials of varying porosity by simply changing perturbation frequency.
- Figure 12 illustrates a plot of hydrohead as a function of perturbation frequency.
- the Hydrohead Test is a measure of the liquid barrier properties of a fabric. The hydrohead test determines the height of water (in centimeters) which the fabric will support before a predetermined amount of liquid passes through. A fabric with a higher hydrohead reading indicates it has a greater barrier to liquid penetration than a fabric with a lower hydrohead.
- the hydrohead test is performed according to Federal Test
- Polymer Copolymer of butylene and propylene polypropylene* - 79% polybutylene - 20% blue pigment - 01%
- Perturbation Frequency 0 Hz, 156 Hz, 462 Hz
- the melt-blown process was configured as described above and corresponds to the embodiment shown in FIG. 6c, in which the primary airflow is supplemented with an auxiliary airflow.
- the unit hpi characterizes the number of holes per inch present in the die.
- Pep is defined as the total pressure measured in a stagnant area of the primary manifold.
- GHM is defined as the flow rate in grams per hole per minute; thus, the GHM unit defines the amount, by weight, of polymer flowing through each hole of the melt-blown die per minute.
- Frazier Porosity is a measure of the permeability of the material (units are cubic feet per minute per square foot) .
- the hydrohead measured as the height of a column of water supported by the web prior to permeation of the water into the web, measures the liquid barrier qualities of the web.
- the web material produced is a more effective barrier.
- the Frazier Porosity has increased and the Hydrohead has decreased from both the 0 Hz (prior art) and 156 Hz production runs.
- the web material is a less effective barrier, but is more suitable for use as an absorbent or wicking material.
- Perturbation Frequency 0 Hz (control) , 70 Hz
- the use of the perturbation techniques of the 3D present invention allows for custom texture or appearance control.
- Figure 13 represents the appearance of the web produced with the 0 Hz perturbation frequency while the web of Figure 14 represents that produced using the 70 Hz perturbation frequency.
- the web of Figure 14 has a leather like appearance and texture which is not present in the web of Figure 13.
- the techniques of the present invention allow for added control and variety in production of various types of webs having such characteristics.
- meltblown webs were produced using the processing conditions shown. These materials were tested for bulk and oil capacity, and in addition, the roll samples were tested for oil absorption rate.
- Oil absorption test results were obtained using a test procedure based on ASTM D 1117-5.3.
- Four square inch samples of fabric were wieghed and submerged in a pan containing oil to be tested (white mineral oil, +30 Saybolt color, NF grade, 80-90 S.U. viscosity in the case of roll samples and 10W40 motor oil in the case of hand samples) for two minutes.
- the samples were then hung to dry (20 minutes in the case of roll samples and 1 minute in the case of hand samples) .
- the samples were weighed again, and the difference calculated as the oil capacity.
- test liquid 0.1 ml of white mineral oil is used as the test liquid.
- Gap 0.090" 30 hpi
- Perturbation Frequency 0 Hz (control), 192 Hz,
- Cup Crush is a measure of softness whereby the web is draped over the top of an open cylinder of known diameter, a rod of a diameter slightly less than the inner diameter of the cup cylinder is used to crush the web or material into the open cylinder while the force required to crush the material into the cup is measured.
- the cup crush test was used to evaluate fabric stiffness by measuring the peak load required for a 4.5 cm diameter hemispherically-shaped foot to crush a 22.9 cm by 22.9 cm piece of fabric shaped into an bb approximately 6.5 cm diameter by 6.5 centimeter tall inverted cup while the cup shaped fabric was surrounded by an approximately 6.5 cm centimeter diameter cylinder to maintain a uniform deformation of the cup shaped fabric.
- the foot and cup were aligned to avoid contact between the cup walls and the foot which could affect the peak load.
- the peak load was measured while the foot was descending at a rate of about 0.64 cm/s utilizing a Model 3108-128 10 load cell available from the MTS Systems Corporation of Cary, North Carolina. A total of seven to ten repetitions were performed for each material and then averaged to give the reported values.
- the lower cup crush number achieved by the material made using the 192 Hz perturbation frequency indicates that the material made thereby is softer. Subjective softness tests such as by hand or feel also confirm that the material made by using the 192 Hz perturbation frequency is softer than that made using the prior art techniques.
- Strength Table 3-1 Perturbation 0 Hz 192 Hz 436 Hz Freguencv MD Peak Load (lbs) 1. 989 2 . 624 2 . 581 MD Elongation (in) 0 . 145 0 . 119 0 . 087 CD Peak Load (lbs) 1 . 597 1. 322 1 . 743 CD Elongation (in) 0 . 202 0 . 212 0.
- Polymer Copolymer of butylene and propylene polypropylene* - 79% polybutylene - 20% blue pigment - 01%
- thermoplastic resins and elastomers may be utilized to create melt-blown non-woven webs in accordance with the present invention. Since it is the structure of the web of the present invention which is largely responsible for the improvements obtained, the raw materials used may be selected from a wide variety. For example, and without limiting the generality of the foregoing, thermoplastic polymers such as polyolefins including polyethylene, polypropylene as well as polystyrene may be used. Additionally, polyesters may be used including polyethylene, terepthalate and polyamides including nylons.
- While the web is not necessarily elastic, it is not intended to exclude elastic compositions. Compatible blends of any of the foregoing may also be used. In addition, additives such as processing aids, wetting agents, nucleating agents, compatibilizers, wax, fillers, and the like may be incorporated in amounts consistent with the fiber forming process used to achieve desired results. Other fiber or filament forming materials will suggest themselves to those of ordinary skill in the art. It is only essential that the composition be capable of spinning into filaments or fibers of some form that can be deposited on a forming surface. Since many of these polymers are hydrophobic, if a wettable surface is desired, known compatible surfactants may be added to the polymer as is well-known to those skilled in the art.
- Such surfactants include, by way of example and not limitation, anionic and nonionic surfactants such as sodium diakylsulfosuccinate (Aerosol OT available from American Cyanamid or Triton X-100 available from Rohm & Haas) .
- the amount of surfactant additive will depend on the desired end use as will also be apparent to those skilled in this art.
- Other additives such as pigments, fillers, stabilizers, compatibilizers and the like may also be incorporated. Further discussion of the use of such additives may be had by reference to, for example, U.S. Patent Nos. 4,374,888 issued on Bornslaeger on February 22, 1983, and 4,070,218 issued to Weber on January 24, 1978
- melt-blown non-woven webs in accordance with the present invention, a multitude of die configurations and die cross-sections may be utilized to create melt-blown non-woven webs in accordance with the present invention.
- orifice diameters 20 to 50 holes per inch (hpi) are preferred, however, virtually any appropriate orifice diameter may be utilized.
- star-shaped, elliptical, circular, square, triangular, or virtually, any other geometrical shape for the cross-section of an orifice may be utilized for melt-blown non-woven webs.
- a coform die 170 is basically a combination of two melt-blown die heads 173, 175. Air flows 176 and 178 are provided around die 172 and air flows 180 and 182 are provided around die 174. A chute 184 is provided through which pulp, staple fibers, or other material may be added to vary the characteristics of the resulting web.
- a centralized chute may be located between the two centralized air flow for introducing pulp or cellulose fibers and particulates.
- Example 5 As described above with reference to Figure 16, coform materials are essentially made in the same manner as melt ⁇ blown materials with the addition of a second die. Thus, there are two airflows around each die, for a total of four air flows, which may be perturbed as described above. Additionally, there is typically a gap between the two dies through which pulp or other material may be added to the fibers produced and incorporated into the web being formed.
- the following example utilizes such a coform-form head, but otherwise, with respect to the airflow perturbation, conforms to the previous description of the melt-blown process.
- FIGs 17a through 17d represent various embodiments which utilize alternatingly augmented air pressure in plenum chambers 58 and 62 of a standard fiber draw unit, as illustrated in Figure 3b.
- the fiber draw unit may receive alternatingly augmented air pressure into plenum chambers 62 and 58 via lines 72 and 74, respectively, through the bifurcation of main air lines 66 via perturbation valve 86.
- main air line 66 may be bifurcated by valve 86 into supply lines 130 and 128 with a third bleeder portion supplying perturbation valve 86.
- perturbation valve 86 receives bleed air from bleeder valve 88 and perturbs that air to create an oscillatory pressure which is then superimposed onto supply lines 128 and 130 to create alternatingly augmented pressure in lines 74 and 72 for supply to plenum chambers 58 and 62, respectively.
- main supply line 66 bifurcates into lines 128 and 130.
- FIG. 17d represents still another embodiment of the present invention which utilizes a perturbation valve 86 which provides an alternatingly perturbing air flow prior to the bifurcation of the main air supply line.
- Figures 18a through 18f illustrate various locations for secondary perturbation jets which may be used with a standard prior art fiber draw unit such as the one illustrated in Figure 3b to create the proper flow conditions for increasing desirable properties of fibers made in accordance with the present invention.
- Figure 18a illustrates the tail pipe 56 of a fiber draw unit which utilizes secondary perturbation jets 132 and 134.
- these secondary perturbation jets impose alternating augmented flow in a direction which is perpendicular to the main air flow through the tail pipe 56 of the present invention.
- This orthogonal relationship between primary and secondary air flow increases both the degree and order of turbulence of the air flow in the vicinity of the tail pipe 56.
- tail pipe 56 may also include alternatingly, or otherwise activated, co-flowing jets 136 and 138 create turbulent flow in accordance with the present invention near the tail pipe of the fiber draw unit.
- Figure 18c illustrates secondary perturbing jets 142 and 140 disposed near a top portion of the fiber draw unit upstream of plenum chamber inlets 60 and 64.
- Figure 18d represents yet another embodiment of the present invention that utilizes alternatingly augmented flow through Coanda nozzles 144 and 146 at an exit of tail pipe 56 to create turbulent air flow in the vicinity of tail pipe 56.
- Figure 18e illustrates Coanda-like nozzles 190 and 192 disposed at mid portion 54 of the fiber draw unit.
- Figure 18f illustrate ⁇ jets at inlet portions 48 and 50 of the fiber draw unit.
- Each of those jets illustrated in Figures 18a through 18f may alternatingly perturb air flow through the fiber draw unit in addition to any perturbation which may be implemented upstream of the jets.
- each of the jets illustrated in Figures I8a-l8f may also be implemented without additional perturbation means upstream therefrom.
- Figure 19 represents yet another embodiment of the present invention.
- the alternatingly augmented pressure in plenum chambers 147 and 150 may be provided by transducers 148 and 152 via inlets 150 and 154, respectively.
- Transducers 148 and 152 are preferably actuated by means of an electrical signal.
- the transducers may actually be large speakers which receive an electrical signal to activate 0° to 180° out of phase in order to provide the alternating augmented pressures in plenum chambers 147 and 150.
- any type of appropriate transducer may create an augmented air flow by using any means of actuation. This may include but is not limited to electromagnetic means, hydraulic means, pneumatic means or mechanical means.
- Figures 20a and 20b illustrate yet another embodiment of the present invention wherein hot and cold jets are alternatingly used to increase fiber crimp.
- fiber draw unit 69 includes secondary perturbation jets 156 and 158.
- Oscillatory jet 156 supplies hot air whereas oscillatory air jet 158 supplies cold air.
- Figure 20b illustrates perturbation air jets 164, 166, which alternatingly supply hot air to the primary air flow and fiber bundle exiting from the tail pipe of the fiber draw unit.
- Both Figures 20a and 20b illustrate the fiber bundle deflection upon application of secondary perturbation. This secondary perturbation creates fiber bundle deflection and heating or cooling effects which lead to added crimp of the fibers being distributed within a web on an endless belt.
- the temperature varied perturbation provides for additional parameters which may be varied and controlled during production.
- the jets may be symmetrically or asymmetrically oriented to achieve desired fiber characteristics, namely fiber crimp.
- the temperature of the air may be controlled without interruption of the production process, although this control is more complex.
- This technique may be applied to processes utilizing the homopolymer fibers as well as to multi-component fibers and materials.
- Figures 21(a) through 21(d) represent yet another embodiment of the present invention, wherein a standard fiber draw unit includes secondary perturbation jets at an exit of the tail pipe thereof wherein at least one bank of perturbation jets is rotated with respect to the machine direction to create a crimp or fiber movement in a cross direction with respect to travel of the belt within the fiber draw unit apparatus to increase tensile strength in the cross direction of the non-woven web.
- a standard fiber draw unit includes secondary perturbation jets at an exit of the tail pipe thereof wherein at least one bank of perturbation jets is rotated with respect to the machine direction to create a crimp or fiber movement in a cross direction with respect to travel of the belt within the fiber draw unit apparatus to increase tensile strength in the cross direction of the non-woven web.
- jet bank 162 is disposed at an angle with respect to the machine direction while jet bank 160 is essentially parallel to the machine direction.
- Figure 21(b) illustrates jet banks 202 and 200 which are both disposed at an angle with respect to the
- Figure 15 illustrates the peak load of a non ⁇ woven web sample as a function of perturbation frequency of secondary perturbation jets for the embodiment utilized in Example 6.
- machine direction strength of the non-woven web increases with increasing perturbation frequency.
- the direction of perturbation was parallel to the machine direction, as illustrated in Figure 21(d).
- the following examples show the application of the techniques of the present invention to the production of fibers and non-woven webs in the spunbond process.
- the processes and apparati are de ⁇ cribed u ⁇ ing terms and units well known in the prior art.
- the initial example describes fibers and a web formed using prior art techniques to provide a basis for comparison for fibers and webs formed using the techniques of the present invention.
- the following examples show the application of perturbing airflows to the spunbond process.
- the perturbing airflows were applied to the air stream carrying the fibers at the exit of the fiber draw unit (FDU) , which corresponds to the embodiment shown in Figure 21(d) .
- the process is equally applicable to perturbing the airflow in the FDU itself, or by application of auxiliary air, or bleeding airflow, at the manifolds prior to the FDU.
- the use of perturbing airflows in the spunbond proces ⁇ provide ⁇ ⁇ ubstantially increased MD strength (in this example, the perturbing airflows were aligned with the machine direction) .
- the CD strength remained relatively constant after a slight decrease.
- the overall strength of the web is increased by the application of the perturbing airflows.
- the processing equipment must be completely shut down and the proces ⁇ condition ⁇ changed, ⁇ uch a ⁇ by changing the die or other substantial change to the equipment.
- the present invention does not preclude those processes, with the present proce ⁇ , ⁇ uch changes to the web material may be accomplished on the fly by merely changing the perturbation frequency while the other proce ⁇ s conditions remain constant. This feature of the present invention allows for much greater flexibility and efficiency in the operation of spunbond equipment.
- Example 7 the spunbond process was adapted, using the techniques disclosed herein to provide for perturbing airflows disposed at the exit of the FDU.
- the perturbing airflows were not disposed immediately opposite each other, as was the case in Example 6, but rather one bank of auxiliary air nozzles was directed parallel to the machine direction, while the other was directed at an angle with respect to the cross direction to provide a slight cross direction trajectory (as shown schematically in Fig. 21(a)).
- Figure 24 is a graph showing the re ⁇ ults of a Differential Scanning Calorimetry (DSC) test conducted on a prior art meltblown fiber (indicated by the dashed line on the graph) and with a fiber made in accordance with the present techniques (the solid line) .
- the test basically observes the absorbance or emi ⁇ ion of heat from the sample while the sample is heated.
- the DSC scan of the prior art fiber is significantly different from that of the present fiber.
- the perturbation techniques in an atomizing embodiment provide for narrow droplet size distribution and more even distribution of the small liquid droplets in the entraining air flow.
- Thi ⁇ embodiment could be employed in many application ⁇ ⁇ uch a ⁇ creating fuel/air mixture ⁇ for engine ⁇ , improved paint ⁇ prayers, improved pesticide applicators, or in any application in which a liquid is entrained in an airflow and an even distribution of the liquid and narrow particle size distribution in the airflow is desired.
Abstract
Description
Claims
Applications Claiming Priority (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US08/510,353 US5667749A (en) | 1995-08-02 | 1995-08-02 | Method for the production of fibers and materials having enhanced characteristics |
US510354 | 1995-08-02 | ||
US510353 | 1995-08-02 | ||
US08/510,354 US5711970A (en) | 1995-08-02 | 1995-08-02 | Apparatus for the production of fibers and materials having enhanced characteristics |
US528829 | 1995-09-15 | ||
US08/528,829 US5652048A (en) | 1995-08-02 | 1995-09-15 | High bulk nonwoven sorbent |
PCT/US1996/012073 WO1997005306A1 (en) | 1995-08-02 | 1996-07-23 | Method and apparatus for the production of artificial fibers, non-woven webs and sorbency non-woven fabrics |
Publications (2)
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EP0842310A1 true EP0842310A1 (en) | 1998-05-20 |
EP0842310B1 EP0842310B1 (en) | 2008-01-02 |
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EP96926103A Expired - Lifetime EP0842310B1 (en) | 1995-08-02 | 1996-07-23 | Method and apparatus for the production of artificial fibers |
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EP (1) | EP0842310B1 (en) |
KR (1) | KR100486802B1 (en) |
CN (1) | CN1198193A (en) |
BR (1) | BR9610447B1 (en) |
CA (1) | CA2224906A1 (en) |
DE (1) | DE69637392T2 (en) |
MX (1) | MX9800839A (en) |
WO (1) | WO1997005306A1 (en) |
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EP1277867A1 (en) | 2001-07-16 | 2003-01-22 | Carl Freudenberg KG | Method and apparatus for the manufacture of spunbond webs |
US7892993B2 (en) | 2003-06-19 | 2011-02-22 | Eastman Chemical Company | Water-dispersible and multicomponent fibers from sulfopolyesters |
US8513147B2 (en) | 2003-06-19 | 2013-08-20 | Eastman Chemical Company | Nonwovens produced from multicomponent fibers |
JP4393513B2 (en) * | 2003-06-30 | 2010-01-06 | ザ プロクター アンド ギャンブル カンパニー | Fine particles in nanofiber web |
US8487156B2 (en) | 2003-06-30 | 2013-07-16 | The Procter & Gamble Company | Hygiene articles containing nanofibers |
US20040266300A1 (en) * | 2003-06-30 | 2004-12-30 | Isele Olaf Erik Alexander | Articles containing nanofibers produced from a low energy process |
US8395016B2 (en) | 2003-06-30 | 2013-03-12 | The Procter & Gamble Company | Articles containing nanofibers produced from low melt flow rate polymers |
CN1846023A (en) | 2003-07-25 | 2006-10-11 | 田纳西大学研究基金会 | Process and apparatus for collection of continuous fibers as a uniform batt |
JP2007533873A (en) | 2004-04-19 | 2007-11-22 | ザ プロクター アンド ギャンブル カンパニー | Articles containing nanofibers for use as barriers |
EP2463427A1 (en) | 2004-04-19 | 2012-06-13 | The Procter & Gamble Company | Fibers, nonwovens and articles containing nanofibers produced from broad molecular weight distribution polymers |
ES2287619T3 (en) * | 2004-09-17 | 2007-12-16 | REIFENHAUSER GMBH & CO. KG MASCHINENFABRIK | DEVICE FOR THE MANUFACTURE OF THERMOPLASTIC MATERIAL FILAMENTS. |
DE102006014236A1 (en) | 2006-03-28 | 2007-10-04 | Irema-Filter Gmbh | Fleece material used as a pleated air filter in a motor vehicle comprises thinner fibers homogeneously incorporated into thicker fibers |
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US9273417B2 (en) | 2010-10-21 | 2016-03-01 | Eastman Chemical Company | Wet-Laid process to produce a bound nonwoven article |
DE102010052155A1 (en) | 2010-11-22 | 2012-05-24 | Irema-Filter Gmbh | Air filter medium with two mechanisms of action |
CN102051766B (en) * | 2011-01-18 | 2012-08-15 | 厦门建霖工业有限公司 | Preparation method of completely degradable biological polymer melt-blown cotton |
US8906200B2 (en) | 2012-01-31 | 2014-12-09 | Eastman Chemical Company | Processes to produce short cut microfibers |
KR101326506B1 (en) * | 2012-04-30 | 2013-11-08 | 현대자동차주식회사 | Manufacturing method of melt-blown fabric web having random and bulky caricteristics and manufacuring apparatus thereof |
US9303357B2 (en) | 2013-04-19 | 2016-04-05 | Eastman Chemical Company | Paper and nonwoven articles comprising synthetic microfiber binders |
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US9605126B2 (en) | 2013-12-17 | 2017-03-28 | Eastman Chemical Company | Ultrafiltration process for the recovery of concentrated sulfopolyester dispersion |
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CN113039315A (en) * | 2018-09-18 | 2021-06-25 | 埃克森美孚化学专利公司 | Bicomponent fibers and nonwovens produced therefrom |
CN111485327A (en) * | 2020-04-22 | 2020-08-04 | 四川中旺科技有限公司 | Melt-blown fabric manufacturing device and method |
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CN114075700B (en) * | 2020-08-19 | 2022-11-29 | 中国科学院宁波材料技术与工程研究所 | Chain type premodulation melt-blowing method, chain type premodulation melt-blowing nozzle and melt-blowing device |
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- 1996-07-23 BR BRPI9610447-3A patent/BR9610447B1/en not_active IP Right Cessation
- 1996-07-23 CN CN96197267A patent/CN1198193A/en active Pending
- 1996-07-23 EP EP96926103A patent/EP0842310B1/en not_active Expired - Lifetime
- 1996-07-23 KR KR1019980700735A patent/KR100486802B1/en not_active IP Right Cessation
- 1996-07-23 DE DE69637392T patent/DE69637392T2/en not_active Expired - Lifetime
- 1996-07-23 MX MX9800839A patent/MX9800839A/en unknown
- 1996-07-23 CA CA002224906A patent/CA2224906A1/en not_active Abandoned
- 1996-07-23 WO PCT/US1996/012073 patent/WO1997005306A1/en active IP Right Grant
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BR9610447B1 (en) | 2010-08-10 |
AU698075B2 (en) | 1998-10-22 |
KR19990036070A (en) | 1999-05-25 |
WO1997005306A1 (en) | 1997-02-13 |
DE69637392D1 (en) | 2008-02-14 |
EP0842310B1 (en) | 2008-01-02 |
AU6648896A (en) | 1997-02-26 |
MX9800839A (en) | 1998-04-30 |
CN1198193A (en) | 1998-11-04 |
CA2224906A1 (en) | 1997-02-13 |
DE69637392T2 (en) | 2008-05-08 |
KR100486802B1 (en) | 2006-01-27 |
BR9610447A (en) | 1999-06-08 |
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