US3885014A - Production of fine fiber mass - Google Patents

Production of fine fiber mass Download PDF

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US3885014A
US3885014A US257419A US25741972A US3885014A US 3885014 A US3885014 A US 3885014A US 257419 A US257419 A US 257419A US 25741972 A US25741972 A US 25741972A US 3885014 A US3885014 A US 3885014A
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water
pressure
mass
polymer
molten polymer
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Tadayuki Fukada
Isao Fujita
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Yupo Corp
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Yupo Corp
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H5/00—Special paper or cardboard not otherwise provided for
    • D21H5/12—Special paper or cardboard not otherwise provided for characterised by the use of special fibrous materials
    • D21H5/20—Special paper or cardboard not otherwise provided for characterised by the use of special fibrous materials of organic non-cellulosic fibres too short for spinning, with or without cellulose fibres
    • 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
    • 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
    • D01D5/11—Flash-spinning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/05—Filamentary, e.g. strands

Definitions

  • This invention relates generally to fine fibrous structures and to synthetic paper-like structures. More particularly, the invention relates to a process for producing fine fiber masses for providing fine fibers suitable for making synthetic papers.
  • One kind of synthetic paper has a structure comprising fibers in intertwined state. That is. is formed by the ordinary paper-making process through the use of fibers of one or more synthetic polymers as a part of or in place of a paper-making material of natural cellulose fibers.
  • a synthetic paper of this character is desirable in that its structure is substantially the same as that of conventional paper.
  • fibers for synthetic papers are required to have a high degree of molecular orientation, to be thin, and to have a highly fibrillated structure, and difficulties are encountered in adapting synthetic polymeric fibers of the type which have been generally used for fabrics and clothing to fulfil these requirements.
  • synthetic polymeric fibers of this character are deficient in hydrophilic properties. For these reasons, satisfactory synthetic papers of this class have not been available.
  • a process for producing fine fiber masses which is characterized by the steps of dispersing water into a molten linear polymer within a highpressure region and extruding the water-dispersed, molten linear polymer thus obtained together with supplementary water into a low-pressure region.
  • FIG. 1 is a flowsheet showing the essential organization of apparatus for carrying out one example of the process according to this invention
  • FIG. 2 is a flowsheet showing apparatus for carrying out another example of the process according to this invention.
  • FIGS. 3, 4, and 5 are longitudinal sections respec- 5 tively showing examples of extrusion suitable for the practice of this invention.
  • a starting material polymer is first melted under hightemperature and high-pressure conditions and kneaded in the presence of water. and water is dispersed uniformly and finely in the molten polymer, it being the ordinary method to effect this dispersion by kneading a molten-polymer and water system.
  • the water which has been thus dispersed beforehand within the polymer abruptly expands in volume and exhibits foaming and cooling effects, when the molten polymer is extruded into a low-pressure region.
  • a surface-active agent surfactant
  • a water-sorption agent a surface-active agent (surfactant) and a water-sorption agent
  • a synthetic paper made from these fine fibers has high rigidity and, correspondingly, a stiffness comparable to that of cellulosic papers.
  • linear polymers examples include polyolefin resins, polychloroethylene resins, polyvinyl aromatic resins, polyamide resins, polyester resins, polyimide resins, and polycarbonate resins. used singly or as copolymers. Of these polymers, the most representative are polyolefin resins, among which isotactic polypropylene, high-density polyethylene resinous ethylenepropylene copolymers are the most representative. These linear polymers can be used singly or as mixtures thereof.
  • the linear polymer may contain a pigment, a filler, a blowing agent, a bridging agent. a stabilizer. and other additions ordinarily used in polymers.
  • Water-sorption agent In order to promote the dispersion of water into the molten polymer, the use of a substance which is watersoluble or has a property ranging from waterabsorptivity to water-adsorptivity (herein called a water-sorption agent) is desirable.
  • This water-sorption agent may be mixed beforehand within the polymer, or it can be mixed by introducing it under pressure together with water.
  • the water-sorption agent may be a substance which contains water of crystallization and is capable, itself, of introducing water into the molten polymer, or it may be a substance which, although having water-sorptivity, does not contain water of crystallization and is capable of functioning as a so-called filler.
  • water-sorption agents having water of crystallization which can be used in this invention are organic and inorganic salts such as Na SO .7I-I O, Na B,O .lI-I O, CaC- O 1l-I O, and CaC I-I O .4H O.
  • organic and inorganic salts such as Na SO .7I-I O, Na B,O .lI-I O, CaC- O 1l-I O, and CaC I-I O .4H O.
  • a hydrated salt of a decomposition temperature above the melting temperature of the polymer such as Na B O .lOH O, is particularly suitable.
  • substances which are simply water sorptive are: ordinary hygroscopic, porous fillers such as titanium oxide, barium sulfate, clays, calcium carbonate, silica, and diatomaceous earth; water-soluble and water-absorbing inorganic salts such as Na CO NaHCO (NH CO NH,HCO BaCO CaSO Na SO MgSO Mg(OI-I) Al(OI-I) and Ca(OH) and watersoluble high-polymer substance such as polyvinyl alcohols, polyacrylic acid and salts thereof, polyacrylamide, 4
  • polyethylene glycol and polyethyleneimine.
  • water-sorption agents can be used in combinations. While these agents may be blended with the polymer in a concentration up to approximately 60 percent, we have found that a preferred concentration is ordinarily in the range of from 10 to 30 percent. It desirable that the water-sorption agent exist within the polymer in a uniformly and finely dispersed state. In general, the effectiveness of the water-sorption agent increases with decreasing particle diameter thereof.
  • a surface-active agent is added to the polymer and/or water in order to promote the introduction and dispersion of water into the molten polymer and to promote the wettability of the molten polymer with the supplementary water, which is introduced under pressure immediately prior to extrusion into a low-pressure region, thereby to derive maximum stretching effect due to the supplementary water introduced under pressure.
  • any non-ionic. anionic, cationic, amphoteric (ampho-ionic), or zwitter ionic surfactant can be used singly or as a mixture provided that it is stable under the high-temperature, high-pressure conditions of this invention.
  • the surfactant is added to the polymer in a quantity of more that 0.1 percent by weight of the polymer, a quantity less than 1.0 percent being ordinarily sufficient for deriving satisfactory effect of the surfactant.
  • auxiliary materials may be used in the process of this invention provided that they have no detrimental effect on the results and do not constitute a departure from the spirit and support of the invention.
  • auxiliary materials are'the auxiliary material mentioned previously with respect to the polymer and materials for adjusting values such as the pH value of the water, specific gravity, and viscosity when necessary.
  • Dispersion of water into the molten polymer 2.1. Dispersion water It is desirable that the water dispersed in the polymer exist as a liquid within the polymer. One reason for this is that, in the case where the water is in liquid form, it occupies a relatively small volumetric proportion within the polymer, and kneading and dispersing can be carried out with greater facility than in the case where the water is in vaporous form. Another important reason for this is that, when the water is in liquid form, the expansion force during extrusion into a low-pressure region is incomparably greater.
  • the water which has been uniformly and finely dispersed in the form of independent cells within the polymer undergoes instantaneous expansion and evaporation upon being abruptly released from high pressure at the time of extrusion and, rupturing the water cell walls, is jetted further in the extrusion direction thereby to stretch the polymer with great force and cause it to split into fine fibers.
  • the kneading process step can be carried out by any appropriate method, examples of which are: (1) the method which comprises mixing at one time the polymer, water, surfactant and/or water-sorption agent and kneading the resulting mixture for a specific time under specific conditions of temperature and pressure; (2) the method wherein the polymer (and water-sorption agent and/or surfactant) are caused to assume a molten state, and then water (and surfactant) are introduced under pressure into the molten mixture to form a mixture which is then kneaded; and (3) the method wherein water (and surfactant and/or awater-sorption agent which dissolves with difficulty) are introduced under pressure into the polymer (and surfactant) in molten state, and the resulting mixture is kneaded.
  • a desirable method includes the step of introducing water underpressure into the polymer in the molten state.
  • an apparatus such as an extruder used for admixing an auxiliary material for polymers such as an antistatic agent or a stabilizer into a molten polymer.
  • a continuous Banbury mixer, or a kneader can be used in this case, we believe that the simplest and most practical procedure is to carry out kneading by means of an extruder as water at a high temperature and high pressure is introduced directly into the extruder, and amply high pressure therewithin is maintained.
  • the water temperature be above the temperature of the polymer in a molten state.
  • the kneading time is prolonged after the water has been introduced into the kneading system, this problem will not arise.
  • the pressure at the time of kneading should be higher than the saturated steam pressure of water at that temperature.
  • the higher the pressure under which the water is introduced is, the deeper will the water infiltrate into the interior of the molten polymer, and the easier will the dispersion due to kneading become. Accordingly, a high water introduction pressure is preferable.
  • the water be dispersed in the form of minute cells with ample fineness and uniformity within the molten polymer.
  • dispersed water particles are spherical particles of equal diameter and have been introduced with maximum density in a polymer.
  • a limiting concentration of the dispersed water of 74 percent is sought, and the dispersed water particles have amply small diameter and thin cell walls, it may be presumed that uniform and fine fibrillation is accomplished by the 6 blowing and stretching force of the dispersed water itself.
  • supplementary water is forcibly introduced into the polymer immediately prior to its extrusion into a low-pressure region, and the stretching effect of the supplementary water is utilized to further facilitate splitting of the polymer into fine fibers and thereby to produce highly orientated fine fibers.
  • the water can no longer maintain its dispersed state in the form of independent fine-cells, and, in addition to the dispersed state of fine cells, mutually communicative continuous phases are formed in one part. At the same time, the cell diameter or distance between the continuous phases decreases. Accordingly, similarly as in the case of dispersion of water in the. form of independent cells as described before, by introducing the supplementary water and utilizing the stretching effect of this supplementary water, the objective highly orientated fine fibers can be obtained.
  • the quantity of water dispersed in the polymer prior to the forcible introduction of the supplementary water according to this invention is over 2 percent, preferably from 25 to 50 percent. When this quantity is less than 2 percent, the resulting foaming power is deficient. While it is possible in this case to achieve fine fibrillation of the polymer by adding a large quantity of the supplementary water and utilizing its jetting power, the resulting fine fibers will be hard and non-uniform, whereby they will require additional after-treatment for application to making of synthetic paper.
  • composition for extrusion into a low-pressure region 3.1.
  • Supplementary water In order to produce a mass of fine fibers of high rigidity by extruding into a low-pressure region a molten polymer obtained in this manner wherein water is finely dispersed, supplementary water should be caused to exist in addition to this dispersed water, as mentioned hereinbefore. This supplementary water assists and facilitates the discharge of the water-dispersed polymer into the low-pressure region and, moreover, as described hereinbefore, is jetted vigorously in the extrusion direction by the abrupt release of pressure occurring when the polymer is extruded into the lowpressure region.
  • This action of the supplementary water imparts a high degreeof stretching and orientation to the polymer containing finely dispersed water and traveling in the sameextrusion direction, whereby the polymer is split into fine fibers by the combined foaming and stretching force of the dispersed water.
  • the blowing action of the water dispersed in the molten polymer and the stretching and orientation actions due to the supplementary water occur almost simultaneously to render the polymer into fine fibers.
  • the quantity of the supplementary water is determined by the balance of its effect with the blowing action of the water (dispersed water) dispersed in the molten polymer. More specifically, in the case where the quantity of the dispersed water is small, and the blowing action is weak, a relatively large quantity of the supplementary water is required. On the other hand. when the blowing action is sufficiently powerful. a relatively small quantity suffices.
  • blowing action of the dispersed water is influenced also by the conditions of temperature and pressure in the high-pressure region relative to those of the low-pressure region. That is, the higher the temperature and pressure are, the better are the results.
  • the supplementary water does not exhibit a splitting effect due to the rupturing of the cell walls from the interior as in the case of the dispersed water, and the polymer splitting effect due to stretching and orientating from the inside is predominant.
  • the contribution of the supplementary water to splitting of the polymer is somewhat less than that of polyolefin such as polypropylene is used for the polymer, the quantity of the dispersed water on the basis of the water-dispersed polymer is from 40 to 50 percent,
  • the quantity of the supplementary water is from 1 to or more times the quantity of the water-dispersed polymer.
  • the supplementary water is added at a high temperature and under a high pressure similar to those of the dispersed water.
  • the supplementary water can be introduced by adding water after the required quantity of the dispersed water has been introduced in the aforedescribed kneading step, the most desirable method is to forcibly introduce the supplementary water under pressure into the interior of the orifice of the device for extrusion in the low-pressure region or into the polymer flowpath immediately upstream from the orifice.
  • the reason for this is that, when the supplementary water is introduced too early, the uniformly and finely dispersed state of the dispersed water within the molten polymer,
  • the area of contact between the supplementary water and the water-dispersed polymer should be made as large as possible, and this can be accomplished by appropriately designing the construction of the extruder part where the supplementary water is to be introduced.
  • this supplementary water also contain a surfactant. Furthermore. as mentioned before. the supplementary water should be introduced at an amply high temperature.
  • FIGS. 3, 4. and 5 are representative examples of construction of the above mentioned part for introducing the supplementary water.
  • FIG. 3 shows an example of a nozzle for an inner feed method wherein, within an extrusion orifice 113, supplementary water is introduced through an inner member or torpedo 213 into the inner part of a water-dispersed polymer, and the aforementioned stretching is imparted to the polymer from its inner part.
  • FIG. 4 shows an example of a nozzle for an outer feed method wherein the supplementary water is introduced along the inner surface of the extrusion die wall, and the polymer is stretched from the outside.
  • the outer structure or die wall of the orifice 113A is substantially the same as that of the orifice 113 in FIG. 3, the orifices 113 and 113A differing only in their inter structure 213 and 213A, respectively.
  • the area of contact between the supplementary water and the water-dispersed polymer is greater in the orifice 113A shown in FIG. 4 than that in the orifice 113 shown in FIG. 3, and, consequently, the stretching effect is greater. Furthermore, by the outer feed method, the supplementary water flows along the inner surface of the extrusion die wall, whereby the frictional drag or resistance to flow becomes extremely low, and this method is thereby inferior in maintaining internal pressure of the die. However, the low die resistance makes possible high-velocity, high-flowrate extrusion.
  • the area of contact between the supplementary water and the water-dispersed polymer can be further increased thereby to further promote the effect of rendering the polymer into fine fibers by the use of extrusion orifices of various constructions, a representative example of which is illustrated in FIG. 5.
  • the dispersion water must be dispersed in liquid form in the molten polymer under high-temperature and high-pressure conditions in order to achieve maximum utilization of the blowing action of water.
  • the flowpath interval from the aforedescribed kneading means to the outlet opening of the orifice should be maintained at a pressure above the saturated steam pressure of water at the temperature of the flowpath. If the pressure maintenance is unsuitable and a pressure decrease to a value below the saturated steam pressure occurs, the water will immediately ex pand and evaporate, thereby cooling the polymer. Consequently, the viscosity of the molten polymer rises, and the resistance at the time of foaming and rendering of the polymer into fine fibers in the low-pressure region increases,
  • the lowering of the blowing action in the low-pressure region due to a lowering of the water temperature and pressure and a secondary aggregation of the dispersed water due to the water expansion give rise to a separation of the water and the molten polymer.
  • the polymer is not sufficiently disintegrated, whereby not only is the objective fine fiber mass unobtainable, but in extreme cases, the molten polymer is cooled to solidification and thereby gives rise to trouble such as clogging of the orifice.
  • the low-pressure region is ordinarily at room temperature and atmospheric pressure, it is also possible use increased temperature and reduced pressure conditions in the low-pressure region in order to promote the expansion and jetting of the water.
  • an orifice having one or a plurality of ejection outer openings of any suitable shape such as round or slit-shaped may be used. While the extrusion velocity from the ejection opening is preferably above the velocity of sound (330 meters/second), a velocity equal one half the velocity of sound or a lower velocity may be used.
  • the resulting fine fiber mass is obtained as an aggregate of separate short fibers and can be readily fed, as it is, directly into a macerator or disintegrator. Furthermore, this fine fiber mass resulting from the above stated condition can be used, in its state as produced, as fine fiber starting material for paper making.
  • the fiber mass cannot be obtained as separate short fibers, since the individual constituent fibers are highly oriented, they can be readily macerated by a machine such as a refiner or heater generally used in the papermaking industry, whereby the fine fibers of high orientation and rigidity are obtained.
  • the maceration conditions become even more advantageous in the case where a blend of two or more polymers is used as the process polymer.
  • Particularly fine fibers produced by the use of blends of polymers having adhesive power for example, polyvinyl alcohol, polyacrylic acid and salts thereof, polyamide acrylate, polyethylene oxide, and polyethylene amine) exhibit high effectiveness in forming the paper film during paper making.
  • the fine fibers of the product are highly hydrophilic. These fine fibers have a shape similar to that of wood pulps and can be supplied as they are to a papermaking machine. Moreover. the wetpaper strength after forming of the paper film with these fibers is of the same order as that of natural paper.
  • the fine fibers produced in accordance with this invention can also be used in mixed state with wood pulp fibers to make paper and, in addition to their use as starting.
  • material for synthetic papers can be used for a wide range of products from unwoven fabrics to disposable sheets and sheet products.
  • Flowsheet One example of embodiment of this invention is indicated by the flowsheet shown in FIG. 1. In the method indicated therein, the polymer melting section and the water-injection and kneading section are separately provided.
  • FIG. 2 In another example of embodiment of this invention as indicated in FIG. 2, the melting of the polymer, injection of water, and kneading and dispersion of water are carried out in a single extruder.
  • the parts in FIGS. 1 and 2 designated by thesame reference numerals are the same or are equivalent except that the reference numerals in FIG. 2 have the letter A appended thereto.
  • the starting material polymer is continuously melted by an extruder l and continuously supplied into a kneading and water-dispersion region.
  • Water stored in a water 1 1 reservoir 2 is amply heated by a heat exchanger 4 and supplied continuously by a pump 3 for constant-rate injection at high pressure into the kneading and waterdispersion region.
  • the pressure of the polymer is indicated by a pressure gauge mounted on the extruder.
  • the water pressure is maintained at a constant value as a constant flowrate is maintained by a pressure-control valve 5.
  • the polymer in molten state and water at high temperature and high pressure are supplied into a kneading region (i.e., the extruder in this example), where the polymer is continuously and thoroughly kneaded under a high pressure and high shearing action by means of a continuous kneader 6, whereby the water is dispersed in the molten polymer to form a polymer finely dispersed water body.
  • a kneading region i.e., the extruder in this example
  • This polymer dispersed Water body is transferred by way of a transfer zone 14 to a high-pressure metering pump 8, by which it is further transferred to an extrusion orifice 13.
  • the pressure in the kneading region is measured and indicated by a pressure gauge 15. This pressure is maintained above a predetermined value by controlling the feed ratesof the extruder l and the high-pressure injection pump 3 and controlling the transfer rate in the high-pressure metering pump 8 of the transfer zone.
  • the polymer-finely dispersed water body and the' water injected at the transfer zone are both continuously sent to the orifice 13 and, through this orifice of specific dimension, are continuously ejected at very high speed and high pressure into a region at atmospheric pressure. Consequently, the molten polymer is finely splintered and cooled by the abrupt expansion and evaporation of the water and is thereby rendered into a mass of uniform fine fibers of high rigidity.
  • the pressures in the flowpath upstream from the orifice l3 and in the transfer zone are sensed by pressure gauges 17 and 18 and are maintained above respective standard values by controlling the rate of transfer of the high-pressure metering pump.
  • Temperature control of the entire system is accomplished automatically by automatic temperature regulators installed at suitable positions therein. Furthermore, the temperature of the water is maintained constant by heat exchangers of specific capacities. By thus maintaining pressures at standard values above predetermined pressures and, at the same time, maintaining the temperatures at respective constant values as the molten polymer is extruded through the orifice, uniform fine fibers can be continuously produced.
  • EXAMPLE 1 To an isotactic polypropylene powder of a melt index (M1) of 20, an 80-percent aqueous solution of sodium 12 oleate in a quantity of 2 percent with respect to the polymer and 10 percent of calcium carbonate were added, and the resulting batch was mixed by means of a mixer into a uniform mixture.
  • M1 melt index
  • This mixture was continuously melted at 210C in a SO-mm. diameter bent type extruder of an L/D ratio of 29 and extruded under kg./cm at a rate of 20 kg./hour.
  • water with 2 percent of sodium oleate prepared separately and added thereto was sent by a high-pressure metering pump through a heat exchanger. and a pressure of 50 kg./cm was maintained by a pressure regulating valve thereby to prepare pressurized water heated to 210C.
  • This pressurized and heated water was introduced through the bent hole of the extruder and kneaded with the polymer under high shearing force with an inner pressure of the extruder of 80 kg/cm'
  • the resulting polymer containing dispersed water was then transferred by a gear pump to an orifice.
  • Water containing 2 percent of an anionic surfactant prepared in a separate reservoir was sent by another high-pressure metering pump at a heat exchanger.
  • the pressure of this water was adjusted to 80 kg./cm by means of a pressure-regulating valve, and the temperature thereof was raised to 210C.
  • the resulting water was injected through an intermediate part of the orifice, and, together with the above described polymer extruded by the gear pump, was extruded into the atmosphere through an orifice of 2-mm. diameter and an L/D ratio of 30.
  • the temperature of the system was maintained constant at 210C by temperature regulators installed at all regions. Furthermore, by varying the quantity of Water injected into extruder and varying the extrusion flowrate of the gear pump and the quantity of the water injected into the orifice, the pressure at which extrusion was carried out through the orifice was adjusted. Thus, by injecting water at a rate of 10 liters/hour into the extruder and at a rate of 100 liters/hour into the orifice part, extrution was carried out at a pressure of 100 kg./cm
  • the fine fibers thus produced was recovered as a mass of highly fibrillated fine fibers.
  • This fine fiber mass was disintegrated by means of a 12-inch singledisk refiner and under the conditions of a concentration-of 10 percent and a clearance of 5/1 ,000 inch.
  • stiff fine fibers having a flat shape similar to that of pulp of an average diameter of 20 microns and a length of from 3 to 4 mm. were obtained.
  • EXAMPLE 2 A mixture of 44 parts of an isotatic polypropylene of a Ml of 20, 24 parts of a high-density polyethylene of a M1 of 20, 10 parts of calcium carbonate, 20 parts of aluminum hydroxide, and 2 parts of polyvinyl alcohol was mixed in a mixer to form a uniform mixture. This mixture was continuously melted at 250C in a -mm. diameter extruder (L/D 29) having an end dalmage and extruded with an tip pressure of 400 kg./cm at a rate of kg./hour.
  • L/D 29 diameter extruder
  • the tip pressure of the extruder dropped to from 150 to 200 kg/cm because of the kneading and dispersion of water.
  • the polymer in which water had been finely dispersed by the kneading was sent to'an orifice connected directly to the downstream end of the extruder and was thus extruded through the orifice.
  • Pressurized water at 250C and 200 kg/cm prepared separately was introduced as supplementary water at a flowrate of 130 liters/hour into a point upstream from the orifice and, together with the above described polymer with finely dispersed water, was extruded through a 2-mm. diameter, L/D 50 orifice into a region at atmospheric pressure.
  • EXAMPLE 3 To 60 parts of an isotatic polypropylene of a MI of 9, 30 parts of a high-density polyethylene of a MI 8, 2 parts of an anionic surfactant, 8 parts of calcium carbonate, and 5 parts of gypsum were added, and the resulting batch was mixed in a mixer to prepare a uniform mixture, which was then melted at 230C in a 50-mm. diameter bent extruder and continuously extruder under a pressure of 100 kg/cm and at a rate of 40 kg./hour.
  • water at 80 kg./cm and 210C containing 2 percent of an anionic surfactant and prepared separately was injected through the bent hole at 30 liters/hour and kneaded with the above described polymer.
  • the resulting preparation was injected by means of a gear pump at a pressure of 130 kg.'/cm through an orifice of 2-mm. diameter and an L/D ratio of 40 into a region at atmospheric pressure, whereupon a mixture of a mass of fine fibers of a highly advanced degree of fibrillation and foamed structures contained at scattered positions therein was obtained.
  • water at 210C containing 2 percent of a monionic surfactant prepared separately was injected into an upstream part of the orifice under a pressure of 130 kg./cm and at a supply rate of 80 liters/hour.
  • This water and the polymer were injected together into a region at atmospheric pressure, whereupon it was possible to produce continuously fine fibers similar to those produced in Example 1.
  • the mixture thus prepared was melted and kneaded in a two-stage extruder having a kneading section of end dalmage type, at 200C in the first stage and at 230C in the second stage.
  • the mixture thus kneaded was sent under 80 kg./cm and at 20 kg./hour to a gear pump, by which the mixture was pressurized further to 150 kg./cm and injected through an orifice into a region at atmospheric pressure.
  • EXAMPLE 5 (reference example) The fine fibers produced in accordance with Example l were dispersed in water to a concentrationof 0.3 percent. These fine fibers were found to'be extremely hydrophilic and to exhibit good dispersion even in their as-prepared state, but 0.01 percent of a surfactant was further added to prepare a fine fiber dispersion liquid, which was used to make paper in a small continuous papermaking machine of a film forming speed of 3 meters/minute. As a result, a synthetic paper of a weight per area of 40 grams/square meter, a thickness of microns, and a bulk density of 0.45 and of good texture was obtained.
  • EXAMPLE 6 60 parts of a polypropylene of a Ml of 9, 30 parts of a highdensity polyethylene of a MI of 8, 5 parts of a clay, 5 parts of calcium carbonate, and 10 parts ofa 30- percent aqueous solution of sodium stearate were mixed thoroughly in a mixer to form a uniform mixture.
  • This mixture was passed through the two-stage extruder used in Example 4 and was melted and kneaded at 230C.
  • the molten mixture thus kneaded was extruded under a pressure of kg./cm and at a rate of 20 kg./hour through a circular orific of 2-mm. diameter.
  • pressurized water prepared separately to contain a small quantity of an active agent and be under a pressure of 100 kg./cm and at a temperature of 230C was introduced into the polymer at an upstream part of the orifice at a rate of 200 liters/hour similarly as in Example 1. This water and the polymer were injected into a region at atmospheric pressure.
  • EXAMPLE 7 (reference example) The fine fibers obtained in Example 6 was dispersed uniformly in water to a fiber concentration of 0.3 percent together with a binder of acrylic emulsion type in a quantity by weight of 5 percent with respect to these fine fibers. The resulting dispersion was then used to make paper in a small papermaking machine operating with a film-forming speed of 3 meters/minute, whereupon a synthetic paper of a weight per area of 45 grams/square meter and a thickness of 100 microns and of a uniform texture was obtained.
  • This synthetic paper had a breaking length of from 2 to 2.5 km., having a strength comparable to that of natural pulp paper, and had ample value as a paper. It was found, moreover, that even after being made into a paper, these fibers could be readily disintegrated into their original form as fine fibers by means of a machine such as a pulper or mixer and, in fact, could be treated in exactly the same manner as wood pulp.
  • a process of producing a mass of fine fibers which comprises:
  • step (3) transferring the resultant molten polymer mass under an elevated temperature and pressure to an orifice with an introduction of supplementary water under an elevated temperature and pressure in a quantity of at least 100 percent by weight of said molten polymer mass produced from step (2) at a part immediately before or just at the orifice; and then i 4. extruding the mixture of water and molten polymer mass obtained from the step (3) into a region of lower pressure so as to evaporate the water dismers and mutual copolymers of ethylene, propylene, and butene-l, copolymers of ethylene, propylene and butene-l as predominant constitutents with monomers copolymerizable therewith, and mixtures of said polymers.
  • a process for producing a mass of fine fibers as claimed in claim 1 in which a fine water-insoluble solid water-sorption agent is added to the molten linear polyolefin polymer, said water-insoluble solid comprising a silicate.
  • a process according to claim 1 wherein the pressure used during the kneading process is above kg/cm 10.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Inorganic Fibers (AREA)
  • Photoreceptors In Electrophotography (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Paper (AREA)
US257419A 1971-06-01 1972-05-26 Production of fine fiber mass Expired - Lifetime US3885014A (en)

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CA (1) CA1027322A (sv)
ES (1) ES403712A1 (sv)
FR (1) FR2141139A5 (sv)
GB (1) GB1379672A (sv)
IT (1) IT958078B (sv)
NL (1) NL7207416A (sv)
NO (1) NO136983C (sv)
SE (1) SE381696B (sv)
SU (1) SU471735A3 (sv)

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3976631A (en) * 1973-04-18 1976-08-24 Stamicarbon B.V. Process for preparing ethylene polymers
US3987139A (en) * 1972-03-20 1976-10-19 Crown Zellerbach Corporation Process of forming synthetic fibers
US4007247A (en) * 1972-09-26 1977-02-08 Imperial Chemical Industries Limited Production of fibrils
US4010229A (en) * 1974-01-18 1977-03-01 Solvay & Cie Process for the manufacture of short fibrils
US4025593A (en) * 1971-08-06 1977-05-24 Solvay & Cie Fabrication of discontinuous fibrils
US4073850A (en) * 1974-12-09 1978-02-14 Rothmans Of Pall Mall Canada Limited Method of producing polymeric material
US4081226A (en) * 1974-01-18 1978-03-28 Solvay & Cie. Process for the manufacture of short fibrils and devices for carrying it out
US4127623A (en) * 1974-08-03 1978-11-28 Sumitomo Chemical Company, Limited Process for producing polyolefin short fibers
US4129629A (en) * 1974-11-28 1978-12-12 Hoechst Aktiengesellschaft Process for making hydrophilic polyolefin fibers containing clay
US4167548A (en) * 1973-11-08 1979-09-11 Societa' Italiana Resine S.I.R. S.P.A. Process for the manufacture of a microfibrous pulp suitable for making synthetic paper
US4189455A (en) * 1971-08-06 1980-02-19 Solvay & Cie. Process for the manufacture of discontinuous fibrils
US4192838A (en) * 1976-10-06 1980-03-11 Celanese Corporation Process for producing filter material
US4211737A (en) * 1974-11-19 1980-07-08 Montedison S.P.A. Process for producing synthetic fibers for use in paper-making
US4301105A (en) * 1980-04-21 1981-11-17 American Cyanamid Company Process for spinning poly(polymethylene terephthalamide) fiber
EP0176350A2 (en) * 1984-09-25 1986-04-02 Mitsui Petrochemical Industries, Ltd. Process for preparation of synthetic fibers
US4600545A (en) * 1972-02-25 1986-07-15 Montecatini Edison S.P.A. Process for the preparation of fibers from polymeric materials
US5650221A (en) * 1995-07-06 1997-07-22 Laroche Industries, Inc. High strength, low pressure drop sensible and latent heat exchange wheel
US5685897A (en) * 1995-07-06 1997-11-11 Laroche Industries, Inc. High strength, low pressure drop adsorbent wheel
US20050109856A1 (en) * 2003-11-25 2005-05-26 Alexander James N.Iv Method for preparing polymer electrosprays
US20080003435A1 (en) * 2006-06-29 2008-01-03 The Procter & Gamble Company Faux fibers and fibrous structures employing same
US20100127434A1 (en) * 2008-11-25 2010-05-27 Rene Broos Extruding organic polymers

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1556710A (en) * 1975-09-12 1979-11-28 Anic Spa Method of occluding substances in structures and products obtained thereby

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US2508462A (en) * 1945-03-17 1950-05-23 Union Carbide & Carbon Corp Method and apparatus for the manufacture of synthetic staple fibers
US2988782A (en) * 1958-12-09 1961-06-20 Du Pont Process for producing fibrids by precipitation and violent agitation
US3042970A (en) * 1961-08-14 1962-07-10 American Cyanamid Co Particulation of polymer by extruding a solution thereof into a liquid stream of fluid
US3070835A (en) * 1960-01-12 1963-01-01 Standard Oil Co Pump quenching of polymer solvent mixtures
US3306342A (en) * 1966-03-02 1967-02-28 Goodrich Gulf Chem Inc Fluid processes useful in precipitation of dissolved solids
US3309734A (en) * 1964-05-21 1967-03-21 Monsanto Co Spinnerette
US3342921A (en) * 1966-03-16 1967-09-19 West Virginia Pulp & Paper Co Process for producing fibrous filler having high wet end retention
US3377323A (en) * 1963-06-11 1968-04-09 Asahi Chemical Ind Method for pulverizing polymers
US3386488A (en) * 1966-03-18 1968-06-04 Leuna Werke Veb Process for producing powders from plastic and wax masses
US3432483A (en) * 1965-02-18 1969-03-11 Nat Distillers Chem Corp Continuous process for preparing finely divided polymers
US3449291A (en) * 1966-06-15 1969-06-10 Nat Distillers Chem Corp Colored polymer powders
US3450184A (en) * 1965-07-24 1969-06-17 Bayer Ag Apparatus for separating polymers from their solutions
US3468986A (en) * 1966-11-15 1969-09-23 David J Watanabe Method for producing a solid particulate material
US3536796A (en) * 1967-11-29 1970-10-27 Grace W R & Co Process for reducing shrinkage in preparing porous plastic sheet
US3549732A (en) * 1965-09-17 1970-12-22 Petro Tex Chem Corp Method for separating a polymer from a solvent
US3627733A (en) * 1964-06-10 1971-12-14 Asahi Chemical Ind Method for particularizing thermoplastic polyesters
US3774387A (en) * 1970-09-11 1973-11-27 Du Pont Hydrophilic textile products

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2508462A (en) * 1945-03-17 1950-05-23 Union Carbide & Carbon Corp Method and apparatus for the manufacture of synthetic staple fibers
US2988782A (en) * 1958-12-09 1961-06-20 Du Pont Process for producing fibrids by precipitation and violent agitation
US3070835A (en) * 1960-01-12 1963-01-01 Standard Oil Co Pump quenching of polymer solvent mixtures
US3042970A (en) * 1961-08-14 1962-07-10 American Cyanamid Co Particulation of polymer by extruding a solution thereof into a liquid stream of fluid
US3377323A (en) * 1963-06-11 1968-04-09 Asahi Chemical Ind Method for pulverizing polymers
US3309734A (en) * 1964-05-21 1967-03-21 Monsanto Co Spinnerette
US3402231A (en) * 1964-05-21 1968-09-17 Monsanto Co Process for preparing synthetic fibers for paper products
US3627733A (en) * 1964-06-10 1971-12-14 Asahi Chemical Ind Method for particularizing thermoplastic polyesters
US3432483A (en) * 1965-02-18 1969-03-11 Nat Distillers Chem Corp Continuous process for preparing finely divided polymers
US3450184A (en) * 1965-07-24 1969-06-17 Bayer Ag Apparatus for separating polymers from their solutions
US3549732A (en) * 1965-09-17 1970-12-22 Petro Tex Chem Corp Method for separating a polymer from a solvent
US3306342A (en) * 1966-03-02 1967-02-28 Goodrich Gulf Chem Inc Fluid processes useful in precipitation of dissolved solids
US3342921A (en) * 1966-03-16 1967-09-19 West Virginia Pulp & Paper Co Process for producing fibrous filler having high wet end retention
US3386488A (en) * 1966-03-18 1968-06-04 Leuna Werke Veb Process for producing powders from plastic and wax masses
US3449291A (en) * 1966-06-15 1969-06-10 Nat Distillers Chem Corp Colored polymer powders
US3468986A (en) * 1966-11-15 1969-09-23 David J Watanabe Method for producing a solid particulate material
US3536796A (en) * 1967-11-29 1970-10-27 Grace W R & Co Process for reducing shrinkage in preparing porous plastic sheet
US3774387A (en) * 1970-09-11 1973-11-27 Du Pont Hydrophilic textile products

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4025593A (en) * 1971-08-06 1977-05-24 Solvay & Cie Fabrication of discontinuous fibrils
US4189455A (en) * 1971-08-06 1980-02-19 Solvay & Cie. Process for the manufacture of discontinuous fibrils
US4600545A (en) * 1972-02-25 1986-07-15 Montecatini Edison S.P.A. Process for the preparation of fibers from polymeric materials
US3987139A (en) * 1972-03-20 1976-10-19 Crown Zellerbach Corporation Process of forming synthetic fibers
US4007247A (en) * 1972-09-26 1977-02-08 Imperial Chemical Industries Limited Production of fibrils
US3976631A (en) * 1973-04-18 1976-08-24 Stamicarbon B.V. Process for preparing ethylene polymers
US4167548A (en) * 1973-11-08 1979-09-11 Societa' Italiana Resine S.I.R. S.P.A. Process for the manufacture of a microfibrous pulp suitable for making synthetic paper
US4081226A (en) * 1974-01-18 1978-03-28 Solvay & Cie. Process for the manufacture of short fibrils and devices for carrying it out
US4010229A (en) * 1974-01-18 1977-03-01 Solvay & Cie Process for the manufacture of short fibrils
US4127623A (en) * 1974-08-03 1978-11-28 Sumitomo Chemical Company, Limited Process for producing polyolefin short fibers
US4211737A (en) * 1974-11-19 1980-07-08 Montedison S.P.A. Process for producing synthetic fibers for use in paper-making
US4129629A (en) * 1974-11-28 1978-12-12 Hoechst Aktiengesellschaft Process for making hydrophilic polyolefin fibers containing clay
US4073850A (en) * 1974-12-09 1978-02-14 Rothmans Of Pall Mall Canada Limited Method of producing polymeric material
US4192838A (en) * 1976-10-06 1980-03-11 Celanese Corporation Process for producing filter material
US4301105A (en) * 1980-04-21 1981-11-17 American Cyanamid Company Process for spinning poly(polymethylene terephthalamide) fiber
EP0176350A2 (en) * 1984-09-25 1986-04-02 Mitsui Petrochemical Industries, Ltd. Process for preparation of synthetic fibers
EP0176350A3 (en) * 1984-09-25 1987-09-23 Mitsui Petrochemical Industries, Ltd. Process for preparation of synthetic fibers
US5650221A (en) * 1995-07-06 1997-07-22 Laroche Industries, Inc. High strength, low pressure drop sensible and latent heat exchange wheel
US5685897A (en) * 1995-07-06 1997-11-11 Laroche Industries, Inc. High strength, low pressure drop adsorbent wheel
US20050109856A1 (en) * 2003-11-25 2005-05-26 Alexander James N.Iv Method for preparing polymer electrosprays
US20080003435A1 (en) * 2006-06-29 2008-01-03 The Procter & Gamble Company Faux fibers and fibrous structures employing same
US20100127434A1 (en) * 2008-11-25 2010-05-27 Rene Broos Extruding organic polymers

Also Published As

Publication number Publication date
JPS5116533B1 (sv) 1976-05-25
SU471735A3 (ru) 1975-05-25
DE2225936A1 (de) 1973-01-04
IT958078B (it) 1973-10-20
ES403712A1 (es) 1975-05-16
GB1379672A (en) 1975-01-08
NL7207416A (sv) 1972-12-05
FR2141139A5 (sv) 1973-01-19
NO136983C (no) 1977-12-07
SE381696B (sv) 1975-12-15
DE2225936B2 (de) 1976-01-08
CA1027322A (en) 1978-03-07
NO136983B (no) 1977-08-29

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