EP3294935A1 - Appareil de production de nanofibres ou de microfibres - Google Patents

Appareil de production de nanofibres ou de microfibres

Info

Publication number
EP3294935A1
EP3294935A1 EP15732153.0A EP15732153A EP3294935A1 EP 3294935 A1 EP3294935 A1 EP 3294935A1 EP 15732153 A EP15732153 A EP 15732153A EP 3294935 A1 EP3294935 A1 EP 3294935A1
Authority
EP
European Patent Office
Prior art keywords
microfibers
producing nanofibers
chamber
rotating disc
rotating
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.)
Withdrawn
Application number
EP15732153.0A
Other languages
German (de)
English (en)
Inventor
Milos Beran
Frantisek Toman
Josef DRAHORÁD
Jifí HOVORKA
Zdenek Husek
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Czech Technical University In Prague
Original Assignee
Czech Technical University In Prague
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Czech Technical University In Prague filed Critical Czech Technical University In Prague
Publication of EP3294935A1 publication Critical patent/EP3294935A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
    • 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
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/14—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated alcohols, e.g. polyvinyl alcohol, or of their acetals or ketals
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones

Definitions

  • a device for producing fibers or microfibers A device for producing fibers or microfibers
  • the invention relates to a device for producing nanofibers or microfibers from solutions, emulsions, liquid suspensions or melts containing a spun substance.
  • nanofibers occurs directly from the surface of spun solutions which can be in the form of a thin film.
  • Two-layer systems are also used, wherein the lower layer is formed by a ferromagnetic suspension and the upper layer by a solution of spun polymer. After application of the magnetic field, sharp vertical cones of the ferromagnetic liquid are formed that serve as nuclei from which the nanofibers are produced.
  • Other device is based on the aeration of a spun polymer solution in order to create a high concentration of bubbles on the surface of the solution / wherein a lowering of the surface tension takes place and the bubbles form seeds of nanofibers created by virtue of the electric field.
  • Another device is based on a slowly rotating cylinder which is partially immersed in a solution of the spun polymer. During the rotation of the cylinder, a deposit of a specific amount of the solution on the roller takes place, resulting in a formation of a continuous film from which on the upper part by virtue of a strong electric field so-called Taylor cones serving as nuclei of nanofibers are formed.
  • Electrostatic spinning methods are characterized by a low speed of the process; they are technically complicated and expensive.
  • the electrostatic spinning is limited by the necessity of a high voltage electric field.
  • the chamber is generally provided with a source of the flowing gas and a collection area.
  • the chamber is provided with a number of side by side arranged hollow shafts on which rotating discs are mounted.
  • At least one hollow shaft is provided with two superposed rotating discs .
  • At least one rotating disc is composed of two successive parts, wherein between the upper part and the lower part the outlet gap is formed around the circumference thereof.
  • the size of the outlet gap between the upper part and the lower part of rotating disc may be formed by a spacer element, in particular a spacer ring.
  • At least one part of the rotating disc has a frustoconical shape.
  • At least one rotating disc may be provided with a pressure element, such as pressure nut.
  • At least one disc or discs disposed in a chamber which is made of heat resistant material may be provided with means for their heating.
  • the inner space of the hollow shaft is connected with the output gap of each of the rotating discs by means of openings and at the other end with a rotary unit for supplying the polymer and further with the drive motor.
  • the source of the flowing gas in the chamber is a compressor or a fan.
  • the collecting area can be either a movable conveyor made of a breathable fabric or a rotating collector or a bag of a porous mesh.
  • the collecting area may be electrically charged.
  • the present invention in comparison with the current state of the art prevents drying films of polymer solutions on the surface of rotating discs. It reduces the amount of defects of produced nanofibers and microfibrous layers, especially drops. It facilitates the centrifugal spinning of melts, because there occurs no cooling of the melt on the surface of the rotating elements.
  • Figure 1 shows an overall diagram of the entire device
  • Figure 2 shows a spindle with a hollow shaft and a disc in the perspective illustration and partial longitudinal section
  • Figure 3 shows a specific embodiment of the disc according to the invention without a spacer
  • Figure 4 shows a specific embodiment of the disc according to the invention with a spacer.
  • Example 1 Preparation of nano- or microfibers from a polyvinyl alcohol solution
  • polyvinyl alcohol micro- or nanofibers To prepare polyvinyl alcohol micro- or nanofibers, a commercial solution of polyvinyl alcohol Sloviol R16, 16% (wt./wt.) of solid content (Fichema) was used.
  • the polyvinyl alcohol solution was pumped from the first liquid reservoir 17 by the first pump 18 through a connecting hose 19 via the first safety valve 20 and the first check valve 21 at a rate of 2-12 ml/min., and fed through an inlet 22 of liquid into the rotation unit 10 from which it further entered into a hollow shaft 3_ disposed in a tube 5 of a spindle.
  • Via openings 16 was the polyvinyl alcohol solution sprayed from the inner space 6 of the hollow shaft 3 into the inner space of the rotating disc 2 having a conical shape with a diameter of 120 mm, between the upper part 7 and the lower part 8 thereof.
  • The. output gap 4 of the conical disc 2 was set up using a spacer ring 13 on the width of 200 micrometers as shown in Figure 4.
  • the rotating disc 2 was positioned over the base plate 23 with channels 32 for the distribution of the drying gas into the chamber 1_ in the form of a tube 5 of a plexi-glass having the diameter of 35 cm and the height 40 cm.
  • the base plate 23 entered at a rate of 0.7 m 3 /s drying air preheated to a temperature of 25°C from a source 11, which is formed by a compressor and a heater.
  • the rotating disc 2 with the hollow shaft 3 was rotated via an intermediate transmission 15_ by means of a drive motor 14_ at a speed of 1 to 5000 revolutions per minute.
  • the stream of preheated air carried away the nano- or microfibers generated by the centrifugal force on the edge of the outlet gap 4_ into a collection chamber 12 provided with an orifice having a width of the slot 24 of 5 cm and a length of 35 cm and a sliding belt 25 formed by a permeable nonwoven Spunbond having a basis weight 18.8 g/m 2 .
  • the shift velocity was 10 cm/min.
  • the nano- or microfibers were stored in the form of a continuous layer on the surface of the sliding belt 25 of the permeable nonwoven .
  • polyamide 6 For the preparation of micro or nanofibers polyamide 6 were used pellets of polyamide 6 (Rhodia Technyl) . From these pellets was prepared a solution 15% (wt./wt.) in 85% (wt./wt.) formic acid (Penta) at a temperature of 80 °C. This solution was pumped from the first liquid reservoir 17 by the first pump 18 through the connecting hose 19 via the first safety valve 20 and the first check valve 21 at a rate of 6-16 ml/min., and fed through the inlet 22 of liquid into the rotation unit 10 from which it further entered into the hollow shaft 3 disposed in the tube 5 of the spindle.
  • Via openings 16 was the polyamide 6 solution sprayed from the inner space 6 of the hollow shaft 3 into the inner space of the rotating disc 2 between the upper part 7 and the lower part 8 ⁇ thereof.
  • the disc 2 having a conical shape with a diameter of 120 mm provided with the pressure element 9 in the form of a nut was used, as it can be seen from Figure 3.
  • the pressure of the presser nut was gradually changed so that an opening of the outlet gap 4 occurs at a pressure in the range of 4-400 bar.
  • the rotating disc 2 was positioned over the base plate 23 with channels 32 for the distribution of the drying gas into the chamber 1 in the form of a tube 5 of a plexi-glass having the diameter of 35 cm and the height of 40 cm.
  • the base plate 23 entered at a rate of 0.6 m 3 /s drying air preheated to a temperature of 35 °C from a source 11_, which is formed by a compressor and a heater.
  • the rotating disc 2 with the hollow shaft 3 was rotated via an intermediate transmission 15 by means of a drive motor 14 at a speed of 1 to 5000 revolutions per minute.
  • the stream of preheated air carried away the nano- or microfibers generated by the centrifugal force on the edge of the outlet gap 4 into a collection chamber 12 provided with an orifice having a width of the slot 24 5 cm and a length 35 cm.
  • a rotating collector of fibers in the form of a roller made of fine steel mesh having a diameter of 10 cm and provided with a motor imparting the collector a rotation of 10 rpm. was positioned longitudinally horizontally.
  • Nano- or microfibers were deposited evenly over the whole surface of the rotary collector in the form of a continuous layer of a thickness of almost 3 mm in the form resembling a soft cotton wool.
  • a reduction in diameter of the fibers has occurred. While at a pressure of 4 bar the fiber diameter was in the range 600 to 900 nm, at a pressure of 400 bar the diameter was already in the range of 200 nm to 400 nm.
  • the rate of the fibers formation was in the range of 50 g to 135 g per hour, depending on the conditions. The optimal flow rate was 14 ml/rain.
  • a chamber 1 made of plexi-glass and having a cuboidal shape with a length of 2 m and a width and a height of 50 cm was used, in which two rotating discs 2 were placed side by side, with pressure elements 9 in the form of nuts. The discs 2 were placed at a distance of 1 m apart. Optimal conditions were used for spinning the polyamide 6 solution as identified in the above described experiment. The flow in each disk was 14 ml/min. The pressure in the inner space of the disk 2 between the upper part 1_ and the lower part 8 thereof was 60 bar.
  • the collection of the fibers in the collecting space 12 was carried out using a slot having a width of the aperture 24 of 20 cm and a length of 2 m and a sliding belt 25 of the permeable Spunbond nonwoven having a basis weight of 18.8 g/m2, also with a width of 2 m.
  • the speed of displacement of the belt was 10 cm/min.
  • the nano- or microfibers have been stored in the form of a continuous layer on the surface of the belt 25 of a permeable fabric.
  • the distribution of the nanofibers was homogeneous both in the microscopic and macroscopic level across the whole belt width, which represented 35 cm.
  • the diameter of the majority of fibers observed was in the range of 400 to 800 nanometers.
  • the basis weight of the fibers was in the range of 4-6 g/m 2 .
  • a 10% (wt./wt.) suspension of the microbial preparation BA (1.10 9 CFU/g) (Milcom) containing the probiotic strains of genera Lactobacillus acidophilus and Bifidobacterium bifidum freeze- dried with powdered milk in distilled water was used. Further, a solution of 30% (wt./wt.) of pig skin gelatin, 300 bloom, type A (Sigma-Aldrich) in 40% (vol. /vol.) acetic acid was used.
  • the gelatin solution at a temperature of 45°C was pumped from the first reservoir 17 of liquid by means of the first pump 18 via the first connecting pipe 19 through the first safety valve 20 and the first check valve 21 at a rate of 5 ml/min.
  • a bacterial suspension was pumped from the second reservoir 26 of liquid by means of the second pump 27 via the connecting hose 19 through the second safety valve 28 and the second check valve 29 at a rate of 5 ml/min.
  • the gelatin solution and bacterial suspension were mixed in a mixing chamber 30 having a volume of 5 ml.
  • the resulting bacterial suspension in the gelatin solution was fed through the inlet 22. of liquid into a rotation unit 10.
  • the suspension was further sprayed from the inner space 6 of the hollow shaft 3_ into the inner space of the rotating disc 2 of a conical shape with a diameter of 120 mm, between its upper part T_ and the lower part 8.
  • the output gap 4_ of the conical disc 2 was set using the spacer element 13 to the width of 150 microns, as shown in Figure 4.
  • the rotating disc 2 was positioned over the base plate 23 with channels 32 for the distribution of the drying gas into the chamber 1 in the form of a tube made of fine steel mesh 35 cm in diameter and the height 40 cm.
  • Into the base plate 23 entered the drying air preheated to a temperature of 40°C from a source 11, which is formed by a compressor and a heater, at a velocity of 0,8 m 3 /s.
  • the rotating disc 2 with the hollow shaft 3 was rotated via an intermediate transmission 15 by means of a drive motor 14_ at a speed of 3500 revolutions per minute.
  • the stream of preheated air carried away the nano- or microfibers generated by the centrifugal force on the edge of the outlet gap 4 of the rotating disc 2 into a collection chamber 12 provided with an orifice having a width of the slot 24 of 10 cm over which a bag made of a permeable nonwoven Spunbond having a basis weight 18.8 g/m 2 .
  • the shift velocity was 10 cm/min.
  • the microfibers were stored in this bag in the form resembling a soft cotton wool.
  • the yield was 80 g of the microfibers with the encapsulated bacterial culture in one hour of the operation.
  • a microscopic analysis confirmed the presence of bacterial cells encapsulated within the microfibers having a diameter of between 5 and 10 microns.
  • Standard methods for microbiological analysis showed that there was only a small decrease in vitality of the original bacterial culture, expressed as a number of colony-forming units (CFU) , by one order.
  • CFU colony-forming units
  • a melt of polyhydroxy alkanoate (Nanjing Huichen Co., Ltd., China) was prepared in the first reservoir 14 of a solution equipped with an induction heating, and maintained at a temperature of 300 degrees Celsius. The entire device was thermally insulated.
  • the melt was pumped from the first reservoir 17 of a solution by the first pump 18 ⁇ via the insulated connecting hose 153 made of a profiled steel strip through the first safety valve 20 and the first check valve 21 at a velocity of 10 ml/min., and fed through the inlet 22 of a liquid into the rotation unit 10 from which it further entered into the hollow shaft 3 disposed in the tube 5 of the spindle.
  • Through openings IS were the melt sprayed from the inner space of the hollow shaft 6 into the inner part of the rotating disc 2 of a conical shape, with a diameter of 120 mm, between the upper part 2 and the lower part 8 thereof.
  • the output gap 4 of the conical disc 2 has been set using the spacing element 13 to the width of 50 microns, as it is apparent from Figure 4.
  • the rotating disc 2 was positioned over the base plate 23 equipped with channels 32 for the distribution of the drying gas into the chamber 1 in the form of an insulated steel tube having the diameter of 35 cm and the height of 40 cm.
  • the drying air preheated to 250°C from a source 11, which was formed by a compressor and a heater, entered at a velocity of 1 m 3 /s.
  • the rotating disc 2 with the hollow shaft 3 was rotated via an intermediate transmission 15 by means of a drive motor 14_ at a speed of 1 to 5 000 revolutions per minute.
  • the stream of preheated air carried away the nano- or microfibers generated by the centrifugal force on the edge of the outlet gap 4 into a collection chamber 12 provided with an orifice having a width of the slot 24 of 5 cm and a length of 35 and a sliding belt made of a fine steel mesh.
  • the basis weight of the fibers was in the range of 8-10 g/m 2 .
  • the distribution of the nanofibers was homogeneous both in the microscopic and macroscopic level across the whole belt width, which represented 35 cm.
  • the diameter of the majority of fibers observed was in the range of 400 to 800 nanometers.
  • the rate of fibres production was 600 g per hour.
  • a device for the production of fibers or microfibres from solutions, emulsions, melts or liquid suspensions containing a spinnable polymer according to the invention may be advantageously used to produce nanofibers or microfibers, where a high productivity work is required.
  • the device also facilitates the centrifugal spinning of melts, because no cooling of the melt on the surface of the rotating elements takes place.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Nonwoven Fabrics (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

L'invention concerne un dispositif de production de nanofibres ou de microfibres à partir de solutions, d'émulsions, de suspensions liquides ou de fonds contenant une substance filée. L'objet de l'invention consiste en ce que ledit dispositif comprend une chambre dans laquelle un arbre creux est assemblé, sur lequel au moins un disque rotatif présentant un espace de sortie est monté. La chambre est généralement pourvue d'une source du gaz d'écoulement et d'une zone de collecte. Dans un autre mode de réalisation en variante, la chambre est pourvue d'un certain nombre d'arbres creux disposés côte à côté sur lequel sont montés des disques rotatifs. Il est préférable qu'au moins un arbre creux soit pourvu de deux disques rotatifs superposés. Au moins un disque rotatif est composé de deux parties successives, un espace de sortie étant formé autour de la circonférence de celui-ci entre la partie supérieure et la partie inférieure. La taille de l'espace de sortie entre la partie supérieure et la partie inférieure d'un disque rotatif peut être formée par un élément d'espacement, en particulier une bague d'écartement.
EP15732153.0A 2015-05-15 2015-05-15 Appareil de production de nanofibres ou de microfibres Withdrawn EP3294935A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CZ2015/000044 WO2016184439A1 (fr) 2015-05-15 2015-05-15 Appareil de production de nanofibres ou de microfibres

Publications (1)

Publication Number Publication Date
EP3294935A1 true EP3294935A1 (fr) 2018-03-21

Family

ID=53491243

Family Applications (1)

Application Number Title Priority Date Filing Date
EP15732153.0A Withdrawn EP3294935A1 (fr) 2015-05-15 2015-05-15 Appareil de production de nanofibres ou de microfibres

Country Status (3)

Country Link
US (1) US20170233896A1 (fr)
EP (1) EP3294935A1 (fr)
WO (1) WO2016184439A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110208245B (zh) * 2019-06-19 2020-09-08 清华大学 一种纸基柔性表面增强拉曼散射效应基片及其制备方法
CN113584615B (zh) * 2021-09-01 2022-05-03 福建永荣锦江股份有限公司 一种共轴驱动离心纺丝卷绕装置

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4790736A (en) * 1984-07-20 1988-12-13 John E. Benoit Apparatus for centrifugal fiber spinning with pressure extrusion
US5326241A (en) * 1991-04-25 1994-07-05 Schuller International, Inc. Apparatus for producing organic fibers
EP1278618A4 (fr) * 2000-02-18 2005-07-20 Charge Injection Technologies Procede et appareil de fabrication de fibres
US7857608B2 (en) * 2006-12-08 2010-12-28 Spindynamics, Inc. Fiber and nanofiber spinning apparatus
US8597552B2 (en) * 2009-03-16 2013-12-03 Evan Koslow Apparatus, systems and methods for producing particles using rotating capillaries
WO2011090995A2 (fr) * 2010-01-19 2011-07-28 Unversity Of Florida Research Foundation Inc. Structures et procédés de collecte de fibres électrofilées
KR20160073971A (ko) * 2013-10-22 2016-06-27 이 아이 듀폰 디 네모아 앤드 캄파니 용융 방사 폴리프로필렌 미세 등급 나노섬유 웨브

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Publication number Publication date
US20170233896A1 (en) 2017-08-17
WO2016184439A1 (fr) 2016-11-24

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