WO2017212465A1 - Procédé et système pour la préparation de fibres polymères - Google Patents

Procédé et système pour la préparation de fibres polymères Download PDF

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Publication number
WO2017212465A1
WO2017212465A1 PCT/IL2016/050602 IL2016050602W WO2017212465A1 WO 2017212465 A1 WO2017212465 A1 WO 2017212465A1 IL 2016050602 W IL2016050602 W IL 2016050602W WO 2017212465 A1 WO2017212465 A1 WO 2017212465A1
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WO
WIPO (PCT)
Prior art keywords
mixture
spinneret
velocity
fiber
parameters
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Application number
PCT/IL2016/050602
Other languages
English (en)
Inventor
Oleg PALCHIK
Leonid VAISTIKH
Alexander ROITFELD
Nimer Jaber
Stela DIAMANT LAZAROVICH
Ido AMRAM
Original Assignee
Intellisiv Ltd.
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 Intellisiv Ltd. filed Critical Intellisiv Ltd.
Priority to PCT/IL2016/050602 priority Critical patent/WO2017212465A1/fr
Publication of WO2017212465A1 publication Critical patent/WO2017212465A1/fr

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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
    • D01D5/38—Formation of filaments, threads, or the like during polymerisation
    • 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
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected

Definitions

  • This invention is directed to a polymer fibers preparation system, and method of preparing the polymer fiber using the system, wherein the system comprises spinneret and a UV source located in proximity to an outlet of the spinneret.
  • Polymeric fibers are widely used to prepare woven fabrics, non-woven fabrics, such as wipers, diapers, industrial garments, medical and health garments or filtration garments. Such low quality graded fibers are mass-produced by relatively low-cost methods and low-cost material. When higher quality, such as optical quality, is required methods of preparation and the polymers used change dramatically.
  • Polymer optical fibers are mostly made from thermoplastic polymers such as PMMA and produced by extrusion methods.
  • the thermoplastic polymer is heated to above the glass transition temperature (Tg) or above the melting temperature (Tm) to be extruded via a spinneret to form polymeric fibers.
  • Tg glass transition temperature
  • Tm melting temperature
  • An alternative production method is direct fiber drawing from a melt using "wire drawing” techniques.
  • the polymeric chains in the extruded fibers may be partially cross-linked using an electron beam. This process is complicated and expensive.
  • thermoset polymers that needs to be cured from a mixture of monomers are hard to fabricate although may possess better mechanical properties and thermal stability.
  • the monomers mixture must be cured, for example, by ultraviolet (UV) light in order to solidify (creates cross-linked chains) and harden the polymer.
  • UV ultraviolet
  • Regular extrusion production methods are not suitable for thermoset polymers.
  • a flow of mixture of monomers coming out of an extruder's spinneret will disintegrate. Partial curing for forming oligomers can be applied to the monomers mixture allowing a better control of the injection of the mixture. However even a partially cured mixture must be cured to the highest possible level after leaving the spinneret.
  • Fig. 1 is a high-level block diagram of a polymer fibers preparation system according to some embodiments of the invention.
  • FIG. 2 is a flowchart of a method of producing polymer fibers according to some embodiments of the invention.
  • Fig. 3 is a flow chart of a method of determining a mixture velocity range for receiving a stable mixture stream in a system for preparation of a polymer fiber according to some embodiments of the invention
  • FIGs. 4A and 4B are illustrations of an exemplary polymer fibers preparation system according to some embodiments of the invention.
  • FIG. 5 is an illustration of an exemplary mixture injection system according to some embodiments of the invention.
  • Fig. 6 is an illustration of an exemplary spinneret according to some embodiments of the invention.
  • Fig. 7 is an illustration of an exemplary coaxial spinneret according to some embodiments of the invention.
  • Fig. 8 is an exemplary shutter according to some embodiments of the invention.
  • Some embodiments of the invention are related to a system for fabricating high quality polymeric fibers, for example, a polymer optical fiber or thin fibers (e.g., 1-100 microns) for insulation or filtering purposes.
  • a system for fabricating high quality polymeric fibers for example, a polymer optical fiber or thin fibers (e.g., 1-100 microns) for insulation or filtering purposes.
  • Such system may fabricate polymeric thermoset fibers from a mixture of monomers or oligomers.
  • Embodiments of the system may directly pump the mixture from a preparation tank and inject the mixture using a spatially designed injection system such that a steady stream of mixture is formed at the exit of the specially designed injection system.
  • the steady stream of mixture may be immediately radiated by UV light to cure the stream and form a fiber.
  • Some embodiments of the invention may include controlling the operation parameters of the system for fabricating high quality polymeric fibers such that a steady stream is formed and timely cured to form the high quality polymeric fiber. Additional embodiments of the invention may be related to a special design of the injection system and the UV curing system to produce a high quality fiber.
  • Fig. 1 is a high-level block diagram of a polymer fibers preparation system according to some embodiments of the invention.
  • Embodiments of system 100 may fabricate fibers in wide variety of diameters, for example, thin fibers having 1-100 microns diameter or millimeteric size optical fibers having 0.5-2 mm diameter.
  • Embodiments of system 100 may include a spinneret 140, one or more controllable ultraviolet (UV) sources 150 and a controller 170.
  • system 100 may further include a mixture holding tank 110, a pumping system 120, a controllable valve 130 and a fiber collecting system 160.
  • Mixture holding tank 110 may include any tank, container or volume that is configured to hold a mixture of monomers or oligomers formulation for fiber preparation, for example, monomers of thermoset polymers, such as acrylic monomers.
  • the mixture may include monomers/oligomers and additives such as photo-initiators, dyes and plasticizers.
  • Tank 110 may include an inlet for receiving raw materials and an outlet for discharging the mixture. The inlet and the outlet may be well sealed and protected to prevent material leakage. The tank may further be UV isolated to prevent undesired curing of the mixture.
  • Tank 110 may further include a mixer for mixing the monomers and/or oligomers mixtures and a vacuum pump and degassing valve to remove air and reduce gas bubbles in the mixture.
  • Mixture holding tank 110 may further include a heating element and a thermometer (both not shown) for monitoring and controlling the temperature of the mixture.
  • the temperature of the mixture may determine the viscosity and viscoelasticity of the mixture thus may affect the quality of the fabricated fiber.
  • Controller 170 may control the heating element to sustain a controlled temperature range of the mixture according to signals received from the thermometer.
  • mixture holding tank 110 may be a portable and optionally sealed tank (e.g., a sealed barrel) containing a premixed formulation, received directly from a supplier. Such a sealed tank may include only an outlet valve connected to a pump line. The mixture may be pumped from mixture holding tank 110 by pumping system 120.
  • system 100 may include more than one holding tanks 110, each tank for holding a different mixture having a different formulation and / or equal mixtures.
  • system 100 may include a first tank for holding a first material and a second tank for holding a second material.
  • the first material may include a first mixture and the second material may include a second mixture.
  • Pumping system 120 may be configured to supply the mixture from holding tank 110 to spinneret 140.
  • Pumping system 120 may include a pump 122 and a filter 125.
  • Pump 122 may include a positive displacement pump configure to supply the mixture in a constant flow rate.
  • the constant flow rate is to produce constant steady stream of mixture, since pulsation may be an undesired affect.
  • Pump 122 may be a low shear pump to prevent polymerization due to heat produced by the pump.
  • pump 122 may be a piston pump, a multi membrane pump or the like. Pump 122 may have the ability to work at flow rates as low as 0.1 liter/hours and at pressures as high as 200 bar.
  • Pump 122 inner surfaces being in contact with the mixture may be corrosive resistant for both the monomer's mixture and cleaning agents for cleaning the mixture's residue.
  • Pump 122 may further include a temperature indicator, such as a thermometer for measuring and controlling the temperature of the mixture inside the pump (thus controlling the viscosity).
  • Pump 122 may further include a cooling element for cooling the mixture and/or a heating element for heating the mixture to enable maintaining the mixture at a desired temperature range.
  • pumping system 120 may be configured to pump more than one mixture (e.g., having different formulations) from more than one holding tanks 110.
  • pumping system 120 may include a plurality of pumps 122, each for pumping mixture from a different holding tank 110.
  • a single pump 122 may pump all mixtures using a plurality of valves for timely connecting the pump to each holding tank 110.
  • Filter 125 may be configured to filter impurities or polymerized particles from the formulation.
  • Filter 125 may include a metal filter or any other suitable filter, for example, having 0.1 micron halls. The filter may be cleaned periodically. A degassing process may be carried out at the beginning of a new production cycle.
  • Valve 130 may be any pneumatic or electric remotely controlled flow valve for controlling the timing, pressure and amount of injection of the mixture. Upon opening valve 130, a flow of mixture may flow in a supply line from pump 122 to spinneret 140. Valve 130 may allow building pressure in the supply line before the injection, thus having a fast and stable flow from the start. Fast and stable flow of mixture in spinneret 140 may prevent polymerization of the mixture in the spinneret thus blocking the spinneret. The starting pressure built in valve 130 may be between 5-10 bar. A detailed illustration of valve 130 as assembled in an injection system according to some embodiments of the invention is given in Fig. 5.
  • Spinneret 140 may be designed to form a stable mixture stream (e.g., liquid formulation jet) of desired diameter that can be cured into a solid fiber.
  • a stable stream or a stable flow is defined as a continuous flow or a stream having no disconnections (e.g., separate drops of mixture and/or expanding or diverging of the stream) that further has a uniform or full cross section, such that the entire cross-section of the stream, at any point along the stream until a complete curing of the mixture, contains material.
  • a stable flow or stream according to embodiments of the invention will result with the formation of a solid fiber of a desired quality.
  • the desired quality may vary according to the requirements from the fiber, for example, the desired quality may be optical quality, thermal insulation quality or the like.
  • An exemplary stable flow may include laminar flow.
  • Spinneret 140 may include at least one nozzle for injecting the mixture and may further be designed to create a stable stream of mixture for a predetermined length (for example, at list 10 cm) after leaving the nozzle, to be cured in a curing area.
  • a detailed exemplary geometrical design of spinneret 140 is illustrated and discussed with respect to Fig. 6.
  • system 100 may include a plurality of spinnerets 140 such that pumping system 120 may supply the mixture to each spinneret of the plurality of spinnerets.
  • spinneret 140 may include a plurality of nozzles each for creating a multitude stream of mixture.
  • the injected stream may have a velocity of between 2-10 m/s.
  • system 100 may include a plurality of spinnerets divided into two or more groups of spinnerets.
  • Pumping system 120 may be configured to supply a first group of spinnerets from the plurality of spinnerets 140 a first mixture from a first tank 110 and to supply a second group of spinnerets 140 from the plurality of spinnerets a second mixture from a second tank 110, such that two or more types of fibers may simultaneously be fabricated in a single cycle of operation.
  • spinneret 140 may be designed to receive from a first and a second holding tank 110 first and second materials such that a stream leaving the spinneret includes both the first and second materials.
  • the spinneret may be designed to inject the first material at an inner portion of the stream and the second material at a peripheral portion of the stream such that the first material stream is encompassed by the second material stream.
  • the first material may be a gas flowing from a gas tank and the second material may be monomers or oligomers mixture such that after curing a hollow fiber may be formed.
  • the first material may be monomers or oligomers mixture and the second material may include an oxygen free gas (e.g., nitrogen) for protecting the mixture from oxygen atoms that may harm the curing and cross linking process of the mixture.
  • spinneret 140 may be designed to receive three or more different mixtures from three or more tanks 110 such that the stream leaving the spinneret includes the three or more different mixtures.
  • spinneret 140 may be designed to coaxially inject the three or more different mixtures such that an inner portion of the stream includes a first mixture that is encompass by one or more different materials to form a coaxial multi-layer fiber.
  • the first mixture may be injected in the inner portion of the cross-section of the stream.
  • the inner portion may be encompassed by a second mixture.
  • the second mixture may be encompassed by a third mixture, followed by a fourth mixture and so on.
  • spinneret 140 may be designed to inject a stream having three or more, four or more, five or more different mixtures as to form multi-layered fiber having. For example, gradually changing refractive index.
  • mixture stream injected from spinneret 140 may be cured by controllable UV source 150 that is configured to instantly apply and/or shut off the application of UV radiation to a mixture stream leaving the spinneret.
  • Controllable UV source 150 may include a UV lamp 152 and a controllable shutter 154 configured to block the UV radiation from the UV lamp from reaching the mixture stream. Additionally or alternatively to shutter 154, controllable UV source 150 may include an electric switch (not illustrated) for operating and shutting off UV lamp 152.
  • Lamp 152 may be any UV lamp known in the art.
  • lamp 152 may be a mercury lamp or a light emitting diode (LED) UV lamp.
  • LED light emitting diode
  • the switch may cause an instant operation and/or shutting off of lamp 152, since the response time of LED lamps is very short (almost immediate) thus making the shutter redundant.
  • LED lamp 152 may instantly radiate, upon being turned on, in full capacity the mixture stream that leaves the spinneret immediately after being.
  • Lamp 152 may supply a required dose of UV radiation for curing the mixture stream into a fiber.
  • the photoinitiators in the mixture formulation may initiate the beginning of the polymerization reaction when exposed to a sufficient UV irradiance.
  • Lamp 152 may include optical elements, such as reflectors (not illustrated) to focus the radiated light on to the mixture stream after leaving the spinneret.
  • the reflector e.g., mirrors
  • Sufficient radiation dose may be needed to get a fully cured fiber.
  • the UV dose may be a function of the lamp 152 irradiance and the exposure time of the stream to the UV light which is determined by the length of the lamp, the number of lamps, the power of the lamp and the mixture velocity.
  • the amount of UV dose required for curing the stream may further be dependent of the stream's diameter and the photoinitiators percentage in the mixture.
  • 1 mm diameter acrylic fiber may be cured using a UV dose of at least 100 mili- Joules/cm 2 .
  • the UV spectrum emitted by lamp 152 may be defined according to the photoinitiators activation wavelength in the mixture.
  • a LED UV lamp 152 having a specific wavelength may be replaced when the photoinitiators in the mixture are replaced.
  • more than one lamp 152 may be included in controllable UV source 150.
  • 2-3 longitude mercury UV lamps may be placed around the mixture stream.
  • a plurality of LED UV lamps may be placed along the mixture stream path.
  • Some exemplary UV lamps may include: electric arc mercury lamp - D and H spectrum, microwave initiated mercury lamp - D and H spectrum, LED UV lamp - 395 and 400 nm wavelength, Excimer UV lamp, UV laser or the like.
  • Shutter 154 and/or the switch may be operated to control the amount and timing of exposure of the injected mixture to UV radiation.
  • shutter 154 may be operated to prevent UV radiation from reaching the mixture when the stream is too slow or before leaving the spinneret. If the stream is slower than the progress of the curing reaction the location on the stream at which curing occurs may reach the spinneret, thus polymerizing the mixture inside spinneret and possibly causing blocking of the spinneret.
  • a mercury lamp may require heat-up time from powering until full capacity of radiation is achieved; therefore in order to achieve an instant exposure and instant concealing of the UV radiation controllable shutter 154 may be operated.
  • a detailed illustration of an exemplary shutter 154 is given in Fig. 8.
  • controllable shutter 154 may be located in proximity to UV lamp 152 and be configured to block radiation from the UV lamp from reaching (e.g., propagate towards) the mixture stream leaving spinneret 140 when curing is not required.
  • controllable shutter 154 may be located in proximity to spinneret 140 exit and configured to cover the mixture stream leaving the spinneret from being exposed to UV radiation from the UV lamp, for example, as illustrated in Fig. 5, when no curing is required.
  • controllable UV source 150 may further include an optical filter to prevent part of the UV lamp radiation from reaching the mixture.
  • controllable UV source may further include infrared (IR) filter 153 and an oxygen free atmosphere system that includes a UV transparent tube 155 and an oxygen free gas supply system 156.
  • IR filter 153 may block IR radiation from reaching and heating the mixture stream.
  • UV transparent tube 155 may encompass the mixture stream allowing UV radiation from source 150 to reach the mixture and the cured fiber while blocking oxygen and air from reaching the mixture stream and the cured fiber.
  • UV transparent tube 155 may be made from quartz, glass, silica glass, ceramics or any other suitable UV transparent material.
  • UV transparent tube 155 may be filled with an oxygen free atmosphere, for example, supplied from oxygen free gas supply system 156.
  • an oxygen free atmosphere may include, for example, nitrogen, carbon-dioxide, helium or the like.
  • the presence of oxygen may inhibit the curing (e.g., polymerization) reaction initiated by the UV radiation.
  • the UV radiation may cause the breaking of photo initiators in the mixture into free radicals that may initiate the polymerization reaction.
  • Oxygen may bond with some of the free radical in a termination reaction, reducing the number of crosslinks that may be formed in the polymer, thus may result in a partial curing of the fiber.
  • Gas supply system 156 may introduce the gas from a pressure tubing system through the inlet of the injector (e.g., near the spinneret).
  • System 156 may include a tank for holding the gas (e.g., a pressurized tank) and a tubing system for supplying the gas from the tank to the injector.
  • a predetermined gas flow rate may be supplied, for example, at 5-15 liters/minute. In some embodiments, a higher flow rate may disturb the mixture stream resulting in fiber vibration or even may cause the fiber to hit of the tube.
  • the gas flow may be as axisymmetric as possible to prevent fiber vibration.
  • a guiding element may be used to evenly distribute the flow around the walls of tube 155. In some embodiments, the gas flow may further help evacuating some of the heat created during the curing process.
  • system 100 may further include fiber collecting system 160.
  • Fiber collecting system 160 may include a winding system 168 and at least one sensor for measuring dimensions of the fiber.
  • Exemplary sensors may include diameter sensor 164 and/or length and speed sensor 166.
  • fiber collecting system 160 may include capstan 162.
  • Capstan 162 may include any device for locking and guiding the cured fiber and allowing tension to be applied on the cured fiber to wind it properly. Following the UV irradiance the mixture stream may be still in a semi solid condition, thus may not withstand direct tension without a buffer system like the capstan.
  • Capstan 162 may include rollers that may be controlled to spin at a rotational velocity correlated to the stream velocity. The capstan velocity may be 1 -2% lower than the stream velocity in order not to create tension on the semi-solid fiber.
  • the center of the rollers may be aligned with the injecting nozzle's center. Controller 170 may control the rollers position relative to the mixture injection line using a precision camera. The control may adjust the fiber fall direction in the capstan area.
  • Diameter sensor 164 may include any diameter measuring device, for example, a laser based 2 axis measuring head.
  • the diameter data collected may be stored in a database for quality control, for example, a database associated with controller 170. Controller 170 may further adjust the mixture stream velocity to minimize diameter error (higher velocity may result in a larger diameter that may be closer to the spinneret nominal diameter).
  • Length and speed sensor 166 may include, for example, a Doppler laser measuring device for monitoring the produced length and the real time and average velocity of the fiber production.
  • sensor 166 may include a mechanical roller measuring device.
  • Winding system 168 may include any system for collecting and winding fibers during the production process.
  • winding system 168 may include a tension controlled winding system to collect the fiber on spools.
  • system 168 may include a linear layering component.
  • system 100 may include controller 170 for controlling one or more components of the system.
  • Controller 170 may include a processor (e.g., a CPU, microcontroller, programmable logic controller (PLC) and the like), a non-transitory memory for storing codes that when executed by the processor perform methods according to embodiments of the invention.
  • Controller 170 may be associated with a user interface (e.g., a graphical user interface) that may include any devices that allow a user to communicate with the controller.
  • a user interface e.g., a graphical user interface
  • Embodiments of the invention may include an article such as a computer or processor non-transitory readable medium, or a computer or processor non-transitory storage medium, such as for example a memory, a disk drive, or a USB flash memory, encoding, including or storing instructions, e.g., computer-executable instructions, which, when executed by a processor or controller, carry out methods disclosed herein.
  • an article such as a computer or processor non-transitory readable medium, or a computer or processor non-transitory storage medium, such as for example a memory, a disk drive, or a USB flash memory, encoding, including or storing instructions, e.g., computer-executable instructions, which, when executed by a processor or controller, carry out methods disclosed herein.
  • the storage medium may include, but is not limited to, any type of disk including floppy disks, optical disks, compact disk read-only memories (CD-ROMs), rewritable compact disk (CD-RWs), and magneto-optical disks, semiconductor devices such as read-only memories (ROMs), random access memories (RAMs), such as a dynamic RAM (DRAM), erasable programmable read-only memories (EPROMs), flash memories, electrically erasable programmable read-only memories (EEPROMs), magnetic or optical cards, or any type of media suitable for storing electronic instructions, including programmable storage unit.
  • ROMs read-only memories
  • RAMs random access memories
  • DRAM dynamic RAM
  • EPROMs erasable programmable read-only memories
  • EEPROMs electrically erasable programmable read-only memories
  • magnetic or optical cards or any type of media suitable for storing electronic instructions, including programmable storage unit.
  • Controller 170 100 may include, for example, a personal computer, a desktop computer, a mobile computer, a laptop computer, a notebook computer, a terminal, a workstation, a server computer, a tablet computer, a network device, or any other suitable computing device.
  • a personal computer a desktop computer
  • a mobile computer a laptop computer
  • a notebook computer a terminal
  • a workstation a server computer
  • a tablet computer a network device, or any other suitable computing device.
  • controller 170 may control pumping system 120 to supply mixture from tank 110 to spinneret 140 at a flow rate that causes the mixture to be injected from the spinneret at a minimal desired velocity. In some embodiments, controller 170 may further control the one or more controllable UV source 150 to apply the UV radiation to the mixture stream leaving spinneret 140 when the mixture stream reaches the minimal desired velocity. In some embodiments, controller 170 may further control the pumping system to supply mixture from tank 110 to spinneret 140 at a flow rate that causes the mixture to be injected from the spinneret at velocity lower than a maximal velocity.
  • the minimal and maximal desired velocities may be determined based on: a diameter of a fiber, properties of the mixture, parameters of controllable UV source 150, operation parameters of pumping system 120 and design parameters of spinneret 140.
  • controller 170 may be configured to determine a mixture flow velocity range in a system for preparation of a polymer fiber (e.g., system 100), for receiving a polymer fiber with desired properties based on the above parameters, as will be discussed with respect to Fig. 3.
  • controller 170 may further be configured to control pumping system 120 to supply mixture from tank 110 to spinneret 140 at a flow rate range such that a velocity of the mixture injected from spinneret 140 may be kept between the minimal velocity and the maximal velocity.
  • controller 170 may further control various other aspects of system 100.
  • controller 170 may control the temperature and mixing in tank 110.
  • the controller may receive temperature measurements from a thermometer located inside or attached to tank 110 and may further control a heating element and/or cooling system included in tank 110 to control the temperature of the mixture in the tank to be at a desired temperature range.
  • controller 170 may control operation parameters of pumping system 120. Controller 170 may control the flowrate at which the mixture is supplied from pump 122 to spinneret 140, the pressure built by pumping system 120 in valve 130, for example, 2-10 bar, and the temperature of the mixture inside pumping system 120.
  • controller 170 may further control valve 130 to supply the mixture to spinneret 140 at a specific timing, for example, when sufficient pressure has been built by pumping system 120 as to cause a continuous flow of mixture in spinneret 140.
  • controller 170 may further be configured to open controllable shutter 154 and allow UV radiation to reach the mixture stream when the mixture stream injected from spinneret 140 reached the minimal velocity. Additionally or alternatively controller 170 may further be configured to operate a switch included in controllable UV source 150 and cause UV lamp 152 to radiate UV radiation when the mixture stream injected from spinneret 140 reached the minimal velocity. In some embodiments, controller 170 may further control the timing of the gas application and gas fiowrate (e.g., capacity) from gas supply system 156. For example, controller 170 may cause system 156 to supply gas (e.g., nitrogen) at a capacity of 5-15 liters/minute.
  • gas e.g., nitrogen
  • controller 170 may further be configured to control one or more UV lamps 152 included in UV source 150. Controller 170 may control the irradiance (e.g., the power at which the UV is applied) and the number and location (e.g., selection) of UV lamps 152 to be activated when more than two lamps 152 are included in UV source 150.
  • Controller 170 may control the irradiance (e.g., the power at which the UV is applied) and the number and location (e.g., selection) of UV lamps 152 to be activated when more than two lamps 152 are included in UV source 150.
  • Fig. 2 is a flowchart of an exemplary method of preparing a polymer fiber according to some embodiments of the invention.
  • Embodiments of the method of Fig. 2 may be performed for example by system 100 or by another system.
  • the method may include pumping a mixture of monomers and/or oligomers from a tank to a spinneret.
  • controller 170 may instruct pumping system 120 to pump the mixture from tank 110 to spinneret 140.
  • the mixture may include monomers and/or oligomers of a polymer (or polymers) for fabricating fibers, for example, acrylates.
  • the mixture may further include photoinitiators that absorb the UV radiation and cause the crosslinking and curing of the mixture.
  • the amount of photoinitiators in the mixture may vary between 0.05 and 5 percent. The higher the amount of photoinitiators in the mixture the higher is the reactivity of the mixture. The reactivity of the mixture may affect the progress and velocity of the curing reaction.
  • the pumping operation may include pumping at least two mixtures of monomers from two tanks to a spinneret comprising a plurality of nozzles.
  • system 100 may include two or more tanks 110 each holding a different mixture and pumping system 120 may pump and supply each mixture to spinneret 140 such that each mixture is injected from a different group of nozzles.
  • the method may include pumping at least two mixtures of monomers from two tanks 100 to a spinneret (e.g., spinneret 140A illustrated in Fig. 7) comprising coaxial nozzles (i.e. the first nozzle is coaxially located inside the second nozzle), such that a first mixture may be injected from a first nozzle and a second mixture may be injected from a second nozzle (see, for example, Fig. 7) forming multilayered fiber.
  • spinneret e.g., spinneret 140A illustrated in Fig. 7
  • coaxial nozzles i.e. the first nozzle is coaxially located
  • the method may include pumping a monomer mixture from a tank and supplying an oxygen free protective gas to a spinneret comprising a coaxial nozzle, such that the gas is injected from a first nozzle and the mixture is injected from a second nozzle, for forming a hollow fiber.
  • the method may include increasing the flow rate until a stream of monomer mixture injected from the spinneret reaches at least a minimal velocity.
  • Controller 170 may control pumping system 120 to increase the pressure and the fiowrate until the desired velocity is reached.
  • a minimal velocity value may be determined and by controller 170 based on : a diameter of the fiber, properties of the mixture, parameters of the controllable UV source, operation parameters of the pumping system and design parameters of the spinneret, as discussed with respect to the method of Fig. 3.
  • Fig. 3 is a flowchart of a method of determining a mixture flow velocity range in a system for preparation of a polymer fiber, for receiving a polymer fiber with desired properties.
  • the dashed lines in Fig. 3 connect each parameter and/or property to at least one velocity value that may be determined based on that parameter and/or property.
  • Embodiments of the method of Fig. 3 may be performed by controller 170 or any other controller.
  • the method may include receiving data indicative of the formulation of the mixture.
  • the data may include the chemical composition of the mixture, a code identifying the mixture or the like.
  • the data may be received from a user, via a user interface, may be read automatically by system 100, using a reader (e.g., a barcode reader) or by any other means.
  • the data may be related to properties of the mixture, stored in a database associated with controller 170. Such properties may include: a reactivity of the mixture and viscosity of the mixture or the like. Exemplary properties of a mixture may include a viscosity (e.g. 800 cP) and reactivity (e.g. very high).
  • the method may include receiving a desired diameter of the fiber.
  • the desired diameter for example, 1 mm, 500 microns, 100 microns, 1 micron, or the like, may be received from a user, via the user interface.
  • the method may include receiving operation parameters of a pumping system included in the system for preparation of a polymer fiber.
  • the operation parameters of the pumping system e.g., pumping system 120
  • the operation parameters of the pumping system may include the minimum flowrate and the maximum pressure that may be produced by the pumping system.
  • Exemplary operation parameters may include a fiowrate of 2 mm/minute and a pressure of 200 bars.
  • the operation parameters may be stored and received from a database associated with controller 170. Alternatively the operation parameters may be received from a user via a user interface.
  • the method may include receiving design parameters of a spinneret included in the system for preparation of a polymer fiber.
  • the design parameters of the spinneret may include geometrical dimensions of the spinneret, for example, a length to diameter ratio of the nozzle and surface roughness values of one or more surfaces of the spinneret, for example, an outer surface area around an exit of the nozzle, as disclosed with respect to Fig. 6.
  • Exemplary design parameters of the spinneret may include a length to diameter ratio of the nozzle of 7:1 and surface roughness value N4 (0.01 mm) at the outer surface area around an exit of the nozzle.
  • the method may include receiving parameters of a controllable UV source included in the system for preparation of a polymer fiber.
  • Such parameters may include the irradiance (amount of radiation) of the UV source (e.g., source 150), the amount of undesired IR radiation from the UV source, the length of the UV lamp (e.g., lamp 152) and the number of UV lamps included in the UV source, or the like.
  • Exemplary parameters of the UV source may include irradiance of 100 mJ/cm 2 and a single 50 cm long UV mercury lamp- H spectrum.
  • controller 170 may receive updated information regarding at least some of the parameters of UV source 150. For example, aging of lamp 152 may result in a decrease in the irradiance of source 150.
  • the method may include selecting a lower limit for the velocity range.
  • the lower limit may be highest from 4 velocities and the method may include determining/calculating the 4 velocities in operations 362-368.
  • the method may include determining a curing reaction progression velocity based on a reactivity of the mixture (e.g., the amount of photoinitiators) and the parameters of the controllable UV source (e.g., the irradiance of the UV source). The progression of the reaction depends on how reactive the mixture and what is the UV dose applied to the mixture.
  • the curing reaction progression velocity may be calculated or may be experimentally found for various mixtures and various UV doses and may be further saved in a lookup table stored in a database (e.g., a memory) associated with controller 170. If the stream velocity is lower than the curing reaction progression velocity the reaction may progress towards the spinneret, curing the mixture inside the spinneret thus blocking the spinneret.
  • a database e.g., a memory
  • the method may include determining an overheating velocity of the fiber based on the fiber's diameter, the reactivity of the mixture and the parameters of the controllable UV source (e.g., IR radiation).
  • the curing reaction is an exothermic reaction producing heat.
  • lamp 152 is mercury based UV lamp, it may produce an undesired IR radiation that may cause the fiber to overheat, thus may cause evaporation of material from the mixture. Low velocity may cause longer exposure to IR and UV radiations and may further raise the temperature of the fiber.
  • the overheating velocity may be determined experimentally by measuring the fiber's temperature at the exit of the curing area for different velocities, fiber diameters, parameters of the controllable UV source and mixtures, and determining a minimal velocity for which the temperature of the fiber may be acceptable such that the fiber's properties may not be damaged.
  • the method may include determining a minimal velocity for receiving stable flow based on viscosity and viscoelasticity of the mixture, the design parameters of the spinneret and the fiber's diameter.
  • a minimum velocity may be required to achieve a stable fully developed flow at the outlet from the spinneret, resulting in a stable stream that has the form of the spinneret's cross section.
  • the velocity may have to be high enough such that the inertial forces in the mixture stream that result from the injection from the spinneret may dominant over the viscos forces and gravity.
  • the result may be a stable continuous stream having a uniform and homogenous cross section (e.g., a fiber having a constant diameter) and not in a mixture cone that is drawn by gravity or flow with vortices and separations.
  • the minimum velocity may be a function of viscosity (or viscosity profile over time if the material is viscoelastic), the spinneret design parameters and the fiber' s diameter.
  • the spinneret design parameters may include length to diameter ratio, opening angle, radiuses, shear, and surface roughness.
  • the velocity may be determined experimentally by flow test without curing.
  • the minimal velocity for receiving stable flow may be the dominant parameter to set the minimal velocity of the system.
  • the method may include determining a velocity related to a minimal flow rate based on operation parameters of the pumping system and the fiber's diameter.
  • the minimal flow rate velocity may be derived from the minimum constant flow rate that the pumping system (e.g., system 120) may generate according to its mechanical limitations, and the required fiber's diameter.
  • the velocity may be calculated based on the following equation:
  • the method may include selecting an upper limit for the velocity range to be the lowest from the following 3 velocities and the method may include determining/calculating the 3 velocities in operations 372-376.
  • the method may include determining a velocity that causes insufficient curing based on the reactivity of the mixture, the parameters of the controllable UV source and the fiber's diameter.
  • each portion of the mixture steam may have to be exposed to a minimum UV radiation dose in the curing area to achieve sufficient curing and formation of a solid fiber.
  • the required dose is a function of composition of the mixture and the diameter of the fiber and may be calculated and determined experimentally.
  • the UV dose applied to each portion of the stream during the curing process is measured in energy units and calculated by:
  • the irradiance is known and the exposure time is a function of the length of the lamp L and the streams velocity V:
  • the method may include determining a minimal velocity that may cause unstable flow based on the viscosity and viscoelasticity of the mixture, the fiber' s diameter and the design parameters of the spinneret.
  • curing the mixture stream into a fiber may require the flow of the mixture to be laminar.
  • the method may include determining a velocity that may cause over pressure based on the viscosity and viscoelasticity of the mixture, operation parameters of the pumping system and design parameters of the spinneret.
  • the stream's velocity and the stream/fiber diameter may determine the constant flow rate that may be supplied by the pump. Since the spinneret may have a small nozzle diameter (e.g., 1 mm or less) and relatively high length to diameter ratio (e.g., higher than 1 :1) in addition to the high viscosity of the mixture (e.g., 800 cP), all these parameters may result in a pressure rise inside the spinneret. This pressure should be kept under a pressure limit of the most pressure sensitive component, for example, under 200 bar.
  • the method may further include receiving updated inputs related to at least one of: data indicative of the formulation of the mixture, the diameter of the fiber, the operation parameters of the pumping system and the parameters of the controllable UV source.
  • the updated inputs may be received from sensors and/or detectors associated with various components of the system, for example, flow meters or pressure sensors associated with the pumping system, thermometers associated with the tank and irradiance sensors associated with the controllable UV source.
  • the sensors and/or detectors may send signals to controller 170 updating the data related to the above parameters.
  • the updated inputs may be received continuously, every predetermined period of time, during predetermined time in the process (e.g., the beginning of each production) or the like.
  • the method may include updating the lower limit for the velocity range accordingly. In some embodiments, the method may include updating the upper limit for the velocity range accordingly.
  • operation 220 may further include increasing the flow rate until a first monomer mixture may be injected from the spinneret at least at the minimal velocity from a first group of nozzles from a plurality of nozzles and a second monomer mixture may be injected from the spinneret at least at the minimal velocity from a second group of nozzles from the plurality of nozzles.
  • Spinneret 140 may include at least two groups of nozzles and controller 170 may cause pumping system 120 to pump at least two types of mixtures from at least two different tanks 110 and inject each type of mixture to a different set group of nozzles to form different type of fibers.
  • the each group of nozzles may include one or more nozzles.
  • the method may include applying UV radiation to cure the stream of the mixture of monomers injected from the spinneret.
  • controller 170 may control controllable UV source 150 to apply UV radiation to the mixture stream only after the stream has a velocity higher than each one of the 4 velocities determined in operations 362-368 of the method of Fig. 3.
  • the controller may open shutter 154 (e.g., when lamp 152 is a mercury lamp) or switch on the power to lamp 152 (e.g., when lamp 152 is a LED UV lamp).
  • controller 170 may cause pumping system 120 to further increase the flow rate.
  • operation 240 may include applying UV radiation to cure streams of mixture of monomers injected from the spinneret only after all the mixture streams injected reached the minimal velocity.
  • the method may include controlling the flowrate such that the mixture may be injected from the spinneret at velocity lower than a maximal velocity.
  • the maximal velocity may be determined in a similar way to determining the upper limit velocity in operation 370 of the flowchart of Fig. 3.
  • the maximal velocity may be determined as the lowest of the velocities determined in operations 372-376 of the method of Fig. 3.
  • the method may include controlling the flowrate such that the mixture stream velocity is kept between the minimal velocity and maximal velocity.
  • the method of Fig. 2 may further include controlling the timing at which the monomer mixture stream is injected from the spinneret.
  • Controller 170 may control valve 130 to timely open and allow mixture to flow from pumping system 120 to spinneret 140, for example, when the pressure of the mixture reached 5-10 bars.
  • FIG. 4A is an illustration of an exemplary polymer fibers preparation system according to some embodiments of the invention.
  • Fig. 4A illustrates an exemplary assembly of some of the components of system 100 that were diagrammatically represented in the boxes of Fig. 1.
  • System 100 may include one or more tanks 110 for holding a monomers or oligomers mixture.
  • the mixture may be pumped from tank 110 by pumping system 120 to an injection system 135 which includes valve 130 and spinneret 140. From spinneret 140 the mixture may be injected to a volume within UV transparent tube 155.
  • the injected mixture may have a form of a stream or a jet progressing along the longitudinal axis of tube 155.
  • UV radiation from lamp 152 may penetrate UV transparent tub 155 to cure the mixture stream inside the tube.
  • the as cured fiber may be locked and guided by capstan 162 before winding by winding system 168.
  • the diameter of the fiber may be measured by diameter sensor 164.
  • Fig. 4B is an enlarge illustration of the area marked with an ellipsoid in Fig. 4A.
  • Fig 4B shows in greater details the location of some elements of system 100 with respect to each other.
  • Fig. 4B further shows the position of shutter 154, when shutter 154 is located in at the exit from spinneret 140, shuttering the mixture stream from UV radiation source 152.
  • Injection system 135 may include valve 130, a spinneret housing 142, spinneret 140 and a spinneret fixation bolt 144.
  • Exemplary system 135 may further include a shutter 154 located in proximity to spinneret 140 exit 148 and configured to block the mixture stream leaving the spinneret from UV radiation from the UV lamp.
  • Shutter 154 may include a shutter blocking element 184 that may be connected to a shutter servo motor 158 for moving shutter blocking element 184 from and to a shutter frame 159 include in shutter housing 158 (illustrated in Fig. 8) to open or close the shutter.
  • Injecting system 135 may further include a gas guiding element of gas supply system 156 and a gas inlet housing 157 for directing oxygen free atmosphere to protect the stream mixture injected from the spinneret from the presence of oxygen.
  • Fig. 6 is an illustration of a spinneret for preparing a polymer fiber according to some embodiments of the invention.
  • Embodiments of spinneret 140 may include a hollow truncated cone 146 and a nozzle 147 having a length (L) to diameter (D) ratio of at least 1 :1.
  • spinneret 140 may include a hollow truncated cone 146 and a nozzle 147 having a length (L) to diameter (D) ratio of between 1 :1 to 10:1.
  • the Nozzle 147 may be coaxially connected at a truncated end 145 of cone 146.
  • an outer surface area around an exit 148 of nozzle 147 may have at most 0.2 microns (N4) surface roughness.
  • nozzle 147 may be smoothly connected to the truncated end of the cone 146 such that a mixture flows uninterruptedly inside spinneret 140. For example, the connection may allow maintaining a stable flow in spinneret 140.
  • this invention provides a spinneret for preparing a polymer fiber, comprising: a hollow truncated cone; and a nozzle having a length to diameter ratio of at least 1, coaxially connected at a truncated end of the cone, wherein an outer surface area around an exit of the nozzle has at most 0.2 microns (N4) surface roughness.
  • hollow truncated cone 146 may have an opening angle a.
  • Angle a may be determined based on at least one of: a viscosity of the mixture stream flowing in the spinneret and the minimal velocity of the mixture stream injected from the spinneret. Methods of determining the minimal velocity were widely discussed with respect to Figs. 2 and 3, for example, in operations: 220, 360-368.
  • nozzle 147 may have a length (L) to diameter (D) ratio of at least 1 :1, of example, 2:1, 3:1 , 4:1, 5:1, 6:1 , 7:1, 8:1, 10:1 or more.
  • the LTD may be determined to ensure a stable flow of mixture stream from the spinneret to form a solid fiber.
  • an inner surface area 149 of nozzle 147 may have at most 0.2 microns (N4) surface roughness.
  • surface area 149 may have at most 0.1 microns (N3) surface roughness.
  • nozzle 147 may have an inner parallelity of at least 0.02 mm in comparison to an outer wall of spinneret 140.
  • the inner parallelity may be measured by visual inspection of a parallelity measuring insert, inserted into the spinneret such that an end of the insert extends beyond exit 148 and the parallelity of the extended end can be visually compared to the parallelity of the spinneret's outer walls using comparison standards.
  • the outer surface area around exit 148 of nozzle 147 may have at most 0.1 microns (N3) surface roughness.
  • the fine surface roughness of the outer surface area around exit 148 may be determined to allow smooth and continuous flow from exit 148 with no disconnections that may result from obstacles on the surface near the exit that may "catch" or disturb the flow coming from the spinneret.
  • the spinneret may include a plurality of hollow truncated cones 146 and a plurality of nozzles 147 having a length to diameter ratio of at least 1:1.
  • each of nozzles 147 may be coaxially connected at a truncated portion 145 for a corresponding cone 147.
  • Such a spinneret may inject simultaneously a plurality of mixture streams to be cured (e.g., by UV system 150) to form a plurality of fibers.
  • the plurality of nozzles 147 and corresponding cores 146 may be divided into two or more groups. Each group may be connected or fed with a different type of mixture (e.g., different formulation). Each group may be in fluid communication with different feeding system.
  • the plurality of hollow truncated cones 146 are coaxially located one inside the other and wherein the plurality of nozzles 147 are coaxially located one inside the other such that a single nozzle 147 is connected at each truncated end 145 of each cone 146.
  • Fig. 6 is an illustration of an exemplary coaxial spinneret according to some embodiments of the invention.
  • Coaxial spinneret 140A may include a first truncated cone 146A coaxially located inside a second truncated cone 146B and a first nozzle 147A coaxially located inside second nozzle 147B such that first nozzle 147 A may be connected at the truncated end of first cone 146 A and second nozzle 147B may be connected at the truncated end of second cone 146B.
  • first nozzle 147 A may be connected at the truncated end of first cone 146 A and second nozzle 147B may be connected at the truncated end of second cone 146B.
  • the two cones and two nozzles illustrated in Fig. 7, are given as an example only and that the invention as a whole is not limited to two cones and two nozzles. Any number of cone and corresponding number of nozzles may be included in a spinneret according to embodiments of the invention.
  • spinneret 140A may include 3 truncated cones and 3 nozzles, 4 truncated cones and 4 nozzles, 5 truncated cones and 5 nozzles, 7 truncated cones and 7 nozzles, or more.
  • Fig. 8 is an illustration of a top view of a shutter for blocking UV radiation according to some embodiments of the invention.
  • Shutter 154 may include shutter housing 185, shutter servo motor 158, shutter frame 159 and a blocking element collecting cup 186.
  • Shutter 154 may be a mechanical shutter located at the exit of spinneret 140, such that when the shutter is closed the UV radiation is blocked from reaching spinneret 140.
  • Controller 170 may control servo motor 158 to move blocking element collecting cup 186 to block the path of the UV radiation by blocking the mixture stream from entering the UV transparent tube (e.g., tube 155).
  • Blocking element collecting cup 186 has a small collecting area that can contain a small amount of mixture (e.g., 1-8 cc), such that when the injection process starts, the shutter is in a closed position until the minimal velocity is reached.
  • controller 170 may control servo motor 158 to open element 184.
  • the stream of mixture may be collected by the cup included in element 184.
  • shutter 154 may be immediately closed upon the end of the injection to prevent polymerization of the mixture left in spinneret 140.
  • shutter 154 may be made of materials that are heat resistant to heat from mercury UV lamps, chemically resistant and has relatively light weight, as not to overload the servo, for example, housing 185, frame 159 and element 184 may be made from Aluminum Alloys.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

Cette invention se rapporte à un système de préparation de fibres polymères, et à un procédé de préparation de la fibre polymère à l'aide du système, le système comprenant une filière et une source d'UV située à proximité d'une sortie de la filière.
PCT/IL2016/050602 2016-06-09 2016-06-09 Procédé et système pour la préparation de fibres polymères WO2017212465A1 (fr)

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Publication number Priority date Publication date Assignee Title
WO2021066031A1 (fr) * 2019-09-30 2021-04-08 日東電工株式会社 Fibre optique en plastique
WO2022082040A1 (fr) * 2020-10-16 2022-04-21 Indizen Optical Technologies S.L. Création de verre de lunettes à l'aide de techniques additives avec une lumière diffuse
CN116163027A (zh) * 2022-12-30 2023-05-26 华南理工大学 一种水凝胶纤维及其制备与应用
WO2023111758A1 (fr) * 2021-12-15 2023-06-22 Aladdin Manufacturing Corporation Systèmes et procédés de production d'un faisceau de filaments et/ou d'un fil

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US3303530A (en) * 1965-01-13 1967-02-14 Du Pont Spinnerette
US5827611A (en) * 1997-03-10 1998-10-27 Hoechst Celanese Corp Multilayered thermoplastic article with special properties
WO2001020064A1 (fr) * 1999-08-19 2001-03-22 Jeong Sik Kim Buse de filage, raccord de filage recevant cette buse et procede de fabrication
WO2012156896A1 (fr) * 2011-05-18 2012-11-22 Palchik Oleg Fibres thermodurcies et thermoplastiques et leur préparation par durcissage par uv

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Publication number Priority date Publication date Assignee Title
US3303530A (en) * 1965-01-13 1967-02-14 Du Pont Spinnerette
US5827611A (en) * 1997-03-10 1998-10-27 Hoechst Celanese Corp Multilayered thermoplastic article with special properties
WO2001020064A1 (fr) * 1999-08-19 2001-03-22 Jeong Sik Kim Buse de filage, raccord de filage recevant cette buse et procede de fabrication
WO2012156896A1 (fr) * 2011-05-18 2012-11-22 Palchik Oleg Fibres thermodurcies et thermoplastiques et leur préparation par durcissage par uv

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021066031A1 (fr) * 2019-09-30 2021-04-08 日東電工株式会社 Fibre optique en plastique
US11747551B2 (en) 2019-09-30 2023-09-05 Nitto Denko Corporation Plastic optical fiber
WO2022082040A1 (fr) * 2020-10-16 2022-04-21 Indizen Optical Technologies S.L. Création de verre de lunettes à l'aide de techniques additives avec une lumière diffuse
CN114761441A (zh) * 2020-10-16 2022-07-15 因迪森光学技术公司 使用带有漫射光的增材技术制作眼镜镜片
US11633907B2 (en) 2020-10-16 2023-04-25 Indizen Optical Technologies S.L. Eyewear lens creation using additive techniques with diffuse light
CN114761441B (zh) * 2020-10-16 2024-05-07 因迪森光学技术公司 使用带有漫射光的增材技术制作眼镜镜片
WO2023111758A1 (fr) * 2021-12-15 2023-06-22 Aladdin Manufacturing Corporation Systèmes et procédés de production d'un faisceau de filaments et/ou d'un fil
CN116163027A (zh) * 2022-12-30 2023-05-26 华南理工大学 一种水凝胶纤维及其制备与应用
CN116163027B (zh) * 2022-12-30 2024-05-03 华南理工大学 一种水凝胶纤维及其制备与应用

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