WO2019027104A1 - Procédé de filage par voie humide assisté par paramètre électrique - Google Patents

Procédé de filage par voie humide assisté par paramètre électrique Download PDF

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Publication number
WO2019027104A1
WO2019027104A1 PCT/KR2017/013965 KR2017013965W WO2019027104A1 WO 2019027104 A1 WO2019027104 A1 WO 2019027104A1 KR 2017013965 W KR2017013965 W KR 2017013965W WO 2019027104 A1 WO2019027104 A1 WO 2019027104A1
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Prior art keywords
spinning
polymer
spinning solution
fiber
solution
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PCT/KR2017/013965
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English (en)
Korean (ko)
Inventor
유웅열
양호성
한흥남
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서울대학교산학협력단
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Priority to JP2020505201A priority Critical patent/JP7122770B2/ja
Publication of WO2019027104A1 publication Critical patent/WO2019027104A1/fr

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet 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
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus

Definitions

  • the present invention relates to a wet spinning method capable of producing a polymer fiber having improved mechanical properties.
  • the production of dense, defect-free precursor fibers is essential for producing high strength, high-resilience carbon fibers, and the degree of densification of the precursor fibers is primarily determined by the state of the coagulated filaments passing through the coagulating bath It is a property. Therefore, it is required to minimize the voids while increasing the homogeneity of the coagulated yarn during the coagulation step.
  • wet spinning is mainly used because it provides a high coagulation speed, is excellent in productivity, can maintain a relatively low viscosity and a process temperature, and minimizes changes in physical and chemical form of the additive.
  • Another object of the present invention is to provide a polymer fiber produced by using an electric variable wet spinning method.
  • An object of the present invention is to provide a method of manufacturing a polymer electrolyte membrane, which comprises ionizing a spinning solution containing a polymer and a solvent by applying a voltage to the spinning solution; Spinning the ionized spinning solution into a coagulating liquid to obtain coagulation; And stretching the coagulum to form a polymer fiber.
  • the present invention provides an electric variable wet spinning method comprising:
  • the step of ionizing the spinning solution by applying a voltage to the spinning solution containing the polymer and the solvent may include applying a voltage to the upper and lower ends of the spinning solution reservoir by connecting a power source of different polarity before spinning have.
  • the voltage applied to the spinning solution may range from 40 to 1000V.
  • the current generated in the spinning solution to which the voltage is applied may be 50 to 3000 ⁇ A.
  • the polymer may include a polymer having a repeating unit derived from a monomer having a group capable of forming an ion.
  • the polymer may be selected from the group consisting of polyacrylonitrile (PAN) homopolymer, polyacrylonitrile copolymer, polyvinyl alcohol (PVA) homopolymer, polyvinyl alcohol copolymer, polyvinyl chloride A polymer, a polyvinyl chloride copolymer, and rayon, or a mixture of two or more thereof.
  • PAN polyacrylonitrile
  • PVA polyvinyl alcohol
  • PVC polyvinyl alcohol copolymer
  • the group capable of forming an ion may include a carboxylic acid group (-COOH), a nitrile group (-CN), a hydroxy group (-OH), and a halogen group (-X) May be selected.
  • the polyacrylonitrile copolymer comprises repeating units derived from acrylonitrile; And a repeating unit derived from a monomer which weakens the bonding force of the nitrile period of the acrylonitrile.
  • the step of spinning the ionized spinning solution into the coagulating liquid to obtain coagulation may include the step of increasing the amount of the ionized polymer in the spinning solution to promote exchange of the solvent in the spinning solution and the non-solvent in the coagulating solution . ≪ / RTI >
  • Another object of the present invention is achieved by the provision of the polymer fibers produced by the electric variable wet spinning method.
  • the polymer fiber may be any one or a mixture of two or more of polyacrylonitrile fiber, polyvinyl alcohol fiber, polyvinyl chloride fiber and rayon fiber.
  • the polymer fiber may have a strength of 200 MPa or more, an elastic modulus of 6 GPa or more, and an elongation of 6% or more as measured according to ASTM D3822-07.
  • the solvent can be easily removed through the coagulation bath, thereby greatly reducing the size of the conventional wet spinning process .
  • FIG. 1 is a flowchart illustrating a method of manufacturing a polymer fiber using an electric variable wet spinning method according to an embodiment of the present invention. Referring to FIG. 1
  • FIG. 2 is a schematic cross-sectional view of a wet spinner according to an embodiment of the present invention.
  • FIG. 3 is a TGA (thermogravimetric analysis) graph of the sample according to Example 1 and Comparative Example 1.
  • FIG. 4 is a graph showing the strain-breaking strength characteristics of the sample according to Example 1 and Comparative Example 1.
  • FIG. 4 is a graph showing the strain-breaking strength characteristics of the sample according to Example 1 and Comparative Example 1.
  • FIG. 6 is a SAXS pattern photograph of a sample according to Example 1.
  • FIG. Like reference numerals refer to like elements throughout the specification.
  • well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail.
  • the terms first, second, etc. in this specification are used to distinguish one element from another element, and the element is not limited by the terms.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a polymer fiber using an electric variable wet spinning method according to an embodiment of the present invention. Referring to FIG. 1
  • a method of manufacturing a polymer fiber using an electric variable wet spinning method includes a step of applying a voltage to a spinning solution (S110), a spinning solution wet spinning step (S120) S130), a drying step (S140), and a winding step (S150).
  • the step of applying voltage to the spinning solution applies a voltage to the spinning solution before spinning spinning solution for fiber formation into the coagulating solution. This means applying a voltage to the spinning solution before it reaches the coagulating solution.
  • the spinning solution is a solution containing a polymer substance used as a starting material for fiber formation, and may also be named as spinning solution or spinning solution.
  • the spinning solution can be prepared by dissolving the polymer substance in a solvent.
  • the spinning solution may be a polymer solution.
  • a polymer material may be a known material used for ordinary precursor fibers without limitation, and preferably a polymer material used for precursor fibers for carbon fibers may be used.
  • the spinning solution of the present invention may comprise a polymer having a repeating unit derived from a monomer having a group capable of forming an ion.
  • the polymer contained in the spinning solution may include homopolymers or copolymers of polyacrylonitrile (PAN), homopolymers or copolymers of polyvinyl alcohol (PVA), polyvinyl chloride PVC), and rayon, and the like, or a mixture of two or more thereof.
  • PAN polyacrylonitrile
  • PAN has higher carbon yield after heat treatment and can preserve its orientation, so that it is more preferable from the viewpoint of high strength and high degree of manifestation of carbon fiber.
  • the polymer substance is ionized by the group capable of forming ions contained in the repeating unit of the polymer contained in the spinning solution, and the ionized polymer substance is oxidized / Current may be generated.
  • the monomer having a group capable of forming an ion contained in the spinning solution is not particularly limited as long as it is a substance capable of forming a negative (-) ion or a positive (+) ion.
  • the polyacrylonitrile (PAN) fiber used as the precursor of the carbon fiber imparts a very strong secondary bond between the polymer chains of the polyacrylonitrile constituting the fiber or between the repeating units derived from the acrylonitrile adjacent in the polymer chain
  • the nitrile group (-CN) prevents the arrangement of the polymer chains during spinning to form a helix structure and causes a cyclization reaction too rapid in the heat treatment.
  • a copolymer having a repeating unit derived from a polyacrylonitrile copolymer that is, a repeating unit derived from acrylonitrile and a monomer which weakens a bonding force between acrylonitrile and a nitrile group as a polymer of the spinning solution desirable.
  • the introduction of such a monomer prevents the lowering of the radioactivity due to the solubility problem, and it is possible to suppress the cyclization reaction too fast in the heat treatment.
  • examples of the monomer which weakens the bonding force between acrylonitrile and nitrile groups include methyl acrylate, itaconic acid, and methacrylic acid, and repeating from these monomers
  • the unit may be contained in the polymer in an amount of about 2% to 15% by weight.
  • the solvent contained in the spinning solution is not particularly limited as long as the fiber-forming polymer material is dissolved, and examples thereof include dimethylacetamide (DMA), dimethyl sulfoxide (DMSO), and dimethylformamide ) May be used.
  • DMA dimethylacetamide
  • DMSO dimethyl sulfoxide
  • -CN nitrile groups
  • PAN polyacrylonitrile
  • the kind, molecular weight, content, degree of polymerization, and the like can be appropriately selected in consideration of the target physical properties of the precursor fiber or carbon fiber to be produced.
  • the polymer concentration can be, for example, 15% by weight or more, preferably 15 to 30% by weight, more preferably 17 to 25% by weight.
  • FIG. 2 is a schematic cross-sectional view of a wet spinner according to an embodiment of the present invention.
  • a wet spinner 200 includes a spinning liquid reservoir 220, a pump 240, a die 250, a power supply 270, a plurality of rolls rolls 280a, 280b, and 280c, and a coagulating solution 260 are contained. Meanwhile, the coagulation bath 210 may further contain the spinning solution 230 radiated and the solvent inside the spinning solution 230 exchanged during the coagulation process.
  • the step of applying the voltage to the spinning solution 230 may be performed by connecting a voltage to the spinning solution storage tank 220 in which the spinning solution 230 before spinning is stored, through the power supply unit 270.
  • the step of applying voltage to the spinning solution 230 may be performed by supplying power of different polarities to the upper and lower ends of the spinning solution storage tank 220 through the power supply unit 270.
  • a power source having a polarity selected from the positive (+) and negative (-) polarities is supplied to the upper end of the spinning liquid reservoir 220 and the positive (+) and negative A predetermined voltage may be applied to the spinning solution 230.
  • a power source having a polarity opposite to the charge of the polymer ion of the spinning solution 230 is supplied to the lower end of the spinning solution storage tank 220.
  • the amount of the polymer ions to be collected in the coagulation bath 210 can be increased by increasing the amount of polymer ions collected at the lower end of the spinning liquid reservoir 220.
  • a negative (-) power is supplied to the upper end of the spinning solution reservoir 220 and an anode (-) is connected to the lower end of the spinning solution reservoir 220 + ≪ / RTI >
  • the spinning solution 230 of the present embodiment when a voltage is applied, a group capable of forming an ion contained in the monomer is ionized and the polymer becomes a negative charge or a positive charge, and then the oxidation of the ionized polymer A current is generated in the spinning solution 230 by the reduction reaction.
  • the polymer ions generated in the spinning solution 230 are moved and collected to the lower end of the spinning solution storage tank 220, that is, the spinneret 250, and are then introduced into the coagulation bath 210 by spinning of the spinning solution 230 .
  • the current generated in the spinning solution 230 by applying a voltage to the spinning solution reservoir 220 is adjusted according to the cross-sectional area of the portion to which the pole is connected (the cross-sectional area of the upper portion of the volume of the spinning solution and the cross- , Where the voltage may be approximately 40-1000 volts. If the voltage is less than 40 V, ion generation and trapping inside the spinning solution 230 may be insufficient. Conversely, if the voltage is excessively higher than 1000 V, the polymer and the solvent may be degraded.
  • the current generated in the spinning liquid 230 by the voltage takes about 20 to 30 seconds to converge to a constant value, and the fibers radiated until this time are not used.
  • the current value may be several tens to several thousands of microamperes, specifically, 50 to 3,000 microamperes.
  • the spinning liquid wet spinning step S120 is performed by applying a voltage to the ionized spinning solution 230 to the nozzles of the spinneret 250 using the pressure of the pump 240, (Not shown) to the coagulation bath 210 containing the coagulation liquid 260.
  • the pump 240 may be a piston pump connected to the spinning liquid storage tank 220 and discharging the spinning liquid 230 from the upper side to the lower side of the spinning liquid storage tank 220.
  • a voltage may be applied to the upper end of the spinning liquid reservoir 220 by applying a voltage to the pump 240.
  • the nip 250 is disposed under the spinneret reservoir 220 with a nozzle having a circular cross section and the nozzle of the nip 250 is buried at a position in the coagulation liquid 260. Further, a fine jet port (not shown) is provided on the back side of the nozzle. Accordingly, the spinning solution 230 can be discharged in the vertical direction with respect to the bottom surface of the coagulation bath 210.
  • Such detents 250 are preferably multi-die, which can reduce the breakage of fibers during spinning compared to a single die.
  • the coagulating solution 260 can be employed without limitation in a solution used for ordinary wet spinning.
  • the temperature of the coagulating solution 260 is 3 ° C to 50 ° C It is desirable to set it appropriately within the range.
  • the spinning solution 230 radiated into the coagulation bath 210 is extruded while passing through the coagulating solution 260 to form a coagulation product 290 solidified in a fibrous form.
  • the spinning solution 230 passes through the coagulating solution 260 while sequentially passing the traveling roll 280a and the pulling roll 280b disposed at one end and the other end of the wall surface of the coagulation bath 210, respectively.
  • a plurality of polymer ions generated in the spinning solution 230 and moved to the lower end side of the spinning solution reservoir 220 are collected in the coagulation bath 210 by applying a voltage to the spinning solution 230 before the spinning, I will enter.
  • the non-solvent in the coagulating solution 260 is diffused into the coagulating solution 290, exchange of the solvent in the coagulating solution 290 and the coagulating solution 260 in the coagulating solution 260 is promoted,
  • the solvent removal in the coagulation bath 290 can be remarkably improved during the coagulation process using the coagulation bath 210 equipped with the coagulation bath 210.
  • the stretching step S130 separates the coagulum 290 obtained through the coagulation process from the coagulating liquid 260 in the coagulation bath 210 containing the coagulating liquid 260 .
  • the stretching process may be performed by rotating the difference between the rotation speeds of the two stretching rolls 280c1 and 280c2 disposed outside the coagulation bath 210 by a factor of 1: It can be carried out at an elongation of 20 times.
  • the elongation is not particularly limited and can be appropriately selected in consideration of the target elastic modulus and the process temperature of the fiber to be produced.
  • the stretching process may be a hot stretching process using a water bath (not shown) which is heated to 70 ° C or higher, preferably 90 ° C.
  • the coagulation yarn 290 in the coagulation bath 210 can be drawn by the stretching roll 280c outside the coagulation bath 210 and stretched by the pulling rolls 280b in the coagulation bath 210 during the stretching process. Thereby, the coagulum 290 is stretched and the molecular chains are oriented in the fiber axis direction, so that the coagulum 290 having excellent elasticity can be obtained.
  • the coagulation liquid 260 diffused into the coagulation bath 290 facilitates removal of the solvent from the coagulation bath 290 through the coagulation bath 210, Cavitation and defect can be suppressed.
  • the coagulation (290) can minimize cavity formation and defects and improve mechanical properties such as strength, elastic modulus, and elongation.
  • the greatest variable controlling the nature of the coagulum 290 formed from the spinning solution 230 is the electrical variable introduced into the spinning solution 230.
  • the solvent in the coagulum 290 and the non-coagulant in the coagulating liquid 260 are promoted by the voltage applied to the spinning liquid 230 before the coagulation, 260, the removal rate of the solvent inside the coagulation bath 290 through the coagulation bath 210 is increased, so that a dense and uniform coagulum 290 can be produced at the time of stretching.
  • the coagulation yarn 290 having a reduced size of voids after stretching can be produced.
  • the stretching process may be performed simultaneously with washing (washing), or may be carried out before or after the washing step of the coagulum 290.
  • the coagulum (290) having been drawn is dried.
  • the drying process may be carried out using a drier at a temperature of 150 ° C or less, preferably 50 ° C to 150 ° C, and various methods known in the art may be used.
  • the dried coagulum 290 is wound up to finally complete the production of the polymer fiber.
  • the polymer fiber of the present embodiment manufactured by the above-described manufacturing method may be, for example, polyacrylonitrile (PAN) fiber, polyvinyl alcohol (PVA) fiber, polyvinyl chloride (PVC) Preferably polyacrylonitrile (PAN) fibers.
  • PAN polyacrylonitrile
  • PVA polyvinyl alcohol
  • PVC polyvinyl chloride
  • the polyacrylonitrile (PAN) fiber, the polyvinyl alcohol (PVA) fiber, and the polyvinyl chloride (PVC) fiber may be formed of the respective homopolymers or copolymers as described above.
  • the polymer fibers of the present embodiment have reduced pores and defects, so that their mechanical properties are improved.
  • the strength of each fiber is improved by 10% or more, in detail, 22% or more, 20% or more, in particular, 55% or more, and the elongation can be improved by 10% or more, in detail, 32% or more.
  • the polymer fibers of this embodiment can have a pore size that is reduced to a lower pore size, for example, less than 0.5 times, as compared to fibers prepared by conventional wet spinning.
  • the polymer fiber of the present embodiment has a strength measured according to ASTM D3822-07 of 200 MPa or more, an elastic modulus of 6 GPa or more, and an elongation of 6% or more.
  • the polymer fiber of the present embodiment can satisfy the range of the strength of 200 MPa to 2000 MPa, elastic modulus of 6 GPa to 20 GPa, and elongation of 6% to 30% or more measured according to ASTM D3822-07.
  • the polymer fibers of this embodiment can be used as precursor fibers for producing carbon fibers. As the mechanical properties are improved, the mechanical properties of the carbon fibers produced by using the polymer fibers as precursors can be improved.
  • PAN polyacrylonitrile
  • DMF dimethylformamide
  • a negative voltage line and a positive voltage line were attached to the upper and lower ends of the spinning liquid reservoir using a power supply, and a voltage of 60 V was applied for 30 seconds to apply a current of 100 ⁇ A to the spinning solution .
  • the upper and lower end cross-sectional areas of the volume occupied by the spinning liquid were 7.065 cm 2 and 1.766 cm 2, respectively.
  • the spinning solution was then wet-spun into a 25 ⁇ ⁇ coagulation solution containing 60% by weight of dimethylformamide (DMF) and 40% by weight of water. Thereafter, the resulting coagulum was stretched 5 times at a temperature of 90 ⁇ , dried at 100 ⁇ in a dryer, and wound into a polyacrylonitrile (PAN) fiber.
  • DMF dimethylformamide
  • PAN polyacrylonitrile
  • FIG. 3 is a TGA (thermogravimetric analysis) graph of the sample according to Example 1 and Comparative Example 1
  • FIG. 4 is a graph showing the strain-breaking strength characteristics of the sample according to Example 1 and Comparative Example 1 Graph.
  • the fibers of Example 1 exhibit a faster weight loss from around 50 ° C. to 140 ° C., but a slower weight loss after 150 ° C. .
  • the fiber of Comparative Example 1 is less substituted with the coagulating solution than the fiber of Example 1 and the solvent in the coagulum has more defects in the fiber finally obtained by the solvent remaining in the coagulum .
  • the fracture strength and strain (elongation) of the fibers of Example 1 increased by an average of 22% and 32%, respectively, as compared with the fibers of Comparative Example 1.
  • Fig. 5 is a SAXS (low angle X-ray scattering) pattern photograph of a sample according to Comparative Example 1
  • Fig. 6 is a SAXS pattern photograph of a sample according to Example 1.

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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)

Abstract

La présente invention concerne un procédé de filage par voie humide assisté par paramètre électrique. Un procédé de filage par voie humide assisté par paramètre électrique selon la présente invention comprend les étapes de : application d'une tension à une solution de filage contenant un polymère et un solvant pour ioniser la solution de filage ; filage de la solution de filage ionisée dans une solution de coagulation pour obtenir un filament coagulé ; et étirage du filament coagulé pour former une fibre de polymère, la solution de filage ionisée favorisant l'échange du solvant à l'intérieur du filament coagulé avec un non-solvant dans la solution de coagulation pour obtenir une fibre de polymère ayant des propriétés mécaniques améliorées.
PCT/KR2017/013965 2017-07-31 2017-11-30 Procédé de filage par voie humide assisté par paramètre électrique WO2019027104A1 (fr)

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Citations (5)

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KR930018065A (ko) * 1992-02-25 1993-09-21 나가이 야타로 아크릴 섬유 및 이의 제조방법
JP2714829B2 (ja) * 1988-12-01 1998-02-16 株式会社小松製作所 中空繊維膜の紡糸方法
JP2714854B2 (ja) * 1989-06-09 1998-02-16 株式会社小松製作所 曝気用中空糸の製造方法
JP2008013877A (ja) * 2006-07-06 2008-01-24 Kaneka Corp 染色性に優れたアクリル系合成繊維
KR20080096814A (ko) * 2006-03-03 2008-11-03 몬테피브레 에스.피.에이. 낮은 필링 형성의 직물을 위한 아크릴섬유의 생산 공정 및 그로부터 수득되는 아크릴섬유

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JP2002161430A (ja) 2000-11-29 2002-06-04 Kuraray Co Ltd 水溶性ポリビニルアルコール系繊維の製造方法
CN102102233B (zh) * 2010-12-17 2013-04-03 东华大学 一种聚丙烯腈基纳米碳纤维原丝的制备方法
JP2015183166A (ja) * 2014-03-26 2015-10-22 東レ株式会社 アクリロニトリル系共重合体およびポリアクリロニトリル系炭素繊維前駆体繊維、炭素繊維の製造方法

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
JP2714829B2 (ja) * 1988-12-01 1998-02-16 株式会社小松製作所 中空繊維膜の紡糸方法
JP2714854B2 (ja) * 1989-06-09 1998-02-16 株式会社小松製作所 曝気用中空糸の製造方法
KR930018065A (ko) * 1992-02-25 1993-09-21 나가이 야타로 아크릴 섬유 및 이의 제조방법
KR20080096814A (ko) * 2006-03-03 2008-11-03 몬테피브레 에스.피.에이. 낮은 필링 형성의 직물을 위한 아크릴섬유의 생산 공정 및 그로부터 수득되는 아크릴섬유
JP2008013877A (ja) * 2006-07-06 2008-01-24 Kaneka Corp 染色性に優れたアクリル系合成繊維

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JP7122770B2 (ja) 2022-08-22
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