WO2021097544A1 - Procédé d'obtention de fibres textiles à base d'oxyde de graphène et de polyester - Google Patents

Procédé d'obtention de fibres textiles à base d'oxyde de graphène et de polyester Download PDF

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Publication number
WO2021097544A1
WO2021097544A1 PCT/BR2020/050483 BR2020050483W WO2021097544A1 WO 2021097544 A1 WO2021097544 A1 WO 2021097544A1 BR 2020050483 W BR2020050483 W BR 2020050483W WO 2021097544 A1 WO2021097544 A1 WO 2021097544A1
Authority
WO
WIPO (PCT)
Prior art keywords
graphene oxide
polyester
particles
polymeric nanocomposite
dispersion
Prior art date
Application number
PCT/BR2020/050483
Other languages
English (en)
Portuguese (pt)
Inventor
Guilhermino José Macêdo FECHINE
Pablo Andrés Riveros MUNÕZ
Ricardo Jorge Espanhol Andrade
Tamíris de Oliveira LAMBERT
Claudio Rogério DINI
Original Assignee
Dini Têxtil Indústria E Comércio Ltda.
Instituto Presbiteriano Mackenzie
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 Dini Têxtil Indústria E Comércio Ltda., Instituto Presbiteriano Mackenzie filed Critical Dini Têxtil Indústria E Comércio Ltda.
Publication of WO2021097544A1 publication Critical patent/WO2021097544A1/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
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • 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
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/04—Melting filament-forming substances
    • 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
    • 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
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • 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

Definitions

  • the invention is aimed at the production of polyester and graphene oxide nanocomposites for the synthetic yarn processing industries, such as the textile, synthetic knitting, automobile and aeronautical industries, and can be applied to obtain yarns with greater mechanical performance, tribological and presenting greater thermal comfort for the user of the textile product.
  • the document WO2017066937A1 describes a process for obtaining fibers from a nanocomposite material formed by graphene and polyester, and the dispersion of the dry charge is carried out in a high speed mixer, with the fiber being obtained by diluting a concentrate in which graphene concentrations range from 0.1 to 20%.
  • the high shear leads to the breakdown (degradation) of the polymer and loss of matrix properties, and the use of dry materials does not guarantee an adequate dispersion of the graphene particles in the polymeric matrix.
  • CN 105200547A describes a process for obtaining fibers from a nanocomposite material formed by reduced graphene oxide and polyester, with the dispersion of the dry charge also being carried out in a high-speed mixer, in concentrations of graphene oxide varying from 0.1 to 20% and with subsequent double screw extrusion.
  • this other process also has the drawback of producing high shear, leading to the breakdown of the polymer and loss of properties of the polymeric matrix.
  • the use of materials dry in the formation of the mixture does not guarantee an adequate dispersion of the graphene particles in the polymeric matrix.
  • a two-dimensional material such as graphene oxide presenting a high surface area, requires few levels in polymeric nanocomposites, to provide an effective reinforcing action. However, this same property induces a very easy re-agglomeration of the particles of graphene oxide during mixing with the polymer.
  • the present invention has the objective of providing a process for obtaining said fibers that allows a correct insertion of particles of graphene oxide in polyester, guaranteeing a good distribution and an adequate dispersion of these particles in the polymeric matrix, avoiding the formation of agglomerates and guaranteeing the production of the threads without the undesirable ruptures during the spinning.
  • a suspension of graphene oxide of high concentration is used, for premixing with the particles of the polyester, covering them, with the consequent maintenance of the morphology of the graphene oxide, without generating the formation of agglomerates in the heterogeneous hybrid compound thus obtained.
  • the process of formation of the heterogeneous hybrid compound before the production of the polymeric nanocomposite by mixing with the polymer in the molten state, ensures adequate dispersion and distribution of the particles of graphene oxide in the polymeric matrix, allowing the subsequent formation of homogeneous wires and micrometric diameters.
  • Figure 1 represents a graph with the distribution of graphene oxide particles generated from X-ray microtomography images of the polyester nanocomposite of graphene and graphene oxide, with a concentration of 0.0125% by weight of graphene oxide. in the polymeric matrix; this technique provides a broader information of the analyzed sample, being able to be evaluated a great number of particles; and
  • Figure 2 represents a transmission electron microscopy (MET) image of the nanocomposite with a concentration of 0.0125% by mass of graphene oxide in the polyester matrix, (this technique is used for observations much smaller areas than tomography), covering a larger region and closer to the graphene oxide particles.
  • MET transmission electron microscopy
  • the process object of the present invention comprises the following phases and steps:
  • the polyester is micronized for the production of particles smaller than 1 mm, thus guaranteeing an increase in the surface area.
  • a dispersion of graphene oxide in a suitable solvent with a concentration varying between 1 and 5 g / L is provided.
  • the solvent can be water and, as a result, the concentration of the dispersion can reach maximum values of 5 g / L, thus facilitating the next step (mixing the dispersion of graphene oxide with the polymer granules, followed by drying). That is, the volume of the dispersion to be used will be low to achieve the specified concentrations of graphene oxide in the composite, so that the drying process is faster.
  • the concentration of the graphene oxide dispersion is defined in lower limits (close to lg / L), which leads to the need for a larger volume of the dispersion to achieve the same concentrations.
  • Another important factor is that when water is used as a solvent, the process of obtaining graphene oxide (liquid exfoliation of graphite oxide) produces better quality material (fewer sheets stacked and larger side size).
  • the graphene oxide present in the dispersion used is characterized by having a thickness varying between 1 to 10 nm and lateral size in the range of 0.5 to 10 micrometers.
  • the concentration of graphene oxide is determined according to the final properties of the product to be prepared or its applicability, whether fiber or fabric. In the case of improvements in thermal properties, the concentration of graphene oxide required varies around 0.5 to 5.0% by weight of the polyester matrix, while for improvement in mechanical properties of traction and wear, this value is in around 0.01 to 1.0%.
  • the heterogeneous hybrid compound is subjected to a final drying step, being exposed, for example, for a period of 36 h, at 60 ° C, in an appropriate equipment such as a circulation oven , to ensure the elimination of water particles adsorbed on the heterogeneous hybrid compound.
  • the compost should reach values between 20,000 and 30,000 ppm of moisture.
  • the polymer nanocomposite is produced from the heterogeneous hybrid compound submitted to the drying and final drying steps.
  • the heterogeneous hybrid compound is subjected to a mixing stage in a molten state by processing in a twin screw extruder.
  • the processing conditions and thread profile are as follows:
  • the polymeric nanocomposite is processed under the following conditions:
  • the yarn produced can have a diameter varying around 200 dtex with 49 filaments.
  • the polymeric nanocomposite has a very homogeneous distribution of the graphene oxide particles in the polyester matrix.
  • the present invention allows the correct insertion of graphene oxide particles in polyester, ensuring a good distribution and dispersion of these in the polymeric matrix using the mixture in the molten state.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Le présent procédé vise à produire des nanocomposites de polyester et d'oxyde de graphène, pour des applications dans l'industrie textile, et comprend la formation d'un pré-mélange de particules de polyester avec une dispersion d'oxyde de graphène dans un solvant, de manière à générer, après le séchage, un composé hybride hétérogène dont les particules de polyester sont recouvertes par des feuilles d'oxyde de graphène. Le composé hybride hétérogène est inséré dans une extrudeuse à double vis en vue de la formation d'un nanocomposite polymère par mélange à l'état fondu. L'extrusion du nanocomposite polymère est alors effectuée dans un équipement accouplé à un dispositif de tirage de fils. Les fils produits présentent des particules d'oxyde de graphène possédant une excellente distribution dans la matrice de polyester, sans agglomérats, et permettant l'utilisation de ces fils pour diverses applications, y compris la production de tissus.
PCT/BR2020/050483 2019-11-21 2020-11-18 Procédé d'obtention de fibres textiles à base d'oxyde de graphène et de polyester WO2021097544A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BRBR1020190244771 2019-11-21
BR102019024477-1A BR102019024477A2 (pt) 2019-11-21 2019-11-21 Processo de obtenção de fibras texteis a base de óxido de grafeno e poliéster

Publications (1)

Publication Number Publication Date
WO2021097544A1 true WO2021097544A1 (fr) 2021-05-27

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PCT/BR2020/050483 WO2021097544A1 (fr) 2019-11-21 2020-11-18 Procédé d'obtention de fibres textiles à base d'oxyde de graphène et de polyester

Country Status (2)

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BR (1) BR102019024477A2 (fr)
WO (1) WO2021097544A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022084751A1 (fr) 2020-10-23 2022-04-28 Senai/Cetiqt Fil textile ayant des propriétés antivirales, et procédés associés

Citations (5)

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KR20110031826A (ko) * 2009-09-21 2011-03-29 성균관대학교산학협력단 그라핀／바이오 고분자 나노섬유 복합체 및 이의 제조방법
US20120244333A1 (en) * 2009-03-16 2012-09-27 Kordsa Global Endustriyel Iplik Ve Kord Bezi Sanayi Ve Ticaret A.S. Polymeric fibers and articles made therefrom
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* Cited by examiner, † Cited by third party
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US20120244333A1 (en) * 2009-03-16 2012-09-27 Kordsa Global Endustriyel Iplik Ve Kord Bezi Sanayi Ve Ticaret A.S. Polymeric fibers and articles made therefrom
KR20110031826A (ko) * 2009-09-21 2011-03-29 성균관대학교산학협력단 그라핀／바이오 고분자 나노섬유 복합체 및 이의 제조방법
CN105200547A (zh) * 2015-10-19 2015-12-30 沙嫣 一种石墨烯-涤纶纳米复合纤维的制备方法
CN105463620A (zh) * 2016-01-15 2016-04-06 东华大学 一种石墨烯/聚对苯二甲酸乙二酯复合纤维及其制备方法
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YOON, O.J. ET AL.: "Nanocomposite nanofibers of poly( D, L -lactic-co- glycolic acid) and graphene oxide nanosheets", COMPOSITES: PART A, vol. 42, 2011, pages 1978 - 1984, XP028330936, DOI: 10.1016/j.compositesa.2011.08.023 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022084751A1 (fr) 2020-10-23 2022-04-28 Senai/Cetiqt Fil textile ayant des propriétés antivirales, et procédés associés

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