EP2990510A1 - Fibres de polymère composite comprenant des particules d'aérogel et procédés de production associé - Google Patents

Fibres de polymère composite comprenant des particules d'aérogel et procédés de production associé Download PDF

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Publication number
EP2990510A1
EP2990510A1 EP14388004.5A EP14388004A EP2990510A1 EP 2990510 A1 EP2990510 A1 EP 2990510A1 EP 14388004 A EP14388004 A EP 14388004A EP 2990510 A1 EP2990510 A1 EP 2990510A1
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Prior art keywords
range
fibre
aerogel particles
aerogel
hollow
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EP14388004.5A
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German (de)
English (en)
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Anna Fricke
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Gabriel AS
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Gabriel AS
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Priority to EP14388004.5A priority Critical patent/EP2990510A1/fr
Priority to PCT/DK2015/000023 priority patent/WO2016029914A1/fr
Publication of EP2990510A1 publication Critical patent/EP2990510A1/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
    • D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • 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
    • D01D5/0015—Electro-spinning characterised by the initial state of the material

Definitions

  • the present invention relates to polymer fibres. More specifically, the invention relates to hollow polymer fibres comprising aerogel particles in the fibre lumen.
  • Aerogels are a special type of solid material with nanometre-scale pores. Porosity is often in excess of 90%, in some cases as high as 99.9%, and densities can be as low as 3 kg/m 3 .
  • the unusual properties of the aerogels afford their suitability for many applications in commercial and high-tech fields, such as waste management (gas absorption, radioactive waste confinement), thermal insulation (cryogenic to high temperatures), super-insulating jackets, laser experiments, sensors (ultrasonic and gas), nuclear particle detection (Cherenkov), optics and light-guides, electronic devices, capacitors, high explosive research and catalysts.
  • aerogel is vulnerable to moisture and tensile stress, and is rapidly spoiled, when the material is exposed to water or water vapour.
  • a research group at the University of Akron has reinforced an aerogel by incorporating a fibre in the block of the aerogel, and thereby improving the elastic properties.
  • the American company Aspen markets various products with aerogel in a polymer matrix under the name Space Loft, but these suffer from the weakness that binding of aerogel is weak, and the material thus loses its properties over time when aerogel, through physical impact, is released.
  • one object of the present invention is to stabilise aerogel to make it suitable for many applications in commercial and high-tech fields.
  • a specific object of the present invention is to produce a material comprising aerogel, which can withstand mechanical stress, and at the same time protect the aerogel from climatic conditions.
  • the above objects are solved by using a composite fibre, in which the aerogel particle is encapsulated by a polymer matrix in the form of a hollow fibre. Since the aerogel particle retains its structure within the composite fibre, the good insulation properties are transferred to the composite fibre.
  • the hollow fibre of polymer component contributes with the mechanical properties.
  • the material is designed in such a way that the aerogel particle is completely encapsulated by the hollow fibre. This encapsulation contributes to the protection against climatic conditions.
  • One aspect of the invention relates to a composite fibre comprising a hollow fibre and aerogel particles, wherein the lumen of the hollow fibre is at least partially filled with said aerogel particles.
  • a second aspect of the invention relates to a fibre comprising a wall and a lumen; wherein the lumen is at least partially filled with aerogel particles.
  • a third aspect of the invention relates to a method of production of a composite fibre, comprising the step of:
  • a composite fibre according to the present invention can then be processed into a material, e.g. as a nonwoven material.
  • One object of the present invention is to stabilise aerogel to make it suitable for many applications in commercial and high-tech fields.
  • a specific object of the present invention is to produce an insulation material comprising aerogel particles, which can withstand mechanical stress, and at the same time protect the aerogel particles from climatic conditions.
  • a composite fibre in which the aerogel particles are encapsulated by a hollow fibre, as a material for producing products suitable for commercial and high-tech fields.
  • a product could e.g. be an insulation material.
  • an encapsulation of the aerogel particle is to be understood as the polymer matrix wall of the hollow fibre being disposed about the aerogel particle, thereby preventing the aerogel particle from being in contact with the surroundings.
  • the term "fibre” refers to a unit of matter characterized by a high ratio of length-to-width.
  • the fibre can be spun into yarn, made into fabric by interlacing (weaving), interloping (knitting), or non-woven or membrane by interlocking (bonding).
  • the term "hollow fibre” is to be understood as fibre with a wall defining one or more lumens within the fibre. Such fibres may be extruded.
  • the term "aerogel” refers to an open-celled, mesoporous, solid foam that is composed of a network of interconnected nanostructures and that exhibit a porosity (non-solid volume) of no less than 50%.
  • the term “mesoporous” refers to a material that contains pores ranging from 2 to 50 nm in diameter.
  • Aerogel does not refer to a particular substance, but rather to a geometry which a substance can take on. Aerogels can be made of a wide variety of substances, including: Silica, transition metal oxides (for example, iron oxide), lanthanide and actinide metal oxides (for example, praseodymium oxide), main group metal oxides (for example, tin oxide), organic polymers (such as resorcinol-formaldehyde, phenol-formaldehyde, polyacrylates, polystyrenes, polyurethanes, and epoxies), biological polymers (such as gelatin, pectin, and agar agar), semiconductor nanostructures (such as cadmium selenide quantum dots), carbon, carbon nanotubes, and metals (such as copper and gold).
  • transition metal oxides for example, iron oxide
  • lanthanide and actinide metal oxides for example, praseodymium oxide
  • main group metal oxides for example, tin oxide
  • an aerogel is made using sol-gel chemistry to form a solvent filled high-porosity gel.
  • the gel is then dried by removing the solvent without collapsing the tenuous solid phase through a process called supercritical drying.
  • Other processes for the production of aerogels have been developed to lower the production costs.
  • the aerogel is provided as particles of variable size, and the inventors have used an aerogel (silica based, and in powder form) supplied by Insulgel High-Tech (Beijing) Co.,Ltd.
  • the term "powder” is to be understood as a dry, bulk solid composed of a large number of very fine particles that may flow freely when shaken or tilted.
  • particle is to be understood as a small localized object to which can be ascribed several physical or chemical properties such as volume or mass.
  • the present invention is not limited to any specific particle size, which may range from 0.1 micrometers ( ⁇ m) to several millimeters (mm).
  • one aspect of the invention relates to a composite fibre comprising a hollow fibre and aerogel particles, wherein the lumen of the hollow fibre is at least partially filled with said aerogel particles.
  • a second aspect of the invention relates to a fibre comprising a wall and a lumen; wherein the lumen is at least partially filled with aerogel particles.
  • the hollow fibre comprises one or more polymer(s).
  • the hollow fibre of the present invention is not limited to a specific type of polymer, and may be made by inorganic or organic polymers, or mixtures thereof.
  • the polymer(s) are homopolymers.
  • the term "homopolymer” refers to a polymer which is formed from only one type of monomer. This is in contrast to a copolymer/heteropolymer where the polymer contains at least two different monomers.
  • the polymer(s) are block co-polymer(s).
  • the aerogel particles are silica aerogel particles.
  • the aerogel particles occupy 1-100% of the hollow fibres lumen, such as within the range of 2-99%, e.g. within the range of 5-95%, such as within the range of 10-90%, e.g. within the range of 15-85%, such as within the range of 20-80%, e.g. within the range of 25-75%, such as within the range of 30-70%, e.g. within the range of 35-65%, such as within the range of 40-60%, e.g. within the range of 45-55% of the hollow fibres lumen.
  • the aerogel particles occupy at least 5% of the hollow fibres lumen, such as at least 10%, e.g. at least 15%, such as at least 20%, e.g. at least 25%, such as at least 30%, e.g. at least 35%, such as at least 40%, e.g. at least 45%, such as at least 50%, e.g. at least 55%, such as at least 60%, e.g. at least 65%, such as at least 70%, e.g. at least 75%, such as at least 80%, e.g. at least 85%, such as at least 90%, e.g. at least 95%, e.g. 97%, e.g. 99% of the hollow fibres lumen.
  • the hollow fibres lumen such as at least 10%, e.g. at least 15%, such as at least 20%, e.g. at least 25%, such as at least 30%, e.g. at least 35%, such as at least 40%, e.g. at least 45%,
  • the aerogel particles are less than 1000 ⁇ m in their largest dimension, such as within the range of 0.1-950 ⁇ m, e.g. within the range of 0.5-900 um, such as within the range of 1-850 ⁇ m, e.g. within the range of 5-800 ⁇ m, such as within the range of 10-750 ⁇ m, e.g. within the range of 15-700 ⁇ m, such as within the range of 20-650 ⁇ m, e.g. within the range of 25-600 ⁇ m, such as within the range of 30-550 ⁇ m, e.g. within the range of 35-500 ⁇ m, such as within the range of 40-450 um, e.g.
  • range of 45-400 um such as within the range of 50-350 ⁇ m, e.g. within the range of 55-300 ⁇ m, such as within the range of 60-250 ⁇ m, e.g. within the range of 65-200 ⁇ m, such as within the range of 70-150 ⁇ m, e.g. within the range of 75-100 ⁇ m in their largest dimension.
  • the aerogel particles are less than 2000 ⁇ m in their largest dimension, such as within the range of 0.1-1950 ⁇ m, e.g. within the range of 0.5-1900 ⁇ m, such as within the range of 1-1850 ⁇ m, e.g. within the range of 5-1800 ⁇ m, such as within the range of 10-1750 ⁇ m, e.g. within the range of 15-1700 ⁇ m, such as within the range of 20-1650 ⁇ m, e.g. within the range of 25-1600 ⁇ m, such as within the range of 30-1550 ⁇ m, e.g. within the range of 35-1500 ⁇ m, such as within the range of 40-1450 ⁇ m, e.g.
  • range of 45-1400 ⁇ m such as within the range of 50-1350 ⁇ m, e.g. within the range of 55-1300 um, such as within the range of 60-1250 ⁇ m, e.g. within the range of 65-1200 ⁇ m, such as within the range of 70-1150 ⁇ m, e.g. within the range of 75-1100 ⁇ m in their largest dimension.
  • the aerogel particles are less than 3000 ⁇ m in their largest dimension, such as within the range of 0.1-2950 ⁇ m, e.g. within the range of 0.5-2900 ⁇ m, such as within the range of 1-2850 ⁇ m, e.g. within the range of 5-2800 ⁇ m, such as within the range of 10-2750 ⁇ m, e.g. within the range of 15-2700 ⁇ m, such as within the range of 20-2650 ⁇ m, e.g. within the range of 25-2600 ⁇ m, such as within the range of 30-2550 ⁇ m, e.g. within the range of 35-2500 ⁇ m, such as within the range of 40-2450 ⁇ m, e.g.
  • within the range of 45-2400 ⁇ m such as within the range of 50-2350 ⁇ m, e.g. within the range of 55-2300 um, such as within the range of 60-2250 ⁇ m, e.g. within the range of 65-2200 ⁇ m, such as within the range of 70-2150 ⁇ m, e.g. within the range of 75-2100 ⁇ m in their largest dimension.
  • the present invention is not limited to any specific particle size, which may range from 0.1 micrometers ( ⁇ m) to several millimeters (mm).
  • ⁇ m micrometers
  • mm millimeters
  • the aerogel particles are smaller in their largest dimension than the orifice or channel through which they are passed.
  • the aerogel particles are within the range of 0.1-100 ⁇ m, or within the range of 50-150 ⁇ m, or within the range of 100-200 ⁇ m, or within the range of 150-250 ⁇ m, or within the range of 200-300 ⁇ m, or within the range of 250-350 ⁇ m, or within the range of 300-400 ⁇ m, or within the range of 350-450 ⁇ m, or within the range of 400-500 ⁇ m, or within the range of 450-550 ⁇ m, or within the range of 500-600 ⁇ m, or within the range of 550-650 ⁇ m, or within the range of 600-700 ⁇ m, or within the range of 650-750 ⁇ m, or within the range of 700-800 ⁇ m, or within the range of 750-850 ⁇ m, or within the range of 800-900 ⁇ m, or within the range of 850-950 ⁇ m, or within the range of 900-1000 ⁇ m in their largest dimension.
  • the aerogel particles are within the range of 0.1-100 ⁇ m, or within the range of 0.1-200 ⁇ m, or within the range of 0.1-300 ⁇ m, or within the range of 0.1-400 ⁇ m, or within the range of 0.1-500 ⁇ m in their largest dimension.
  • the aerogel particle size distribution is monomodal.
  • the average aerogel particle size is less than 1000 ⁇ m in its largest dimension, such as within the range of 0.1-950 ⁇ m, e.g. within the range of 0.5-900 ⁇ m, such as within the range of 1-850 ⁇ m, e.g. within the range of 5-800 ⁇ m, such as within the range of 10-750 ⁇ m, e.g. within the range of 15-700 ⁇ m, such as within the range of 20-650 ⁇ m, e.g. within the range of 25-600 ⁇ m, such as within the range of 30-550 ⁇ m, e.g. within the range of 35-500 ⁇ m, such as within the range of 40-450 ⁇ m, e.g.
  • within the range of 45-400 ⁇ m such as within the range of 50-350 ⁇ m, e.g. within the range of 55-300 ⁇ m, such as within the range of 60-250 ⁇ m, e.g. within the range of 65-200 ⁇ m, such as within the range of 70-150 ⁇ m, e.g. within the range of 75-100 ⁇ m in its largest dimension.
  • the average aerogel particles are less than 2000 ⁇ m in their largest dimension, such as within the range of 0.1-1950 ⁇ m, e.g. within the range of 0.5-1900 ⁇ m, such as within the range of 1-1850 ⁇ m, e.g. within the range of 5-1800 ⁇ m, such as within the range of 10-1750 ⁇ m, e.g. within the range of 15-1700 ⁇ m, such as within the range of 20-1650 ⁇ m, e.g. within the range of 25-1600 ⁇ m, such as within the range of 30-1550 ⁇ m, e.g. within the range of 35-1500 ⁇ m, such as within the range of 40-1450 ⁇ m, e.g.
  • range of 45-1400 um such as within the range of 50-1350 ⁇ m, e.g. within the range of 55-1300 ⁇ m, such as within the range of 60-1250 ⁇ m, e.g. within the range of 65-1200 ⁇ m, such as within the range of 70-1150 ⁇ m, e.g. within the range of 75-1100 ⁇ m in their largest dimension.
  • the average aerogel particles are less than 3000 ⁇ m in their largest dimension, such as within the range of 0.1-2950 ⁇ m, e.g. within the range of 0.5-2900 ⁇ m, such as within the range of 1-2850 ⁇ m, e.g. within the range of 5-2800 ⁇ m, such as within the range of 10-2750 ⁇ m, e.g. within the range of 15-2700 ⁇ m, such as within the range of 20-2650 ⁇ m, e.g. within the range of 25-2600 ⁇ m, such as within the range of 30-2550 ⁇ m, e.g. within the range of 35-2500 ⁇ m, such as within the range of 40-2450 ⁇ m, e.g.
  • within the range of 45-2400 ⁇ m such as within the range of 50-2350 ⁇ m, e.g. within the range of 55-2300 ⁇ m, such as within the range of 60-2250 ⁇ m, e.g. within the range of 65-2200 ⁇ m, such as within the range of 70-2150 ⁇ m, e.g. within the range of 75-2100 ⁇ m in their largest dimension.
  • the aerogel particles are within the range of 0.1-100 ⁇ m and with an average particle size of 50-80 ⁇ m, or within the range of 0.1-150 ⁇ m and with an average particle size of 100-130 ⁇ m, or within the range of 0.1-200 ⁇ m and with an average particle size of 150-180 ⁇ m, or within the range of 0.1-250 ⁇ m and with an average particle size of 200-230 ⁇ m, or within the range of 0.1-300 pm and with an average particle size of 250-280 ⁇ m, or within the range of 0.1-350 ⁇ m and with an average particle size of 300-330 ⁇ m, or within the range of 0.1-400 ⁇ m and with an average particle size of 350-380 ⁇ m, or within the range of 0.1-450 ⁇ m and with an average particle size of 400-430 ⁇ m, or within the range of 0.1-500 ⁇ m and with an average particle size of 450-480 ⁇ m, or within the range of 0.1-550 ⁇
  • a third aspect of the invention relates to a method of production of a composite fibre, comprising the step of:
  • the hollow fibre is formed by wet spinning, dry spinning, melt spinning, gel spinning or electrospinning.
  • the inventors have used a spinneret with multiple orifices/channels - one or more orifices/channels for spinning the hollow fibre, and one or more orifices/channels for introducing the aerogel particles.
  • An orifice/channel for introducing the aerogel particles is encircled by one or more orifices/channels for spinning the hollow fibre.
  • Non-limited examples of such spinnerets are shown in Figure 1 .
  • the aerogel particles and the material for forming the hollow fibre are passed through a multi-orifice/multi-channel spinneret.
  • the material for forming the hollow fibre may be passed through the spinneret as a polymeric solution or a pure polymer or polymeric mixture being pre-heated or melted.
  • the aerogel particles are introduced into the lumen of the hollow fibre by use of supercritical fluid, gravity, pump means, an injection pump, or combinations thereof.
  • the inventors have developed a process where the aerogel particles are introduced into the lumen by the aid of supercritical fluid.
  • the solvents of the polymeric solution should be volatile.
  • the temperature of the electro-spinning step is usually performed within the range from room temperature to the melting temperature of the polymer. Temperatures lower than room temperature may also be used.
  • the utilized pressure is typically about 1 bar under these conditions, but can be lowered in the case of a less volatile solvent to aid the evaporation process.
  • the selection of the solvents may in some embodiments be limited to solvents that have a relatively high vapour pressure, in order to promote the stabilization of an electro-spinning jet to create a fibre as the solvent evaporates.
  • the solvent(s) has a boiling point below 120 degrees Celsius, such as within the range of 50-110 degrees Celsius, e.g. within the range of 55-105 degrees Celsius, such as within the range of 60-100 degrees Celsius, e.g. within the range of 65-95 degrees Celsius, such as within the range of 70-90 degrees Celsius.
  • the solvent(s) are selected from the group consisting of an alcohol having a boiling point below 120 degrees Celsius, such as within the range of 50-110 degrees Celsius, e.g. within the range of 55-105 degrees Celsius, such as within the range of 60-100 degrees Celsius, e.g. within the range of 65-95 degrees Celsius, such as within the range of 70-90 degrees Celsius.
  • the alcohol is mixed with water.
  • the aerogel retains its structure within the composite fibre, the good insulation properties are transferred to the composite fibre.
  • the polymer component/matrix contributes with the mechanical properties.
  • the material is designed in such a way that the aerogel is encapsulated by the polymer matrix of the hollow fibre. This encapsulation contributes to the protection against climatic conditions.
  • One aspect relates to the use of a composite fibre according to the present invention, for the production of a nonwoven textile.
  • Another aspect relates to a composite fibre prepared by a process comprising the step of:
  • a composite fibre according to the present invention can then be processed into an insulation material, e.g. as a nonwoven material.
  • nonwoven refers to a manufactured sheet, web or batt of directionally or randomly oriented fibres, bonded by friction, and/or cohesion and/or adhesion, excluding paper and products which are woven, knitted, tufted, stitch-bonded incorporating binding yarns or filaments or felted by wet-milling, whether or not additionally needled.
  • the fibres may be of natural or fabricated origin. They may be staple or continuous filaments or be formed in situ. In the present context, at least a part of the fibres, are fibres of the present invention.
  • the main object of this study was to provide a composite fibre with aerogel particles encapsulated by polymer(s) in the form of a hollow fibre.
  • the proof of concept was achieved, using an aerogel (silica based, and in powder form) supplied by Insulgel High-Tech (Beijing) Co.,Ltd, and a poly(ethylene-glycol) with a chain length of 900 kDa obtained from Sigma Aldrich.
  • the hollow fibres were produced with electrospinning through a spinneret with two orifices/channels (coaxial); an inner and an outer orifice/channel.
  • a PET solution was passed through the outer orifice/channel.
  • the samples were spun with 6 cm collector distance.
  • the needle voltage was 4.1 kV and the collector voltage was -4.6kV.
  • the flow rate was 0.5 ml/hour for the shell solution.
  • the needle was moved with a velocity of 400 mm/s, over the silicon wafer substrates in order to collect parallel-aligned fibres.
  • the aerogel particles were simultaneously introduced (i.e. at the same time as the electrospinning process) into the lumen of the formed hollow fibre through the inner orifice/channel.
  • FIG. 2 cross sections of aerogel containing hollow fibres are shown.
  • the thickness of the wall varies between 0.1 ⁇ m and 3.2 ⁇ m. The thicknesses are measurable on the SEM images.

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  • 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)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
EP14388004.5A 2014-08-27 2014-08-27 Fibres de polymère composite comprenant des particules d'aérogel et procédés de production associé Withdrawn EP2990510A1 (fr)

Priority Applications (2)

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EP14388004.5A EP2990510A1 (fr) 2014-08-27 2014-08-27 Fibres de polymère composite comprenant des particules d'aérogel et procédés de production associé
PCT/DK2015/000023 WO2016029914A1 (fr) 2014-08-27 2015-06-17 Fibres polymères composites comprenant des particules d'aérogel, et procédé de production associé

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