EP1658395B1 - Verfahren zur herstellung von formkörpern mit thermoregulativen eigenschaften - Google Patents

Verfahren zur herstellung von formkörpern mit thermoregulativen eigenschaften Download PDF

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Publication number
EP1658395B1
EP1658395B1 EP04786178A EP04786178A EP1658395B1 EP 1658395 B1 EP1658395 B1 EP 1658395B1 EP 04786178 A EP04786178 A EP 04786178A EP 04786178 A EP04786178 A EP 04786178A EP 1658395 B1 EP1658395 B1 EP 1658395B1
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EP
European Patent Office
Prior art keywords
phase change
fibers
change material
polysaccharides
polymer
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Not-in-force
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EP04786178A
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German (de)
English (en)
French (fr)
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EP1658395A1 (de
Inventor
Detlev Gersching
Frank Meister
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Thueringisches Institut fuer Textil und Kunststoff Forschung eV
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Thueringisches Institut fuer Textil und Kunststoff Forschung eV
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Application filed by Thueringisches Institut fuer Textil und Kunststoff Forschung eV filed Critical Thueringisches Institut fuer Textil und Kunststoff Forschung eV
Priority to PL04786178T priority Critical patent/PL1658395T3/pl
Publication of EP1658395A1 publication Critical patent/EP1658395A1/de
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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
    • D01F4/04—Monocomponent artificial filaments or the like of proteins; Manufacture thereof from casein

Definitions

  • the invention relates to a process for the production of moldings, consisting of native network-forming polymers and phase change materials incorporated therein, which as. Fibers can be processed into fabrics with improved thermoregulatory properties and give textiles made from them a better comfort and have in other applications a high degree of functionality in terms of heat storage and delivery.
  • phase change materials can absorb or release relatively large amounts of heat when their phase state or conformation changes at a constant temperature.
  • an increased heat capacity is found, which finds its physically measurable expression in the enthalpy of fusion and allows the storage or release of larger amounts of heat than correspond to the normal heat capacity of the material outside the temperature range of the phase transition or the conformational change would.
  • phase change material paraffins or salts or solutions of suitable salts can be used.
  • the temperature range of the phase transition from the solid to the molten state can be adjusted in a targeted manner to the respective required temperature at which the heat is to be released or stored by varying the chain length.
  • Salts or their solutions can be selected specifically according to the desired temperature range of the conformational change.
  • the microencapsulated form is particularly suitable.
  • phase change material is enclosed in ceramic or polymer spheres with diameters in the micron range and thus brought into a manageable form that allows inclusion in crosslinked polymeric matrix materials, the amount of the thermoregulatory potential on the type and amount of enclosed PCM material is dependent.
  • Suitable matrix materials include both synthetic polymers and native network-forming polymers.
  • US 5,885,475 describes apparel composed of fibers consisting of a polymer blend additionally containing phase change material.
  • the fiber-forming substances are made selected from the group of synthetic melt-spinnable thermoplastic polymers.
  • Multicomponent fibers with increased, reversible thermal properties and textile fabrics produced therefrom are described in WO 03027365, US 200212079 and US 200129648.
  • the fiber bodies consisting of a multiplicity of elongated components, contain at least in one of these stretched components a temperature-regulating material distributed therein.
  • This may be a phase change material and optionally the classes of hydrocarbons, hydrated salts, waxes, oils, water, fatty acids, fatty acid esters, 2-basic acids and esters, halides, clusters and semiclusters, gas clusters, stearin anhydrite, ethylene carbonate, higher alcohols, polymers and metals and their mixtures belong.
  • the arrangement of the various components of the fiber can optionally take place in a core-sheath structure, polysetational, bundled or strip-shaped at different shaped cross-section.
  • the matrix material of the multicomponent fiber described can consist of different, linear chain molecules.
  • a disadvantage of these fibers and textile fabrics made therefrom is that only a portion of the fibers formed therefrom contain phase change material as a result of the described arrangement of the individual components and the proportion of temperature-regulating material in the overall fiber is naturally limited. Due to the presence of multicomponent structures of a plurality of elongated constituents, the proportion of phase change material that can be introduced into the polymer structure is limited to a proportion of at most 50 percent by mass, based on the respective matrix material.
  • WO 02095314 and CH 0200245 likewise describe processes in which the temperature-regulating properties are to be achieved by printing on a textile fabric with microencapsulated phase change material.
  • the temperature-regulating effect is thus achieved by applying a coating containing phase change material.
  • such a method has the disadvantage that only comparatively small amounts of phase change material can be fixed on the surface of the structures, in particular if only a part of the surface is printed with a suspension of microencapsulated phase change materials and thus the temperature regulating effect, based on the Amount of material, comparatively localized.
  • the printing of a textile surface with a suspension of microencapsulated phase materials applied in a comparatively large layer thickness has an adverse effect on the flexibility of textile products made therefrom and thus also on the wearing properties.
  • suspensions of microencapsulated phase change materials applied to textile surfaces have only limited mechanical resistance and are washable.
  • PCM fibers described so far are made on the basis of synthetic melt-spun polymer fibers.
  • network-forming structures can be prepared, for example, from cellulosic forming and spinning compositions by dissolving cellulose in tertiary amine oxides, preferably N-methylmorpholine-N-oxide, and a non-solvent, preferably water.
  • a spinning solution of cellulose in N-methylmorpholine-N-oxide and water is deformed by a dry-wet spinning process, coagulated in, for example, an aqueous spinning bath, the solvent completely removed by washing several times and the solidified shaped bodies dried.
  • the resulting shaped articles then have a network structure characterized by hydrogen bonds.
  • the globular proteins have, as the name implies, a spherical tertiary structure and occur in nature in relatively frequent numbers. Examples are the casein (milk protein), the zein (maize protein) and the ardenin (peanut protein).
  • the invention has for its object to develop a process for the preparation of thermoregulatory moldings, in particular fibers and their fabrics, from native network-forming polymers with trapped in the network Phasen prial, one, compared to generated on a synthetic basis PCM fibers, increased proportion of introduced phase change material contain and thus, while avoiding the disadvantages of the prior art, have an increased thermoregulatory potential.
  • the object is achieved by introducing phase change materials up to a content of 200% by mass into network-forming polymers, wherein the network is formed by the chemical coupling of functional groups, hydrogen bonds or helically interconnected polymeric or oligomeric structures.
  • a suitable network-forming polymeric matrix material is native cellulose. This forms bonds which on the one hand cause crosslinking of the polymer structure and on the other hand through the formation of hydrogen bonding the formation of a superstructure. By this structure formation, the embedding of larger amounts of microencapsulated phase change materials is possible.
  • the microencapsulation causes the demarcation between the phase change material and the polymer matrix.
  • a phase change material find, for example Paraffins of different chain length application, wherein the temperature of the phase transition depends on the chain length of the molecules and can be adjusted by changing the chain lengths the required temperature range of the phase transition. But also inorganic hydrated salts are applicable, which can be selected depending on the desired temperature range of the conformational change. Due to their higher density compared to paraffins, it is possible in particular to introduce far more than 50% by mass of phase change material into the polymer matrix.
  • a secondary structure in the form of folds of the amino acid chain based on hydrogen bonding results in a spatially cross-linked tertiary structure that is stabilized, for example, by disulfide bridges, hydrogen bonds, or ionic or hydrophobic interactions.
  • precrosslinked globular proteins are likewise soluble in tertiary amine oxides and can be shaped by a dry-wet process.
  • the solution of the precrosslinked globular protein can be added as a further constituent of a polysaccharide such as cellulose. This gives the possibility of being able to influence the properties of the moldings in a targeted manner.
  • a cellulose solution in a water-containing tertiary amine oxide phase change materials up to a content of 200 Percent by weight, based on the mass of the cellulose containing added and this solution over an air gap and then the cellulose precipitated with the phase change material enclosed in a precipitation bath, for example, water or a water / alcohol mixture, precipitated to form physical networks.
  • a precipitation bath for example, water or a water / alcohol mixture
  • phase change material associated with an optimal heat transfer to the phase change material or away from it.
  • precrosslinked globular proteins in N-methylmorpholine N-oxide are admixed with microencapsulated phase change material, optionally with the addition of polysaccharides such as e.g. Cellulose, transferred into a spinning solution and spun by known methods into filaments.
  • polysaccharides such as e.g. Cellulose
  • the native polymer-based PCM fibers produced according to the invention have a wide range of uses, for example for fabrics for the production of textiles, for nonwovens, in textiles for the automotive industry, in yarns and blended yarns.
  • phase-change heat characterizing the thermoregulatory properties of the native PCM fibers of the present invention has a value up to a factor of 8 compared to the synthetic polymer-based PCM fibers.
  • microencapsulated phase change material of a phase change temperature of 28 ° C (Thermasorb ® TY 83 from Outlast Technologies Inc.) with the addition of 6.8 g of propyl gallate in a dissolving vessel with agitator of 37 1 volume introduced.
  • the microencapsulated phase change material was previously screened to a grain size of 50 microns maximum.
  • the dissolving vessel is evacuated to 20 mbar and heated in the course of 6 hours from 20 ° C to 94 ° C at a stirrer speed of 18 min -1 and the evaporating water condensed in a connected condenser.
  • the spinning solution obtained has a viscosity of 1560 Pas and a refractive index of 1.484.
  • the spinning solution is extruded at 80 ° C through a spinneret with a number of holes of 150 and a hole diameter of 200 microns via an air gap in a precipitation bath of water.
  • the take-off speed is 25 m / min, which results in a distortion in the air gap of 3.75.
  • the spun fibers have a denier of about 14 dtex and are washed in subsequent rinse baths and then cut into stacks.
  • the phase change heat of the obtained fibers is 30 J / g.
  • the cellulose fibers without introduced phase change material have a heat capacity of 6 J / g.
  • the fineness-related tear strengths of the resulting fibers are about 15 cN / tex.
  • the modified fibers After being carded on a carding machine, the modified fibers could be processed into a needle-punched nonwoven having a basis weight of 300 g / m 2 .
  • casein 100 g of casein are dispersed in 250 ml of water and crosslinked by the addition of 2 g of glutaraldehyde and 0.1 g of MgCl 2 at 25 ° C. After pressing to a moisture content of 50%, the casein is suspended in 430 g of 60% NMMNO. As a stabilizer, 0.5 g of propyl gallate is added.
  • phase change material such as Lurapret TX PMC 28 ® from BASF AG
  • the suspension is transferred in a jacketed kneading apparatus under a vacuum of 30 mbar and a temperature of 90 ° C by distilling off 130 g of water in a spinning solution.
  • the homogeneity of the spinning solution is checked by light microscopy and is usually reached 15 minutes after the end of the distillation.
  • the solution is extruded through a spinneret with 150 holes of 90 microns in diameter as filaments through an air gap at 80 ° C spinning temperature in an aqueous precipitation bath and then washed with distilled water residue and cut to a staple length of 40 mm.
  • the fibers are dried at 60 ° C in a convection oven.
  • the strength of the spun fibers is 15 cN / tex at an elongation of 10% and a titer of about 15 dtex.
  • the Heat-absorbing capacity of the resulting fibers is 60 J / g versus 8 J / g for unmodified fibers.
  • casein 50 g of casein are dispersed in 250 ml of water and crosslinked by addition of 1 g of glutaraldehyde and 0.1 g of MgCl 2 at 25 ° C. After pressing to a moisture content of 50%, the casein is suspended in 430 g of 60% NMMNO. In addition, 25 g of dry ground sulphite be (DP 760) and 100 g microencapsulated phase change material such as Lurapret TX PMC 28 ® from BASF AG, was added. This corresponds to a content of 133% PCM based on cellulose. 0.5 g of propyl gallate are added for stabilization.
  • This suspension is transferred in a jacketed kneading apparatus under a vacuum of 30 mbar at a temperature of 90 ° C by distilling off 140 g of water in a spinning solution. Homogenization of the solution was achieved 15 minutes after the end of the distillation and was checked by light microscopy.
  • the spinning solution obtained was extruded through an air hole into an aqueous precipitation bath through a spinneret of 150 holes, each 90 ⁇ m in diameter, and the resulting fiber strand was washed without residue in distilled water and cut to a staple length of 40 mm.
  • the fibers were dried in a convection oven at 60 ° C.
  • the fibers have a strength of 30 cN / tex.
  • the titer is about 20 dtex.
  • the heat capacity of the modified fibers is 70 J / g versus 7 J / g for unmodified fibers.
  • 7607 g of a 60% solution of N-methylmorpholine-N-oxide are introduced together with 784 g of pulp of average polymerization degree 500 with the addition of 4.6 g of propyl gallate in a 37 l stirred volume dissolving vessel.
  • the dissolving vessel is evacuated to 20 mbar and heated in the course of 6 hours from 20 ° C to 94 ° C at a stirrer speed of 18 min -1 and condenses the evaporating water in a condenser. A total of 2361 g of water are evaporated.
  • the spinning solution obtained has a viscosity of 8072 Pas, the refractive index of the spinning solution was 1.487.
  • a stock solution of 1500 g of an 80% solution of N-methylmorpholine-N-oxide and 750 g of a microencapsulated phase change material such as Lurapret ® TX PMC 28 from BASF AG, and 45 g of xanthan gum is prepared. Both solutions are extruded after intimate mixing in a dynamic mixer at 80 ° C through a spinneret with a number of holes of 150 and a hole diameter of 200 microns, warped over an air gap, regenerated in an aqueous precipitation bath and washed solvent-free with distilled water. The adjustment of the mixing ratio is such that the extruded fibers have a concentration of microencapsulated phase change material of 60% based on cellulose.
  • the spun fibers have a fineness of about 10 dtex and are cut into stacks after washing.
  • the phase change heat of the obtained fibers is 80 J / g.
  • the cellulose fibers without introduced phase change material have a heat capacity of 6 J / g in the corresponding temperature range.
  • the fineness-related tear strengths of the resulting fibers are about 15 cN / tex.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Blow-Moulding Or Thermoforming Of Plastics Or The Like (AREA)
  • Heating, Cooling, Or Curing Plastics Or The Like In General (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Nonwoven Fabrics (AREA)
  • Polyesters Or Polycarbonates (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
EP04786178A 2003-08-30 2004-08-25 Verfahren zur herstellung von formkörpern mit thermoregulativen eigenschaften Not-in-force EP1658395B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL04786178T PL1658395T3 (pl) 2003-08-30 2004-08-25 Sposób wytwarzania wytworów formowanych o właściwościach termoregulacyjnych

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10340110 2003-08-30
PCT/DE2004/001893 WO2005024102A1 (de) 2003-08-30 2004-08-25 Formkörper, insbesondere fasern und deren flächengebilde, mit thermoregulativen eigenschaften

Publications (2)

Publication Number Publication Date
EP1658395A1 EP1658395A1 (de) 2006-05-24
EP1658395B1 true EP1658395B1 (de) 2006-11-08

Family

ID=34202272

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04786178A Not-in-force EP1658395B1 (de) 2003-08-30 2004-08-25 Verfahren zur herstellung von formkörpern mit thermoregulativen eigenschaften

Country Status (6)

Country Link
US (1) US20060279017A1 (pl)
EP (1) EP1658395B1 (pl)
AT (1) ATE344844T1 (pl)
DE (3) DE102004041684A1 (pl)
PL (1) PL1658395T3 (pl)
WO (1) WO2005024102A1 (pl)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7579078B2 (en) 2001-09-21 2009-08-25 Outlast Technologies, Inc. Temperature regulating cellulosic fibers and applications thereof
US7244497B2 (en) * 2001-09-21 2007-07-17 Outlast Technologies, Inc. Cellulosic fibers having enhanced reversible thermal properties and methods of forming thereof
US9434869B2 (en) 2001-09-21 2016-09-06 Outlast Technologies, LLC Cellulosic fibers having enhanced reversible thermal properties and methods of forming thereof
AT501252B1 (de) * 2004-12-23 2008-02-15 Chemiefaser Lenzing Ag Cellulosischer formkörper und verfahren zu seiner herstellung
TWI287996B (en) * 2005-10-19 2007-10-11 Taiwan Textile Res Inst Temperature regulating gel and article comprising the same
US20090051068A1 (en) * 2006-01-12 2009-02-26 Thüringisches Institute Für Textil-Und Kunststoff-Forschung E.V. Method for Producing Molded Bodies from Proteins
FR2911153B1 (fr) * 2007-01-10 2009-04-10 Lainiere De Picardie Bc Soc Pa Substrat textile incorporant une composition de regulation thermique entourant des ilots de transfert.
DE102007054702B4 (de) 2007-11-14 2018-10-18 Smartpolymer Gmbh Verfahren zur Herstellung von cellulosischen Formkörpern, cellulosischer Formkörper und dessen Verwendung
AT509289B1 (de) 2009-12-28 2014-06-15 Chemiefaser Lenzing Ag Funktionalisierter cellulosischer formkörper und verfahren zu seiner herstellung
DE102010054661A1 (de) * 2010-12-15 2012-06-28 Anke Domaske Verfahren zur Herstellung von Milchproteinfasern und daraus gewonnene Milchproteinfaserprodukte
WO2016054657A1 (en) 2014-10-03 2016-04-07 Erie Foods International, Inc. High protein food
DE102018100140B3 (de) 2017-12-14 2019-03-28 Institut Für Luft- Und Kältetechnik Gemeinnützige Gmbh Lüftungsanlage mit Wärmespeicher

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4908238A (en) * 1984-07-02 1990-03-13 The United States Of America As Represented By The Secretary Of Agriculture Temperature adaptable textile fibers and method of preparing same
US4756958A (en) * 1987-08-31 1988-07-12 Triangle Research And Development Corporation Fiber with reversible enhanced thermal storage properties and fabrics made therefrom
US5354524A (en) * 1993-05-24 1994-10-11 Alan Sellars Monitoring concentration of dope in product manufacture
US5885475A (en) * 1995-06-06 1999-03-23 The University Of Dayton Phase change materials incorporated throughout the structure of polymer fibers
GB9617043D0 (en) * 1996-08-14 1996-09-25 Courtaulds Plc Manufacture ofd extruded articles
US6077597A (en) * 1997-11-14 2000-06-20 Outlast Technologies, Inc. Interactive thermal insulating system having a layer treated with a coating of energy absorbing phase change material adjacent a layer of fibers containing energy absorbing phase change material
US6855422B2 (en) * 2000-09-21 2005-02-15 Monte C. Magill Multi-component fibers having enhanced reversible thermal properties and methods of manufacturing thereof
US20030124318A1 (en) * 2002-01-02 2003-07-03 Magill Monte C. Thermal barriers with reversible enhanced thermal properties
US20030124278A1 (en) * 2002-01-02 2003-07-03 Clark Dustin L. Thermal barriers with solid/solid phase change materials

Also Published As

Publication number Publication date
EP1658395A1 (de) 2006-05-24
DE112004002148D2 (de) 2006-07-13
US20060279017A1 (en) 2006-12-14
DE502004001972D1 (de) 2006-12-21
ATE344844T1 (de) 2006-11-15
WO2005024102A1 (de) 2005-03-17
PL1658395T3 (pl) 2007-04-30
DE102004041684A1 (de) 2005-03-17

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