EP3134567B1 - Nouveau procédé de fabrication de fils ignifugés - Google Patents

Nouveau procédé de fabrication de fils ignifugés Download PDF

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Publication number
EP3134567B1
EP3134567B1 EP15725769.2A EP15725769A EP3134567B1 EP 3134567 B1 EP3134567 B1 EP 3134567B1 EP 15725769 A EP15725769 A EP 15725769A EP 3134567 B1 EP3134567 B1 EP 3134567B1
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EP
European Patent Office
Prior art keywords
polymer
flame
sheath
yarn
anyone
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EP15725769.2A
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German (de)
English (en)
French (fr)
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EP3134567A1 (fr
Inventor
François-Xavier DAMOUR
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MERMET
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Individual
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Priority to PL15725769T priority Critical patent/PL3134567T3/pl
Publication of EP3134567A1 publication Critical patent/EP3134567A1/fr
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    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
    • D02G3/40—Yarns in which fibres are united by adhesives; Impregnated yarns or threads
    • D02G3/404—Yarns or threads coated with polymeric 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
    • D01D11/00—Other features of manufacture
    • D01D11/06—Coating with spinning solutions or melts
    • 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
    • D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44—Yarns or threads characterised by the purpose for which they are designed
    • D02G3/443—Heat-resistant, fireproof or flame-retardant yarns or threads

Definitions

  • the present invention relates to the technical field of son adapted to the realization of textile surfaces for sun protection. More specifically, the present invention relates to a new method of manufacturing fireproof son, said son being preferably without halogen.
  • Such a technique is, in particular, described in the documents EP 2 562 208 and EP 0 900 294 , wherein a composite yarn is obtained by sheathing a glass core yarn by a plastisol of PVC flame retarded by a ternary mixture comprising an oxygenated antimony compound, a hydrated metal oxide whose metal is selected in the group consisting of aluminum, magnesium, tin, zinc and lead, and zinc borate.
  • Flame-retardant properties for halogen-free yarns can also be obtained by the use of halogen-free flame retardant compounds, as has been described in the documents JP 2011-202397 and US 6,150,448 for example.
  • Other solutions propose obtaining satisfactory flame retardant properties for halogen-free yarns, sought for environmental reasons, by the use of large amounts of flame retardant fillers, incompatible with obtaining fine yarns (corresponding to an average the order of 80 to 120 tex).
  • they are found, in part, near the filaments, and behave as abrasives weakening the final wire obtained.
  • halogenated polymers requiring fewer flame retardants are preferred.
  • halogenated flame retardants such as, for example, deca bromo diphenyl ether or deca bromo diphenyl ethane or chlorinated paraffins, which are particularly effective and can therefore be used at lower concentrations, alone. or in synergy with antimony salts, such as antimony trioxide.
  • antimony salts such as antimony trioxide.
  • one of the objectives of the present invention is to provide a new method of manufacturing small diameter fireproof son that can be used to achieve highly fireproof textile surfaces compatible with applications in the field of sun protection.
  • the method according to the invention makes it possible to avoid using halogenated components, recognized as harmful.
  • the process according to the invention makes it possible in particular to produce halogen-free yarns.
  • the constituent materials of the multi-filament core, the polymeric sheath and the flame retardant or agents present will be chosen to be free of halogen.
  • the son produced by the process according to the invention consist of a multi-filament core, said multi-filament core being coated with a polymeric sheath.
  • said sheath comprises two successive coaxial polymeric zones, called internal zone and external zone, the external zone incorporating at least one flame-retardant agent, the concentration of flame-retardant agent in the external zone being greater than the concentration in flame retardant agent in the internal area.
  • the multi-filamentary core is of organic nature.
  • the method according to the invention makes it possible, thanks to a single deposition step made from a particular mixture of miscible polymers when they are in the fused state, to obtain, in the end, a multi-filament core which is protected. by the inner zone of the sheath obtained, said inner zone being free or weakly loaded with flame retardant.
  • the concentration of flame retardant in the outer zone of the sheath makes it possible to concentrate its action on the peripheral zone of the wire, thus leading to obtaining excellent properties of fire resistance.
  • the amounts of polymers introduced will be chosen so as to obtain a yarn whose sheath is 40 to 80% by weight, and preferably 50 to 70% by weight, of the total weight of the yarn.
  • the amounts of flame retardant agent (s) introduced will be chosen so as to obtain a yarn whose external zone comprises a quantity of flame-retardant agent corresponding to a weight% of 15 to 50% by weight. %, preferably 20 to 30%, of the total weight of the sheath. This mass percentage corresponds to the mass of flame retardant agent on the total mass of sheath 100 times.
  • the yarns obtained with the process according to the invention have a mean diameter in the range of 150 to 500 ⁇ m, preferably in the range of 200 to 400 ⁇ m.
  • the mean diameter is the arithmetic mean of all the diameter measurements made, for example 10 in number, in particular with an MSD type apparatus marketed by ZUMBACH.
  • the sheath makes it possible, in a conventional manner, to protect the multi-filament core and to give cohesion to the filaments and, thus, to make the wire usable on industrial transformation machines.
  • the sheath made around the multi-filament core also has a dual role: i) to obtain a sheathed wire of circular section and of constant diameter and ii) to give its flame retardancy to the wire.
  • the yarn made by the process according to the invention has a circular section which has a constant diameter over the entire length of the yarn at plus or minus 10%. That is, each measured diameter value belongs to the range: average value plus or minus 10%. The average value is the arithmetical average of all diameter measurements made, in particular with an MSD25 type apparatus marketed by ZUMBACH.
  • the multi-filament core surrounded by the inner zone will have an average diameter of 100 to 400 ⁇ m to more than at least 10%, and preferably from 125 to 300 ⁇ m to more than at least 10%, so obtaining with the outer zone a wire of average total diameter of 150 to 500 microns more than at least 10%, and preferably from 200 to 400 microns to more than at least 10%.
  • the high concentration of the flame retardant at the periphery of the yarn is compatible with small diameter yarns and important fireproofing properties.
  • the inner zone of the sheath protects the multi-filament core from the aggression that could be caused by the presence of the flame-retardant agent, since in the context of the invention, the latter is mainly located in the outer zone of the flame retardant. sheath.
  • the yarn I produced by the process according to the invention comprises a multi-filamentary core 1 surrounded by a sheath comprising two coaxial zones: an inner polymeric zone or layer 2 and an outer polymeric zone or layer 3 in which a flame-retardant agent 4 is distributed.
  • Each of the two zones of the sheath (inner and outer zone) will preferably be uniform in size and in composition.
  • the flame retardant will be regularly distributed in the polymeric matrix forming the outer zone.
  • the internal polymeric zone is a minority in the composition of the sheath. It preferably represents from 6 to 26% of the total mass of the composite yarn (ie, core + sheath) and the amounts of base polymer and co-flame retardant polymer and flame retardant introduced into the blend deposited will be adjusted to obtain such a percentage.
  • the concentration of flame-retardant agent in the outer zone of the polymeric sheath surrounding the filament yarn consisting of a set of filaments is greater than the concentration of flame-retardant agent in the inner zone, due to the migration involved in the process according to the invention. 'invention.
  • the inner zone of the sheath may or may not incorporate a flame retardant, depending in particular on the amount of flame retardant present in the deposited mixture.
  • the wire produced by the method according to the invention (both the core and the polymeric sheath) is halogen-free, that is to say that none of its constituents (material constituting the multi-filament core, polymer (s) constituting the sheath, agent (s) flame retardants)) involved in the process comprises halogen atom.
  • the core of the wire made according to the invention is in the form of a set of filaments extending in a preferred direction.
  • Such multi-filament cores correspond to multi-filament yarns currently commercially available.
  • a multi-filament core will preferably be used. having a titer of 20 to 150 tex, preferably 30 to 60 tex, depending on the constituent material of the core.
  • the multi-filamentary cores will be favored in a weakly combustible material.
  • the multi-filament core will be made of a material containing no halogen.
  • the multi-filament core is made of an organic material, in particular a thermoplastic polymer, preferably chosen from polyamides, polyesters (such as polyethylene terephthalate-PET), polyurethanes, polyolefins (such as polypropylenes) and vinyl polymers (such as vinyl acetate) as well as other artificial polymers such as cellulose acetate, and mixtures thereof.
  • a thermoplastic polymer preferably chosen from polyamides, polyesters (such as polyethylene terephthalate-PET), polyurethanes, polyolefins (such as polypropylenes) and vinyl polymers (such as vinyl acetate) as well as other artificial polymers such as cellulose acetate, and mixtures thereof.
  • the core is an inorganic material, and is, for example, consisting of a set of glass filaments. Nevertheless, the invention is particularly suitable for the fireproofing of a core of a combustible material, in particular of the polyester or polyolefin type.
  • the multi-filament core is covered with a composition comprising a mixture of molten polymers and at least one flame-retardant agent which will allow the sheathing of the yarn and which is formulated to obtain, during cooling, a migration of the agent flame retardant on the periphery of the wire.
  • the constituent polymer (s) of the sheath will be halogen-free, which therefore excludes, in particular, the family of PVCs used in the prior plastisol-based techniques.
  • the constituent polymer (s) of the inner and outer zones are, for example, chosen from esters of acrylic or methacrylic acids, non-halogenated vinyl polymers, ethylene / vinyl acetate copolymers, polyolefins, styrene copolymers, polyurethanes, polyamides, polyesters, copolyamides, copolyesters, oleamides, erucamides, silicones and acetals.
  • each of the two zones of the cladding will, in particular, be dependent on the method used for the constitution of these different zones.
  • a miscible mixture of molten polymers is deposited, said mixture comprising at least one flame-retardant agent, and at least two polymers belonging to different chemical families with one of the two polymers (called co-flame retardant polymer) which has on the one hand a vitreous transition temperature significantly lower than that of the other polymer (named base polymer) and on the other hand a melting temperature also significantly lower than that of the base polymer .
  • co-flame retardant polymer a vitreous transition temperature significantly lower than that of the other polymer
  • melting temperature also significantly lower than that of the base polymer.
  • significantly lower is meant lower by at least 10 ° C, and preferably on the order of -20 to -30 ° C.
  • the difference between the melting temperature of the co-flame retardant polymer and that of the base polymer will be in the range of 15 to 50 ° C, preferably 30 to 50 ° C.
  • the difference will be determined by taking the arithmetic averages of the measurements, for example on the basis of 5 measurements, for each temperature to be compared.
  • the co-flame retardant polymer having the lowest melting temperature will be chosen not to degrade to the melting temperature of the base polymer.
  • the deposited polymer blend is referred to as a miscible blend of melt polymers, i.e. the blend is homogeneous, and does not demix or separate the different polymers. On the other hand, this does not necessarily mean that the base polymer and the co-fire retardant polymer are miscible in a mixture of these two only molten polymers. It may be necessary to add another polymer to obtain a miscible mixture.
  • co-flame retardant polymer which although miscible in the melt with the base polymer, will then migrate outward due to the absence of permanent chemical bonds between the two polymers at the same time. melted state, taking with it a part of the flame retardant agent.
  • the co-flame retardant polymer preferably behaves as an adhesion promoter, which melt is attached to the surface of the flame retardant.
  • the flame retardant agent when the latter is in solid form, will advantageously have a large specific surface, ideally greater than 50 m 2 / g.
  • the wetting angle formed by the melt polymer on the flame retardant will be less than 90 °.
  • the base polymer in the final sheath will be in crystallized or partially crystallized form.
  • the base polymer will have a number average molecular weight Mn of between 10,000 and 30000 g / mol, while the co-fire retardant polymer will have a number average molecular weight Mn of between 300 and 1000 g / mol.
  • the base polymer will form the inner zone and the co-flame retardant polymer in admixture with the polymer of the invention.
  • the base will form the polymeric matrix of the outer zone of the sheath. It is of course possible that each of the zones is formed of a mixture of polymers, at least one of which in each zone, or all of them, satisfy the conditions set forth in the context of the invention.
  • the base polymer (s) constituting the inner zone of the cladding will be chosen from: esters of acrylic or methacrylic acids, non-halogenated vinyl polymers, polyurethanes, polyamides, thermoplastic polyolefins, olefinic elastomer thermoplastics (TPO), styrenic copolymers of styrene-butadiene (SBR) or styrene-ethylene-butylene-styrene (SEBS) type, polyesters and silicones and the polymer matrix of the outer zone of the sheath will be formed of at least one polymer base identical to that present in the inner zone and at least one co-flame retardant polymer chosen from copolyamides, copolyesters, polyurethanes, polyolefins, oleamides, erucamides and copolymers based on styrene.
  • the inner zone of the sheath may contain a low concentration of flame retardant but which will always be lower than the concentration of flame retardant in the outer zone.
  • polymers (s) used for forming the sheath will also be adapted, depending on the final application envisaged for the wire.
  • polymers having a high moisture uptake such as polyamides
  • non-hydrolyzable polymers such as ethylene vinyl acetate (EVA) or styrenes and their copolymers, will be preferred, for outdoor applications.
  • EVA ethylene vinyl acetate
  • the flame-retardant agent (s) present in the process according to the invention are preferably halogen-free.
  • one or more agent (s) flame retardant (s) chosen from the agents can be used Phosphorus or nitrogen-containing flame retardants, such as ammonium polyphosphates, melamine isocyanurate, pentaerythritol and melamine derivatives and ammonium molybdates, depending on the nature of the polymer (s) present in the outer zone of the cladding.
  • the flame-retardant agent (s) present may therefore be of a mineral or organic nature. In known manner, they will be chosen, depending on the nature of the polymer or polymers that will (will) constitute the outer zone of the sheath.
  • the outer zone will be formed of a polyamide
  • nitrogen-containing flame retardants such as melamine isocyanurates.
  • Many already flame retarded polymer compositions are commercially available and may be used as a component of the deposited blend.
  • Such polyamide-based compositions are especially available from ADDIPLAST, ALBIS, or ULTRAPOLYMERS or ARKEMA, such EVA-based compositions are, for their part, available from ARKEMA, ALPHAGARY or EUROFIND. It is also possible to prepare the deposition compositions using separately sold flame retardant polymer (s) and agent (s) which will be mixed or compounded.
  • the flameproofing agent (s) may be in the form of one or more liquid compounds and / or of one or more solid compounds preferably having a small particle size.
  • Small particle size means particles whose largest size is less than 50 microns.
  • the flame retardant agent will be selected so as to be evenly distributed in the deposit formulation containing it. In particular, if it is one or more liquid compounds, the latter will be soluble or miscible in the molten polymer mixture. If it is one or more solid compounds, their small particle size will allow to obtain a regular dispersion in the molten polymer mixture.
  • the process for constituting the yarns according to the invention consists in producing the sheath with a single deposition operation, but in choosing a deposition formulation that makes it possible to migrate the molecules or particles of flame retardant agent into the peripheral portion of the sheath.
  • a deposit is, preferably, carried out with implementation of a calibration step by extrusion of a sheath on the core wire and calibration of the sheath by passage through a die. Nevertheless, it is possible to perform the recovery and calibration of the textile core with any suitable method well known to those skilled in the art for depositing a molten polymer mixture.
  • the flame retardant will be evenly distributed in the molten polymer mixture. This homogeneous distribution can be obtained by a mixing operation, for example with mechanical stirring.
  • the formulation comprising the mixture of polymers in the molten state and the selected flame retardant (s) is (are) applied to the multi-filament core wire by any suitable technique which will allow both the coating and the sheathing of the multi-filamentary core.
  • the outer zone will therefore be composed of at least 3 components: a base polymer, a co-flame retardant polymer and a flame retardant agent.
  • polymer which can be used as base polymer By way of examples of polymer which can be used as base polymer, mention may be made of: esters of acrylic or methacrylic acids, non-halogenated vinyl polymers, polyurethanes, polyamides, thermoplastic polyolefins, olefinic elastomeric thermoplastics ( TPO), styrenic copolymers of styrene butadiene (SBR) or styrene-ethylene / butylene-styrene (SEBS) type, polyesters and silicones.
  • esters of acrylic or methacrylic acids non-halogenated vinyl polymers
  • polyurethanes polyurethanes
  • polyamides thermoplastic polyolefins
  • TPO olefinic elastomeric thermoplastics
  • SBR styrenic copolymers of styrene butadiene
  • SEBS styrene-ethylene / butylene-styren
  • a polymer that can be used as a co-flame retardant polymer mention may be made of: copolyamides, copolyesters, polyurethanes, polyolefins, oleamides and erucamides, as well as styrene-based copolymers.
  • the cooling step may be carried out by passing the wire into a cooling zone, in particular maintained at a temperature in the range from 3 to 25 ° C.
  • a cooling zone in particular maintained at a temperature in the range from 3 to 25 ° C.
  • the outer zone will not be obtained by depositing a polymer dispersion in the form of plastisol or in the form of an aqueous dispersion.
  • the plastisol route will not be retained because it requires the use of plasticizer (s) which are low molecular weight compounds, which will migrate and exude to the surface of the wires, leading to a greasy feel.
  • the aqueous dispersion route will not be retained either, because it does not allow to obtain a continuous sheath at the outer zone which is the guarantor of the protection of the core wire of environmental assaults. outside.
  • the method according to the invention therefore uses neither plastisol nor plasticizer, so that the sheath contains neither plastisol nor plasticizer.
  • the different steps of the process according to the invention can be carried out continuously and lead to long lengths of wire.
  • the son obtained at the end of the process according to the invention may be wound in the form of coil, waiting to be used.
  • the various components used to make the yarns according to the invention will be chosen to possess all the technical characteristics of the products intended for this purpose. use, and in particular UV resistance as measured by artificial aging with XENOTEST according to the standard NF EN ISO 105B02, a resistance to soiling and a cleaning ability, the mechanical properties necessary for the production of textiles for blinds, and resistance to bad weather, heat and cold, especially when the wire is intended for outdoor applications.
  • the method according to the invention may lead to son having a high level of fireproofing type M1 according to standard NFP92507 or B1 according to DIN 4102.
  • the fire-retardant sheathed yarns obtained by the process according to the invention may be used for the constitution of textiles intended for sun protection, chosen from woven fabrics, woven and nonwoven grids and knits constituted at least in part, or even totally, of son according to the invention.
  • the flame retardant wire obtained by the process according to the invention can be used for the constitution of textiles adapted to sun protection, in particular for the manufacture of blinds.
  • the yarn obtained by the process according to the invention will be woven, crisscrossed, knitted, or glued according to the selected architecture, by any appropriate technique well known to those skilled in the art.
  • Fabrics, grids or knits, made with yarns obtained by means of the process of the invention and having a low aperture factor, in particular of the order of 0 to 15%, and preferably of between 3 and 10%, will have the following characteristics: properties required, especially in terms of sun protection and fire resistance.
  • Such textiles may be intended to be positioned indoors or outdoors.
  • the yarns according to the invention make it possible to produce textiles whose fireproofing performance corresponds to a classification of type M1 according to the French standard NFP92507 and type B1 according to the German standard DIN 4102.
  • the manufacturing process used is schematized Figure 2 the wire 1 constituting the multi-filament core is unwound from a coil 10 , to pass into a preheating zone 20 , before reaching a wrapping extrusion device 30 ending in a die, from which it leaves to be directed to a cooling zone 40 , to obtain a wire I according to the invention which can be stored after winding in the form of a coil 50.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Multicomponent Fibers (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Artificial Filaments (AREA)
EP15725769.2A 2014-04-22 2015-04-21 Nouveau procédé de fabrication de fils ignifugés Active EP3134567B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL15725769T PL3134567T3 (pl) 2014-04-22 2015-04-21 Nowy proces produkcji ogniotrwałych nici

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1453617 2014-04-22
PCT/FR2015/051075 WO2015162371A1 (fr) 2014-04-22 2015-04-21 Nouveau procédé de fabrication de fils ignifugés

Publications (2)

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EP3134567A1 EP3134567A1 (fr) 2017-03-01
EP3134567B1 true EP3134567B1 (fr) 2018-06-06

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US (1) US9920458B2 (es)
EP (1) EP3134567B1 (es)
JP (1) JP6581995B2 (es)
KR (1) KR102239700B1 (es)
CN (1) CN106460235B (es)
AU (1) AU2015250659B2 (es)
BR (1) BR112016024456A2 (es)
CA (1) CA2945911C (es)
DK (1) DK3134567T3 (es)
ES (1) ES2685570T3 (es)
MX (1) MX2016013917A (es)
PL (1) PL3134567T3 (es)
WO (1) WO2015162371A1 (es)

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CN111455477A (zh) * 2020-04-07 2020-07-28 山东宏业纺织股份有限公司 一种阻燃纱线生产方法
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EP4320307A1 (en) 2021-07-02 2024-02-14 Eastman Kodak Company Non-foamed aqueous composition, coated textile and method of making

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EP2922908A2 (en) * 2012-11-20 2015-09-30 The Procter & Gamble Company Polymer-soap compositions and methods of making and using the same
CN104812548A (zh) * 2012-11-20 2015-07-29 艾姆弗勒克斯有限公司 模塑包含羟基化类脂的热塑性聚合物组合物的方法

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AU2015250659B2 (en) 2019-03-21
AU2015250659A1 (en) 2016-11-03
KR20160143834A (ko) 2016-12-14
DK3134567T3 (en) 2018-09-03
EP3134567A1 (fr) 2017-03-01
CA2945911C (fr) 2022-06-14
CN106460235B (zh) 2019-03-01
US20170044694A1 (en) 2017-02-16
KR102239700B1 (ko) 2021-04-13
ES2685570T3 (es) 2018-10-10
CN106460235A (zh) 2017-02-22
US9920458B2 (en) 2018-03-20
BR112016024456A2 (pt) 2017-08-15
MX2016013917A (es) 2017-05-23
WO2015162371A1 (fr) 2015-10-29
JP6581995B2 (ja) 2019-09-25
JP2017514034A (ja) 2017-06-01
PL3134567T3 (pl) 2018-11-30

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