EP1639160B1 - Flammfeste synthesegarne, -fasern und -filamente - Google Patents
Flammfeste synthesegarne, -fasern und -filamente Download PDFInfo
- Publication number
- EP1639160B1 EP1639160B1 EP04767460A EP04767460A EP1639160B1 EP 1639160 B1 EP1639160 B1 EP 1639160B1 EP 04767460 A EP04767460 A EP 04767460A EP 04767460 A EP04767460 A EP 04767460A EP 1639160 B1 EP1639160 B1 EP 1639160B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- yarns
- flame
- polyamide
- fibres
- weight
- Prior art date
- 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.)
- Expired - Lifetime
Links
- 239000003063 flame retardant Substances 0.000 claims description 58
- 239000000654 additive Substances 0.000 claims description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 38
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 37
- 230000000996 additive effect Effects 0.000 claims description 31
- 239000000758 substrate Substances 0.000 claims description 31
- -1 flame-retardant compound Chemical class 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 23
- 239000008187 granular material Substances 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 21
- 239000000835 fiber Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 14
- 238000009987 spinning Methods 0.000 claims description 12
- 238000005470 impregnation Methods 0.000 claims description 11
- 239000011148 porous material Substances 0.000 claims description 10
- 229920001169 thermoplastic Polymers 0.000 claims description 10
- 239000004416 thermosoftening plastic Substances 0.000 claims description 9
- 239000004952 Polyamide Substances 0.000 claims description 8
- 229920002647 polyamide Polymers 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 4
- 229920002292 Nylon 6 Polymers 0.000 claims description 3
- 229920000388 Polyphosphate Polymers 0.000 claims description 3
- 239000012760 heat stabilizer Substances 0.000 claims description 3
- 239000004611 light stabiliser Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052753 mercury Inorganic materials 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 3
- 239000001205 polyphosphate Substances 0.000 claims description 3
- 235000011176 polyphosphates Nutrition 0.000 claims description 3
- 229920000571 Nylon 11 Polymers 0.000 claims description 2
- 229920000299 Nylon 12 Polymers 0.000 claims description 2
- 229920001007 Nylon 4 Polymers 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000378 calcium silicate Substances 0.000 claims description 2
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 claims description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000391 magnesium silicate Substances 0.000 claims description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 2
- 235000019792 magnesium silicate Nutrition 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims 5
- 230000001747 exhibiting effect Effects 0.000 claims 2
- 229920000877 Melamine resin Polymers 0.000 claims 1
- 229920002302 Nylon 6,6 Polymers 0.000 claims 1
- 229920000572 Nylon 6/12 Polymers 0.000 claims 1
- 229910000323 aluminium silicate Inorganic materials 0.000 claims 1
- 239000000975 dye Substances 0.000 claims 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims 1
- 150000007974 melamines Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 description 16
- 150000001875 compounds Chemical class 0.000 description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 239000004753 textile Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000012815 thermoplastic material Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 238000004079 fireproofing Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000012757 flame retardant agent Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- OWICEWMBIBPFAH-UHFFFAOYSA-N (3-diphenoxyphosphoryloxyphenyl) diphenyl phosphate Chemical class C=1C=CC=CC=1OP(OC=1C=C(OP(=O)(OC=2C=CC=CC=2)OC=2C=CC=CC=2)C=CC=1)(=O)OC1=CC=CC=C1 OWICEWMBIBPFAH-UHFFFAOYSA-N 0.000 description 1
- YNBIMOFHQZVUMJ-UHFFFAOYSA-N 1-(5-ethyl-2-methyl-2-oxo-1,3,2$l^{5}-dioxaphosphinan-5-yl)ethylphosphonic acid Chemical class OP(=O)(O)C(C)C1(CC)COP(C)(=O)OC1 YNBIMOFHQZVUMJ-UHFFFAOYSA-N 0.000 description 1
- BQPNUOYXSVUVMY-UHFFFAOYSA-N [4-[2-(4-diphenoxyphosphoryloxyphenyl)propan-2-yl]phenyl] diphenyl phosphate Chemical class C=1C=C(OP(=O)(OC=2C=CC=CC=2)OC=2C=CC=CC=2)C=CC=1C(C)(C)C(C=C1)=CC=C1OP(=O)(OC=1C=CC=CC=1)OC1=CC=CC=C1 BQPNUOYXSVUVMY-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229920006018 co-polyamide Polymers 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical compound CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000004758 synthetic textile Substances 0.000 description 1
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
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- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
-
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-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/2971—Impregnation
Definitions
- the present invention relates to yarns, fibers or filaments of thermoplastics and their manufacture.
- thermoplastic yarns, fibers or filaments are increasingly used for making articles such as fabrics, knits, nonwovens, tufted surfaces or the like.
- fire resistance is meant mainly a property of extinction and non-propagation of the combustion of the article.
- This property is particularly illustrated by standardized tests such as, for example, to measure this property on molded articles, the test called "UL94" ("Underwriters Laboratories"), or for textile articles, ie woven surfaces , knitted, tufted, flocked or non-woven, tests such as that described in standard EN533, standard NF G07-128 of December 1978, standard ADB0031 published on 22/02/2001, standard AITM 2.0007 B, the standard AITM 2.0003 or the standards NF P92.504 / 501/503/507 applicable in particular in the field of the building.
- One of the first objects of the invention is to provide a filament, fiber, filament of polymeric material comprising an additive with flame retardant properties consisting of at least particles of a solid substrate on which is adsorbed a flame retardant compound, as defined in the claim 1 appended hereto.
- adsorbed is meant that the flame retardant compound is bonded at least temporarily to the solid substrate by any type of binding such as absorption in the porous structure of the particle if it exists, wetting or adsorption of the flame retardant compound on the surface of the particles by at least one layer of the flame retardant compound, or fixation or grafting of the flame retardant compound to the surface of the particles by chemical or physico-chemical bonds.
- adsorption or fixation is facilitated by the choice of a solid substrate having surface properties compatible with the properties of the flame retardant compound.
- a substrate with a hydrophilic surface property is advantageously associated with a flame retardant compound of hydrophilic nature and vice versa for compounds with a hydrophobic nature.
- the particle of the solid substrate may advantageously comprise elements, radicals that promote the adsorption of the flame-retardant compound on the surface of said particle.
- the weight concentration of flame retardant additive is between 0.5% and 25% relative to the final composition weight, advantageously between 1% and 10%.
- solid substrate is meant, preferably a solid mineral substrate at the transformation temperature of the polymeric materials.
- inorganic substrate suitable for the invention mention may be made of mineral oxides such as silica, alumina, zirconia, magnesium oxide, calcium oxide, cerium oxide and titanium oxide. or mixtures thereof, inorganic compounds such as calcium silicate, magnesium silicate, alkali silico-aluminates.
- those which can be dispersed in the thermoplastic material in the form of small diameter particles advantageously to obtain dispersed particles having a diameter of less than 5 ⁇ m, and even more advantageously, that at least 80% by number of the dispersed particles. have a diameter less than 1 micron are suitable.
- Such a dispersion can be obtained by mixing particles already having such size characteristics in the polymeric material or, more advantageously, using granules or agglomerates of substrates which, after addition in the polymeric material and under the action of shear forces applied to carry out the dispersion disintegrate into aggregates or elementary particles.
- the agglomerates or granules preferably have a high specific surface area and a porosity between the aggregates or elementary particles important to allow the flame retardant compound to adsorb at least on the surface of the aggregates or particles.
- the aggregates or particles may also have a porosity permitting the absorption of the flame retardant compound.
- the average diameter of the granules or agglomerates is not critical and is advantageously chosen to be able to easily handle the additive with flame retardant properties, especially when it is added to the polymeric material.
- the average diameter of these granules is also chosen to facilitate the addition and adsorption of the flame retardant compound, for example, to prevent sticking between the different granules.
- granules of average diameter D50 greater than 60 .mu.m, advantageously between 80 .mu.m and 300 .mu.m are preferred.
- certain silicas have these characteristics and are therefore particularly preferred.
- silicas having the property of dispersing in the form of particles or aggregates with a diameter or size of between 0.01 ⁇ m and 1 ⁇ m will be preferred for the implementation of the present invention.
- the mineral substrates that are particularly suitable for the invention are those whose granules or agglomerates have a porosity and a high specific surface area.
- the substrates employed according to the invention are those in which the granules or agglomerates have a total pore volume of at least 0.5 ml / g, preferably at least 2 ml / g, this pore volume is measured by the method of mercury porosimetry with a MICROMERITICS Autopore III 9420 porosimeter, according to the following procedure:
- the sample is dried beforehand for 2 hours in an oven at 200 ° C.
- the measurements are then carried out according to the procedure described in the manual provided by the manufacturer.
- the diameters or pore sizes are calculated by the WASHBURN relationship with a teta contact angle of 140 ° and a gamma surface tension of 485 Dynes / cm.
- inorganic substrates having a pore volume of at least 0.50 ml / g for pores whose diameter is equal to or less than 1 ⁇ m are preferred.
- the inorganic substrate is a silica, advantageously an amorphous silica.
- the silicas are obtained by various processes, two of which lead to silicas, called precipitated silica and fumed silica.
- the silica may also be prepared in gel form.
- Silicas with a specific surface area measured by the TBAC method greater than 50 m 2 / g are preferred.
- Precipitated silicas are preferred because they may be in the form of agglomerated particles forming granules with a size of at least 50 ⁇ m or greater than 150 ⁇ m.
- silicas which have remarkable properties of flowability, dispersibility and high impregnation capacity are described in particular in European patents. 966207 , 984773 , 520862 and international applications WO95 / 09187 and WO95 / 09128 .
- silicas may be suitable for the invention, such as those described in French patent application no. 01 16881 which are pyrogenic silicas or partially dehydroxylated silicas by calcination or surface treatment.
- silicas used as solid mineral substrate are only described for guidance and as preferred embodiments. It is also possible to use other silicas obtained by other processes having properties of porosity and dispersibility suitable for carrying out the invention.
- the flame retardant additive comprises an ingotifier compound adsorbed on the mineral substrate particles.
- this adsorption is obtained by impregnating the granules or agglomerates.
- This impregnation is carried out by any conventional means and, for example, by mixing the substrate with the flame retardant compound in the liquid state or in dispersed or solubilized form in a solvent. In the latter case, the solvent will be removed, after impregnation of the substrate, by evaporation.
- a flame retardant compound is one or more flame retardant compounds, or a mixture of compounds forming a system having flame retardant properties.
- Suitable flame retardant compounds for the invention include, for example, methyl-bis (5-ethyl-2-methyl-2-oxido-1,2,3-dioxaphosphorinan-5-yl) methyl phosphonic acid alone or in admixture with methyl (5-ethyl-2-methyl-2-oxido-1,3,2-dioxaphosphorinan-5-yl) methyl phosphonic acid, resorcinol bis (diphenyl phosphate), bisphenol A bis (diphenyl phosphate), polyphosphate esters.
- these compounds may be impregnated directly onto the substrate such as silica for example, or dissolved in a solvent such as, for example, for example, water, organic solvents such as ketones, alcohols, ethers, hydrocarbons, halogenated solvents, for example.
- a solvent such as, for example, for example, water, organic solvents such as ketones, alcohols, ethers, hydrocarbons, halogenated solvents, for example.
- a liquid flame retardant is used.
- the solid substrate is then impregnated with the solution obtained. In this case, it is possible to remove the solvent by drying.
- the impregnation is carried out dry, that is to say that the flame retardant compound is added gradually to the solid substrate to allow impregnation or total adsorption.
- the flame retardant compound or the solution of the flame retardant compound has a sufficient fluidity.
- this impregnation or adsorption can be carried out at temperatures higher than the ambient temperature, and in a range between 20 ° C. and 200 ° C., preferably below 100 ° C.
- the solid substrate can also be preheated in the same temperature range to facilitate impregnation.
- Drying can be carried out by any of the conventional techniques known to those skilled in the art.
- the impregnation can be done in a single step or in several successive stages.
- the amount of flame retardant impregnated or adsorbed may vary in large proportions. However, it is limited and at most equal to the amount necessary to fill the total pore volume of the mineral substrate in the case of impregnation of granules or agglomerates having a porosity.
- the flame retardant additive that must be added to the polymeric material should preferably be a powder or a solid in the form of granules having a good fluidity to allow this addition.
- the amount of flame retardant added is determined to obtain an impregnated solid product that can be handled and added to the polymeric material.
- the weight concentration of flame retardant compound in the flame retardant additive is between 20% and 70% with respect to the flame retardant additive, advantageously between 20% and 50%.
- said flame retardant additive is added to the polymeric material.
- This addition can be carried out by a mixture of granules or powders of thermoplastic material and particles or granules of flame retardant additive, then melting of the mixture with stirring or application of shearing forces to allow the dispersion of the flame retardant additive and in a preferred embodiment, the deagglomeration of the flame retardant additive granules.
- the preferred mode of addition of the flame retardant additive is to add said additive to the polymeric material in the molten state and to effect mixing by application of shear forces. This mixture is advantageously carried out in a device with single or double worm.
- additives may be added to said mixture either simultaneously or separately, such as mattifying agents, light or heat stabilizers, pigments or the like.
- spin pack comprising at the output of the worm, a filter and a die having one or more die holes.
- the wire leaving the die is cooled and then returned to a reel after possibly being stretched, according to conventional methods of manufacturing the filaments.
- the speed of winding or spinning is advantageously greater than 300 m / min and even more advantageously greater than 1000 m / min.
- the yarns of the invention with other spinning processes such as wet spinning by supplying a solution of the composition of polymeric materials comprising flame retardant additives in a die and extracting the solvent at the outlet of die either by evaporation or by coagulation.
- the method used for the manufacture of the son is that compatible with the nature of the polymeric material.
- polymeric materials suitable for the invention are those generally used for the manufacture of synthetic textile yarns or fibers, yarns, fibers, filaments for technical applications, in particular thermoplastic polymeric materials.
- thermoplastic polymer (s) are selected from the group of (co) polyamides comprising: polyamide 6, polyamide 6.6, polyamide 4, polyamide 11, polyamide 12, polyamides 4-6, 6-10, 6-12, 6-36, 12-12, their copolymers and mixtures, as well as polyesters such as polyethylene terephthalate, polybutylene terephthalate, polypropylene terephthalate.
- the thermoplastic matrix may also comprise additives, such as pigments, delustrants, mattifying agents, catalysts, heat and / or light stabilizers, anti-bacterial, anti-fungal and / or anti-mite agents.
- the products of the invention are yarns, filaments, fibers which may have a heading within a broad range. Thus, these products may have a low titre, for example of the order of 1 dtex or less to diameters of the order of a few hundred micrometers.
- the yarns, fibers or filaments obtained can be used in any application. More particularly, they can make it possible to produce woven, knitted or tufted textile surfaces of the nonwoven surfaces in association or otherwise with other non-flame-retarded yarns, fibers or filaments.
- the textile surfaces obtained by using the yarns, fibers or filaments of the invention having improved fireproofing characteristics.
- the yarns, fibers or filaments of the invention as well as the textile surfaces obtained with these yarns, fibers or filaments can be treated in ways analogous to those containing no flame retardant additive.
- the silica of great porosity used is a silica marketed under the name Tixosil 38X by Rhodia company having a total pore volume of 3.6 ml / g and a useful pore volume of 2.0 ml / g. It is a Microperle silica that has excellent flowability and does not dust.
- the organophosphorus compound called Antiblaze 1045 was heated in an oven to increase its fluidity. It is introduced into the silica at a temperature of 99 ° C. A fixed amount of Antiblaze 1045 is introduced into the silica to obtain the desired flame retardant concentrations indicated in Table I below.
- the final product is then screened on a 1.25 mm sieve.
- a polycaprolactam powder having a viscosity index of 140 ml / g measured in 90% formic acid at a temperature of 25 ° C. is mixed with a quantity of flame retardant additive A.
- the powder mixture is fed after drying. in an oven, in a twin-screw extruder with a diameter of 18 mm.
- the mixture is melted in the extruder and fed under pressure into a die having 10 0.4 mm diameter and 1.6 mm long holes.
- the flow of material in the die is about 1.0 Kg / h.
- the filaments emerging from the die head are converged, the wire obtained is taken up on a winder having a speed of 300 m / min.
- a hexamethylenediamine polyadipamide powder having a viscosity index of 140 ml / g measured in 90% formic acid at a temperature of 25 ° C. is mixed with a quantity of flame retardant additive A.
- the powder mixture is fed, after drying in an oven, in a twin-screw extruder with a diameter of 18 mm.
- the mixture is melted in the extruder and fed under pressure into a die having 10 0.4 mm diameter and 1.6 mm long holes.
- the flow rate of material in the die is about 1 kg / h.
- the filaments emerging from the die head are converged, the wire obtained is taken up on a winder having a speed of 300 m / min.
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- 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)
- Compositions Of Macromolecular Compounds (AREA)
- Multicomponent Fibers (AREA)
Claims (17)
- Fäden, Fasern aus Polymerstoff, dadurch gekennzeichnet, dass der Polymerstoff ein thermoplastischer Stoff ist, der aus der Gruppe ausgewählt ist, welche das Polyamid 6, das Polyamid 6.6, das Polyamid 4, das Polyamid 11, das Polyamid 12, die Polyamide 4-6, 6-10, 6-12, 6-36, 12-12, deren Copolymere und Mischungen umfasst, und der ein Additiv mit flammfest machenden Eigenschaften umfasst, welches mindestens aus den Partikeln eines feststofflichen Substrats besteht, wobei eine flammfest machende Verbindung an diesen adsorbiert ist, wobei das Substrat in Form von Granulatkörnern oder Agglomeraten vorliegt, bevor es dem Polymerstoff zugesetzt wird, und ein Porenvolumen von mindestens 0,5 ml/g aufweist, wenn dieses mittels Quecksilberporosimetrie bestimmt wird.
- Fäden, Fasern nach Anspruch 1, dadurch gekennzeichnet, dass die gewichtsmäßige Konzentration des flammfest machenden Additivs im Bereich von 0,5 % bis 25 %, unter Bezugnahme auf das Gewicht des Polymerstoffs, liegt.
- Fäden, Fasern nach Anspruch 2, dadurch gekennzeichnet, dass die gewichtsmäßige Konzentration des flammfest machenden Additivs im Bereich von 1 % bis 10 %, unter Bezugnahme auf das Gewicht des Polymerstoffs, liegt.
- Faden, Fasern nach Anspruch 1 bis 3, dadurch gekennhzeichhet, dass das feststoffliche Substrat ein mineralisches Substrat ist, das aus der Gruppe ausgewählt ist, welche Siliciumdioxid, Aluminiumoxid, Zirkoniumdioxid, Magnesiumoxid, Calciumoxid, Ceroxid, Titanoxid oder deren Mischungen, Calciumsilicat, Magnesiumsilicat, alkalische Silicoaluminate umfasst.
- Fäden Fasern nach Anspruch 1 bis 4, dadurch gekennzeichnet, dass das flammfest machende Additiv in den Fäden oder Fasern aus Partikeln oder Aggregaten besteht, von denen mindestens 80 % nach Stückzahl eine Größe von weniger als 1 µm aufweisen.
- Fäden, Fasern nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Granulatkörner oder Agglomerate einen mittleren Durchmesser (D50) von mindestens 60 µm haben.
- Fäden, Fasern nach Anspruch 6, dadurch gekennzeichnet, dass das feststoffliche Substrat ein Siliciumdioxid ist.
- Fäden, Fasern nach Anspruch 7, dadurch gekennzeichnet, dass das Siliciumdioxid in Form von Granulatkörnern oder Agglomeraten vorliegt, die eine spezifische Oberfläche von mehr als 50 m2/g aufweisen.
- Fäden, Fasern nach einem der Ansprüche 7 oder 8, dadurch gekennzeichnet, dass die Granulatkörner oder Agglomerate aus Siliciumdioxid ein Porenvolumen von mindestens 0,5 ml/g aufweisen, das mittels Quecksilberporosimetrie bestimmt wird.
- Fäden, Fasern nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die flammfest machende Verbindung aus der Grupppe von Melamin, Organophosphorverbindungen, Melaninderivaten ausgewahlt ist.
- Faden oder Faser nach Anspruch 10, dadurch gekennzeichnet, dass die Organophosphorverbindungen aus den Polyphosphatestern, den Phosphorsaureestern, den Phosphonsäureestern ausgewählt sind.
- Fäden, Faser nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass sie Additive umfassen, die aus der Gruppe ausgewählt sind, welche Pigmente, Farbstoffe, Wärme- und/oder Lichtstabilisatoren, hydrophile Mittel, hydrophobe Mittel, Mattierungsmittel umfasst.
- Verfahren zur Herstellung von Fäden oder Fasern gemäß der Begriffsbestimmung in einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass es darin besteht, das Additiv mit flammfest machender Eigenschaft dem thermoplastischen Stoff in geschmolzenem Zustand zuzusetzen, diese Mischung durch eine Düse zu spinnen und eine Spinn- oder Auswickelgeschwindigkeit von mehr als 300 m/min. anzuwenden.
- Verfahren nach Anspruch 13, dadurch gekennzeichnet, dass die Spinngeschwindigkeit mehr als 1000 m/min. beträgt.
- Verfahren nach Anspruch 13 oder 14, dadurch gekennzeichnet, dass das flammfest machende Additiv erhalten wird, indem Granulatkörner oder Agglomerate eines mineralischen Substrats mit der flammfest machenden Verbindung in flüssigem Zustand oder in Lösung getränkt werden.
- Verfahren nach Anspruch 13, dadurch gekennzeichnet, dass die gewichtsmaßige Konzentration der flammfest machenden Verbindung in dem flammfest machenden Additiv im Bereich von 20 % bis 70 Gewichts-%, unter Bezugnahme auf das Gewicht des mineralischen Substrats, liegt.
- Verfahren nach Anspruch 14, dadurch gekennzeichnet, dass die gewichtsmäßige Konzentration der flammfest machenden Verbindung im Bereich von 20 % bis 50 % liegt.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0307825A FR2856703B1 (fr) | 2003-06-27 | 2003-06-27 | Fils, fibres, filaments en matiere synthetique ignifugee |
PCT/FR2004/001612 WO2005001173A2 (fr) | 2003-06-27 | 2004-06-25 | Fils, fibres, filaments en matiere synthetique ignifugee |
Publications (2)
Publication Number | Publication Date |
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EP1639160A2 EP1639160A2 (de) | 2006-03-29 |
EP1639160B1 true EP1639160B1 (de) | 2012-10-31 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP04767460A Expired - Lifetime EP1639160B1 (de) | 2003-06-27 | 2004-06-25 | Flammfeste synthesegarne, -fasern und -filamente |
Country Status (6)
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US (1) | US7758959B2 (de) |
EP (1) | EP1639160B1 (de) |
JP (1) | JP4351250B2 (de) |
CN (1) | CN100497766C (de) |
FR (1) | FR2856703B1 (de) |
WO (1) | WO2005001173A2 (de) |
Families Citing this family (19)
Publication number | Priority date | Publication date | Assignee | Title |
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US9056988B2 (en) * | 2007-02-05 | 2015-06-16 | Ppg Industries Ohio, Inc. | Solar reflective coatings and coating systems |
US8822025B2 (en) * | 2007-02-05 | 2014-09-02 | Ppg Industries Ohio, Inc. | Coating system exhibiting cool dark color |
JP5150975B2 (ja) * | 2007-08-31 | 2013-02-27 | Esファイバービジョンズ株式会社 | 多孔質成形体用収縮性繊維 |
JP5312142B2 (ja) * | 2009-03-27 | 2013-10-09 | ダイワボウホールディングス株式会社 | ポリカーボネート繊維およびその製造方法、ならびに繊維集合物 |
JP6061440B2 (ja) * | 2010-02-25 | 2017-01-18 | 太陽ホールディングス株式会社 | ポリエステル基材用樹脂組成物、それを用いたドライフィルム及びプリント配線板 |
US8679617B2 (en) | 2010-11-02 | 2014-03-25 | Prc Desoto International, Inc. | Solar reflective coatings systems |
WO2012084646A1 (en) * | 2010-12-21 | 2012-06-28 | Solvay Sa | Polymer mixture |
CN102653890B (zh) * | 2011-03-01 | 2014-06-18 | 上海安凸塑料添加剂有限公司 | 一种高可纺性无卤阻燃锦纶纤维的制备方法 |
US9057835B2 (en) | 2011-06-06 | 2015-06-16 | Ppg Industries Ohio, Inc. | Coating compositions that transmit infrared radiation and exhibit color stability and related coating systems |
CN102500086B (zh) * | 2011-10-18 | 2013-11-20 | 西安科技大学 | 一种灭火剂及其制备方法 |
CN102899891A (zh) * | 2012-08-29 | 2013-01-30 | 昆山铁牛衬衫厂 | 阻燃纺织材料的整理方法 |
CN102851944A (zh) * | 2012-08-29 | 2013-01-02 | 昆山铁牛衬衫厂 | 涤纶织物的阻燃整理方法 |
CN104744840B (zh) * | 2015-03-24 | 2017-11-03 | 合肥创新轻质材料有限公司 | 一种阻燃吸附母粒及其制备方法 |
CN106515145A (zh) * | 2016-08-31 | 2017-03-22 | 浙江兆新织造有限公司 | 一种防火抗菌消防服面料及其制备方法 |
CA3039666C (en) * | 2016-10-28 | 2022-08-23 | Ppg Industries Ohio, Inc. | Coatings for increasing near-infrared detection distances |
KR20210087991A (ko) | 2018-11-13 | 2021-07-13 | 피피지 인더스트리즈 오하이오 인코포레이티드 | 은닉 패턴을 검출하는 방법 |
US11561329B2 (en) | 2019-01-07 | 2023-01-24 | Ppg Industries Ohio, Inc. | Near infrared control coating, articles formed therefrom, and methods of making the same |
US11725337B2 (en) * | 2021-04-06 | 2023-08-15 | GM Global Technology Operations LLC | Flame retardant material and system |
CN113668081B (zh) * | 2021-07-20 | 2023-06-23 | 浙江理工大学 | 一种尼龙阻燃复合纤维的制备方法 |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4233199A (en) * | 1979-07-03 | 1980-11-11 | Visvaldis Abolins | Flame resistant thermoplastic compositions with well balanced physical properties |
CA1233009A (en) * | 1983-09-14 | 1988-02-23 | Cornell Whitley | High speed process for forming fully drawn polyester yarn |
JPH07145511A (ja) * | 1993-11-24 | 1995-06-06 | Nippon Ester Co Ltd | ポリエステルモノフィラメント |
JPH10140420A (ja) * | 1996-11-07 | 1998-05-26 | Japan Exlan Co Ltd | 無機微粒子含有繊維とその製造方法 |
JPH10182875A (ja) * | 1996-12-27 | 1998-07-07 | Ajinomoto Co Inc | 耐湿、耐熱性の改善された難燃性熱可塑性樹脂組成物 |
JP3993762B2 (ja) * | 2001-11-22 | 2007-10-17 | 株式会社カネカ | 難燃性ポリエステル系繊維及びそれを用いた人工毛髪 |
JP2003268155A (ja) * | 2002-03-13 | 2003-09-25 | Showa Denko Kk | リン化合物被覆フィラーおよびそれを用いた高分子複合材料 |
FR2843121B3 (fr) * | 2002-08-02 | 2004-09-10 | Rhodia Chimie Sa | Agent ignifugeant, procede de preparation et l'utilisation de cet agent |
-
2003
- 2003-06-27 FR FR0307825A patent/FR2856703B1/fr not_active Expired - Lifetime
-
2004
- 2004-06-25 CN CNB2004800212921A patent/CN100497766C/zh not_active Expired - Fee Related
- 2004-06-25 EP EP04767460A patent/EP1639160B1/de not_active Expired - Lifetime
- 2004-06-25 US US10/560,762 patent/US7758959B2/en not_active Expired - Fee Related
- 2004-06-25 WO PCT/FR2004/001612 patent/WO2005001173A2/fr active Application Filing
- 2004-06-25 JP JP2006516323A patent/JP4351250B2/ja not_active Expired - Fee Related
Also Published As
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EP1639160A2 (de) | 2006-03-29 |
CN1849420A (zh) | 2006-10-18 |
CN100497766C (zh) | 2009-06-10 |
FR2856703B1 (fr) | 2005-12-30 |
WO2005001173A3 (fr) | 2005-04-07 |
JP2007527470A (ja) | 2007-09-27 |
WO2005001173A2 (fr) | 2005-01-06 |
FR2856703A1 (fr) | 2004-12-31 |
JP4351250B2 (ja) | 2009-10-28 |
US7758959B2 (en) | 2010-07-20 |
US20060251895A1 (en) | 2006-11-09 |
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