CH364237A - Process for making textiles made of polyamide fibers flame-resistant when they are finished with stiff finishes - Google Patents
Process for making textiles made of polyamide fibers flame-resistant when they are finished with stiff finishesInfo
- Publication number
- CH364237A CH364237A CH296760A CH296760A CH364237A CH 364237 A CH364237 A CH 364237A CH 296760 A CH296760 A CH 296760A CH 296760 A CH296760 A CH 296760A CH 364237 A CH364237 A CH 364237A
- Authority
- CH
- Switzerland
- Prior art keywords
- contain
- aqueous treatment
- treatment baths
- stiff
- water
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 15
- 239000004753 textile Substances 0.000 title claims description 10
- 239000004952 Polyamide Substances 0.000 title claims description 9
- 229920002647 polyamide Polymers 0.000 title claims description 9
- 239000000835 fiber Substances 0.000 title claims description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 29
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000007859 condensation product Substances 0.000 claims description 16
- -1 methylol group Chemical group 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 9
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000003351 stiffener Substances 0.000 claims description 7
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 claims description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- QQOWHRYOXYEMTL-UHFFFAOYSA-N triazin-4-amine Chemical compound N=C1C=CN=NN1 QQOWHRYOXYEMTL-UHFFFAOYSA-N 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical compound O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 1
- 210000002700 urine Anatomy 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000008098 formaldehyde solution Substances 0.000 description 2
- 150000007974 melamines Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- VZXTWGWHSMCWGA-UHFFFAOYSA-N 1,3,5-triazine-2,4-diamine Chemical compound NC1=NC=NC(N)=N1 VZXTWGWHSMCWGA-UHFFFAOYSA-N 0.000 description 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- YZEZMSPGIPTEBA-UHFFFAOYSA-N 2-n-(4,6-diamino-1,3,5-triazin-2-yl)-1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(NC=2N=C(N)N=C(N)N=2)=N1 YZEZMSPGIPTEBA-UHFFFAOYSA-N 0.000 description 1
- FVFVNNKYKYZTJU-UHFFFAOYSA-N 6-chloro-1,3,5-triazine-2,4-diamine Chemical compound NC1=NC(N)=NC(Cl)=N1 FVFVNNKYKYZTJU-UHFFFAOYSA-N 0.000 description 1
- GZVHEAJQGPRDLQ-UHFFFAOYSA-N 6-phenyl-1,3,5-triazine-2,4-diamine Chemical compound NC1=NC(N)=NC(C=2C=CC=CC=2)=N1 GZVHEAJQGPRDLQ-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical group COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- SQSPRWMERUQXNE-UHFFFAOYSA-N Guanylurea Chemical compound NC(=N)NC(N)=O SQSPRWMERUQXNE-UHFFFAOYSA-N 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- YGCOKJWKWLYHTG-UHFFFAOYSA-N [[4,6-bis[bis(hydroxymethyl)amino]-1,3,5-triazin-2-yl]-(hydroxymethyl)amino]methanol Chemical class OCN(CO)C1=NC(N(CO)CO)=NC(N(CO)CO)=N1 YGCOKJWKWLYHTG-UHFFFAOYSA-N 0.000 description 1
- NJYZCEFQAIUHSD-UHFFFAOYSA-N acetoguanamine Chemical compound CC1=NC(N)=NC(N)=N1 NJYZCEFQAIUHSD-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- YSKUZVBSHIWEFK-UHFFFAOYSA-N ammelide Chemical compound NC1=NC(O)=NC(O)=N1 YSKUZVBSHIWEFK-UHFFFAOYSA-N 0.000 description 1
- MASBWURJQFFLOO-UHFFFAOYSA-N ammeline Chemical compound NC1=NC(N)=NC(O)=N1 MASBWURJQFFLOO-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- MQRJBSHKWOFOGF-UHFFFAOYSA-L disodium;carbonate;hydrate Chemical compound O.[Na+].[Na+].[O-]C([O-])=O MQRJBSHKWOFOGF-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- YSRVJVDFHZYRPA-UHFFFAOYSA-N melem Chemical compound NC1=NC(N23)=NC(N)=NC2=NC(N)=NC3=N1 YSRVJVDFHZYRPA-UHFFFAOYSA-N 0.000 description 1
- 150000005217 methyl ethers Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/423—Amino-aldehyde resins
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Description
Verfahren zum Flammfestmachen von Textilien aus Polyamidfasern beim Ausrüsten mit Steifappreturen Es ist bekannt, auf Textilien aus Polyamidfasern Steifappreturen herzustellen. Zu diesem Zweck wer dien die Textilien z.
B. reit wässerigen Bädern: behan delt, die als Steifappreturmittel wasserlösliche, gege benenfalls mit niedrigmolekularen aliphatischen Alko holen verätherte Harnstoff- oder Melamin-Forrn- aldehyd-Kondlensationsiprodukte und -H"ärtungskatal!y- satoren enthalten, und anschliessend einer Wärme behandlung unterworfen (vgl.
beispielsweise die fran- zösische Patentschrift Nr.<B>1</B>114 860<B>)</B>.
Es wurde gefunden, dass man Textilien aus, Poly- amidfas:ern beim Ausrästen mit Steifappreturen flammfest machen .kann;
wenn man wässerige Be handlungsbäder verwendet, die neben dem Steif- appreturmittet und einem Härtun:gskatalysator als flammfestmache-ndes Mittel mindestens ein wasser- lösliches, gegebenenfalls mit einem niedrigmolekula- ren aliphatischen Alkohol veräthertes Dimethylol- thi:
otriazon der Formel
EMI0001.0044
enthalten, worin X Für einen organischen Rest steht. Besonders gute Resultate werden bei Verwendung von wässerigen Behandlungsbädern erzielt, die neben dem Steifappreturmittel und Härtungskatalysator mindestens ein D.imethy.olthiotriazon der Formel
EMI0001.0053
enthalten, worin Y für einen Alkyl- oder Hydroxy- alkylnast mit höchstens 4 Kohlenstoffatomen steht.
Die wasserlöslichen, verätherten Dimethylol-thio- triazone der Formel
EMI0001.0063
worin R einen niedrigmolekularen aliphatischen Kohlenwasserstoffrest und X einen organischen Rest darstellen, sind entweder bekannt oder können nach an sich bekannten Methoden hergestellt werden, z. B.
durch Verätherung eines Dimethylolthiotriazons der Formel
EMI0002.0001
worin X die oben angegebene Bedeutung :besitzt, mit einem niedrigm:olekularen aliphatischen Alkohol, wie z. B. Methylalkohol, Äthylalkohol oder n Propyl- alkohol, in Gegenwart eines sauren Kondensations- mittels.
Die Dimethylol-thiotriazone dien Formel (4) erhält man in bekannter Weise dadurch, dass man Thio- harnstoff mit Formaldehyd und primären Aminen in der berechneten Menge bei Temperaturen von etwa 15 bis 50 C umsetzt.
Lässt man 1 Mol Thioharnstoff mit 1 Mol eines primären, höchstens 4 Kohlenstoffatome aufweisen den Alkyl-:oder I-T-ydiroxyalkylamnn:s, wie z.
B. Methyl- amin, Äthylamin, Isobutyl:amin oder Hydroxyäthyl- amin, und 4 Mol Formaldehyd reagieren, so gelangt man unmittelbar zu den für das vorliegende Verfah- ren besonders geeigneten -Dimiethylol-thiotriazonen der oben angegebenen Formel (2).
Als Steifappreturmittel kommen für das vorlie gende Verfahren wasserlösliche Kondensate, vorzugs- weise wasserlösliche Kondensationsprodukte aus Formaldehyd .und einem Aminotriazin oder Harnstoff in Betracht, die mindestens eine freie Methylolgruppe oder mindestens eine mit einem niedrigmolekularen aliphatischen Alkohol ver;
ätherte Methylolgruppe auf weisen. Derartige wasserlösliche Kondensationspro- dukte können bekanntlich monomere oder nicht zu weitgehend kondensierte Produkte oder Gemische beider sein.
A ix wasserlösliche Kondensationsprodukte aus Formaldehyd und einem Harnstoff, die mindestens eine freie Methylolgruppe oder mindestens eine mit einem niedrigmolekularen aliphatischen Alkohol ver- ätherte Methylolgruppe aufweisen, seien vor allem Kondensationsprodukte aus Harnstoff selbst,
Form- aldehydund' gegebenenfal s einem medrigmolekularen aliphatischen Alkohol, wie z.
B. Methylalkohol, Äthylalkohol oder n Butanol, :genannt. Es können gegebenenfalls mit einem niedtrigmolekularen alipha- tischen Alkohol verätherte Kondensationsprodukte aus Formaldehyd und Verbindungen mit der nicht- ringförmigen Atomgruppierung
EMI0002.0092
wie z.
B. Dicyandiamid, Dicyandiamidin oder Guanidin, als Steifappreturmittel verwendet werden.
Besonders geeignete Steifappreturmittel sind z. B. der D:imethyläther des Dimethylolharastoffes und die beschränkt wasserlöslichen Harnstoff-Formaldehyd- Kondensationsprodukte.
Unter dien wasserlöslichen Kondensationsproduk ten aus Formaldehyd und einem Aminotriazin seien insbesondere Umsetzungsprodukte von Formaldehyde und 2,4,6-Triamino-1,3,5-triazin, gewöhnlich; Melamin genannt, erwähnt. Solche Kondensationsprodukte kön nen Beine bis 6 Methylolgruppen enthalten, gewöhn lich stellen sie Mischungen von verschiedenen Verbinn dungen dar.
Weiterhin kommen Methylolverbindun- gen von solchen Abkömmlingen des Melamins in Betracht, die noch mindestens eine Aminogruppe ent- halten, z.
B. Metlhyl:olverbindu.ngen von Melam, Melem, Ammelin, Ammelid oder von halogensubsti tuierten Aminotriazinen, wie 2-Chlor 4,6-diamino- 1,3,5-triazin; ferner Methylolverbindungen von Guan- aminen, wie z. B. von Benzoguanamin, Acetoguan- amin odar Formoguanamin.
Die ebenfalls benützbaren Äther mit medrig- molekularen., aliphatischen Alkoholen können sich von den genannten Verbindungen und Methylalkohol, Äthylalkohol, Propylalkohol oder Butanolen ableiten. Zum Beispiel können Methyläther von Methylo:
l melaminen mit 3 bis 6 Methylolgruppen, in welchen 2 bis 6 Methyl.olgruppen veräthert sind, verwendet werden. Ein geeignetes Steifappreturmittel dieser Art ist z. B. das wasserlösliche, etwa 4 Methyläther- gruppen aufweisende Derivat des Hexamethylol- melamins oder das wasserlösliche, 2 Butyläthergrup- pen aufweisende Derivat dies Tetramethylolamins.
Die erfindiungs;gemäss zu verwendenden wässerigen Behandlung sbäd'er, die H'ärtungskatalysatoren wie z. B. Ammoniumnitrat, Ammoniumchlorid, Ammo- niumbromnid, Ammoniumsulfat, Magnes:iumchlorid, Zinknitrat oder Zinkchlorid aufweisen, enthalten pro Liter etwa 50 :bis 400 g Steifappreturmittel und etwa 70 bis 200 g Thiotriazonverbindung der Formel (3) oder (4).
Besonders gute Resultate werden :beispiels weise :bei Verwendung von wässerigen Behandlungs bädern erzielt, die pro Liter etwa 200 g eines. be schränkt wasserlöslichen Harnstoff Formaldehyd@Kon- densationsproduktes als Sbeifappreturmittel, etwa 85 g D:imethylol-thiotriazon der Formel
EMI0002.0182
und etwa 4,5g Ammoniumsul'fat enthalten.
Die Textilien aus Polyamidfasern werden mit diesen Bädern, die sich im allgemeinen durch eine besonders hohe Stabilität auszeichnen, .in üblicher Weise getränkt, auf etwa 50 bis 10011/a Gewichts zunahme abgepresst und gegebenenfalls nach dem Trocknen bei erhöhter Temperatur einer Hitzebehand- lung, z. B. bei etwa<B>100</B> bis 160 C, unterworfen.
Die nach dem vorliegenden Verfahren erhältlichen Textilien aus Po@lyamidfasern besitzen einen steifen Griff und eine sehr gute Flammfestigkeit, die z. B. auch nach einer Wäsche bei 75 C mit sulfonat- und natriumcarbonathaltigem Wasser erhalten bleiben.
Im nachfolgenden Beispiel bedeuten Teile, sofern nichts anderes angegeben wird, Gewichtsteile und die Prozente Gewichtsprozente.
<I>Beispiel</I> Man tränkt ein Polyamidgewebe (aus Nylonfasern) mit einem wässerigen Bade, das zusammengesetzt ist aus 595,5 Teilen Wasser, 200 Teilen einer etwa 43 o/oigen wässerigen Lösung des D.imethylol-tho- triazons der Formel
EMI0003.0029
200 Teilen eines beschränkt wasserlöslichen Harn- stoff-Formaldehyd-Kondensationsproduktes und 4,5 Teilen Ammoniumsulfat,
presst auf 70 % Gewichts- zunahme ab, trocknet auf einem Nadelrahmen und härtet 41/2 Minuten bei 150 C.
Es wird ein Gewebe erhalten:, das eine bestän- d'ige Steifappretur und eine sehr gute Flammfestigkeit besitzt.
Nach einer Wäsche in einem Bad, (15 Minuten bei 75 C), das 2 .g/Liter eines Sulfonatwaschmittels und 2 g/Liter wasserfreies Natriumcarbonat enthält, bleiben die Steifappretur und die Flammfestigkeit erhalten.
Das in diesem Beispiel verwendete beschränkt wasserlösliche Harnstoff-Formaldehyd-Kondensations- produkt kann wie folgt hergestellt werden: Harnstoff (1 Mol) wird mit wässeriger Form aldehydlösung (etwas mehr als 2 Mol) anfänglich bei einem pH-Wert von 5,8 bis 6,3, dann, von 7,0 bis 7,2 unter schwachem Überdruck auf etwa 100 C erhitzt. Die erhaltene Lösung wird eingeengt und dann .im Zerstäubungstrockner vom restliche Lö sungsmittel befreit.
Die obengenannte, etwa 43 -o/aige wässerige Lö sung .des. Dimethylol-thiotriazons der Formel (a) wird erhalten, wenn man 76 Teile Thioharnstoff (1 Mol), 325 Teile einer 37 o/oigen wässerigen Formaldehyd, Lösung (4 Mol) und 65 Teile einer 69,5o/uigen wässe rigen Athylaminlösung (1 Mol) ,
etwa 4 bis 5 Stunden bei 40 bis 45 C reagieren lässt.
Process for making textiles made of polyamide fibers flame resistant when they are finished with stiff finishes. It is known to produce stiff finishes on textiles made of polyamide fibers. For this purpose who serve the textiles z.
B. reit aqueous baths: treated which contain water-soluble urea or melamine formaldehyde condensation products and hardening catalysts as stiff finishing agents, if necessary urea or melamine formaldehyde condensation products and hardening catalysts, and are then subjected to a heat treatment see.
for example the French patent specification no. <B> 1 </B> 114 860 <B>) </B>.
It has been found that textiles made from polyamide fibers can be made flame-resistant when milling with stiff finishes;
if you use aqueous treatment baths which, in addition to the stiffening agent and a hardening catalyst as a flame-retardant agent, have at least one water-soluble dimethylol thi, optionally etherified with a low molecular weight aliphatic alcohol:
otriazon of the formula
EMI0001.0044
contain, wherein X stands for an organic radical. Particularly good results are achieved when using aqueous treatment baths which, in addition to the stiffening agent and curing catalyst, contain at least one D.imethy.olthiotriazon of the formula
EMI0001.0053
contain, in which Y stands for an alkyl or Hydroxyalkylnast with at most 4 carbon atoms.
The water-soluble, etherified dimethylol-thio-triazone of the formula
EMI0001.0063
where R is a low molecular weight aliphatic hydrocarbon radical and X is an organic radical are either known or can be prepared by methods known per se, e.g. B.
by etherification of a dimethylolthiotriazone of the formula
EMI0002.0001
wherein X has the meaning given above: with a low molecular weight aliphatic alcohol, such as. B. methyl alcohol, ethyl alcohol or n propyl alcohol, in the presence of an acidic condensation agent.
The dimethylol-thiotria zone of formula (4) is obtained in a known manner by reacting thiourea with formaldehyde and primary amines in the calculated amount at temperatures of about 15 to 50.degree.
If one mole of thiourea with 1 mole of a primary, at most 4 carbon atoms, has the alkyl-: or I-T-ydiroxyalkylamnn: s, such as e.g.
B. methylamine, ethylamine, isobutyl: amine or hydroxyethylamine, and 4 moles of formaldehyde react, then one arrives directly at the -dimiethylol-thiotriazones of the formula (2) given above, which are particularly suitable for the present process.
Water-soluble condensates, preferably water-soluble condensation products of formaldehyde and an aminotriazine or urea, which contain at least one free methylol group or at least one with a low molecular weight aliphatic alcohol, are suitable as stiffening agents for the present process;
ethereal methylol group. Such water-soluble condensation products can, as is known, be monomeric or not too largely condensed products or mixtures of the two.
A ix water-soluble condensation products of formaldehyde and a urea, which have at least one free methylol group or at least one methylol group etherified with a low molecular weight aliphatic alcohol, are above all condensation products of urea itself,
Formaldehyde and 'optionally s a medium-molecular aliphatic alcohol, such as.
B. methyl alcohol, ethyl alcohol or n butanol,: called. If appropriate, condensation products of formaldehyde and compounds with the non-ring-shaped atom group, etherified with a low molecular weight aliphatic alcohol, can be used
EMI0002.0092
such as
B. dicyandiamide, dicyandiamidine or guanidine, can be used as a stiff finishing agent.
Particularly suitable stiff finishing agents are e.g. B. the D: imethyl ether of Dimethylolharastoffes and the limited water-soluble urea-formaldehyde condensation products.
Among the water-soluble condensation products of formaldehyde and an aminotriazine, in particular, reaction products of formaldehyde and 2,4,6-triamino-1,3,5-triazine are common; Called melamine, mentioned. Such condensation products can contain legs up to 6 methylol groups; they are usually mixtures of different compounds.
Methylol compounds of those derivatives of melamine which still contain at least one amino group are also suitable, e.g.
B. Methyl: oil compounds of melam, melem, ammeline, ammelide or of halogen-substituted aminotriazines, such as 2-chloro 4,6-diamino-1,3,5-triazine; also methylol compounds of guanamines, such as. B. of benzoguanamine, acetoguanamine or formoguanamine.
The ethers with medium-molecular, aliphatic alcohols that can also be used can be derived from the compounds mentioned and methyl alcohol, ethyl alcohol, propyl alcohol or butanols. For example, methyl ethers of methylo can:
l melamines with 3 to 6 methylol groups in which 2 to 6 methylol groups are etherified can be used. A suitable stiff finishing agent of this type is e.g. B. the water-soluble derivative of hexamethylol melamine, which has about 4 methyl ether groups, or the water-soluble derivative of tetramethylolamine, which has 2 butyl ether groups.
The aqueous treatment to be used according to the invention, the curing catalysts such. B. ammonium nitrate, ammonium chloride, ammonium bromnide, ammonium sulfate, magnesium chloride, zinc nitrate or zinc chloride, contain about 50 to 400 g of stiff finishing agent and about 70 to 200 g of thiotriazone compound of formula (3) or (4) per liter.
Particularly good results are achieved: for example: when using aqueous treatment baths that contain around 200 g of one per liter. limited water-soluble urea formaldehyde @ condensation product as a finishing agent, about 85 g of D: imethylol-thiotriazon of the formula
EMI0002.0182
and contain about 4.5g ammonium sulphate.
The textiles made of polyamide fibers are soaked in the usual way with these baths, which are generally characterized by particularly high stability, pressed to an increase in weight of about 50 to 10011 / a and, optionally after drying at an elevated temperature, a heat treatment, e.g. . B. at about <B> 100 </B> to 160 C.
The textiles available by the present process made of polyamide fibers have a stiff handle and very good flame resistance, which z. B. be retained even after washing at 75 C with sulfonate and sodium carbonate water.
In the following example, parts are parts by weight and the percentages are percentages by weight, unless otherwise specified.
<I> Example </I> A polyamide fabric (made of nylon fibers) is soaked in an aqueous bath that is composed of 595.5 parts of water, 200 parts of an approximately 43% aqueous solution of the D.imethylol-thotriazone formula
EMI0003.0029
200 parts of a urea-formaldehyde condensation product with limited water solubility and 4.5 parts of ammonium sulfate,
Presses to a 70% weight gain, dries on a needle frame and cures for 41/2 minutes at 150 C.
A fabric is obtained which has a permanent stiff finish and very good flame resistance.
After washing in a bath (15 minutes at 75 ° C.) which contains 2 g / liter of a sulfonate detergent and 2 g / liter of anhydrous sodium carbonate, the stiff finish and flame resistance are retained.
The urea-formaldehyde condensation product with limited water solubility used in this example can be prepared as follows: Urea (1 mol) is mixed with aqueous formaldehyde solution (slightly more than 2 mol) initially at a pH of 5.8 to 6, 3, then, heated from 7.0 to 7.2 under a slight excess pressure to about 100 ° C. The solution obtained is concentrated and then freed from the remaining solvent in the spray dryer.
The above-mentioned, about 43-o / aige aqueous solution .des. Dimethylol-thiotriazons of the formula (a) are obtained if 76 parts of thiourea (1 mol), 325 parts of a 37% aqueous formaldehyde solution (4 mol) and 65 parts of a 69.5% aqueous ethylamine solution (1 Mole),
lets react for about 4 to 5 hours at 40 to 45 C.
Claims (1)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| BE601360D BE601360A (en) | 1960-03-16 | ||
| CH296760A CH364237A (en) | 1960-03-16 | 1960-03-16 | Process for making textiles made of polyamide fibers flame-resistant when they are finished with stiff finishes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH296760A CH364237A (en) | 1960-03-16 | 1960-03-16 | Process for making textiles made of polyamide fibers flame-resistant when they are finished with stiff finishes |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CH364237A true CH364237A (en) | 1962-04-30 |
Family
ID=4245661
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CH296760A CH364237A (en) | 1960-03-16 | 1960-03-16 | Process for making textiles made of polyamide fibers flame-resistant when they are finished with stiff finishes |
Country Status (2)
| Country | Link |
|---|---|
| BE (1) | BE601360A (en) |
| CH (1) | CH364237A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2314214A1 (en) * | 1972-03-23 | 1973-10-04 | Toray Industries | METHOD FOR MANUFACTURING MELT RESISTANT SYNTHETIC FIBERS |
-
0
- BE BE601360D patent/BE601360A/xx unknown
-
1960
- 1960-03-16 CH CH296760A patent/CH364237A/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2314214A1 (en) * | 1972-03-23 | 1973-10-04 | Toray Industries | METHOD FOR MANUFACTURING MELT RESISTANT SYNTHETIC FIBERS |
Also Published As
| Publication number | Publication date |
|---|---|
| BE601360A (en) |
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