DK146450B - PROCEDURE FOR COLORING WINNED TEXTILE MATERIALS OF SYNTHETIC FIBER OR SYNTHETIC FIBER MIXTURES - Google Patents
PROCEDURE FOR COLORING WINNED TEXTILE MATERIALS OF SYNTHETIC FIBER OR SYNTHETIC FIBER MIXTURES Download PDFInfo
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- DK146450B DK146450B DK082474AA DK82474A DK146450B DK 146450 B DK146450 B DK 146450B DK 082474A A DK082474A A DK 082474AA DK 82474 A DK82474 A DK 82474A DK 146450 B DK146450 B DK 146450B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/82—Textiles which contain different kinds of fibres
- D06P3/8204—Textiles which contain different kinds of fibres fibres of different chemical nature
- D06P3/8223—Textiles which contain different kinds of fibres fibres of different chemical nature mixtures of fibres containing hydroxyl and ester groups
- D06P3/8238—Textiles which contain different kinds of fibres fibres of different chemical nature mixtures of fibres containing hydroxyl and ester groups using different kinds of dye
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B21/00—Successive treatments of textile materials by liquids, gases or vapours
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B5/00—Forcing liquids, gases or vapours through textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing impregnating
- D06B5/12—Forcing liquids, gases or vapours through textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing impregnating through materials of definite length
- D06B5/16—Forcing liquids, gases or vapours through textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing impregnating through materials of definite length through yarns, threads or filaments
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
- D06P3/54—Polyesters using dispersed dyestuffs
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/20—Physical treatments affecting dyeing, e.g. ultrasonic or electric
- D06P5/2022—Textile treatments at reduced pression, i.e. lower than 1 atm
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/20—Physical treatments affecting dyeing, e.g. ultrasonic or electric
- D06P5/2066—Thermic treatments of textile materials
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Coloring (AREA)
- Treatment Of Fiber Materials (AREA)
Description
V R&>V R &>
(19) DANMARK(19) DENMARK
§(12) FREMLÆGGELSESSKRIFT (n) 146450 B§ (12) PUBLICATION (s) 146450 B
DIREKTORATET FOR PATENT- OG VAREMÆRKEVÆSENETDIRECTORATE OF THE PATENT AND TRADEMARKET SYSTEM
(21) Patentansøgning nr.: 0824/74 (51) Inl.CL3: D06B 5/12 (22) Indleveringsdag: 15 feb 1974 D 06 P 5/00 (41) Aim. tilgængelig: 23 dec 1974 (44) Fremlagt: 10 okt 1983 (86) International ansøgning nr.:- (30) Prioritet: 22jun 1973 DE 2331669 (71) Ansøger: *HOECHST AKTIENGESELLSCHAFT; 6230 Frankfurt am Main 80; DE.(21) Patent Application No .: 0824/74 (51) Filing Date CL3: D06B 5/12 (22) Filing Date: 15 Feb 1974 D 06 P 5/00 (41) Aim. available: 23 Dec 1974 (44) Submitted: 10 Oct 1983 (86) International Application No :- (30) Priority: 22 Jun 1973 DE 2331669 (71) Applicant: * HOECHST AKTIENGESELLSCHAFT; 6230 Frankfurt am Main 80; THE.
(72) Opfinder: Hans-Uirich von der *Eltz; DE, Albert *Reuther; DE, Hans-Joachim ‘Wassmuth; DE.(72) Inventor: Hans-Uirich von der * Eltz; DE, Albert * Reuther; DE, Hans-Joachim 'Wassmuth; THE.
(74) Fuldmægtig: Ingeniørfirmaet Budde, Schou & Co (54) Fremgangsmåde til farvning af opviklede tekstilmaterialer af syntetfibre eller syntet-fiberblandinger(74) Plenipotentiary: Engineering Company Budde, Schou & Co (54) Process for dyeing wrapped textile materials of synthetic fibers or synthetic-fiber blends
Fremgangsmåder til farvning af syntetfibre ved udtrækningsfremgangsmåder under højtemperatur(HT)-betingelser har længe været kendt i talrige variationer.Methods of dyeing synthetic fibers by extraction methods under high temperature (HT) conditions have long been known in numerous variations.
Den foreliggende opfindelse angår en fremgangsmåde til farvning af opviklede tekstilmaterialer af syntetfibre eller af blan-® dinger, der indeholder sådanne syntetiske fibre, med vanduopløselige ® dispersionsfarvestoffer ved udtrækningsmetoden, ved temperaturer på J 110-145°C, ved hvilken fremgangsmåde de opviklede emner opvarmes i en tryktæt farvebeholder før farvningen og afluftes samt dernæst ^ bringes i kontakt med den i en blandingsbeholder separat til 110- Q -145°C opvarmede samlede farveflotte, som er sat under et relativt overtryk på 5-10 atm (= 4,9-9,8 bar), ved at farveflotten fra bian- 2 146450 dingsbeholderen føres over i farvebeholderen, hvorefter farvebe-handlingen føres til ende ved cirkulation af farveflotten.The present invention relates to a method of dyeing wound textile materials of synthetic fibers or of mixtures containing such synthetic fibers, with water-insoluble® dispersion dyes by the extraction method, at temperatures of J 110-145 ° C, by which process the wound articles are heated. in a pressure-tight color container prior to dyeing and deaerating and then contacting the combined color tank heated separately at 110 ° C -145 ° C, which is placed under a relative overpressure of 5-10 atm (= 4.9 ° C). 9.8 bar) by transferring the color fleet from the intermediate container into the color container, after which the color processing is terminated by circulation of the color fleet.
En sådan fremgangsmåde er beskrevet i DE-offentlig-gørelsesskrift nr. 1.785.278 og 2.203.401. Ifølge den derfra kendte teknik sker afluftningen, ved at behandlinqsbeholderen ocr tekstilmaterialet sættes under vakuum. Dette sker i den hensigt at kunne overføre den varme behandlingsflotte fra blandingsbeholderen til behandlingsbeholderen så modstandsløst og hurtigt som muligt. Da man i anlæg af en teknisk praktisk størrelse ved hjælp af vakuumpumper kun kan opnå et delvis vakuum, er der stadigvæk et resttryk tilbage, som giver en vis modstand.Such a process is disclosed in DE Publication No. 1,785,278 and 2,203,401. According to the prior art, deaeration is effected by vacuum treatment of the treatment container and the textile material. This is done in order to be able to transfer the hot treatment float from the mixing container to the treatment container as resiliently and quickly as possible. Since only a partial vacuum can be obtained in systems of a technically practical size with the help of vacuum pumps, there is still a residual pressure which gives some resistance.
Vakuum fører desuden uundgåeligt til en stærk afkøling af det samlede system som følge af luftens udvidelse eller fordampning af fugtighed, hvadenten det er fra tekstilmaterialet eller fra vedhæftende flotte. Dette er også tilfældet, når systemet (apparat og tekstilmateriale) er blevet forvarmet før evakueringen, f.eks. ved hjælp af vanddamp. Der opstår en væsentlig temperaturforskel mellem vare og flotte, hvilket giver anledning til store uegaliteter ved den hurtige kontakt.In addition, vacuum inevitably leads to a strong cooling of the overall system due to the expansion of the air or the evaporation of moisture, whether from the textile material or from the adhesive float. This is also the case when the system (apparatus and textile material) has been preheated before the evacuation, e.g. using water vapor. There is a significant difference in temperature between product and good looking, which gives rise to large irregularities in the fast contact.
Ifølge FR-patentskrift nr. 1.067.236 imødegås denne kendte fejlkilde ved en yderligere opvarmning af det våde tekstilmateriale ved hjælp af højfrekvensstrøm.According to FR Patent No. 1,067,236, this known source of error is countered by a further heating of the wet textile material by high frequency current.
Det har nu vist sig, at man kan opnå særlig egale farvninger selv med kombinationer af flere farvestoffer, der ellers er vanskelige at farve med, samt ved samtidig væsentlig farvetids-afkortelse på opviklede emner af syntetfibre eller af blandinger, der indeholder sådanne syntetiske fibre, med vanduopløselige dispersionsfarvestoffer ved en højtryks-udtrækningsmetode, som ikke lider af de ovenfor omtalte ulemper.It has now been found that even uniform dyes can be obtained even with combinations of several dyes which are otherwise difficult to dye, and at the same time substantial color-time shortening on wound articles of synthetic fibers or of mixtures containing such synthetic fibers. with water-insoluble dispersion dyes by a high-pressure extraction method which does not suffer from the disadvantages mentioned above.
Dette sker ifølge opfindelsen ved en fremgangsmåde, som er ejendommelig ved, at opvarmningen og afluftningen af de opviklede emner sker ved, at de umiddelbart før overføringen af farveflotten udsættes for en atmosfære af varm damp, som har ca. farvetemperatur, og at farveflotten via stort dimensionerede rørledninger i løbet af 3-60 sekunder ledes samtidigt såvel indefra som udefra ind i de opviklede emner imod trykket af den luftfrie atmosfære af varm damp.This is done according to the invention by a method which is characterized in that the heating and venting of the wound objects are done by exposing them immediately before the transfer of the color fleet to an atmosphere of hot steam which has approx. color temperature and that the color fleet is passed through large-dimensioned pipelines within 3-60 seconds at the same time, both internally and externally, into the wound elements against the pressure of the air-free atmosphere of hot steam.
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Den udslaggivende forskel i princippet ifølge opfindelsen og den i DE-offentliggørelsesskrifter nr. 1.785.278 og 2.203.401 beskrevne teknik består i, at farvebeholderen ikke evakueres, men fyldes med mættet højtryksdamp af omtrent samme temperatur, som anvendes ved den efterfølgende farveproces, indtil temperaturen er udlignet. Farvebeholderen indeholder altså altid en atmosfære af damp. Ved den hurtige overledning af farveflotten, som ligeledes står under et højt tryk, fra blandingsbeholderen over i farvebeholderen kondenseres dampen i sidstnævnte restfrit som følge af den påførte trykforskel, hvorved der endog frigøres kondensationsvarme. Der sker altså ingen temperatursænkning, der som ovenfor beskrevet kan virke forstyrrende.The decisive difference in principle of the invention and of the technique described in DE Publication Nos. 1,785,278 and 2,203,401 is that the color container is not evacuated, but filled with saturated high pressure vapor of about the same temperature used in the subsequent color process until the temperature is equalized. The color container therefore always contains an atmosphere of steam. At the rapid transfer of the color fleet, which is also under high pressure, from the mixing vessel into the color container, the vapor in the latter residual is condensed as a result of the applied pressure difference, thereby even releasing the heat of condensation. There is thus no temperature decrease, which as described above can be disruptive.
Foruden at tekstilmaterialet i forvejen udsættes for damp til opvarmning af de opviklede emner til farvetemperatur, har det ved fremgangsmåden ifølge opfindelsen desuden vist sig at være væsentligt, at den i forvejen opvarmede flotte samtidig skydes ind i de opviklede emner både indefra og udefra, på den ene side for at opnå en ensartethed i farvningen, på den anden side for at skåne emnerne. Kun på denne måde er en isotermisk hurtigfarvning på opviklede emner af syntetiske fibre mulig med egalt farvningsresultat.In addition to the textile material already being exposed to steam to heat the wound items to color temperature, it has also been found in the method according to the invention that the pre-heated raft is simultaneously pushed into the wound items both from the inside and the outside, on the one side to achieve a uniformity in coloration, on the other hand to spare the items. Only in this way is isothermal rapid staining on wound synthetic fiber blanks possible with uniform staining result.
I modsætning hertil er det ved den kendte fremgangsmåde i forvejen givet, at den indskudte flottes strømningsretning i emnerne er indefra og udefter (som følge af det pålagte vakuum), og den sker ensidigt og forskelligt svarende til de foreliggende forskelle i viklingernes tæthed og under samtidigt ligeledes forskellig afkøling og tilsvarende nedgang i flottens farvestofindhold. Resultatet er, først og fremmest ved lyse nuancer, en uegalitet i farvningen, som ikke mere kan fjernes. Erfaringsmæssigt kan meget lyse farvetoner overhovedet ikke bruges til upåklagelig farvning ved vakuummetoden. En yderligere påviselig ulempe ved vakuumteknikken er den ukontrollerbare deformation af de opviklede emner og påvirkningen af det først og fremmest højfølsomme teksturede tekstilmateriale, som skal farves.In contrast, in the known method, it is given in advance that the flow direction of the inserted fleet in the blanks is from inside and out (due to the applied vacuum) and it occurs unilaterally and differently according to the present differences in the density of the windings and at the same time. also different cooling and corresponding decrease in the dye content of the float. The result is, first and foremost, by light shades, an inequality in the staining that can no longer be removed. Experience shows that very bright tones cannot be used at all for impeccable staining by the vacuum method. A further demonstrable disadvantage of the vacuum technique is the uncontrollable deformation of the wound items and the influence of the primarily highly sensitive textured textile material to be dyed.
De overfor omtalte ulemper undgås ved den her omhandlede fremgangsmåde. Ved i forvejen at udsætte tekstilmaterialet for damp afluftes det ikke alene, men først og fremmest opvarmes det til farvetemperaturen, hvilket sidste også gælder for apparaturet. Derved udelukkes de temperaturforskelle, som optræder ved tilledning af opvarmede farveflotter ved vakuumteknikken, og som bevirker store affinitetsforskelle, først og fremmest ved temperaturer på over 100°C. Ved den her omhandlede fremgangsmåde møder farveflotten samme temperaturbetingelser overalt og afkøles altså ikke lokalt.The disadvantages mentioned above are avoided by the method of the present invention. By exposing the textile material to steam in advance, it is not only vented, but first and foremost it is heated to the color temperature, which lastly applies to the apparatus as well. This eliminates the temperature differences that occur in the supply of heated color floats by the vacuum technique and which cause large affinity differences, primarily at temperatures above 100 ° C. In the process of the present invention, the color fleet meets the same temperature conditions everywhere and is thus not cooled locally.
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Tilfældigheder i strømningsvejene ved vakuummetoden imødegås ved den her omhandlede fremgangsmåde bevidst ved, at farve-flotten trykkes ind samtidigt både indefra og udefra, hvortil kommer, at cirkulationspumpen sættes i gang, endnu medens flotten trykkes ind i det materiale, som skal farves. De opviklede emner udsættes altså kun for strømningstrykforskelle, men ikke for den høje trykforskel mellem blandingsbeholder og vakuum. Trykket i farvebeholderen er alene bestemt af flottens temperatur. En trykforskel opstår kun som følge af en forskel i trykket i blandingsbeholderen og det damptryk, som er givet af flottens temperatur. Da denne trykforskel virker på de opviklede emner såvel indefra og udefter som den modsatte vej, behøver man altså ikke at frygte en deformation af emnerne.Coincidences in the flow paths by the vacuum method are deliberately countered by the method of the present invention by pressing the color float simultaneously at both the inside and the outside, in addition to the circulation pump being started, while the float is being pressed into the material to be dyed. Thus, the wound items are exposed only to flow pressure differences, but not to the high pressure difference between the mixing vessel and vacuum. The pressure in the color container is solely determined by the temperature of the float. A pressure difference only arises from a difference in the pressure in the mixing vessel and the vapor pressure given by the temperature of the float. As this difference in pressure acts on the wound elements both from the inside and the outside as well as the opposite way, there is no need to fear a deformation of the blanks.
Den foreliggende opfindelses princip består i, at en farveflotte anbringes i en HT-beholder med de valgte tryk- og temperaturbetingelser og derfra ved hjælp af tryk (trykdamp, trykluft, pumpetryk) ledes over i en anden autoklav, der er fyldt med damp samt med de opviklede emner af syntetfibre, f.eks. opspolede filamenter eller stykvareruller på farvebomme. Dette sker således, at man via tilsvarende stort dimensionerede rørledninger, pumper og en fordelerventil presser flotten samtidigt såvel indefra som udefra ind i de opviklede emner. På denne måde lykkes det selv ved teksturerede syntettråde at fordele flotten ensartet i det materiale, der skal farves, på ekstremt kort tid uden deformering af ruller og filamenter. Til dette kræves der tidsrum på mindre end 60 sekunder, for det meste endog mindre end 30 sekunder. Denne hurtige "indskydning" af farve-flotten opnås ved et højt pressetryk på blandingsbeholderens side (trykforskel 5-10 atm), hvilket ifølge opfindelsen.mest hensigtsmæssigt frembringes ved hjælp af trykluft. Farvebeholderen befries i forvejen for indesluttet luft med trykdamp, og varen forvarmes samtidig. Tekstilmaterialet kan være tørt eller forvasket, hvilket kan foregå i selve farvebeholderen.The principle of the present invention is that a color float is placed in an HT container with the selected pressure and temperature conditions and from there conveyed by pressure (vapor, compressed air, pump pressure) to another autoclave filled with steam and with the wound fibers of synthetic fibers, e.g. coiled filaments or piece rolls on color bars. This is done by pushing the raft simultaneously, both internally and externally, into the wound elements via similarly large dimensioned pipelines, pumps and a distributor valve. In this way, even with textured synthetic threads, the float is evenly distributed in the material to be dyed in an extremely short time without deformation of rolls and filaments. This requires time of less than 60 seconds, usually even less than 30 seconds. This rapid "push-in" of the color fleet is achieved by a high pressure on the side of the mixing vessel (pressure difference 5-10 atm), which according to the invention is most conveniently produced by compressed air. The color container is pre-frozen for trapped air with pressure vapor, and the product is preheated at the same time. The textile material can be dry or pre-washed, which can take place in the color container itself.
Farvebeholderen er tryktæt, godt isoleret og forsynet med en varmeveksler med høj kapacitet for at kunne holde farvetemperaturen konstant. Selve flotten opvarmes i blandingsbeholderen til ca. 140°C og presses derpå ind i den dampfyldte farvebe-holder. Inden for rammerne af denne proces kan farvebeholderen, for så vidt der hersker en tilsvarende forskel i trykket, også fyldes fuldstændigt ved lukket ventil, fordi den i forvejen tilstedeværende damp kondenserer med stigende tryk.The color container is pressure-proof, well insulated and equipped with a high capacity heat exchanger to keep the color temperature constant. The float itself is heated in the mixing vessel to approx. 140 ° C and then pressed into the vapor-filled color container. Within the scope of this process, the color container, insofar as there is a corresponding difference in pressure, can also be completely filled by closed valve because the vapor present in it condenses with increasing pressure.
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En særlig udførelsesform for fremgangsmåden ifølge opfindelsen er ejendommelig ved, at de opviklede emner udsættes for en mættet vanddampatmosfære, og at farvebeholderen er tilsluttet en blokerbar kondensationsledning til forøgelse af det relative overtryk, hvorved det igen er muligt at fylde farvebeholderen helt med farvestoftilberedningen ved lukket afluft-ningsventil.A particular embodiment of the process according to the invention is characterized in that the wound items are exposed to a saturated water vapor atmosphere and that the color container is connected to a blockable condensation line to increase the relative overpressure, which in turn makes it possible to completely fill the color container with the dye preparation at closed air. -ningsventil.
Efter at den samlede farveflotte befinder sig i farvebeholderen, altså efter afsluttet indskydning, pumpes farvebadet ved hjælp af en cirkulationspumpe skiftevis indefra og udefter og udefra og indefter gennem materialerullen. Den valgte farvetemperatur opretholdes samtidigt. Pra nu af sker den endelige fiksering af farvestoffet på kort tid. Ved de under disse temperaturbetingelser høje udtrækningshastigheder er det fordelagtigt at arbejde med tilstrækkelig høje transportydelser af pumpen. Over 60 liter/kg/min fremkommer der gode farveresultater. Ved farvestoffer eller farvestofkombinationer, hvormed det er vanskeligere at farve egalt, skal der arbejdes med en transportydelse på mere end 80 liter/kg/min.After the entire color float is in the color container, that is, after completion of the insertion, the dye bath is pumped alternately from the inside and the outside and from the outside and in through the material roll by means of a circulation pump. The selected color temperature is maintained at the same time. Now, the final fixation of the dye will take place in a short time. At the high extraction rates under these temperature conditions, it is advantageous to work with sufficiently high transport services of the pump. Over 60 liters / kg / min good color results are obtained. For dyes or dye combinations, which make it more difficult to color evenly, a transport performance of more than 80 liters / kg / min must be worked.
Ved det ejendommelige træk, at den samlede farveflotte føres ind i farvebeholderen med stor hastighed og ind i det mere eller mindre tørre materiale i form af opviklede emner, adskiller fremgangsmåden sig fra de hidtil gennemførte HT-farveprocesser, der sammen med deres fremgangsmådevarianter er blevet grundigt behandlet i litteraturen. Ifølge opfindelsen bringes altså f.eks. ikke kun en del af farveflotten eller en koncentreret farvestofdispersion ind i farvebeholderen, men den samlede farveflotte presses ind næsten slagagtigt. At der kan opnås egale farvninger under disse betingelser har ikke været forudseeligt, da alle dispersionsfarvestoffer har en overordentlig høj udtrækningsevne ved disse temperaturer.By the peculiar feature of introducing the entire color fleet into the color container at high speed and into the more or less dry material in the form of coiled blanks, the method differs from the hitherto color processes performed so far, which, together with their process variants, have been thoroughly addressed in the literature. Thus, according to the invention, e.g. not only a portion of the color fleet or a concentrated dye dispersion into the color container, but the overall color fleet is pressed in almost stroke. It is not foreseeable that even staining under these conditions can be achieved, as all dispersion dyes have an extremely high drawability at these temperatures.
Det kunne endvidere ikke forventes, at farvestofopløsningerne ved så høje temperaturer, trykforskelle og mulige turbulenser stadig er egnede til indtrængning i opviklede emner. Det er endvidere overraskende, at farvestofdispersionerne også ved kombination af flere dispersionsfarvestoffer forbliver stabile tinder disse skærpede apparative betingelser og ikke har tilbøjelighed til agglornerering.Furthermore, at such high temperatures, pressure differences and possible turbulences, it is not expected that the dye solutions are still suitable for penetration into wound subjects. Furthermore, it is surprising that even when combining several dispersion dyes, the dye dispersions remain stable, pinning these aggravated operative conditions and not prone to agglomeration.
Den kendsgerning, at farvestoffernes udtrækningsevne kan udnyttes fuldstændigt ved de anvendte høje temperaturer, viser sig at være en væsentlig fordel ved den her omhandlede fremgangsmåde.The fact that the extraction ability of the dyes can be fully utilized at the high temperatures used, is found to be a significant advantage of the process of the present invention.
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Den beskrevne fremgangsmåde gennemføres normalt i vandigt medium. Den kan dog også uden videre anvendes til farvning ud fra organiske opløsningsmidler. I sidstnævnte tilfælde skal man selvfølgelig ved fremgangsmådebetingelserne tage hensyn til det for det pågældende opløsningsmiddel typiske kogepunkt samt dets damptryk.The process described is usually carried out in aqueous medium. However, it can also easily be used for coloring based on organic solvents. In the latter case, of course, the process conditions must take into account the boiling point typical of the particular solvent and its vapor pressure.
Som farvestoffer anvendes ifølge fremgangsmåden de gængse handelsmærker af dispersionsfarvestoffer i pulverform eller flydende præparater. Sådanne farvestoffer er beskrevet i Colour Index, 3. oplag, bind 2 under klassebetegnelsen "Disperse Dyes".As the dyes, the conventional trademarks of dispersion dyes in powder or liquid formulations are used. Such dyes are described in Color Index, 3rd edition, Volume 2 under the class designation "Disperse Dyes".
Egnede til gennemførelsen af den her omhandlede fremgangsmåde er samtlige fiberarter af syntetisk oprindelse i enhver forarbejdningsform, som kan farves ved HT-farvemetoden. Den hidtil ukendte fremgangsmåde anvendes imidlertid fortrinsvis til teksturerede fibre af polyamid- og af lineært polyestermateriale, fordi sådanne fibre er særlig tilbøjelige til at blive farvet uegalt som følge af deres termiske forbehandling ved tekstureringen.Suitable for carrying out the process of this invention are all synthetic fiber fibers in any processing form which can be stained by the HT staining method. However, the novel method is preferably used for textured fibers of polyamide and of linear polyester material because such fibers are particularly prone to being stained unevenly due to their thermal pretreatment in the texture.
Ved farvningen af polyesterfibre kræves der ingen yderligere tilsætninger udover dispergerings- og egaliseringsmidler og kemikalierne til pH-værdiindstilling. Parvebadets pH-vær dikonstans på mellem 4,5 og 5,5 gør det muligt at reproducere farvningerne med dispersionsfarvestoffer, og den opnås ved kendte, egnede puffersystemer,. Såvel tørt som vådt materiale kan behandles.In the dyeing of polyester fibers, no additional additives other than dispersants and equalizers and the chemicals for pH adjustment are required. The pH value of the steam bath between 4.5 and 5.5 allows the stains to be reproduced with dispersion dyes and is obtained by known suitable buffer systems. Both dry and wet material can be treated.
Det er vigtigt til opnåelse af en egal farvning, at flotte-cirkulationen ikke afbrydes ved omskiftningen, hvilket, som det er alment kendt, opnås ved en firevejsomskifter eller en ventilregulering.It is important to achieve even coloration that the raft circulation is not interrupted by the switching, which, as is well known, is achieved by a four-way switch or a valve control.
. I nogle tilfælde, især ved farvning af opspolet garnmateriale, har det vist sig hensigtsmæssigt ved den her omhandlede fremgangsmåde at forbehandle varen i løbet af ca. 10 minutter ved temperaturer på ca. 60°C med en vandig flotte indeholdende 1-3 vægtprocent af den tørre vares vægt, fortrinsvis 2 vægtprocent, af et bærerlignende hjælpemiddel, der begunstiger gennemfarvningen, og som består af 85 vægtprocent perchiorethylen og 15 vægtprocent af en emulgatorblanding, f.eks.. In some cases, especially when staining woolen yarn material, it has been found appropriate to pre-treat the product in the process of the present invention in about 5 minutes. 10 minutes at temperatures of approx. 60 ° C with an aqueous raft containing 1-3% by weight of the dry product weight, preferably 2% by weight, of a carrier-like aid favoring the dyeing, consisting of 85% by weight perchiorethylene and 15% by weight of an emulsifier mixture, e.g.
7.5 vægtdele af omsætningsproduktet af 1 mol ricinusolie med 36 mol ethylenoxid og 7.5 vægtdele tetrapropylenbenzensulfosurt calcium.7.5 parts by weight of the reaction product of 1 mole of castor oil with 36 moles of ethylene oxide and 7.5 parts by weight of tetrapropylene benzenesulfosuric calcium.
Derpå kan man med eller uden mellemskylning indskyde den varme flotte, der indeholder farvestofpræparatet.Then, with or without intermediate rinsing, one can insert the hot raft containing the dye preparation.
7 1464507 146450
Eksempel 1Example 1
Opviklede emner af teksturerede filamenter af lineær polyester anbringes i en farvebeholder, der er egnet til højtemperaturfarvninger . Denne beholder befries dernæst for indesluttet luft ved hjælp af mættet damp med et tryk på 2 kp/cm^ (ca. 120°C) og forvarmes med varen. Samtidigt forberedes i en blandingsbeholder den samlede, til farvningen nødvendige flottemængde, der andrager det 10-dobbelte af varens vægt og - beregnet på vægten af den tørre vare - indeholder 1,3% dispersionsfarvestof med formlenCoiled items of textured linear polyester filaments are placed in a color container suitable for high temperature staining. This container is then freed from trapped air by saturated steam at a pressure of 2 kp / cm 2 (about 120 ° C) and preheated with the product. At the same time, prepare in a mixing container the total amount of float required for coloring which is 10 times the weight of the product and - based on the weight of the dry product - contains 1.3% dispersion dye of the formula
N = w *TH3 CNN = w * TH3 CN
0 OH0 OH
3 1 cm /liter eddikesyre (60%'s) 1 g/liter 2,2'-dinaphthylmethan-6,6'-disulfonsurt natrium og 1 g/liter omsætningsprodukt af 1 mol isotridecylalkohol med 8 mol ethylenoxid.3 1 cm / liter acetic acid (60%) 1 g / liter 2,2'-dinaphthylmethane-6,6'-disulfonic acid sodium and 1 g / liter reaction product of 1 mole of isotridecyl alcohol with 8 moles of ethylene oxide.
Over flotteniveauet indstilles ved hjælp af trykluft et lufttryk på 2 5,5 kp/cm .Above the float level, an air pressure of 2.5 5.5 kp / cm is set using compressed air.
Den under tryk stående flotteblanding opvarmes nu til 140°C.The pressurized beautiful mixture is now heated to 140 ° C.
Ved åbning af en blokeringsventil i en egnet fordelerledning lader man den opvarmede flotte løbe ind i farvebeholderen i løbet af 7-10 sekunder. Indstrømningen af farvestofpræparatet i det opviklede emne sker såvel indefra som udefra. Efter flottecirkulationens begyndelse indstiller der sig en blandingstemperatur på 130°C. Ved afvekslende flottecirkulation forhøjes badtemperaturen nu til 135°C, og varen farves i 20 minutter ved denne temperatur. Til sidst efterbehandles det farvede materiale reduktivt på gængs måde og tørres.When opening a blocking valve in a suitable distributor line, let the heated raft run into the color container in 7-10 seconds. The influx of the dye composition into the wound up takes place both inside and outside. After the start of the float circulation, a mixing temperature of 130 ° C is set. By alternating float circulation, the bath temperature is now raised to 135 ° C and the product is stained for 20 minutes at this temperature. Finally, the dyed material is reductively treated in the usual manner and dried.
Der fås en ensartet gulfarvning.A uniform yellow color is obtained.
Hvis man i ovenstående eksempel i stedet for det nævnte dispersionsfarvestof anvender dispersionsfarvestoffet med formlenIf in the above example, instead of the said dispersion dye, the dispersion dye of the formula is used
" ^^/0_(CH2) 6-0H6 H
II III I
0 OH0 OH
fås en ensartet rødfarvning.a uniform red color is obtained.
8 1464508 146450
Eksempel 2Example 2
Opviklede emner af teksturerede filamenter af lineær polyester anbringes i en farvebeholder, der er egnet til højtemperatur-farvninger. I denne beholder skylles varen først med vand ved 60°C, og skylleflotten ledes bort. Dernæst gås der videre frem på den i eksempel 1 angivne måde til farvning af fibermaterialet, idet farve-operationen dog gennemføres under anvendelse af 0,7% af varens vægt af et dispersionsfarvestof ud fra lige andele af forbindelser med formlerneCoiled items of textured linear polyester filaments are placed in a color container suitable for high temperature stains. In this container, the product is first rinsed with water at 60 ° C and the rinsing raft is discharged. Next, the method for dyeing the fiber material is further advanced, however the dyeing operation is carried out using 0.7% of the weight of the product of a dispersion dye from equal proportions of compounds of the formulas
NH„ 0 NH-CH90H NH„ O OHNH₂O NH-CH90OH NH₂O OH
^ i ~ II i^ i ~ II i
OH O OH OH O NH-CH2OHOH O OH OH O NH-CH2OH
Der fås en ensartet blåfarvning.A uniform blue color is obtained.
Eksempel 3Example 3
En strikket vare af teksturerede filamenter af polyester anbringes opviklet på en farvebom i en farvebeholder ifølge eksempel 1. Efter lukning af beholderen behandles varen i 10 minutter ved 60°C med en vandig flotte, der indeholder 2% af varens vægt af en hjælpemiddelblanding af 85 vægtprocent perchlorethylen 7.5 vægtprocent omsætningsprodukt af 1 mol ricinus olie med 36 mol ethylenoxid og 7.5 vægtprocent tetrapropylenbenzensulfosurt calcium.A knitted product of textured polyester filaments is placed wound on a color boom in a color container of Example 1. After closing the container, the product is treated for 10 minutes at 60 ° C with an aqueous raft containing 2% of the weight of the product of an auxiliary mixture of 85 wt% perchlorethylene 7.5 wt% turnover product of 1 mole of castor oil with 36 moles of ethylene oxide and 7.5 wt% tetrapropylene benzenesulfosuric calcium.
Derpå trykkes denne vaskeflotte ind i blandingsbeholderen ved hjælp af presseluft, og der tilsættes 0,95% af varens vægt af dispersionsfarvestoffet med formlenThen, this wash float is pressed into the mixing vessel by compressed air and 0.95% of the weight of the product is added by the dispersion dye of the formula
Br «Br «
IIII
o 9 146450 0,4 af varens vægt af dispersionsfarvestoffet med formleno of the weight of the product of the dispersion dye of the formula
0 O0 O
TI IITI II
j, Μ I N - R (R = lavere alkyl)j, Μ I N - R (R = lower alkyl)
II IIII II
o o og 1 g/liter 2,2'-dinaphthylmethan-6,6,-disulfonsurt natrium samt eddikesyre til indstilling af pH-værdien på 4,5. Over blan-dingsflotten frembringes et tryk på 6 kp/cm med trykluft, og den på denne måde forberedte flotte opvarmes til 140°C.o and 1 g / liter of 2,2'-dinaphthylmethane-6,6, -disulfonic acid sodium and acetic acid to adjust the pH to 4.5. A pressure of 6 kp / cm with compressed air is generated over the mixing raft and the raft thus prepared is heated to 140 ° C.
Viderebehandlingen til farvning af varen sker dernæst på den i eksempel 1 beskrevne måde, dog med 30 minutters farvetid ved 130°C.The further coloring of the product is then carried out in the manner described in Example 1, however with 30 minutes of dyeing time at 130 ° C.
Der fås en ensartet grønfarvning.A uniform green color is obtained.
U6450 ίοU6450 ίο
Eksempel 4Example 4
En vævet vare af filamenter af lineær polyester, hvor kæden består af utekstureréde og skuddet af teksturerede filamenter, anbringes opviklet på en farvebom i en farvebeholder ifølge eksempel 1. Efter lukning af beholderen fjernes luften fra beholderen på den måde, at man blæser overhedet vanddamp (l30°C)ind ved beholderens bund i 10 minutter og fortrænger luften gennem overløbsledningen til den åbne cirkulation. Så snart der kommer damp ud, lukkes overløbsledningen. Indblæsningen af damp fortsættes derpå, indtil o der er opnået et indre tryk på 2,7 kp/cm i farvebeholderen. Dette damptryk opretholdes i 5 minutter. Ved denne behandling opnås, at tekstilmaterialet befries for indesluttet luft, samt at apparatet forvarmes. Efter 5 minutter sænkes trykket af den mættede damp til ca.A woven article of linear polyester filament, in which the chain consists of textured filaments and the shoot of textured filaments, is placed wound on a color boom in a color container of Example 1. After closing the container, the air is removed from the container by blowing superheated water vapor ( 130 ° C) at the bottom of the container for 10 minutes, displacing the air through the overflow conduit to the open circulation. As soon as steam comes out, the overflow line is closed. The supply of steam is then continued until an internal pressure of 2.7 kp / cm is achieved in the color container. This vapor pressure is maintained for 5 minutes. In this treatment, the textile material is freed from trapped air and the apparatus is preheated. After 5 minutes, the pressure of the saturated steam is lowered to approx.
2 1,5 kg/cm , og den kondenseres ved hjælp af et køleorgan.2 1.5 kg / cm and it is condensed by means of a cooling means.
Dernæst gennemføres farveoperationen som angivet i eksempel 1, og overføringen af den varme farveflotte sker imod det resttryk, som udøves af dampatmosfæren i farvebeholderen.Next, the color operation is carried out as in Example 1, and the transfer of the hot color float takes place against the residual pressure exerted by the vapor atmosphere in the color container.
Eksempel 5Example 5
Opviklede garnemner af filamenter af lineær polyester og rayon i et blandingsforhold på 67:33 behandles og farves på den i eksempel 1 angivne måde.Coiled yarns of linear polyester and rayon filaments in a mixing ratio of 67:33 are processed and stained in the manner set forth in Example 1.
Der fås en qulfarvning af polyesterfilamentandelen i varen. Farvningen af cellulosefilamentandelen kan ske i et eller to bade under anvendelse af egnede farvestoffer, f.eks. direkt-, reaktiv- og leukokypeester-farvestoffer og andre.A polyolefin of the polyester filament fraction is obtained in the product. The staining of the cellulose filament portion can be done in one or two baths using suitable dyes, e.g. direct, reactive and leukocyte ester dyes and others.
Eksempel 6Example 6
En maskevare af teksturerede filamenter af lineær polyester forbehandles på den i eksempel 4 angivne måde. Efter forvarmningen farves varen som angivet i eksempel 1, dog under anvendelse af 2,5% af varens vægt af et dispersionsfarvestof, li 1Α6Λ50 der består af en blanding af forskelligt bromerede diaminodihydroxy-anthraquinoner med under 1 brom pr. molekyle farvestof.A linear polyester textured filament mask is pretreated in the manner given in Example 4. After preheating, the product is stained as in Example 1, however, using 2.5% of the weight of the product by a dispersion dye, 1Α6Λ50 consisting of a mixture of differently brominated diaminodihydroxy anthraquinones with less than 1 bromine per liter. molecule dye.
Der fås en ensartet blåfarvning.A uniform blue color is obtained.
Eksempel 7Example 7
Opviklede emner af teksturerede filamenter af lineær polyester anbringes i en farvebeholder, der er egnet til højtemperaturfarvninger. Denne beholder befries derpå for indesluttet luft ved hjælp af mættet damp med et tryk på 1,4 kg/cm og forvarmes med varen. I en blandingsbeholder forberedes samtidigt den til farvningen nødvendige flottemængde, der andrager det 10-dobbelte af varens vægt og - beregnet på den tørre vares vægt - indeholder 0,25$ af dispersionsfarvestoffet med formlen ^CN ,—v / C2H5Coiled items of textured linear polyester filaments are placed in a color container suitable for high temperature staining. This container is then freed from trapped air by saturated steam at a pressure of 1.4 kg / cm and preheated with the product. At the same time, in a mixing vessel, the amount of float required for coloring is prepared which is 10 times the weight of the product and - based on the weight of the dry product - contains 0.25 $ of the dispersion dye of formula ^ CN, -v / C2H5
°2K—= N —ΛΛ—N° 2K— = N —ΛΛ — N
\=/ \=/ CgH^CN\ = / \ = / CgH ^ CN
1 enP/liter eddikesyre (60$'s) 1 g/liter dispergeringsmiddel på basis af kondensations-produktet af naphthalensulfonsyre med formaldehyd.1 enP / liter acetic acid (60 $) 1 g / liter dispersant based on the condensation product of naphthalenesulfonic acid with formaldehyde.
Over flotteniveauet indstilles ved hjælp af trykluft et lufttryk på 5,5 kp/cm^.Above the raft level, a compressed air pressure of 5.5 kp / cm 2 is set.
Den under tryk stående flotteblanding opvarmes nu til 135°C. Ved åbning af en blokeringsventil i en egnet fordelerledning lader man den opvarmede flotte løbe fra den under tryk stående blandingsbeholder ind i farvebeholderen i løbet af 7-10 sekunder. Derved skal en indstrømning af farvestofpræparatet ind i de opviklede em- 146450 12 ner ske såvel indefra som udefra. En blandingstemperatur på 125°C indstiller sig dernæst. Ved afvekslende flottecirkulation forhøjes badtemperaturen til lj55°C. Til sidst efterbehandles det farvede materiale reduktivt og tørres.The pressurized beautiful mixture is now heated to 135 ° C. When opening a blocking valve in a suitable distributor line, the heated raft is allowed to flow from the pressurized mixing vessel into the color container within 7-10 seconds. Thereby, an inflow of the dye composition into the wound subjects must occur both from the inside as well as from the outside. A mixing temperature of 125 ° C is then adjusted. By alternating float circulation, the bath temperature is raised to lj55 ° C. Finally, the colored material is reductively post-dried and dried.
Der fås en ensartet rødfarvning.A uniform red color is obtained.
Eksempel 8Example 8
Den ifølge eksempel 1 gennemførte farveproces kan gennemføres under anvendelse af 1% - beregnet på den tørre vares vægt - af dispersionsfarvestoffet 2,6-dicyan-4-ni tro-2-ace tylamino-4-die thylamino-azobenzen (vesttysk patentskrift nr. 1.290.915) istedåfor det i eksempel 1 nævnte dispersionsfarvestof, med en tidsindsats på 50 minutter til farveoperationen.The dyeing process carried out according to Example 1 can be carried out using 1% - based on the weight of the dry product - of the dispersion dye 2,6-dicyan-4-ni tro-2-acetylamino-4-die thylamino-azobenzene (West German patent no. 1,290,915) instead of the dispersion dye mentioned in Example 1, with a time commitment of 50 minutes for the color operation.
Plotteblandingen opvarmes i trykblandingsbeholderen allerede under den endnu løbende forudgående farvning. Tidsindsatsen til den egentlige farveproces består af nedenstående, i tidsmæssig rækkefølge efter hinanden programmerede behandlingstrin: 1. Fyldning af farvebeholderen med til lj55°C opvarmet blandingsflotte, begyndelse på flottecirkulation og dannelse af det nødvendige statiske tryk 0,5 min.The plot mixture is heated in the pressure mixing vessel already during the still ongoing prior staining. The time commitment to the actual color process consists of the following processing steps in succession in succession: 1. Filling the color container with a heated raft to a temperature of 55 ° C, start of raft circulation and the formation of the necessary static pressure 0.5 min.
2. Opvarmning af flotten fra 125 til 135°C 10 min.2. Heating the float from 125 to 135 ° C for 10 minutes.
3. Farvning ved 135°C 20 min.3. Staining at 135 ° C for 20 min.
4. Udlukning af farveflotten 2 min.4. Shut off the color fleet 2 min.
5. Fyldning af farvebeholderen med allerede i blandingsbeholderen forberedt efterbehandlingsflotte 0,5 min.5. Fill the color container with the finishing vessel already prepared in the mixing container 0.5 min.
6. Reduktiv efterbehandling 5 min.6. Reductive finishing 5 min.
7. Udlukning af efterbehandlingsflotten og skylning ved kontinuerligt vandtilløb og-fraløb 7 min.7. Shutdown of the after-treatment float and rinse at continuous water flow and drain 7 minutes.
8. Behandling med antistatisk virkende hjælpemidler 5 min.8. Treatment with antistatic agents 5 min.
50 min.50 min.
Funktionsstyringen og temperaturreguleringen sker vinder anvendelse af de af måle- og reguleringsteknikken til apparatfarveri udviklede programmeringsorganer, styrings- og overvågningselementer.The function control and temperature control takes place using the programming, control and monitoring elements developed by the measurement and control technique for appliance color.
13 U645013 U6450
Eksempel 9Example 9
Opviklede emner af teksturerede, surt modificerede filamenter af lineær polyester anbringes i en farvebenolder, der er egnet til højtemperaturfarvninger. Denne beholder befries derpå for indesluttet luft ved hjælp af mættet damp med et tryk på 1,2 kp/cm og forvarmes i 10 minutter med varen. I en blandingsbeholder forberedes samtidigt den samlede til farvningen nødvendige flotte-mængde, der andrager det 10-dobbelte af varens vægt og - beregnet på den tørre vares vægt - indeholder 0,5# af dispersionsfarvestoffet med formlen ^ OT2-CH2.—^^· 0,1 cm^/liter eddikesyre (60#’s) og 5 g/liter glaubersalt.Coiled blanks of textured, acidically modified linear polyester filaments are placed in a color bender suitable for high temperature staining. This container is then freed from trapped air by saturated vapor at a pressure of 1.2 kp / cm and preheated for 10 minutes with the product. At the same time, in a blending vessel, the total amount of stain required for coloring is prepared which is 10 times the weight of the product and - based on the weight of the dry product - contains 0.5 # of the dispersion dye of the formula ^ OT2-CH2. 0.1 cm 2 / liter acetic acid (60 # 's) and 5 g / liter glauber salt.
Over flotteniveauet indstilles et ved hjælp af trykluft et lufttryk 2 på 5,5 kp/cm .Above the raft level, an air pressure 2 of 5.5 kp / cm is set by means of compressed air.
Den under tryk stående flotteblanding opvarmes nu til 110°C. Ved åbning af en blokeringsventil i en egnet fordelerledning lader man den opvarmede flotte løbe fra den under tryk stående blandingsbeholder ind i farvebeholderen i løbet af 7-10 sekunder. Derved skal en indstrømning af farvestofpræparatet i de opviklede emner ske såvel indefra som udefra. Der indstiller sig dernæst en blandingstemperatur på 105°C. Ved afvekslende flottecirkulation forhøjes badtemperaturen nu til 110°C, og varen farves i 20 minutter ved denne temperatur. Til farvebadet sættes derpå via den åbne cirkulation 1 g/liter af en farveaccelerator på basis af emulgerede chlorbenzener, og der farves i yderligere 20 minutter. Den reduktive efterbehandling og tørring sker på den for det samlede tekstilmateriale gængse måde.The pressurized beautiful mixture is now heated to 110 ° C. When opening a blocking valve in a suitable distributor line, the heated raft is allowed to flow from the pressurized mixing vessel into the color container within 7-10 seconds. In this way, an inflow of the dye preparation into the wound items must be done both from the inside and the outside. A mixing temperature of 105 ° C is then adjusted. By alternating float circulation, the bath temperature is now raised to 110 ° C and the product is stained for 20 minutes at this temperature. To the dye bath is then added, via the open circulation, 1 g / liter of a color accelerator based on emulsified chlorobenzene and stained for another 20 minutes. The reductive finishing and drying is done in the usual way for the overall textile material.
Der fås en ensartet violetfarvning.A uniform violet color is obtained.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE2331669 | 1973-06-22 | ||
DE19732331669 DE2331669C3 (en) | 1973-06-22 | Process for dyeing synthetic fibers |
Publications (3)
Publication Number | Publication Date |
---|---|
DK82474A DK82474A (en) | 1975-03-17 |
DK146450B true DK146450B (en) | 1983-10-10 |
DK146450C DK146450C (en) | 1984-03-19 |
Family
ID=5884688
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DK82474A DK146450C (en) | 1973-06-22 | 1974-02-15 | PROCEDURE FOR COLORING WINNED TEXTILE MATERIALS OF SYNTHETIC FIBER OR SYNTHETIC FIBER MIXTURES |
Country Status (15)
Country | Link |
---|---|
JP (1) | JPS587748B2 (en) |
AT (1) | AT335399B (en) |
BE (1) | BE804816A (en) |
BR (1) | BR7402002A (en) |
CA (1) | CA1031109A (en) |
CH (2) | CH584786B5 (en) |
CS (1) | CS182244B2 (en) |
DD (1) | DD109700A5 (en) |
DK (1) | DK146450C (en) |
ES (1) | ES418692A1 (en) |
FR (1) | FR2234418B1 (en) |
GB (1) | GB1450399A (en) |
IT (1) | IT993173B (en) |
SE (1) | SE404041B (en) |
ZA (1) | ZA737215B (en) |
-
1973
- 1973-08-22 AT AT730773A patent/AT335399B/en not_active IP Right Cessation
- 1973-08-23 CH CH1214973A patent/CH584786B5/xx not_active IP Right Cessation
- 1973-08-23 CH CH1214973D patent/CH1214973A4/xx unknown
- 1973-09-07 IT IT28715/73A patent/IT993173B/en active
- 1973-09-10 CA CA180,600A patent/CA1031109A/en not_active Expired
- 1973-09-11 ZA ZA737215*A patent/ZA737215B/en unknown
- 1973-09-12 GB GB4283773A patent/GB1450399A/en not_active Expired
- 1973-09-12 ES ES0418692A patent/ES418692A1/en not_active Expired
- 1973-09-13 SE SE7312463A patent/SE404041B/en unknown
- 1973-09-13 FR FR7332897A patent/FR2234418B1/fr not_active Expired
- 1973-09-13 JP JP48102739A patent/JPS587748B2/en not_active Expired
- 1973-09-13 BE BE135616A patent/BE804816A/en not_active IP Right Cessation
-
1974
- 1974-02-15 CS CS7400001115A patent/CS182244B2/en unknown
- 1974-02-15 DD DD176582A patent/DD109700A5/xx unknown
- 1974-02-15 DK DK82474A patent/DK146450C/en not_active IP Right Cessation
- 1974-03-15 BR BR2002/74A patent/BR7402002A/en unknown
Also Published As
Publication number | Publication date |
---|---|
ES418692A1 (en) | 1976-02-16 |
FR2234418B1 (en) | 1977-05-20 |
CH1214973A4 (en) | 1976-08-13 |
IT993173B (en) | 1975-09-30 |
SE404041B (en) | 1978-09-18 |
SE7312463L (en) | 1974-12-23 |
BR7402002A (en) | 1975-12-02 |
JPS5052379A (en) | 1975-05-09 |
DK146450C (en) | 1984-03-19 |
BE804816A (en) | 1974-03-13 |
DE2331669B2 (en) | 1976-09-30 |
CA1031109A (en) | 1978-05-16 |
CS182244B2 (en) | 1978-04-28 |
DD109700A5 (en) | 1974-11-12 |
DE2331669A1 (en) | 1975-01-23 |
ATA730773A (en) | 1976-07-15 |
AT335399B (en) | 1977-03-10 |
JPS587748B2 (en) | 1983-02-12 |
DK82474A (en) | 1975-03-17 |
AU6564274A (en) | 1975-08-21 |
ZA737215B (en) | 1974-08-28 |
GB1450399A (en) | 1976-09-22 |
CH584786B5 (en) | 1977-02-15 |
FR2234418A1 (en) | 1975-01-17 |
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