DE1619605A1 - Process for dyeing fibers - Google Patents

Description

W. 12707/66 Da / 15 / Gö

F-onsanto Company St. Louis, Iissouri (V.St.A.)

Process for dyeing fibers

The invention "relates to a new method for Dyeing of synthetic, natural and mixtures of synthetic and natural fibers or threads. In particular The invention relates to a new method in which a dyeing aid for fixing the dye in the Fibers is used.

In general, dyeing operations consist in that one Bringing fibers into a dye (usually an aqueous solution) and fiber and dye in one for a long enough time

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009838/1984

bring them into contact with each other at a sufficient temperature. The dyestuff solution may contain electrolytes, acids, carriers, etc. to promote dyeing. The fiber absorbs color in a measurable manner until an equilibrium is finally established, at which the greatest part of the dye is absorbed by the fiber and a minor part remains in the dye solution. The extent of the dye absorption in the fiber depends on the respective fiber and the respective dye; the uptake is measured as a percentage, that is, a 100% uptake means that a 1 g robe of fibers has absorbed 1% of dye. In the early stages of dyeing a cross-section of the fiber zeirt a P.imT-färbur.g and that is, when the equilibrium is almost achieved in the spätereriFärbestadien _9, zeiprt a cross-section of the fiber, that the dyestuff of the Rinp · or outer ümranp the fiber is penetrated into the core. The extent of the coloration through the cross-section of the fiber is determined by means of color penetration. Measured from 1 to 5, that is, a color penetration of 1% would mean that the fiber is colored only on the surface or the outer circumference of the fibers, while a color penetration of 5 means that the entire cross-section of the fiber is colored is permeated.

To obtain a satisfactory level of staining with full grain To achieve penetration of the fibers, it was previously necessary to

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/ äurchzüfuhren the cases of raised temperatures and barren high pressure for a sufficient period of time * Iiochtemperaturfärbang has the advantages = that the Färbezei% is feürzer ^ a full Parbbereich on generally hydrophobic _s synthetic parsers are without the use of expensive carrier is possible and better Egalisierungselfjenscharten be achieved. However, there are disadvantages associated with high-temperature dyeing, which consist in the fact that such a procedure usually causes higher costs in the preparatory process; such a procedure requires greater care and. Certain dyes and fibers are not stable at these high temperatures. The high temperature and high pressure dyes usually have the same advantages and disadvantages, but generally reduce installation costs due to the high pressure of the system.

Printing ink processes are used for porous fabrics, loose fabrics. In this method, pressure is used as a means to uir. pushing the dye through the fabric. Dense fabrics, e.g. 3. Polyamide fabrics weighing 170.1 7 * by about 0.34 in (6 oz. Per sq. Yd.) Cannot be dyed by this iiethode due to their narrow permeability. . To this wax part ■ ^z: u overcome, high temperatures used in these Druckfärbeverfahren; the

However, it is still difficult to use such a system with fabrics without a fairly open structure. Because of the high pressure required for these systems are installation and equipment costs are very high.

A number of methods of dyeing fibers have been proposed in the past, including synthetic fibers such as acrylic fibers, polyamides, polyesters and the like. However, many of these methods have been found to be disadvantageous for several reasons. In many cases, it was found that the light fastness and / or wash fastness of dyed by this method ^p asern was low. Other methods have resulted in changes in the chemical properties of the fibers and therefore have proven ineffective for dyeing fibers with desirable properties.

The object of the invention is therefore to provide a novel and economical process for ^p 'irben of synthetic, natural and Ge-een of synthetic and natural Fasarn or ^ .the rit a ~ ro? .En class of dyes ·, the dye perfectly the fiber penetrates and a rod Liahectneity ..and '.'water resistance is achieved wire. As a synthetic foserr. According to the invention, acrylic, polyamide and polyester fibers in particular, which can each be re-colored with natural fibers, are to be re-dyed.

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This object is solved according to the invention characterized in that in © ¥ ej? Fahpen 311m dyeing of fibers provides be brought wherein the fibers with a ¹ dye in contact, and then acts with water and furfural dämp fen be ** ' will.

For the invention, suitable fibers include synthetic fibers, natural fibers, and mixtures of synthetic and natural fibers. For purposes according to the invention are synthetic fibers * _a i _s fibers are defined from natural and polymer fibers made of synthetic polymer.

Fibers made from natural polymers include rayon fibers, e.g. Pipes made from regenerated cellulose and from regenerated cellulose ^ the substituents were added to replace not more than 15 % of the hydrogen of the hydroxyl groups, and acetate fibers (fibers in which the "" fiber-forming / forming substance is cellulose acetate and not less than 92 % of the hydroxyl groups are acetylated). Examples of rayon fabrics include Viscose, Cuproxam (C ^ p ^ rammonium), and rayon fabrics with trade names such as Avril, Zantrel, Corval, and Fortlsan. Examples of acetate fibers include acetate and acetate fibers with trade names such as Arne! and Arne! 60 "

Synthetic polymer fibers include spandex (a fiber in which the fiber-forming substance is any

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long-chain synthetic polymer, made of at least 83 % by weight of a parcellular polyurethane), polyester (a fiber in which the fiber-forming substance is any long-chain synthetic polymer made of at least 35 % by weight of an ester of a dihydric alcohol and terephthalic acid, polyamide (a fiber , in which the fiber-forming substance is any long-chain synthetic polyamide with repeating amide groups (-C-IIH-) as inter-

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major part of the polymer chain), O acrylic fibers (a fiber in which the fiber-forming substance is any long-chain synthetic polymer composed of at least R5 wt. * of acrylonitrile _{units (-CH 9} -CH-.)), and modaeryl fibers (a fiber in; velcher the CN fiber-forming substance is any long-chain synthetic polymer) of at least 85 Gew.p, but at least 35 Gew, # of acrylonitrile units (-CIIp-gH-). Examples of spandex include tradename CII fibers such as Lycra, Vyren, and Blue "C" spandex. Trade names for polyester fibers include names such as Dacron, Kodel, Fortrel, Vyeron, Terylene, and Blue "C" polyester. Examples of trade names for acrylic fibers include Orion, Acrilan, Zefran, Courteile, and Creslan. Examples of polyamide fabric include nylon 6 and nylon 6,6. Examples of i'odacrylic fibers include candelabra such as Dynel, Verel, KaneUalon, and Teklan.

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Natural fibers useful in the invention include cotton, wool, and silk. Mixtures of natural and synthetic fibers or threads can also be used for the invention. Examples of such mixtures include acrylic fibers and cotton, acrylic fibers and "wool, polyamide fibers and cotton j polyester and silk, polyester and wool", "· polyester and cotton, ie 65% polyester and 35% cotton. Yieara, one made from i ^ ais protein The fiber produced is also useful in accordance with the invention.

In particular, the invention can be applied to fibers made from polyacrylonitrile as well as to copolymers, internal rpo Iyrers and their mixtures, in particular to mixtures with a content of at least one level of a polymerized or radically polymerized acrylonitrile. Such polymeric IT materials include fiber-forming acrylonitrile kit, easy-to-color basic nisch polymers and Kischunran nit. a content of irleichnäßi'j polymerized acrylonitrile of at least'-about PO wt. £. The polymer can, for example, be a mixed polymer with "etvia ⁰ O bia 9 ^P 1 * acrylonitrile and with about 2 to 20 % of another, highly-polymerizable rionoolefinic", such as acrylic acid, • 'vi-chloroacrylic acid and methacrylic acid, the acrylates (i.e. methylniethacrylate, 3uthy! methacrylate, IletlTöxynethylnethacrylate, /? '-Chloroäthy 1-methacrylate and the corresponding esters of acrylic acids and

BAD ORfGINAL 009833/1984.;, ::

^ -Chloroacrylic acids), vinyl chloride, vinyl fluoride, vinyl bromide, vinylidene chloride, l-chloro-l-bromoethylene; Methacrylic acid nitrile; Acrylamide and methacrylamide; txC-chloroacrylamide or its monoalkyl-substituted products, methyl vinyl ketone; Vinyl carboxylates such as vinyl acetate, vinyl chloroacetate, vinyl propionate and vinyl stearate; N-vinylimides such as N-vinylphthalimide and N-vinylsuccinic acid; p.iethylenemalonic acid ester; Itaconic acid and itaconic acid esters; N-vinyl carbazole; Vinyl furan; Alkyl vinyl ester; Vinylsulfonic acid, ethylene, ^ -dicarboxylic acids or their anhydrides or their derivatives such as diethyl citraconate, diethyl mesaconate; Styrene; Vinyl naphthalene; vinyl-substituted tert. heterocyclic amines such as vinylpyridines and alkyl-substituted vinylpyridines, ie 2-vinylpyridine, 4-vinylpyridine, 2-methyl-5-vinylpyridine, etc .; 1-vinylimidazole and alkyl substituted 1-vinylimidazoles such as 2-, k-, or 5-methyl-1-vinylimidazole, vinyl pyrrolidone, vinyl piperidone, and other monoolefinic copolymerizable monomeric materials.

The acrylic polymer can be a ternary interpolymer, ie a product which has been obtained by interpolymerizing acrylonitrile and two or more of the above-mentioned monomers with the exception of acrylonitrilic acid. In particular and preferably, the ternary polymers of about 30 to 98 % acrylonitrile, about 1 to 10 % Vi-

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nylpyridine or 1-vinylimidazo !; and about 1 to 18% of another substance such as mischpolymerisierbarenmonoolefinIschen methacrylonitrile, vinyl acetate, Methylmethaerylät, vinyl chloride, vinylidene chloride od _v the like ": he ^^

The cryopolymer can also be a mixture of polyacrylonitrile or a LiLsciipolynierisats from about 80 to 99 % acrylonitrile or about 1 to 20 % of at least one other monoolefinic, polymerizable monomeric substance with about 2 to ^ 50 % of the weight of the mixture ? a copolymer of about 30 his 90 £ of a vinyl-substituted the tertiary heterocyclic amine unci about 10 to east% copolymerizable least one other monoolefinisehen: its monomers; Menn the polymeric Hafcarial a mixture of about 80 to 99% of a copolymer of ■ "about 80 to. 9ß ^ acrylonitrile and about 2 to 20 % of another monoolefinic monomer, ie vinyl acetate with about 1 to 20 % of a copolymer of about 30 to 50% of a vinyl-substituted tertiary heterocyclic amine such as vinylpyridine, 1-vinylimidazoi or a vinyl lactam and ^ About 10% TO % of acrylonitrile results in a dyeable mixture containing an overall vinyl sub substituted tertiary heterocyclic amine of about 2 to 10 "Ji, based on the weight of the mixture»

Particularly applicable to the method according to the invention are also polyamide fibers *; Piping stripes are defined as

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linear polyamides formed by the condensation of a diamine with a dibasic acid by self-condensation of a Alginic acid or by a concentration in which species are formed. Polyamide fibers can also be defined as polyamides, e e with regularly occurring (-N-C-) units, where

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RO

R is hydrogen or a monovalent hydrocarbon radical and the average number of carbon separating the amide groups At least 2 atoms are concerned. Specific examples of polyamide fibers include the jenipen made from polymers of Tetramet hylenediamine with sebacic acid, hexamethylenediamine with adipic acid, Hexamethylenediamine can be obtained with suberic acid and hexamethylenediamine with sebacic acid. Also come into consideration Polyamide fibers resulting from the polymerization of 2 or more different diamines with a dicarboxylic acid or 2 or several dicarboxylic acids with one diamine or 2 or more different dicarboxylic acids can be obtained with 2 or more different diamines.

In the method according to the invention, polyester fibers are used Also particularly applicable, as well as various C elmixes made of polyester and natural fibers, i.e. polyester and cotton, polyester and silk, and polyester and wool. Polyester fibers are defined as those which are a long chain synthetic

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Polymer of at least 85 wt.% Of an ester of a dihydric alcohol and terephthalic acid, ie terephthalic acid with ilthylenglykol, dimethyl Te re pt hai acid with Sthylenglykol having. Mixtures of 2 parts polyester to 1 part cotton are particularly applicable according to the invention.

The dyes useful in accordance with the invention include all kinds of dyes, i.e. acid dyes, basic ones Dyes, direct dyes, disperse dyes, pre-metallized Dyes, etc. Certain fibers have an affinity to certain dyes. Acid dyes are therefore preferably used in acrylic fibers and polyamides; basic dyes in acrylic fibers and soap; Direct dyes Cotton, polyamides and silk; Disperse dyes for acetate, acrylic, polyester, and polyamide fibers; and pre-metallized Dyes in aöryl and polyamide fibers. A list of useful dyes is in "Technical Kanual of the American Association of Textile Chemists and Colorists, "Volume 38, 1962.

The on Uringen of the dye on the fiber may be performed by numerous methods, ie, by dipping the fiber into an aqueous solution of the dye, spraying the dye on the fiber, the dye by means of rollers on the fiber applying (kiss rolling), the dye on the fiber padded etc. The dye can be in an aqueous

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are located _? which contains additives known to the person skilled in the art,. eg leveling agents, such as cationic compounds, acids (formic acid, acetic acid or the like.), weakly alkaline salts (sodium carbonate, sodium acetate, tetrahydrofuran pyrophosphate or the like) - »additives to adjust the viscosity and the prevention of migration of the dye (a purified natural rubber ether, sodium alginate, or the like), various surfactants, retarders, or the like. It is well known in the art that certain additives are desirable for certain dyes after the fiber has been used When the dye is in contact with the dye, it is treated with water and furfural vapors. This treatment fixes the dye in the fiber and results in a dyed fiber with good washfastness and lightfastness For furfural cases it is preferred to heat the fiber during the treatment and to keep it at a temperature between e between about 66 ° C (150 ° F) and 149 ^D C (300 ° P) (with 79.5 ° * C (175 ° F) to about 121 ° C (250 ° F) being the preferred range), or the To dry fiber, preferably at a temperature in the range of about 100 ° C (212 ° F) to 1 * J9 ^O C (300 ° τ?), The fiber is not dried or is it kept at a temperature below that of about 66 ° C (150 ° r), furfural is likely to form a resin "cap" on the fiber and the.

009838/1984

Prevents color from penetrating indie fiber.

The 'Water and Furfuroläänipfe should ife BeieictL of etviSLj 99 ° C (210 ° F) until ^ about i2L ° C (250 ° F) liegerr .. At these temperatures, should the concentration of furfural in water vapor in the range of about J - 55 dew * % of the furfural lie. It; Lower concentrations of fur oil can be used, but if the concentration is lower, the full penetration of the fiber by the dye will probably not be as effective ^. in the case of the use of higher concentrations of b'urfurol *, Β * of about 75% concentration, there is the possibility that a certain part of the dye on the fiber will be dissolved in the furfurol. The Purfurolkonzentepatlbn.In the Masserdämpfen can below the Sättigurigspünktes the vapors are _"ä can be saturated in the Wasserdämpf s> or it may vapors are above your Satt-I-branch point - (which are taken from the water vapors) For example, a. Saturated furfural solution in water at about 10 ° C (50 ° F) a composition of 8 ^ 3 wt % furfural in the solution: and when boiling: (about 98 ° Cj 208.8 °? ) and 76Cf ^mm), a composition of 2SyG weight: * $ furfural in the water vapor and a saturated Bösüng at about 97.6 ° Gj (2ö8: 2 ^o F) and 76q has mm; water vapors Eilt a content of 35 Gew.f furfural; at higher temperatures, for example at about 102 ° σ (215 ° F) Vgrains the water-

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vapors contain approximately 45 wt. l of furfural oil. For the purposes According to the invention, v / a ss he steams preferably with furfural saturated; however, furfural is carried along in the water vapors also preferred in the concentrations given above.

The treatment of the fibers brought into contact with the dye with steam and furfural should be carried out for a sufficiently long period of time and at a sufficient temperature, e.g. 3. for about 1-10 minutes and at a temperature of about 99 ° C (210 ° F) to about 135 ° C (275 ° F), the preferred range being between about 96 ° C (205 ° F) and about 118 ° C .5 ° C (245 ° F) lies-t. If the temperature of the vapors is about 118.5 ° C (245 ° F), the length of time can be shorter, such as about 3 minutes; when the temperature of the vapors <b ^r ei about 100 ° C (212 ° F), the time period can be longer and be about 7 minutes. An extended period of time at higher temperatures, for example 30 minutes longer at a temperature of about 121 ° C (250 ° F), has a detrimental effect on the fiber »

There are many processes for the production of water and furfural oil, that is, by keeping a mixture of water and furfural oil at its boiling point, in steam it leads water (steam at different pressures) into the bottom of a ¹ brings furfural grains, etc. The methods can be a

009838/1984

continuous dyeing system can be adapted.

The invention is based on the following Examples explained in more detail.

It can be seen that the invention is not restricted to the dyes mentioned, but rather any ... material or a mixture of dyes which are useful for synthetic and natural threads or fibers, according to the invention, with water and furfural vapors. can be ended. Examples 1, ^ _9, 6 and 7 explain the effectiveness of furfural and hater vapors over furfural-free water vapors. All percentages are based on weight unless otherwise specified.

• Example 1

Samples of the polyester fiber and the polyamide fiber were immersed for 5 seconds at room temperature with a dye containing 20 g per liter Resolin Blue FBL paste (CJ. Disperse Blue 71), 160 g per liter sodium alginate solution (2 % chemical ) and 820 g of water, and then padded at 2.81 kg / cm (40 psi). Half of the samples were treated for 5 minutes with vapors of a 100 ° C (212 ° F) solution containing 200 cm of furfural in 2000 cm of water. The other half of the samples were treated with 100 ° C (212 ° F) steam for 5 minutes. Both

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Halves were subsequently heated for 10 minutes at 71 ° C (160 ° F) washed in an aqueous solution with a content of 2 g per liter of a nonionic detergent (Igepal CO-710). The samples treated with 100 ° C (212 ° F) steam showed severe paint bleeding, while those with the Steaming water and furfural treated samples showed no leakage and had a shade of blue that was double so deep was that after treatment with water vapors of 100 ° C (212 ° F).

Example 2

Strips of acrylic fiber carpet samples, with a composition of 76.5 % of a copolymer of 93 % acrylonitrile and 7 % vinyl acetate, 10.4 % of a copolymer of 50 % acrylonitrile and 50 % vinylpyridine and 13 % polyvinyl chloride, were marked with an x ^ Aqueous dye with a content of 1 g per liter of Anthraquinone Blue SWT (CI. Acid Blue 25), enough formic acid to adjust the pH to 2.0 and a sufficient amount of a 20% solution of natural rubber ether to increase the viscosity To regulate 175 cps, sprayed. The sample was treated with water vapors of a boiling aqueous solution containing 9 % furfural for 5 1 minutes. The sample showed a deep sound and an examination of the sample showed a cross section penetration of 4 - 5. ·

009838 / 1984- ^0A °

^: ' Example 3 . -:

A strip of the acrylic fiber carpet sample described in Example 2 was treated with an aqueous dye containing. 0.25 g per liter of Calcozine, Acrylic Red 3G, (CI. Basic Red 30), 0.25 g per liter of Genacryl Blue 3: '"G - (CI. Basic Yellow 28), a sufficient amount of sodium carbonate to regulate the pH to 9.5 and a sufficient amount of a 20% solution of purified natural gum ether to regulate the viscosity to 175 cps. After treating the sample for 5 minutes with fuming a boiling aqueous solution with a content of 9 % furfural, it was observed that the sample had a deep hue -. A further examination of the fiber showed a cross-sectional penetration of k - 5.

^; Example 4 "... .-.""" V A aqueous solution of a dye containing 10 g per liter of Pontamine Fast Yellow RL (CI. Direct Yellow 50) and 160 g per liter of sodium alginate was padded onto a cotton sample. After drying, half of the sample was treated with atmospheric steam for 5 minutes and the other half for 5 minutes with steam saturated with furfural oil. The sample treated with the steam saturated with furfural showed a hue of 40 %

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was deeper than that banded with furfural-free water vapor Sample. ·. . ..-: ■ - ■

Example 5 '■

The procedure of Example 4 was repeated with the modification that the aqueous dye solution 1Of; per liter of Diphenyl Fast Light Red 6 Bf (CI Direct Red 30) instead of Pontamine Fast Yellow RL. The sample treated with the atmospheric water vapor saturated with furfural showed a hue that was 100 % deeper than that treated with furfural-free water vapor Sample.

Example 6

The procedure of Example U was repeated with the modification that 10 g per liter of Chlorantine Fast Blue 7 GLL- (CI Direct Blue 76) was used instead of Pontamine Fast Yellow RL. The sample treated with the atmospheric steam saturated with furfural showed a shade 40% deeper than the sample treated with the furfural free steam treated sample. ·

Example 7

Two fiber samples, each made of 76.5 % of a copolymer of 93 % acrylonitrile and 7 % vinyl acetate,

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JO, 5 * of a mixed polyvinyl chloride composed of 50% acrylonitrile and 50 % liethy! Vinylpyridine and 13 % polyvinyl chloride, were mixed with a dye with a content of 1 g per 14th Anthraquinone Blue SWF (CI * Acid Blue 25), a sufficient kenge Acetic acid to regulate: - the pH value to 2, and a sufficient amount of a 20% solution of purified liaturguminiether to regulate the viscosity to 171 cps, sprayed. The color uptake of the samples was 175 %. Sine sample was treated with atmospheric water vapor for 3 minutes; the other sample was treated with vapors of a boiling aqueous solution of 9 % furfural for 5 minutes. The fiber or thread sample treated with atmospheric steam showed a permeation rate of 1, the same as that treated with the vapors of the boiling water vapor solution of 9% furfural. Sample of a long spinning; from U to 5 and a 50 % deeper color shade than the sample treated with atmospherically safe Viasserdamrf.

Example B

From a 93-% acrylonitrile and: ■ $ acetate composite fiber sample was a v at 60 ° C (liJ0 ^o F). ^T äÄri?; Er dye r.with a content of 10 r per liter Seyron Orange L (C, I. Basic Orange 2H) ₉ 1 "per liter rereini |: ter JiaturftUFo-iiither (? Cly?: Ur; 26o) and £ 0.5 per liter of a modified one

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Polyglycol ether (Tanapon. X-70) padded., The sample ^r whrde itfel 116 °. Heated at 250 ° F (C) for 5 minutes and then at 212 ° P (100 ° C) with saturated furfural for 1 minute
Treated with steam. Danacafr the "sample was rinsed cold,
washed for 10 fi minutes at the boiling point in an aqueous solution with a content of 1 rc per liter of a modified polyglycol ether (Tanapon X-JO) and 1 g per liter of tetrasodium pyrophosphate and then dried. The Paser sample showed a deep orange shade "which was washable and rub-resistant"

Example 9

A fiber protfe composed of 93 % acrylonitrile and 1% vinyl acetate was applied at 60 ° C (140 ° F) to an aqueous one. Dye with a content of 10 fr per liter of Basaeryl Blue GL (CI. Basic Blue 5 ^), 1 g per liter of a purified liatur-. nummife'thers (Polyf-un 26O) and 0.5 P per liter of a modified polyglycol ether (Tanapon X-70) padded. The sample was re-dried at tiB ° C C2 ^ Q ^Q F) and for 1 minute with
ateJmosphärisehern treated with furfural saturated via steam *. The sample was then rinsed cold for 10 minutes at the boiling point in an aqueous solution containing / 1 g per liter of a modified polyglycol ether (Tanapon
X-70) and 1 g per liter of tetrasodium pyrophosphate gev; ash and then dried * On the sample a deep wash and
Abrasion-resistant shade of blue observed.

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Example 10

On a fiber sample composed of 93 % acrylonitrile and 7 % vinyl acetate, an aqueous dye with a content of 10 g per liter of laxilon Red BL (Cl '. Basic Red 22) _Λ Ig was tested at 60 ° C (140 ° F) per liter of a purified rubber gum ether (Polyguai 260) and 0.5: g per liter of a modified polyglycol ether (Tanapon X-7Q) padded on. The sample was dried at 116 ° C (240 ° F) and then treated with atmospheric water vapor saturated with furfural for 1 minute. The sample was then rinsed with cold water, washed for 10 minutes at the boiling point in an aqueous solution containing modified polyglycol ether (Tanäpon X-70) and 1 g per liter of tetranatrium pyrophosphate and then dried. The sample showed a deep, washable and rub-resistant red shade . '- -

'.- ■ - ^ c: .. Example 11 .

On ilne fiber sample _S of a composed of the polymerization of terephthalic acid and ethylene glycol obtained polyester and 35% cotton, the .from 65%, an aqueous Färbstoff was in a content of 16 g per liter Latyl Blue LS -50% paste (CI Disperse Blue 62), 1 | per liter of sodium alginate and 0.5g per liter of a sodium alkylnaphthalene sulfonate (Nekal MF). The sample was at 116 ° G

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(2 ^ 0 ° P) dried for 1 minute with atmospheric treated with furfural saturated steam and then during 10 minutes at the boiling point in an aqueous solution with a content of 1 g per liter of a nonionic cleaning agent and 1 g per liter of tetrasodium pyrophosphate. When dry, the polyester fibers showed a medium blue tint that was washable and rub-resistant.

Example 12

The procedure of Example 11 was repeated, except that the fiber sample was treated for 5 minutes at 100 ^Q G (212 ° F) with saturated furfural with water vapor. It was observed that the sample had a darker blue color than in Example XI, which was washable and rub-resistant.

Example 13

Contained, on a periodic fiber strips, the Faserpoben of acrylic, polyamide, silk, Vicara and wool, an aqueous dye was padded at h9 ° C (120 ° F) containing 5 grams per liter Irgalan Yellow GL (CI Acid Yellow 11 * 0, a vormetallisiertem The strip was dried by holding it at 99 ° C (210 ° F) > for 5 minutes, then steaming from a boiling aqueous solution containing 100 cm per

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Liier treated furfurol. The strip was then rinsed and for 5 minutes at the boiling point in an aqueous solution washed, the 1 g per liter and tetrasodium pyrophosphate e hoaprt and Iq per liter of one contained nonionic detergent. After the strip After rinsing and drying, each speed sample showed a good one yellow shade »

Example 11 .

On a non-ferrous fiber strip of the acrylic fiber samples, Polyamide and Vikara became an aqueous at 49 ° C (120 ° F) Dye padded, of 5 g each, liter of the Brilliant Alizarine Milling Blue BL (CI. Acid Blue 80), an Acid Fairtoff, contained. The strip was dried at 99 ° C (210 ° F) and then for 5 minutes with steaming a boiling solution

treated, which contained IGO cm per liter of furfural in water. The strip was then rinsed and for 5 minutes at the boiling point in an aqueous solution with a content of 1 g per liter of tetrariat rag pyrophosphate and 1 · g_ per liter of one washed non-ionic detergent. Naehdem all fiber pro When the ovens were rinsed and dried, they showed a deep blue hue.

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Example 15

An aqueous dye containing 5 g per liter of Sevron Red GL (CI Basic Red 18), a basic dye, was padded onto a multi-fiber strip of fiber samples made of acrylic, silk and vicara contained. The strip was dried at 99 ° C (210 ° F) and then treated with vapors % ai of an aqueous boiling solution containing 100 cm per liter of furfural for 5 minutes. The strip was rinsed and washed for 5 minutes at the boiling point with an aqueous solution containing 1 g of tetrasodium dyrophosphate per liter and 1 g of a non-ionic acid per liter. After the strip was washed and dried, all fiber samples showed a deep red hue.

Example 16

On a guide fiber strip, the fiber samples made of acrylic, "

contained

Cotton, polyamide, silk and vicara] are heated at <+ 9 ° C aqueous dye padded on, the 5 g per liter of Direct Fast Yellow 3WP (CI. Direct Yellow 28), a direct dye, contained. After the strip was dried at 99 ° C (210 ° F), it was steamed for 5 minutes with a sieve

3 denden solution with a content of IOC er, per liter of furfural treated in water. The strip was then rinsed and washed

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5 minutes, long at the boiling point in an aqueous solution with a content of Ig per liter of tetrasodium pyrophosphate and 1 g per liter of nonionic detergent: washed. After the strip was rinsed and washed, everyone showed Fiber samples have a deep yellow hue.

. . Example 17 :.

On a multi-fiber strip, the fiber samples made of acetate, Acrylic, polyester and polyamide contained, was stored at 49 ° C (120 ° F) padded an aqueous dye that is 5 grams per liter Latyl Cerise B (CI. Disperse Red 59), a disperse dye, contained. The strip was dried by steaming it to 99 ° C (210 ° F) for 5 minutes

'■ "" "■" ■ "" • an aqueous boiling solution with a content of 100 cm Furfural per liter held. Thereafter, the strip was rinsed and for 5 minutes at the boiling point in an aqueous solution a content of 1 g per liter of a non-peculiar wash by means of,., washed. After the strip was rinsed and dried, all fiber samples were a deep red hue.

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Claims (5)

Claims 1. Process for dyeing synthetic and / or natural fibers, characterized in that the Brings fibers into contact with a dye and the Fibers then treated with water and furfural vapors. 2. The method according to claim 1, characterized in that that as dyes acid, basic, dispersing, direct, and pre-metallized dyes can be used. 3. The method according to claim 1 or 2, characterized tj that the treatment with water and furfural vapors at temperatures between about 96 ° C (205 ° F) and 100 ° C (212 ° F). ft. The method according to any one of claims 1 to 3, characterized in characterized in that one treatment with V / water and furfural vapors at a concentration of about 7.5 to 55% by weight of furfural. 5. The method according to any one of claims 1 to 4, characterized ; characterized in that the fiber is at a temperature of about 79.5 ° C (175 ° F) to 14-9 ° C (300 ° F) and on top of that ι temperature is maintained before the fibers with vapors from, a boiling aqueous mixture of furfural and water are treated, the Furfurolkonzentration about 7.5 to j is 45 Gewy%. 009838/1984