EP0023469A1 - After-treatment with liquid ammonia of cellulosic fibre materials which have been finished with fire-retardants - Google Patents

Abstract

Process for finishing cellulose-containing fiber materials, in which (a) commercial textile finishing agents are applied and fixed to the fiber materials, (b) the materials are optionally washed and dried, and (c) the textile materials are after-treated with liquid ammonia. The aftertreatment with liquid ammonia significantly improves the textile-mechanical properties of the refined fiber materials, in particular the tear resistance and the grip.

Description

The present invention relates to the aftertreatment of refined, cellulose-containing fiber materials with liquid ammonia.

The treatment of cellulose-containing fiber material with liquid ammonia has experienced a great boom in recent years. It can be used to achieve the effect of hot mercerization in a simple and inexpensive manner (see, for example, 5th communication in the series "Treatment of Cotton with Swelling Agents" by K. Bredereck in Melliand Textile Reports 8/1978, pp. 648-653). So far, the mercerization and the liquid ammonia treatment process have always been for the pretreatment of cellulosic fiber materials, i.e. used before dyeing and finishing. However, the fiber materials pretreated with liquid ammonia cannot be completely satisfactorily equipped with textile finishing agents. With e.g. Most flame retardant formulations, which are usually applied to achieve permanent effects, can only achieve insufficient fixing rates of the finishing agent on the fibers pretreated with liquid ammonia, so that the durability of the flame retardant equipment has to be accepted. In addition, many cellulosic fiber materials pretreated with liquid ammonia and subsequently treated with flame retardants have an unacceptable, stiff grip.

According to the invention, these disadvantages are unexpectedly avoided by providing the cellulose-containing material with a textile finishing agent in a first stage, then washing it if necessary in a second stage and then treating it with liquid ammonia in a third stage.

• (a) mindestens ein Textilveredelungsmittel auf die Faser aufbringt und fixiert,
• (b) das Material gegebenenfalls nachwäscht und trocknet und
• (c) das so erhaltene Material mit flüssigem Ammoniak nachbehandelt.

The invention therefore relates to a process for finishing cellulose-containing, optionally dyed and lightened fiber material, which is characterized in that

• (a) applying and fixing at least one textile finishing agent to the fiber,
• (b) the material is optionally washed and dried and
• (c) aftertreated the material thus obtained with liquid ammonia.

The present invention furthermore relates to a process for the aftertreatment of cellulose-containing, refined, optionally dyed and lightened fiber materials, to which at least one textile finishing agent has been applied and fixed beforehand and the fiber materials have subsequently optionally been washed and dried, which is characterized in that uses liquid ammonia for aftertreatment.

The use of liquid ammonia for the aftertreatment of cellulose-containing, refined, optionally dyed and lightened fiber material and the cellulose-containing, refined, optionally dyed and lightened fiber material which has been after-treated with liquid ammonia by the process according to the invention form further objects of the present invention.

The textile finishing agents which are used in stage (a) of the process according to the invention are the commercial textile finishing agents. Among other things, commercially available crease-resistant, shrink-proof, wet-strength, soft-grip, hydrophobic, oleophobic and / or flame retardant agents.

Preference is given to crease-resistant, soft-grip, hydrophobic or, in particular, flame retardants or mixtures of these finishing agents, such as hydrophobic- together with oleophobicizing agents or flame-retardant- together with crease-resistant, hydrophobic and / or soft grip agents used. Various finishing agents for the same purpose, such as various commercially available _K nitterfest-, water repellents or oil repellents can be used together.

These finishing agents have a wide variety of chemical constitutions. Thus, for example fluoroalkyl phosphates and / or Fluroalkylmethacrylate as hydrophobicity round / or _O leophobiermittel, optionally fatty acid-modified and etherified aminoplast precondensates as Knitterfest-, hydrophobicity round / or softener and / or methylolated phosphonium salts or hydroxides or water-soluble condensation products with aminoplast or methylolated Alkylphosphonsäureamide or water-soluble Polymers or copolymers with aminoplast formers used as flame retardants.

In the present case, aminoplast formers are understood to be methylolizable nitrogen compounds, preferably those of the urea and s-triazine series. Examples of such nitrogen compounds are e.g. Cyanamide, dicyandiamide, guanidine, biuret, urethane, optionally substituted by hydroxy substituted alkylene or propylene urea, ethylene diurea, preferably urea itself, unsubstituted ethylene urea, and also cyanuric acid, ammeline, ammelide, acetoguanamine, benzoguanamine, acetoguaniazine, uronogiaziazine, preferably acetoguaniazine, uretogiazine , Triazine and especially melamine mentioned.

According to the invention, aminoplast precondensates are understood to be the addition products of formaldehyde to these methylolated nitrogen compounds. Preferred aminoplast precondensates are thus e.g. a methylolated urea or ethylene urea or a methylolated triazine or melamine.

The preferred textile finishing agents are mono- or bis (fluoroalkyl) ammonium phosphates with 6 to 24 fluorine atoms and 4 to 28 carbon atoms in each fluroalkyl radical, fluoroalkyl methacrylates with 4 to 15 fluorine atoms and 5 to 16 carbon atoms in the fluoroalkyl radical and / or condensation products of stearic acid with one methylolated etherified with methyl or ethyl melamine as Hydrcphobier or oil repellent compositions, condensation products of urea stearic acid adduct with a methylolated by H ^y droxy substituted ethyleneurea and / or with a substituted by methyl or ethyl triazone as crease-resisting agents, condensates of a methylolated Stearinsäureamids with a methylolated melamine etherified with methyl or ethyl as a softening agent and / or tetrakis (hydroxymethyl) phosphonium salts or their condensation products with urea or an N-methylolated dimethyl or diethylphosphonopropionic acid amide as a flame retardant tel.

Examples of specific representatives of oleophobicizing and hydrophobicizing agents include Bis- (perfluoroalkylmethyl) -, bis- (1H, 1H-pentadecafluorooctyl) -, bis- (1H, 1H, 9H-hexadecafluorononyl) ammonium phosphate and 1H, 1H, 2H, 2H-heptadeca- fluorodecyl methacrylate and similar fluorine compounds, for example in British patents 939 902, 971 732, 1 010 539 and 1 011 612.

An example of a specific hydrophobizing agent is a condensation product of stearic acid with hexamethylolmelamine-hexamethyl ether, an example of a specific softening agent is a condensation product of stearic acid methylolamide with hexamethylolmelamine hexamethyl ether, and an example of a specific anti-crease agent is a condensation product of a reactive stearylurea derived from a mixture of dimethylolamine with a derivative of dimethylolamine called dihydroxyethylene urea and dimethylolmethyltriazon. Examples of specific flame retardants include tetrakis (hydroxymethyl) phosphonium chloride, sulfate or hydroxide, a condensation product of tetrakis (hydroxymethyl) phosphonium chloride with urea or self-condensation products of tetrakis (hydroxymethyl) phosphonium chloride or hydroxide mentioned, which are described, for example, in British Patents 1 075 033, 1 545 793 and 1 453 296, and, inter alia, in particular 0.0'-dimethyl-N-hydroxymethyl-phosphonopropionic acid amide, which is of primary interest and, for example, in German Patent 1,469,281.

The textile finishing agents are generally used as commercially available aqueous formulations. Such formulations are preferably in the form of aqueous emulsions and in particular in the form of aqueous solutions which are diluted with water to form aqueous preparations before use and applied to the fiber materials. Such formulations or preparations can contain, in addition to the finishing agents that can be used, especially if a phosphorus-containing flame retardant is used as the finishing agent, an aminoplast former or an aminoplast precondensate of the type already specified.

For this purpose, preferred aminoplast formers or preconsensates include e.g. optionally methylolated and etherified with methyl or ethyl ureas or melamines, especially dimethylol urea, di- and trimethylol melamine and hexamethylol melamine hexamethyl ether.

In a particularly preferred embodiment of the process according to the invention, an N-methylolated 0.0'-dimethyl- or diethylphosphono-propionic acid amide, in particular, is used as the aqueous preparation which contains the textile finishing agent special 0,0'-dimethyl-N-hydroxymethyl-phosphonopropionamide as a flame retardant in the presence of a methylolated and optionally etherified with methyl or ethyl melamine as aminoplast precondensate, in particular a mixture of di- and trimethylolmelamine or hexamethylolmelamine hexamethyl ether, is used.

As a rule, the aqueous preparations which are applied to the fiber material contain 50 to 500 g / l of a finishing agent and 0 to 100 g / 1 of an aminoplast former or precondensate, and in particular 200 to 400 g / 1 of a flame retardant as finishing agent and 20 up to 100 g / 1 of an aminoplast precondensate.

These aqueous, dilute preparations usually have an acidic to neutral or weakly alkaline pH, which is generally from 2 to 7.5, preferably from 4 to 7 and is adjusted in a customary manner by adding base or acid if necessary.

In addition to an aminoplast former or precondensate, the aqueous preparations of the textile finishing agents may also contain further additives. To achieve a larger substance overlay on fabrics e.g. an addition of 0.1 to 0.5 g / 1 preparation of a high molecular weight polyethylene glycol advantageous. Other usual plasticizers can be added to the preparations, e.g. an aqueous polyethylene or silicone oil emulsion.

Suitable copolymers can also be added to the preparations to improve the mechanical strength of the fibers, e.g. Copolymers of N-methylolacrylamide or cationic copolymers.

An addition of hardening catalysts or so-called latent acid catalysts, e.g. Ammonium chloride, ammonium dihydrogen phosphate. Phosphoric acid, magnesium chloride, zinc nitrate, 2-amino-2-methyl-l-propanol hydrochloride can often prove to be advantageous.

The same also applies to the addition of buffer substances, e.g. Sodium bicarbonate, di- and trisodium phosphate or triethanolamine.

To improve the durability of the finishing with the textile finishing agents and to achieve a particularly soft feel, it may be advantageous to add halogenated paraffins to the aqueous preparations, if appropriate in combination with a polyvinyl halide compound.

Furthermore, the aqueous preparations can also contain proportions of organic solvents, which serve primarily as solubilizers for the plasticizer, e.g. Dioxane, acetone, n-butyl glycol, isopropanol, ethanol or ethyl acetate.

It may also be advantageous to add small amounts (e.g. 0.5 to 2 g / l) of wetting agents to the preparations, e.g. nonionic adducts of ethylene oxide with an alkylphenol, such as a condensation product of 1 mole of p-tert-nonylphenol and 6 to 12 moles of ethylene oxide.

The aqueous preparations of the textile finishing agent are applied to the fiber materials in a manner known per se. For example, the fiber materials are impregnated with the aqueous preparations by, for example, spraying, popping or dipping. However, it is preferable to work with piece goods and impregnate them on a foulard that usually comes with the preparation Room temperature is loaded. In addition to this preferred padding process, the exhaust process can also be considered.

After the textile finishing agents have been applied to the fiber material, they still have to be fixed on the fiber material. This fixation can be done by various methods, e.g. by the so-called wet or wet storage process, by the ammonia fixing process or by the heat setting process.

If the wet fixation process is followed, the completely wet fiber material is stored at about 40 to 60 ° C. for 12 to 48 hours, possibly rinsed and washed and then dried at about 60 to 100 ° C. The moisture fixation procedure is similar, with the difference that the wet fiber material is dried to a residual moisture of about 2 to 20% before storage. In the ammonia fixing process, the treated fiber material is first gassed with ammonia in the moist state, whereby the temperature automatically increases to temperatures of e.g. rises to 80 ° C, or rinsed in an ammonia solution at 20 to 80 ° C, preferably 20 to 40 ° C and then e.g. dried at 60 to 100 ° C.

The ammonia fixation process is preferred over the wet or wet storage process. However, the so-called heat-setting process is of primary interest.

In this heat setting process, the impregnated fiber material is dried and subjected to a heat treatment. The material is expediently used at temperatures up to 100 ° C, e.g. 60 to 100 ° C dried. The material is then subjected to a heat treatment at temperatures above 100 ° C, e.g. Subject to 100 to 200 ° C, preferably 130 to 180 ° C, the duration of which can be shorter the higher the temperature. This duration of heating is e.g. 30 seconds to 10 minutes.

After the textile finishing agent has been fixed on the fiber material, the material is optionally washed and dried again in the optional step (b) of the process according to the invention. This rewashing takes place especially in the case in which a phosphorus-containing flame retardant has been used as a textile finishing agent. Since phosphorus-containing flame retardants are usually applied from acidic aqueous preparations, it is necessary to wash the flame retardant equipment on the fiber material in most cases. For this purpose, the fiber material is washed with an aqueous solution which contains an acid-binding agent and optionally an oxidizing agent, and the material is used in e.g. 60 to 100 ° C dried. The acid binding agent used is e.g. Sodium hydroxide or sodium carbonate. In the presence of an unpleasant odor from the finishing of the textile finishing agent, especially the flame retardant, it is advantageous to add an oxidizing agent, e.g. Hydrogen peroxide to add. As a rule, the aqueous wash solution contains 0.1 to 0.8, preferably 0.3 to 0.6 g / 1 of the acid-binding agent and 0 to 8, preferably 3 to 6 g / 1 of the oxidizing agent. The after-washing is carried out at 20 to 90 ° C., preferably 60 to 80 ° C.

After washing, the material is expediently rinsed with water at 20 to 90 ° C, preferably 60 to 80 ° C and e.g. dried at 60 to 100 ° C.

The treatment of a fiber material with liquid ammonia is described, for example, in Melliand Textile Reports 8/1976, page 684. The treatment must be carried out below the boiling point of the ammonia, ie at a maximum of -33 ° C (under atmospheric pressure). As a rule, the treatment is carried out in a closed device, in which the ammonia is recovered in the gas state, liquefied and returned to the process. Such a device is also described on page 684 of Melliand Textile Reports 8/1976.

The fiber material is preferably post-treated with liquid ammonia for 0.1 to 10, in particular 1 to 6, seconds in the device described, in which the material is appropriately padded under tension in order to enable dimensional control. This tension is preferably 0.5 to 2 daN / cm ² (1 daN (deca Newton) = 1 Kp). After padding, the excess ammonia is removed, liquefied and recovered by the action of heat, for example dry heat or preferably by steaming the fiber material, if appropriate under a slight vacuum.

After the aftertreatment with liquid ammonia has been completed, the textile material is preferably subjected to mechanical shrinkage, especially if tension is used in the aftertreatment, as e.g. in the textbook on textile chemistry by H. Rath, Springer-Verlag 1963, pages 146 to 148.

This mechanical shrinkage, also called forced shrinkage or shrinkage, is carried out in suitable apparatuses, which are also described in the textbook by Rath, in which the fiber material is steamed and pressed in the wet state between hot calendars. This operation is also known as sanforizing. Desired shrinkage, preferably 1 to 10 percent of the length of the treated material, can be achieved with high calender temperatures, preferably 110 to 140 ° C.

The aftertreatment according to the invention with liquid ammonia of the fiber materials finished with textile finishing agents has significant advantages. Among other things the textile mechanical properties of the fiber materials such as handle, tear resistance etc. are improved without adversely affecting the finishing effect and, if applicable, its permanence. This also applies to the whiteness of optically brightened material. If colored material is used, it may even be possible an increase in the color strength can be achieved without influencing the shade.

Unless otherwise stated, the parts and percentages given in the examples below are always units by weight.

example 1

• 400 g/1 0,0'-Dimethyl-N-Hydroxymethyl-phosphonopropionsäureamid (als 80%ige, wässerige Lösung)
• 80 g/1 Hexamethylolmelamin-hexamethyläther (als 60%ige, wässerige Lösung)
• 30 g/1 eines Kondensationsproduktes aus 1 Mol Hexamethylolmelamin-hexamethyläther und 2 Mol Stearinsäuremethylolamid (als 24%ige, wässerige Dispersion)
• 2 g/1 eines Adduktes aus 1 Mol Nonylphenol und 10 Mol Aethylenoxyd (als 25%ige, wässerige Lösung)
• 20 g/1 einer 85%igen Phosphorsäure

enthält. Der so imprägnierte Satin wird bei 100°C getrocknet und anschliessend einer wärmebehandlung bei 150°C während 5 Minuten unterworfen. Der.Satin wird dann mit einer wässerigen 0,4 %igen Natriumcarbonatlösung,die 3 bis 6 ml eines 30 volumenprozentigen Wasserstoffsuperoxydlösung enthalten kann, bei 70°C nachgewaschen, mit Wasser bei 60°C gespült und bei 100°C getrocknet. Ein Teil des Satins wird nun mit flüssigem Ammoniak bei -35°C so foulardiert, dass der Satin unter einer Längsspannung von 1 daN/cm² während 10 Sekunden mit dem Ammoniak in Kontakt bleibt. Der Satin wird dann unter leichtem Vakuum gedämpft und bei 100°C getrocknet.A with a vat and a sulfur dye blue-colored satin from a cotton / polyester blend 85/15 with a basis weight of 290 g / m ² is padded with a liquor absorption of 70% with an aqueous preparation at 20 ° C, the

• 400 g / 1 0.0'-dimethyl-N-hydroxymethyl-phosphonopropionic acid amide (as an 80% aqueous solution)
• 80 g / 1 hexamethylolmelamine hexamethyl ether (as a 60% aqueous solution)
• 30 g / 1 of a condensation product from 1 mol of hexamethylolmelamine hexamethyl ether and 2 mol of stearic acid methylolamide (as a 24% aqueous dispersion)
• 2 g / 1 of an adduct of 1 mol of nonylphenol and 10 mol of ethylene oxide (as a 25% aqueous solution)
• 20 g / 1 of an 85% phosphoric acid

contains. The satin impregnated in this way is dried at 100 ° C. and then subjected to a heat treatment at 150 ° C. for 5 minutes. The satin is then washed with an aqueous 0.4% sodium carbonate solution, which can contain 3 to 6 ml of a 30 volume percent hydrogen peroxide solution, at 70 ° C, rinsed with water at 60 ° C and dried at 100 ° C. Part of the satin is now padded with liquid ammonia at -35 ° C so that the satin remains in contact with the ammonia under a longitudinal tension of 1 daN / cm ² for 10 seconds. The satin is then steamed under a slight vacuum and dried at 100 ° C.

According to the vertical test DIN 53906 (ignition time 15 seconds), both the satin aftertreated with ammonia and the nontreated satin is flame retardant even after 40 washes according to SNV 198 861. The results of the provisions of the Stiffness according to ASTM D 1388-64, the tear resistance according to SNV 198 461, the tear propagation resistance according to Elmendorf according to SNV 198 482 and the color strength of the untreated and the aftertreated satin are summarized in Table I below. The color strength is determined colorimetrically, the relative value 100% being ascribed to the untreated satin as a reference.

Example 2

The procedure described in Example 1 is followed, except that a moleskin made from pure cotton and dyed gray with a vat dye is used with a weight _{per unit} area of 350 g _/ m ² .

When testing the flame resistance, the same results as given in Example 1 are achieved. The textile mechanical properties and the color strength are tested as in Example 1, the results being summarized in Table II below.

Example 3

enthält. Die so imprägnierte Popeline wird bei 100°C getrocknet und anschliessend einer Wärmebehandlung bei 145°C während 4 1/2 Minuten unterworfen.A poplin made of pure cotton, dyed gray with a vat dye and having a basis weight of 180 g _/ m ² , is padded with an aqueous preparation at 20 ° C. at a liquor absorption of 65%

contains. The poplin impregnated in this way is dried at 100 ° C. and then subjected to a heat treatment at 145 ° C. for 4 1/2 minutes.

The poplin is then rinsed and dried as indicated in Example 1. Now a part of the poplin _as' described in Example 1-treated, steamed, and dried with liquid ammonia.

When testing the flame resistance, the same results as given in Example 1 are achieved. The textile mechanical properties and the color strength are tested as indicated in Example 1, the results being summarized in Table III below.

Example 4

enthält. Der imprägnierte Köper wird wie in Beispiel 1 angegeben getrocknet, der Wärmebehandlung unterworfen, nachgewaschen, gespült und erneut getrocknet.An olive-dyed twill made of pure cotton with a basis weight of 3 ₂₃ g _{/ m} ² is padded with an aqueous preparation at 20 ° C. at a liquor absorption of 70, which

contains. The impregnated twill is dried as indicated in Example 1, subjected to the heat treatment, washed, rinsed and dried again.

Part of the body is then aftertreated with liquid ammonia, steamed and dried, as indicated in Example 1.

When testing the flame resistance, the same results as given in Example 1 are achieved. In addition, both the body aftertreated with ammonia and the untreated body when testing water absorption according to Bundesmann according to DIN 53 888 and according to AATCC spray test 22-1971 can be described as water-repellent. The textile mechanical properties and the color strength are tested as indicated in Example 1, the results being summarized in Table IV below.

Example 5

enthält. Der imprägnierte Köper wird bei 100°C getrocknet und anschliessend während 4 Minuten in einer geeigneten, geschlossenen Apparatur mit Ammoniakgas behandelt. In dieser _Appara- tur wird dem Köper mindestens 100 1 Ammoniakgas pro Minute zugeführt. Der Köper erwärmt sich dabei von selber auf 60 bis 70°C. Anschliessend wird der Köper mit einer 7%igen, wässerigen Wasserstoffsuperoxydlösung, deren pH-Wert mit Natriumcarbonat auf 8,0 gestellt wurde, bei einem Flottenverhältnis von 1:4 bei 20°C oxidativ behandelt, im gleichen Flottenverhältnis mit einer O,5%igen, wässerigen Natriumcarbonatlösung bei 50°C nachbehandelt, bei 50°C und nochmals bei 20°C gespült und bei 100°C getrocknet.A body made of pure cotton, dyed olive with a vat dye and having a basis weight of 323 g / m ² , is padded with an aqueous preparation at 20 ° C. with a liquor absorption of 80%, the -

contains. The impregnated twill is dried at 100 ° C and then closed in a suitable, closed for 4 minutes treated his equipment with ammonia gas. In this structure _A ppara- the twill is supplied to at least 100 1 ammonia gas per minute. The body warms itself to 60 to 70 ° C. The body is then oxidatively treated with a 7% aqueous hydrogen peroxide solution, the pH of which has been adjusted to 8.0 with sodium carbonate, at a liquor ratio of 1: 4 at 20 ° C., in the same liquor ratio with an 0.5% solution , aqueous sodium carbonate solution aftertreated at 50 ° C, rinsed at 50 ° C and again at 20 ° C and dried at 100 ° C.

Part of the body is then aftertreated with liquid ammonia, steamed and dried, as indicated in Example 1.

When testing the flame resistance, the same results as given in Example 1 are achieved. The textile mechanical properties and the color strength are tested as indicated in Example 1, the results being summarized in Table V below.

Example 6

The procedure described in Example 5 is followed, but a satin made of pure cotton and dyed gray with a vat dye is used with a weight per unit area of 327 g / m ² .

When testing the flame resistance, the same results as given in Example 1 are achieved. The textile mechanical properties and the color strength are tested as indicated in Example 1, the results being summarized in Table VI below.

Example 7

enthält. Die so imprägnierte Popeline wird in Kunststoff-Folien eingepackt, bei 20°C während 24 Stunden gelagert und anschliessend bei 100°C getrocknet.A poplin dyed with a vat and disperse dye made of a cotton / polyester blend 50/50 with a basis weight of 170 g / m ² is padded with an aqueous preparation at 20 ° C. at a liquor absorption of 60%, which

contains. The poplin impregnated in this way is packed in plastic films, stored at 20 ° C. for 24 hours and then dried at 100 ° C.

Now part of the poplin is aftertreated with liquid ammonia, steamed and dried as indicated in Example 1.

In the Monsanto crease picture according to SNV 198 670, in which 1 represents the worst and 5 the best grade, both the ammonia-treated and the non-treated poplin have a rating of 4. The textile mechanical properties and the color strength are measured as indicated in Example 1, the results being summarized in Table VII below.

Example 8

• 60 g/l Paraffin enthaltend ein Kondensationsprodukt aus Hexamethylolmelamin-hexamethyläther und Stearinsäure
• 15 g/1 Aluminiumtriglykolat (als 25%ige, wässerige Lösung) und
• 50 g/l eines Gemisches aus Bis-(perfluoralkylmethyl)-ammoniumphosphat Bis-(1H,1H-pentadecafluoroctyl)-ammoniumphosphat Bis-(IH,IH,9H-hexadecafluornonyl)-ammoniumphosphat und IH,IH,2H,2H-heptadecafluordecyl-methacrylat (als 13%ige, wässerige Lösung)

enthält. Der imprägnierte Köper wird wie in Beispiel 1 angegeben getrocknet, der Wärmebehandlung unterworfen, nachgewaschen, gespült und erneut getrocknet.A twill made of pure cotton with a weight per unit area of 300 g / m ² is padded with an aqueous preparation at 20 ° C. with a liquor absorption of 60%

• 60 g / l paraffin containing a condensation product of hexamethylolmelamine hexamethyl ether and stearic acid
• 15 g / 1 aluminum triglycolate (as a 25% aqueous solution) and
• 50 g / l of a mixture of bis- (perfluoroalkylmethyl) ammonium phosphate bis- (1H, 1H-pentadecafluoroctyl) -ammonium phosphate bis- (IH, IH, 9H-hexadecafluoronyl) -ammonium phosphate and IH, IH, 2H, 2H-heptadecafluorodecyl methacryl (as a 13% aqueous solution)

contains. The impregnated twill is dried as indicated in Example 1, subjected to the heat treatment, nachge wash, rinse and dry again.

_N un is a part of the Köpers as stated in Example 1-treated, steamed, and dried with liquid ammonia.

Both the body aftertreated with ammonia and the body not aftertreated have the mark 5 in the Monsanto crease according to SNV 198 670 (5 represents the best and 1 the worst mark) and the mark 6 when testing oil repellency according to AATCC 118-1972 ( 8 represents the best and 1 the worst grade) and can be described as water-repellent when testing water absorption in accordance with DIN 53 888 and spray test AATCC 22-1971.

The textile mechanical properties were tested as indicated in Example 1, the results being summarized in Table VIII below.

Claims (10)

1. Process for finishing cellulose-containing, optionally dyed and lightened fiber material, characterized in that (a) applying and fixing at least one textile finishing agent to the fiber, (b) the material is optionally washed and dried and (c) aftertreated the material thus obtained with liquid ammonia. 2. The method according to claim 1, characterized in that one uses an aminoplast former or an aminoplast precondensate in addition to the textile finishing agent. 3. The method according to claim 2, characterized in that the textile finishing agent is an N-methylolated dimethyl or diethylphosphono-propionic acid amide as a flame retardant in the presence of a methylolated and optionally etherified with methyl or ethyl melamine as aminoplast precondensate. 4. The method according to any one of claims 1 to 3, characterized in that the textile finishing agent is fixed by the heat setting method on the textile material by drying the fiber material at 60 to 100 ° C and a heat treatment at 130 to 180 ° C for 0.5 subjects to 10 minutes. 5. The method according to any one of claims 1 to 4, characterized in that the fiber material is washed and dried if a phosphorus-containing flame retardant has been used as a textile finishing agent. 6. The method according to claim 5, characterized in that one nachwäscht the fiber material with an aqueous solution containing an acid binding agent and optionally an _O xydationsmittel and the material dried at 60 to 100 ° C. 7. The method according to any one of claims 1 to 6, characterized in that the fiber material is aftertreated with liquid ammonia at a maximum of -33 ° C, optionally under tension. 8. The method according to claim 7, characterized in that the ammonia is removed after the aftertreatment by steaming the fiber material or by dry heat. 9. The method according to claim 7, characterized in that the fiber material is subjected to mechanical shrinkage after the after-treatment under tension. 10. The method according to any one of claims 1 to 9, characterized in that mixtures of cellulose fibers with at most 70 percent by weight synthetic fibers are used as cellulose-containing fiber materials.