EP0572923A1 - Process for the "wash-and-wear" finishing of cellulose textile, without formaldehyde - Google Patents

Process for the "wash-and-wear" finishing of cellulose textile, without formaldehyde Download PDF

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Publication number
EP0572923A1
EP0572923A1 EP93108577A EP93108577A EP0572923A1 EP 0572923 A1 EP0572923 A1 EP 0572923A1 EP 93108577 A EP93108577 A EP 93108577A EP 93108577 A EP93108577 A EP 93108577A EP 0572923 A1 EP0572923 A1 EP 0572923A1
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Prior art keywords
acid
cellulose
crosslinking
boric acid
treatment
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German (de)
French (fr)
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D. Dr. Lämmermann
Bernhard Dr. Mees
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Hoechst AG
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Hoechst AG
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/192Polycarboxylic acids; Anhydrides, halides or salts thereof

Definitions

  • crosslinking agents which form a more or less stable chemical bond with the free OH groups of cotton.
  • Methylolized urea compounds such as the glyoxylurea derivatives, are used in particular.
  • catalysts are used for the complete crosslinking of the cellulose fibers with these compounds, which also have the task of shortening the crosslinking time.
  • Magnesium or aluminum compounds, in particular their water-soluble halides, have proven particularly useful as catalysts. Since under the reaction conditions of the crosslinking (140-180 ° C. for 30 to 300 seconds) the methylol grouping present in the molecule can be split back into formaldehyde, so-called formaldehyde-free crosslinkers have been increasingly used recently.
  • US-A-4 820 307 describes the use of polycarboxylic acids, such as maleic acid, citric acid or butanetetracarboxylic acid with the addition of phosphorus-containing catalysts, such as alkali metal hypophosphites, phosphites, polyphosphates and dihydrogen phosphates for crosslinking cellulose.
  • polycarboxylic acids such as maleic acid, citric acid or butanetetracarboxylic acid
  • phosphorus-containing catalysts such as alkali metal hypophosphites, phosphites, polyphosphates and dihydrogen phosphates for crosslinking cellulose.
  • boron-containing compounds in particular boric acid and its salts, can be used as catalysts.
  • the invention relates to a process for the easy care finishing of cellulose-containing textile material by treating the cellulose-containing textile material with an aqueous liquor containing polycarboxylic acids as crosslinking agent and a crosslinking catalyst, subsequent drying and heat treatment, characterized in that boric acid and / or derivatives thereof are used as crosslinking catalysts .
  • Cellulose-containing textile goods are understood to mean, for example, fabrics, knitted fabrics, knitted fabrics, yarns and fibers in all processing stages. They can consist of cellulose fibers or of mixtures of cellulose fibers with other fibers such as polyester fibers, polyamide fibers, polyacrylic fibers, polyolefin fibers or wool, the mixtures having a cellulose fraction of more than 30%, preferably 50 to 90%.
  • Suitable crosslinking agents for the cellulose-containing textile material are aliphatic, alicyclic and aromatic carboxylic acids with at least 3 carboryl groups, as are mentioned in US Pat. No. 4,820,307.
  • Particularly suitable polycarboxylic acids are citric acid, propane tricarboxylic acid, cyclopentane tetracarboxylic acid, cyclohexane hexacarboxylic acid and in particular butane tetracarboxylic acid.
  • Suitable crosslinking catalysts are boric acid and / or its derivatives, such as salts of boric acid (borates) and boric acid esters.
  • Suitable boric acids are metaboric acid (HBO2), orthoboric acid (H3BO3) and polyboric acids of the general formula H n-2 B n O 2n-1 , where n is a natural number.
  • Alkali and alkaline earth metal salts are preferably used as salts of metaboric acid and orthoboric acid. Since the polyboric acids of the general formula H n-2 B n O 2n-1 cannot be prepared in the free state, the corresponding salts, such as alkali and alkaline earth metal salts, are preferably used.
  • boric acid esters used according to the invention have the general formula B (OR) 3, where R preferably denotes an alkyl radical, in particular C1-C6-alkyl, or aryl radical, preferably phenyl.
  • the cellulose-containing textile In order to make the cellulose-containing textile easy to care for, it is treated with an aqueous liquor with a pH in the range from 2 to 5, preferably 3 to 4.
  • the pH is optionally adjusted by adding suitable bases, such as ammonia, alkali metal hydroxide or their aqueous solution.
  • the aqueous liquor contains the above-mentioned polycarboxylic acids as individual substances or as mixtures in an amount of 20 g to 150 g / l liquor, and the crosslinking catalysts in an amount of 0.5 to 100% by weight, based on the polycarboxylic acid. Furthermore, the aqueous liquor can contain customary auxiliaries, such as water repellents, plasticizers and finishing agents. As a result, the finished textile not only receives additional specific properties such as water repellency, oil repellency and a pleasant feel, but often also an additional improvement in the creasing behavior.
  • the cellulose-containing textile material is treated with the aqueous liquor.
  • the treatment is usually carried out by impregnation, the aqueous liquor being applied to the cellulose-containing textile material by padding and then the excess liquor being squeezed off. Usually is squeezed to 50% of the liquor intake, preferably to 70 to 80% liquor intake.
  • the components of the aqueous liquor can be dissolved together in water and applied to the cellulose-containing textile material, or each component is applied as a separate solution.
  • the treatment can be carried out by spraying, splashing or foaming the cellulose-containing textile material.
  • drying takes place at temperatures up to approximately 130 ° C., preferably 100 to 130 ° C., which usually lasts 0.5 to 5 minutes.
  • a heat treatment is then carried out at temperatures of about 130 to 190 ° C., preferably 160 to 180 ° C., which usually lasts about 0.3 to 10 minutes, preferably 0.6 to 5 minutes.
  • the drying and heat treatment are usually carried out in a stenter or circulating air dryer.
  • the drying and heat treatment can also be carried out in one step, for example by means of a so-called shock-drying condensation (STK process) at a temperature in the range from 140 to 200 ° C. over a period of 0.5 to 8 minutes.
  • STK process shock-drying condensation
  • Shirt poplin made of 100% cotton with a basis weight of 110 g / m2 was impregnated with the aqueous liquors described in Table 1 by means of a foulard, squeezed to 70% liquor absorption and subsequently subjected to drying and heat treatment in a laboratory tenter (from Mathis, Zurich, Switzerland) .
  • the technological properties of the fabrics treated in this way were determined after storage for at least 24 hours in a standard climate (20 ° C., 65% relative atmospheric humidity) using the following methods.
  • DIN 53 890 Determination of the crease recovery angle of textile fabrics (measurement method on the air-dry sample with a horizontal fold edge and a free leg standing up).
  • DIN 53 858 Determination of the maximum tensile force of textile fabrics (except nonwovens); Grab method.
  • boric acid catalysis achieves wrinkle recovery values comparable to those of phosphorus-containing inorganic salts, but with higher strengths.

Abstract

The present invention relates to a process for the formaldehyde-free wash-and-wear (easy-care) finishing of cellulose-containing textile material by treatment with an aqueous liquor containing polycarboxylic acids as crosslinker and a crosslinking catalyst, subsequent drying and heat treatment, characterised in that the crosslinking catalysts used are boric acid and/or derivatives thereof.

Description

Seit vielen Jahren wird cellulosehaltiges Textilgut oder Mischungen von Cellulosefasern mit Synthesefasern in der Hochveredelung mittels sogenannter Vernetzer formstabil gemacht, damit das Textilgut auch nach dem Waschen und Trocknen seine ursprüngliche Form wieder erhält (Pflegeleicht-Ausrüstung). Als Vernetzer sind eine Reihe von chemischen Verbindungen bekannt, die mit den freien OH-Gruppen der Baumwolle eine mehr oder minder stabile chemische Bindung eingehen.For many years, cellulose-containing textile goods or mixtures of cellulose fibers with synthetic fibers have been made dimensionally stable in high-quality finishing using so-called crosslinking agents, so that the textile goods return to their original shape after washing and drying (easy-care finish). A number of chemical compounds are known as crosslinkers which form a more or less stable chemical bond with the free OH groups of cotton.

Besonders finden methylolisierte Harnstoffverbindungen, wie die Glyoxylharnstoffderivate Verwendung. Im Regelfall werden zur vollständigen Vernetzung der Cellulosefasern bei diesen Verbindungen Katalysatoren eingesetzt, welche auch die Aufgabe haben, die Vernetzungszeit zu verkürzen. Als Katalysatoren haben sich vor allem Magnesium- bzw. Aluminiumverbindungen, insbesondere ihre wasserlöslichen Halogenide bewährt. Da unter den Reaktionsbedingungen der Vernetzung (140 - 180°C während 30 bis 300 Sekunden) eine Rückspaltung der im Molekül vorhandenen Methylolgruppierung zu Formaldehyd möglich ist, wurden in jüngster Zeit zunehmend sogenannte formaldehydfreie Vernetzer eingesetzt.Methylolized urea compounds, such as the glyoxylurea derivatives, are used in particular. As a rule, catalysts are used for the complete crosslinking of the cellulose fibers with these compounds, which also have the task of shortening the crosslinking time. Magnesium or aluminum compounds, in particular their water-soluble halides, have proven particularly useful as catalysts. Since under the reaction conditions of the crosslinking (140-180 ° C. for 30 to 300 seconds) the methylol grouping present in the molecule can be split back into formaldehyde, so-called formaldehyde-free crosslinkers have been increasingly used recently.

Neuere Arbeiten zeigen, daß Polycarbonsäuren in der Lage sind, unter geeigneten Reaktionsbedingungen stabile Vernetzungen mit der Cellulose einzugehen.Recent work shows that polycarboxylic acids are able to form stable crosslinks with cellulose under suitable reaction conditions.

Die US-A-4 820 307 beschreibt die Verwendung von Polycarbonsäuren, wie Maleinsäure, Zitronensäure oder Butantetracarbonsäure unter Zusatz phosphorhaltiger Katalysatoren, wie Alkalimetallhypophosphite, -phosphite, -polyphosphate und -dihydrogenphosphate zum Vernetzen von Cellulose.US-A-4 820 307 describes the use of polycarboxylic acids, such as maleic acid, citric acid or butanetetracarboxylic acid with the addition of phosphorus-containing catalysts, such as alkali metal hypophosphites, phosphites, polyphosphates and dihydrogen phosphates for crosslinking cellulose.

Der Einsatz von phosphorhaltigen Katalysatoren bei der Vernetzung von cellulosehaltigem Textilgut mit Polycarbonsäuren ist nicht ohne Nachteile. Erstens können bei den hohen Temperaturen während der Vernetzung (Kondensation) Phosphorwasserstoffverbindungen freigesetzt werden, die unangenehm riechen und gesundheitsschädlich sind. Zum zweiten ist man in der Industrie bemüht - wegen der zunehmenden Überdüngung der Gewässer - Phosphorverbindungen so weit als möglich zu ersetzen.The use of phosphorus-containing catalysts in the crosslinking of cellulose-containing textile material with polycarboxylic acids is not without disadvantages. Firstly, at the high temperatures during the crosslinking (condensation) hydrogen phosphide compounds can be released, which smell unpleasant and are harmful to health. Secondly, efforts are being made in industry to replace phosphorus compounds as much as possible due to the increasing over-fertilization of water.

Aufgrund der bekannten Nachteile besteht weiterhin ein Interesse an geeigneten Katalysatoren, die bei der Vernetzung von cellulosehaltigem Textilgut eingesetzt werden können.Because of the known disadvantages, there is still interest in suitable catalysts which can be used in the crosslinking of cellulose-containing textile goods.

Überraschenderweise hat sich gezeigt, daß borhaltige Verbindungen, insbesondere Borsäure und deren Salze als Katalysatoren eingesetzt werden können.Surprisingly, it has been shown that boron-containing compounds, in particular boric acid and its salts, can be used as catalysts.

Gegenstand der Erfindung ist ein Verfahren zur Pflegeleicht-Ausrüstung von cellulosehaltigem Textilgut durch Behandeln des cellulosehaltigen Textilgutes mit einer wäßrigen Flotte, enthaltend Polycarbonsäuren als Vernetzer und einen Vernetzungskatalysator, anschließender Trocknung und Wärmebehandlung, dadurch gekennzeichnet, daß als Vernetzungskatalysatoren Borsäure und/oder deren Derivate verwendet werden.The invention relates to a process for the easy care finishing of cellulose-containing textile material by treating the cellulose-containing textile material with an aqueous liquor containing polycarboxylic acids as crosslinking agent and a crosslinking catalyst, subsequent drying and heat treatment, characterized in that boric acid and / or derivatives thereof are used as crosslinking catalysts .

Unter cellulosehaltigem Textilgut werden beispielsweise Gewebe, Gewirke, Gestricke, Garne und Fasern in sämtlichen Verarbeitungsstadien verstanden. Sie können aus Cellulosefasern oder aus Mischungen der Cellulosefasern mit anderen Fasern, wie Polyesterfasern, Polyamidfasern, Polyacrylfasern, Polyolefinfasern oder Wolle bestehen, wobei die Mischungen einen Celluloseanteil von mehr als 30 %, bevorzugt 50 bis 90 %, besitzen.Cellulose-containing textile goods are understood to mean, for example, fabrics, knitted fabrics, knitted fabrics, yarns and fibers in all processing stages. They can consist of cellulose fibers or of mixtures of cellulose fibers with other fibers such as polyester fibers, polyamide fibers, polyacrylic fibers, polyolefin fibers or wool, the mixtures having a cellulose fraction of more than 30%, preferably 50 to 90%.

Als Vernetzungsmittel für das cellulosehaltige Textilgut eignen sich aliphatische, alicyclische und aromatische Carbonsäuren mit mindestens 3 Carborylgruppen, wie sie in US-A-4 820 307 genannt werden. Besonders geeignete Polycarbonsäuren sind Zitronensäure, Propantricarbonsäure, Cyclopentantetracarbonsäure, Cyclohexanhexacarbonsäure und insbesondere Butantetracarbonsäure.Suitable crosslinking agents for the cellulose-containing textile material are aliphatic, alicyclic and aromatic carboxylic acids with at least 3 carboryl groups, as are mentioned in US Pat. No. 4,820,307. Particularly suitable polycarboxylic acids are citric acid, propane tricarboxylic acid, cyclopentane tetracarboxylic acid, cyclohexane hexacarboxylic acid and in particular butane tetracarboxylic acid.

Geeignete Vernetzungskatalysatoren sind Borsäure und/oder deren Derivate, wie Salze der Borsäure (Borate) und Borsäureester.
Geeignete Borsäuren sind Metaborsäure (HBO₂), Orthoborsäure (H₃BO₃) und Polyborsäuren der allg. Formel Hn-2BnO2n-1, wobei n eine natürliche Zahl ist. Als Salze der Metaborsäure und Orthoborsäure werden bevorzugt Alkali- und Erdalkalimetallsalze eingesetzt.
Da sich die Polyborsäuren der allg. Formel Hn-2BnO2n-1 im freien Zustand nicht darstellen lassen, werden bevorzugt die entsprechenden Salze, wie Alkali- und Erdalkalisalze, eingesetzt. Beispielhaft seien genannt: Panderit, Colemanit, Ulexit, Borocalcit, Boracit und Borax.
Die erfindungsgemäß verwendeten Borsäureester besitzen die allg. Formel B(OR)₃, worin R bevorzugt einen Alkylrest, insbesondere C₁-C₆-Alkyl, oder Arylrest, bevorzugt Phenyl, bedeutet.
Suitable crosslinking catalysts are boric acid and / or its derivatives, such as salts of boric acid (borates) and boric acid esters.
Suitable boric acids are metaboric acid (HBO₂), orthoboric acid (H₃BO₃) and polyboric acids of the general formula H n-2 B n O 2n-1 , where n is a natural number. Alkali and alkaline earth metal salts are preferably used as salts of metaboric acid and orthoboric acid.
Since the polyboric acids of the general formula H n-2 B n O 2n-1 cannot be prepared in the free state, the corresponding salts, such as alkali and alkaline earth metal salts, are preferably used. Examples include: panderite, colemanite, ulexite, borocalcite, boracite and borax.
The boric acid esters used according to the invention have the general formula B (OR) ₃, where R preferably denotes an alkyl radical, in particular C₁-C₆-alkyl, or aryl radical, preferably phenyl.

Um das cellulosehaltige Textilgut pflegeleicht auszurüsten, wird es mit einer wäßrigen Flotte mit einem pH-Wert im Bereich von 2 bis 5, bevorzugt 3 bis 4, behandelt. Die Einstellung des pH-Wertes erfolgt gegebenenfalls durch Zugabe geeigneter Basen, wie Ammoniak, Alkalimetallhydroxid oder deren wäßrigen Lösung.In order to make the cellulose-containing textile easy to care for, it is treated with an aqueous liquor with a pH in the range from 2 to 5, preferably 3 to 4. The pH is optionally adjusted by adding suitable bases, such as ammonia, alkali metal hydroxide or their aqueous solution.

Die wäßrige Flotte enthält die vorstehend genannten Polycarbonsäuren als Einzelstoffe oder als Mischungen in einer Menge von 20 g bis 150 g/l Flotte, sowie die Vernetzungskatalysatoren in einer Menge von 0,5 bis 100 Gew.-%, bezogen auf die Polycarbonsäure.
Desweiteren kann die wäßrige Flotte übliche Hilfsmittel, wie Hydrophobier-, Weichmachungs- und Appreturmittel enthalten. Dadurch erhält das ausgerüstete Textilgut nicht nur zusätzliche spezifische Eigenschaften, wie Wasserabweisung, Ölabweisung und einen angenehmen Griff, sondern oftmals eine zusätzliche Verbesserung des Knitterverhaltens.
The aqueous liquor contains the above-mentioned polycarboxylic acids as individual substances or as mixtures in an amount of 20 g to 150 g / l liquor, and the crosslinking catalysts in an amount of 0.5 to 100% by weight, based on the polycarboxylic acid.
Furthermore, the aqueous liquor can contain customary auxiliaries, such as water repellents, plasticizers and finishing agents. As a result, the finished textile not only receives additional specific properties such as water repellency, oil repellency and a pleasant feel, but often also an additional improvement in the creasing behavior.

Das cellulosehaltige Textilgut wird mit der wäßrigen Flotte behandelt. Die Behandlung erfolgt üblicherweise durch Imprägnieren, wobei die wäßrige Flotte durch Foulardieren auf das cellulosehaltige Textilgut aufgebracht wird und anschließend die überschüssige Flotte abgequetscht wird. Üblicherweise wird auf 50 % der Flottenaufnahme, bevorzugt auf 70 bis 80 % Flottenaufnahme abgequetscht. Zum Zwecke des Imprägnierens können die Komponenten der wäßrigen Flotte gemeinsam in Wasser gelöst werden und auf das cellulosehaltige Textilgut aufgebracht werden, oder jede Komponente wird als getrennte Lösung aufgebracht.The cellulose-containing textile material is treated with the aqueous liquor. The treatment is usually carried out by impregnation, the aqueous liquor being applied to the cellulose-containing textile material by padding and then the excess liquor being squeezed off. Usually is squeezed to 50% of the liquor intake, preferably to 70 to 80% liquor intake. For the purpose of impregnation, the components of the aqueous liquor can be dissolved together in water and applied to the cellulose-containing textile material, or each component is applied as a separate solution.

Neben dem Imprägnieren kann die Behandlung durch Sprühen, Pflatschen oder Schäumen des cellulosehaltigen Textilgutes erfolgen. Diese Arbeitsvorgänge sind dem Fachmann auf dem Gebiet der Pflegeleicht-Ausrüstung von Textilien bestens bekannt und brauchen nicht näher erläutert zu werden.In addition to impregnation, the treatment can be carried out by spraying, splashing or foaming the cellulose-containing textile material. These processes are well known to the person skilled in the field of easy care finishing of textiles and need not be explained in more detail.

Nach dem Behandeln des cellulosehaltigen Textilgutes, z.B. durch Imprägnieren, erfolgt eine Trocknung bei Temperaturen bis ca. 130°C, bevorzugt 100 bis 130°C, die üblicherweise 0,5 bis 5 Minuten andauert.After treating the cellulose-containing textile material, e.g. by impregnation, drying takes place at temperatures up to approximately 130 ° C., preferably 100 to 130 ° C., which usually lasts 0.5 to 5 minutes.

Anschließend wird bei Temperaturen von ca. 130 bis 190°C, vorzugsweise 160 bis 180°C, eine Wärmebehandlung durchgeführt, die üblicherweise etwa 0,3 bis 10 Minuten, vorzugsweise 0,6 bis 5 Minuten, andauert.A heat treatment is then carried out at temperatures of about 130 to 190 ° C., preferably 160 to 180 ° C., which usually lasts about 0.3 to 10 minutes, preferably 0.6 to 5 minutes.

Die Trocknung und Wärmebehandlung werden üblicherweise in einem Spannrahmen oder Umlufttrockenschrank durchgeführt.
Die Trocknung und Wärmebehandlung können auch in einer Stufe durchgeführt werden, z.B. durch eine sogenannte Schock-Trocknung-Kondensation (STK-Verfahren) bei einer Temperatur im Bereich von 140 bis 200°C über einen Zeitraum von 0,5 bis 8 Minuten.
The drying and heat treatment are usually carried out in a stenter or circulating air dryer.
The drying and heat treatment can also be carried out in one step, for example by means of a so-called shock-drying condensation (STK process) at a temperature in the range from 140 to 200 ° C. over a period of 0.5 to 8 minutes.

Anwendungsbeispiele:Examples of use:

Hemdenpopeline aus 100% Baumwolle mit einem Flächengewicht von 110 g/m² wurde mit den in Tabelle 1 beschriebenen wäßrigen Flotten mittels Foulard imprägniert, auf 70 % Flottenaufnahme abgequetscht und nachfolgend einer Trocknung und Wärmebehandlung in einem Laborspannrahmen (Fa. Mathis, Zürich, Schweiz) unterzogen.

Figure imgb0001
Shirt poplin made of 100% cotton with a basis weight of 110 g / m² was impregnated with the aqueous liquors described in Table 1 by means of a foulard, squeezed to 70% liquor absorption and subsequently subjected to drying and heat treatment in a laboratory tenter (from Mathis, Zurich, Switzerland) .
Figure imgb0001

Die technologischen Eigenschaften der so ausgerüsteten Gewebe wurden nach Lagerung von mindestens 24 Stunden bei Normklima (20°C, 65 % relative Luftfeuchtigkeit) nach folgenden Methoden bestimmt.The technological properties of the fabrics treated in this way were determined after storage for at least 24 hours in a standard climate (20 ° C., 65% relative atmospheric humidity) using the following methods.

DIN 53 890: Bestimmung des Knittererholungswinkels von textilen Flächengebilden (Meßverfahren an der lufttrockenen Probe mit waagerechter Faltenkante und hochstehendem freien Schenkel).
DIN 53 858: Bestimmung der Höchstzugkraft von textilen Flächengebilden (außer Vliesstoffen); Grab-Methode.
DIN 53 890: Determination of the crease recovery angle of textile fabrics (measurement method on the air-dry sample with a horizontal fold edge and a free leg standing up).
DIN 53 858: Determination of the maximum tensile force of textile fabrics (except nonwovens); Grab method.

Die Ergebnisse dieser Bestimmungen sind in Tabelle 2 zusammengefaßt. Tabelle 2 Technologische Effekte Beispiel Knittererholungswinkel (Grad) Anfang Knittererholungswinkel (Grad) 3 x 95°C-Wäsche Reißfestigkeit (N) 1 151 152 268 2 173 153 265 3 167 141 277 4 120 126 340 5 220 149 226 6 229 258 226 7 212 156 242 8 218 163 246 9 218 172 213 10 101 120 343 The results of these determinations are summarized in Table 2. Table 2 Technological effects example Wrinkle recovery angle (degrees) beginning Wrinkle recovery angle (degrees) 3 x 95 ° C wash Tensile strength (N) 1 151 152 268 2nd 173 153 265 3rd 167 141 277 4th 120 126 340 5 220 149 226 6 229 258 226 7 212 156 242 8th 218 163 246 9 218 172 213 10th 101 120 343

Wie aus Tabelle 2 zu entnehmen ist, erzielt man durch Borsäurekatalyse vergleichbare Knittererholungswerte wie mittels Katalyse von phosphorhaltigen, anorganischen Salzen, aber bei gleichzeitig höheren Festigkeiten.As can be seen from Table 2, boric acid catalysis achieves wrinkle recovery values comparable to those of phosphorus-containing inorganic salts, but with higher strengths.

Claims (8)

Verfahren zur formaldehydfreien Pflegeleicht-Ausrüstung von cellulosehaltigem Textilgut durch Behandeln mit einer wäßrigen Flotte enthaltend Polycarbonsäuren als Vernetzer und einen Vernetzungskatalysator, anschließender Trocknung und Wärmebehandlung, dadurch gekennzeichnet, daß als Vernetzungskatalysatoren Borsäure und/oder deren Derivate verwendet werden.Process for the formaldehyde-free easy-care finishing of cellulose-containing textile goods by treatment with an aqueous liquor containing polycarboxylic acids as crosslinking agent and a crosslinking catalyst, subsequent drying and heat treatment, characterized in that boric acid and / or derivatives thereof are used as crosslinking catalysts. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Polycarbonsäuren Zitronensäure, Butantetracarbonsäure, Cyclopentantetracarbonsäure und/oder Cyclohexanhexacarbonsäure eingesetzt werden.Process according to claim 1, characterized in that citric acid, butanetetracarboxylic acid, cyclopentanetetracarboxylic acid and / or cyclohexane hexacarboxylic acid are used as polycarboxylic acids. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß als Vernetzungskatalysatoren Borsäure, bevorzugt Orthoborsäure, Borate, bevorzugt Alkalimetall- und Erdalkalimetallsalze der Polyborsäuren und/oder Borsäureester der allg. Formel B(OR)₃, worin R ein Alkyl- oder Arylrest ist, eingesetzt werden.Process according to Claim 1 or 2, characterized in that the crosslinking catalysts used are boric acid, preferably orthoboric acid, borates, preferably alkali metal and alkaline earth metal salts of polyboric acids and / or boric acid esters of the general formula B (OR) ₃, in which R is an alkyl or aryl radical, be used. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die wäßrige Flotte einen pH-Wert von 2,0 bis 5,0, vorzugsweise von 3,0 bis 4,0 besitzt.Method according to one of claims 1 to 3, characterized in that the aqueous liquor has a pH of 2.0 to 5.0, preferably 3.0 to 4.0. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Konzentration der eingesetzten Borsäure oder deren Derivate zwischen 0,5 und 100 Gew.-%, bezogen auf die Polycarbonsäure, liegt.Process according to one of Claims 1 to 4, characterized in that the concentration of the boric acid or its derivatives used is between 0.5 and 100% by weight, based on the polycarboxylic acid. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Behandlung des cellulosehaltigen Textilgutes durch Imprägnieren, Sprühen, Pflatschen oder Schäumen erfolgt.Method according to one of claims 1 to 5, characterized in that the treatment of the cellulose-containing textile material is carried out by impregnation, spraying, splashing or foaming. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß die Trocknung bei einer Temperatur bis 130°C, vorzugsweise 100 und 130°C erfolgt.Method according to one of claims 1 to 6, characterized in that the drying takes place at a temperature of up to 130 ° C, preferably 100 and 130 ° C. Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß die Wärmebehandlung bei einer Temperatur zwischen 140 und 200°C, vorzugsweise zwischen 160 und 180°C erfolgt.Method according to one of claims 1 to 7, characterized in that the heat treatment is carried out at a temperature between 140 and 200 ° C, preferably between 160 and 180 ° C.
EP93108577A 1992-06-02 1993-05-27 Process for the "wash-and-wear" finishing of cellulose textile, without formaldehyde Withdrawn EP0572923A1 (en)

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CN108797109A (en) * 2018-06-27 2018-11-13 阜南美凯服饰有限公司 A kind of knitting fabric afterfinish method
CN113073467A (en) * 2021-03-18 2021-07-06 江南大学 Method for improving strength of non-ironing finished cotton fabric

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CN113073467B (en) * 2021-03-18 2022-03-04 江南大学 Method for improving strength of non-ironing finished cotton fabric

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