EP0047922B1 - Composition pour le traitement anti-feutrant de la laine - Google Patents

Composition pour le traitement anti-feutrant de la laine Download PDF

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Publication number
EP0047922B1
EP0047922B1 EP81106880A EP81106880A EP0047922B1 EP 0047922 B1 EP0047922 B1 EP 0047922B1 EP 81106880 A EP81106880 A EP 81106880A EP 81106880 A EP81106880 A EP 81106880A EP 0047922 B1 EP0047922 B1 EP 0047922B1
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EP
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Prior art keywords
radicals
mol
organopolysiloxanes
formula
units
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EP81106880A
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German (de)
English (en)
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EP0047922A1 (fr
Inventor
Friedhelm Nickel
Götz Dr. Koerner
Günter Dr. Schmidt
Hans Dr. Rott
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Evonik Operations GmbH
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TH Goldschmidt AG
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Priority to AT81106880T priority Critical patent/ATE5336T1/de
Publication of EP0047922A1 publication Critical patent/EP0047922A1/fr
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Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain

Definitions

  • GB-A-746 307 describes a method for preventing the shrinkage of the wool, the wool fibers being provided with certain organopolysiloxanes. A certain degree of shrink resistance is achieved in this way, but this effect is not washable.
  • a siloxane-in-water emulsion containing (A) a polydiorganosiloxane, (B) an organosiloxane with at least 3 silicon-bonded hydrogen atoms and alkyl radicals with less than 19 carbon atoms as organic substituents and ( C) one or more cationic and / or nonionic emulsifiers, characterized in that the polydiorganosiloxane (A) has a molecular weight of at least 2,500 and terminal OX radicals, where X is a hydrogen atom, an alkyl radical having 1 to 15 carbon atoms or an alkoxyalkyl radical 3 to 15 carbon atoms means at least two of the silicon-bonded substituents of the polydiorganosiloxane are monovalent radicals of carbon, hydrogen, nitrogen and optionally oxygen, which contain at least two amino groups and are bonded to silicon via a silicon-carbon bond and at least 50% of all substituents
  • This emulsion is intended for the treatment of goods made of keratin fibers, e.g. B. sweaters, can be used.
  • a disadvantage of these emulsions and also of the diluted liquors produced therefrom is that the hydrogen groups from the hydrogen siloxanes are accelerated by the amino groups of the aminoalkyl-modified siloxane diols. This affects and shortens the stability of the emulsions and the diluted liquors. At the same time, the effectiveness of the fleets decreases, as will also be shown in a comparative example below. In addition, it can be seen that, in particular, light and natural-colored wool yellows when treated with these products.
  • the invention is therefore based on the object of finding a preparation for shrink-proofing wool which is stable in storage, does not cause yellowing in natural-colored or white wool and leaves the treated wool in its original state even after repeated washing. At the same time, the feel of the treated wool or of the knitted fabrics and fabrics made from the wool should not be adversely affected.
  • An essential feature of the preparation according to the invention is thus the simultaneous presence of polysiloxanes with mercapto hydrocarbon residues and hydrogen residues bound to silicon. It is possible either to use copolymers in which the units aa) and ab) are present side by side on average, or to use mixtures of polysiloxanes in which the one polysiloxane mixture partner contains units aa) and the second polysiloxane mixture partner has units ab).
  • the preparation according to the invention thus corresponds to the preparation according to FR-A-2 412 641 in that the organopolysiloxane units of the formula contained in the preparation contain, in which the radical R 'has a certain proportion the meaning of a mercaptoalkyl or mercaptoaryl radical.
  • the radical R ' has a certain proportion the meaning of a mercaptoalkyl or mercaptoaryl radical.
  • radicals R 1 which may have the meaning of the mercaptoalkyl or mercaptoaryl radical.
  • organopolysiloxanes in which the units aa) and ab) are combined in one molecule in the form of copolymers, but that it is also possible to use mixtures of polysiloxanes which consist of polysiloxanes with Units of the formula aa) and polysiloxanes with units of the formula ab) exist.
  • the preparation according to FR-A-2412641 and the preparation according to the invention is also common in that they contain 50 to 99% by weight of water, optionally emulsifiers, and / or organic solvents and, if appropriate, conventional additives.
  • Preparations are particularly preferred which contain organopolysiloxanes in which the radicals R 'consist of 0.1 to 0.5 mol% of mercaptoalkyl or mercaptoaryl radicals and the remaining part of R' radicals are methyl radicals.
  • Examples of mercaptoalkyl or mercaptoaryl residues attached to the polysiloxane skeleton are the mercaptomethyl, 2-mercaptoethyl, 3-mercaptopropyl, 3-mercaptoisobutyl or mercaptophenyl residue.
  • the 3-mercaptopropyl radical is particularly preferred.
  • a preferred preparation according to the invention is characterized in that it contains organopolysiloxanes in which the residues R 2 to 36 to 48 mol% consist of hydrogen residues, m has a value of 2.03 to 2.2 and the remaining portion R 2 residues Are methyl residues.
  • a preparation with the characteristic that it is siloxanes of the structural unit ab) is particularly preferred for those of the formula where p has a value from 3 to 50.
  • siloxanes with units aa) are preferred in which n has a value from 1.990 to 1.998.
  • radicals R i and R 2 are methyl radicals. However, it is permissible that up to 10 mol% can be replaced by longer-chain alkyl or aryl radicals. Examples of such alkyl or aryl radicals are the ethyl, propyl, dodecyl or phenyl radical.
  • the preparation according to the invention can be in the form of an emulsion. However, it can also be used in the form of a solution in organic solvents.
  • the preparation of the preparation according to the invention in emulsion form succeeds in a known manner by emulsification with the aid of emulsifiers, for.
  • B. nonionic emulsifiers such as those obtained by the addition of ethylene oxide and / or propylene oxide to compounds having an acidic hydrogen radical, for.
  • B. fatty alcohol such as lauryl alcohol or stearyl alcohol
  • Cationic emulsifiers such as. B. quaternary ammonium compounds which have at least one longer-chain, causing hydrophobicity on nitrogen.
  • a suitable emulsifier is e.g. B. Trimethyllaurylammonium chloride.
  • chlorinated hydrocarbons such as. B. 1,1,1 -Trichloräthan, preferred.
  • the preparation can be conventional additives, such as. B. optical brighteners, flame retardants, agents influencing the handle of the textiles, fixing aids, odorants.
  • Organopolysiloxane copolymers which are suitable for the preparations according to the invention and have units of the formulas aa) and ab) can, for example, have the following structures: or where R 'consists of 0.33 mol% of mercaptopropyl residues and the remaining residues R' are methyl residues.
  • octamethylcyclotetrasiloxane 146 g (0.492 mol) of octamethylcyclotetrasiloxane are added dropwise to a 95 ° C. hot emulsifier solution corresponding to Example 1 with vigorous stirring. After a one-hour stirring phase, 27 g (0.097 5 mol) of methyldodecyldiethoxysilane and 2.7 g (0.013 8 mol) of 3-mercaptopropyltrimethoxysilane are added dropwise and the mixture is stirred vigorously for a further 30 min. After cooling to 40 ° C., the potassium hydroxide solution contained in the emulsion is neutralized by the addition of 15 g of a 10% acetic acid and a pH of 4 to 5 is simultaneously set.
  • a siloxane copolymer is prepared by heating 7.5 parts by weight of CH 3 (CH 3 O) Z Si (CH 2 ) 3 NHCH 2 CH 2 NH 2 and 1,000 parts by weight of a polydimethylsiloxane together with a Hydroxyl group on each terminal silicon atom and a viscosity of about 4 500 mm 2 / s at 25 ° C. The heating is carried out at 150 ° C under nitrogen and vigorous stirring for 2 hours. The copolymer formed is a clear liquid with a viscosity of approximately 6,000 mm 2 / s at 25 ° C.
  • the amount of water used is 64.11 parts by weight and the pH of the emulsion is adjusted to about 4.0 by adding acetic acid.
  • Knitted fine wool material is treated with the preparations mentioned in Examples 1 to 4, but further diluted on a padder, so that after a 5-minute drying of the impregnated knitted fabric at 140 ° C., a solids covering of 2% results.
  • the preparation c) from example 1 is used to finish the fine wool material in the exhaust process in a laboratory reel runner.
  • a 200 g knitted strip is treated in a liquor composed of 1.5 l water, 8 g emulsion according to the preparation 1 c) and 8 g Na 2 S 2 0 5 .
  • the active ingredient is absorbed 100% on the wool within 15 to 20 minutes.
  • the organopolysiloxane coating is also 2 % in this case, based on the amount of fine wool material used.
  • 360 parts by weight of water in a large beaker are mixed with 2.7 parts by weight of emulsion C, 0.135 parts by weight of emulsion D from comparative example 4 and 0.505 parts by weight of magnesium sulfate, with stirring.
  • the pH of the mixture obtained is adjusted to about 5.5 by adding acetic acid, and a piece of fine wool material measuring 30 x 40 cm is immersed in the liquid.
  • the temperature of the liquid is slowly raised to 40 ° C and the woolen fabric is agitated. In about 35 minutes the liquid becomes clear, which indicates the deposition on the fabric.
  • the fabric is then removed, dried at 80 ° C. for about 6 minutes and exposed to the ambient atmosphere (60% relative humidity, 20 ° C.) for 3 days.
  • Preparation c) from example 1 and a mixture of 92.5% by weight of emulsion C and 7.5% by weight of emulsion D from comparative example 4 are used again for treatment of the knitted fine wool material 8 days after mixing.
  • the knitted wool is treated with the further diluted emulsions on the padder in such a way that, after drying, the active substance requirements are 2%, as already described.
  • the shrink resistance of the samples treated in application examples 1 to 8 is determined according to the recommendations of the International Wool Secretariat, Test Method 185.
  • fabric samples are subjected to 3-hour washes in an International Cubex machine. From the dimensions of the fabric before and after the washes, the surface felt shrinkage can be done according to the formula be determined.
  • % L percentage length shrinkage
  • % B percentage width shrinkage.
  • the unfinished sample shows a strongly matted surface.
  • the handle of the treated samples is also significantly softer after washing than the handle of the untreated material before washing.
  • the samples treated according to the invention show no yellowing in comparison to the sample which is treated with the preparation from comparative example 4 in application example 5.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (7)

1. Composition servant à rendre la laine irrétrécissable, comprenant 1 à 50 % en poids d'organopolysiloxane comportant des unités de la formule
Figure imgb0030
dans laquelle R est un radical méthyle mais certains radicaux R peuvent être des radicaux mercaptoalkyle ou mercaptoaryle et n = 1,8 à 2,0, et 50 à 99 % en poids d'eau, éventuellement des émulsifiants et/ou des solvants organiques et éventuellement des additifs usuels, caractérisée par le fait que les organopolysiloxanes, ou bien sont constitués en moyenne, sous forme de produits de copolymérisation, par
aa) 80 à 99,8 % en poids d'unités de formule
Figure imgb0031
et
ab) 0,2 à 20 % en poids d'unités de formule
Figure imgb0032
ou bien que les organopolysiloxanes sont présents sous forme de mélanges comprenant chaque fois des polysiloxanes à unités de formule aa) et des polysiloxanes à unités de formule ab), les radicaux R' étant formés à raison de 0,03 à 3 mol% de radicaux mercaptoalkyle ou mercaptoaryle et les radicaux R2 à raison de 5 à 50 mol% d'atomes d'hydrogène et la proportion restante de radicaux R' et R2 étant des radicaux méthyle, aont toutefois jusqu'à 10 mol% peuvent être remplacés par des atomes d'hydrogène, des radicaux aryle ou des radicaux alkyle à chaîne plus longue, n ayant une valeur de 1,8 à 2,0 et m une valeur de 2,0 à 2,5.
2. Composition selon la revendication 1, caractérisée par le fait qu'elle contient des organopolysiloxanes dans lesquels les radicaux R' sont formés à raison de 0,1 à 0,5 mol% de radicaux mercaptoalkyle ou mercaptoaryle et la proportion restante des radicaux R' sont des radicaux méthyle.
3. Composition selon l'une des revendications 1 et 2, caractérisée par le fait qu'elle contient des organopolysiloxanes dans lesquels les radicaux R2 sont formés à raison de 36 à 48 mol% d'atomes d'hydrogène, m a une valeur de 2,03 à 2,2 et la proportion restante des radicaux R2 sont des radicaux méthyle.
4. Composition selon la revendication 3, caractérisée par le fait que comme siloxanes à unité structurale ab), elle contient des siloxanes de la formule :
Figure imgb0033
dans laquelle p a une valeur de 3 à 50.
5. Composition selon une ou plusieurs des revendications précédentes, caractérisée par le fait qu'elle contient des organopolysiloxanes dans lesquels n a une valeur de 1,990 à 1,998.
6. Composition selon une ou plusieurs des revendications précédentes, caractérisée par le fait que les radicaux mercaptoalkyle sont des radicaux 3-mercaptopropyle.
7. Composition selon une ou plusieurs des revendications précédentes, caractérisée par le fait que comme organopolysiloxanes à unité structurale aa), elle contient des corps dans lesquels les radicaux mercaptoalkyle ou mercaptoaryle sont rattachés aux extrémités.
EP81106880A 1980-09-12 1981-09-03 Composition pour le traitement anti-feutrant de la laine Expired EP0047922B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81106880T ATE5336T1 (de) 1980-09-12 1981-09-03 Zubereitung zum schrumpffestmachen von wolle.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3034380 1980-09-12
DE19803034380 DE3034380A1 (de) 1980-09-12 1980-09-12 Zubereitung zum schrumpffestmachen von wolle

Publications (2)

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EP0047922A1 EP0047922A1 (fr) 1982-03-24
EP0047922B1 true EP0047922B1 (fr) 1983-11-16

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US (1) US4405328A (fr)
EP (1) EP0047922B1 (fr)
AT (1) ATE5336T1 (fr)
AU (1) AU541233B2 (fr)
DE (2) DE3034380A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3529869A1 (de) * 1985-08-21 1987-02-26 Basf Ag Verfahren zum hydrophobieren von leder und pelzen
DE4100703A1 (de) * 1991-01-11 1992-07-16 Chu Tjoei Ho Textilausruestungsmittel
US5837370A (en) * 1995-06-30 1998-11-17 E.I. Du Pont De Nemours And Company Fabrics of wool and/or polyester fibers

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL133796C (fr) * 1965-01-21 1900-01-01
DE1594953A1 (de) * 1966-05-28 1969-07-03 Rotta Chem Fab Theodor Verfahren zur Ausruestung von Fasergut mit Polysiloxanen
CH615968D (fr) * 1967-04-26 1900-01-01
US4311760A (en) * 1976-10-04 1982-01-19 Dow Corning Corporation Method for applying mercaptoalkyl-containing polydiorganosiloxanes to textile fibers
DE2844952C2 (de) * 1977-12-22 1983-12-22 Th. Goldschmidt Ag, 4300 Essen Zubereitung zum Schrumpffestmachen von Wolle und Verfahren zur Herstellung der Zubereitung
DE2903334C2 (de) * 1978-03-16 1982-09-16 Th. Goldschmidt Ag, 4300 Essen Zubereitung zum Schrumpffestmachen von Wolle
DE3060191D1 (en) * 1979-03-23 1982-03-25 Goldschmidt Ag Th Preparation for making wool shrink-proof

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AU541233B2 (en) 1984-12-20
US4405328A (en) 1983-09-20
DE3034380A1 (de) 1982-03-25
AU7515281A (en) 1982-03-18
ATE5336T1 (de) 1983-12-15
DE3161434D1 (en) 1983-12-22
EP0047922A1 (fr) 1982-03-24

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