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
  • D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups

Definitions

• the invention relates to a process for the dimensional stabilization of sheet-like textile material by treatment with polydiorganosiloxanes with terminal groups capable of crosslinking, in particular hydroxyl groups from an aqueous system with a special crosslinking agent.
• GB-PS 14 34 017 corresponds to DE-OS 23 35 751
• a process for the treatment of keratin fibers with polydiorganosiloxanes with terminal hydroxyl groups bonded to silicon atoms and aminoalkyl-substituted alkoxysilanes is known.
• This mixture is preferably used together with another silane derivative, namely an alkyl trialkoxy or a tetraalkoxysilane.
• the treatment is preferably carried out from organic solvent.
• such a method can often not be used, since the mechanical requirements for carrying out a solvent method are not met.
• the organic substituents in the polydiorganosiloxanes are alkyl radicals, such as methyl, ethyl or propyl radicals. Some of the residues can also be aryl or phenyl residues.
• the terminal groups capable of crosslinking can be, for example, etherified or esterified, but in particular free hydroxyl groups.
• Preferred are polydiorganosiloxanes with terminal hydroxyl groups bonded to silicon and containing predominantly methyl radicals as organo residues, in particular polydimethylsiloxanes with viscosities of 4,000 to 100,000 mPa.s.
• polydiorganosiloxanes which also contain at least one radical which is composed of carbon, hydrogen, nitrogen and optionally oxygen and which contains at least one amino group and via a carbon bond to a silicon atom can also be used as the polydiorganosiloxanes of the polydiorganosiloxane is bound.
• These aminoalkyl-substituted polydiorganopolysiloxanes are accessible, for example, by reacting polydiorganosiloxanes with terminal hydroxyl groups with aminoalkyl-dialkoxy-alkyl-silanes of the formula (I), as is apparent from DE-OS 27 28 597.
• the aminoalkyl-dialkoxy-alkyl-silanes satisfy the general formula where R is a monovalent radical composed of carbon, hydrogen, nitrogen and optionally oxygen, which has at least one amino group and is bonded to the silicon atom via a silicon-carbon bond, R 'is an alkyl radical having 1 to 4 carbon atoms, X is an alkyl radical with 2 to 4, in particular 3, C atoms or an alkoxyalkyl radical with 3 to 8 C atoms.
• Examples of individual compounds which are accessible, for example, according to this process and can be used in technical quality are: Of these compounds, preferred are those in which R represents the rest means, where R "is an alkylene radical having 3 or 4 carbon atoms. This includes the compounds I b), I c), I d) and I e) listed above. These compounds combine easy producibility and high effectiveness.
• the aminoalkyl-dialkoxyalkylsilanes of the formula (I) mentioned can also partially condense with themselves during their preparation or can also be present in partially hydrolyzed form. This does not affect their effectiveness.
• GB-PS 14 34 017 it is preferred to use aminoalkylalkoxysilanes with 3 alkoxy groups, obviously because this results in a three-dimensional crosslinking of the poly. diorganopolysiloxane with the terminal hydroxyl groups is to be brought about, which leads to an improved shrink resistance of the treated keratin material.
• the use of the third component, namely the alkyltrisalkoxy- or tetraalkoxysilane, ie a silane derivative with 3 or 4 functional groups, should serve the same purpose.
• an organometallic siloxane condensation catalyst is also preferably used.
• crosslinking component an organosiloxane with at least 3 silicon-bonded hydrogen atoms in the molecule together with a siloxane curing catalyst is used as the crosslinking component.
• a methyl hydrogen polysiloxane is also used, insufficient felt-free effects on wool are achieved.
• purely catalytically active siloxane curing catalysts such as the known organometallic compounds, can also be used. They have no adverse influence, but are also unnecessary.
• the emulsions of the polydiorganosiloxanes can be prepared in a conventional manner using the emulsifiers known to the person skilled in the art.
• Non-ionic and cationic emulsifiers are preferred for the emulsification of the polydiorganosiloxanes, since this gives emulsions which are combined with other auxiliaries customary for textile finishing, such as agents for improving the creasing resistance and the catalysts required, the handle, the flame resistance and the hydrophobization and the like are generally compatible.
• nonionic emulsifiers examples include polyvinyl alcohol, the ethylene oxide reaction products of alkylphenols, higher fatty acids, fatty alcohols, fatty acid amides and fatty amines, the latter also in the form of their salts with inorganic or organic acids.
• Quaternary ammonium compounds are particularly worth mentioning as cationic emulsifiers.
• examples of such compounds are: cetyl or laurylbenzyldimethylammonium chloride, hexadecyl (dichlorobenzyl) dimethylammonium chloride, octadecyloxymethyl and hexadecyloxymethylpyridinium chloride and lauryloxymethyl-N- ⁇ -hydroxyethylmorpholinium chloride.
• epoxy amine condensates as described for example in GB-PS 10 71 162, come as cationic emulsions gates into consideration.
• the emulsifiers can also be used in a mixture with one another.
• Emulsions of the polydiorganosiloxanes mentioned are commercially available; they generally have a content of 25 to 60 percent by weight of emulsified polydiorganosiloxane. However, emulsions with a higher content of emulsified polydiorganosiloxane are also known and can be used for the purpose according to the invention.
• the crosslinking agents to be used according to the invention form dispersions, if appropriate in the form of their salts with water. However, these are so coarsely dispersed that a sufficiently uniform distribution in the polydiorganosiloxane emulsion is not always guaranteed. This insufficiently fine distribution would lead to unevenness in the equipment effects.
• siloxane curing catalysts based on organometallic compounds can also be added to the treatment liquors. These are familiar to the person skilled in the art. Therefore, organozinc, titanium and preferably tin compounds should only be mentioned in general. These are used in a commercial form.
• the treatment liquids containing the polydiorganopolysiloxane, the crosslinking agents to be used according to the invention, if appropriate the organometallic compound and, if appropriate, other conventional auxiliaries can be applied to the textile material to be treated in a customary manner, for example by spraying or padding.
• the textile material to be treated is treated in a short or long liquor and, due to its substantivity, absorbs the substances contained in the liquor until an equilibrium between fiber and the substances in the liquor is achieved.
• By controlling the temperature by adding electrolytes or pH regulators, but also by the choice of those used to emulsify the polydiorganosiloxanes.
• Emulsifiers can shift the balance in favor of the deposition of the substances on the fiber, which is favored, for example, with cationic emulsifiers.
• crosslinking agents to be used according to the invention 0.2 to 50, in particular 3.5 to 35 parts by weight, based on the polydiorganosiloxane, are generally used.
• the process according to the invention is carried out in such a way that, depending on the requirements for the effects, approximately 0.2 to 4 percent by weight of polysiloxane are deposited on the treated material.
• Curing of the applied to the fiber material treatment by drying and optionally heating preferably at temperatures from 80 ° C to 170 0 C, which may well be sufficient also a drying at 80 ° C to initiate crosslinking when enough for the treated textile material time to an after-reaction is available.
• This variant is used primarily for textile materials that contain or consist of keratin fibers.
• Sheet-like textile materials of all kinds can be treated by the process according to the invention. These can be in the form of nonwovens, woven fabrics or knitted fabrics. They can be made from fibers of natural origin or from synthetic fibers. Of course, the sheet-like textile materials can also consist of mixtures of synthetic fibers and natural fibers. Of the natural fibers are fibers based on cellulose, including regenerated cellulose fibers and keratin fibers, in particular wool.
• fibers based on polyamide, polyacrylonitrile, polyester and polyolefin fibers based on polyamide, polyacrylonitrile, polyester and polyolefin.
• the materials can also be made of crimped or twisted yarn, for example, so that the woven or knitted fabrics made from them are stretchable.
• dimensional stability is to be understood to mean that the fabrics and knitted fabrics treated by the process according to the invention remain wet and dimensionally stable even after washing and dry cleaning.
• the process according to the invention improves the reshaping ability and imparts a high level of resilience.
• the goods are first provided with measuring marks and then placed in a liquor containing a phosphate buffer mixture and a nonionic detergent without tension (liquor ratio 1:15).
• a short movement of the test pieces follows.
• the samples are then rinsed, centrifuged, dried in a flat state and measured (relaxation shrinkage).
• the samples are washed at 40 ° C. and a liquor ratio of 1:15 without added wetting agent, spun, dried and measured again.
• the linear shrinkages are determined according to the following formulas:
• the area shrinkage results from the following formula: With low shrinkage, A can be disregarded.
• the finished wool samples have generally been laid out for 2 to 3 days after the condensation before the test.
• the tests are carried out after a brief steaming and a further lying time of 3 to 4 hours. In this way, fluctuations in the measurement results are largely avoided.
• the permanent stretch is decisive for the assessment of the stretching ability of knitted fabrics. In order to be able to determine this, it is first necessary to determine the total elongation.
• a specimen (150 x 20 mm punched out in the elastic direction) is clamped vertically on a Du Pont strain gauge over a length of exactly 100 mm, then slowly loaded with 500 g, left at this load for 5 seconds and then relieved. The process is repeated four more times. Then the total length under load is read from the scale in mm.
• the measuring section (exactly 100 mm) is signed on a sample (150 x 120 mm). This pattern is stretched to 80% of its total elongation and, when stretched, is attached to a smooth, flat board using thumbtacks. After 1 hour of stretching, the load is released and the test specimen is left hanging vertically for 1 hour. The remaining total length is then measured in mm.
• Example 1 of GB-PS 15 23 678 an emulsion of a siloxane copolymer, prepared according to Example 1 of DE-OS 27 28 597, with a viscosity of 7,000 mPa-s at 20 ° C, using 8% by weight, based on the siloxane copolymer, of octylphenol polyglycol ether (on average 10 moles of ethylene oxide per mole of octylphenol) as emulsifier. This is then diluted to a content of 27% by weight polysiloxane (emulsion A).
• emulsion A 125 g of emulsion A are diluted to about twice their volume with water, after adding 2 g of 60% acetic acid, 20 g of crosslinking agent I c) are carefully stirred in and then made up to a volume of 1 liter with water.
• each pattern is a wool jersey fabric (about 30 0 g / m 2) is padded to a wet pickup of 80%, largely energized for 20 minutes at 100 ° C dried and then heated for 5 minutes at 125 0 C.
• the sample treated with the liquor I by the process according to the invention has a relaxation shrinkage of only 4.6% and a felt shrinkage of 6.3% according to the method given above.
• the relaxation shrinkage in the sample treated with Fleet II was 9.2% and the felt shrinkage 18.6%.
• emulsion B a 35% emulsion of a dimethylpolysiloxane with terminal hydroxyl groups (viscosity approx. 5,000 mPa.s) is produced using 6% (based on organopolysiloxane) fatty acid polyglycol ester with an average of 10 bound ethylene oxide units as emulsifier (emulsion B).
• Example 5 of GB-PS method described 14 04 356 is a 35% emulsion of a dimethylpolysiloxane having terminal hydroxyl groups (viscosity of 120 000 mPa.s at 20 0 C), using 20%, based on polysiloxane, an ethoxylated alkyl amine with through On average, 16 carbon atoms in the alkyl radical and an average of 10 moles of ethylene oxide units per mole of fatty amine, in the form of the hydrochloride, are produced (emulsion C).
• an equipment fleet is produced using emulsion C (instead of emulsion B).
• Example A 2 samples of the same wool-jersey fabric as described in Example 1 are equipped.
• sample B 2 samples of the same wool-jersey fabric as described in Example 1 are equipped.
• sample A is only dried at 100 ° C. for 15 minutes and then left to rest for 4 days; the other sample (sample B) is condensed for 5 minutes at 125 ° C after drying.
• both samples are chemically cleaned three times with perchlorethylene (without cleaning enhancer) (sample AR or BR). Then the relaxation and felt shrinkage are determined.
• sample AR or BR cleaning enhancer
• a dimethylpolysiloxane with terminal hydroxyl groups (viscosity 5,000 mPa.s at 20 ° C.) with 9% of a cationic emulsifier (Araliphatic quaternary ammonium compound), based on organopolysiloxane, produced an emulsion which is adjusted to a content of 27% of organopolysiloxane (emulsion D).
• emulsion D emulsion D
• This emulsion is used to treat textile materials made of synthetic fibers, namely a polyacrylonitrile knitted fabric with a square meter weight of 150 g and a polyester knitted fabric with a square meter weight of 180 g according to the pull-out method.
• 4% of the emulsion D based on the weight of the textile material to be treated, are diluted with water and 0.4% (based on the weight of the textile material) of the crosslinking agent used in Example 1, pasted with a fatty acid polyglycol ester with 10 ethylene oxide units (5% based added to crosslinking agent) with stirring.
• 0.4% (based on the weight of the textile material) of the dibutyltin dilaurate emulsion also used in Example 1 the liquor is adjusted to a pH of 7.5.
• the extraction process is carried out at a liquor ratio of 1:25 with the polyacrylonitrile fabric at 40 ° C.
• the fleet is clear after only 30 minutes, i.e. the siloxane and the crosslinking agent are completely absorbed on the goods.
• the final pH of the liquor is 8.6.
• the mixture After drying without tension, the mixture is heated to 120 ° C. for 10 minutes.
• the stretch test gives a permanent stretch of 5.5%. This value is not affected by washing three times at 40 ° C or cleaning three times with perchlorethylene.
• the stretch test gives a permanent stretch of 1.5%, which is also washable and dry cleanable.
• the wool jersey fabric (300 g / m 2) is treated at 20 ° C. in the exhaust process, as described in Example 4.
• the crosslinking agent I d) was used for crosslinking in an amount of 0.6%, based on the weight of the goods.
• the fleet was also exhausted after half an hour.
• the sample was heated at 100 ° C for 10 minutes and then at 140 ° C for 2 minutes.
• the jersey fabric is extremely shrink-free and has lost none of its elasticity.
• a 35% emulsion, prepared according to Example 5 of GB-PS 14 04 356, is used to finish a polyester / rayon fabric (50:50; m 2 weight 350 g) in the exhaust process. 5% of the emulsion and 0.6% of crosslinking agent I e), based in each case on the weight of the goods, are used. A smooth cloth with very good recovery is obtained.
• Example 1 The emulsion of Example 1 is used to finish a stretch cotton article using the pull-out method. Of this, 5%, of the crosslinking agent I b) 0.6%, based in each case on the weight of the goods. At an initial pH value of 5.5 and at a temperature of 20 ° C, the liquor is removed after approx. 40 minutes.
• the stretch article is largely dried without tension and condensed at 140 ° C for 5 minutes.
• the article has a very pleasant soft feel. Its recovery capacity is very good.

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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)

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Citations (6)

• 1980
  • 1980-04-16 DE DE19803014675 patent/DE3014675A1/de not_active Withdrawn
• 1981
  • 1981-04-08 EP EP81102634A patent/EP0039783A3/fr not_active Withdrawn

Patent Citations (6)

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