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
  • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
  • D06M15/568—Reaction products of isocyanates with polyethers
• • 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
  • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, e.g. by ultrasonic waves, corona discharge, irradiation, electric currents or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
  • D06M10/02—Sonic or ultrasonic waves; Corona discharge
  • D06M10/025—Corona discharge or low temperature plasma
• • 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
  • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, e.g. by ultrasonic waves, corona discharge, irradiation, electric currents or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
  • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
  • D06M10/08—Organic compounds
  • D06M10/10—Macromolecular compounds
• • 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
  • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
• • 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
  • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
  • D06M2101/02—Natural fibres, other than mineral fibres
  • D06M2101/10—Animal fibres
  • D06M2101/12—Keratin fibres or silk

Definitions

• the invention relates to felt-free finished wool and a process for its production comprising a) a plasma treatment of the wool and b) an aftertreatment with aqueous dispersions of self-dispersing isocyanates.
• Isocyanates have long been known as auxiliaries for the finishing of textiles with felt and can, for example, as described in DE-OS-19 04 802, in organic solvents are used, or, as described in DE-OS-17 69 121, in aqueous dispersion with the addition of emulsifiers. Both organic Solvents and optionally wastewater-polluting emulsifiers are today out of date for ecological and industrial hygiene reasons. Developed self-dispersing isocyanates and formulations, which with as small amounts of solvents or emulsifiers as Aids and additives get by.
• DE-OS-1 794 221 describes the treatment of fiber materials with isocyanate prepolymers, which still contain free isocyanate groups; this equipment can be in Solvents such as perchlorethylene or in aqueous emulsion using Auxiliary emulsifiers are used.
• US-A-3,847,543 discloses a method for non-felting of wool in which in aqueous dispersion at the same time aliphatic isocyanates, OH-functional crosslinkers and organometallic catalysts are present. Although this procedure In the aqueous phase, auxiliary solvents and emulsifiers are required.
• DE-OS-26 57 513 describes a process for the felt-free finishing of wool the wool yarn is treated with an aqueous liquor containing the felt-proofing agent.
• Reactive polyolefins, reaction products made from polyisocyanates are used as felt-strength agents and hydroxyl compounds, silicone polymers, aziridine compounds, Reaction products of epoxides with fatty amines and dicarboxylic acids or Polyamides, reaction products with thiosulfate end groups or preferably reaction products used with mercapto end groups.
• WO 95/30045 describes a process in which special isocyanates are used for finishing with felt be used by wool.
• This can be solvent-free and without an emulsifier be worked because the isocyanates used are water dispersible.
• First the wool is pre-treated with oxidizing agents, followed by a reduction treatment before the water dispersing isocyanates are used.
• a disadvantage of this process is that the oxidative and reductive pretreatment causes wastewater, which is in accordance with regulations must be neutralized and clarified.
• DE 196 16 776 C1 also describes a method for finishing felt-free wool, in which moist wool material with a water content of 4 to 40% by weight is subjected to a low-pressure plasma treatment prior to further processing into textile fabrics or webs.
• a pressure of 10 -2 - 10 mbar the wool is subjected to a high-frequency discharge of a frequency of 1 kHz - 3 GHz and a power density of 0.001 - 3 W / cm 3 over a period of 1 - 600 seconds, optionally with the addition of non-polymerizing gases .
• the disadvantage of this method is the complex equipment. Special vacuum pumps are required and vacuum locks must be installed to allow the material to flow in and out
• the invention is based on the object of a technically improved method Provide felt-free finished wool, which after processing Made-up goods do not become matted and shrink in machine wash.
• the wool used can be a wide variety of wool materials act, e.g. Raw wool after raw wool washing, dyed or undyed wool sliver, dyed or undyed wool yarn, knitted fabric, knitted fabric or fabric.
• the water content of the wool is usually 4 to 40% by weight, preferably 5 up to 30% by weight, particularly preferably 6 - 25% by weight and in particular 8 - 15% by weight.
• the wool is subjected to a corona treatment exposed to a plasma.
• the corona treatment is done with a pressure in the range of 100 mbar - 1.5 bar, preferably carried out at normal pressure.
• the wool is subjected to a high-frequency discharge with a power density of usually 0.01-5 Ws / cm 2 over a period of 1-60 seconds, preferably 2-40 seconds and in particular 3-30 seconds, optionally with the addition of non-polymerizing gases .
• Suitable non-polymerizing gases are air, oxygen, nitrogen, noble gases or mixtures thereof.
• the actual plasma is generated by applying an alternating voltage of 1-20 kV Frequency range between 1 kHz and 1 GHz, preferably 1-100 kHz generated on electrodes, one or both poles being provided with an insulator material.
• the AC voltage can either be continuous or with individual pulses or with pulse trains and breaks in between.
• Corona treatment is preferred performed on electrical discharges in the normal pressure range, the to be treated Wool is first inserted into a closed, sealed treatment housing, there with the working gas, i.e. the non-polymerizing mentioned above Gas, loaded and then in a gap between at least two treatment electrodes is exposed to an electrical barrier discharge.
• the distance the wool material to the treatment electrodes is 0 - 15 mm, preferred 0.1 - 5 mm and especially 0.3 - 2 mm.
• the treatment electrodes are preferred formed as rotatable rollers, one or both of which are electrically fixed dielectric material are coated.
• the special effect of the plasma treatment in step a) of the invention Procedure could be explained as follows.
• the liquid present in the fiber desorbs as water vapor / gas from the fiber surface during the process. It comes to the formation of high-energy electrons, ions and highly excited neutral molecules or radicals that act on the surface of the fiber, the water vapor desorbed from the fiber causes immediate Particularly reactive particles are formed near the respective fiber surface, that act on the surface.
• self-dispersing in the present context means that the Isocyanates in a concentration of up to 70% by weight, preferably up to 50 Wt .-%, in water finely divided dispersions with particle sizes of ⁇ 500 nm (measured using an ultracentrifuge).
• the unmodified polyisocyanates I) to be used according to the invention can also in combination with external, i.e. additional ionic or nonionic Emulsifiers are used.
• additional ionic or nonionic Emulsifiers are used.
• Such emulsifiers are for example in Methods of Organic Chemistry, Houben-Weyl, Vol. XIV / 1, Part 1, page 190-208 Thieme-Verlag, Stuttgart (1961) and in US-A-3,428,532 and EP-A-0 013 112 described.
• the emulsifiers are used to ensure dispersibility Quantity used.
• polyisocyanates I) are first reacted with polyalkylene oxide alcohols II), this reaction can be carried out in a manner known per se, while maintaining an NCO / OH equivalent ratio of at least 2: 1, generally from 4: 1 to about 1000: 1.
• polyethylene oxide-modified polyisocyanates When using polyethylene oxide alcohols, polyethylene oxide-modified polyisocyanates are obtained which have an average NCO functionality of 1.8-4.2, preferably 2.0-4.0, and an aliphatic or cycloaliphatic isocyanate group content of 12.0-21 , 5% by weight and a content of ethylene oxide units arranged within polyethylene oxide chains, calculated as C 2 H 4 O with a molecular weight of 44 g / mol, of 2 - 20% by weight, the polyethylene oxide chains on average 3 - 70 have ethylene oxide units.
• the starting components I), II) and optionally III) can be in any Order excluding moisture, preferably without solvent, be implemented.
• the viscosity increases of the end product. If the viscosity rises above 100 m Pas, so it makes sense to work in the presence of a solvent, preferably with Water miscible but inert to the polyisocyanate.
• Suitable solvents are e.g. Alkyl ether acetates, glycol diesters, toluene, carboxylic acid esters, acetone, Methyl ethyl ketone, tetrahydrofuran and dimethylformamide.
• the implementation of the components can be accelerated.
• the reaction is carried out in the temperature range up to 130 ° C., preferably in the range from 10-100 ° C. and particularly preferably from 20 to 80 ° C.
• the course of the reaction is followed by determining the NCO content by titration or by recording IR spectra and evaluating the NCO band at 2260-2275 cm -1 .
• the reaction is complete when the isocyanate content is not more than 0.1% by weight above the value which is achieved for a given stoichiometry in the case of complete conversion. As a rule, response times of less than 24 hours are sufficient.
• the solvent-free synthesis of the self-dispersing isocyanates to be used according to the invention is preferred.
• the number of NCO-reactive equivalents is the Polyalkylene oxide content, the NCO content and the NCO functionality by appropriate Weighing in of the above three components by a person skilled in the art that the mixture obtained has the composition required for water dispersibility has, whereby the preferred areas already mentioned apply.
• the self-dispersible isocyanates are technically easy to handle and many Stable for months without moisture.
• the self-dispersible isocyanates are in step b) of the invention Process preferably used without organic solvents. Because of your These isocyanates are self-dispersible at temperatures up to 100 ° C in water easy to emulsify without exposure to high shear forces.
• the isocyanate concentration in the emulsion can be up to 70% by weight. But it is more advantageous, emulsions with an isocyanate concentration of up to 50% by weight produce, which may then be further diluted before the dosing point can be.
• Mixing units customary in technology are suitable for emulsification (Stirrer, mixer with rotor-stator principle or high pressure emulsifying machines). A static mixer is usually sufficient.
• the received Emulsions have a processing time of up to 24 hours, which of the Structure of the self-dispersible isocyanates used, in particular of their Content of basic N atoms depends.
• Treatment of wool with an aqueous dispersion of self-dispersing Isocyanates in step b) are carried out by customary methods of the prior art.
• a batch operation in the exhaust process is suitable or a continuous way of working through dipping, roller application, Padding, spraying, spraying or lisseuse application if necessary using dyeing machines, agitators etc. to move the treatment liquor.
• the fleet ratio can be selected within wide limits and can be in Range from 1: (5-20), preferably from 1: (5-10).
• the self-dispersing Isocyanate is 0.1-5% by weight, preferably 0.5-2.5% by weight, based on the total weight of the fleet used.
• an isocyanate with an NCO content of 22.5% consisting of essentially from trimeric hexamethylene diisocyanate, at 60 ° C with 15 Parts by weight of an ethylene oxide polyether started on morpholine with a average molecular weight of 420 implemented.
• the resulting product has one NCO content of 16.5% and a viscosity of 2550 mPas at 25 ° C.
• the product can be easily mixed in one by simply stirring with a glass rod disperse the water-sensitive beaker.
• a wet wool sliver is subjected to a corona plasma treatment, the following being followed.
• the baths are so-called liss recipients, which hold 450 l and one inside Have sieve drum around which the sliver is guided. At the same time the bath contents are kept in motion and circulated by strong circulation pumps, so that the ridge is intensely flowed through. After leaving the bath the Comb pull on a crushing machine freed from adhering excess liquor.
• the well-rinsed ridge is first placed in a drum dryer forwarded where it is dried in three areas; which are separate from each other selected temperatures are given in the table below.
• the equipped comb is used in accordance with the IWS standard TM 31 (The Woolmark Company, IWS test method TM 31, July 1996) spun a yarn which is processed into a knitted fabric. This knitted fabric is subjected to 5 washing cycles and then its area shrinkage is determined in%. This surface shrinkage is a measure of the tendency to felt. The lower the Is the lower the tendency to felt and the better the Non-felt equipment.

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Physics & Mathematics (AREA)
• Plasma & Fusion (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)
• Polyurethanes Or Polyureas (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Applications Claiming Priority (2)

Publications (2)

Family

ID=7891748

Family Applications (1)

Country Status (7)

Cited By (3)

Families Citing this family (6)

Family Cites Families (16)

• 1998
  • 1998-12-18 DE DE19858736A patent/DE19858736A1/de not_active Withdrawn
• 1999
  • 1999-12-06 EP EP99123974A patent/EP1010799A3/fr not_active Withdrawn
  • 1999-12-08 US US09/457,287 patent/US6242059B1/en not_active Expired - Fee Related
  • 1999-12-09 JP JP11350321A patent/JP2000178869A/ja active Pending
  • 1999-12-15 NZ NZ501815A patent/NZ501815A/en unknown
  • 1999-12-16 TR TR1999/03117A patent/TR199903117A2/xx unknown
  • 1999-12-17 AU AU65352/99A patent/AU767898B2/en not_active Ceased

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