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
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
  • C08L83/04—Polysiloxanes
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
  • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
  • C08G77/04—Polysiloxanes
  • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
  • Y10S8/01—Silicones

Definitions

• repellentfabrics with improved laundering and dry cleaning characteristics and improved crease resistance may be obtained by treating them with certain organosiloxanes.
• certain improvements are to be desired in the results obtained. For instance, some treated fabrics, particularly the smooth-fibered fabrics, such as acetate rayon and nylon, became too slippery. It was found that in the die cutting of stacks of such fabrics, the slippage of some of the individual pieces resulted in imperfect cuttings, with errors in dimensions and form causing an undesirable number of rejects.
• a methylpolysiloxane fluid which contains between 2 and 2.1 methyl radicals per silicon atom and which has a viscosity of at least 1,000
• centistokes and. preferably less than 100,000
• centistokes Such fluids have been described in the art and are now commercially available. They have the general formula (CI-IsJ tSiO4-n, where nhas a value of from 2.0 1102.1.
• Such resins are well knowntothe art. They maycontain units such as (CI-IalzSiO, '(CHaiaSiOs, or unsubstituted silicon in addition to theGHaSiOrs units which constitute a major portion of the notoriously poor in resistance to laundering.
• Treated cotton fabrics have also been found to have too soft a hand, and a more crisp effect has been desired.
• fabrics are rendered water-repellent by wetting the fabrics with a mixture of three organosiloxane polymers.
• the wetted fabrics are then heated at a temperature ranging from 100 to 475 F. fora period of from 5 seconds to one hour.
• the fabrics which may be treated in accord with themethod of this invention include fabrics of natural flberssuch as cotton, silk, linen, or .wool; and fabrics of synthetic fibers such as nylon, *Orlonfand either viscose or acetate rayon.
• methyl radicals and. sucnhydrogen atoms resin may be prepared by methods such as those disclosed in U. S. Patent No. 2,486,162 or French Patent No. 927,276.
• the preferredrange of methyl radicals per silicon atom is from.1.05 to 1.15.
• These resins are normallyemployed in solution in an appropriate organic solvent, and are added as a solution to (I) and (II) above.
• the mixture is made up of from to 45 per cent by weight of the methylhydrcgenpolysilox ane fluid (I), 10 to per cent of the methylpolysiloxane fluid (II), and 20 to 65per centof the methylpolysiloxane resin (III).
• the methylsiloxane resin (III) is preferably added asa solution. Both the amount and type ofsolvent for this solution are immaterial, and the actual weight of solvent present is not included in the to per cent (III) calledfor.
• the composition of the mixture may be varied within the prescribed limits above in accordance with the fabric to be treated and the desired hand to be obtained.
• Catalysts may be added to the organosiloxane mixtureabove, and the mixture then usedto wet the. fabric.
• catalysts include metallic salts vsuch as sodium bicarbonate and sodiumaluminate, andthe me- Alternatively, the fabric may be; wetted with the organosiloxane mixture and the lysts are not necessary to the practice of the invention; however, since they merely speed-up the curing rate.
• the organosiloxane mixture may be applied rectly to the fabric. extend the organosiloxane mixture by diluting with a liquid hydrocarbon, chlorohydrocarbon, ether, or alcohol, such as benzene, dioxane, ethanol, methylene dichloride or the like in order to minimize the amount of siloxane employed.
• a liquid hydrocarbon, chlorohydrocarbon, ether, or alcohol such as benzene, dioxane, ethanol, methylene dichloride or the like in order to minimize the amount of siloxane employed.
• the organosiloxan-e mixture may likewise be extended by the preparation of an aqueous emulsion, which emulsion preferably contains an emulsifying agent decomposable by heating.
• the quaternary ammonium halides are examples of such emulsifying agents. They are decomposed on heating for a brief period. Examples of such halides arethe alkylarylammonium chlorides, such as trimethylbenzylammonium chloride and hexadecyldimethylbenzylammonium chloride.
• Noncationic emulsifying agents such as the amide condensation products of fatty acids with organic amines, are preferred in the treatment ofv cotton, wool, and rayon.
• noncationic emulsifying agent is the product known as Pluramine 8-100, marketed by the Kearny Manufacturing Company, Inc., Kearny, New Jersey.
• the siloxane mixture may be thinned with any of the above indicated solvents in order to facilitate emulsification. After emulsification, the solvent may be removed under vacuum, if desired.
• Emulsions of methylhydrogenpolysiloxanes fre quently liberate hydrogen upon standing.
• an organic acid such as acetic acid
• the quaternary ammonium salts function well as emulsifying agents in such acid systems.
• the siloxane mixture either straight or as solution or emulsion may be applied to the fabric in any appropriate manner.
• the mixture may be applied to the fabric b the use of conventional equipment such as a padder or quetch.
• the fabric may then be dried to remove water or solvent.
• the material should be applied to the fabric in such an amount that there is a pick-up of between one and five per cent of the organosiloxane mixture (not including solvent on water) based upon-the weight of the fabric.
• the fabric is then heated to between l'00'and 475 F. for from five seconds to one hour. This heating effects liberation of a major portion of the hydrogen which is bonded to the silicon in the methylhydrogenpolysiloxane.
• the siloxane present is polymerized by this heating to an insoluble polymer in the fabric, whereby the fabric is rendered permanently hydrophobic. When a heat decomposable emulsifying agent is employed, it is also decomposed during this heating.
• the present invention is of particular importance in the hydrophobing of nylon, acetate rayon, and cotton. It has been found that by the use of the mixture of organosiloxanes disclosed fabric which has a more'crisp hand.-
• organosiloxanes were prepared for use in the examples below. Part given are by weight.
• a mixture was prepared of 1.2 parts by weight of decamethyltetrasiloxane and 735 parts of octamethylcyclotetrasiloxane. To this mixture there were then added .56 part of KOI-I. The mixture was then agitated and heated at 160 C. for "8 hours. i The mixture was then cooled to 100 C. and CO2 in the form of Dry Ice added over a period of 30 minutes. The mixture was then filtered and flash distilled to 250 C. at 1 mm. pressure. There were thereby obtained 620 parts of a trimethylsiloxy end-blocked dimethylpolysiloxane having a viscosity of 30,000 centistokes, which is referred to as product (IIC) in the examples.
• IIC trimethylsiloxy end-blocked dimethylpolysiloxane having a viscosity of 30,000 centistokes
• Example 1 Amixture wasmadeof 30 parts of the methylhydrogenpolysiloxanefluid (1),.20 partslof 30,000 centistokes methylpolysiloxane fluid (I), and 150 partsofthe 33 percent methylpclysiloxane resinsolution (IIIA). To this mixture was added 3133 parts of toluene, giving a 3 per cent solution based onthe organosilicon content. When samples of nylon and acetate rayon are treated with this solution, and then heated at a temperature of 150 C. for IOuminutes, a spray rating (AATCC standard test method 22-41) of 90-100 is obtained. The fabrics have a soft, full hand, and show no slippage eifect when incontact 'With one another.
• AATCC standard test method 22-41 AATCC standard test method 22-41
• Example 1 As the percentage of methylpolysiloxane fluid (IIA, B, C) is decreased, the fabrics become less slippery but begin to show a stiffer hand and have less resistance to mark-off or creasing. Increasing this component causes a drop in water-repellency and results in a more slippery fabric, but improves the resistance to markoif. As the percentage of .methylpolyslloxane resin (1111A) is decreased, the slippage of the fabric increases; raising this percentage produces a stiffer fabric with less Water-repellency and a somewhat brash hand.
• the monomethyl-trimethyl polysiloxane resin (IIIB) compares favorably with the monomethyl-dimethyl polysiloxane resin (IIIA). with the exception that on cotton it imparts somewhat less resistance to laundering. It was indicated that the composition of Example 1 is preferable for maximum water-repelency, wash resistance and resistance to mark-01f; and for minimum slippage of smooth-fibered fabrics.
• polysiloxane resin IIIA
• Example 4 When samples of nylon fabric are treated with the 3 per cent solution of Example 1, and cured for 1 minute at a temperature of 450 results are obtained comparable to the results of the treatment in Example 3.
• Example 5 In order to illustrate the eifectof the presence of the methylpolysiloxane resins, two emulsions were prepared as follows:
• the method of rendering organic fabrics water-repellent which comprises wetting the fabrics with a mixture of from 15 to 45 per cent byweight of a methylhydrogenpolysiloxane fluid of the general formula where a has a, value of from 1.0 to 1.5, b has a value of from 0.75 to 1.25, and the sum of a.
• b has a value of from 2.0 to 2.25; to 30 per cent by weight of a methylpolysiloxane fluid containing between 2.0 and 2.1 methyl radicals per silicon atom and having a viscosity of from 1,000 to 100,000 centistokes; and 20 to 65 per cent by weight of a methylpolysiloxane resin of the gen eral formula where a: has a valueof from 1.0 to 1.25; and heating the wetted fabrics at a temperature of 100 F. to 475 F. for a period of from 5 seconds to 1 hour, whereby the fabrics are rendered water-repellent and slip-resistant.
• the method of rendering organic fabrics water-repellent which comprises wetting the fabrics with an aqueous emulsion of a mixture of from to 45 per cent by weight of a methylhydrogenpolysiloxane fluid of the general formula where a has a value of from 1.0 to 1.5, b has a value of from 0.75 to 1.25, and the sum of a and b has a value of from 2.0 to 2.25; '10 to 30 per cent by weight of a methylpolysiloxane fluid containing between 2.0 and 2.1 methyl radicals per silicon atom and having a viscosity of from 1,000 to 100,000 centistokes; nd to 65 per cent by weight of a methylpolysiloxane resin of the general formula 15 to 45 per cent by weight of a methylhydrogenpolysiloxane fluid of the general formula where a.
• a and b has a value of from 2.0 to 2.25; 10 to 30 per cent by weight of a methylpolysiloxane fluid containing between 2.0 and 2.1 methyl radicals per silicon atom and having a viscosity of from 1,000 to 100,000 centistokes; and 20 to per cent by weight of a methylpolysiloxane resin of the general formula I l where a: has a value of from 1.0 to 1.25.
• the methylhydrogenpolysiloxane fluid is a trimethylsiloxy end-blocked methylhydrogenpolysiloxane
• the methylpolysiloxane fluid is a trimethylsiloxy endblocked dimethylpolysiloxane
• the methylpolysiloxane resin is a copolymer containing (CH3) $101.5 units and units of the group consisting of (CH3)2SiO and (CHa)sSiO.5 units.
• the methylhydrogenpolysiloxane fluid is a trimethylsiloxy end-blocked methylhydrogenpolysiloxane
• the methylpolysiloxane fluid is a trimethylsiloxy endblocked dimethylpolysiloxane
• the methylpolysiloxane resin is a copolymer containing.(CH3) Si01.5 units and units of the group con- 7 sisting of (CH3) 2SiO and (CH3)3SiO.5 units.
• methylhydrogenpolysiloxane fluid is a trimethylsiloxy end-blocked methylhydrogenpolysiloxane
• the methylpolysiloxane fluid is a trimethylsiloxy end-blocked dimethylpolysiloxane
• the methylpolysiloxane resin is a copolymer containing (CH3) SiO1.5 units and units of the group consisting of (CHanSiO and (CH3)3SiO.5 units.

Landscapes

• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Health & Medical Sciences (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Silicon Polymers (AREA)

Priority Applications (4)

Applications Claiming Priority (1)

Publications (1)

Family

ID=22527106

Family Applications (1)

Country Status (4)

Cited By (39)

Families Citing this family (11)

Citations (2)

• 1950
  • 1950-03-09 US US148733A patent/US2588366A/en not_active Expired - Lifetime
• 1951
  • 1951-01-18 GB GB1433/51A patent/GB686212A/en not_active Expired
  • 1951-01-22 FR FR1032744D patent/FR1032744A/fr not_active Expired
  • 1951-03-03 DE DED8112A patent/DE878791C/de not_active Expired

Patent Citations (2)

Also Published As

Similar Documents