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US3449061A - Wool fibers sensitized for setting by applying thereto one member of a reducing agent-producing coreactant pair,mechanically finishing and applying the second member of said pair - Google Patents

Wool fibers sensitized for setting by applying thereto one member of a reducing agent-producing coreactant pair,mechanically finishing and applying the second member of said pair Download PDF

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US3449061A
US3449061A US278359A US3449061DA US3449061A US 3449061 A US3449061 A US 3449061A US 278359 A US278359 A US 278359A US 3449061D A US3449061D A US 3449061DA US 3449061 A US3449061 A US 3449061A
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fabric
reducing agent
minutes
gas
applying
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Earl Peters
James Palmer Cain
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Deering Milliken Research Corp
Milliken Research Corp
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Milliken Research Corp
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    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating 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 sulfur or phosphorus
    • D06M13/248—Treating 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 sulfur or phosphorus with compounds containing sulfur

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  • This invention relates to novel processes for modifying the characteristics of keratin fibers and, more particularly, to novel processes for presensitizing fabrics containing keratin fibers for subsequent durable setting, the presensitizion being accomplished in such a manner that desirable finishes on the fabrics may be provided.
  • This: invention relates particularly to such presensitizing processes whereby the final setting of the fabrics, such as in the form of garments produced therefrom, may be accomplished under normal moisture conditions, i.e., without the addition of moisture beyond the moisture regain level of the fibers.
  • Typical finishing operations include full decating, wherein the fabric, in rolled form and in contact with a particular leader cloth, is exposed to steam in a pressurized autoclave for several minutes after which vacuum conditions are imposed on the fabric.
  • An alternative operation, called semi-decating, is similar to full decating, except that steam at atmospheric pressure is forced through the rolled fabric.
  • These finishing techniques are somewhat similar to the conditions necessary to set the fabric, e.g., in garment form, to a desired configuration.
  • the full decating operation substantially destroys the presensitization in the fabric. Consequently, the somewhat milder semi-decating operation has been used. Even this mild finishing operation, however, can cause the loss of a substantial degree of the presensitization if care is not taken.
  • Normal fabrics have some residual relaxation shrinkage, but this difficulty is overcome by wetting the fabric thoroughly prior to cutting into garment form and drying in a relaxed state.
  • This technique is not practicable for presensitized fabrics since the presensitizing chemicals are substantially removed by the wetting operation. Consequently, it has been necessary to exercise a high degree of control over these novel presensitizing processes to avoid building into the fabrics a high residual relaxation shrinkage.
  • the keratin fibers of the fabric are not in reduced form until after all finishing operations have been completed, so that no extraordinary care must be taken to avoid inducing high residual relaxation shrinkage properties into the fabric.
  • reducing agent precursor as utilized herein is meant a chemical compound which forms a reducing agent for keratin fibers upon reaction with another chemical compound. It is generally preferred that the precursor compound have a pH of about 7 or greater as a 1% solution in water.
  • Particularly suitable compounds include lower alkanolamines, such as monoethanolamine, diethanolamine, triethanolamine, N-methyl ethanolamine, N- ethyl ethanolamine, N,N-dimethyl ethanolamine, N,N- diethyl ethanolamine, N,N-diisopropyl ethanolamine, N- aminoethyl ethanolamine, N-methyl diethanolamine, npropanolamine, isopropanolamine, triisopropanolamine, n-butanolamine, dimethyl-butanolamine, dimethylhexanolamine, polyglycolamines of the general formula HO(C H O),RNH wherein at is a positive integer and R is alkyl, e.g
  • additional compounds include other amines,-for example those characterized by the formula R(NH wherein x is a positive integer of from 1 to about 4 and R is alkyl (e.g., ethylamine, hexylamine and the like); aryl (e.g., aniline, toluidines, benzidine, and the like); R'CONH- wherein at: 1, and R is alkyl or aryl, (e.g., hydrazides, such as acetoyl hydrazide H CCONHNH butyrohydrazide, benzoylhydrazide, and the like); hydrazines of the formula 'R"NHNH wherein R" is selected from hydrogen, alkyl, aryl, and the like; e.g., hydrazine, methylhydrazine, phenylhydrazine and the like; piperazine compounds, such as
  • Additional suitable basic precursor compounds include alkalis, such as the alkali-earth metal and alkali-metal compounds, including the hydroxides, carbonates, borates, phosphates, e.g., sodium hydroxide, potassium hydroxide, lithium hydroxide, strontium hydroxide, barium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, sodium borate, potassium borate, sodium per-borate, disodium monohydrogen phosphate and the like.
  • alkalis such as the alkali-earth metal and alkali-metal compounds
  • hydroxides e.g., sodium hydroxide, potassium hydroxide, lithium hydroxide, strontium hydroxide, barium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, sodium borate, potassium borate, sodium per-borate, disodium monohydrogen phosphate and the like.
  • Additional reducing agent precursor chemicals include aldehydes, particularly formaldehyde and glyoxal, although other aldehydes are suitable, e.g., saturated aliphatic aldehydes containing up to about 18 carbon atoms, such as acetaldehyde, propionaldehyde, butyraldehyde, valeraldehyde, caproaldehyde, enanthaldehyde, nonalde- "hyde, palmitic aldehyde and the like; unsaturated aliphatic aldehydes, such as acrolein, crotonaldehyde, tiglic aldehyde, citral, propioaldehyde and the like; alicyclic monofunctional aldehydes, such as formylcyclohexane and the like; aliphatic dialdehydes, such as glyoxal, pyruvaldehyde, malonaldehyde, succinalde
  • ammonia per se can be utilized as a reducing agent precursor, e.g., in combination with S or N 0 activator gases.
  • Ammonia may be provided as a gas, preferably anhydrous, or as amrnonium hydroxide, methylammoniurn hydroxide, ethylammonium hydroxide and similar compounds. When applied as a gas, it may be applied before, after or during the desired finishing operation.
  • ammonia gas may be utilized in combination with other reducing agent precursors.
  • a wool fabric can be impregnated with an alkanolamine, finished, and then exposed to both ammonia and S0 gases. This technique provides particularly excellent presensitization in that better creases, or other configurations, of improved durability can be accomplished in this matter.
  • ammonia may be utilized as a reducing agent activator per se, particularly in combination with nitrites to form ammonium nitrites, ammonium complexes and the like.
  • the reducing agent precursor except for ammonia gas, is preferably applied to the fabric prior to finishing in that these compounds are most conveniently applied to the fabric in liquid media which would substantially destroy the finish on the fabric.
  • Most of the precursors are soluble in water and can be applied to the fabric as aqueous solutions, although dispersions, emulsions and other systems are suitable. Uniform impregnation of the fabric is readily accomplished by conventional techniques, such as padding, spraying and the like. It should be appreciated, however, that the precursor chemical may be applied in gaseous form before or after finishing if the practitioner prefers to volatilize the normally liquid precursor systems.
  • reducing agent activator as utilized herein is meant a chemical compounds, preferab y in a g o t which can react with one of the above reducing agent precursors to form a different chemical compound which is a reducing agent for keratin fibers, i.e., is capable of rupturing the disulfide bonds of the keratin fiber molecular structure. It is not known with certitude if a reducing agent per se is formed in situ on the keratin fibers being treated, although the formation thereof is highly probable.
  • Most of the preferred activator gases are reducing agents for keratin fibers and it is possible that the pretreatment of the fibers with one of the precursor chemicals may merely sensitize the fibers for more efficient reaction of the keratin fibers with the reducing agent gas, whereby presensitization of the fibers for subsequent durable setting is effected.
  • presensitization is effected by the process of this invention where treatment with a reducing agent per se is essentially ineffective for such purpose.
  • excellent presensitization of keratin fibers for subsequent durable setting in the absence of large amounts of water is effected by the process of this invention wherein the fabric is first impregnated with monoisopropanolamine, subjected to the desired finishing operation and then exposed to S0 possibly to produce monoisopropanolamine sulfite in situ on the fabric.
  • S0 is a highely preferred reducing agent activator gas.
  • suitable activator gases include, however, hydrogen sulfide; mercaptans, such as methyl mercaptan (B.P. 6 C.), ethyl mercaptan (B.P. 37 C.) and the like; mercaptan alcohols, such as Z-mercaptoethanol (B.P. 5052 C. at 10 mm. Hg) and the like; nitrogen oxides, such as N 0 and the like; phosphoruscontaining gases, such as phosphine and the like; nitrosating agents, such as NOCl, NOBr and the like.
  • the amount of reducing agent precursor and activator gas can be readily determined by one skilled in the art depending on the fabric being treated and the extent of presensitization desired.
  • the preferred precursor chemicals are fairly strong bases. Keratin fibers tend to degrade considerably during prolonged storage under basic conditions. It is preferred, therefore, that a sufficient amount of the reducing agent activator gas, which generally is acidic, be utilized for substantially complete reaction with the precursorchemreal or until substantially neutral fabric is produced. Obvlously, the fabric may be shipped under slightly acidic or basic conditions, or even under highly acidic or basic conditions, but the optimum degree of physical properties in combination with the presensitized characteristic is obtained when the fabric is shipped essentially neutral.
  • the fabric treated in accordance with this invention has a higher degree of creasability after prolonged storage than fabrics treated by previous technrques,
  • the performance of the fabric after storage 1s generally superior to the performance immediately after gassing. Consequently, conventional storage time has become an asset rather than a liability in the present presensrtlzing technique.
  • Fabric containing the precursor chemical may be exposed to the gaseous activator in conventional equipment.
  • steam boxes, decating apparatus, beam and package dye machines, drying ovens and the like may be utilized.
  • low molecular weight polyhydroxy compound a compound containing more than one hydroxy group and having a molecular weight no greater than about 4000'.
  • the most readily available and desirable compound comprises ethylene glycol.
  • a particularly preferred group of glycols includes the polyfunctional glycols having terminal hydroxyl groups separated by 2 to methylene groups, including, of course, the preferred ethylene glycol as well as trimethylene glycol, tetramethylene glycol, pentamethylene glycol, hexamethylene glycol, heptamethylene glycol, octamethylene glycol, nonamethylene glycol, and decamethylene glycol, or such glycols as 1,2-propylene glycol, dipropylene glycol, 1,3- butylene glycol, diethylene glycol, polyethylene glycol or the like.
  • Polyfunctional compounds containing more than 2 hydroxyl groups include the polyfunctional alcohol glycerols such as glycerine, quintenyl glycerin, diethylglycerol and mesicerin, as well as trimethylol ethane, trimethylol butane, tris(hydroxymethyl)aminomethane and others.
  • Glycol ethers such as the water-soluble or dispersible polyethylene glycols or polypropylene glycols having molecular weights no greater than about 4000 also provide satisfactory results when utilized in accordance with this invention.
  • Urea constitutes the most readily available and desirable swelling agent, although any other material which will swell wool fibers in an aqueous medium is suitable.
  • guanadine compounds such as the hydrochloride; formamide, N,N-dimethylformamide, acetamide, thiourea, phenol, lithium salts, such as the chloride, bromide and iodide and the like are similarly useful.
  • the swelling agent or low molecular weight polyhydroxy compound may be utilized in any desired amount depending on requirements for particular fabrics. For example, as little as about 0.5 to about 1% of the additives, based on the weight of the fabric, provides some improvement, although, in general, larger amounts, e.g., from about 3 to about 10% by weight provide noticeable improvement. Larger amounts of up to about 50% or higher may be utilized, of course, if the particular end use justifies the increased chemical cost in the use of these additives.
  • the application of the swelling agent and/or the polyhydroxy compound is generally a wet process, it is preferably conducted prior to finishing.
  • finishing as utilized herein is meant a mechanical operation whereby at least one surface of the fabric is treated to impart thereto a more lustrous appearance and/ or pleasing hand. 'In this context, finishing is a well-known and conventional operation.
  • any desired finishing technique may be utilized, e.g., rotary pressing and the like, steaming techniques such as semi-decating and full decating are preferred. These techniques apply little or no tension to the fabric, thereby minimizing residual relaxation shrinkage.
  • Full decating involves wrapping the fabric around a perforated drum located in a pressure autoclave. Steam is forced through the drum and the fabric under a constant pressure, generally up to about 30 pounds per square inch gauge for several minutes, e.g., about 1-5 minutes, after which vacuum conditions across the fabric are maintained for another several minutes, e.g., 2-20- minutes.
  • Treatment of fabrics in accordance with this invention may be conducted under atmospheric conditions if desired. It is generally preferred, however, to conduct the treatment under conditions of elevated temperatures and pressures. Improved results are obtained when the fabric containing a precursor chemical is heated slightly before, during or after treatment with the activator gas.
  • the level of temperature is preferably below the volatilization temperature of the precursor chemical and below the decomposition temperature of the expected reaction product. For most of the preferred combinations of precursor and activator gas, this temperature will be below about 212 F., preferably below 180 F.
  • the fabric since the keratin fibers of the fabrics being treated in accordance with the process of this invention are not in a reduced state until after gassing, the fabric, after padding with the precursor chemical, may be dried at levels normally encountered in mill operations, for example, about 200 F. and usually not in excess of 250 F. When this drying procedure is conducted with the fabric under substantially relaxed conditions, the resulting fabric is characterized by even lower area shrinkage than is untreated fabric. In this condition, the fabric may be shipped to a garment manufacturer who can cut the fabric as received without conducting the sponging or shrinking operations which he would be forced to conduct with conventional fabrics.
  • fabric treated as disclosed herein has low residual relaxation shrinkage since it is not handled in a wet, reduced state.
  • the garment manufacturer may cut the fabric of this invention into the desired configuration necessary for the production of a garment, sew the garment, press the garment without any additional step of treatment required and obtain a garment characterized by durable creases or pleats, as the case may be.
  • the flat areas of the garment manufactured from the fabric of this invention are also characterized by a tendency to maintain a desirably flattened configuration, even under hot, wet conditions.
  • While the process of this invention is particularly adapted to fabrics composed essentially of keratin fibers, particularly those composed entirely of Wool fibers, it is also applicable to fabrics wherein synthetic, natural, or other keratin fibers are blended with the wool component.
  • Other keratin fibers include mohair, alpaca,
  • Preferred synthetic fibers for blending with wool fiber-s include polyamides, such as polyhexamethylene adipamide; polyesters, such as polyethylene terephthalate; and acrylic fibers, such as acrylonitrile homopolymers or copolymers containing at least about 85% combined acrylonitrile, such as acrylonitrile/rnethyl acrylate (85/ 1S), and cellulosics, such as cellulose acetate and viscose rayon.
  • polyamides such as polyhexamethylene adipamide
  • polyesters such as polyethylene terephthalate
  • acrylic fibers such as acrylonitrile homopolymers or copolymers containing at least about 85% combined acrylonitrile, such as acrylonitrile/rnethyl acrylate (85/ 1S)
  • cellulosics such as cellulose acetate and viscose rayon.
  • cotton is preferred.
  • the fibers need not be in fabric form during treatment.
  • the process may be conducted on top, tow, roving, sliver, yarn and the like.
  • the process of this invention may be performed on woven, non-woven, or knitted fabrics of any type, dyed or undyed, provided, of course, that the dyes are stable to the precursor and activator chemicals.
  • the dyes are far less sensitive to the precursor chemicals than they are to the reducing agents utilized in previous processes.
  • the fabric may be treated over a wide range of pH.
  • a conventional finishing treatment applied to wool fabrics involves the application to the fabric of concentrated sulfric acid in order to carbonize cellulosic impurities present in the fabric. After this treatment, from 2 to 3% by weight of sulfuric acid is often left on the fabric.
  • fabrics so treated may be subjected to the process of this invention without being neutralized, although, obviously, the fabric may be neutralized if, for some reason, the operator prefers.
  • the preferred reducing agent precursors are basic. Wool fabrics, for example, degrade if maintained under basic conditions for extensive periods of time. Consequently, it is preferred that the gas reaction be conducted to an extent sufficient to provide an essentially neutral fabric shipment.
  • a typical apparatus for conducting the processes of this invention is shown schematically in the drawing.
  • the apparatus includes reaction chamber 1 partially surrounded by jacket 2 for heating or cooling the chamber and its contents. Steam or other heating or cooling fluid can be admitted through inlet valve 3 and withdrawn through outlet valve 4.
  • a perforated spindle 6 Mounted within the reaction chamber 1 in circulating relationship with conduit 14 is a perforated spindle 6. Full width lengths of fabric 7 supported on a perforated beam 8 is mounted over the perforated spindle 6.
  • a four-way reverse valve 9 is provided within the recirculation system for changing the direction of flow of the gas or gases utilized in the process, valves 10 and 11 being provided for flow rate control.
  • Hand lever 12 is provided for manual operation of the valve, although automatic control can be readily provided.
  • the recirculating system connected to four-way valve 9 includes recirculating conduits 13 and 14, motor-driven air pump 15 (motor not shown), heat exchanger 16 connected to steam or water line 17 and return line 18, gas supply conduit 19 connected through an automatic valve 20 and heat exchanger 21 to pressurized gas container 22 mounted on scale 23 electrically connected to valve 20 for automatic control.
  • Heat exchanger 21 is provided with steam or water line 24 and return line 25.
  • a similar system for an additional gas is connected into the recirculating system through conduit 26, automatic valve 27, heat exchanger 28 having steam or water line 29 and return line 30 to pressurized gas container 31 mounted on scale 32 electrically connected to valve 27 for automatic control.
  • Additional valves 33 and 34 are provided for control of the flow of the gas or liquids fed into heat exchangers 21 and 28, respectively.
  • Blow-out disk 35 is provided in the recirculating system and a similar disk 36 is provided in the vent for reaction chamber 1.
  • An air intake valve is provided in the recirculating system at 37 and a vent valve is provided in the reaction chamber at 38.
  • the fabric beam is mounted within reaction chamber 1 onto perforated spindle 6 in circulating relationship with conduit 14 of the recirculating system.
  • the fabric can be preheated if desired by admitting steam to jacket 2.
  • Ammonia gas from container 22 is fed into heat exchanger 21 and through automatic valve 20 into conduits 19 and 14 until a predetermined amount is registered on scale 23 at which time the coordinated automatic valve 20 closes. This gas is then passed through conduit 14 into perforated spindle 6, perforated beam 8 and fabric 7 and back into the recirculating system conduit 13 where it passes through heat exchanger 16 for maintenance of of the desired gas temperature. This direction of fiow is called inside-out flow.
  • valve 9 After a predetermined period of time, the direction of flow is reversed by switching valve 9 to the position shown by the dotted lines at 9'. In this position, the flow of the gas is reversed through the valve 9 so that the gas enters the area surrounding the fabric beam where it is pulled through fabric 7, perforated beam 8 and perforated spindle 9 back into conduit 14 of the recirculating system. This direction of flow is called outside-in flow.
  • valve 10 After a predetermined period of exposure to the ammonia gas, the machine is vented by closing valve 10, opening inlet valve 37 and venting valve 38 of the reaction chamber 1, while continuing the cycling operation. After a few minutes, valve 10 is opened and valves 37 and 38 are closed.
  • Liquid sulfur dioxide from container 31 is then passed into heat exchanger 28 which is heated by steam.
  • the liquid immediately vaporizes and is then admitted through valve 27 which automatically closes upon signal from scale 32 that a predetermined amount of liquid has been utilized.
  • the machine After recirculation for the desired time, the machine is vented to the atmosphere as before, after which additional ammonia is fed into the system for recirculation.
  • This apparatus can be used for any embodiment of this invention, e.g., wherein the fabric has been pretreated with a reducing agent precursor chemical and wherein one or more gases are utilized.
  • Tongue tear strength is measured according to the A.S.T.M. Test for Woven Fabrics (Designation 39), Tongue Method; flex abrasion according to A.S.T.M. Test for Abrasion of Textile Fabrics (Designation 1175),
  • Reducing power (expressed as percent 50 is determined by extracting a 50 gram sample of presensitized wool fabric in a Soxhlet extractor with methanol for four hours under nitrogen atmosphere. After extracting and cooling, the extract is diluted to 250 ml. in volumetric equipment. A ten-ml. aliquot of the extract is placed in a ml. Erlenmeyer flask along with 50 ml. water, 10 draps of 6 N H 50 and 1 ml. starch indicator solution.
  • Dry crease performance data are obtained from presensitized fabric samples having dimensions of 4 /2 inches in the filling direction by 6 inches in .the warp direction. These samples are folded in half with the fold parallel to the warp yarns. The samples are then placed on a Hoffman press, the cover is closed and locked and the samples are pressed with 30 seconds top steam and 30 seconds baking, followed by 10 seconds vacuuming.
  • the creased samples are then opened and placed in a standing water bath which contains a wetting agent and is heated to 170 F. After 30 minutes the samples are removed, folded along the original crease line and allowed to air dry. After drying, the creases remaining in the samples are rated subjectively by at least three observers, the crease ratings running from 1 (no appreciable crease) to (very sharp crease).
  • Wet creases are measured by either of the above techniques by wetting the .presensitized fabric Samples with water to 40% wet pick-up prior to Hoffman pressing.
  • EXAMPLE I An all wool fabric, Deering Milliken Style 8012 worsted fabric, is impregnated with an aqueous solution containing 5.5% monoethanolamine and 0.1% Sulfonic N-95 non-ionic ethylene oxide condensate type Wetting agent. After drying, the fabric is steamed on a Hofiman press to impart a desirable finish thereto. The finished fabric is then rolled onto a perforated spindle and S0 gas at 3 liters/minute is forced through the spindle and fabric for 3 minutes.
  • the fabric After storage for 24 hours, the fabric is creased without the addition of water and tested as set forth above to provide a crease rating of 3.0.
  • EXAMPLE II A sample of worsted fabric Style 8012 is padded to 80% pick-up with an aqueous solution of 6.0% monoisopropanolamine and 0.1% Syn-Fac 905, a non-ionic ethylene oxide condensate type wetting agent. The temperature of the pad-bath is 75 F. The impregnated fabric is then dried in a tensionless dryer at 215 F. to a moisture level of 10%. After drying, the fabric is semidecated, the cycle consisting of steam breakthrough plus 1% minutes of steam at p.s.i. gauge, followed by three minutes vacuum pumping at 500 mm. mercury.
  • the fabric After semi-decating, the fabric is rolled onto a perforated spindle for a full-decater autoclave.
  • the spindle is placed in the autoclave, the unit is sealed, and the fabric is heated to F.
  • Sulfur dioxide gas is then introduced into the system in stoichiometric proportions to that amount of monoisopropanolamine previously padded onto the fabric.
  • the fabric After introduction of the sulfur dioxide into .the closed system, the fabric is allowed to stand in the sulfur dioxide vapors for an additional 10 minutes, after which air is forced through the fabric,
  • the autoclave being ventilated to permit removal of any remaining and/or unreacted sulfur dioxide.
  • Example III The procedure of Example II is repeated except that a Gaston County (Theis) Drying Machine is utilized for the gassing step. In this machine, S0 gas is recirculated back and forth through the fabric until all the amine has, theoretically, reacted. Fabric treated in this manner has a crease rating of 2.5.
  • Example IV The procedure of Example II is repeated except that the semidecating cycle is 5 seconds steaming after breakthrough, followed by 2 minutes vacuum pumping. In addition, the fabric is placed in a Burlington Dyeing Machine and pre-heated to 80 F. prior to gassing. Crease ratings of 2.0 are obtained in this manner. This value increases to 2.5 after 1 weeks storage.
  • Example V The procedure of Example II is repeated except that 5% ethylene glycol is added to the pad bath. Crease ratings after 24 hours are 2.3; after 1 week, 2.5.
  • the fabric After drying at 200 F. and semi-decating at a cycle of 5 seconds steam followed by 2 minutes vacuum pumping, the fabric (weight of 70 lbs.) are rolled onto the beam of a Burlington Dyeing Machine. The unit is then sealed and S0 is forced through the beam at 15 liters per minute, corrected to atmospheric pressure, for a time period computed at 0.28 minutes per pound of fabric. This amount of S0 gives the stoichiometric amount necessary to combine with the amine. The gassing operation is continued for 20 minutes, after which the fabric is permitted to stand for an additional 20 minutes in the SO -laden atmosphere within the machine. Compressed air is then introduced into the beam inlet to expel excess S0 from the fabric prior to removal of the beam from the machine.
  • the pres sure decreases as the S0 reacts, thereby providing the practitioner with a method of controlling the amount of S0 utilized through measurement of pressure drop.
  • break vacuum of 71 cm. with S0 allow pressure to increase; break vacuum of 47 cm. to 0 with NHs.
  • Example IX The fabric of Example I is treated as in Example VIII under varying conditions of pressure of the package dye machine and with the fabric pre-heated to various temperatures. The conditions are set forth in Table IX, the pH of the fabric after such treatments, the reducing power, various physical properties and crease performances, both with and without added moisture, being shown in Table X. The wet crease ratings are obtained by wetting the fabric to 40% moisture prior to pressing on the Hoffman press.
  • Example 14 The fabric of Example I is semi-deca-ted, rolled onto TABLE IX T the perforated spindle of a pack-age dye machine and Description sealed as in Example VIII.
  • the temperature of the fabric is 77 F. when anh drous ammonia as is admitted to G Fabric treated with 6% monoisopropanolamine, padded to 100% h y g o ;i F ,t at ggg sg, g g igt issob quglg i t e machine. After the temperature rises to 105 F.,
  • Temperature is brqught 8 moniagas.
  • the temperature of the fabric is 77 F prror 139 F. lnSlde the fabric and S0218 added. After so, is added, to addition of S0 and 92 F, when S0 admission is distemperature rises to 183 F. Pressure at start 60 mm. d h f h o N Fabrtictrclatedwgth 01%m02r68isoFr3ro 1lzano1amitne,paddoedtofitgo? continue T e temperature 0 t e fabric 18 77 F. and
  • Example II The fabric of Example I is padded to 82.0% Wet pickm ens up with a solution containing 6.0% monoisopropanol- Tongue Elon- Greases amine, ,5.0% eth lene lycol and 0.1% Syn-Fae 905. Treat Percent tear Strength gation ment pH S 2 (gm) (1b.) (percent) Dry Wet After padding, this fabric is dried at 200-225" F. to about C t 1 65 9 47 0 1 1 2 3 10% moisture regain, semi-de'cated at 1.25 minutes steam to 68 5 5 6 0 followed by minutes vacuum pumping.
  • Pre-treated fabric (1869 gins.) is placed in the machine and heated to 150 F.
  • Sulfur dioxide gas is introduced in an amount (51 gms.) sufiicient to titrate the amine in the fabric plus sufficient excess to occupy the void spaces in the fabric and in the machine.
  • This gaseous material is circulated for 15 minutes and then ammonia gas is introduced in amount (7 gms.) sufficient to titrate the excess sulfur dioxide in the system.
  • Ammonia is circulated for minutes, the experimental treatment is stopped, and the fabric is removed from the machine.
  • Pro-treated fabric (1869 gms.) is placed in the machine and heated to 83 F. Sulfur dioxide gas and ammonia are introduced in the same sequence and amounts as in (1). A very slight amount of snow (believed to be ammonium sulfite and/or bisulfite) is noted along the fringes of the fabric.
  • Pre-treated fabric (1823 gms.) is placed in the machine and heated to 135 F.
  • Sulfur dioxide gas is introduced into the system in an amount (41.4 gms.) sufficient to titrate the amine in the fabric plus an amount sufiicient to occupy the void spaces in the fabric.
  • the gases are circulated for minutes and an amount (6.3 gms.) of ammonia gas is introduced sufficient to titrate the excess sulfur dioxide in the system. After an additional circulation time of 10 minutes, the top is removed and the fabric blown with air for 5 minutes.
  • Pre-treated fabric (1908 gms.) is placed in the machine and sulfur dioxide gas is introduced into the system in an amount (43.0 gms.) sufficient to titrate the amine in the fabric and occupy the void spaces in the fabric.
  • sulfur dioxide gas is introduced into the system in an amount (43.0 gms.) sufficient to titrate the amine in the fabric and occupy the void spaces in the fabric.
  • ammonia gas is introduced in an amount (6.6 gms.) sufiicient to titrate the excess sulfur dioxide.
  • the gases are circulated for 5 minutes and the system and fabric blown with air for 5 minutes.
  • Pre-treated fabric (1886 gms.) is placed in the machine and sulfur dioxide gas is introduced into the system in an amount (42.5 gms.) sufficient to titrate the amine in the fabric and occupy the void spaces in the fabric. This gas is circulated for 5 minutes after which ammonia gas is introduced in an amount (6.5 gms.) sufficient to titrate the excess sulfur dioxide.
  • the fabric temperature is about 100 F.
  • the fabric is then heated to 140 F. by means of the electric heating system connected to the machine. After this temperature is reached, the fabric is blown with air for 5 minutes.
  • Pre-treated fabric 1791 gms. is placed in the machine and heated to 134 F.
  • Sulfur dioxide gas is introduced into the system in an amount (40.5 gms.) sufiicient to titrate the amine in the fabric and occupy the void spaces in the fabric.
  • ammonia gas is introduced in an amount (6.2 gms.) sufficient to titrate the excess sulfur dioxide.
  • the system is opened and the fabric blown with air for 5 minutes.
  • Pre-treated fabric (1920 gms.) is placed in the machine and heated to 140 F.
  • Sulfur dioxide gas is introduced in an amount (38.4 gms.) sufficient to titrate the amine in the fabric and occupy the void spaces in the fabric.
  • This gas is circulated for 5 minutes, after which ammonia gas is introduced in an amount (6.4 gms.) sufficient to titrate the excess sulfur dioxide.
  • ammonia gas is introduced in an amount (6.4 gms.) sufficient to titrate the excess sulfur dioxide.
  • Pre-treated fabric (1874 gms.) is placed in the machine and heated to 145 F.
  • Sulfur dioxide gas is introduced in an amount (37.0 gms.) suflicient to titrate the amine in the fabric.
  • the gases are circulated for 5 minutes and ammonia gas is introduced in an amount (14.0 gms.) suflicient to titrate all the sulfur dioxide previously adtional 5 minutes and the system is opened and the fabric blown with air for 5 minutes.
  • Pre-treated fabric (1982 gms.) is placed in the machine and heated to 145 F.
  • Sulfur dioxide gas is introduced in an amount (39.5 gms.) sufficient to titrate the amine in the fabric.
  • ammonia gas is introduced in an amount (10.5 gms.) corresponding to half of the amount necessary to titrate the sulfur dioxide previously admitted to the system. These gases are circulated for 5 minutes and the system opened and blown with air for 5 minutes.
  • Pre-treated fabric (1883 gms.) is placed in the machine and sulfur dioxide gas is introduced in an amount (38.0 gms.) sufiicient to titrate the amine in the fabric. After circulating this gas for 5 minutes, ammania gas is introduced in an amount (3.3 gms.) only sufficient to occupy the void spaces in the fabric. These gases are circulated for 5 minutes, and then the system is opened and blown with air for 5 minutes.
  • Pre-treated fabric (2021 gms.) is placed in the machine and heated to 136 F.
  • Sulfur dioxide gas is admitted to the system in an amount (40.0) gms.) sufficient to react with the amine in the fabric.
  • This gas is circulated for 5 minutes, after which ammonia gas is introduced in an amount (3.6 gms.) sufiicient to occupy the void spaces in the fabric. After 5 minutes additional circulation, the system is opened and the fabric blown with air for 5 minutes.
  • Example I The fabric of Example I is treated with 4.50% monoisopropanolamine, 0.10% Syn-Fae 905 and 7.20% urea, based on the weight of fabric.
  • the fabric is dried at ZOO-225 F. and semi-decated on a Hoffman press at 15 seconds steam followed by 60 seconds vacuum while contained between two pieces of decater fabric.
  • This fabric weighing 1482 grams, is then rolled onto the beam of a laboratory gas treating machine, placed in the machine and heated to 140 F.
  • Ammonia gas (2.6 grams) is added to the system and circulated for six minutes. The excess ammonia is vented to the outside.
  • Sulfur dioxide gas (51.4 grams) is then added to the system and, after complete addition, is circulated for six minutes. The excess sulfur dioxide gas is vented to the outside.
  • Additional ammonia (1.3 grams) is then added to the system and circulated for six minutes. A final venting and exhausting is conducted for 10 minutes. The fabric is removed from the machine and tested.
  • the initial dr crease rating is 3.5. This rating after 7 aging at room conditions for one (1) week, increased mitted to the system.
  • the gases are circulated for an addi- That which is claimed is: 1.
  • a novel process for presensitizing keratin fibers for subsequent durable setting comprising (1) contacting keratin fibers with a reducing agent precursor; (2) subjecting said fibers to any desired mechanical finishing operation; and (3) then exposing said fibers to a gaseous reducing 17 agent activator chemical which can react with the precursor to form a different chemical compound which is a reducing agent for the keratin fibers whereby said fibers are presensitized for subsequent durable setting.
  • a novel process for presensitizing fabrics containing keratin fibers for subsequent durable setting while providing a desirable finish on said fabric comprising (1) impregnating said fabric with a reducing agent precursor;

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
US278359A 1963-05-06 1963-05-06 Wool fibers sensitized for setting by applying thereto one member of a reducing agent-producing coreactant pair,mechanically finishing and applying the second member of said pair Expired - Lifetime US3449061A (en)

Applications Claiming Priority (1)

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US27835963A 1963-05-06 1963-05-06

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US3449061A true US3449061A (en) 1969-06-10

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Country Status (13)

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US (1) US3449061A (xx)
AT (1) AT277928B (xx)
BE (1) BE647531A (xx)
CH (1) CH468508A (xx)
DE (1) DE1469316A1 (xx)
DK (1) DK117950B (xx)
ES (1) ES299113A1 (xx)
FI (1) FI43064C (xx)
FR (1) FR1396016A (xx)
GB (1) GB1059222A (xx)
LU (1) LU46031A1 (xx)
NL (1) NL6405046A (xx)
SE (1) SE310873B (xx)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050144733A1 (en) * 2001-12-18 2005-07-07 Artley John W. Method of making polyethylene glycol treated fabrics
CN104674398A (zh) * 2015-02-13 2015-06-03 浙江高和羊毛科技有限公司 一种毛纺助剂加料装置
WO2017020018A1 (en) * 2015-07-30 2017-02-02 Selwyn Gary S Hyperbaric process for applying and curing an organic polymerizable treatment

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB493098A (en) * 1937-03-30 1938-09-30 Wool Ind Res Association Improvements in or relating to the gaseous treatment in vacuo of wool and like fibres or materials made therefrom
US2351718A (en) * 1935-12-09 1944-06-20 Speakman John Bamber Treatment of fibers or fibrous materials containing keratin
US2508713A (en) * 1946-10-07 1950-05-23 Harris Res Lab Treatment of keratinous material
GB775486A (en) * 1954-05-21 1957-05-22 Marks Spencer Ltd Improvements in or relating to the permanent setting of fabrics containing or consisting of keratin fibres
US2806762A (en) * 1951-10-24 1957-09-17 Armour & Co Method of chemically curling animal hair with sulfur dioxide in aqueous solution
GB839516A (en) * 1957-07-02 1960-06-29 Commw Scient Ind Res Org A process for the durable creasing or other permanent setting of woollen or worsted fabrics or other materials containing wool or other keratin fibres
US3051544A (en) * 1959-02-12 1962-08-28 Stevens & Co Inc J P Lustered wool product and method of making the same
US3059990A (en) * 1959-11-03 1962-10-23 Nathan H Koenig Method of setting wool textiles with ethanolamine
US3077655A (en) * 1961-05-09 1963-02-19 Stevens & Co Inc J P Method and apparatus for imparting stretch to wool fabric
US3098694A (en) * 1960-07-11 1963-07-23 Drew Chem Corp Continuous treatment of wool to shrinkproof and sensitize the same

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2351718A (en) * 1935-12-09 1944-06-20 Speakman John Bamber Treatment of fibers or fibrous materials containing keratin
GB493098A (en) * 1937-03-30 1938-09-30 Wool Ind Res Association Improvements in or relating to the gaseous treatment in vacuo of wool and like fibres or materials made therefrom
US2508713A (en) * 1946-10-07 1950-05-23 Harris Res Lab Treatment of keratinous material
US2806762A (en) * 1951-10-24 1957-09-17 Armour & Co Method of chemically curling animal hair with sulfur dioxide in aqueous solution
GB775486A (en) * 1954-05-21 1957-05-22 Marks Spencer Ltd Improvements in or relating to the permanent setting of fabrics containing or consisting of keratin fibres
GB839516A (en) * 1957-07-02 1960-06-29 Commw Scient Ind Res Org A process for the durable creasing or other permanent setting of woollen or worsted fabrics or other materials containing wool or other keratin fibres
US3051544A (en) * 1959-02-12 1962-08-28 Stevens & Co Inc J P Lustered wool product and method of making the same
US3059990A (en) * 1959-11-03 1962-10-23 Nathan H Koenig Method of setting wool textiles with ethanolamine
US3098694A (en) * 1960-07-11 1963-07-23 Drew Chem Corp Continuous treatment of wool to shrinkproof and sensitize the same
US3077655A (en) * 1961-05-09 1963-02-19 Stevens & Co Inc J P Method and apparatus for imparting stretch to wool fabric

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050144733A1 (en) * 2001-12-18 2005-07-07 Artley John W. Method of making polyethylene glycol treated fabrics
US7585330B2 (en) * 2001-12-18 2009-09-08 John W Artley Method of making polyethylene glycol treated fabrics
CN104674398A (zh) * 2015-02-13 2015-06-03 浙江高和羊毛科技有限公司 一种毛纺助剂加料装置
WO2017020018A1 (en) * 2015-07-30 2017-02-02 Selwyn Gary S Hyperbaric process for applying and curing an organic polymerizable treatment
US9902874B2 (en) * 2015-07-30 2018-02-27 Gary S. Selwyn Hyperbaric process for applying and curing an organic polymerizable treatment
CN107849802A (zh) * 2015-07-30 2018-03-27 加里·S·塞尔温 用于施用和固化有机可聚合处理的高压方法
KR20180034578A (ko) * 2015-07-30 2018-04-04 개리 에스. 셀윈 유기 중합 가능한 처리제를 도포하고 경화시키기 위한 고압 프로세스
JP2018528077A (ja) * 2015-07-30 2018-09-27 ゲイリー エス． セルウィンＧａｒｙ Ｓ． ＳＥＬＷＹＮ 有機重合性処理剤を塗布および硬化する高圧プロセス
CN107849802B (zh) * 2015-07-30 2020-12-08 加里·S·塞尔温 用于施用和固化有机可聚合处理的高压方法

Also Published As

Publication number Publication date
CH593064A4 (xx) 1968-09-30
CH468508A (fr) 1969-03-31
ES299113A1 (es) 1964-12-01
DK117950B (da) 1970-06-22
FR1396016A (fr) 1965-04-16
SE310873B (xx) 1969-05-19
LU46031A1 (xx) 1972-01-01
FI43064B (xx) 1970-10-01
DE1469316A1 (de) 1969-04-24
FI43064C (fi) 1971-01-11
AT277928B (de) 1970-01-12
BE647531A (xx) 1964-08-31
GB1059222A (en) 1967-02-15
NL6405046A (xx) 1964-11-09

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