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
  • 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
  • D06M13/10—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 oxygen
  • D06M13/11—Compounds containing epoxy groups or precursors thereof
• • 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
  • Y10S8/08—Oxirane

Definitions

• This invention relates to the treatment of fibrous materials. More particularly, the invention relates to an improved process for treating cellulosic fibrous materials to impart dimensional stability, and to the improved products obtained thereby.
• the invention provides a new and highly efiicient process for treating cellulosic fibrous materials, and particularly cellulosic textile materials as cotton fibers and fabrics, with an epihalohydrin or material which liberates epihalohydrin to form products having excellent wet crease recovery without undue loss of strength.
• This process comprises impregnating the desired fibrous material with a caustic solution and exposing the impregnated material to hot vapors composed of water and an epihalohydrin or material which liberates an epihalohydrin, for a short period, e.g., less than minutes, and then washing the treated material.
• the invention further provides fibrous materials having improved properties which are prepared by the above-described new process.
• Nitrogenous resins have been applied to cellulosic textile materials to produce wash-and-wear fabrics. These resins, however, lack the ability to produce an acceptable wet crease recovery. Thus, the conventional thermosetaing resins impart a satisfactory appearance to fabrics which are tumble dried, but fail to eliminate Wrinkles when the fabrics are drip or line dried.
• an object of the invention to provide a new process for treating fibrous materials. It is a further object to provide a new process for treating cellulosic textile materials to impart a high wet crease recovery. It is a further object to provide a new process for imparting high wet crease recovery that can be operated on a continuous manner and will give products having uniform properties. It is a further object to provide an improved, short cure cycle process for treating textile materials with an epihalohydrin. It is a further object to provide a process for treating textile materials with an epihalohydrin which imparts high crease recovery without undue loss of strength. It is a further object to provide a process for textile treatment which gives products having good dyeability.
• the process of the invention which comprises impregnating the desired fibrous material with a caustic solution and exposing the impregnated material to hot vapors composed of a mixture of water and an epihalohydrin or material which liberates an epihalohydrin, for a short period, say less than 5 minutes, and then washing the treated material. It has been found that this new process avoids all of the above-noted difiiculties and provides a highly efficient method for obtaining fibrous materials having improved dimensional stability, particularly when wet.
• the textile materials obtained by this process for example, have a high de gree of wet crease recovery which is obtainable even with the use of less epihalohydrin than the previous processes.
• the resulting products retain a greater part of the strength than heretofore and possess improved dyeability.
• the process is operable in a continuous manner and employs very short cure cycles. Particular advantage is found in the fact that the new process gives more favorable conditions for reaction and makes for easier process control. There is, for example, no problem as .to control of water content nor danger from the epichlorohydrin vapors as in the prior known liquid process.
• the compounds to be used in the treatment of the textile material include the epihalohydrins and the material which liberate epihalohydrins when in an alkaline medium.
• the epihalohydrins which are halo-substituted monoepoxy compounds, may be exemplified by epichlorohydrin, epibr-omohydrin, 2,3-epoxy-2-methyl-l-chloropropane, 2,3-epoxy l-chlorobutane, 2,3-epoxy-l-bromobutane, 2,3-epoxy-l-chloropentane and the like.
• the materials which liberate epihalohydrins when in an alkaline medium include the dihalohydrins as 1,3-dichloro-2-hydroxypropane, 1,3-dibromo-Z-hydroxypropane, l,3-dichloro-Z-hydroxybutane, 1,3-dichloro-Z-hydroxypentane, 2-methyl- 1 ,3-dichlo-ro-2- hydroxypropane and the like, and mixtures thereof.
• Epichlorohydrin is particularly preferred.
• the material to 'be treated is brought into contact with aqueous caustic solution.
• the causti employed is preferably sodium hydroxide but potassium hydroxide or other alkali or alkali earth metal hydroxides may be utilized.
• the strength of the caustic solution may vary but preferred concentrations vary from about 1% to 25% by weight. Within this range, the crease recovery is roughly proportional to the caustic concentration. While the higher concentrations tend to give higher wet crease recovery in a shorter cure period, in some cases they tend to have a more deleterious effect on the strength of the heated fabric. Accordingly, the more preferred concentrations generally range from about 5% to by weight.
• the impregnation with the aqueous caustic may be accomplished by any suitable means, such as, for example, by dipping, spraying, padding and the like. It is generally preferred to pass the textile material into and through the aqueous solution as by padding.
• the amount of wet pick-up will vary with the different cases, but generaly it is preferred to have a wet pick-up varying from about 40% to 100% by weight based on dry fabric. Varying pick-up has little effect on crease recovery. Increasing pick-up of, say, a 10% NaOH solution from 40% to 100% results in gain of about in the crease recovery.
• the temperature of the caustic solution as well as the temperature of the textile material to be impregnated may vary, but in general it is preferred to have both at elevated temperature. The efiiciency of the process is thereby improved at higher temperatures.
• wetting agents in the caustic solution to assist in speeding the cure.
• These agents may be any of the known cationic, anionic or non-ionic materials and may have a great variety of different compositions.
• Preferred materials include the ionic agents and especially those having a polar structure including a hydrophobic residue and charged ionic radical thereon, such as anionic surface active compounds include alkali metal and nitrogen-base soaps of higher fatty acids, such as potassium and sodium myristate, laurate, palmitate, oleate, stearate, ammonium stearate, etc., as well as the surface-active compounds of the cation-active variety, such as salts of long-chain aliphatic amines and quaternary ammonium bases, such as lauryl amine hydrochloride, stearyl amine hydrochloride, and the like.
• non-ionic agents examples include the partial esters of polyhydric alcohols and fatty acids, such as the hexitans and hexitide esters as sorbitan monolaurate, hydroxypolyoxyalkylene ethers of the above-described partial esters as the polyethylene glycol ethers of sorbitan monolaurate, the hydroxypolyoxyalkylene ethers of phenols as the reaction product of ethylene oxide and .bis-phenol-A and the like and mixtures thereof. These materials are preferably employed in amounts varying from about .l% to by weight, and still more preferably from 1% to 5% by Weight.
• the hot vapors comprising a mixture of water and an epihalohydrin or material which liberates an epihalohydrin.
• the mixture should contain at least 10% by weight of Water, and preferably 10% to 80% by weight of water and 90% to 20% by weight of epihalohydrin or material which liberates epihalohydrin.
• the hot vapor preferably contains at least and preferably 80% by weight of the epihalohydrin or material which liberates epihalohydrins component, and still more preferably is a mixture which exists at a temperature between 180 F. and 250 F.
• the preferred vapor mixture of water and epichlorohydrin is the constant boiling vapor composition at 190 F. at 760 mm. and has a composition of about 76% by Weight of epiohlorohydrin and 24% by weight of water.
• this vapor can be generated by boiling a liquid mixture containing 10 to weight epichlorohydrin.
• the length of time for exposing the impregnated fibrous material to the hot vapors will vary depnding on the degree of crease recovery desired and the specific mechanical construction of the said material. Generally, crease recovery increases with time up to about 2 or 3 minutes. After that .it tends to level off. The period of exposure in all cases will not be more than a few minutes, and preferably between 15 seconds to about 5 minutes. Using water-epichlorohydrin vapors and caustic solutions of concentration of 1% to 25% preferred reaction times vary from about 30 seconds to 3 minutes.
• the impregnated fibrous material may be hung or suspended in the presence of or continuously passed through vapors obtained by refluxing the water-epihalohydrin (or material liberating epihalohydrin) mixture.
• the impregnated material may be hung in the presence of or continuously passed through a stream of hot vapors formed by passing live steam into boiling epihalohydrin and the steam used as a carrier for the epihalohydrin or material liberating the epihalohydrins.
• the impregnated material After the impregnated material is removed from the curing zone, it may then be washed to remove any excess epihalohydrin or other material, dried and then used immediately in the intended commercial applications. Washing is preferably accomplished by use of water or Water and detergents and then drying at temperatures ranging from about 20 C. to 125 C.
• the textile material obtained by the above-described process will have the same appearance and feel as before the treatment but will demonstrate excellent wet crease recovery and improved hand.
• the material will also have satisfactory strength and non-chlorine retention properties.
• the products treated as above may then be utilized for any of the intended applications.
• the textile materials may be 'used in the manufacture of dresses, drapes, upholsteries, shoe fabrics, carpets, coats, shirts, uniforms, shoes, towels, cords, construction fabrics and the like.
• the use will, in many cases, determine the amount of the epihalohydrin or material liberating the epihalohydrin to be applied to the textile material.
• the paper treated by the process of the invention may be used in the preparation of improved wrapping materials, containers, cards and the like.
• the wood products may be used in conventional structural applications and the like.
• the above-described process may be utilized for the treatment of any cellulosic fibrous material.
• This includes paper, wood and textile materials.
• the textile materials may be woven and non-woven fabrics, threads, gauze, yarn, cord, string, netting, and the like.
• the material may also be pretreated, e.g., mercerized, dyed and resin-treated.
• cellulosic material which has a part, and preferablyat least 40% derived from cellulosic materials, such as natural cellulose such as cotton, linen, and the like, and other as viscous, cuprammonium rayon, and other regenerated cellulose, as well as mixtures of any of the foregoing as well as mixtures with wool, synthetics as fibers derived from acrylonitrile (Odom-% acrylonitrile polymer), vinylidene cyanide polymers, polyamides (nylon-super polyamides), polyester-polyamides, polymers prepared from corn protein and formaldehyde, as well as copolymers of the above monomers as, for example, Acrilan (85% acrylonitrile and 15% vinyl acetate), Dynel (60% vinyl chloride and 40% acrylonitrile), Saran (85% vinylidene chloride and 15% vinyl chloride), and other synthetic fabrics or fibers prepared from polyalkylenes as polyethylene, polypropylenes, polyurethanes, mineral fibers
• the preferred materials to be employed in the process include those textile materials containing at least 30% cellulosic materials and preferably those derived from cotton and rayon.
• the wrinkle recovery values reported in the examples were determined by the Tentative Method of Test for Recovery of Textile Fabrics From Creasing, Using the Verticle Strip Apparatus, ASTM Designation D1295- 53T (reported as sum of average warp and fill measurements), and textile strength values were determined by Federal Specification CCC-T-l916, Instron Tensile Testing Machine Method 5100. ,All tests were carried out at 6S: ;2% relative humidity and 70: :2 F.
• the wet crease recovery values were determined by soaking the fabric in water for 5 minutes and then blotting before testing.
• Example I This example illustrates the superior results obtained by using the process of the invention for treating cotton print fabric.
• Bleached 80 x 80 count cotton print cloth was impregnated with an aqueous solution of 10% NaOH at a wet pick-up of 100% (based on weight of dry fabric) using a Morrison Laboratory 3-roll padder.
• the impregnated fabric is introduced continuously into a chamber containing hot (190-192 F.) vapors of an epichlor'ohydrin-water azeotrope composed of about 76% epi and 24% by weight of water.
• the fabric is passed over a series of rollers through the hot vapor as to permit a contact time of one minute.
• the fabric is then rinsed in hot running tap water and hung at room temperature to dry.
• the finished fabric had an excellent white hue and excellent drip drying properties.
• the tensile strength (filling direction) of the treated fabric was 29 pounds as compared to 43 pounds for the untreated control While the Elmendorf tear strength was 320 grams and 448 grams, respectively.
• the treated fabric gave a wet crease recovery angle of 291 (warp+ fill).
• the untreated control had a wet crease recovery angle of 143 C.
• Example II Example II was repeated using 10% by weight NaOH, 100% wet pick up, 1 minute reaction time but the temperature of the caustic pad bath was modified as shown in the table. The wet crease recovery values and tensile strength values are shown in the table.
• Example IV Percent Wet Crease Reaction Time (min) Add-On Recovery Angle
• Example IV Example I was repeated with the exception that the fabric was impregnated at ambient temperature with a 7.5% NaOH solution. The cure time was also varied as shown in the table below.
• Example V.Example I was repeated with the exception that the fabric was impregnated at ambient temperature with a 5.0% NaOH solution. The cure time was also varied as shown in the table below.
• Example VII .-Example I was repeated with the exception that the impregnated cotton fabric was suspended in a heated chamber and the hot w'ater-epichlorohydrin azeotrope vapors were swept into the chamber and in contact with the suspended impregnated fabric. Related results are obtained.
• Example IX This example illustrates the use of the process of the invention for treating rayon fabric.
• Rayon fabric was impregnated with an aqueous solution of 5% by weight NaOH at a wet pick-up of about 80% using a Morrison Laboratory 3-roll padder. Samples of the rayon fabric were suspended in a reaction chamber containing hot vapors of water-epichlorohydrin ezeotrope for a period of about two minutes. Vapor temperature was about F. The fabric was then rinsed in hot water and hung at room temperature to dry. The resulting fabric had excellent drip drying properties.
• Example X is repeated using a fabric which Related results are obtained.
• Example XI.Example I is repeated using a fabric which was a blend of 70% cotton and 20% wool. Related results are obtained.
• Example XlI.Example I was repeated using waterepichlorohydrin azeotrope vapor at 200 F. and a one minute cure cycle. Related results are obtained.
• Example XIII.Example I was repeated using a concentration of aqueous NaOH of 2.5%. Related results are obtained.
• Example XI V.-Example VII is repeated with the exception that the hot water epichlorohydrin vapors are replaced with hot vapors of a mixture of water and glycerol dichlorohydrin. Related results are obtained.
• Example X V.Example I is repeated with the exception that the impregnated cotton fabric is passed into a chamber containing hot vapors of a mixture of 50% water and 50% epichlorohydrin. Related results are obtained.
• Example X VII.-Example VII is repeated with the exception that unbleached kraft paper is employed in place of the cotton fabric. Paper having improved dimensional stability is obtained.
• Example X VIII.Example VII is repeated with the exception that strips of pine wood are employed in place of the cotton fabric. Wood products having improved dimensional stability are obtained.
• a process for treating cellulosic fibrous materials to impart dimensional stability thereto which comprises impregnating the fibrous material with a 1% to 25% aqueous caustic solution and exposing for a period of from about seconds to 3 minutes the resulting wet impregnated material to hot vapors of a mixture of water and a member of the group consisting of epihalohydrins and materials which liberate epihalohydrins in an alkaline medium, said mixture containing at least 10% by weight of water,
• a process as in claim 1 wherein the material employed in the form of hot vapors is a mixture of water and glycerol dichlorohydrin.
• a process for treating cellulosic, textile materials containing at least 40% by weight of a cellulosic material to improve the drip dry properties comprises impregnating the material with a 1% to 25% by weight aqueous NaOH solution and a 40% to wet pickup and then exposing the impregnated material to vapors of a water-epichlorohydrin azeotrope for a period of 15 seconds to five minutes, removing the treatment material, washing and drying.
• a process as in claim 8 wherein the textile material is rayon.

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)

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  • BE BE622324D patent/BE622324A/xx unknown
  • NL NL283032D patent/NL283032A/xx unknown
• 1961
  • 1961-09-11 US US137024A patent/US3271101A/en not_active Expired - Lifetime
  • 1961-09-11 US US137025A patent/US3234043A/en not_active Expired - Lifetime
• 1962
  • 1962-09-10 DE DES81388A patent/DE1184729B/de active Pending
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