Classifications

• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06Q—DECORATING TEXTILES
  • D06Q1/00—Decorating textiles
• • 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
  • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
  • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
  • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
  • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
• • 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
  • D06M13/12—Aldehydes; Ketones
• • 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
  • D06M13/12—Aldehydes; Ketones
  • D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
• • 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
  • D06M13/144—Alcohols; Metal alcoholates
• • 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
  • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
• • 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
  • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
  • D06M15/423—Amino-aldehyde resins
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
  • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
  • B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
• • 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
  • Y10S8/17—Glyoxal and polyaldehyde treatment of textiles

Definitions

• the invention is particularly concerned with processes for the enhancement of certain properties-notably the wet resilience or wash and wear properties of the fabric.
• the improved process involves certain special operational techniques which are to be used as pretreatments in conjunction with conventional resinating processes and which permit enhancement of the influence of the resin on the fabric properties.
• a given degree of stabilization can be obtained with less resin when the fabrics have been given the special preparatory treatment than can be obtained if the pretreatment has not been employed; or, stated in another way, the pretreatment will enhance the resination effects produced by a given quantity of resin.
• the special pretreatment conditions the fabric and makes it more receptive to the resin. This is accomplished by modifying the celluloseespecially the crystal lite phase and thereby enables obtaining a more uniform dispersion of the resin in the cellulose complex.
• the modification tends to affect the crystallite phase and impart to it some of the characteristics of the amorphous phases. As a result of this treatment, it is possible for the relatively large resin particles to penetrate into and exert their influence on areas which, in the absence of the pretreatment, they could not effectively reach.
• the resination process involves the steps of applying a resinous material to the fabric, usually in the form of an aqueous solution of a water soluble heathardenable resin precondensate, drying the fabric, and then heating the fabric in the presence of a curing catalyst to fix the resin in the fabric.
• resinous material is intended to mean not only the thermosetting type impregnants but also those impregnants which react with the cellulose or other impregnants to form a water insoluble complex.
• the fabric can, if desired, be subjected to mechanical treatments which tend to change the form and relative disposition of the fabric fibers, e.g. calendering, pleating, compressive shrinking, and the like; and if the fabric is cured while maintained in the deformed condition, the
• the preferred type of resinous material is one which is not discolored by halogen (e.g. the chlorine frequently used in bleaches).
• halogen e.g. the chlorine frequently used in bleaches.
• Many of the textile finishing resins will,to some extent, pick-up and retain chlorine in commercial laundering operation s. Therefore, it is also preferred to employ resins which either do not pickup chlorine, or if theydo pick-up chlorine, which will not readily release the chlorine during subsequent ironing, in quantities or at rates which will objectionably degrade the cellulose.
• especially suitable resins for treating white goods include the cyclic ureasespecially triaZone precondensates; ketone aldehydes, and the like. It is also customary to tintwhite goods. Where tinting agents are to be applied in the process of. the present invention, it is preferred that they be applied to the goods intermediate the decrystallization and resination operation.
• the pretreatments are of such a nature that beneficial results are obtained only in the processing of natural cellulose. Regenerated celluloses and esterified celluloses cannot be effectively treated by these special techniques.
• the pretreatment techniques which are especially useful in conjunction with resination processes utilize certain physico-chemical and chemical techniques (either singly or in combination) which permit a portion of the dense, highly oriented cellulose crystallites to be modified opened up or spread apart (hereinafter this phenomenon will sometimes be referred to as decrystallization) so as to impart to the crystallite some of the characteristics of the disoriented amorphous phase-particularly the ability to recover from a deformed state on passing from the
• decrystallization physico-chemical and chemical techniques which permit a portion of the dense, highly oriented cellulose crystallites to be modified opened up or spread apart
• these special techniques are treatments which affect the cellulose crystallites and bring about physical and/or chemical modification of the crystallite phase in a way that enhances the wet resilience of the fabric without exerting any commercially significant adverse influence on the strength, sewability and other characteristics.
• the special treatment techniques also tend to enhance certain other fabric characteristics such as the hand, dye and resin receptivity, drapability, etc.
• an average of at least one methylene crosslink should be introduced for every 10 to 200 glucose residues (i.e. equivalent to reacting a quantity of formaldehyde equal to about 2 to 0.1% of the fabric weight and giving an add on of from 0.8 to 0.4% of the fabric weight) in the cellulose complex. If the average number of crosslinks formed is less than 1 to 200 the crystallite phase Will not be affected sufiiciently to significantly enhance the wash and wear or fiat drying properties. Whereas, if the average number of crosslinks is greater than 1 to 10 the fabric will be tendered appreciably and it will not have the strength necessary to undergo machine laundering and drying.
• R represents hydrogen atoms, alkyl or substi tuted alkyl chains of no more than about carbons, or simple cyclic substituents as would be introduced into the cellulose by reacting it with aldehydes and dialdehydes such as formaldehyde, glyoxal, acetaldehyde, chloral, benazaldehyde, furfural, and the like.
• aldehydes and dialdehydes such as formaldehyde, glyoxal, acetaldehyde, chloral, benazaldehyde, furfural, and the like.
• the preferred methylenating agent is formaldehyde since it can be effectively carried in aqueous solution, and since it will not cause an appreciable weight change in the fabric.
• the simple methylene crosslinks are highly stable and do not adversely interfere withfinishing adjuncts which may sometimes be employed in subsequent processing of the fabric.
• aldehydes and dialdehydes can be employed as methylenating agents.
• the preferred agents are those which are small enough to enable them to penetrate into the crystallite phase.
• the aldehydes and dialdehydes '(either straight chain or cyclic) and which contain up to 6 carbons in general have the characteristic of being able to penetrate the crystallite phase and are reactable with cellulose to form methylene and substituted methylene crosslinks.
• the desired degree of crosslinking can be obtained by applying the formaldehyde in quantities which, before curing, deposit from /2% to 5% formaldehyde (based on fabric weight) in the fabric.
• the formaldehyde can be applied in Various ways I prefer to apply it by impregnating the fabric with aqueous solutions which contain formaldehyde.
• the impregnating bath can also contain other substances such as the catalyst, tinting agents, wetting agents, softeners, buffers, etc. which are compatible with one another.
• Buifers which are especially useful in connection with the methylenation of cellulose fabrics are those materials which can react with the formaldehyde or other aldehydes at low temperatures to form compounds or complexes which will release the aldehyde under the curing conditions employed to effect the methylenation.
• a preferred class of buffering compounds are the alcohols and similar organic hydroXy compounds. Of the alcohols I prefer to employ isopropyl alcohol. This preference is due to the fact that it is somewhat less volatile than the lower alcohols, therefore minimizing fire hazards, and because it can be driven off readily in the subsequent processing.
• catalyst systemone component being an acid and the other component being an acid salt of the Lewis acid type.
• Suitable acids for the purposes of this invention include organic and inorganic acids and acid anhydrides such as maleic, tartaric, hydrochloric, phosphoric, citric, itaconic, succinic, and the like.
• organic and inorganic acids and acid anhydrides such as maleic, tartaric, hydrochloric, phosphoric, citric, itaconic, succinic, and the like.
• polybasic acids since catalyst combinations prepared therefrom develop the desired degree of acidity for efiicient methylenation control and will not objectionably degrade the fabric.
• the preferred acid salts for use in the catalyst system of this invention are the metal salts of either organic or inorganic acids of the Lewis acid type (i.e. electron acceptors); and especially the polyvalent metal salts of such acids and the acid salts of monovalent metals with polybasic acids. Where white goods are being processed, I also prefer to employ those salts whoseaqueous solutions are substantially colorless.
• especially useful acid salts include'aluminum chloride, strontium nitrate, tin chloride, aluminum acetate, magnesium nitrate, zirconium oxychloride, zinc nitrate, sodium bisulfate, and the like.
• One or more of these salts can be used in combination with the preferred acids.
• Catalyst systems which have been found to be especially effective in insuring that the desired degree of methylenation will be obtained without seriously degrading the cellulose are those which have the acidity characteristics below 200 P. which will not appreciably catalyze the methylenation reaction and which develop an acid methylenating environment at temperatures between 200 and 275 F.
• the total catalyst system is approximately 1% of the weight of the bath and is sometimes hereinafter referred to as the 2-3-4 catalyst), have been found to be especially useful.
• the ratios and the total catalyst concentration can be varied widely provided the resulting system has the desired acidity characteristics as aforesaid.
• the catalyst can be applied in multistep operations and in any desired sequence, as is well known in the art.
• the methylenating agent When the methylenating agent is applied from an aqueous solution, it is preferred to dry the fabric before instituting the 'cure as this will insure greater uniformity of the end product.
• the drying can be carried out on conventional drying equipment. However when this step is employed, it is important that the fabric should not be permitted to drop below the point of the moisture regain under the humidity conditions then prevailing in the mill. If the fabric is overdried, reproducible results cannot be obtained.
• the curing operation involves heating the fabric for times and temperatures which insure that the desired degree of methylenation is obtained but in no case should it be carried to a point where the cellulose is objectionably degraded.
• the catalyst having the acidity characteristics approximating the 2-3-4 catalyst effective curing can be obtained by 5 minute cures at 235 F. on
• the fabric After curing the fabric can be Washed and dried to insure removal of the unreacted irnpregnants.
• the wet resilience can be further enhanced by also treating the fabric with strong caustic soda solutions which are also capable of exerting a decrystallizing effect on the PHYSICO-CHEMICAL DECRYSTALLIZATIQN
• the technique employed to obtain the desired enhancement. of resin receptivity and wet resilience can be described generally as a modified mercerizing treatment-in which the casutic soda solutions are considerably stronger than those conventionally used in the mercerization of cotton.
• caustic soda solutions of from 32 to 45 Tw are generally used. I cannot ob tain the desired effect by using caustic solutions of less than about 45 TW and best results are obtained with caustic solutions stronger than 60 TW.
• the swelling is also accompanied by an appreciable deconvolution of the fiber hairs and this in turn exerts an undesirable infiuence on the hand.
• the stronger caustic solutions Which I specify, swelling precedes the deconvolution or untwisting of the fiber hairs.
• I can convert a portion of the crystallitesto an amorphous condition without drastically modifying the hand.
• the arresting is effected by Washing the alkali out of the fabric with Water and dilute acidic solutions. Preferably Washing should commence within about 20-30 seconds after impregnation and the alkali should be substantially completely removed within about 60 seconds.
• EXAMPLE 1 A white cotton bleached (80 x 80 running 3.50 yds./lb.) which had not been previously mercerized was impregnated and squeezed at 60% pick-up in the follow- Triton X-100 (wetting agent, iso octyl phenyl polyethoxyethanol) u Water to make 100 gal.
• Triton X-100 wetting agent, iso octyl phenyl polyethoxyethanol
• the impregnated fabric was frame dried to the desired width. The drying was carried out to a point where the moisture content of the fabric was not permitted to fall below the moisture regain percentage under the prevailing humidity conditions.
• the dried fabric was cured for minutw at 250 F.
• the cured fabric was then washed and dried.
• Example 1 The fabric produced in Example 1 was passed through a caustic mangle containing 66 Tw caustic soda solution at room temperature and passed onto a frame moving at 60 yards per minute, water Washing to remove the caustic soda was commenced within about -17 seconds after the fabric had left the mangle.
• the fabric was sour washed with A2 to 1% H 80 chemic washed (0.25% available C1 and dried to the desired width. The fabric was substantially completely neutralized within about 1 minute after leaving the mangle.
• Example 2 was repeated using the same untreated fabric as was used in Example 1.
• Example 1 0.56% formaldehyde (giving a total dry add on of approximately 0.2% as compared with weight of the untreated fabric) was reacted with the cellulose. This prepresents an average of one methylene crosslink for every 33 glucose residues. The methylenation was determined according to the method of Kress (page 33, American Dyestuff Reporter, February 23, 1959). The wet and dry strength losses were well within acceptable commercial tolerances for this type of fabric and were approximately less than those obtained by resination of the same fabric to the degree necessary to obtain a comparable level of wash and wear properties. The treatment provides a fabric having a pleasing hand and the wash and wear properties were good. The resilience and stabilization were comparable to those obtained by resination.
• Example 2 the wash and Wear properties and the strength values were still further enhanced over those obtained in Example 1.
• the resultant fabric had a pleasing full bodied hand.
• Example 3 the treatment imparted some Wash and Wear properties, a full hand and the strength losses (wet and dry) were approximately 50% less than those obtained-by resination of the same fabric to the degree necessary to obtain comparable wash and wear properties.
• Example 4 The fabric produced according to Example 4 was very similar in hand to that obtained in Example 2 but with a slightly lower strength. The resilience, stabilization and wash and wear properties were increased over those ob-' tained in Example 2;
• the fabric was treated as in Example 1 except that the cure was for 2 minutes at 275 F.
• Example 5 0.095% formaldehyde (giving a total dry add on of 0.05% as compared with the weight of the untreated fabric) was reacted with the cellulose. This represents an average of one methylene vcrosslink for every 195 glucose residues.
• the wet and dry strength losses were approximately 35% less than those obtained by resination of the same fabric to the degree necessaryto obtain a comparable level of wash and wear properties.
• the durability was good but the resilience was slightly reduced from that obtained in Example 1.
• the finished fabric had a pleasing supple hand.
• the fabric was dried and cured at 300 F. for 3 minutes and thereafter washed and dried.
• EXA'MPLE 7 The fabric treated as in Example 2 was further treated according to the process in Example 6.
• the method of finishing partially methylenated natural cellulose fabrics containing an average of one methylene crosslink for every to 200 glucose residues which comprises contacting the fabric With strong caustic soda solutions of at least 45 T w for a time sufficient to cause decrystallization of cellulose crystallites, removing the caustic before appreciable fiber deconvolution occurs, impregnating the decrystallized cellulose with a textile finishing resin and thereafter fixing the resin in the fabric.
• Goldthwait Amer. Dyestufi Reporter, Sept. 19, 1949, p. 678.

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)

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• 0
  • NL NL243632D patent/NL243632A/xx unknown
  • NL NL247426D patent/NL247426A/xx unknown
• 1959
  • 1959-04-17 US US804858A patent/US3139322A/en not_active Expired - Lifetime
  • 1959-09-16 US US838823A patent/US3186954A/en not_active Expired - Lifetime
  • 1959-09-22 GB GB32207/59A patent/GB936993A/en not_active Expired
  • 1959-09-23 FR FR805839A patent/FR1236421A/fr not_active Expired
  • 1959-09-24 CH CH7860059A patent/CH369103A/fr unknown
• 1960
  • 1960-01-06 GB GB459/60A patent/GB945040A/en not_active Expired

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