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
  • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
  • D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts thereof
• • 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
• • D—TEXTILES; PAPER
  • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
  • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
  • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
• • 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
  • D06M13/322—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 nitrogen
  • D06M13/402—Amides imides, sulfamic acids
  • D06M13/425—Carbamic or thiocarbamic acids or derivatives thereof, e.g. urethanes
• • 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
  • D06M13/322—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 nitrogen
  • D06M13/402—Amides imides, sulfamic acids
  • D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides

Definitions

• This invention is concerned with methods of reducing the degree of fibrillation and fibrillation tendency of fabric made from solvent-spun cellulose fibre, also known as lyocell fibre.
• cellulose fibre can be made by extrusion of a solution of cellulose in ⁇ suitable solvent into a coagulating bath. This process of extrusion and coagulation is referred to as "solvent-spinning", and the cellulose fibre produced thereby is referred to as "solvent-spun” cellulose fibre.
• solvent-spinning the process of extrusion and coagulation
• solvent-spun the cellulose fibre produced thereby is referred to as "solvent-spun” cellulose fibre.
• a solvent such as a tertiary amine N-oxide, for example N-methylmorpholine N- oxide.
• the resulting solution is exi ided through a suitable die to produce filaments, which ard.
• cellulose fibre can be made by extrusion of a solution of a cellulose derivative into a regenerating and coagulating bath.
• a viscose process in which the cellulose derivative is cellulose xanthate. Both such types of process are examples of wet-spinning processes. Solvent-spinning has a number of advantages over other known processes for the manufacture of cellulose fibre such as the viscose process, for example reduced environmental emissions.
• lyocell fibre means a cellulose fibre obtained by an organic solvent-spinning process, in which the organic solvent essentially comprises a mixture of organic chemicals and water, and in which solvent-spinning involves dissolving cellulose and spinning without formation of a derivative of the cellulose.
• solvent-spun cellulose fibre and “lyocell fibre” are synonymous.
• lyocell fabric means a fabric woven or knitted from a plurality of yarns, at least some of which yarns contain lyocell fibre, alone or in blend with other type(s) of fibre.
• Fibre may exhibit a tendency to fibrillate, particularly when subjected to mechanical stress in the wet state. Fibrillation occurs when fibre structure breaks down in the longitudinal direction so that fine fibrils become partially detached from the fibre, giving a hairy appearance to the fibre and to fabric containing it, for example woven or knitted fabric. Dyed fabric containing fibrillated fibre tends to have a "frosted" appearance, which may be aesthetically undesirable. Such fibrillation is believed to be caused by mechanical abrasion of the fibres during treatment in a wet and swollen state. Wet treatment processes such as scouring, bleaching, dyeing and washing inevitably subject fibres to mechanical abrasion. Higher temperatures and longer times of treatment generally tend to produce greater degrees of fibrillation. Lyocell fabric appears to be particularly sensitive to such abrasion and is consequently often found to be more susceptible to fibrillation than fabric made from other types of cellulose fibre. In particular, cotton fabrics have an inherently very low fibrillation tendency.
• EP-A-538,977 discloses that fibrils can be removed from fibrillated woven lyocell fabric by treatment with a solution of a cellulase.
• Cellulases are enzymes which catalyse the hydrolysis of cellulose.
• such treatment is not as effective as could be desired, and disposal of used solutions of the enzyme may pose environmental problems.
• Crosslinking agents may sometimes be referred to under other names, for example crosslinking resins, chemical finishing agents and resin finishing agents.
• Crosslinking agents are small molecules containing a plurality of functional groups capable of reacting with the hydroxyl groups in cellulose to form crosslinks.
• a cellulosic fabric is first treated with a crosslinking agent, for example by application from a pad bath, dried, and then heated to cure the resin and induce crosslinking (pad-dry-cure) .
• a crosslinking agent for example by application from a pad bath
• crease- resistant finishing treatments embrittle cellulose fabric with consequent loss of abrasion resistance, tensile strength and tear strength.
• the first crosslinking systems were based on formaldehyde, urea-formaldehyde and melamine-formaldehyde resins. These suffered a number of problems.
• the treatment caused temporary stiffening of the fabric because of the presence of externally adhering resin. Treated fabric was liable to liberate objectionable odours on storage. These odorous substances included the amine catalysts used to cure the resin and the toxic chemical formaldehyde. It was therefore considered necessary to wash the treated fabric to remove externally adhering resin and byproducts of resin formation capable of giving rise to objectionable odours. Such washing and subsequent drying of the treated fabric added to the cost of the process.
• Such systems have largely been replaced by systems containing the so-called “low-formaldehyde resins” and "zero- formaldehyde resins” as crosslinking agents.
• One known class of such agents consists of the N-methylol resins, that is to say small molecules containing two or more N-hydroxymethyl or N-alkoxymethyl, in particular N-methoxymethyl, groups.
• N- methylol resins are generally used in conjunction with acid catalysts chosen to improve crosslinking performance.
• a solution containing about 5-9% by weight N-methylol resin crosslinking agent and 0.4-3.5% by weight acid catalyst is padded onto dry cellulosic fabric to give 60-100% by weight wet pickup, after which the wetted fabric is dried and heated to cure and fix the crosslinking agent.
• Fabrics treated with low-formaldehyde or zero-formaldehyde resins generally do not exhibit temporary stiffening and do not release objectionable odours. Cured flat fabrics and finished garments are rarely washed prior to sale to the consumer.
• a method for reducing the fibrillation tendency of lyocell fabric includes the steps of:
• the fabric is treated with the crosslinking resin and heated to cause reaction between the resin and the cellulose in the form of flat fabric.
• the fabric is washed and dried in the form of flat fabric and is thereafter suitable for cutting into pieces for the manufacture of garments or other textile articles.
• the fabric is first made up into garments or other textile articles which are then washed and dried to complete the method of the invention.
• a method for reducing the degree of fibrillation of lyocell fabric includes the steps of:
• a method for providing a lyocell fabric which exhibits a low degree of fibrillation and has a low fibrillation tendency includes the steps of:
• the fabric may optionally be bleached between the scouring and dyeing processes in step (a) and may optionally be dried between steps (a) and (b) .
• the fabric may exhibit such a high degree of fibrillation that textile articles made from it would be commercially unacceptable.
• the fabric in the form of flat fabric or of textile articles exhibits a very low and commercially desirable degree of fibrillation.
• One class of preferred crosslinking resins consists of the N-methylol resins.
• suitable N-methylol resins are those described in the abovementioned articles in Kirk- Othmer and by Petersen.
• Examples of such resins include 1,3- dimethylolethyleneurea (DMEU) , 1,3-dimethylolpropyleneurea (DMPU) and 4,5-dihydroxy-l,3-dimethylolethyleneurea (DHDMEU) .
• Other examples include compounds based on urones, triazinones and carbamates.
• Another example of a preferred class of crosslinking agents consists of compounds based on 1,3- dialkyl-4,5-dihydroxy(alkoxy)ethyleneurea and its derivatives.
• a further example of a suitable crosslinking agent is melamine.
• Yet another example of a suitable crosslinking agent is butanetetracarboxylic acid (BTCA) . More than one type of crosslinking resin may be used.
• Crosslinking agents for crease-resistant finishing of cellulose fabric are generally used in conjunction with a catalyst.
• the catalyst serves to accelerate the crosslinking reaction and curing and fixation of the resin.
• the method of the invention preferably utilises such a catalyst when recommended for use with the chosen crosslinking agent.
• N-methylol resins are preferably used in conjunction with an acid catalyst, for example an organic acid such as acetic acid or a mineral acid such as zinc nitrate or magnesium chloride.
• Latent acids such as ammonium salts, amine salts and metal salts may be used.
• Mixed catalyst systems may be used.
• the crosslinking agent and any catalyst are preferably applied to the fabric from solution, preferably in water.
• the solution may be applied to the fabric in known types of ways, for example the solution may be padded on to the fabric or the fabric may be passed through a treatment bath of the solution.
• the fabric may be a woven or knitted fabric.
• the solution may contain at least about 2%, preferably about 3 to about 6%, by weight crosslinking agent.
• the solution may contain at least about 1%, preferably about 1 to about 2%, by weight catalyst.
• the fabric After treatment with crosslinking resin according to the invention, the fabric is heated to fix and cure the crosslinking agent.
• the fabric may also be dried.
• the heating step may precede, be part of, or follow the drying step.
• the time and temperature required in the heating step depend on the nature of the crosslinking agent and optional catalyst employed.
• Afte _ heating and optionally drying the fabric may contain at least about 0.5%, preferably at least about 1.0%, more preferably at least about 2.0%, by weight of fixed crosslinking agent calculated on the weight of the cellulose.
• the fabric generally contains no more than about 4% by weight of fixed crosslinking agent calculated on the weight of the cellulose. It has generally been found that about 70 to 90% of the crosslinking agent in the wet fabric may become fixed to the cellulose.
• the concentration of the resin in the bath is chosen according to the activity and curing efficiency of that resin, to give the desired value for resin fixed on fabric.
• the fabric After heating and fixation, the fabric is washed and dried according to conventional procedures for cellulose fabrics.
• Fabric treated according to the invention exhibits a very low degree of fibrillation. This is particularly
• the method of the invention is applicable to fabric which has already been dyed, including fabric dyed by processes such as rope-dyeing which are known to cause mechanical abrasion.
• This is an advantage of the invention, because it is known that rope-processing of a fabric generally improves bulking and relaxation of the fabric, leading to superior handle.
• the method of the invention can be used on fabric which is already fibrillated, even severely fibrillated. It has surprisingly been found that when fabric exhibiting a high degree of fibrillation is treated according to the method of the invention, the treated fabric generally exhibits a very low level of fibrillation. For most applications, fabric which exhibits a high degree of fibrillation is considered to be of substandard quality, with the consequence that additional expensive processing steps are not considered to be justified. It is a particular advantage of the invention that it permits substandard fabric to be converted into first quality fabric and textile articles.
• Test Method 1 Materials were assessed for degree of fibrillation using the method described below as Test Method 1.
• Fibrillation Index There is no universally accepted standard for assessment of fibrillation, and the following method was used to assess Fibrillation Index (F.I.). Samples of fibre were arranged into a series showing increasing degrees of fibrillation. A standard length of fibre from each sample was then measured and the number of fibrils (fine hairy spurs extending from the main body of the fibre) along the standard length was counted. The length of each fibril was measured, and an arbitrary number, being the product of the number of fibrils multiplied by the average length of each fibril, was determined for each fibre. The fibre exhibiting the highest value of this product was identified as being the most fibrillated fibre and was assigned an arbitrary Fibrillation Index of 10. A wholly unfibrillated fibre was assigned a Fibrillation Index of zero, and the remaining fibres were evenly ranged from 0 to 10 based on the microscopically measured arbitrary numbers.
• the measured fibres were then used to form a standard graded scale.
• To determine the Fibrillation Index for any other sample of fibre five or ten fibres were visually compared under the microscope with the standard graded fibres. The visually determined numbers for each fibre were then averaged to give a Fibrillation Index for the sample under test. It will be appreciated that visual determination and averaging is many times quicker than measurement, and it has been found that skilled fibre technologists are consistent in their rating of fibres.
• Fibrillation Ir ax of fabrics can be assessed on fibres drawn from the surface of the fabric. Woven and knitted fabrics having F.I. of more than about 2.0 to 2.5 exhibit an unsightly appearance.
• the never-dried fibre used was prepared by extruding a solution of cellulose in N-methylmorpholine N- oxide (NMMO) into an aqueous bath and washing the fibre so formed with water until it was essentially free of NMMO.
• NMMO N-methylmorpholine N- oxide
• a 100% lyocell spun yarn woven fabric exhibiting zero F.I. was desized, scoured and dyed in a jet dyeing machine.
• Desizing was carried out using a 1.5 g/1 aqueous solution of a commercially-available amylase preparation at pH 6.5-7.5 for 45 minutes at 70°C.
• Scouring was carried out using an aqueous solution containing 2 g/1 sodium carbonate and 2 g/1 anionic detergent for 60 minutes at 95°C.
• Dyeing was carried out using an aqueous solution containing 4% by weight on fabric of the dyestuff Procion Navy HE-R 150 (Procion is a Trade Mark of Zeneca pic) , 80 g/1 sodium sulphate and 20 g/1 sodium carbonate for 120 minutes at 85°C.
• the fabric was rinsed with water, first at 70°C and then at ambient temperature; soaped off using an aqueous solution containing 2 g/1 Sandopur SR
• Samples of dyed fabric were padded with aqueous solutions containing varying amounts of the low-formaldehyde resin DHDMEU (supplied under the Trade Mark Arkofix NG cone by Hoechst AG) .
• the solutions contained an acid-liberating catalyst as recommended by the resin supplier at 25% by weight on weight of Arkofix NG cone.
• the samples of fabric were then dried at 110°C and the resin flash cured for 30 seconds at 180°C. They were then reloaded on the jet dyeing machine and scoured twice as before.
• the figures for the amount of resin fixed on fabric are estimated figures, based on 70% active solids in Arkofix NG cone, 80% expressed liquor, and 85% curing efficiency.

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)
• Coloring (AREA)
• Fish Paste Products (AREA)
• Polysaccharides And Polysaccharide Derivatives (AREA)

Priority Applications (8)

Applications Claiming Priority (2)

Publications (1)

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Family Applications (1)

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Cited By (13)

Families Citing this family (6)

Citations (7)

• 1993
  • 1993-06-24 GB GB939313128A patent/GB9313128D0/en active Pending
• 1994
  • 1994-06-16 TW TW083105579A patent/TW286335B/zh not_active IP Right Cessation
  • 1994-06-21 DE DE69407045T patent/DE69407045T2/de not_active Expired - Lifetime
  • 1994-06-21 BR BR9406831A patent/BR9406831A/pt not_active IP Right Cessation
  • 1994-06-21 WO PCT/GB1994/001342 patent/WO1995000697A1/en not_active Application Discontinuation
  • 1994-06-21 JP JP50257495A patent/JP3479076B2/ja not_active Expired - Lifetime
  • 1994-06-21 CN CN94192508A patent/CN1077184C/zh not_active Expired - Lifetime
  • 1994-06-21 ES ES94918464T patent/ES2110765T3/es not_active Expired - Lifetime
  • 1994-06-21 CA CA002166099A patent/CA2166099A1/en not_active Abandoned
  • 1994-06-21 PL PL94312226A patent/PL312226A1/xx unknown
  • 1994-06-21 EP EP94918464A patent/EP0705358B1/en not_active Expired - Lifetime
  • 1994-06-21 CZ CZ953430A patent/CZ343095A3/cs unknown
  • 1994-06-21 SK SK1603-95A patent/SK160395A3/sk unknown
  • 1994-06-21 AU AU69774/94A patent/AU688771B2/en not_active Expired - Fee Related
  • 1994-06-21 KR KR1019950705093A patent/KR100316542B1/ko not_active IP Right Cessation
  • 1994-06-21 HU HU9503716A patent/HUT74118A/hu unknown
  • 1994-06-21 AT AT94918464T patent/ATE160600T1/de not_active IP Right Cessation
  • 1994-06-22 ZA ZA944482A patent/ZA944482B/xx unknown
  • 1994-06-24 TR TR00634/94A patent/TR28229A/xx unknown
  • 1994-06-24 MX MX9404809A patent/MX9404809A/es not_active Application Discontinuation
• 1995
  • 1995-12-21 FI FI956184A patent/FI956184A0/fi not_active Application Discontinuation

Patent Citations (7)

Non-Patent Citations (3)

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