EP4305099A1 - Fibre de cellulose régénérée modifiée - Google Patents

Fibre de cellulose régénérée modifiée

Info

Publication number
EP4305099A1
EP4305099A1 EP22770717.1A EP22770717A EP4305099A1 EP 4305099 A1 EP4305099 A1 EP 4305099A1 EP 22770717 A EP22770717 A EP 22770717A EP 4305099 A1 EP4305099 A1 EP 4305099A1
Authority
EP
European Patent Office
Prior art keywords
regenerated cellulose
cellulose fiber
modifier
fiber
range
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP22770717.1A
Other languages
German (de)
English (en)
Inventor
Dhrubajyoti KALITA
Parag Patil
Vikas Dnyaneshwar CHAVAN
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Grasim Industries Ltd
Original Assignee
Grasim Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Grasim Industries Ltd filed Critical Grasim Industries Ltd
Publication of EP4305099A1 publication Critical patent/EP4305099A1/fr
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B16/00—Regeneration of cellulose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/10—Crosslinking of cellulose

Definitions

  • the present disclosure relates to a modified regenerated cellulose fiber and a continuous process for preparation of said modified regenerated cellulose fiber. Particularly, the present disclosure relates to a modified regenerated cellulose fiber which are fibril free or have a reduced fibrillation tendency.
  • Regenerated cellulose fiber like natural fibers such as cotton and hemp have been a key material in textile industry. This is predominantly because of its superior moisture absorbing property and biodegradability along with soft to touch and drapability. However, regenerated cellulose fiber has certain defects such as poor water resistance leading to high degree of swelling in water and shrinkage percentage after washing and whitening due to fibrillation. Fibrillation is a phenomenon in which a filament or fiber shows evidence of smaller-scale fibrous structure by a longitudinal raveling of the filament under rapid, excessive tensile or shearing stress, giving rise to frosted appearance on dyed fabrics.
  • lyocell fiber is of high significance. Lyocell fiber shows some key advantageous characteristics over other cellulosic fibers, for instance, a high dry and wet tenacity and high wet modulus. However, the fiber also shows an extensive tendency to fibrillate in the wet state. This tendency to fibrillate has been attributed to the spinning process, which causes the formation of longer and more oriented crystalline regions and smaller but more oriented amorphous regions in the fiber structure. Additionally, mechanical abrasions in wet processing (such as scouring, dyeing etc.) in commercial dye houses, which are also high temperature and longtime processes, cause more damage to the fabric.
  • wet processing such as scouring, dyeing etc.
  • Crosslinkers are small molecules containing a plurality of functional groups capable of reacting with the hydroxyl groups in cellulose to form crosslinks.
  • crosslinking agent is a low formaldehyde resin such as N-methylol resin, urea formaldehyde resin.
  • formaldehyde based crosslinking agents are not suitable as they release formaldehyde from fiber even after downstream processing to fabric and multiple laundry washes.
  • crosslinking agents have been reported in literature for reducing the fibrillation of lyocell fiber to expected level.
  • crosslinking agents have disadvantages such as they tend to reduce the elongation and tenacity of fiber considerably due to constrained spatial structure of the cellulose-cross-linked network or need very high dosage and hence affects elongation.
  • they can only partially reduce the fibrillation due to inherent instability of crosslinks under scouring and acidic/alkaline dyeing conditions.
  • EP0538977B1 and US5310424 describe usage of colorless chlorotriazine compounds with 2 or higher reactive arms, such as Sandospace R, for fibrillation reduction on lyocell fiber.
  • the use of these chemical reagents is not commercially viable due to inherent instability of the chlorotriazine compounds.
  • US5779737 discloses usage of triazine based acrylamide compounds such as, l,3,5-Triacryloylhexahydro-l,3,5-triazine (by TCI chemical) in presence of inorganic alkali, for fibrillation reduction at fiber stage.
  • This class of compounds are reported significantly toxic and the crosslinks formed are partially stable to alkaline hydrolysis and also prone to release formaldehyde under downstream processing conditions.
  • cross-linkers such as polyfunctional aziridines (“PZ-28”, “PZ-33” from Polaziridine LLC.), (N-methoxymethyl) melamines (“Rucon- DMO” from Rudolf and “RA-65” from Dalian Richon), Poly(isobutylene-alt- maleic anhydride), Poly[(isobutylene-alt-maleimide)-co-(isobutylene-alt-maleic anhydride)] (by Sigma Aldrich), L-Lysine Triisocyanate (by ABCR GmBH & Co.
  • PZ-28 polyfunctional aziridines
  • PZ-33 from Polaziridine LLC.
  • Rucon- DMO from Rudolf and “RA-65” from Dalian Richon
  • Poly(isobutylene-alt- maleic anhydride) Poly[(isobutylene-alt-maleimide)-co-(isobutylene-alt-maleic anhydride)] (by Sigma Ald
  • a modified regenerated cellulose fiber comprises of regenerated cellulose crosslinked with a modifier, wherein the modifier comprises a crosslinking agent having a formula I or II: wherein
  • each A is independently H, CH 3 , OH , or ⁇ each B is independently H, OH, O-A, CH 2 OH, CH 2 O-A, or
  • C is H or OH
  • Y is O or (CH 2 ) n ; a is an integer in the range of 0-6; b is an integer in the range of 0-4; m is an integer in the range of 0-3; n is an integer in the range of 1-5.
  • a process for preparing a modified regenerated cellulose fiber comprises treating a never-dried regenerated cellulose fiber with a modifier comprising a crosslinking agent having a formula I or II: wherein D ⁇ each A is independently H, CH3, OH , or ; Y each B is independently H, OH, O-A, CH2OH, CH2O-A, or OH C is H or OH;
  • Y is O or (CH 2 )n; a is an integer in the range of 0-6; b is an integer in the range of 0-4; m is an integer in the range of 0-3; n is an integer in the range of 1-5.
  • the treated regenerated cellulose fiber is cured at a temperature between 100-160°C to obtain the modified regenerated cellulose fiber.
  • never-dried regenerated cellulose fiber is intended to refer to a regenerated cellulose fiber obtained using any known process, that has not been dried using heat or other thermal energy during the various stages of processing of regenerated cellulose fiber, such as tow, staple or yarn filament.
  • modified regenerated cellulose fiber which are fibril free or have a reduced fibrillation tendency.
  • said modified regenerated cellulose fiber comprises of regenerated cellulose fiber crosslinked with a modifier, wherein the modifier comprises a crosslinking agent having a formula I or II: wherein
  • a continuous process for preparing said modified regenerated cellulose fiber is also disclosed.
  • Said process comprises treating a never-dried regenerated cellulose fiber with the modifier comprising a crosslinking agent having a formula I or II: wherein each A is independently H, CH 3 , each B is independently H, OH, O-A, CH 2 OH, CH 2 O-A, or OH C is H or OH;
  • Y is O or (CH 2 )n; a is an integer in the range of 0-6; b is an integer in the range of 0-4; m is an integer in the range of 0-3; n is an integer in the range of 1-5.
  • the treated regenerated cellulose fiber is cured at a temperature between 100-160°C to obtain the modified regenerated cellulose fiber.
  • the present inventors found that the disclosed modified regenerated cellulose fibers exhibits sufficient degree of fibrillation resistance. It was further found that the modified regenerated cellulose fibers exhibit tenacity and elongation comparable to regenerated cellulose fibers which have not been modified. Specifically, it was observed that when never-dried regenerated cellulose fiber is treated with the modifier of present disclosure, the fibrillation resistance expressed as wet abrasion number (WAN) improved and there was no negative effect on fiber properties like tenacity and elongation loss as seen in case of conventional crosslinking agents reported in literature.
  • the modified regenerated cellulose fiber comprises the modifier in an amount ranging between 1-25% by weight of cellulose. In some embodiments, the modified regenerated cellulose fiber comprises the modifier in an amount ranging between 5-18% by weight of cellulose.
  • the modifier is an epoxy-based crosslinking agent having the formula I or II or a halohydrin-based crosslinking agent having the formula I or II.
  • the epoxy-based crosslinking agents having a formula I or II comprises epoxy-based agents with multiple epoxy rings, selected from the group of short to medium chain water insoluble or sparingly soluble reactive diluents or polyglycidyl ethers of polyhydric alcohols.
  • epoxy-based crosslinking agents are trifunctional epoxy compounds such as trimethylolpropane triglycidyl ether - TMPTGE (“Epotec RD113” from Aditya Birla Chemicals, tetrafunctional pentaerythritol based polyglycidyl ether (“Epotec RD129” from Aditya Birla Chemicals), sorbitol polyglycidyl ethers (“Denacol EX-614, EX-622” from Nagase Chemtex), Glycerol/polyglycerol polyglycidyl ethers (“Denacol EX-313, EX-314, EX-421, EX-512, EX-521” from Nagase Chemtex.
  • Suitable glycidyl amines derivatives can also be used but have lesser bath stability due to self crosslinking (“Erisys GA 240” from CVC Thermoset specialties). Presence of amine-based catalysts/curing agents (“Anquamine 728, 287, 721” from Evonik, “Lupasol-P” from BASF, “Danfix PAA” from Nittobo) should be avoided in order to facilitate bath stability for continuous process; however, short duration usage of such one-pot system of epoxy-based agent and curing agent can also be used.
  • precursors of above-mentioned epoxy compounds which are halohydrin-based crosslinking agents having a formula I or II comprises polymeric halohydrins with 3 or more halohydrin groups per repeat unit with/without pendant hydroxyl group.
  • halohydrin-based crosslinking agent gets converted to reactive epoxide in situ, which further reacts with cellulose hydroxyl groups. This reaction can be controlled by proper selection of pH, catalyst system, curing assembly type and curing temperature.
  • the halohydrin-based crosslinking agents are capable of making stable ether crosslinks between hydroxyl groups of cellulose fiber under alkaline conditions of pH 9-13.
  • the halohydrin-based crosslinking agents comprise water soluble/miscible chlorohydrin compounds which are derivatives of polychlorohydrin ether of polyhydric alcohols with pendent chlorohydrin functional groups.
  • the modifier further comprises one or more of a solvent, inorganic alkali/alkaline earth hydroxides/carbonates/phosphates, metal fluoroborates etc.
  • the modifier further comprises of one or more of a phase transfer catalyst, lubricating/non-ionic surface-active agent, reactive cationization agent, and an exhaustion agent.
  • the exhaustion agent is selected from the group consisting of alkali salts, alkaline earth salts and the combination thereof.
  • the alkali salt is selected from the group consisting of sodium chloride, sodium sulphate and mixtures thereof.
  • the alkaline earth salt is selected from the group consisting of magnesium sulphate, magnesium carbonate, calcium sulphate and mixtures thereof.
  • the modifier is an alkaline solution of 3- 20% (w/v) of crosslinking agent having a formula I or II.
  • the modifier is prepared in an aqueous solution at pH 9-13, or a solvent mixture such as 10-40 % water and 50-95% alcohol selected from the group consisting of methanol, ethanol and isopropyl alcohol, or a surfactant mixture and/or polymeric dispersion (or emulsion) at pH 9-13.
  • the moisture content of never-dried regenerated cellulose fiber is in a range of 70-300% by weight of cellulose.
  • the incoming fiber tow has a moisture content of 80-300%.
  • the incoming fiber tow has a moisture content of 90-150%.
  • the incoming fiber tow has a moisture content of 100-130%.
  • the modifier is applied to a never-dried regenerated cellulose fiber in the application bath at a temperature in a range of 25-45°C. In some embodiments, the modifier is applied at an ambient temperature in a range of 25-35°C. In accordance with an embodiment, the treatment of tow/ fiber bed is carried out in application bath for a time period of 3-300 seconds, for efficient wetting and moisture replacement. In some embodiments, the treatment is carried out for 60-120 seconds.
  • curing is carried out at a temperature between 100-160 C to induce covalent crosslinking. In some embodiments, curing is carried out at the temperature between 120-140 C. In some embodiments, the curing is carried out for 5-120 minutes. In some embodiments, curing is carried out for 10-20 minutes.
  • the modified regenerated cellulose fiber is further subjected to one or more of washing, neutralization, bleaching, lubricating and drying steps.
  • the modified regenerated cellulose fiber is subjected to a washing step.
  • the modified regenerated cellulose fiber is subjected to a neutralization step for removal of residual catalyst and crosslinking agent.
  • Neutralization agents for inorganic alkali can be dilute organic acids, and neutralization agents for traces of epoxy can be known polymeric amines/imines.
  • the dilute organic acids are selected from the group consisting of acetic acid, citric acid, lactic acid and mixtures thereof.
  • the washed and neutralized fiber is bleached to desired whiteness, neutralized to pH 6-7 with dilute aqueous organic acid followed by bleaching, spin finish application and drying.
  • organic route is used for application of modifier.
  • organic solvents are used to form the modifier.
  • the coupling of epoxide with cellulose hydroxyl groups is carried out in a base catalyzed condition at temperature 80°C-150°C. In some embodiments, said coupling is carried out at 100-145°C. In some embodiments, said coupling is carried out at 110-140°C using dry heat, saturated steam or super-heated steam.
  • the modifier in the organic route comprises of a phase transfer catalyst such as tetraethylammoniumbromide (TEAB) or cationic polymers such as Poly(DADMAC) in the application bath for faster penetration and better reaction.
  • TEAB tetraethylammoniumbromide
  • DADMAC cationic polymers
  • This fiber upon curing is washed using the same solvent in multiple baths followed by hot water wash and using aqueous acid neutralization to remove unreacted crosslinking agent and catalyst, and the solvent can be recovered easily for reuse by distillation as it doesn’t interfere with the crosslinking agent having very high boiling point. Also, the removal of solvent by suction from the treated fiber prior to entering dryer is possible, hence eliminating any fire hazard in a continuous drying set up.
  • crosslinking agent can be ascertained by washing with dilute solution of polymeric amines such as Polyallylamine (“Danfix PAA” series from Nittobo), polethylenimine ( “Lupasol” from BASF), Polyvinylamines etc., as they react with free epoxy at room temperature thereby removing the remnant epoxy, without causing any disturbance to crosslinked structure.
  • polymeric amines such as Polyallylamine (“Danfix PAA” series from Nittobo), polethylenimine ( “Lupasol” from BASF), Polyvinylamines etc.
  • aqueous route is used for application of modifier.
  • aqueous solvents are used to form the modifier.
  • suitable halohydrin/epoxy compound containing water loving pendant groups are dissolved/dispersed in water at room temperature, followed by elevating the pH of bath with alkali to 11-12.5.
  • the application bath contains an exhaustion agent for uniform exhaustion.
  • suitable non-ionic/cationic surfactant blends, alkali/alkaline earth metal salts or polymeric quats such as Poly(DADMAC) are added to avoid inter-fiber entanglement during drying process.
  • suitable dye pick up enhancing agents that are reactive to cellulose can be used in the application bath (“Quat 188”, “CR2000”, “Ecofast Pure” from Dow chemicals and “Cationon KCN” from Lion specialty chemicals). Caution should be taken when selecting these dyeing strength boosting agents, not to interfere with the crosslinking reaction because of competing reactions, and can be judiciously chosen by a person skilled in the art.
  • epoxy agents that are insoluble in water are dispersed in surfactant blends selected from the group consisting of branched secondary alcohol ethoxylates (“Tergitol TMN-6, Tergitol TMN-10” from Dow), Octylphenol ethoxylates (“Triton X-405” from Sigma Aldrich), alkylpolyglycosides (“Elotant milcoside 200/300” from LG chemicals and additionally polymeric thickeners selected from the group of polysaccharides (such as sodium carboxymethylcellulose), without allowing the ring opening of epoxide (as caused by regular anionic and Hydroxylated nonionic surfactants).
  • the surfactant blend of epoxide is dispersed in water by stirring and pH adjusted with NaOH, prior to application as explained above, but at slightly higher temperature 30-50 °C.
  • the regenerated cellulose fiber of the present disclosure is lyocell fiber and a known N-methylmorpholine-N-oxide (NMMO) dissolution method or lyocell process is used to prepare disclosed modified regenerated cellulose fiber.
  • said process comprises the steps of: a. dissolving the cellulose in amine oxides or ionic liquids as solvents such as NMMO, followed by extruding of dope from a multiplicity of fine apertured spinnerets into air. b. washing of fiber to remove the solvent therefrom; c. passing the tow/fiber bed in application bath comprising the modifier; d. adjusting wet pick up of the fiber; e. optionally, removing the residual solvent for recycling; f. curing followed by drying of the fiber to a predetermined moisture content; g. washing followed by neutralizing of the fiber.
  • NMMO N-methylmorpholine-N-oxide
  • step (b) removal of the solvent from fiber is carried out in multiple aqueous baths.
  • NMMO reacts with the crosslinking agent by ring opening, hence removal of traces of NMMO from wet tow/fiber is must to maintain bath stability in a continuous process.
  • step (c) the tow/fiber bed is passed through the application bath multiple times for uniform wetting with/without intermittent squeeze. Examples:
  • the wet abrasion number was determined in a wet abrasion testing machine FNP02 from SMK Prazisionsmechanik GmbH.
  • a fiber is clamped under a fixed pretention of 70mg, over an abrasive shaft tightly wrapped with a tube fabric in wet form (with demineralized water) and number of rotations are counted till fracture of the fiber.
  • the number of rotation sustained is the Wet Abrasion Number.
  • the rotational speed of fabric wrapped shaft is fixed at 400 RPM, with angle of contact 45°.
  • Example 1 Effect of modifier on fibrillation resistance and tensile properties
  • TMPTGE TMPTGE
  • TEAB tetraethylammonium bromide
  • Table 1 Effect of modifier concentration on WAN and tensile properties, in a sequential treatment condition
  • Example 1 was repeated except that the curing is done in a hot air oven at 165°C for 15 minutes. Effect of higher temperature of curing was investigated at chemical loading of 2.5-10% (Experiments 2A-2C), as indicated in Table 2.
  • Example 3 Treatment with purer grade of TMPTGE 0
  • Example 1 was repeated except that trimethylolpropanetriglycidyl ether (TMPTGE) available from Sigma Aldrich was used as a much purer grade, as indicated in Table 3. Observation: The WAN increased as compared to commercially available chemical (experiment 1C), at same % loading. Table 3: Result of a sequential treatment of fiber with purer grade of
  • Example 4 Effect of modifier on bleaching: Single bath treatment in methanol-water None-dried lyocell filament was washed as in Example 1. Filament containing 90-120% moisture was passed through a bath containing 2.5-10% trimethylolpropanetriglycidyl ether in a mixture of 90% methanol + 10% water at room temperature (30-35°C). The bath contained 2-3g/L sodium hydroxide and 0.2-0.3% tetraethylammonium bromide (TEAB). After padding at 100% wet pick up, filament was cured at 140-145°C for 15-20 minutes in hot air. The filament was washed with methanol once followed by water at 60°C, followed by cold wash to remove unreacted crosslinking agent.
  • TEAB tetraethylammonium bromide
  • Example 4 was repeated except that the solvent was 50-90% ethanol aqueous, instead of methanol.
  • the bath comprised of 7.5% TMPTGE, 0.2-0.4% TEAB and 3g/L NaOH in respective alcohohwater mixture.
  • Table 5 shows the result of Experiments 5A-5C in which alcohol concentration was varied.
  • Example 6 Single bath treatment in water 10-15% of a Polychlorohydrin ether of polyhydric alcohol, hereafter named as Poly(CH-O-PHA) (as exemplified in Figure 1) was dissolved in water at room temperature to obtain a clear-to- slightly hazy solution, followed by elevating the pH of bath with 45% NaOH under continuous mixing and pH monitoring. The bath pH is maintained at 11.5-12.5. Lubricating agent is added and mixed well. The conversion to reactive epoxide is ensured by no sudden drop in pH. Washed and never-dried lyocell filament is passed through the application bath with 5 residence time of 1.5-3 s and squeezed to desired wet uptake before entering the curing chamber.
  • Poly(CH-O-PHA) as Poly(CH-O-PHA)
  • the drying and curing is complete in 15-20 minutes at 125- 145°C, while higher curing time has no negative impact.
  • the treated tow is washed, cut, bleached to desired whiteness, neutralized to pH 6-7 with dilute aqueous organic acid followed by spin finish application and drying.
  • Example 7 Estimation of chemical uptake as function of treatment duration, prior to curing
  • Example 4 was repeated and in Experiment 4 A and 4C, the residence time of cellulose filament in application bath was maintained at 5 minutes and 20 minutes respectively.
  • Example 8 Reaction efficiency - Estimation of bound crosslinking agent on the basis of free epoxide
  • the crosslinking agent used contains multiple epoxy groups and same was quantified by adaptation of existing non-aqueous titration method on as is fiber and washed fiber, to estimate the extent of reaction- indicates almost complete reaction. Also, washing removes the traces completely, as indicated in Table 8.
  • Example 9 Single bath treatment in water using surfactant blend
  • TMPTGE trimethylolpropanetriglycidyl ether
  • 1-2% Tergitol TMN 6 with 3% Triton X405 or 3% Sorbelon MN or 1% 02-16 alkyl benzoate 0.4% TEAB and 0.2% NaOH(s) at room temperature (30-35°C) under constant agitation.
  • filament containing 90-120% moisture was passed through an application bath containing above dispersion at 35-45°C. After padding at 100% wet pick up, filament was cured at 145-150°C for 22-25 minutes in hot air. The filament was washed with hot water followed by cold wash to remove unreacted crosslinking agent.
  • Protocol for acid stability 5g crosslinked fiber treated at 1:20 MLR in dilute acetic acid solution at pH 4-4.5, at 130°C for 30 minutes, followed by washing in plain DM water and drying at 105°C. WAN was measured. Protocol for scouring or alkaline stability: 5g crosslinked fiber treated at
  • Control and crosslinked fibers were scoured, and dyed with three reactive dyes separately: Reactive red F3B - 3% o.w.f., Reactive red HE3BI - 3% o.w.f. and Blue HERDI- 4% o.w.f. (Reactive red F3B with C.I. 181055, Reactive red HE3BI with C.I. 292775, and Reactive blue HERDI with C.I. 137160).
  • Dye bath comprised of 70g/L sodium sulphate and 18g/L soda ash for red dye, and 80g/L sodium sulphate as well as 20g/L soda ash for blue dye. Dyeing was carried out at 60°C for 45 min, followed by water wash, 2g/L non-phosphate ECE detergent at 60°C for 30 min, hot water wash, cold water wash and then drying at 105°C.
  • Table 11C Dyeing results with Reactive Red HE3BI dye - 3% o.w.f. shows negligible impact on color strength and tone.
  • the disclosed modified regenerated cellulose fibre exhibits improved fibrillation resistance expressed as wet abrasion number (WAN) and has similar or improved mechanical properties such as elongation and tenacity as compared to fiber without said modification.
  • WAN wet abrasion number
  • the disclosed modified regenerated cellulose fiber exhibits sufficient degree of fibrillation resistance expressed as wet abrasion number (WAN) and the tenacity and elongation in desired range. This was confirmed on both fiber (after wet abrasion test) and fabric surface by SEM before and after home laundering.
  • the disclosed modified regenerated cellulose fiber exhibits anti-fibrillation property even after downstream processing like commercial scouring, dyeing processes and multiple home laundering (washes).
  • the present disclosure provides a process for the preparation of fabric obtained from various regenerated cellulose fibers, in particular, lyocell fibers having reduced fibrillation, which is simple and cost-effective.
  • the disclosed process of preparing said modified regenerated cellulose fibers is a continuous process. It is cost effective and environmentally sustainable. Specifically, neither the modifier nor the dispersants/catalysts of the modifier have the tendency to liberate toxic formaldehyde, which has remained a major concern for most of the formaldehyde-based resins/cross-linkers used in fiber/textile industry.
  • the disclosed method provides safer crosslinking chemistry for reducing the fibrillating tendency of fiber.
  • the modifier used in the present method is non volatile, do not need a high temperature dissolution process for application onto wet lyocell tow/staple fiber in a batch/continuous set up, and has the ability to undergo almost complete reaction from alcoholic solvent/aqueous approach under continuous drying and curing conditions.
  • organic solvents used in the present disclosure have widely separated boiling points from water and can easily be completely removed by vacuum without altering the homogeneous distribution of the high boiling cross-linker in the cellulose domain, prior to entering dryer and can be recycled back.
  • the ease of solvent removal by vacuum further makes the process safe in terms of curing condition in a continuous process.
  • the modifier of the present disclosure also does not negatively affect the dye binding ability of the fiber. This is understood to be due to free -OH sites generated after ring opening of epoxide groups on the modifier, thereby keeping the reactive dyeing tendency of fibers almost intact both in acidic and alkaline environments.

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

Abstract

L'invention concerne une fibre de cellulose régénérée modifiée. Ladite fibre de cellulose régénérée modifiée comprend de la cellulose régénérée réticulée avec un modificateur, le modificateur comprenant un agent de réticulation répondant à une formule I ou II : (I) (II) chaque A étant indépendamment H, CH3,(III), ou ; chaque B étant indépendamment H, OH, O-A, CH2OH, CH2O-A, ou C étant H ou OH ; Y étant O ou (CH2)n ; a étant un nombre entier dans la plage de 0 à 6 ; b étant un nombre entier dans la plage de 0 à 4 ; m étant un nombre entier dans la plage de 0 à 3 ; n étant un nombre entier dans la plage de 1 à 5.
EP22770717.1A 2021-03-15 2022-03-15 Fibre de cellulose régénérée modifiée Pending EP4305099A1 (fr)

Applications Claiming Priority (2)

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IN202121010861 2021-03-15
PCT/IB2022/052309 WO2022195465A1 (fr) 2021-03-15 2022-03-15 Fibre de cellulose régénérée modifiée

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WO2024110873A1 (fr) * 2022-11-22 2024-05-30 North Carolina State University Polymérisation par greffage de monomères cationiques en fibres cellulosiques pour une coloration et une finition durables simultanées

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GB9408742D0 (en) * 1994-05-03 1994-06-22 Courtaulds Fibres Holdings Ltd Fabric treatment
AT403296B (de) * 1995-08-11 1997-12-29 Chemiefaser Lenzing Ag Verfahren zur herstellung eines celluloseformkörpers
US6514610B2 (en) * 1999-12-13 2003-02-04 Fuji Spinning Co., Ltd. Method for manufacturing improved regenerated cellulose fiber
JP5646572B2 (ja) * 2012-10-16 2014-12-24 日本蚕毛染色株式会社 改質繊維およびその製造方法

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