WO2017019802A1 - Procédés et systèmes de traitement de matière première textiles mixtes, isolement des molécules constituantes, et régénération de fibres polyester et cellulosique - Google Patents

Procédés et systèmes de traitement de matière première textiles mixtes, isolement des molécules constituantes, et régénération de fibres polyester et cellulosique Download PDF

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Publication number
WO2017019802A1
WO2017019802A1 PCT/US2016/044325 US2016044325W WO2017019802A1 WO 2017019802 A1 WO2017019802 A1 WO 2017019802A1 US 2016044325 W US2016044325 W US 2016044325W WO 2017019802 A1 WO2017019802 A1 WO 2017019802A1
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WIPO (PCT)
Prior art keywords
cellulose
treatment
pulping
methylimidazolium
polyester
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PCT/US2016/044325
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English (en)
Inventor
Stacy Flynn
Christopher Stanev
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Evrnu, Spc
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.)
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Publication date
Priority claimed from US14/811,723 external-priority patent/US20160369456A1/en
Application filed by Evrnu, Spc filed Critical Evrnu, Spc
Priority to US15/747,736 priority Critical patent/US11034817B2/en
Priority to EP16831317.9A priority patent/EP3328924A4/fr
Publication of WO2017019802A1 publication Critical patent/WO2017019802A1/fr
Priority to US17/344,646 priority patent/US20210340350A1/en
Priority to US18/066,119 priority patent/US20230124761A1/en

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    • 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
    • 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

Definitions

  • the present disclosure relates to methods and systems for processing mixed textile feedstock, including textile garments (used and un-used) and scraps comprising cotton, polyester and other materials, biomass comprising cellulosic materials, wood pulp, and the like and for isolating cellulose and other constituent molecules for use in a variety of downstream applications.
  • the present disclosure relates to methods and systems for treatment of mixed textile feedstock (e.g., mixed cotton and polyester textiles) to isolate cellulose and polyester molecules, separately, and to produce regenerated polymers, fibers, and the like from the isolated cellulose and polyester molecules. Recycling and regeneration of textiles is described in detail and provides significant social, environmental and economic benefits.
  • Cotton clothing is estimated to represent about 35% of the total apparel market.
  • Cotton fibers are composed of cellulose, a naturally occurring polymer found in all plants, wood, and natural fibers. Cotton fibers are harvested from cotton plants and consist of long, interwoven chains of cellulose polymers. These fibers are spun into thread or yarn, dyed, and ultimately woven, knit, and assembled into textiles. Natural fibers, including cotton, have a generally high and variable raw material cost due, in part, to natural disasters and climate unpredictability, regional socio-economic and political instability, human rights issues, and resource requirements.
  • Cotton has been recycled to provide raw material for paper pulping plants. Reprocessing methods that convert used cotton into rags, mattress ticking, seat stuffing, insulating materials, and the like are also available, but these processing methods have been adopted in limited applications because the value of the converted material is relatively low.
  • rayon fibers are manufactured from wood pulp using the viscose process.
  • purified cellulose is solubilized and then converted or regenerated into cellulose fiber.
  • This process requires steeping, pressing, shredding, aging, xanthanation, dissolving, ripening, filtering, degasing, spinning, drawing and washing.
  • This process is time sensitive, requires multiple chemical treatments, produces lignin and other waste from unusable wood material and is, at best, a semi-continuous manufacturing process.
  • Most recycled textile resources contain mixed textile compositions and, particularly, many textile feedstocks and resources comprise both cotton and polyester in substantial proportions.
  • the present disclosure is directed to providing systems and methods for processing mixed textile feedstocks, such as recycled fabric, fabric scraps and materials, many of which would otherwise be wasted or used to produce low value products, to isolate their constituent cellulosic and polyester polymeric structures.
  • Implementation of the disclosed processing schemes with a variety of garment/fabric feedstock materials may produce regenerated fibers and textile products having improved and/or customize-able properties using processes having low environmental impacts.
  • Methods and systems of the present disclosure relate to processing of mixed textile feedstocks including, for example, postconsumer mixed cellulosic waste, cellulose- and polyester-containing textiles and garments (e.g., recycled or used or waste textiles and garments), and the like, to produce isolated cellulose and/or polyester polymers for use in downstream processing applications.
  • mixed textile feedstocks comprising discarded garments and/or scrap fabric materials are used as raw feed, and processing produces isolated cellulose and/or polyester polymers that can be further processed and extruded to provide regenerated cellulosic and/or polyester fibers having improved and/or customize-able properties for use in textile industries or for other purposes.
  • a multi-stage process is described, generally incorporating one or more pretreatment stages providing removal of contaminants and preparation of mixed textile feedstocks, followed by pulping and/or molecular separation of the primary constituents, e.g., cellulose or polyester polymers. Different constituents may be isolated, sequentially, using appropriate pulping and/or molecular separation techniques.
  • the pretreatment and pulping processes may be carried out in a continuous, semi-continuous or batch system.
  • the pretreatment and pulping processes may be carried out in one or more closed reaction vessel(s), and processing reagents may be recovered and re-used or processed for other uses.
  • pretreatment processing stages are described and may be used alone or in combination to remove non-cellulosic and/or non-polyester constituents of the mixed textile feed and to prepare the primary textile constituents for pulping and dissolution.
  • Pretreatment of the mixed textile feedstock may be followed by at least one cellulose pulping or dissolution stage that promotes the molecular separation and isolation of cellulose polymers, such as by disrupting intermolecular hydrogen bonds.
  • cellulosic polymers isolated during the pulping and/or dissolution stage(s) are substantially thermoplastic and are moldable when energy (e.g., heat below the char point) is introduced to the system.
  • Polyester constituents and other constituents of mixed textile feedstocks may be isolated in one or more pulping/dissolution stages, either prior or subsequent to a cellulose pulping or dissolution stage.
  • the predominant component of a mixed textile feed e.g., cotton or polyester
  • the non- dissolved product of the first pulping stage is then treated in an appropriate pulping or dissolution stage to recover one or more additional constituents.
  • Isolated cellulose and polyester (and other polymeric) materials produced using the processes described herein may be used in a variety of downstream applications, as described in more detail below.
  • isolated cellulose and polyester components may be extruded to form regenerated cellulosic and polyester fibers.
  • isolated cellulose polymers may be regenerated to provide longer chain polymers and fibers (or polymers and fibers having other desirable characteristics different from the characteristics of the cellulose-containing feedstock) that are useful in various industrial processes, including textile production.
  • processing steps having generally low environmental impacts are preferred.
  • methods and systems of the present disclosure provide a closed-loop garment recycling process that transforms reclaimed garments and textiles into high-quality regenerated fibers for use in creating new textiles, apparel, and other fiber-based products.
  • Used and waste garment collection, sorting, transport and processing may all be involved as part of a closed loop process.
  • Retail enterprises and others may serve as collection stations and may offer incentives, rewards, or the like for donations. Further garment processing may take place at the donation site or at one or more remote sites. Cotton, cotton-like regenerated fabrics, rayon and other fibers may be produced using the reclaimed garments and textiles.
  • Fig. 1 illustrates an exemplary schematic flow diagram outlining process steps as disclosed herein for processing blended textile input to produce liquefied cellulosic and polyester output.
  • Fig. 2 illustrates an exemplary schematic flow diagram outlining process steps as disclosed herein for converting blended textile input comprising predominantly cellulose- containing materials to liquefied cellulose and liquefied polyester suitable for use in a variety of downstream applications.
  • Fig. 3 illustrates an exemplary schematic flow diagram outlining process steps as disclosed herein for converting blended textile input comprising predominantly polyester- containing materials to liquefied polyester and liquefied cellulose suitable for use in a variety of downstream applications.
  • Figs. 4A and 4B schematically illustrate the processing of liquefied cellulose and liquefied polyester, respectively, to produce regenerated cellulosic fiber and regenerated polyester fiber, respectively.
  • Fig. 5 illustrates an exemplary schematic flow diagram outlining process steps as disclosed herein for converting cellulose-containing materials to regenerated cellulosic fiber incorporating a high temperature aqueous or supercritical carbon dioxide pretreatment step and incorporating optional additional treatment steps.
  • Fig. 6 illustrates an exemplary schematic flow diagram outlining process steps as disclosed herein for converting cellulose-containing materials to regenerated cellulosic fiber incorporating a combination of pretreatment steps.
  • Fig. 7 illustrates an exemplary schematic flow diagram outlining process steps as disclosed herein for converting cellulose-containing materials to regenerated cellulosic fiber incorporating another combination of pretreatment steps.
  • Fig. 8 illustrates an exemplary schematic flow diagram outlining process steps as disclosed herein for converting cellulose-containing materials to regenerated cellulosic fiber incorporating another combination of pretreatment steps.
  • Fig. 9 illustrates an exemplary schematic flow diagram outlining process steps as disclosed herein for converting cellulose-containing materials to regenerated cellulosic fiber incorporating yet another combination of pretreatment steps.
  • Fig. 10 illustrates an exemplary schematic flow diagram illustrating additional features of dissolving stage.
  • Fig. 11 illustrates an exemplary schematic flow diagram illustrating dissolving solvents and the production of regenerated cellulosic fiber.
  • systems and methods disclosed herein process mixed textile feedstock materials to produce isolated cellulosic and polyester polymers suitable for use in downstream processing and in a variety of downstream applications and production pathways.
  • Mixed textile feedstock materials that are useful as raw materials for this process include a wide range of materials, such as cellulose- and polyester-containing postconsumer waste, industrial and post-industrial fiber and fabric scraps, unworn or worn and discarded cotton-containing and polyester-containing apparel, and the like.
  • the mixed textile feedstock preferably undergoes at least one pretreatment stage (and optionally multiple pretreatment stages) and at least one pulping or dissolution stage, sequentially, to isolate each of the predominant constituent components.
  • a first pulping or dissolution stage following pretreatment isolates the predominant constituent (e.g., cotton or polyester), and the undissolved material remaining after the first pulping stage undergoes a second (different) pulping or dissolution stage to isolate another predominant constituent, thereby producing isolated cellulose and polyester molecules in separate product streams, each product stream being suitable for use in various different downstream application pathways.
  • the predominant constituent e.g., cotton or polyester
  • a second pulping or dissolution stage to isolate another predominant constituent, thereby producing isolated cellulose and polyester molecules in separate product streams, each product stream being suitable for use in various different downstream application pathways.
  • the raw mixed textile feed material may be substantially homogeneous or at least somewhat heterogeneous (e.g., pre- or post-consumer waste, scrap textile fiber and fabric, cotton- and polyester- and mixed cotton/polyester-containing fabrics, etc.).
  • used clothing collection and sorting may be accomplished via clothing retailers, manufacturers, recyclers, and various other organizations, providing access to large volumes of used, cellulose-containing garments and scrap materials that would otherwise be discarded.
  • optional sorting and removal of undesired components may be carried out prior to pretreatment of the mixed textile feedstock.
  • reclaimed material e.g., garments and textiles
  • cellulosic content e.g., reclaimed materials may be separated into groups having different cellulosic contents, such as >90% or >80% or >70% or >50%, or other cellulosic contents, and less than 50% cellulosic content.
  • Reclaimed fabric material having other fiber contents and compositions e.g., having various polyester contents, may also be sorted and separated.
  • Reclaimed textile materials may also be sorted by composition, such as separating cotton-wool blends, cotton-polyester blends, cotton-elastane blends, cotton-spandex blends, and the like.
  • Fabric feedstocks such as reclaimed garments and textiles typically incorporate a variety of dyes and/or chemical finishes and may be contaminated with other materials, such as dirt, grease, and the like.
  • Raw textile feedstock (optionally treated to remove non-textile- containing materials, and optionally sized) is typically processed in one or more pre-treatment stage(s) to remove dyes, finishes, contaminants (oils, grease, etc.) and the like from the feedstock.
  • Feedstocks including textile materials may optionally be mechanically treated to provide smaller sized, or more uniformly sized, feedstock.
  • the fabric feedstock may be sized if desired, such as by shredding, to provide a sized feedstock having a fragmented, high surface area for fiber pulping.
  • Feedstock sizing is typically accomplished using mechanical cutting, shredding, or other mechanical size reduction techniques. Processing to remove non- fabric components, such as buttons, zippers, fasteners, and the like may take place, if desired, prior to and/or following pretreatment.
  • pre-treatment stages are described below, and various combinations of pretreatment stages may provide benefit, depending on the nature of the textile feedstock. Depending on the properties and composition of the mixed textile feedstock, one or more of the pretreatments may be used, alone or in combination with other pretreatments.
  • pretreatment stages are described below, and several advantageous pre-treatment combinations are also described. It will be appreciated that additional pre-treatments may be used in combination with the pre-treatments described, and that various specific combinations other than those specifically illustrated and described may be used.
  • Fig. 1 shows a schematic flow diagram illustrating the processing of a blended textile input according to methods described herein.
  • blended textile input is separated into cotton-heavy and polyester-heavy blends during or following one or more sorting and pretreatment step(s).
  • the constituent cotton and polyester polymers in each of the separated stages are dissolved and isolated to produce "liquefied" cellulose (i.e., isolated cellulose molecules) from the cotton-heavy feedstock and "liquefied" polyester (i.e., isolated polyester molecules) from the polyester-heavy feedstock.
  • These isolated cellulosic and polyester materials may be extruded into regenerated fibers, as desired, or used for other downstream applications.
  • the undissolved, non-cellulosic constituents remaining after dissolution of the cotton-heavy blend feedstock may be treated for dissolution of polyester to produce liquefied polyester.
  • the undissolved, non-polyester constituents remaining after dissolution of the polyester-heavy blend feedstock may be treated for dissolution of cellulose to produce liquefied cellulose.
  • Undissolved components such as other fibers, zippers, buttons, and the like, may be collected and re-used or discarded. Additional processing details, conditions and reagents for pretreatment and pulping/dissolution stages are described below.
  • Fig. 2 illustrates an exemplary overall process flow diagram for treating predominantly cellulosic blended textile input to produce isolated cellulose polymers, identified in Fig. 2as "Liquefied Cellulose,” and isolated polyester polymers, identified in Fig. 2 as “Liquefied Polyester.”
  • the liquefied cellulose and polyester products may be suitable for use in a variety of downstream applications, such as fiber production (e.g., textiles, technical fibers and geo-textiles), production of other extrusion and/or constructional manufacturing methods (e.g., 3D printing media, membranes, injection molding media), use as a chemical feedstock for production of biofuels, lubricants and other chemical manufacturing, and for use as food additives, in films, coating, fillers, membranes, packaging, construction materials, non-woven materials, and the like.
  • fiber production e.g., textiles, technical fibers and geo-textiles
  • production of other extrusion and/or constructional manufacturing methods e.g., 3D printing media, membranes
  • Fig. 3 illustrates an exemplary overall process flow diagram for treating predominantly polyester blended textile feed materials to produce liquefied polyester and liquefied cellulosic components suitable for fiber extrusion and including additional processing stages for production of regenerated fibers.
  • mixed textile feed materials may undergo optional feedstock preparation stages, such as feedstock sorting and/or removal of non-cellulosic components.
  • the mixed textile feedstock then undergoes at least one pretreatment stage, followed by a first pulping and/or dissolution stage to isolate one constituent of the pretreated mixed feedstock (e.g., cellulose or polyester) and a second pulping and/or dissolution stage to isolate another constituent of the pretreated mixed feedstock. Additional pulping and/or dissolution stages may be implemented to isolate additional constituents.
  • pretreatment stages are described below and are illustrated in the accompanying diagrams. Depending on the composition of the mixed textile feedstock and desired attributes of the desired product, one or more than one of the pretreatment stages may be used alone or in combination with other pretreatment stages. Specific combinations of pretreatments that may be useful in particular applications are described in greater detail below with reference to Figs. 5-9. Each of the pretreatment stages is described in more detail below.
  • methods disclosed herein provide pretreatment of mixed textile feed materials using a high temperature aqueous washing process.
  • This pretreatment stage is particularly useful for pretreatment of mixed textile feed materials comprising recycled garments and may facilitate removal of contaminants such as soils, deodorants, lanolin, silicone and cationic softeners from the textile feedstock, as well as stripping various fabric treatments, such as optical brighteners, moisture wicking enhancers, and the like, from the feed material.
  • Aqueous media maintained at a temperature above 100°C, optionally above the boiling point of the aqueous media, generally above 120° C, often between 120° C and 170° C, sometimes between 130°C and 150°C, and up to 200° C, may be used.
  • the high temperature aqueous washing pretreatment stage is conducted in a closed vessel batch system with circulation or agitation or mixing of the hot aqueous media.
  • Pressure conditions in a closed vessel system may range from about 100 kPa to about 2000 kPa, depending on the temperature of the aqueous media, with higher pressure conditions accompanying higher temperature media.
  • Aqueous media used in a high temperature pretreatment stage may comprise water alone, or it may comprise an aqueous solution having one or more additives.
  • the aqueous media may comprise water enriched with ozone.
  • the aqueous media may comprise water enriched with oxidative agents such as hydrogen peroxide or sodium perborate.
  • surfactants e.g., Sodium stearate, Fatty Alcohols ,4-(5-Dodecyl) benzenesulfonate, Alcohol ethoxylates and the like
  • various hydroxide compositions e.g., Ca, Mg, Na, K, and Li hydroxides
  • the high temperature aqueous washing stage incorporates an aqueous solution comprising NaOH at a concentration of from about 1% to about 15%, at a pH in excess of about 11, and in some embodiments in excess of about 12. Residence times are sufficient to substantially remove impurities from the mixed textile feedstock.
  • the aqueous wash solution may be evacuated following a suitable residence time.
  • multiple aqueous washing stages may be implemented, using the same or different aqueous solutions, all at high temperature and pressure conditions.
  • Optional rinsing of the solids with an aqueous solution may be implemented following evacuation of the wash solution. Rinsing may take place at ambient temperatures and pressures, with optional agitation and mixing, and the rinse solution is removed following a suitable residence time.
  • Treated solids may undergo one or more additional pretreatment stage(s) or may be further processed in one or more pulping and/or dissolution stage(s).
  • a water-less and/or "non-toxic" pretreatment may be used to remove contaminants such as dyes, finishes, surface impurities and other contaminants from mixed textile feed materials.
  • textile feed material may be introduced to a closed and pressurized chamber, where the feed material contacts supercritical carbon dioxide, alone or in combination with additional reagent(s).
  • the supercritical C02 may be enriched with ozone.
  • the supercritical C02 may enriched with oxidative agents such as hydrogen peroxide or sodium perborate.
  • surfactants e.g., Sodium stearate, Fatty Alcohols, 4-(5-Dodecyl) benzenesulfonate, Alcohol ethoxylates and the like
  • surfactants may be mixed and circulated with the supercritical C02 in a pretreatment stage.
  • supercritical carbon dioxide containing dissolved contaminants is withdrawn to a separator, where the carbon dioxide may be decompressed and returned to a gaseous state, while the contaminants may be collected and removed.
  • the gaseous carbon dioxide may be recycled in a closed loop process and re-used for additional pretreatment cycles.
  • Treated solids may undergo one or more additional pretreatment stage(s) or may be further processed in one or more pulping and/or dissolution stage(s).
  • mixed textile feedstocks and/or cellulose-containing treated solids are treated, prior to pulping or dissolution, with a high temperature (>320°C), high pressure (>2.5 Mps) aqueous treatment, in a closed and substantially rigid reaction vessel.
  • This pretreatment stage promotes breakdown of the crystalline structure of cellulose and facilitates modification of cellulosic constituents to an amorphous, non- or less-crystalline structure that is more amenable to pulping and/or dissolution.
  • a pretreatment stage involves exposing the textile feed material (and/or cellulose-containing treated solids) to a "bleaching" agent, such as an oxidative or reducing agent, typically in an aqueous solution, at an oxidative/reducing agent concentration and for a residence time sufficient to remove materials such as dyes, finishes, and other contaminants from the cellulosic feedstock.
  • a "bleaching" agent such as an oxidative or reducing agent
  • Suitable oxidative and/or reducing agents include, for example, peroxide compositions (e.g., H202, Na202) and perborate (e.g., NaB03) compositions.
  • Additional oxidative and/or reducing agents that may be used in pretreatment stages as described herein include one or more of the following compositions: per carbonate compositions; sodium carbonate; per acetic acid compositions; potassium permanganate; persulfate compositions; ozone; sodium chloride; chlorine dioxide; calcium oxychloride, sodium hypochlorite; calcium hypochlorite; lithium hypochlorite; cloramine; isocynual trichloride; Sulphur dioxide; sodium hydrosulfite; sulphoxylates; acidic sodium sulphite; sodium bosulphite; sodium meta bisulphite; TAED (tetra-acetyl-ethylene-diamine); and sodium hydrosulfite.
  • per carbonate compositions sodium carbonate
  • per acetic acid compositions potassium permanganate
  • persulfate compositions ozone
  • sodium chloride chlorine dioxide
  • calcium oxychloride sodium hypochlorite
  • calcium hypochlorite
  • bleaching agent treatment may involve treatment in an aqueous solution of calcium hypochloride (bleach powder) or sodium hypochlorite (NaOCl) in combination with sodium carbonate (soda ash) at a pH in excess of 8 and, in some embodiments, at a pH in excess of 9. Agitation or mixing of the materials in the bleaching agent pretreatment stage may be provided, and treatment with an oxidative and/or reducing agent may take place in a closed reaction vessel.
  • the bleaching agent solution may be evacuated following a suitable residence time and optional rinsing of the solids with an aqueous solution may be implemented. Aqueous rinsing may take place at ambient temperatures, with the rinse solution removed following a suitable residence time.
  • the bleaching agent may be neutralized, following this treatment, by introduction of a weak acid such as hydrogen peroxide.
  • a weak acid such as hydrogen peroxide.
  • multiple bleaching agent treatment cycles may be implemented using different oxidative or reducing reagents to treat the solids at different concentrations, pH conditions, temperature and/or residence times, as appropriate. Recycling and regeneration of the oxidative or reducing agent(s) may be incorporated in the process, as is known in the art.
  • Introduction of other weak acids may be effective to reduce the pH of the treated, cellulose-containing solids, if desired, following optional rinsing steps.
  • methods disclosed herein provide pretreatment of textile feed materials (and/or cellulose-containing treated solids) by exposure to aqueous media containing one or more organic solvents.
  • Suitable organic solvents may be selected from the group consisting of: acetic acid; acetone; acetonitrile; benzene; 1-butanol; 2-butanol; 2- butanone; /-butyl alcohol; carbon tetrachloride; chlorobenzene; chloroform; cyclohexane, 1,2-dichloroethane; di ethylene glycol; diethyl ether; diglyme (di ethylene glycol dimethyl ether); 1,2-dimethoxy-ethane (glyme, DME); dimethyl formamide (DMF); dimethyl sulfoxide (DMSO); 1,4-dioxane; ethanol, ethyl acetate; ethylene glycol; glycerin; heptane; hexamethylphosphoramide
  • methods disclosed herein may optionally employ enzymatic treatment to shorten cellulose molecules, increase cellulose solubility and/or reduce reaction times in subsequent treatment stages.
  • Suitable enzymes may include endogluconases (e.g., Cel 5A, Cel 7B, Cel 12A, Cel 45, Cel 61A); Cellobiohydrolases (e.g., Cel 6A, Cel 7A); LPMO/GH61; cellulases; and the like.
  • temperatures of from about 30° to 90 °C, pH between about 4 to about 9 and dwell times of from about 20 min to 48 hours may be suitable for enzymatic treatment.
  • Enzymatic treatment(s) involving xylanases, alkaline pectinases, lipases, and/or esterases may also be used for feedstock pretreatment prior to pulping.
  • feedstock may be treated using enzymatic cultures containing biological organisms (fungi, bacteria, etc.) that secrete cellulolytic enzymes (e.g., cellulases).
  • Enzyme cultures such as Trichoderma Reesei, Trichoderma viride, Penicillium janthinellum, Halorhabdusutahensis, A Niger, Humicola, and mixtures of such enzyme-producing cultures, are suitable.
  • Mechanical treatments such as pulverization and/or emulsification treatment(s) may be implemented following enzymatic treatment.
  • a swelling agent such as an ionic liquid
  • treatment with a swelling agent may be preceded by or implemented in combination with one or more other pretreatment stage(s).
  • Ionic liquids may comprise hydroxides, such as Ca, Mg, Na, K, and/or Li hydroxides, and/or Mg salts.
  • Swelling agents suitable for use as reagents in a pretreatment stage may alternatively or additionally comprise one or more of the following reagents: [AMIM]C1 1- Allyl-3-methylimidazolium chloride; [BzPy]Cl Benzylpyridinium chloride; [BMIM]Ace l-Butyl-3-methylimidazolium acesulphamate; [BMIM]DBP l-Butyl-3- methylimidazolium dibutylphosphate; [BMIM]C1 l-Butyl-3-methylimidazolium chloride; [BMIM]PF6 l-Butyl-3-methylimidazolium hexafluorophosphate; [BMIM]BF4 1-Butyl- 3-methylimidazolium tetrafluoroborate; [BMPy]Cl l-Butyl-3-methylpyridinium chloride; [DBNH]AcO l,8-Diazabicyclo[5.4.0]
  • textile feed materials may be treated with an ionic solution such as an aqueous solution comprising Ca, Mg, Na, K, and/or Li hydroxides, followed by exposure to a sodium hydrosulfite (NaaSaOzt) reducing agent and/or a bleaching agent such as peroxide, perborate, persulfate, chlorine dioxide and sodium or calcium hypochlorite.
  • an ionic solution such as an aqueous solution comprising Ca, Mg, Na, K, and/or Li hydroxides
  • a sodium hydrosulfite (NaaSaOzt) reducing agent and/or a bleaching agent such as peroxide, perborate, persulfate, chlorine dioxide and sodium or calcium hypochlorite.
  • Ba sodium hydrosulfite
  • bleaching agent such as peroxide, perborate, persulfate, chlorine dioxide and sodium or calcium hypochlorite.
  • Bromium (Br) may be used as a catalyst during this treatment.
  • Treatment with swelling agents such as ionic liquids may be achieved using high temperature or cooler aqueous wash media.
  • treatment with a swelling agent e.g., an ionic liquid
  • a swelling agent e.g., an ionic liquid
  • the treatment may be carried out at an acidic pH, typically at a pH less than 6, and in some embodiments at a pH less than 5.
  • the proportion of cellulose- containing feed materials (and/or cellulose-containing treated solids) in the ionic solution is from about 2% to about 40%; in some embodiments, the proportion of cellulose-containing feed materials (and/or cellulose-containing treated solids) in the ionic solution is from about 5% to about 25%.
  • Pretreatment of textile feedstock material may implement any of these pretreatment processes, singly or in combination with one or more other pretreatment processes.
  • carrying out elevated temperature aqueous pretreatment in a closed vessel is preferred, alone or in combination with other pretreatment stages, prior to (separate) pulping and dissolution of cellulose and polyester polymers.
  • carrying out elevated temperature aqueous pretreatment with the use of ozone enrichment, oxidative agents and/or surfactants is preferred, alone or in combination with other pretreatment stages, prior to (separate) pulping of textile constituents.
  • treatment in ionic solution followed by exposure to a reducing and/or bleaching agent is a preferred textile pretreatment step, preferably in combination with a washing step.
  • pretreatment involves elevated temperature aqueous pretreatment, followed by ionic pretreatment, followed by enzymatic pretreatment.
  • one or more of the pretreatment stages, or all pretreatment stages are carried out a pH of at least about 9.
  • one or more of the pretreatment stages, of all of the pretreatment stages are carried out at a pH of at least about 10.
  • Pretreatment preferably takes place in a closed vessel and, in batch treatment schemes, one or more pretreatment reagents may be introduced to and withdrawn from a closed vessel during various pretreatment stages, with or without intermediate rinsing or washing stages.
  • the vessel may be provided in the form of a rotating cylinder with a pressurized hull (housing) capable of withstanding pressures in the range of from 1000 - 5000 kPa, having inlet and outlet ports, pH and rpm control features, and having liquid agitation or circulation features.
  • the inner reaction vessel surfaces may comprise anticorrosive metal(s) capable of withstanding concentrated acidic and alkali solutions. In some processes, both pretreatment and pulping may take place in the same vessel.
  • Figs. 5-9. Each of these flow diagrams describes different pretreatment combinations for cellulose-containing feed materials.
  • These pretreatment combinations may also be used with mixed textile feedstocks, followed by molecular isolation and separation of cellulose, polyester and other constituent polymers in (separate) pulping or dissolution stages.
  • Cellulose polymers may be separated from the cellulose pulping stage, such as by filtration, and regenerated cellulosic fibers may be extruded, such as in connection with a precipitation bath (e.g., an acid bath).
  • Polyester fibers may be separated from a polyester pulping stage and processed to form regenerated polyester fibers. Extruded fibers may be designed and parameters changed, depending on the type, character and physical attributes of the fibers desired. Drying and winding produces regenerated fibers.
  • Fig. 2 illustrates treatment of blended textile input comprising predominantly cellulosic content materials (with optional sorting and removal of non-cellulosic and non- polyester components) using one or more of the pretreatment stages described above.
  • Pretreatment is followed by a cellulose dissolving/pulping stage in which cellulose molecules are "dissolved” and isolated from other constituents.
  • the "liquefied” cellulose is separated by filtration (or another separation technique) and used in downstream application(s) to produce fiber, other extrusion products, chemicals, additives, membranes, or the like.
  • Non- cellulosic components e.g., polyester constituents
  • the isolated polyester may, similarly, be used to produce regenerated fiber or in other application pathways.
  • Fig. 3 illustrates treatment of blended textile input comprising predominantly polyester content materials (with optional sorting and removal of non-cellulosic and non- polyester components) using one or more of the pretreatment stages described above. Pretreatment is followed by a polyester dissolving/pulping stage in which polyester molecules are "dissolved” and isolated from other constituents. The "liquefied" polyester constituents are separated by filtration (or another separation technique) and used in downstream application(s) to produce fiber, other extrusion products, chemicals, additives, membranes, or the like.
  • Cellulosic components are separated from the polyester dissolving/pulping stage and treated in a separate cellulosic dissolving/pulping stage to produce isolated, "liquefied" cellulose.
  • the isolated polyester may, similarly, be used to produce regenerated fiber or in other application pathways.
  • Figs. 4A and 4B show exemplary schematic flow diagrams illustrating the treatment of liquefied cellulose and liquefied polyester, respectively, to produce regenerated cellulosic fiber and regenerated polyester fiber, respectively.
  • Fig. 5 illustrates treatment of cellulose-containing materials (with optional sorting and removal of non-cellulosic components) using a high temperature aqueous wash or supercritical carbon dioxide pretreatment stage in combination with ozone enrichment and/or oxidative agent(s) and/or surfactant(s).
  • the cellulosic solids may optionally be treated with swelling agents (as described above), and/or with organic solvents (again, as described above).
  • These treatment stages may be done at elevated temperatures or in cooler aqueous media.
  • Fig. 6 illustrates treatment of cellulose-containing materials (with optional sorting and removal of non-cellulosic components) using a high temperature aqueous wash or supercritical carbon dioxide pretreatment stage in combination with oxidative agent(s) and/or surfactant(s).
  • the cellulosic solids may optionally undergo enzymatic treatment as described above.
  • the cellulosic solids may subsequently be exposed to swelling agents such as ionic liquids (e.g., NaOH) prior to a pulping or dissolution stage.
  • Fig. 7 illustrates treatment of cellulose-containing materials (with optional sorting and removal of non-cellulosic components) using a high temperature aqueous wash or supercritical carbon dioxide pretreatment stage in combination with oxidative agent(s) and/or surfactant(s).
  • the cellulosic solids may optionally be exposed to swelling agents such as ionic liquids (e.g., NaOH), followed by enzymatic treatment as described above prior to a pulping or dissolution stage.
  • swelling agents such as ionic liquids (e.g., NaOH)
  • Fig. 8 illustrates treatment of cellulose-containing materials (with optional sorting and removal of non-cellulosic components) using a high temperature aqueous wash or supercritical carbon dioxide pretreatment stage in combination with optional ozone enrichment and/or oxidative agent(s) and/or surfactant(s).
  • the cellulosic solids may optionally be exposed to swelling agents such as ionic liquids (e.g., NaOH), followed by exposure to bleaching agents and/or reducing agents and/or an optional enzyme treatment, all as described above, prior to a pulping or dissolution stage.
  • swelling agents such as ionic liquids (e.g., NaOH)
  • Fig. 9 illustrates treatment of cellulose-containing materials (with optional sorting and removal of non-cellulosic components) using a high temperature aqueous wash or supercritical carbon dioxide pretreatment stage in combination with optional ozone enrichment and/or oxidative agent(s) and/or surfactant(s).
  • the cellulosic solids may optionally undergo a high- temperature, high-pressure aqueous treatment stage, as described above, to promote destruction of the cellulosic crystalline structure and favor conversion of cellulosic polymers to an amorphous phase.
  • the cellulosic solids may be exposed to enzyme treatment, as described above, prior to a pulping or dissolution stage.
  • Pre-treated mixed constituent solids are subjected to at least two pulping or dissolving stages, in which the solids are treated with pulping reagents to promote molecular separation of cellulose and other constituents, such as polyester, from the solids.
  • Pulping to isolate the highest content constituent e.g., cellulose, polyester, etc.
  • Pulping to isolate cellulose polymers involves the destruction of intermolecular hydrogen bonds and other non-covalent bonds, isolating cellulose polymers from cellulose-containing solids in a dissolved or "liquefied" cellulose state.
  • the number of intermolecular hydrogen bonds present in the cellulose polymers is reduced by at least 20% in the fiber pulping stage; in some embodiments the number of intermolecular hydrogen bonds present in the cellulose polymers is reduced by at least 50% in the fiber pulping stage; in yet other embodiments, the number of intermolecular hydrogen bonds present in the cellulose polymers is reduced by at least 70% in the fiber pulping stage.
  • the viscosity of pulped cellulose, following the pulping treatment, is generally from about from 0.2 to as high as 900 cP, often from about 0.5 to about 50 cP. Solids remaining following isolation (e.g., dissolution) of cellulose, may be treated to isolate other constituents (e.g., polyester).
  • pulping techniques and pulping chemistries for isolating cellulose are available, and one or more of the pretreatment stages described above may be used with a variety of known pulping reagents, including those described in PCT Int'l Patent Publication WO 2013/124265 Al, the disclosure of which is incorporated herein by reference in its entirety.
  • copper-containing reagents are preferred for use as pulping reagents for isolation of cellulose.
  • Schwiezer's Reagent the chemical complex tetraaminecopper (II) hydroxide - [Cu(NH 3 )4(H 2 O)2] 2+ ) or tetraamminediaquacopper dihydroxide, [Cu(NH 3 )4( H 2 O)2](OH)2 is a preferred pulping agent to isolate and promote molecular separation of cellulose polymers.
  • Schweizer's reagent may be prepared by precipitating copper(II) hydroxide from an aqueous solution of copper sulfate using sodium hydroxide or ammonia, then dissolving the precipitate in a solution of ammonia.
  • a combination of caustic soda, ammonium and cupramonium sulfate may be formulated to provide Schwiezer's Reagent.
  • Solutions comprising copper(II) hydroxide and ammonia may be introduced and used in the cellulose pulping stage to form Schweizer's Reagent according to the following reaction: Cu(OH) 2 + 4 NH 3 + 2 H 2 0 ⁇ [Cu(NH 3 )4(H 2 O) 2 ] 2+ + 2 OH.
  • the copper hydroxide reagent may be manufactured from recycled copper recovered, for example, from electronics and computer component waste materials. Copper hydroxide is readily made from metallic copper by the electrolysis of water using copper anodes.
  • Ammonia may be manufactured by an innovative use of the Haber-Bosch process (3 H 2 + N 2 ⁇ 2NH 3 ), capturing hydrogen from organic wastes and combining it with atmospheric nitrogen.
  • This method may produce ammonia at low cost and eliminate greenhouse gas emissions from organic waste feedstock.
  • all or substantially all of the materials used in the fiber pulping process described herein may be sourced as waste products, resulting in minimal or no use of nonrenewable resources.
  • FeTNa iron tartrate complex solvents
  • FeTNa solutions may be prepared according to the procedure published by Seger et al. (B. Seger, et al., Carbohydrate Polymers 31 (1996) 105.) FeTNa solutions are prepared and stored while protecting them from light.
  • the FeTNa complex may be prepared, for example, by dissolving sodium tartrate dehydrate (Alfa Assar, Cat. # 16187) in deionized water, stirring and optionally heating.
  • iron nitrate nonahydrate Alfa Aesar, Cat. # 122266
  • the solution is then cooled to 10-15°C to prevent precipitation of the iron complex.
  • 12 M sodium hydroxide solution is slowly added to the tartrate-ferric acid under controlled conditions to prevent the temperature from rising over 20°C.
  • the solution color shifts from reddish-brown to yellowish-green, signifying the formation of the FeTNa complex.
  • the remaining sodium hydroxide may be added without regard to temperature.
  • Sodium tartrate is added at the end to ensure long- term stability of the solution.
  • Pulping conditions using a FeTNa pulping reagent are generally basic and may be carried out at pH above 12, or above 13, or at a pH of about 14 in a closed reaction vessel. Reactions carried out using FeTNa pulping reagent at a pH of 14 in a closed reaction vessel kept at 4°C successfully dissolved cotton feedstock. Carrying out the pulping reaction in an inert atmosphere is generally preferred, and circulating an inert gas such as argon through the pulping solution prior to and during addition of preheated feedstock may improve dissolution rates and/or yields.
  • an inert gas such as argon
  • zinc-containing reagents such as Zincoxen solutions may be used as cellulose pulping reagents.
  • the active ingredients of the zincoxen solution are zinc oxide (ZnO) and EDA.
  • Zincoxen solutions may be prepared according to the procedures published by Shenouda and Happey (S.G. Shenouda and F. Happey, European Polymer Journal 12 (1975) 289) or Saxena, et al. (V.P Saxesa, et al., Journal of Applied Polymer Science 7 (1963) 181). Ethylenediamene-water solutions are chilled to 0°C followed by stirring in zinc oxide powder. Continuous stirring for 72 hours while maintaining the temperature at 0°C produces a suitable Zincoxen solution.
  • Pulping conditions using a Zincoxen pulping reagent are generally basic and may be carried out at pH above 12, or above 13, or at a pH of about 14 in a closed reaction vessel.
  • residence times of up to 4 - 48 hours in the pulping stage are suitable to dissolve and promote molecular separation of cellulose molecules present in the treated cellulose-containing feedstock.
  • the pulping stage takes place in a closed chamber and an inert gas, such as nitrogen or argon, is introduced in the airspace to inhibit or prevent oxidation of pulping solution constituents.
  • Oxygen-containing gases may be substantially evacuated from the pulping stage.
  • agitation and/or mixing of the pulping mixture may be provided; in some embodiments, an inert gas, such as nitrogen or argon, may be bubbled through the pulping mixture prior to and/or during pulping.
  • Fig. 10 illustrates a cellulose pulping stage in which pretreated cellulosic-containing material is treated with a dissolving solvent in the pulping stage, wherein the solvent is selected from the group consisting of: ionic liquids; metal alkali system complexes; organic solvents; and other solvents, such as sulfuric acid, xanthogenation; or combinations thereof.
  • Fig. 11 cites exemplary ionic liquids, alkaline metal system complexes, organic solvents, alkaline xanthogenation reagents, and other solvents. A list showing these potential cellulose pulping/dissolution reagents is reproduced below.
  • the following reagents may be used in addition to or alternatively to the exemplary ionic liquids, alkaline metal system complexes, organic solvents, alkaline xanthogenation reagents and other solvents shown on the following list: 1-Ethyl-3-methylimidazolium chloride and 1-Ethyl-3-methylimidazolium ethyl sulfate. In some embodiments, the use of 1-Ethyl-3-methylimidazolium acetate is used.
  • Any of these solvents may be used, alone or in combination, to break hydrogen bonds between cellulose molecules and produce isolated cellulose molecules.
  • Treatment with a cellulose dissolving solvent may be accompanied by one or more of the following: introduction of an inert gas, such as nitrogen or argon (or another noble gas); introduction of mechanical and/or electrical energy; introduction of one or more conditional agents, such as glycerine; and filtration and scraping. Filtration and extrusion may then be carried out using the isolated cellulose molecules to produce cellulose for use in various applications, including in the manufacture of regenerated cellulosic fiber.
  • an inert gas such as nitrogen or argon (or another noble gas)
  • introduction of one or more conditional agents such as glycerine
  • Filtration and extrusion may then be carried out using the isolated cellulose molecules to produce cellulose for use in various applications, including in the manufacture of regenerated cellulosic fiber.
  • the cellulose molecules are substantially isolated and may be fully or partially dissolved to form substantially linear cellulose chains in the pulping stage, depending on the reagent used and the residence time.
  • the pulping solution is filtered, following a suitable residence time, to remove non-cellulosic constituents with the solution and isolate substantially purified cellulose polymers, which are typically suspended in a viscous media. Filtration may involve multiple stages, including an optional centrifugation stage and one or more size exclusion filtration stages. A final filtration stage using pore sizes of 1 micron or less may be employed.
  • the isolated, substantially purified cellulose polymers may be used in a wide range of downstream applications and, in particular applications, are used in fiber production applications to produce regenerated cellulosic fiber.
  • the conditions of the cellulose pulping stage and the composition of the fabric feedstock are important factors in determining whether a cotton-like fiber or rayon is produced form the pulped cellulosic materials in subsequent processing.
  • Full dissolution of the cellulosic fibers is generally desirable for the production of rayon-like fibers, cotton-like fibers and other regenerated cellulosic fibers.
  • Suitable solvent concentrations, reagent to feedstock ratios, residence times, and the like, may be determined using routine experimentation. While Schwiezer's Reagent and the other iron- and zinc-containing pulping reagents described above are suitable pulping solvents for many applications, it will be appreciated that other pulping reagents may be available, or may be developed, and would be suitable for use in the processes described herein.
  • energy is introduced to the pulped solution during and/or following a desired degree of cellulose pulping.
  • mechanical and/or electrical energy such as radio frequency energy
  • suitable filtration, screening and/or size exclusion treatment may be performed, during or following pulping, to remove non-organic materials (e.g., buttons, fasteners, zippers, etc.), as well as impurities and non-cellulosic materials from the fiber pulp solution.
  • Suitable filtration, screening and/or size exclusion treatments will depend on the types and level of contaminants remaining in the fiber pulp solution. Filtration may involve scraping the top and/or bottom of the reaction vessel to remove floating and/or sinking debris; simple size exclusion filtration; and/or gravitation separation or centrifugation to separate solids from the dissolved cellulosic materials. In some embodiments, a cascade of progressively smaller pore size filtration stages may follow preliminary separation by gravitation or centrifugation. Separated by-products may be isolated and purified (if appropriate) for re-sale or distribution to secondary markets.
  • the cellulose pulping solution may be optionally treated with glycerin or glycerol or another agent to impart softness to the texture of the fiber.
  • non-cellulosic constituents of a mixed textile feedstock may be isolated, following pretreatment, in additional pulping/dissolution stages that are carried out prior to or following pulping and dissolution of cellulosic materials.
  • a blended textile feedstock comprising predominantly polyester constituents undergoes optional sorting, pretreatment and removal of non-polyester and non- polyester and non-cellulosic components.
  • the mixed feedstock is then treated in a polyester pulping/dissolution stage to isolate (and "liquefy") polyester molecules. Pulping and isolation of polyester molecules may be accomplished by means of high temperature alkaline hydrolysis techniques in the presence of sodium hydroxide (NaOH) or other highly alkaline reagents.
  • NaOH sodium hydroxide
  • Phase transfer catalysts such as Benzyl Tributyl Ammonium Chloride may be introduced during polyester pulping to accelerate the reaction and improve yields. Isolated, liquefied polyester is separated and may be used in downstream processing, such as for production of regenerated polyester fibers and fabrics. Cellulosic-containing solids not dissolved during the polyester pulping stage may be treated to isolate cellulose molecules using the techniques (including pretreatment and pulping) as described herein.
  • isolated cellulose molecules may be extruded to form regenerated fibers and textile materials.
  • the isolated cellulose molecules are generally filtered or otherwise separated, and may be acidified and processed in a wet extrusion stage to precipitate cellulose fibers and produce cotton fibers, rayon fibers, or a mixture of cotton and rayon fibers.
  • Various acids may be used in this precipitation stage, such as sulfuric, citric or lactic acids.
  • a sulfuric acid bath is used in combination with a wet extrusion process, wherein the viscous cellulose polymer solution is pumped through a spinneret, and the cellulose is precipitated to form fibers as it contacts the acid bath.
  • the extrusion process and/or system may be modified and adjusted to produce fibers having different lengths, diameters, cross-sectional configurations, durability, softness, moisture wicking properties, and the like.
  • the newly formed fibers are stretched and/or blown to produce desired configurations, washed, dried, and cut to the desired length.
  • Closed vat, continuous fiber extrusion techniques may be used. Closed vat systems allow recovery and/or recycling of any produced gases and by-products.
  • Using fiber extrusion techniques is highly advantageous when applied to the regeneration of cellulosic materials to produce cotton and/or rayon fibers, since it allows a high degree of custom design and engineering of cellulosic fibers to achieve targeted comfort and performance characteristics (e.g., fiber length, diameter, cross-sectional shape, durability, softness, moisture wicking, etc.).
  • Naturally grown fibers cannot be produced in desired or specified fiber lengths, diameters, cross-sectional profiles, or the like and cellulosic fibers regenerated using this process may therefore have different, and superior, properties compared to the natural fibers present in the initial recycled fabric feedstock.
  • fiber extrusion may produce fibers having a denier of from about 0.1 to 70 or more denier.
  • fiber extrusion may involve extruding multifilaments having from about 20 to 300 single monofilaments, each having a denier of from about 0.1 to about 2. Extruding fine denier filaments produces woven fabric that feels softer to the touch and is desired in many embodiments.
  • fiber extrusion may additionally involve adding a false twist to the extruded filaments and texturizing them to resemble spun yarn. These treatments may obviate the necessity of using opening and spinning processes to produce yarn from the extruded fibers. Further handling of the fibers may involve cutting the continuous fiber to specific uniform lengths (stapling), missing, opening, carding, drawing, rowing, spinning, etc.
  • waterless dyeing techniques may be used to further reduce the environmental impact of the overall process.
  • Waterless dyeing technologies are available and typically use supercritical carbon dioxide as a solvent and carrier for dyestuff.
  • color treatment of regenerated fibers may involve determining the absorbency of the regenerated fiber and determining the color properties of fibers using spectrophotometric techniques. Color signatures and dye formulations may then be customized according to the specific properties of regenerated fibers to eliminate differences in coloration that may result from different batch qualities.
  • regenerated fibers or yarns may be surface treated (e.g., using a bleaching composition) and then dyed or overprinted using, for example, reactive, direct, pigment, sulfur and/or vat dye types and prints.
  • all fiber regeneration process steps, from garment reclamation to fiber extrusion may be located at a common geographic site (or at nearby sites). For some purposes, it may be desirable to locate different stages of the process at different physical locations. It may be desirable, in some applications, for example, to locate garment reclamation sites in populous areas, while locating other processing facilities and, in particular, the wet extrusion facility, in locations proximate textile processing facilities - e.g. near textile mills and/or garment manufacturing facilities. In some applications, garment reclamation and initial processing may take place at one location and cellulosic pulp may then be shipped or transported to a different location for wet extrusion and other downstream processing (e.g., dying, garment manufacturing, etc.)
  • Regenerated cellulosic fibers e.g., cotton and/or rayon
  • Regenerated cellulosic fibers may be twisted into thread, dyed, bleached, woven into textiles and, ultimately, cut and sewn into garments.
  • low grade natural cotton fibers e.g., low staple length cotton fibers
  • low grade natural cotton fibers may be pulped as described herein, and then acidified and subjected to a wet extrusion process to produce newly formed fibers which may be stretched and/or blown to a desired diameter, cross- sectional profile or the like, washed, dried, and cut to a desired length.
  • low grade (natural and/or recycled) cotton fibers may be regenerated and converted to newly formed, higher value fibers having more desirable properties than those of the original natural and/or recycled cotton fibers.
  • a small scale experiment was conducted to establish feasibility of cellulose pulping and fiber regeneration using shredded cotton garment material as a feedstock.
  • the shredded feedstock material was treated with Schweizer's Reagent to form a dissolved pulping solution, and the pulp solution was acidified by treatment with sulfuric acid. Fibers were regenerated as a result of the acidification.
  • the clumps or threads can be washed free of the solution to show the blue-cast white color of the regenerated fibers. Subsequent analysis will demonstrate whether the regenerated fibers have the structure of cotton or rayon.
  • chemical reaction (1) may be omitted when using copper hydroxide and ammonia reactants to form Schweitzer's reagent as follows: Cu(OH) 2 + 4 NH 3 + 2 H 2 0 ⁇ [Cu(NH 3 )4(H 2 O) 2 ] 2+ + 2 OH.
  • This alternative chemistry does not require filtration (step 5, above) and produces no by-products that require disposal or removal.

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Abstract

Les procédés et les systèmes de la présente invention utilisent une matière première textiles mixtes, qui peut comprendre des vêtements de déchet de consommation, des chutes de tissu et/ou d'autres matériaux textiles sous forme de matière première brute pour produire de la cellulose isolée et d'autres molécules isolées présentant des propriétés recherchées qui peuvent être utilisées dans les industries du vêtement et du textile, et dans d'autres industries. L'invention concerne également un procédé à plusieurs étapes, dans lequel la matière première textiles mixtes est soumise à une ou plusieurs étapes de prétraitement, suivi par au moins deux traitements de défibrage pour isoler les molécules de cellulose et d'autres constituants moléculaires, tels que le polyester. Les molécules de polyester et de cellulose isolées peuvent être utilisées dans toute une gamme d'applications en aval. Dans une application, les molécules de polyester et de cellulose isolées sont extrudées pour fournir des fibres de cellulose régénérées et des fibres de polyester régénérées présentant de bonnes propriétés recherchées (et sélectionnables) qui sont utilisables dans diverses applications industrielles, y compris la production de textiles.
PCT/US2016/044325 2013-04-17 2016-07-27 Procédés et systèmes de traitement de matière première textiles mixtes, isolement des molécules constituantes, et régénération de fibres polyester et cellulosique WO2017019802A1 (fr)

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EP16831317.9A EP3328924A4 (fr) 2015-07-28 2016-07-27 Procédés et systèmes de traitement de matière première textiles mixtes, isolement des molécules constituantes, et régénération de fibres polyester et cellulosique
US17/344,646 US20210340350A1 (en) 2013-04-17 2021-06-10 Methods and systems for processing mixed textile feedstock, isolating constituent molecules, and regenerating cellulosic and polyester fibers
US18/066,119 US20230124761A1 (en) 2013-04-17 2022-12-14 Methods and systems for processing mixed textile feedstock, isolating constituent molecules, and regenerating cellulosic and polyester fibers

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WO2019138092A1 (fr) * 2018-01-15 2019-07-18 Lenzing Aktiengesellschaft Récupération de particules non solubles présentes dans une matière de départ contenant de la cellulose
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WO2019138096A1 (fr) * 2018-01-15 2019-07-18 Lenzing Aktiengesellschaft Codage d'un produit contenant de la cellulose
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CN111655912A (zh) * 2018-01-15 2020-09-11 兰精股份公司 用于再利用含纤维素的纺织材料
CN111655771A (zh) * 2018-01-15 2020-09-11 兰精股份公司 由含纤维素原材料构成的不溶性颗粒的重复使用
CN111868314A (zh) * 2018-01-15 2020-10-30 兰精股份公司 用于莱赛尔法的重复使用的莱赛尔纤维素
US11519104B2 (en) 2018-01-15 2022-12-06 Lenzing Aktiengesellschaft Method of reusing a textile material which comprises cellulose
US11828005B2 (en) 2018-01-15 2023-11-28 Lenzing Aktiengesellschaft Method of producing a chemical pulp from a textile material which comprises cellulose and a molded body from the chemical pulp
CN111655912B (zh) * 2018-01-15 2023-09-15 兰精股份公司 用于再利用含纤维素的纺织材料
TWI723322B (zh) * 2018-01-15 2021-04-01 奧地利商蘭仁股份有限公司 製造纖維素再生物成形體之方法
JP2021511445A (ja) * 2018-01-15 2021-05-06 レンツィング アクツィエンゲゼルシャフト セルロースおよび合成プラスチックを含有する混紡織物を再利用する方法
JP2021511446A (ja) * 2018-01-15 2021-05-06 レンツィング アクツィエンゲゼルシャフト リヨセル法のためのリヨセルセルロースの再使用
JP2021511448A (ja) * 2018-01-15 2021-05-06 レンツィング アクツィエンゲゼルシャフト セルロースに組み込まれたエラステインを含有する成形体および製造方法
EP3511449A1 (fr) * 2018-01-15 2019-07-17 Lenzing Aktiengesellschaft Recyclage de la cellulose lyocell pour procédé lyocell
EP3511451A1 (fr) * 2018-01-15 2019-07-17 Lenzing Aktiengesellschaft Procédé de recyclage d'un produit textile mélangé comportant de la cellulose et de la matière plastique synthétique
TWI721359B (zh) * 2018-01-15 2021-03-11 奧地利商蘭仁股份有限公司 用於再利用具有纖維素和合成塑膠的混合紡織品之方法及再生的纖維素型成形體
US11321658B2 (en) 2018-01-15 2022-05-03 Lenzing Aktiengesellschaft Encoding a cellulose product
EP4234778A3 (fr) * 2018-01-15 2023-09-13 Lenzing Aktiengesellschaft Procédé de recyclage du matériau textile comprenant de la cellulose
CN111868314B (zh) * 2018-01-15 2023-05-16 兰精股份公司 用于莱赛尔法的重复使用的莱赛尔纤维素
CN111655771B (zh) * 2018-01-15 2023-05-12 兰精股份公司 由含纤维素原材料构成的不溶性颗粒的重复使用
US11519100B2 (en) 2018-01-15 2022-12-06 Lenzing Aktiengesellschaft Reusing of lyocell-cellulose for lyocell-methods
CN113242894B (zh) * 2018-12-19 2024-02-27 雷纽赛尔公司 纤维的分离
CN113242894A (zh) * 2018-12-19 2021-08-10 雷纽赛尔公司 纤维的分离
WO2020221932A1 (fr) 2019-05-02 2020-11-05 Worn Again Technologies Limited Procédé de recyclage
GB2583719B (en) * 2019-05-02 2023-05-31 Worn Again Tech Ltd Recycling process
GB2583719A (en) * 2019-05-02 2020-11-11 Worn Again Tech Ltd Recycling process
WO2021115931A1 (fr) * 2019-12-13 2021-06-17 Lenzing Aktiengesellschaft Procédé de récupération de matières premières à partir de déchets textiles mixtes
CN115003879A (zh) * 2020-03-09 2022-09-02 无限纤维有限公司 涤棉混纺物的分离
US11713528B2 (en) 2021-08-31 2023-08-01 Apani Systems Inc. Textile recycling
WO2023104635A1 (fr) * 2021-12-06 2023-06-15 Heiq Materials Ag Procédé de fabrication de fils de cellulose régénérée dérivés de charges de déchets recyclés
CN116655465A (zh) * 2022-02-18 2023-08-29 青岛阿脒诺材料技术有限公司 一种聚酯混纺面料的循环回收利用方法
CN115304681B (zh) * 2022-07-25 2023-08-11 万华化学集团股份有限公司 一种改性醋酸丁酸纤维素的制备方法
CN115304681A (zh) * 2022-07-25 2022-11-08 万华化学集团股份有限公司 一种改性醋酸丁酸纤维素的制备方法
CN115198425B (zh) * 2022-07-28 2023-09-12 安徽省天助纺织科技集团股份有限公司 利用废旧纺织品制造隔热保温面料的方法
CN115198425A (zh) * 2022-07-28 2022-10-18 安徽省天助纺织科技集团股份有限公司 利用废旧纺织品制造隔热保温面料的方法
CN116397450A (zh) * 2023-04-11 2023-07-07 东华大学 黑色废旧棉混纺织物的脱色及制备纤维素溶解浆的方法

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