Recycling of Blended Fabrics for a Circular Economy of Textiles: Separation of Cotton, Polyester, and Elastane Fibers
Abstract
:1. Introduction
- Closed-loop recycling: This involves recycling the material into a nearly identical product.
- Open-loop recycling: This involves recycling the material in a different product category. Figure 4 illustrates the closed-loop and open-loop recycling methods.
- Upcycling: Upcycling is the process of creating a product out of recycled resources that is more valuable than the original.
- Downcycling: In downcycling, the recycled material is less valuable than what was used to make the original item.
2. Textile Fibers and Textile Production
- Weaving: This is a technique for weaving cloth in which long strands are woven over and under one another in a herringbone pattern, parallel to each other.
- Knitting: Knitting is a traditional type of textile production completed by hand with a needle or crochet hook, but many industries today use large knitting machines.
- Braiding: This method of producing textiles involves taking two comparable materials and twisting them into knots according to a predetermined pattern [40].
- Embroidery: Embroidery is important in the textile industry for adding aesthetic value, texture, and customization to fabrics. It involves decorating materials with needle and thread or yarn, either by hand or with machines [40].
- Washing: Everything to clean the fabric from the residues of the previous steps and steps of treatment, most of the time with water and detergents or solvents.
- De-sizing: Removing the sizing chemicals from the warp yarns in fabrics using enzymes, so that they are ready for finishing.
- Scouring: Fatty waxes and greases are removed from natural fibers such as cotton seed and husk using a detergent, base, or solvent.
- Bleaching: Usually done with bleaches; bleaching whitens fabrics to improve absorbency and make coloring easier.
- Mercerizing: Cellulosic fibers are treated to improve their strength, luster, and dyestuff affinity by causing them to swell (e.g., with bases); this can help lower the dyestuff level.
- Carbonizing: vegetable residues such as seed pods are removed from the wool fibers and the contents of the fiber are ‘blackened’ by the application of heat and chemicals (often based on acids) [43].
3. Textile Recycling Methods
3.1. Mechanical Recycling of Textiles
- Cut fabrics: Cut fabrics are pieces of fabric. If cut fabrics are present, the material needs to go through the tearing machine one or numerous times to produce single fibers. These fibers need blending with virgin fibers to re-spin into yarns because of the decline in fiber quality.
- Spinnable fibers: The output fraction consisting of long fibers of sufficient quality to be spun is known as the spinnable fiber fraction.
- Fluff: Although this product still comprises fiber, it cannot be utilized in a spinning process because the fibers are either too short or too twisted. Typically, fluff material is used to make filler items like insulation for the building sector or specialized non-wovens for the automotive sector.
- Filler materials: During certain procedures (such as milling), the fibers break down, resulting in tiny particles rather than fibers. These particles can be employed as reinforcements or fillers in plastics and composites, depending on their size, shape, and composition [48].
3.2. Chemical Processes for Textile Recycling
3.3. Biological/Enzyme-Based Processes for Textile Recycling
4. Separating Cotton from Polyester in Blended Textiles
- 50% polyester, 50% cotton: Commonly used to make T-shirts, sweatshirts, and bed linens.
- 60% polyester, 40% cotton: Used in sportswear, work uniforms, or casual fashion.
- 65% polyester, 35% cotton: Suitable for casual wear, workwear, or uniforms.
- 35% polyester, 65% cotton: Suitable for various applications from casual wear to home textiles.
- 20% polyester, 80% cotton: Used in sleepwear, casual wear, or summer clothing.
4.1. Dissolution of Cotton
4.2. Dissolution of Polyester
4.3. Hydrolysis of Cotton or Polyester
4.4. Hydrothermal Treatment
4.5. Enzymatic Hydrolysis of Cotton or Polyester
5. Separating Elastane from Other Fibers
5.1. Selective Dissolution of Elastane
5.2. Elastane Degradation by Aminolysis or Solvolysis
6. Recycling of Blended Textiles in Industry
7. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Polymer | Polysaccharides: Cellulose | Polyester | Polyamide | Polyurethane | Polyolefin | Polyacrylic |
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Linkage | ||||||
Fiber Example | Cotton, Linen, Viscose | PET | Wool, Silk, Nylon | Elastane | Polypropylene, Polyethylene | Acryl, Modacryl |
# | Method | Starting Material and Composition | Process/Reaction | Process/Reaction Conditions | Products | Analysis | Any Other Component Present | Issue/ Problem | Reference |
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1 | Dissolution of Cotton | Textiles blended with 40/60 polyester and viscose and 50/50 polyester and cotton. | N-methylmorpholine-N-oxide (NMMO), was utilized in this procedure to separate cellulose (cotton and viscose) from blended textiles. | 85% w/w NMMO solution in water was mixed with 15 g of the textile pieces at 120 °C in an oil bath for 2 h under atmospheric conditions. | The products were cellulose solution and undissolved polyester. The cellulose was then either hydrolyzed by cellulase enzymes followed by fermentation to ethanol, or digested directly to produce biogas. | Gas chromatography was used to measure the amount of methane produced during anaerobic digestion. Within 6 days of digestion, 53–62% of the theoretical yield of methane was obtained. | After 2 h treatment, non-cellulosic fibers, and other impurities, e.g., buttons and zippers remained as the solid phase while cellulose is dissolved in the liquid phase. | [63] | |
2 | Dissolution of Cotton | White post-consumer textiles. The composition of the poly-cotton blend was 50:50. | [DBNH] [OAc], (1,5-diazabicyclo[4.3.0]non-5-enium acetate) an amidine-based Ionic Liquid, was used as a selective cellulose solvent to separate cotton from polyester. | Using a vertical kneader system, the cotton polyester blend was combined with [DBNH] [OAc] (for 1 h, at 80 °C). | The products were cellulose solution and undissolved polyester. Hydraulic pressure filtering separated the undissolved polyester fraction from the cellulose solution. After solidification, by storing at 8 °C for a couple of days, the resultant cellulose was spun through dry-jet wet spinning. | The molar mass distributions (MMD) of the polyester and cellulose fractions were ascertained using size exclusion chromatography.PET degrades visibly in this method as evidenced by a decline in its MMD (<51%). The linear density, elongation at break, and tenacity of every spun fiber were measured. Linear densities ranging from 0.75 to 2.95 dtex, (dtex or deci-tex is a unit of linear density, which is grams per 10,000 m of yarn) and elongations of 7 to 9%. | PET degraded visibly in this method once it was dispersed in [DBNH] [OAc], as evidenced by a decline in its MMD (<51%) and tensile characteristics (<52%). | [65] | |
3 | Dissolution of Cotton | The cotton polyester blended yarn consisted of 50 wt% cotton and 50 wt% polyester. | To recover cotton from the cotton-polyester blend, cellulose-dissolving ionic liquid 1-allyl-3-methylimidazolium chloride (AMIMCl) and 1-butyl-3- methylimidazolium acetate (BMIMAc) was used to selectively dissolve the cotton component. | Dissolution in AMIMCl at 80 °C for 6 h. | The products were cellulose solution and undissolved polyester. 100% of the cotton from the blend dissolved. Undissolved polyester was removed by filtering. Fibers and/or films can be made from the cotton/AMIMCI solution. | SEM was used to examine the morphology of the materials. Before separation, both cotton and polyester fibers can be observed. After the separation, only polyester fibers are observed in the SEM image. Following the cellulose’s dissolution, a small quantity (less than 2%) of cotton may still be present in the recovered polyester, according to the 13 C Nuclear magnetic resonance NMR spectra and FTIR spectroscopy. On a thermogravimetric analyzer, the treated sample underwent thermogravimetric analyses (TGA) to characterize the structure of the recovered polyester and cotton. The TGA curves showed little to no difference between the sample and recovered material for both cotton and polyester. | The 13C NMR spectrum and FTIR indicated that a small amount (less than 2%) of cotton may remain with the recovered polyester. | [66] | |
4 | Dissolution of Cotton | Experiments were conducted using the long-worn lab suits as raw materials consisting of 35% cotton and 65% polyester. | Cotton can be selectively dissolved from waste poly-cotton fabrics using 1-allyl-3-methylimidazole chloride ([Amim]Cl)/Dimethyl sulfoxide (DMSO) and 1-ethyl-3-methylimidazolium diethyl phosphate ([Emim] DEP)/DMSO system as solvents. | ([Amim]Cl) and ([Emim] DEP) as solvent, DMSO as a cosolvent. 0.4 g of waste poly-cotton fabrics combined with solvent (10 g ILs, 10 g DMSO) and dissolved for 5 h at 80 °C. To eliminate the cotton that remained on the regenerated polyester, it was treated for one hour at 50 °C with diluted sulfuric acid. After washing with water, it was dried for 48 h at 105 °C. It was put in a melt-spinning machine. | Wet spinning was used to immediately use the cellulose solution that was produced by the procedure. Melt-spinning was used to prepare the polyester into regenerated polyester fibers. | The cellulose’s relative viscosity was determined, and the degree of polymerization DP of the material was calculated. DP of the sample fabric’s cellulose portion was 1087. DP of the regenerated cellulose using [Amim]Cl/DMSO and [Emim]DEP/DMSO was decreased by 24.4% and 2.9%, respectively. The breaking strength of the regenerated fiber was found to be 1.7 cN/dtex, and the elongation at break was 16.7%. The surface and cross-section of the regenerated cellulose fibers were captured with SEM which showed that the regenerated cellulose fibers were cylindrical with a dense and smooth surface. The FT-IR characteristic peaks of regenerated cellulose and regenerated cellulose fibers were basically similar, indicating that no chemical reaction occurred during normal regeneration and wet spinning process. The dissolution of cotton from waste poly-cotton fabrics utilizing the [Emim]DEP/DMSO system as the solvent was further validated by XRD analysis. The XRD patterns revealed that the waste poly-cotton fabrics initially exhibited diffraction peaks corresponding to both cellulose I-type structure and polyester crystal structure. After the cotton was dissolved and separated, the crystallization peak positions of the regenerated cellulose shifted, indicating a transformation from type I to type II cellulose structure. | The degree of Polymerization of the regenerated cellulose decreased by 25.5% while using [Amim]Cl/ DMSO and 5.0% while using [Emim]DEP/DMSO. | [67] | |
5 | Dissolution of Cotton | Polyester-cotton blended fabric with a composition of 65% polyester, 35% cotton. | Selective dissolution of cotton from a poly-cotton blend using a deep eutectic solvent (DES) based on metal salt hydrates. | Synthesis of the metal-salt-hydrate-based DES: For 30 min, ZnCl2, H2O, and H3PO4 in the molar ratio of 1:3:0.5 were magnetically agitated to create a homogeneous ternary solvent. Dissolution: The combined fabric was put into DES. To begin the dissolving separation, the mixture was agitated at a speed of 600 rpm with a cellulose-to-solvent ratio of 5:100. The separated polyester fiber was used as the raw material for the melt-spinning process, which produced the recycled polyester fiber. To create regenerated cellulose fibers, cellulose was extracted from the DES solution system using the coagulation process and then dissolved in a NaOH/urea/H2O solvent for wet spinning. | Cellulose fiber, Polyester fiber | The FTIR spectra of the blended fabric as well as separated polyester were obtained. The FTIR spectra of regenerated PET is very similar to that of original PET indicating the stability of the PET structure before and after separation. The cotton fabric’s XRD diffractogram displayed the standard cellulose I pattern. The regenerated cellulose that came from the DES showed peaks that corresponded to cellulose II patterns. These results pointed to a conversion of cellulose I into cellulose II, which was accompanied by a fast dissociation and reformation of intra- and intermolecular hydrogen bonds between cellulose molecules. | [68] | ||
6 | Dissolution of Cotton | Waste polyester/cotton blended fabrics (WBF), with a composition of 65/35 wt%. | Acetylation of cellulose using a Bronsted acidic ionic liquid (IL) N-methyl-imidazolium bisulfate, [Hmim]HSO4, as a novel catalyst. | Using [Hmim]HSO4, an acidic IL N-methyl-imidazolium bisulfate, as the heterogeneous catalyst, acetylation of cellulose was performed at atmospheric pressure. 4.63 g of the pulverized WBFs powders, 20.42 g of acetic anhydride, and 0.18–1.08 g of the [Hmim]HSO4 were mixed and heated at 100 °C for 12 h. The reaction mixture was then added to 100 milliliters of ethanol. The cellulose acetate (CA) and PET-containing material were filtered, washed three times with ethanol, and then dried for 12 h at 60 °C in a vacuum oven. A portion of the sample was refluxed for 12 h using the Soxhlet extraction method and acetone as the solvent to extract the acetone-soluble CA. The acetone-soluble CA product was then obtained by drying the filtrate for 12 h at 60 °C in a vacuum oven. Using DMF as the solvent, the solid portion of the sample was refluxed for 12 h using the same procedure. This led to the extraction of DMF-soluble CA and regeneration of PET. | Acetone-soluble CA and PET. With 84.5% of the cellulose in the WBFs converted, the highest yield of acetone-soluble CA was 49.3%; in the meantime, almost 96% of the PET was recovered. | The degrees of substitution (DS) values of the cellulose acetate (CA) products were determined by 1 H NMR spectroscopy. The acquired CA and the commercial CA sample’s FTIR spectra were gathered. When the spectra of the produced CA were compared to the spectrum of commercial cellulose, they clearly demonstrated acetylation due to the existence of two significant ester bonds at 1752 cm−1, which were given to C=O ester stretching, and 1235 cm−1, which was assigned to the –CO– stretching of the acetyl group. XRD patterns were collected for obtained CA and commercial CA. Comparable structural features were indicated by the similar XRD signals of the obtained CA and commercial CA. The obtained CA’s XRD pattern demonstrated a drop in peak intensities that matched to the crystalline cellulose I structure. The replacement of acetyl groups for hydroxyl groups during the acetylation process was the cause of this decrease in crystallinity. | [69] | ||
7 | Dissolution of Cotton | Polycotton fabric (polyester cotton ratio was 80:20 and 50:50) | The separation was done by dissolution of cotton using a co-solvent system of ionic liquid and dimethyl sulfoxide | Fabric samples were treated with an aqueous solution containing 0.5 wt% sulfuric acid to reduce the degree of polymerization (DP) of the cotton component. Subsequently, the samples were treated with a solvent system of 80% DMSO and 20% ionic liquid. After 24 h, the solution was filtered. The cellulose dope filtrate was collected for spinning, while the solid polyester material was washed, dried, and rinsed with DMSO to remove residual cellulose solution before being air-dried. | Regenerated cellulose fiber and intact polyester. | The morphologies of the fabrics and recovered materials were examined by SEM. Which confirmed the removal of cotton from the polycotton blend. | [70] | ||
8 | Dissolution of Polyester | Black 100% cotton jeans and blue 80/20 cotton/polyester jeans. | Three-step process: (a) Textile dye leaching using Nitric Acid. (b) Dissolution process using Dimethyl Sulfoxide (DMSO) to dissolve the polyester and remaining organic part from textile dyes. (c) Bleaching using sodium hypochlorite and diluted hydrochloric acid for recovered cotton purification. | Dyes from blue and black samples were dissolved using 1.0 M and 1.5 M HNO3, with an average treatment duration of 20 min. 1 g samples of two different types of jeans were treated with 10–80 milliliters of solvent at a constant temperature of 50 °C. The black sample could be fully separated optimally in 7 h with 40 mL solvent, while the blue sample needed 9 h and 60 mL solvent. Under soundwave treatment for 2 h at 40 °C, the cotton fibers were bleached with sodium hypochlorite and diluted HCl to remove any leftover contaminants. | Dissolved polyester in the spent solvent, cotton fiber. | FTIR spectroscopy was used to examine the chemical structure of the fiber samples both before and after the treatment. It showed that all dyes and contaminating elements were successfully removed by leaching, dissolving, and bleaching and that the recovered fiber was made of highly pure cotton. Thermogravimetric/Derivative Thermogravimetric analysis (TGA-DTG) was used to investigate the thermal degradation and stability trends of the precipitated polyester. The decomposition methods of the black and blue samples were similar and observed within the 80–365 °C range. | [74] | ||
9 | Dissolution of Polyester | Colored 50/50 polyester/cotton blended fabric. | Using dimethyl sulfoxide (DMSO), the polyester component and dispersion dyes were extracted from blends of polyester and cotton. Following the breakdown of dye-cellulose linkages, the remaining colored cotton was swollen to remove its dyes. Regenerated fibers were created from colorless polyester and cotton. | One part polyester/cotton and three parts DMSO were combined at 150 °C. In about five minutes, the dissolution took place. After cooling down recycled polyester and dispersed dyes in DMSO, the polyester precipitated. The dispersed dyes were extracted by washing the material with a small amount of heated dimethyl sulfoxide. Following the separation of polyester and dispersion dyes, cellulose molecules were swelled by adding solvents containing varying ratios of DMSO to water to the cotton fibers that retained their color. Since reactive dyes and cellulose had covalent connections, the covalent bindings between the dye and cellulose were broken by adding 0.07–0.6 weight percent of NaOH to the DMSO/water solvent. To completely separate the color from the cotton, the material was swollen three times. Every cycle lasted 10 min at 90 °C. Each cycle’s weight ratios for the solution to cotton were 3. At 270 °C, the dried polyester was wet spun into recycled polyester fibers. By stirring at 110 °C for two hours, a solution comprising 5% color-removed cellulose, 87 wt% NMMO and 13 wt% water was created. Through dry-jet wet spinning, the cellulose solution was extruded into fibers. | Colorless polyester and cotton which were regenerated into fibers. | Morphologies of the regenerated polyester and cellulose fibers were characterized by a field-emission scanning electron microscope. The structures of fibers were determined by X-ray diffraction. The recycled and virgin fibers had similar crystallization behavior. The cellulose’s FTIR spectra were determined to be identical both before and after the separating procedure. The polyester’s FTIRs before and after the separation procedure were identical. | Dyes were extracted as a dye solution. | [75] | |
10 | Hydrolysis | The cotton polyester blended bed sheets comprised 48 wt% cotton and 52 wt% polyester. | PET was degraded to terephthalic acid (TPA) and ethylene glycol (EG) using NaOH | 5–15 wt% NaOH in water and temperature in the range between 70 and 90 °C for the hydrolysis of PET, for 40 min. | Three product streams were generated from the process. First is the cotton; second, the TPA; and third, the filtrate containing EG and the process chemicals. Solid Cotton residue (Separated by filtering), TPA was precipitated, and EG was in the filtrate. | NMR spectroscopy was used to characterize the polycotton bed sheets prior to separation. The degraded PET was analyzed using NMR spectroscopy, which revealed that the recovered TPA was free of any impurities. Following PET hydrolysis, the solid (cotton) residue’s ATR FT-IR spectra were compared to a sample of pure cotton. This demonstrated that cellulose I had somewhat changed into cellulose II. | Under the highly alkaline conditions used in the PET-removing procedure, undesired cellulose degradation reactions may also occur in the cellulose portion of a polycotton sample. These processes cause cellulose chains to break, which lowers the cellulose’s DP. | [77] | |
11 | Hydrolysis | Polyester-cotton blended fabric. Composition is not mentioned in the study. | Acid treatment with Sulfuric acid then a grinder was used to crush it to separate the polyester from cotton fiber. | The waste polyester/cotton mixed fabric was split into 2 × 2 cm pieces and subjected to varying sulfuric acid concentrations over varying periods of time. After being treated, the blended polyester/cotton cloth was washed and dried. Using a grinder, the cotton fiber powder and the polyester fiber ball stained with the powder were produced. Subsequently, a certain volume of powdered cotton fiber was weighed and swelled using a NaOH solution. The pH was then brought to a neutral level. After using 64% sulfuric acid for a predetermined amount of time, the reaction was completed by adding 10 times as much deionized water. After being diluted, the mixture was dialyzed to neutrality and centrifuged. After a specific number of homogenizations using a high-pressure homogenizer, the treated solution’s concentration was blended to 0.5% and freeze-dried. | The separated products were polyester as a fibrous mass and cotton powder. Nanocellulose from the cotton was obtained by further processing. | The separated cotton fibers’ retention of their cellulose structure was validated by the FTIR analysis, which also showed signs of lignin or hemicellulose removal post treatment. XRD was used to examine the crystallinity of the separated cotton fiber which indicated that the crystallinity of cellulose fiber was very high, and it was the structure of cellulose type I. The morphology of the separated polyester and cotton fibers was investigated using SEM. Following acid hydrolysis and mechanical agitation, the cotton fiber had surface damage, fractures, and a marked reduction in length. The surface of the treated polyester fiber remained intact, and it was stained with a little amount of powdered cotton fiber. | [78] | ||
12 | Hydrolysis | Garments with a blended fabric containing 70% viscose and 30% polyester | Alkaline hydrolysis of viscose/PET | The aqueous NaOH (5 wt%) was heated to 90 °C before adding the oven-dried (2 h at 105 °C) sample to the reaction vessel. Hydrolysis was performed for a selected time (60–1440 min). After the reaction, the solid residue was separated from the reaction solution via filtration. | The reaction yielded a solid cellulose residue, and the PET monomers terephthalic acid (TPA) and ethylene glycol (EG). | NMR was utilized to ascertain the purity of TPA derived from PET depolymerization, using a commercial TPA as the reference standard. The spectrum of the precipitate showed a distinct singlet at 7.58 ppm which was assigned to pure TPA. | The alkaline treatment reduces cellulose’s intrinsic viscosity by up to 35%, hence it would not be appropriate for traditional fiber-to-fiber recycling. | [79,80] | |
13 | Hydrothermal Treatment | A blue 65/35 cotton/polyester blend fabric served as the waste textile sample. | To recover cotton from the cotton-polyester blend, the cotton component was hydrolyzed and turned into cellulose powder or oligosaccharide using diluted hydrochloric acid as a novel hydrothermal treatment catalyst for cellulose. | 1.5 wt% dilute hydrochloric acid at 150 °C, 3 h of reaction time. | Cellulose powder, polyester fiber. | Using techniques such as SEM, FTIE, XRD, and high-performance liquid chromatography, the morphology and structure of the hydrothermal products—both solid and liquid—were characterized and compared to untreated polyester and cotton. The results indicate that after three hours of hydrolysis, the polyester fiber preserved its fiber properties while the cotton fiber entirely degraded. The hydrolysis did not alter the crystalline structure of cellulose, as seen by the essentially similar XRD patterns of cotton and cellulose powder. | The fate of the blue dye was not reported in this study. | [81] | |
14 | Hydrothermal Treatment | White shirts with a composition of 66% cotton and 34% polyester. | Hydrothermal treatment which separated polyester and cotton from the blend. | After being cut into pieces measuring around 5 by 5 cm2, the sample cloth was added to a reactor that held 300 mL of pure water. The cloth was treated for 10–180 min after being heated to the appropriate temperature (180–250 °C). The reactor was then allowed to naturally cool to 40 °C. After the reactant fabric was taken out, filtering was used to recover the solid residue in the water. | Cotton as mesh fabric. Polyester as a solid powder. | Using SEM, the surface conditions of the treated mesh fabric were compared to those of the raw material. Following treatment, SEM images demonstrate that the cotton fiber condition is preserved. It is also evident that the fibers have suffered some little damage from the 230 °C treatment. It wass hypothesized that the cotton fibers have gradually deteriorated due to the subcritical water treatment. FTIR examination verified the minute fragments and powdery material obtained after treatment to be PET, and the mesh fabric to be cotton. | [82] | ||
15 | Enzymatic Hydrolysis | Textile waste of cotton and polyester (PET) blend by 60/40. | Using cellulase and β-glucosidase, textile waste was hydrolyzed enzymatically to extract glucose and polyester. | Textile fabrics were enzymatically hydrolyzed at 50 °C for 96 h. The maximum glucose recovery of 98.3% was obtained with 20 FPU/g of cellulase dosage and 10 U/g of β-glucosidase dosage at 3% (w/v) substrate loading, temperature of 50 °C and pH 5 | Glucose, Glucose yield was 98.3%. The recovered PET fiber can be reused by melt-spinning to new PET fiber. | Glucose concentration was determined by HPLC. SEM analysis before and after enzymatic hydrolysis showed significant changes in textile morphology. Prior to hydrolysis, cotton and polyester fibers formed a compact structure. After hydrolysis, the structure loosened with fewer fibers, and small holes appeared due to the digestion of cellulose fibers. PET fibers remained intact. | [86] | ||
16 | Enzymatic Hydrolysis | Clothing: with a composition of 65% PET, 35% Cotton. And 80% PET, 20% Cotton. | Using a commercial cutinase from Humicola insolens (HiC) under moist-solid reaction conditions, PET in mixed PET/cotton textiles could be directly and selectively depolymerized to terephthalic acid (TPA). This process was easily combined with cotton depolymerization through simultaneous or sequential application of the Cellic CTec2 cellulases blend, yielding glucose. | After cutting the textile samples into squares measuring 0.7 × 0.7 cm, they were ball milled for 5 or 30 min (30 Hz) in 15 mL stainless-steel milling jars with HiC (0.65% w/w) and/or CTec2 (0.7% w/w) enzymes present. This was followed by seven days of static incubation at 55 °C. | TPA (with a maximum yield of 30 ± 2%) and glucose (with a maximum yield of 83 ± 4%) were obtained through the mechanoenzymatic hydrolysis of the PET/cotton blended textile. Additionally, ethylene glycol (yield unknown) and a small reaction product, up to 0.5% yield of MHET were produced by the hydrolysis of PET. | Cotton hydrolysis products were assessed using a commercially available glucose test, while PET hydrolysis products were quantified by HPLC. | [56] | ||
17 | Enzymatic Hydrolysis | A white 40/60 polyester/cotton blended fabric. | Alkali pretreatment and enzymatic hydrolysis followed by saccharification and fermentation. | Waste textiles were pretreated using aqueous alkaline mixes of NaOH (12 wt%), NaOH/urea (7/12 wt%), NaOH/thiourea (9.5/4.5 wt%), and NaOH/urea/thiourea (8/8/6.5). 5 g of waste textile and 95 g of an alkaline solution were combined for the pretreatments, which lasted one hour at various temperatures of 20 °C, 0 °C, 23 °C, and 100 °C. Using 30 FPU cellulase and 60 IU b-glucosidase per gram of cellulose, waste textiles were treated to a 72 h enzymatic hydrolysis at 45 °C and pH 4.8 (in 50 mM sodium citrate buffer supplemented with 0.5 g/L sodium azide) with 3% (w/v) solid (substrates) loading. | Polyester and Ethanol. When saccharification and fermentation were carried out simultaneously on the textile, the greatest yield of ethanol production was 70%. The recovered polyester accounted for 98%. | The characteristics of recovered polyester were evaluated by FTIR, DSC, and viscosity analyses. The FTIR result revealed that after the polyester was treated with NaOH, the trans/gauche ratio dropped, indicating a reduction in the crystalline area. | [87] | ||
18 | Enzymatic Hydrolysis | Textile waste blends of cotton and PET, with compositions of 35/65 and 60/40. | Sample waste fabrics were cut into little pieces (about 0.5 × 0.5 cm2) and soaked in freezing alkali/urea for three separate modification methods: autoclaving, freezing, and alkaline pretreatment. Then the sample was subsequently exposed to enzymatic hydrolysis. | After adding the mineral solution to achieve the appropriate initial moisture level, the textile waste was autoclaved for 15 min at 121 °C as part of the autoclave pretreatment. Textile waste was mixed with urea (12% w/v) and NaOH (7% w/v) for the freezing alkali/urea soaking process. The mixture was then frozen at −20 °C for six hours. The textile waste was autoclaved for 15 min at 121 °C or soaked for 3 h at 80 °C in a 15% NaOH solution for alkaline pretreatment. Enzymatic hydrolysis was used to regenerate cellulose from cotton/PET textile waste mixtures. In this study, commercial cellulase (Cellic CTec2, 185 FPU/mL) was employed. Two grams of regenerated cellulose were added, at a substrate-enzyme dose of 25 FPU/g, to a citric buffer (100 mL, 50 mM, pH 4.8). For 96 h, hydrolysis was carried out at 50 °C and 200 rpm. | Glucose and PET as a solid mass. | Utilizing a high-performance liquid chromatography column (HPLC), the amount of glucose was determined. After processing with NaOH, SEM analysis showed notable changes in the surface morphology of textile sample. At first, the fabric had a surface that was a little uneven and harsh. However, after treatment, the cotton/PET digestion by NaOH caused a partial breakdown of the textile’s structure into rough fibers. The textile samples were examined using FTIR both before and after processing. PET and cellulose polymer-corresponding absorption bands were visible in the spectra. Significant alterations in the cellulose polymer bands were found upon analysis of the pretreated textile waste, demonstrating the pretreatment process’s efficacy in changing the polymer structure. | [88] | ||
19 | Enzymatic Hydrolysis | Used jeans, composition not mentioned in the study. | Phosphoric acid pretreatment and subsequent enzymatic hydrolysis of cotton-based waste textiles to recover sugar and polyester. Two enzymes were used for enzymatic hydrolysis: cellulase from Trichoderma reesei and cellobiase from Aspergillus niger. | Phosphoric acid pretreatment: 85% phosphoric acid, at 50 °C, for 7 h, and a ratio of fabric and acid of 1:15. Enzymatic hydrolysis In 150 mL flasks with a 50 mL work volume, the regenerated cellulose was enzymatically hydrolyzed in 50 mM sodium citrate buffer (pH 4.8). With a cellulose loading of 7.5 FPU/g regenerated cellulose and a cellobiase loading of 15 CBU/g regenerated cellulose, the substrate consistency for enzymatic hydrolysis was maintained at 1.0% (w/v). For 96 h, the hydrolysis was carried out at 50 °C in an air-bath shaker at 130 rpm. | Polyester in solid form. At the optimized conditions (85% phosphoric acid, 50 °C, 7 h, and a ratio of 1:15), 100% polyester recovery with a maximum sugar recovery of 79.2% was accomplished. | The glucose content was determined by HPLC. Surface morphology was analyzed using SEM. Distinct cotton and polyester fibers were visible in the original waste textiles sample. The cellulose fibers changed significantly and became rougher after pretreatment. The majority of cotton fibers remained intact after enzymatic hydrolysis without pretreatment, underscoring the necessity of pretreatment for effective sugar recovery. Cotton fibers were effectively extracted from polyester using phosphoric acid pretreatment, resulting in 100% polyester recovery without changing the surface of the polyester as seen on the SEM images. | [89] | ||
20 | Enzymatic Hydrolysis | Blended textiles (65% polyester, 35% cotton) | NaOH/urea solution pretreatment is followed by cellulase-based enzymatic hydrolysis. It was found that using concentrations of NaOH varying from 20.7% to 26.6% with either 0% urea or a mixture of 13.9% NaOH and 12% urea was efficient and almost entirely eliminated the cellulose in the blended textile. | 400 mL of NaOH/urea solution was used for pretreatment and 4 g of textile substrate were weighed in a beaker for every experiment. Using sodium azide (0.02%) and a 50 mM citric acid buffer at pH 5.0, hydrolysis was carried out in a 1-L flask. In a 500 mL buffer, the textile substrate was added with a solid load of 0.8% (w/v). The activity of the enzyme dose was adjusted to 0.68 filter paper units (FPU) per g of cellulose. For 24 h, hydrolysis was carried out in a heating incubator at 50 °C and 70 rpm orbital shaking. | Polyester as solid residue, and Glucose | To find the released glucose, high performance anion exchange chromatography (HPAEC) was employed. After being hydrolyzed by enzymes, the quality of the recovered synthetic fibers was assessed using Fourier transformed infrared spectroscopy (FTIR). FTIR analysis compared untreated textile blend, pure polyester, and regenerated polyester fibers. It revealed decreased peaks characteristic of cellulose and increased peaks characteristic of PET. | [90] |
# | Method | Starting Material and Composition | Process/Reaction | Process/Reaction Conditions | Products | Analysis | Any Other Component Present | Issue/Problem | Reference |
---|---|---|---|---|---|---|---|---|---|
1 | Selective dissolution of elastane | Polyester-elastane blend and Polyamaide-elastane blend. (PET/elastane: 85/15), (Polyamide/ elastane: 88/12) | The selective dissolution of elastane from blended textile can be done using tetrahydrofurfuryl alcohol THFA and γ-valerolactone. (GVL). | 4 h and 100 °C, tetrahydrofurfuryl alcohol THFA and γ-valerolactone (GVL) as solvents. | Elastane solution. PET fiber and polyamide fiber in the solid form. | Thermogravimetric analysis with Fourier transform infrared spectroscopy (TGA-FTIR) was used to determine the maximal solubilities (4.9 mg/g THFA and 4.3 mg/g γ-valerolactone). The quality of the extracted elastane fibers was assessed by liquid 1H-NMR. Before solvent treatment, liquid 1H-NMR of the pure elastane fiber revealed that it exclusively included methylene diisocyanate derived carbamates. THFA solvent treatment, however, caused the carbamate bond to break, which indicated elastane fiber partially depolymerized. | [21] | ||
2 | Selective dissolution of elastane | Polyester/elastane, and polyamide/elastane textile waste samples Green-colored polyester/elastane and black-colored polyamide/elastane post-industrial textile waste samples. The textile compositions were 82% PET/18% EL and 92% PA/8% EL. | Dissolution of elastane. | 1 g sample in 200 mL solvent, dimethyl sulfoxide (DMSO), at 120 °C for 30 min | Elastane solution. By filtering the solution, washing, and drying the filtride, polyester or polyamide components are recovered. | Polymer degradation behavior was analyzed using TGA. In textiles that have not been treated, elastane (EL) degradation peaks could be seen at approximately 300 °C. Because of the high elastane content in the PET/EL textile, an earlier degradation start (412 °C) was seen. The successful separation of elastane was confirmed by this comparison. There appeared to be no deterioration in the polymer matrix since the degradation peak associated with the PET reference (442 °C) coincided with that of the recovered material. Comparably, limited variation between degradation peaks (around 423 °C) for the black PA/EL textile indicated that the polymer matrix had not changed. Morphology of the samples was analyzed using scanning electron microscopy (SEM). The PET/EL fabric’s rich collocation of polyester and elastane fibers was apparent in the SEM images. Following the elastane separation, recovered PET showed no signs of elastane-related residues being adhered to the fibers. | The solvent enriched with colorant and elastane particles during the treatment; therefore it could not be used indefinitely. Elastane could dissolve in DMSO up to an 18 g/L concentration. DMSO could not be used any more beyond this point because elastane particles collected in the treated solvent. | [92] | |
3 | Selective dissolution of elastane | Pre-consumer-waste fibers and fabrics. One PA6/elastane blend with 6.3% elastane. Two PA66/elastane blends (with 23% and 32% elastane). | Using a solvent blend (THF: DMSO in a 70%:30% by volume ratio), elastane in a mixed polyamide fabrics can be selectively dissolved. | 1 g fabric in 20 mL solvent, dissolution at 25 °C for 1 h, THF:DMSO in a 70%:30% by volume ratio. | Precipitated Elastane, solid polyamide in the spent solvent. | SEM micrographs of the untreated and solvent treated sample show that, most of the elastane was dissolved in a first cycle, and the washing process in non-solvent precipitated the elastane left on the fabric surface. DSC and FTIR analysis also indicated that elastane was removed from the sample. | [91] | ||
4 | Elastane degradation | A white pre-consumer textile blend, composed of 95% (w/w) of cotton and 5% (w/w) of elastane. | Selective Elastane Degradation by Aminolysis. | 4 h at 80 °C. 8 g of the ground fabric was added to 160 mL of a solvent mixture containing a cleaving agent (DETA) and an elastane solvent (DMF or DMSO) in a 1:1 volume ratio. | The solid and liquid phases were separated by filtration. The liquid phase contained the solvent mixture and the degraded elastane products, by adding water to the liquid phase, the elastane products were precipitated. Cellulosic material was dissolved in [DBNH] [OAc] and turned into new fibers via dry-jet wet spinning. | TGA was used to study thermal behavior. Both the recovered elastane and pure elastane showed similar thermal behavior. The recovered elastane underwent FTIR and NMR tests to understand more about its chemical composition. The distinctive polyurethane peaks were visible in the FTIR spectra of the sample elastane and the recovered elastane. | [95] | ||
5 | Elastane degradation | Polyester fabric coated with polyurethane. | Selective degradation of PU elastomers by cleavage of C–O and C–N bonds in 70% ZnCl2 aqueous solution. This catalyst-assisted solvolysis did not degrade the polyether bonds and PU was converted to the amine form of the used isocyanate and the original polyether polyol. | 10 g PU coated polyester was added to ZnCl2 solution (70 wt% in water, 250 g), heated to 140 °C and for 2 h. The degradation products were cooled to room temperature and then agitated for five minutes in 250 mL water following the reaction. After the mixture was filtered, an insoluble residue (fabric and insoluble degradation products of PU) and a water mixture were obtained. The fabric was filtered off after the residue was added to 200 mL ethyl acetate. The ethyl acetate mixture was washed three times with brine, then the organic phase was evaporated with a rotary evaporator. The water mixture was evaporated and diethyl ether was added. The precipitated product was separated via filtration and dried overnight at 70 °C at atmospheric pressure. | Polyester fabric, polyol, and amine | The thermal, chemical, and mechanical characteristics of the virgin PET and recycled PET were analyzed through tensile strength tests, IR, TGA, and GPC. The virgin polyester fabric’s tensile force and elongation were 360 N and 33.5%, respectively. The tensile strength of recycled polyester fabric was 350 N, and its elongation was 34%. Therefore, the mechanical characteristics of the polyester fabric were unaffected by the heat treatment in the presence of ZnCl2. The IR spectra of virgin polyester and recycled polyester showed significant similarities which indicates that the PET recovered after the degradation of polyurethane in ZnCl2 solution was not degraded. TGA Analysis showed that the polyester did not degrade during solvolysis, while the PU was converted into polyol and amine. As analyzed in GPC, when compared to virgin PET, the recycled PET’s molecular weight did not decrease, indicating that it did not break down during solvolysis. | [96] | ||
6 | Elastane degradation | Fabric sample consisting of 27% Elastane and 73% Nylon. | Solvolysis using tert-amyl alcohol in the presence of KOH. | 1.02 g fabric sample consisting of 27% elastane and 73% Nylon was added to tert-amyl alcohol (5 mL) and KOH (0.19 wt%) at 225 °C for 4.5 h. | The products were 50.9 mg 4,4′-MDA, 266 mg polyTHF in the liquid phase and 698 mg leftover fabric. | FTIR analysis was performed on sample and treated fabric sample. The results suggested that the elastane had been effectively removed from the polyamide matrix. The polyamide remained unaltered, while the elastane fibers in the fabric were depolymerized. For pure elastane, DSC showed a crystalline peak at 20 °C. Both a wide crystalline phase for the polyamide at 225 °C and a crystalline peak for the elastane at 20 °C were seen in the untreated sample. For the treated fabric at 255 °C, the polyamide could form a crystalline peak, and there was no evidence of elastane. This suggests that the elastane has been successfully removed and that the polyamide fiber was intact with no symptoms of contamination or deterioration. | [94] |
# | Company | Founded | Location | Process | Output | Scale |
---|---|---|---|---|---|---|
1 | Ambercycle | 2015 | Los Angeles, CA, USA | Biological recycling process | PET pellets and fiber | Pilot plant |
2 | BlockTexx | 2018 | Loganholme, Australia | Chemical Process | PET and Cellulose | Commercial scale plant |
3 | Circ | 2011 | Danville, Virginia | Hydrothermal process | Cellulose, terephthalic acid TPA, and ethylene glycol EG. | Commercial scale plant |
4 | Worn Again Technologies | 2005 | Nottingham, England | Solvent-based dissolution | PET and Cellulose | Pilot plant |
5 | Purfi | 2018 | Waregem, Belgium | D’Elastane™ technology | PET fiber | Not mentioned |
6 | Textile Change | 2019 | Vejle, Denmark | Chemical Process | PET and Cellulose | Pilot plant |
7 | Sodra (OnceMore®) | 2022 | Växjö, Sweden | Chemical Process | Cotton fiber | Commercial scale plant |
8 | Phoenxt | 2018 | Blomberg, Germany | Solvent-based process | PET, Cellulose | Not mentioned |
9 | Eeden | 2022 | Münster, Germany | Chemical Process | Cotton fiber, terephthalic acid TPA, and ethylene glycol EG. | Not mentioned |
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Choudhury, K.; Tsianou, M.; Alexandridis, P. Recycling of Blended Fabrics for a Circular Economy of Textiles: Separation of Cotton, Polyester, and Elastane Fibers. Sustainability 2024, 16, 6206. https://doi.org/10.3390/su16146206
Choudhury K, Tsianou M, Alexandridis P. Recycling of Blended Fabrics for a Circular Economy of Textiles: Separation of Cotton, Polyester, and Elastane Fibers. Sustainability. 2024; 16(14):6206. https://doi.org/10.3390/su16146206
Chicago/Turabian StyleChoudhury, Khaliquzzaman, Marina Tsianou, and Paschalis Alexandridis. 2024. "Recycling of Blended Fabrics for a Circular Economy of Textiles: Separation of Cotton, Polyester, and Elastane Fibers" Sustainability 16, no. 14: 6206. https://doi.org/10.3390/su16146206
APA StyleChoudhury, K., Tsianou, M., & Alexandridis, P. (2024). Recycling of Blended Fabrics for a Circular Economy of Textiles: Separation of Cotton, Polyester, and Elastane Fibers. Sustainability, 16(14), 6206. https://doi.org/10.3390/su16146206