Method and system for selective nylon extraction from blended textile
A method and system using a mild solvent and moderate conditions effectively separate and recycle nylon from blended textiles, addressing inefficiencies in existing techniques by achieving high recycling rates and environmental sustainability.
Patent Information
- Application Number
- PCT/CN2024/094653
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2024-05-22
- Publication Date
- 2025-11-27
AI Technical Summary
Existing nylon recycling techniques face high energy consumption, environmental pollution, and inefficiency in separating nylon from mixed textile waste due to the use of harmful solvents and high operating temperatures, limiting the recycling rate and applicability to specific types of nylons.
A method and system using a mild solvent comprising inorganic salts and aliphatic alcohols at moderate temperatures and pressures to selectively dissolve nylon from blended textiles, followed by treatment to produce porous nylon clusters, which are then spun into fibers with properties comparable to virgin nylon.
Achieves a recycling rate of over 90% with reduced energy consumption and environmental impact, enabling the reuse of solvents and buffers, and producing nylon fibers with desired tensile strength and polymerization, suitable for industrial applications.
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Figure CN2024094653_27112025_PF_FP_ABST
Abstract
Description
METHOD AND SYSTEM FOR SELECTIVE NYLON EXTRACTION FROM BLENDED TEXTILE
[0001] FIELD OF THE DISCLOSURE
[0002] The present disclosure generally relates to blended textiles, and more particularly to selective nylon separation or extraction from one or more blended textiles.BACKGROUND
[0003] Reference to any prior art in the specification is not an acknowledgment or suggestion that this prior art forms part of the common general knowledge in any jurisdiction or that this prior art could reasonably be expected to be understood, regarded as relevant, and / or combined with other pieces of prior art by a skilled person in the art.
[0004] Nylon, silk-like and petroleum-based thermoplastic, is known for its strength, elasticity and lightweight. From women’s stockings to fishing nets and parachutes, nylon has been widely used in different industries including textiles, plumbing and military since its first appearance in the 1930s. In the textile industry today, nylon has been used for clothing and accessories such as sportswear, swimsuits and handbags. The production of this second-most-used synthetic fibre has increased from 3.74 million tons in 1990 to 5.4 million tons in 2020. It made up 5%of the global fibre market share in 2020.
[0005] It is estimated that ninety-two million tons of textile waste are generated globally each year. Currently, however, only a very limited percentage of 12%of the textile waste is recycled. The rest ends up being incinerated or disposed of in landfills, causing pollution to the environment and occupying valuable land space. Although there is a growing awareness of textile recycling and circular fashion supply chain, the recycled nylon remains as low as 1.9%due to technical challenges and the low cost of new nylon.
[0006] Many existing nylon recycling techniques focus on recycling of pre-consumer nylons and nylon fishing nets, due to the technology challenge on separating nylon from material mixture. Those processes rely largely on the depolymerization and repolymerization process, for which the energy consumption is high.SUMMARY
[0007] According to one or more embodiments, there is provided with a method for selective extracting nylon from one or more blended textiles. The method comprises: dissolving nylon from the one or more blended textiles into a nylon dissolution solvent to obtain a dissolved nylon solution; treating the dissolved nylon solution to obtain porous nylon clusters; and treating the porous nylon clusters to obtain nylon fibres.
[0008] Additionally or optionally, the nylon dissolution solvent comprises one or more inorganic salts, one or more aliphatic alcohols, and water.
[0009] Additionally or optionally, the mole fractions of the one or more inorganic salts, the one or more aliphatic alcohols, and the water are x, y, and (1-x-y) respectively, and wherein 0.05 ≤ x ≤ 0.12 and 0.25 ≤ y ≤ 0.95.
[0010] Additionally or optionally, the one or more inorganic salts is selected from a group consisting of calcium bicarbonate, calcium carbonate, calcium chloride, calcium iodide, calcium nitrate, calcium salicylate, calcium sulphate, lithium chloride, sodium thiocyanate, and zinc chloride.
[0011] Additionally or optionally, the one or more aliphatic alcohols is selected from a group consisting of methanol, ethanol, 1-propanol, and Iso-propanol.
[0012] Additionally or optionally, the step of preparing the nylon dissolution solvent comprises: agitating a mixture for 5 to 600 minutes, the mixture comprising the one or more inorganic salts, the one or more aliphatic alcohols, and water; performing adjustment to the mixture such that pH value ranges from 2 to 8, temperature ranges from 4℃ to 90℃, and metal ion concentration ranges from 0.1M to 3M in the mixture; and removing insoluble substances from the mixture.
[0013] Additionally or optionally, the step of dissolving nylon from the blended textile comprises: immersing the one or more blended textiles into the nylon dissolution solvent to obtain a textile solution having a bath ratio less than 1: 5; agitating the textile solution at a temperature from 4℃ to 90℃ and a pressure from 5kPa to 300kPa; and filtering out undissolved solid from the textile solution to obtain the dissolved nylon solution.
[0014] Additionally or optionally, the step of filtering out the undissolved solid comprises using a sieve or filter having pore size of 1μm to 1mm to perform filtration for 60 to 600 minutes.
[0015] Additionally or optionally, the step of agitating is performed by using one or more of the following: direct mixing with impeller and / or roller; direct gas bubbling; gas dispersion with jet, nozzle and / or porous sparger; and sonication.
[0016] Additionally or optionally, the dissolved nylon solution has a nylon concentration less than 50% (w / w) .
[0017] Additionally or optionally, the step of treating the dissolved nylon solution comprises: precipitating nylon from the dissolved nylon solution to obtain nylon slurry; filtering the nylon slurry to obtain separated nylon; modifying the separated nylon to obtain porous nylon clusters; and drying the porous nylon clusters to obtain dried porous nylon clusters.
[0018] Additionally or optionally, the step of precipitating nylon comprises: adding into the dissolved nylon solution at least 5%total volume of a precipitation buffer under agitation from 5 to 300 revolutions per minute (RPM) ; and heating the dissolved nylon solution at a temperature from 20℃ to 90℃ and a pressure from 5kPa to 300kPa.
[0019] Additionally or optionally, the precipitation buffer is a solution comprising one or more aliphatic alcohols or water.
[0020] Additionally or optionally, the content of the one or more aliphatic alcohols in the precipitation buffer is less than 70%.
[0021] Additionally or optionally, the step of filtering the nylon slurry comprises performing filtration by using a filter with a pore size ranging from 0.2μm to 1mm and at pressure from 5kPa to 400kPa.
[0022] Additionally or optionally, the step of modifying the separated nylon comprises adding at least 10%volume of a modification buffer to the dissolved nylon solution.
[0023] Additionally or optionally, the modification buffer is solution comprising one or more aliphatic alcohols, a dilute mild acid, water, or combination thereof.
[0024] Additionally or optionally, the content of the one or more aliphatic alcohols in the modification buffer is less than 50%.
[0025] Additionally or optionally, the dilute mild acid is selected from a group consisting of an acetic acid, a carbonic acid, and a citric acid.
[0026] Additionally or optionally, the concentration of the dilute mild acid is in the range of 0.016M to 0.5M.
[0027] Additionally or optionally, the step of drying the porous nylon clusters comprises performing the drying at a temperature from 60℃ to 80℃ with agitation from 5 to 300 RPM for 30 to 600 minutes.
[0028] Additionally or optionally, the method further comprises cooling the dried porous nylon clusters to a temperature falling within 20℃ to 40℃.
[0029] Additionally or optionally, the step of treating the porous nylon clusters comprises: drying, degassing, and pelletizing the porous nylon clusters to obtain nylon chips; dissolving the nylon chips to obtain polymer dopes; and spinning the polymer dopes to obtain the nylon fibres.
[0030] Additionally or optionally, the nylon fibres have molecular weight and degree of polymerisation in the range of ± 10%of virgin nylon.
[0031] Additionally or optionally, the nylon fibres have the following parameters: tensile strength ≥ 40 MPa; degree of polymerization > 100; glass transition temperature: 40℃ to 80℃; and melting temperature: 160℃ to 260℃.
[0032] Additionally or optionally, the method further comprises: collecting used solvent, the used solvent comprising one or more of residual nylon, dye residue, inorganic salts, aliphatic alcohols, and water; and separating and purifying the used solvent reuse through flocculation, sedimentation, membrane filtration, adsorption, reverse osmosis, and fractional distillation to obtain regenerated solvent for use as the nylon dissolution solvent.
[0033] Additionally or optionally, the nylon is one of nylon 5.6, nylon 6, or nylon 6.6.
[0034] Additionally or optionally, the one or more blended textiles comprise one or more materials selected from a group consisting of acrylic, polyester, polypropylene, spandex, cotton, hemp, linen, regenerated cellulosic fibre, silk, and wool.
[0035] Additionally or optionally, the blended textile is in the form of fibre, yarn, fabric, or garment.
[0036] According to one or more embodiments, there is provided with a system for extracting nylon from one or more blended textiles. The system comprises: a nylon dissolution module for dissolving nylon from the one or more blended textiles into a nylon dissolution solvent to obtain a dissolved nylon solution; a nylon modification module for treating the dissolved nylon solution to obtain porous nylon clusters; and a nylon regeneration module for treating the porous nylon clusters to obtain nylon fibres.
[0037] Additionally or optionally, the system further comprises a solvent regeneration module for that regenerating the nylon dissolution solvent from used solvent.
[0038] Additionally or optionally, the nylon dissolution module comprises: a textile feeder for receiving the one or more blended textiles; a solvent feeder for receiving the nylon dissolution solvent; a nylon dissolution unit for dissolving the nylon from the one or more blended textiles into the nylon dissolution solvent; a gas feeder for facilitating mixing of the blended textiles and the nylon dissolution solvent; a discharge for discharging the dissolved nylon solution from the nylon dissolution unit towards the nylon modification module; and a slurry pump for facilitating the discharging of the dissolved nylon solution towards the nylon modification module.
[0039] Additionally or optionally, the nylon modification module comprises: a mixing chamber for mixing the dissolved nylon solution and a precipitation buffer to obtain nylon slurry; a filtration unit for separating the nylon from liquid content in the nylon slurry to obtain separated nylon; a reaction chamber for mixing the separated nylon and a modification buffer under heating and agitation to obtain porous nylon clusters; a drying chamber for drying the porous nylon clusters to obtain dried porous nylon clusters; and a transporting means for transporting the dried porous nylon clusters to the nylon regeneration module.
[0040] Other example embodiments are discussed herein.BRIEF DESCRIPTION OF THE DRAWINGS
[0041] The detailed description is set forth with reference to the accompanying drawings. The drawings are provided for purposes of illustration only and merely depict example embodiments of the disclosure. The drawings are provided to facilitate understanding of the disclosure and shall not be deemed to limit the breadth, scope, or applicability of the disclosure. The drawings are not to scale, unless otherwise disclosed. Certain parts of the drawings are exaggerated for explanation purposes and shall not be considered limiting unless otherwise specified.
[0042] FIG. 1 is a flowchart illustrating a method for extracting nylon from one or more blended textiles according to certain embodiments of the present disclosure.
[0043] FIG. 2 is a flowchart illustrating preparation of a nylon dissolution solvent according to certain embodiments of the present disclosure.
[0044] FIG. 3 is a flowchart illustrating obtaining of a dissolved nylon solution according to certain embodiments of the present disclosure.
[0045] FIG. 4 is a flowchart illustrating obtaining of porous nylon clusters according to certain embodiments of the present disclosure.
[0046] FIG. 5 is a flowchart illustrating obtaining of nylon fibres according to certain embodiments of the present disclosure.
[0047] FIG. 6 illustrates a system for extracting nylon from one or more blended textiles according to certain embodiments of the present disclosure.
[0048] FIG. 7A illustrates a nylon dissolution module according to certain embodiments of the present disclosure.
[0049] FIG. 7B illustrates a nylon modification module according to certain embodiments of the present disclosure.
[0050] FIG. 8A illustrates a lab-scale machine for nylon dissolution according to certain embodiments of the present disclosure.
[0051] FIG. 8B illustrates operation flow of the lab-scale machine of FIG. 8A.
[0052] FIG. 9 depicts scanning electron microscope (SEM) images of cotton fiber (a) before and (b) after nylon extraction according to certain embodiments of the present disclosure.
[0053] FIG. 10 depicts SEM images of wool fiber (a) before and (b) after nylon extraction according to certain embodiments of the present disclosure.
[0054] FIG. 11 depicts SEM images of silk fiber (a) before and (b) after nylon extraction according to certain embodiments of the present disclosure.
[0055] FIG. 12 depicts SEM images of polyester fiber (a) before and (b) after nylon extraction according to certain embodiments of the present disclosure.
[0056] FIG. 13 depicts SEM images of acrylic fiber (a) before and (b) after nylon extraction according to certain embodiments of the present disclosure.
[0057] FIG. 14 depicts SEM images of spandex fiber (a) before and (b) after nylon extraction according to certain embodiments of the present disclosure.DETAILED DESCRIPTION
[0058] The present disclosure will now be described with reference to the following examples which should be considered in all respects as illustrative and non-restrictive.
[0059] Throughout the description and the claims, the words “comprise” , “comprising” , and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is to say, in the sense of “including, but not limited to” .
[0060] Furthermore, as used herein and unless otherwise specified, the use of the ordinal adjectives “first” , “second” , etc., to describe a common object, merely indicate that different instances of like objects are being referred to, and are not intended to imply that the objects so described must be in a given sequence, either temporally, spatially, in ranking, or in any other manner.
[0061] Example embodiments relate to improved method and system for nylon separation or extraction from one or more blended textiles that are technically advantageous over prior art techniques.
[0062] Many existing nylon recycling and / or bio-based processes focus on recycling pre-consumer waste, depolymerization and repolymerization of post-consumer textile waste, recycling fishing net and bio-based nylon synthesis, etc. These processes often utilize strong chemical and energy without selectively separating nylon from the collected waste. As such, these existing methods or systems are unsatisfactory in various aspects. One flaw lies in the resultant high energy consumption and operation cost due to the requirements of high operating temperature and pressure. Another is that harmful or toxic organic solvents are used to dissolve nylon-containing textiles. This, on one hand, causes environmental pollutions and human health concerns, and on the other hand, requires extra decontamination processes. A further disadvantage for the existing techniques is that only a limited type of nylons can be handled and recovered. A yet further disadvantage for the existing techniques lies in their limited unsatisfactory capacity. For example, before starting the recycling process, many existing techniques require the size of the textile sample is reduced by cutting or trimming. This is inconvenience and inefficient and also introduces extra processing steps.
[0063] Example embodiments solve one or more of these problems associated with the existing methods and systems and provide technical solutions with new designs.
[0064] One or more embodiments provide method and / or system that achieve selective extraction of nylon from one or more blended textiles. The one or more blended textiles may comprise various types of nylons, including but not limited to, nylon 5.6, nylon 6, or nylon 6.6. The nylon content as contained may vary from a very low percentage to a very high percentage. The nylon content as contained may be close to zero or 100%. In some embodiments, the one or more blended textiles comprises nylon only. In some embodiments, in addition to nylon, the one or more blended textiles may comprise one or more materials including but not limited to acrylic, polyester, polypropylene, spandex, cotton, hemp, linen, regenerated cellulosic fibre, silk, wool. In some other embodiments, the one or more blended textiles may comprise other materials. The one or more blended textiles may be in the form of fibre, yarn, fabric, or garment.
[0065] One or more embodiments separate nylon from any proper nylon-containing blended textile materials, including but not limited to nylon-PET blended materials, nylon-spandex-rayon blended materials, or nylon-cotton-silk-acrylic blended materials. One or more embodiments provide a robust method and / or system for selective nylon separation from any blended textile materials, which has significantly advanced the nylon recycling technology.
[0066] One or more embodiments dissolve nylon from whole garment directly, which is advantageous over existing techniques where the size of the textile sample has to be reduced by cutting or trimming before the recycling process starts. Further, chemical pre-treatment to remove coating material on the textile is not necessary. One or more embodiments remove finishing materials.
[0067] One or more embodiments provide a selective nylon dissolution method that utilises a mild and relatively environment friendly solvent without the need for high temperature (>100℃) and high pressure (> 300kPa) to separate nylon from blended textile (s) . For example, the solvent applied is prepared from raw materials which are much cheaper. As a result of the inexpensive raw materials and mild operating conditions, a reduced operation cost is achieved.
[0068] One or more embodiments extract or recover nylon from one or more blended textile samples with a mild solvent at mild operating temperature and pressure. For example, the operating temperature may be less than 100℃, such as in a range from 4℃ to 90℃, such as 4℃, 10℃, 20℃, 30℃, 40℃, 50℃, 60℃, 70℃, 80℃, 90℃, or any subset of the temperature range from 4℃ to 90℃. The operating pressure may range from 5kPa to 300kPa, such as 5kPa, 10kPa, 50kPa, 100kPa, 150kPa, 200kPa, 250kPa, 280kPa, 290kPa, 295kPa, 300kPa, or any subset of the pressure range from 5kPa to 300kPa.
[0069] One or more embodiments extract or recover nylon from one or more blended textile samples having different nylon content. The blended textile with any percentage of nylon content can be handled for nylon recovery. This contrasts with many existing nylon recycling processes that recycle pure nylon only (i.e., pre-consumer waste) . By way of example, a blended textile may comprise nylon and other materials of a significant proportion. Typical existing recycling methods, such as mechanical recycling, hydrolysis, methanolysis, glycolysis, or ammonolysis, are not selective, and therefore materials other than nylon may affect the recycling efficiency. The selective process according to one or more embodiments is able to dissolve nylon from any blended textile (such as Nylon / polyester, Nylon / acrylic, Nylon / Spandex, Nylon / cotton, or mixture of two or more thereof) . That is, one or more embodiments can extract nylon selectively from any mixture of textiles.
[0070] One or more embodiments provide a method of producing porous nylon clusters from the blended textile for purpose of nylon recovery or regeneration with improved efficiency. For example, a recycling rate of over 90%can be achieved, where the recycling rate refers to the “dry mass of nylon recovered after the whole process” per “dry mass of nylon in blended textile” × 100%.
[0071] According to one or more embodiments, the solvent and buffers used in the method and system can be reused with high recycling rate. This further improves the recycling efficiency and reduces the operation cost.
[0072] One or more embodiments provide a sustainable method and system for selective nylon separation and production of porous nylon clusters for nylon regeneration from one or more blended textiles. The dissolved nylon is treated for subsequent suitable spinning processes. The goal is to re-spin the recovered nylon for industrial textile applications and completing the circular supply chain. The low-cost and low-energy consumption system configuration serves as a good basis for industrial scale-up opportunities. Hence, it potentially enables environmental friendly large-scale textile recycling and reduction in the use of new fossil-based materials. Moreover, it contributes to reducing the old garments ending up in landfills which uses up valuable land space and causes pollution to the environment.
[0073] According to one or more embodiments, the system selectively separates and regenerates nylon from one or more blended textiles, which is integrated with five modules consisting of a nylon dissolution module, a nylon modification module, a nylon regeneration module, a solvent regeneration module and a solvent preparation module. The high selectivity of the solvent system enables to separate nylon from blended textiles efficiently and the system configuration allows blended textiles to be recycled in an environmental friendly way. In addition, it enables the recycled textile materials of satisfied tensile properties to be turned into new textiles or other applications by non-governmental organizations (NGOs) and interested third parties. Most of the used solvents and buffers can be recycled for reuse.
[0074] According to one or more embodiments, the nylon dissolution module treats the blended textiles by at least partially dissolving the nylon in them. The dissolution module is provided with feed inlets and outlets and is configured to accommodate nylon dissolution solvent. The nylon modification module precipitates nylon from the dissolved nylon solution, modifies nylon into porous nylon clusters and dries them. The nylon regeneration module utilizes the porous nylon clusters and spins them into regenerated nylon fibres. The solvent regeneration module recovers the used solvent from the system. With reference to FIGS. 1-5, a method for extracting nylon from a blended textile according to certain embodiments will be described below.
[0075] Referring to FIG. 1, block 102 states dissolving nylon from one or more blended textiles into a nylon dissolution solvent to obtain a dissolved nylon solution. The dissolved nylon solution may have a nylon concentration less than 50% (w / w) .
[0076] The nylon dissolution solvent may be made from inexpensive raw materials. By way of example, the nylon dissolution solvent may comprise one or more inorganic salts, one or more aliphatic alcohols, and a water. The mole fractions of the one or more inorganic salts, the one or more aliphatic alcohols, and the water are x, y, and (1-x-y) respectively, wherein 0.05 ≤ x ≤ 0.12 and 0.25 ≤ y ≤ 0.95. The one or more inorganic salts may be selected from a group consisting of calcium bicarbonate, calcium carbonate, calcium chloride, calcium iodide, calcium nitrate, calcium salicylate, calcium sulphate, lithium chloride, sodium thiocyanate, and zinc chloride. The one or more aliphatic alcohols may be selected from a group consisting of methanol, ethanol, 1-propanol, and Iso-propanol.
[0077] The nylon dissolution solvent may be prepared in various ways. FIG. 2 provides one example of such preparation. Block 202 states agitating a mixture that comprises one or more inorganic salts, one or more aliphatic alcohols, and water. The agitation may be performed in a stirred tank for 5 to 600 minutes. Block 204 states performing adjustment to the mixture, such that the conditions, properties, etc. of the mixture are placed in a desirable state. The present inventors have recognized that the dissolution efficiency is affected by parameters of pH value, temperature, and metal ion concentration of the mixture. To achieve improved or even optimal results, the adjustment may be such intended that the pH value of the mixture ranges from 2 to 8, the temperature ranges from 4℃ to 90℃, and the metal ion concentration ranges from 0.1M to 3M, where “M” refers to molar concentration. Block 206 states removing insoluble substances from the mixture. This may be done by proper mechanisms, such as filtration, centrifugation, etc. As a result, the nylon dissolution solvent is well-formed and ready for use in block 102.
[0078] An example of implementing block 102 is illustrated in FIG. 3. At block 302, the one or more blended textiles are immersed into the nylon dissolution solvent to obtain a textile solution. The present inventors have recognized that bath ratio is an important parameter for the textile solution, where the bath ratio refers to “weight of blended textile” per “weight of dissolution solvent” . The present inventors have recognized that to achieve an improved or optimal nylon extraction, the bath ratio in the textile solution is preferably less than 1: 5. When the bath ratio is 1: 5 or larger, albeit it is still workable, it would be less satisfactory as the mixture becomes very viscous and requires much more energy for agitation. At block 304, the textile solution is agitated. The agitation may be preferably performed at a temperature range from 4℃ to 90℃ and a pressure from 5kPa to 300kPa to facilitate the dissolution of nylon together with homogenization of the dissolved nylon and solvent. The agitation mechanism may comprise direct mixing with impeller and / or roller, direct gas bubbling or gas dispersion with jet, nozzle and / or porous sparger, and sonication. For gas bubbling or dispersion, the gas feed pressure is preferably larger than 100kPa to better the mixing performance. The gas source may be compressed air, nitrogen, carbon dioxide or oxygen. At block 306, the undissolved solid is filtered out from the textile solution. This may be performed by using a sieve or filter with pore size of 1μm to 1mm for 60 to 600 minutes. As a result, the dissolved nylon solution is realised.
[0079] Further, the undissolved solid may be rinsed with a solvent for 5 to 300 minutes at a temperature range from 4℃ to 90℃ to remove nylon and other solid residues from the undissolved solid to acquire nylon-free textile, which is a by-product that may be used for further processing. This by-product may be used for making new textiles or other proper applications. This by-product may be used to form one or more of the following, but not limited to: fibre, yarn, fabric and garment in acrylic, polyester, polypropylene, spandex, cotton, hemp, linen, regenerated cellulosic fibre, silk, wool, or mixture thereof.
[0080] Referring again to FIG. 1, block 104 states treating the dissolved nylon solution to obtain porous nylon clusters. An example of implementing block 104 is illustrated in FIG. 4. Block 402 states precipitating nylon from the dissolved nylon solution to obtain nylon slurry. By way of example, at least 5%total volume of a precipitation buffer may be added into the dissolved nylon solution under agitation from 5 to 300 revolutions per minute (RPM) , where 5%refers to the volume ratio of the precipitation buffer relative to the mixture of the buffer and the dissolved nylon solution. The precipitation buffer is a solution comprising one or more aliphatic alcohols or water. The content of the aliphatic alcohols in the precipitation buffer is less than 70% (weight ratio) . During addition of the precipitation buffer or after addition of the precipitation buffer, the dissolved nylon solution is heated at a temperature from 20℃ to 90℃ and a pressure from 5kPa to 300kPa. In some embodiments, the nylon slurry, comprising dissolved nylon, contains up to 50% (w / w) of nylon and requires agitation with a impeller at 10 to 150RPM, or sonication at 250 to 700 watts, or gas bubbling above 100kPa, or vertical / horizontal tank mechanical mixing, with a wash buffer at temperature from 20℃ to 60℃ and a pressure from 5kPa to 300kPa for 5 to 300 minutes to precipitate nylon from the slurry.
[0081] Block 404 states filtering the nylon slurry to obtain separated nylon. This may be performed by using a filter with a pore size ranging from 0.2μm to 1mm and at a pressure from 5kPa to 400kPa and / or vacuum from the filtrate side functioning as the filtration driving force. The filter may be made from stainless steel or polypropylene or PTFE or Alloy 22 or any other compatible material, with a pore size ranging from 0.2μm to 1mm.
[0082] Block 406 states modifying the separated nylon to obtain porous nylon clusters. For example, the modification may be performed by using at least 10%volume of a modification buffer to produce the porous nylon clusters by repeating re-slurry and filtration cycles under sufficient agitation from 5RPM to 300 RPM and assistance of heating at a temperature from 20℃ to 90℃ and a pressure from 5kPa to 300kPa. The modification buffer is a solution that may comprise one or more aliphatic alcohols, a dilute mild acid, water, or combination thereof. The content of the aliphatic alcohols in the modification buffer may be less than 50%(weight ratio) . When the dilute mild acid is used, it is selected from a group consisting of an acetic acid, a carbonic acid, and a citric acid. The concentration of the dilute mild acid in the modification buffer is in the range of 0.016M to 0.5M.
[0083] In some embodiments, the re-slurry is performed in a reaction chamber. In the reaction chamber, the retained nylon is mixed with the modification buffer subject to agitation at 5 to 200 RPM, a temperature from 20℃ to 60℃ and a pressure from 5 to 300kPa for 5 to 300 minutes. The modification and filtration process are repeated up to seven cycles to ensure the modification buffer is fully contacted with the separated nylon, such that the concentration of inorganic salts is reduced to less than 500 ppm, before drying at block 408.
[0084] Block 408 states drying the porous nylon clusters to obtained dried porous nylon clusters. This may be performed in a drying chamber at a temperature from 60℃ to 80℃with agitation from 5 to 300 RPM for 30 to 600 minutes. In some embodiments, the drying chamber de-moisturizes the porous nylon cluster at temperature from 60℃ to 200℃ by indirect heating from a jacket with hot water or steam or heat transfer oil, under agitation from 5 to 300 RPM for 30 to 600 minutes. In some embodiments, the dried porous nylon clusters are then cooled with chilling water and / or air flow to a temperature falling within 20℃ to 40℃. It would be understood that the processes of precipitation, filtration, modification and drying may be carried out in one integrated unit or separated equipment.
[0085] Referring again to FIG. 1, block 106 states treating the porous nylon clusters to obtain nylon fibres. The nylon fibres may have molecular weight and degree of polymerisation in the range of ± 10%of virgin nylon. The nylon fibres may have a tensile strength no less than 40 MPa, a degree of polymerization greater than 100, a glass transition temperature from 40℃ to 80℃, such as 70℃, and a melting temperature from 160℃ to 260℃.
[0086] An example of implementing block 106 is illustrated in FIG. 5. Block 502 states drying, degassing, and pelletizing the porous nylon clusters to obtain nylon chips. A nylon chip may be understood as a nylon particle with reduced size. For example, depending on pelletizing methods, a nylon chip may have an elliptical or cylindrical shape. The size may be no larger than 5mm x 5mm x 5mm, and the chip may be a non-porous solid. Block 504 states dissolving the nylon chips into polymer dopes. Polymer dopes are polymer (s) in liquid state for fiber spinning, where the dopes may be prepared either by dissolving polymer (s) into a solvent or melting them. Block 506 states spinning the polymer dopes to obtain the nylon fibres. For example, the step of spinning may be performed by melt spinning, or any other proper nylon spinning methods, such as wet spinning, dry spinning.
[0087] The solvent used after going through the process indicated by block 102 and / or 104 is used solvent. The used solvent may comprise one or more of residual nylon, dye residue, inorganic salts, aliphatic alcohols, and water. In some embodiments, the used solvent can be recycled. By way of example, the used solvent is collected in a holding tank, and then separated and purified for reuse through flocculation, sedimentation, membrane filtration, adsorption, reverse osmosis, and fractional distillation, etc. The salt concentration of the fraction of solvent is measured based on the physical parameters such as density, salinity, osmolarity, temperature and conductivity. The solvent comprises inorganic salts and aliphatic alcohols. Then it is mixed with water in a proper ratio. If necessary, raw materials (such as one or more inorganic salts, one or more aliphatic alcohols, and water) are added to the regenerated solvent to achieve the target solvent compositions, and ready for use as the nylon dissolution solvent in block 102.
[0088] Referring to FIG. 6, a system 600 is used to extract nylon from one or more blended textiles. The system 600 may perform one or more methods as described above, such as methods described with reference to FIGS. 1, 3, 4, and 5. The system 600 comprises a nylon dissolution module 620, a nylon modification module 640, and a nylon regeneration module 660. The nylon dissolution module 620 may perform one or more methods or steps as described above, such as methods or steps described with reference to block 102 and FIG. 3. The nylon modification module 640 may perform one or more methods or steps as described above, such as methods or steps described with reference to block 104 and FIG. 4. The nylon regeneration module 660 may perform one or more methods or steps as described above, such as methods or steps described with reference to block 106 and FIG. 5.
[0089] FIG. 7A illustrates a nylon dissolution module 720 according to certain embodiments of the present disclosure. The nylon dissolution module 720 may be a specific implementation of the nylon dissolution module 620 as described above.
[0090] The nylon dissolution module 720 comprises a textile feeder 722, a solvent feeder 724, a gas feeder 726, a nylon dissolution unit 730, a discharge 732, and a slurry pump 734. The feeders 722, 724 and 726 may be considered as inlets of the module 720. The discharge 732 may be considered as outlet of the module 720.
[0091] The textile feeder 722 may be called a sample feeder in some embodiments, and it feeds the nylon-containing blended textile into the nylon dissolution unit 730. The solvent feeder 724 fills the nylon dissolution module 730 with the prepared nylon dissolution solvent. The nylon dissolution unit 730 allows the nylon-containing blended textile to contact with the nylon dissolution solvent such that the blended textile is dissolved into the nylon dissolution solvent. The gas feeder 726 facilitates mixing of the blended textile and the nylon dissolution solvent. For example, the gas feeder 726 may be considered as a dispenser that provides sufficient mixing to enhance the contact between the nylon-containing blended textile and the nylon dissolution solvent. The discharge 732 discharges the dissolved nylon solution from the nylon modification module 720. The slurry pump 734 provides a drive force and facilitates the discharging of the dissolved nylon solution from the nylon dissolution unit 730 towards the nylon modification module.
[0092] It would be understood by those skilled in the art that the nylon dissolution module 720 may additionally or optionally comprise one or more utilities supply systems, such as gases supply and electricity, and one or more control and / or monitoring systems, such as temperature control loop, level sensor, pressure indicator, etc.
[0093] FIG. 7B illustrates a nylon modification module 740 according to certain embodiments of the present disclosure. The nylon modification module 740 may be a specific implementation of the nylon modification module 640 as described above.
[0094] The nylon modification module 740 comprises a mixing chamber 742, a filtration unit 744, a reaction chamber 746, a drying chamber 748, and a transporting means 750. The mixing chamber 742 enables blending of the dissolved nylon solution and a precipitation buffer to obtain nylon slurry. The filtration unit 744 separates the nylon from liquid content in the nylon slurry to obtain separated nylon. The reaction chamber 746 mixes the separated nylon and a modification buffer under heating and agitation to obtain porous nylon clusters. The drying chamber 748 dries the porous nylon clusters to obtain dried porous nylon clusters by removing moisture content from the porous nylon clusters. The transporting means 750 transports the dried porous nylon clusters to the nylon regeneration module. The transporting means 750 may be a conveyor belt, a mechanical arm, etc. These components may be configurated for batch, semi-batch, or continuous operations. One or more of them may be integrated into one compact unit capable of carrying out the same or similar duties.
[0095] It would be understood by those skilled in the art that the nylon modification module 740 may additionally or optionally comprise one or more utilities supply systems, such as gases supply and electricity, and one or more control and / or monitoring systems, such as temperature control cascade, pressure control and relief valve, level sensor, humidity transmitter, etc.
[0096] One or more embodiments provide a system for selective separation of nylon from blended textile or blended textiles, such as fibre, yarn, fabric and garment, but not limited to, and regenerate the separated nylon with high purity. The system comprises a nylon dissolution module for treating the textile materials so as to at least partially dissolve the nylon in the textile materials. The nylon dissolution module is provided with feed inlets and outlets and is configured to accommodate nylon dissolution solvent. The system further comprises a nylon modification module for precipitating nylon from the dissolved nylon solution, modifying the dissolved nylon solution into porous nylon cluster and drying the porous nylon clusters. Yet further the system comprises a nylon regeneration module that utilises the porous nylon clusters and spins the clusters into regenerated nylon fibres. The system may optionally comprise a solvent regeneration module that recovers the used solvent from the system.
[0097] According to one or more embodiments, the nylon blended textile is sorted and fed into a nylon dissolution unit through a sample feeder which prevents non-textile material from entering the system. Nylon from the blended textile is dissolved in the nylon dissolution unit under a monitored condition by mixing with the nylon dissolution solvent of a certain composition, which is prepared in the solvent preparation module. The nylon-free textiles are filtered out after the nylon dissolution and may be used for other applications.
[0098] In these embodiments, the homogeneous mixture of dissolved nylon and solvent is then fed into a porous nylon cluster preparation unit for nylon modification into porous nylon clusters through a process including nylon precipitation, filtration, modification and drying. The recovered nylon is precipitated from the homogeneous mixture by adding a precipitation buffer. The slurry containing recovered nylon is filtered. The recovered nylon is modified to produce porous nylon clusters by addition of modification buffer. The dried porous nylon clusters are transferred to the nylon regeneration module for further processing and spinning into recovered nylon fibres via various spinning methods.
[0099] In these embodiments, the solvent and buffer consumed in the nylon dissolution and modification process are collected after use and regenerated in the solvent regeneration module. For the regenerated solvent, the impurities are removed and the solvent components are separated into concentrated fractions. The regenerated solvent component fractions are transferred to the solvent preparation module and blended into solvents and buffers for various processes. Nylon dissolution solvent may be prepared in a solvent tank, nylon precipitation buffer may be prepared in a first buffer tank, and nylon modification buffer may be prepared in a second buffer tank.
[0100] Referring to FIGS. 8A and 8B, the present inventors have made a lab-scale machine 800 for nylon dissolution according to certain embodiments of the present disclosure. The machine 800 may operate to selectively extract nylon from a blended textile sample 80. FIG. 8A illustrates a dissolution chamber 802, wheels 803, rubber rollers 804, a gear box 806, and a discharge 808. FIG. 8B illustrate the operation process. The process flow is indicated by the arrow 810. A plurality of legends are illustrated including wall 811, wheel 803, gas sparger 813, rubber roller 804, stainless steel passive roller 815, impeller 816, and gear box 806. It would be appreciated that not all elements are illustrated or referred with reference numerals.
[0101] By way of example, for the operation, the blended textile sample 80 is first fed to the stainless steel dissolution chamber 803 via a set of rubber roller 804. The dissolution chamber 803 is filled with nylon dissolution solvent. The blended textile sample 80 is then loaded on stainless steel passive rollers 815 to increase the contact area with solvent in the chamber 802. Two impellers 816 are installed at the bottom of the dissolution chamber 802 to provide agitation. The roller speed, impeller agitation speed, temperature may be adjusted from the gear box 806, which has a Human Machine Interface (HMI) on the surface for user control. The pressure may be controlled physically via a mass flow control valve (not shown) . The illustrated machine 800 may be provided with a lid (not shown) to cover the open space of the equipment. After dissolution, nylon from the blended textile sample 80 is dissolved into liquid mixture, which may be discharged via a discharge valve of the discharge 808 at the bottom middle of the equipment and will be pumped to further process. The remaining sample mesh (blended textile without nylon) will then be removed via the other two set of rubber rollers.
[0102] FIG. 9 to FIG. 14 show SEM images of cotton, wool, silk, polyester, acrylic and spandex fibers before and after treatment according to certain embodiments. As demonstrated, nylon can be selectively dissolved and in the meanwhile no substantial effect is made on those non-nylon textile materials.
[0103] It will further be appreciated that any of the features in the above embodiments of the disclosure may be combined and are not necessarily applied in isolation from each other. Similar combinations of two or more features from the described embodiments or preferred forms of the disclosure can be readily made by one skilled in the art.
[0104] Unless otherwise defined, the technical and scientific terms used herein have the plain meanings as commonly understood by those skill in the art to which the example embodiments pertain. It will be appreciated by persons skilled in the art that numerous variations and / or modifications may be made to the above-described embodiments, without departing from the broad general scope of the present disclosure. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive.
Claims
1.A method for selective extracting nylon from one or more blended textiles, the method comprising:dissolving nylon from the one or more blended textiles into a nylon dissolution solvent to obtain a dissolved nylon solution;treating the dissolved nylon solution to obtain porous nylon clusters; andtreating the porous nylon clusters to obtain nylon fibres.2.The method of claim 1, wherein the one or more blended textiles comprise nylon and one or more of acrylic, polyester, polypropylene, spandex, cotton, hemp, linen, regenerated cellulosic fibre, silk, or wool,wherein preferably the nylon is one of nylon 5.6, nylon 6, or nylon 6.6,wherein preferably the one or more blended textiles are in the form of fibre, yarn, fabric, or garment,wherein preferably the nylon fibres have molecular weight and degree of polymerisation in the range of ± 10%of virgin nylon.3.The method of claim 1 or 2, wherein the nylon dissolution solvent comprises:one or more inorganic salts;one or more aliphatic alcohols; andwater,wherein mole fractions of the one or more inorganic salts, the one or more aliphatic alcohols, and the water are x, y, and (1-x-y) respectively,wherein preferably 0.05 ≤ x ≤ 0.12 and 0.25 ≤ y ≤ 0.95,wherein preferably the one or more inorganic salts is selected from a group consisting of calcium bicarbonate, calcium carbonate, calcium chloride, calcium iodide, calcium nitrate, calcium salicylate, calcium sulphate, lithium chloride, sodium thiocyanate, and zinc chloride,wherein preferably the one or more aliphatic alcohols is selected from a group consisting of methanol, ethanol, 1-propanol, and Iso-propanol.4.The method of claim 3, further comprising preparing the nylon dissolution solvent by:agitating a mixture for 5 to 600 minutes, the mixture comprising the one or more inorganic salts, the one or more aliphatic alcohols, and the water;performing adjustment to the mixture such that pH value ranges from 2 to 8, temperature ranges from 4℃ to 90℃, and metal ion concentration ranges from 0.1M to 3M in the mixture; andremoving insoluble substances from the mixture.5.The method of any one of the preceding claims, wherein the step of dissolving nylon from the one or more blended textiles comprises:immersing the one or more blended textiles into the nylon dissolution solvent to obtain a textile solution having a bath ratio less than 1: 5;agitating the textile solution at a temperature from 4℃ to 90℃ and a pressure from 5kPa to 300kPa; andfiltering out undissolved solid from the textile solution to obtain the dissolved nylon solution,wherein preferably the step of filtering out the undissolved solid comprises using a sieve or filter having pore size of 1μm to 1mm to perform filtration for 60 to 600 minutes.6.The method of claim 5, wherein the step of agitating the textile solution is performed by using one or more of the following:direct mixing with impeller and / or roller;direct gas bubbling;gas dispersion with jet, nozzle and / or porous sparger; andsonication.7.The method of any one of the preceding claims, wherein the dissolved nylon solution has a nylon concentration less than 50% (w / w) .8.The method of any one of the preceding claims, wherein the step of treating the dissolved nylon solution comprises:precipitating nylon from the dissolved nylon solution to obtain nylon slurry;filtering the nylon slurry to obtain separated nylon;modifying the separated nylon to obtain porous nylon clusters; anddrying the porous nylon clusters to obtain dried porous nylon clusters.9.The method of claim 8, wherein the step of precipitating nylon comprises:adding into the dissolved nylon solution at least 5%total volume of a precipitation buffer under agitation from 5 to 300 revolutions per minute (RPM) ; andheating the dissolved nylon solution at a temperature from 20℃ to 90℃ and a pressure from 5kPa to 300kPa,wherein preferably the precipitation buffer is a solution comprising one or more aliphatic alcohols or water,wherein preferably the content of the one or more aliphatic alcohols in the precipitation buffer is less than 70%.10.The method of claim 8 or 9, wherein the step of filtering the nylon slurry comprises performing filtration by using a filter with a pore size ranging from 0.2μm to 1mm and at pressure from 5kPa to 400kPa.11.The method of any one of claims 8 to 10, wherein the step of modifying the separated nylon comprises adding at least 10%volume of a modification buffer to the dissolved nylon solution,wherein preferably the modification buffer is solution comprising one or more aliphatic alcohols, a dilute mild acid, water, or combination thereof,wherein preferably the content of the one or more aliphatic alcohols in the modification buffer is less than 50%,wherein preferably the dilute mild acid is selected from a group consisting of an acetic acid, a carbonic acid, and a citric acid, andwherein preferably concentration of the dilute mild acid is in the range of 0.016M to 0.5M.12.The method of any one of claims 8 to 11, wherein the step of drying the porous nylon clusters comprises performing the drying at a temperature from 60℃ to 80℃ with agitation from 5 to 300 RPM for 30 to 600 minutes.13.The method of any one of claims 8 to 12, further comprising cooling the dried porous nylon clusters to a temperature falling within 20℃ to 40℃.14.The method of any one of the proceeding claims, wherein the step of treating the porous nylon clusters comprises:drying, degassing, and pelletizing the porous nylon clusters to obtain nylon chips;dissolving the nylon chips to obtain polymer dopes; andspinning the polymer dopes to obtain the nylon fibres.15.The method of any one of the proceeding claims, wherein the nylon fibres have the following parameters:tensile strength ≥ 40 MPa;degree of polymerization > 100;glass transition temperature: 40℃ to 80℃; andmelting temperature: 160℃ to 260℃.16.The method of any one of the proceeding claims, further comprising:collecting used solvent, the used solvent comprising one or more of residual nylon, dye residue, inorganic salts, aliphatic alcohols, and water; andseparating and purifying the used solvent reuse through flocculation, sedimentation, membrane filtration, adsorption, reverse osmosis, and fractional distillation to obtain regenerated solvent for use as the nylon dissolution solvent.17.A system for extracting nylon from one or more blended textiles, the system comprising:a nylon dissolution module for dissolving nylon from the one or more blended textiles into a nylon dissolution solvent to obtain a dissolved nylon solution;a nylon modification module for treating the dissolved nylon solution to obtain porous nylon clusters; anda nylon regeneration module for treating the porous nylon clusters to obtain nylon fibres.18.The system of claim 17, further comprising a solvent regeneration module for regenerating the nylon dissolution solvent from used solvent.19.The system of claim 17 or 18, wherein the nylon dissolution module comprises:a textile feeder for receiving the one or more blended textiles;a solvent feeder for receiving the nylon dissolution solvent;a nylon dissolution unit for dissolving nylon from the one or more blended textiles into the nylon dissolution solvent;a gas feeder for facilitating mixing of the one or more blended textiles and the nylon dissolution solvent;a discharge for discharging the dissolved nylon solution from the nylon dissolution unit towards the nylon modification module; anda slurry pump for facilitating the discharging of the dissolved nylon solution towards the nylon modification module.20.The system of any one of claims 17 to 19, wherein the nylon modification module comprises:a mixing chamber for mixing the dissolved nylon solution and a precipitation buffer to obtain nylon slurry;a filtration unit for separating the nylon from liquid content in the nylon slurry to obtain separated nylon;a reaction chamber for mixing the separated nylon and a modification buffer under heating and agitation to obtain porous nylon clusters;a drying chamber for drying the porous nylon clusters to obtain dried porous nylon clusters; anda transporting means for transporting the dried porous nylon clusters to the nylon regeneration module.
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