Bamboo reed graphene viscose fiber preparation method, blended yarn and blended yarn preparation method
By employing processes such as ozone oxidation, ultrasonic-assisted alkali treatment, and PEG coating, the problems of cellulose extraction and graphene dispersion in *Arundo donax* graphene viscose fiber were solved, resulting in high-performance viscose fiber that meets the needs of high-end applications.
Patent Information
- Application Number
- CN202511054951.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-29
- Publication Date
- 2025-12-02
AI Technical Summary
Existing technologies make it difficult to efficiently extract cellulose from Arundo donax and uniformly disperse graphene in the spinning solution, resulting in poor performance of Arundo donax graphene viscose fiber, which is difficult to meet the needs of high-end application scenarios.
Cellulose from Reishi mushroom was extracted using an ozone oxidation combined with an ultrasonic-assisted alkali treatment process. Graphene dispersion was prepared using a dispersion process combining PEG coating and ultrasonic exfoliation. The dispersion was then subjected to a three-cycle freeze-thaw treatment using an alkali/urea system, and finally wet spinning was performed in a sodium sulfate gradient coagulation bath.
This method improves the extraction efficiency and purity of Reed cellulose, ensures uniform dispersion of graphene in the spinning solution, solves the problem of spinneret clogging, and produces high-performance viscose fiber with excellent strength, electrical conductivity, and thermal conductivity.
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Figure CN121046969A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of fiber preparation technology, and in particular to a method for preparing Reed hyacinth graphene viscose fiber, blended yarn, and a method for preparing blended yarn. Background Technology
[0002] In the field of fiber materials, with the advancement of technology and the diversification of market demands, the development of novel fiber materials with superior performance has become a research hotspot. Viscose fiber, as an important regenerated cellulose fiber, possesses excellent moisture absorption, breathability, and softness, and is widely used in textiles, clothing, and medical and health fields. However, traditional viscose fiber has certain limitations in terms of strength and functionality, making it difficult to meet the needs of high-end applications.
[0003] Reed shoots (Prunus armeniaca) are a widely distributed herbaceous plant with advantages such as rapid growth, high yield, and low cost. Reed shoots are rich in cellulose, and using them as a raw material to prepare viscose fiber not only broadens the sources of fiber raw materials but also achieves efficient resource utilization. However, in addition to cellulose, reed shoots also contain impurities such as lignin and hemicellulose. How to efficiently extract cellulose from reed shoots and improve its purity is a key challenge in preparing high-performance reed shoot viscose fiber.
[0004] Graphene, as a novel nanomaterial, possesses excellent mechanical, electrical, and thermal properties. Combining graphene with viscose fiber holds promise for endowing viscose fiber with new functions, such as increased strength and conductivity, thereby expanding its application areas. However, the uniform dispersion of graphene in the spinning solution is a problem that urgently needs to be solved. Uneven dispersion can easily lead to spinneret blockage, affecting fiber preparation and performance.
[0005] Currently, existing technologies have shortcomings in the extraction of cellulose from *Arundo donax* and the dispersion of graphene in spinning solutions, making it difficult to prepare high-performance *Arundo donax* graphene viscose fibers. Summary of the Invention
[0006] The purpose of this invention is to provide a method for preparing *Arundo donax* graphene viscose fiber, a blended yarn, and a method for preparing the blended yarn, thereby solving the problem of poor performance of *Arundo donax* graphene viscose fiber.
[0007] To achieve the above objectives, the present invention provides a method for preparing Reed Root graphene viscose fiber, comprising the following steps:
[0008] S1. Extract cellulose from Phyllostachys amurensis, subject Phyllostachys amurensis to ozone and chemical treatment to obtain cellulose, and pulverize the cellulose to obtain cellulose powder with a particle size of 20-100 micrometers.
[0009] S2. Prepare graphene dispersion by ultrasonically dispersing graphene in a solution containing surfactant to obtain graphene dispersion.
[0010] S3. Prepare spinning solution by dissolving alfalfa cellulose powder in an alkali / urea solvent, then adding graphene dispersion to the alkali / urea solvent and mixing evenly to obtain spinning solution.
[0011] S4. Wet spinning: The spinning solution is extruded through the spinneret into the coagulation bath for molding to obtain viscose fiber.
[0012] Preferably, in step S1, the extraction of reed cellulose from reed includes the following specific steps:
[0013] S11. Cut the reed into strips, put the strips into deionized water, and introduce ozone into the deionized water to pre-treat the reed. After pre-treatment, wash and dry the reed.
[0014] S12. The pretreated Reed is placed in a NaOH solution with a mass concentration of 6wt.%-10wt.% for swelling treatment, and ultrasonic treatment is performed during the swelling process; the swelling treatment time is 40min-60min.
[0015] S13. After the swelling treatment, filter the reed and soak it in an ethanol solution with a solid-liquid ratio of 1:(3-8)g / mL, a soaking temperature of 50℃~80℃, and a treatment time of 1 hour~3 hours. After treatment, wash it clean with deionized water.
[0016] S14. The washed Reed is placed in a NaClO2 solution with a mass concentration of 6wt.%-10wt.% for treatment. The solid-liquid ratio is 1:5, the treatment temperature is 80℃~100℃, and the treatment time is 1h~3h. After treatment, it is washed with deionized water, filtered, and dried to obtain Reed cellulose.
[0017] Preferably, in S11, the ozone concentration is 110 mg / L to 150 mg / L, the liquid content of reed is 60% to 80%, the treatment time is 15 min to 25 min, and the pH value is 1.5 to 2.5.
[0018] Preferably, in step S2, the preparation of the graphene dispersion includes the following specific steps:
[0019] S21. Add graphene oxide powder to deionized water and place it in a magnetic stirrer for pre-dispersion to obtain a pre-dispersion solution.
[0020] The mass concentration of graphene oxide powder in deionized water is 0.08 g / ml to 0.12 g / ml, the speed of the magnetic stirrer is 500-1000 r / min, and the pre-dispersion time is 5 min to 10 min; wherein, the particle size of graphene oxide is 0.5 μm to 5 μm;
[0021] S22. Add the surfactant polyethylene glycol to the pre-dispersion liquid and stir for 5 min to 10 min to obtain a mixture; the mass ratio of polyethylene glycol to graphene oxide powder is 1:(3 to 7);
[0022] S23. Place the mixture into an ultrasonic reactor for intermittent ultrasonic dispersion treatment. The ultrasonic power is 300W-500W and the frequency is 30kHz-50kHz. The ultrasonic treatment time is 30min-120min, with a stop every 15min. After cooling, continue ultrasonic treatment to obtain a graphene dispersion with a sheet diameter of 0.5μm-5μm.
[0023] Preferably, in step S3, the preparation of the spinning solution includes the following specific steps:
[0024] S31. Prepare an alkali / urea solvent by mixing a 7wt.% to 9wt.% NaOH solution with a 12wt.% to 14wt.% urea solution, wherein the mass ratio of NaOH:urea:water is 7:12:81, and freezing the mixture at -12℃ to -8℃ for 2 to 3 hours to obtain the alkali / urea solvent.
[0025] S32. Add the cellulose from the reed to the alkali / urea solvent, stir, and then freeze at -12℃ to -8℃. After three cycles of freezing and thawing, centrifuge and take the supernatant. Add the graphene dispersion to the supernatant and mix evenly to obtain the spinning solution.
[0026] Preferably, in S32, the mass ratio of graphene oxide to reed cellulose is 1:19 to 3:17.
[0027] Preferably, in step S4, the wet spinning process includes the following specific steps:
[0028] S41. The spinning solution is metered by a metering pump and then squeezed out of the spinneret to form a fine stream. The fine stream is then coagulated in a coagulation bath to form nascent fibers.
[0029] The metering pump has a flow rate of 0.5cc / min to 1.0cc / min, the spinneret has an orifice diameter of 0.10mm to 0.20mm, and 30 to 50 orifices. The coagulation bath is an aqueous solution containing 100 to 120g / L sulfuric acid and 150 to 200g / L sodium sulfate, and the bath temperature is 25℃ to 35℃.
[0030] S42. The nascent fibers are stretched, shaped, wound, and air-dried to obtain viscose fibers;
[0031] The initial fiber drawing speed is 4m / min to 6m / min, the secondary drawing speed is 12m / min to 15m / min, the drawing temperature is 45℃ to 50℃, the take-up roller linear speed during winding is 12m / min to 15m / min, and the lateral spreading rate is 700m / min to 800m / min.
[0032] A blended yarn, wherein the mass ratio of fine cotton, camel hair and viscose fiber is (13-15):(20-22):(17-18).
[0033] The method for preparing the above-mentioned blended yarn includes the following steps:
[0034] S5. Camel hair impurity removal and degreasing treatment: loosening treatment of camel hair to obtain single-fiber camel hair.
[0035] Soak camel hair in water at 40℃-45℃ for 20-40 minutes, add 0.3%-0.6% nonionic surfactant by weight of camel hair, and stir; heat to 50℃-60℃, add 1%-3% sodium carbonate solution by weight of camel hair, and keep warm for 40-50 minutes; wash with water until neutral, and dry at 50℃-70℃ until the moisture regain is 12±1%; after treatment with an opening machine, monofibrillated camel hair is obtained.
[0036] S6. The viscose fiber filaments are processed by a cutting machine and then screened by a vibrating screen to obtain viscose short fibers of 35mm to 40mm.
[0037] S7. Perform static elimination treatment on viscose short fibers and monofibrillated camel hair.
[0038] S8. Fine cotton, single-fiber camel hair, and viscose staple fiber are processed through drawing, roving, and spinning to obtain blended yarn.
[0039] Preferably, in S8,
[0040] The drawing process includes single-layer drawing, double-layer drawing, and triple-layer drawing. The draft ratio of single-layer drawing / back zone draft ratio is 4.14 / 1.92, the draft ratio of double-layer drawing / back zone draft ratio is 5.57 / 1.51, and the draft ratio of triple-layer drawing / back zone draft ratio is 6.55 / 1.18. The spacing between single-layer and double-layer drawing is 12mm*20mm, and the spacing between triple-layer drawing is 8*18. The bell mouth diameter is 3.6mm.
[0041] The roving twist is 6.35 twists / 10m, the roving twist coefficient is 118, the roving evenness CV% is 4.79, the roving roller spacing is 9mm*23mm*35mm, the draft ratio / back zone draft ratio is 8.9 / 1.2, the spindle speed is 750r / min, and the nip is 4mm.
[0042] The yarn draft ratio / back zone draft ratio is 50.4 / 1.184, the roller spacing is 18mm*40mm, the spindle speed is 10550r / min, the yarn evenness CV% is 13.29, and the yarn twist coefficient is 403.
[0043] The advantages and positive effects of the method for preparing Reed Root Graphene Viscose Fiber, the blended yarn, and the method for preparing the blended yarn described in this invention are as follows:
[0044] 1. This invention achieves efficient separation of cellulose from lignin and hemicellulose in Reed spp. through ozone oxidation combined with ultrasonic-assisted alkali treatment, thereby improving the extraction efficiency and purity of Reed spp. spp. spp.
[0045] 2. This invention employs a dispersion process combining PEG coating and ultrasonic exfoliation, which improves the dispersibility of graphene and stabilizes the graphene sheet size within the range of 0.5μm-5μm, thus solving the problem that uneven dispersion of graphene in spinning solution easily leads to spinneret blockage.
[0046] 3. This invention employs an alkali / urea system to perform a three-cycle freeze-thaw treatment on Arundo donax cellulose, which improves the uniformity of dispersion of Arundo donax cellulose and graphene, increases the solubility of Arundo donax cellulose, and facilitates the increase of graphene addition; it also solves the problem of low graphene addition and easy clogging of spinnerets in viscose fiber.
[0047] 4. The present invention uses a sodium sulfate gradient coagulation bath and multi-stage stretching treatment, which is beneficial to improving the strength and toughness of viscose fibers.
[0048] 5. The viscose fiber prepared by this invention has a far-infrared emissivity > 0.88, a temperature rise of 2.1 ± 0.3℃, and a negative ion generation of 1200 ± 50 ions / cm². 3 The antibacterial rate against Escherichia coli / Staphylococcus aureus is >99%.
[0049] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description
[0050] Figure 1 This is a flowchart of an embodiment of the present invention;
[0051] Figure 2 SEM images of viscose fibers prepared in Example 1 and Comparative Example 1 of the present invention; (a) is a SEM image of viscose fiber in Example 1, (b) is a cross-sectional SEM image of viscose fiber in Example 1, (c) is a SEM image of viscose fiber in Comparative Example 1, and (d) is a cross-sectional SEM image of viscose fiber in Comparative Example 1.
[0052] Figure 3 SEM image of the blended yarn prepared in Example 1 of this invention;
[0053] Figure 4 The TG curve of the blended yarn prepared in Example 1 of this invention. Detailed Implementation
[0054] In this application, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains. In case of any inconsistency, the meaning set forth in this specification or derived from the content described herein shall prevail. Furthermore, the terminology used herein is for the purpose of describing embodiments of this application only and is not intended to limit the scope of this application.
[0055] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings.
[0056] like Figure 1 As shown, a method for preparing *Phyllostachys edulis* graphene viscose fiber includes the following steps:
[0057] S1. Extracting cellulose from Phyllostachys amurensis by subjecting Phyllostachys amurensis to ozone and chemical treatment to obtain cellulose from Phyllostachys amurensis.
[0058] The raw material for preparing viscose fiber spinning solution is α-cellulose, so cellulose extraction is a crucial step. Reed contains a variety of components, including cellulose, lignin and hemicellulose. By extracting cellulose and removing lignin and hemicellulose, the purity and quality of the fiber can be significantly improved, thereby producing high-performance viscose fiber.
[0059] The extraction of cellulose from Phyllostachys amurensis involves the following specific steps:
[0060] S11. Cut the reed into strips, place the strips in deionized water, and introduce ozone into the deionized water to pretreat the reed. After pretreatment, wash and dry the reed.
[0061] The ozone concentration was 110 mg / L–150 mg / L, the liquid retention rate of *Arundo donax* was 60%–80%, the treatment time was 15–25 min, and the pH value was 1.5–2.5. Drying was performed in an oven at 60℃. Ozone oxidation can directionally destroy the phenolic hydroxyl structure of lignin, removing lignin from *Arundo donax*.
[0062] S12. The pretreated reed is placed in a 6wt.%-10wt.% NaOH solution for swelling treatment, and ultrasonic treatment is performed during the swelling process. The swelling treatment time is 40min-60min.
[0063] Strong bases disrupt the glycosidic and hydrogen bonds in hemicellulose, forming soluble sodium salts and breaking down the intermolecular forces of hemicellulose. Ultrasonic waves at 80 kHz, relying on cavitation, increase the specific surface area of the contact between the fibers and the solution, accelerating the reaction process.
[0064] S13. After the swelling treatment, filter the reed and soak it in an ethanol solution with a solid-liquid ratio of 1:(3-8)g / mL, a soaking temperature of 50℃~80℃, and a treatment time of 1 hour~3 hours. After treatment, wash it clean with deionized water.
[0065] Ethanol can be used to further remove fat-soluble impurities from reed fiber and improve fiber purity.
[0066] S14. The washed reed is placed in a NaClO2 solution with a mass concentration of 6wt.%-10wt.%, with a solid-liquid ratio of 1:5, a treatment temperature of 80℃-100℃, and a treatment time of 1h-3h. After treatment, it is washed with deionized water, filtered, and dried to obtain reed cellulose. The reed cellulose is then pulverized into reed cellulose powder with a particle size of 20μm-100μm.
[0067] The phenolic hydroxyl groups in lignin are oxidized by ClO2 to quinone compounds, which further decompose into small molecule carboxylic acids or carbon dioxide. Oxidating the phenolic hydroxyl groups and aldehyde groups in lignin into soluble substances allows them to detach from the cellulose network, improving the purity of the fiber.
[0068] By employing an ozone-assisted, ultrasound-assisted alkali treatment process, efficient separation of cellulose from lignin and hemicellulose in Reed amurensis was achieved, with a removal rate of over 98% for fat-soluble impurities. After purification, the cellulose purity increased from 58±3% in the raw material to 92.5±1.2%, and the degree of polymerization retention rate was >95%, laying the foundation for the preparation of high-strength viscose fibers.
[0069] S2. Prepare a graphene dispersion by ultrasonically dispersing graphene in a solution containing a surfactant to obtain a graphene dispersion.
[0070] The preparation of graphene dispersion includes the following specific steps:
[0071] S21. Add graphene oxide powder to deionized water and place it in a magnetic stirrer for pre-dispersion to obtain a pre-dispersion solution.
[0072] The mass concentration of graphene oxide powder in deionized water was 0.08 g / ml to 0.12 g / ml, the magnetic stirrer speed was 500-1000 r / min, and the pre-dispersion time was 5 min to 10 min. The particle size of the graphene oxide was 0.5 μm to 5 μm.
[0073] S22. Add the surfactant polyethylene glycol to the pre-dispersion liquid and stir for 5 min to 10 min to obtain a mixture; the mass ratio of polyethylene glycol to graphene oxide powder is 1:(3 to 7).
[0074] PEG molecules fully coat the graphene oxide sheets, inhibiting π-π stacking and aggregation, and promoting the dispersion of graphene oxide.
[0075] S23. Place the mixture in an ultrasonic reactor for intermittent ultrasonic dispersion treatment, stopping for 5 minutes after every 15 minutes, cooling to <30℃, and then continuing. The ultrasonic power is 300W-500W, the frequency is 30kHz-50kHz, and the ultrasonic treatment time is 30min-120min, stopping once every 15 minutes, cooling, and then continuing ultrasonication to obtain a graphene dispersion with a sheet diameter of 0.5μm-5μm.
[0076] The micro-jet impact force generated by ultrasonic cavitation effect directionally disrupts the van der Waals forces between graphene oxide sheets, promoting the dispersion of graphene oxide.
[0077] By employing surfactant coating and ultrasonic dispersion, the sedimentation rate of the graphene dispersion after 72 hours of standing was less than 3%. Compared with the traditional mechanical stirring method, the agglomerate particle size was reduced from 28±5μm to 1.2±0.3μm, solving the problem of spinneret clogging caused by uneven dispersion of graphene in the spinning solution.
[0078] S3. Prepare the spinning solution by dissolving arundo cellulose in an alkali / urea solvent, then adding the graphene dispersion to the alkali / urea solvent and mixing them evenly to obtain the spinning solution.
[0079] The preparation of spinning solution includes the following specific steps:
[0080] S31. Prepare an alkali / urea solvent by mixing a 7wt.% to 9wt.% NaOH solution with a 12wt.% to 14wt.% urea solution, with a NaOH:urea:water mass ratio of 7:12:81. Freeze the mixture at -12℃ to -8℃ for 2 to 3 hours to obtain the alkali / urea solvent.
[0081] S32. Add the cellulose from the reed to the alkali / urea solvent, stir, and then freeze at -12℃ to -8℃. After three cycles of freezing and thawing, centrifuge and take the supernatant. Add the graphene dispersion to the supernatant and mix evenly to obtain the spinning solution.
[0082] The mass ratio of graphene oxide to reed cellulose is 1:19 to 3:17.
[0083] The dissolution of cellulose is essentially a synergistic process of hydrogen bond network reconstruction and low-temperature inclusion reaction. In this process, NaOH dissociates to produce OH- ions, which attack the hydrogen bonds between cellulose molecular chains to form sodium cellulose salt. Urea molecules form hydrogen-bonded inclusion complexes with cellulose hydroxyl groups through -NH2 groups, preventing the molecular chains from re-aggregating. At low temperatures of -12 to -8℃, urea combines with NaOH and water molecules to form cage-like hydrates, which encapsulate cellulose chains through van der Waals forces to form "worm-like micelles".
[0084] Conventional single-freezing methods have two major problems: first, the hydrogen bond network is incomplete, leading to uneven urea distribution and the formation of unbound fiber bundles larger than 100 nm in some areas; second, the dissolution efficiency is low, with only 78±5% dissolution rate for cellulose with a degree of polymerization >100,000, increasing the risk of residual fiber bundles clogging the spinnerets. A three-cycle deep freezing method is adopted, where a "freeze-thaw" cycle induces the stepwise growth of the hydrogen bond network, achieving the fully dissolved preparation of high molecular weight cellulose (degree of polymerization ≤372,000) in an alkali / urea system. This reduces the risk of spinneret clogging and improves the uniformity and spinnability of high-content graphene dispersions.
[0085] S4. Wet spinning: The spinning solution is extruded through the spinneret into the coagulation bath for molding to obtain viscose fiber.
[0086] Wet spinning includes the following specific steps:
[0087] S41. The spinning solution is metered by a metering pump and then extruded from the spinneret to form a fine stream. The fine stream is then coagulated in a coagulation bath to form nascent fibers.
[0088] The spinning solution is injected into a storage tank, which is set to room temperature and maintained at a pressure of 0.4–0.5 MPa. The solution is allowed to stand at this temperature and pressure for 20 minutes to ensure that dissolved gases can escape fully and reduce the generation of bubbles during the spinning process.
[0089] The metering pump has a flow rate of 0.5cc / min to 1.0cc / min, the spinneret has an orifice diameter of 0.10mm to 0.20mm, and 30 to 50 orifices. The coagulation bath is an aqueous solution containing 100 to 120g / L sulfuric acid and 150 to 200g / L sodium sulfate, and the bath temperature is 25℃ to 35℃.
[0090] S42. The nascent fibers are stretched, shaped, wound, and air-dried to obtain viscose fibers.
[0091] The initial fiber drawing speed is 4 m / min to 6 m / min, the secondary drawing speed is 12 m / min to 15 m / min, and the drawing temperature is 45℃ to 50℃. After both primary and secondary drawing, the fibers are dried and cured in an oven at a temperature of 45℃ to 50℃.
[0092] The take-up roller linear speed during winding is 12m / min to 15m / min, and the lateral spreading rate is 700m / min to 800m / min.
[0093] After being wound up, the viscose fiber filaments are placed in a ventilated environment and allowed to air dry naturally for more than 48 hours to ensure that the viscose fiber is completely dry, which facilitates subsequent processing and application.
[0094] By using a sodium sulfate gradient coagulation bath in conjunction with low-temperature multi-stage drafting, fiber orientation ≥85% and polymerization retention >90% were achieved. Through precise control of the winding and spreading rate and transverse shift ratio, functional yarns with a breaking strength ≥2.8 cN / dtex and far-infrared emissivity >0.88 were prepared, meeting the requirements for high-end textile weaving.
[0095] A blended yarn, wherein the mass ratio of fine cotton, camel hair and viscose fiber is (13-15):(20-22):(17-18).
[0096] The method for preparing blended yarn includes the following steps:
[0097] S5. Camel hair is degreased and cleaned by opening it to obtain single-fiber camel hair.
[0098] Camel hair, as a natural animal fiber, contains natural oils (approximately 1.5%-2.0%), exhibits excellent warmth retention, is soft and fluffy (fineness 18-22μm), and has strong moisture absorption (moisture regain 14%-16%), but it has relatively low strength and is prone to felting. Blending graphene viscose fiber with camel hair achieves complementary performance through "functional fiber reinforcement + natural fiber tuning," overcoming the bottleneck of single fibers being either "highly functional but lacking in comfort" or "good in warmth but low in strength."
[0099] The camel hair was soaked in water at 40℃-45℃ for 20-40 minutes, and a nonionic surfactant (Pingping O) at a mass ratio of 0.3%-0.6% was added. The mixture was gently stirred to remove dust and impurities. The temperature was then raised to 50℃-60℃, and a sodium carbonate solution at a mass ratio of 1%-3% was added. The mixture was kept at this temperature for 40-50 minutes for degreasing. The hair was washed with water until neutral and dried at 50℃-70℃ until the moisture regain was 12±1%. After processing with an opening machine, single-fiber camel hair was obtained, with the length uniformity increasing from 65% to 82%.
[0100] S6. Viscose fiber filaments are processed by a cutting machine and then sieved through a vibrating screen to obtain viscose staple fibers of 35mm to 40mm, with a length deviation of >±5% and a content of <3%. The viscose staple fibers are matched with camel hair fibers of average length of 35mm to 40mm.
[0101] S7. Perform static elimination treatment on viscose short fibers and monofibrillated camel hair. Add 0.8% antistatic agent, 1.3% wool oil, and leave for more than 12 hours to avoid delamination caused by the conductivity of graphene and the static electricity of camel hair.
[0102] S8. Fine cotton, single-fiber camel hair, and viscose staple fiber are processed through drawing, roving, and spinning to obtain blended yarn.
[0103] The drawing process includes single-row drawing (1 + 1 + 2 strands), double-row drawing, and triple-row drawing (6 strands). The draft ratio of the single-row drawing / back zone draft ratio is 4.14 / 1.92, the draft ratio of the double-row drawing / back zone draft ratio is 5.57 / 1.51, and the draft ratio of the triple-row drawing / back zone draft ratio is 6.55 / 1.18. The spacing between the single-row and double-row drawing is 12mm*20mm, and the spacing between the triple-row drawing is 8*18. The bell mouth diameter is 3.6mm.
[0104] The roving twist is 6.35 twists / 10m, the roving twist coefficient is 118, the roving evenness CV% is 4.79, the roving roller spacing is 9mm*23mm*35mm, the draft ratio / back zone draft ratio is 8.9 / 1.2, the spindle speed is 750r / min, and the nip is 4mm.
[0105] The yarn draft ratio / back zone draft ratio is 50.4 / 1.184, the roller spacing is 18mm*40mm, the spindle speed is 10550r / min, the yarn evenness CV% is 13.29, and the yarn twist coefficient is 403.
[0106] Example 1
[0107] A method for preparing Reed Root graphene viscose fiber includes the following steps:
[0108] S1. Extracting cellulose from Phyllostachys amurensis by subjecting Phyllostachys amurensis to ozone and chemical treatment to obtain cellulose from Phyllostachys amurensis.
[0109] The extraction of cellulose from Phyllostachys amurensis involves the following specific steps:
[0110] S11. Cut the reed into 3cm long strips, place the strips in deionized water, and introduce ozone into the deionized water to pretreat the reed. After pretreatment, wash and dry the reed.
[0111] The ozone concentration was 130 mg / L, the liquid content of the reed was 80%, the treatment time was 15 min, and the pH value was 2. The mixture was then dried in an oven at 60℃.
[0112] S12. The pretreated reed is placed in a 10 wt.% NaOH solution for swelling treatment, and ultrasonic treatment is performed during the swelling process. The ultrasonic frequency is 80 kHz. The swelling treatment time is 50 min.
[0113] S13. After the swelling treatment, filter the reed and soak it in an ethanol solution with a solid-liquid ratio of 1:5 g / mL, a soaking temperature of 60℃, and a treatment time of 2 hours. After treatment, wash it clean with deionized water.
[0114] S14. The washed Reed is placed in a NaClO2 solution with a mass concentration of 8 wt.% for treatment. The solid-liquid ratio is 1:5, the treatment temperature is 90℃, and the treatment time is 2h. After treatment, it is washed with deionized water, filtered, and dried to obtain Reed cellulose.
[0115] The dried arum cellulose is placed in a high-speed blender and stirred at high speed. The arum powder is then removed and placed in a dry place for later use. The powder particle size is 20μm to 100μm.
[0116] S2. Prepare a graphene dispersion by ultrasonically dispersing graphene in a solution containing a surfactant to obtain a graphene dispersion.
[0117] The preparation of graphene dispersion includes the following specific steps:
[0118] S21. Add graphene oxide powder to deionized water and place it in a magnetic stirrer for pre-dispersion to obtain a pre-dispersion solution.
[0119] Add 5.0 g of graphene oxide powder to 50-60 ml of deionized water and stir in a magnetic stirrer. The stirring speed of the magnetic stirrer is 500-1000 r / min, and the pre-dispersion time is 5 min to 10 min. The particle size of the graphene oxide is 0.5 μm to 5 μm.
[0120] S22. Add 1.0 g of surfactant polyethylene glycol to the pre-dispersion liquid and stir for 5 min to 10 min to obtain a mixture.
[0121] S23. Place the mixture in an ultrasonic reactor for intermittent ultrasonic dispersion treatment, stopping for 5 minutes after every 15 minutes, cooling to <30℃, and then continuing. The ultrasonic power is 300W-500W, the frequency is 30kHz-50kHz, and the ultrasonic treatment time is 30min-120min, stopping once every 15 minutes, cooling, and then continuing ultrasonication to obtain a graphene dispersion with a sheet diameter of 0.5μm-5μm.
[0122] S3. Prepare the spinning solution by dissolving arundo cellulose in an alkali / urea solvent, then adding the graphene dispersion to the alkali / urea solvent and mixing them evenly to obtain the spinning solution.
[0123] The preparation of spinning solution includes the following specific steps:
[0124] S31. Prepare an alkali / urea solvent by mixing a 7wt.% to 9wt.% NaOH solution with a 12wt.% to 14wt.% urea solution, with a NaOH:urea:water mass ratio of 7:12:81, and freezing at -12℃ for 2 hours to obtain the alkali / urea solvent.
[0125] S32. Add the cellulose of Reed Fiber to the alkali / urea solvent, stir for 10 min, then freeze at -12℃. After three cycles of freezing and thawing, centrifuge at 10000 r / min for 10 min and take the supernatant.
[0126] The graphene dispersion was added to the supernatant and mixed evenly to obtain the spinning solution.
[0127] S4. Wet spinning: The spinning solution is extruded through the spinneret into the coagulation bath for molding to obtain viscose fiber.
[0128] Wet spinning includes the following specific steps:
[0129] S41. The spinning solution is metered by a metering pump and then extruded from the spinneret to form a fine stream. The fine stream is then coagulated in a coagulation bath to form nascent fibers.
[0130] The spinning solution is injected into a storage tank, which is set to room temperature and maintained at a pressure of 0.4–0.5 MPa. The solution is allowed to stand at this temperature and pressure for 20 minutes to ensure that dissolved gases can escape fully and reduce the generation of bubbles during the spinning process.
[0131] The metering pump has a flow rate of 0.75 cc / min, the spinneret has an orifice diameter of 0.16 mm and 40 orifices, and the coagulation bath is an aqueous solution containing 100-120 g / L sulfuric acid and 150-200 g / L sodium sulfate, with a bath temperature of 25℃-35℃.
[0132] S42. The nascent fibers are stretched, shaped, wound, and air-dried to obtain viscose fibers.
[0133] The initial fiber drawing speed was 5.3 m / min, the secondary drawing speed was 13.3 m / min, and the drawing temperature was 45℃~50℃. After both the primary and secondary drawing processes, the fibers were dried and cured in an oven at a temperature of 45℃~50℃.
[0134] The take-up roller linear speed during winding is 13.3 m / min. The lateral spreading rate is 780 mm / min, and the lateral stroke is 100 mm / min.
[0135] After being rolled up, the viscose fiber filaments are placed in a ventilated environment and allowed to air dry naturally for at least 48 hours.
[0136] The graphene content in viscose fiber is 12.5% by mass.
[0137] A blended yarn, wherein the mass ratio of fine cotton, camel hair and viscose fiber is 14:21:17.7.
[0138] The method for preparing blended yarn includes the following steps:
[0139] S5. Camel hair is degreased and cleaned by opening it to obtain single-fiber camel hair.
[0140] The camel hair was soaked in water at 40℃-45℃ for 30 minutes, and then a nonionic surfactant (Pingping O) at a mass ratio of 0.5% was added. The mixture was gently stirred to remove dust and impurities. The temperature was raised to 55℃, and a sodium carbonate solution (pH = 10-11) at a mass ratio of 2% was added. The mixture was kept at this temperature for 45 minutes to degrease. The hair was washed with water until neutral and dried at 60℃ until the moisture regain was 12±1%. After processing with an opening machine, monofibrous camel hair was obtained.
[0141] S6. Viscose fiber filaments are processed by a cutting machine and then sieved through a vibrating screen to obtain viscose staple fibers of 35mm to 40mm, with a length deviation of >±5% and a content of <3%. The viscose staple fibers are matched with camel hair fibers of average length of 35mm to 40mm.
[0142] S7. Perform static elimination treatment on viscose short fibers and monofibrillated camel hair. Add 0.8% antistatic agent, 1.3% wool oil, and leave for more than 12 hours to avoid delamination caused by the conductivity of graphene and the static electricity of camel hair.
[0143] S8. Fine cotton, single-fiber camel hair, and viscose staple fiber are processed through drawing, roving, and spinning to obtain blended yarn.
[0144] The drawing process includes single-row drawing (1 + 1 + 2 strands), double-row drawing, and triple-row drawing (6 strands). The draft ratio of the single-row drawing / back zone draft ratio is 4.14 / 1.92, the draft ratio of the double-row drawing / back zone draft ratio is 5.57 / 1.51, and the draft ratio of the triple-row drawing / back zone draft ratio is 6.55 / 1.18. The spacing between the single-row and double-row drawing is 12mm*20mm, and the spacing between the triple-row drawing is 8*18. The bell mouth diameter is 3.6mm.
[0145] The roving twist is 6.35 twists / 10m, the roving twist coefficient is 118, the roving evenness CV% is 4.79, the roving roller spacing is 9mm*23mm*35mm, the draft ratio / back zone draft ratio is 8.9 / 1.2, the spindle speed is 750r / min, and the nip is 4mm.
[0146] The yarn draft ratio / back zone draft ratio is 50.4 / 1.184, the roller spacing is 18mm*40mm, the spindle speed is 10550r / min, the yarn evenness CV% is 13.29, and the yarn twist coefficient is 403.
[0147] Example 2
[0148] The difference between this embodiment and Embodiment 1 is that the graphene mass percentage in the viscose fiber of this comparative embodiment is 5%.
[0149] Comparative Example 1
[0150] The difference between this comparative example and Example 1 is that the graphene mass percentage in the viscose fiber of this comparative example is 25%.
[0151] Comparative Example 2
[0152] The difference between this comparative example and Example 1 is that no graphene is added to the viscose fiber in this comparative example.
[0153] Scanning electron microscopy was performed on the 12.5% graphene viscose fiber prepared in Example 1, and the results were as follows: Figure 2 As shown, (a) and (b) are regenerated cellulose fibers with a graphene content of 12.5%; (c) and (d) are regenerated cellulose fibers with a graphene content of 25%. In comparison, the former has a smoother surface and a more regular cross-sectional shape.
[0154] The 0% graphene viscose fiber prepared in Comparative Example 2 was subjected to scanning mechanical property and irritation tests. The tensile strength of the 0% graphene viscose fiber was 5.183 MPa, the four-point bending strength was 49.463 MPa, and the bending strength was 16.488 MPa. This indicates that the fiber matrix strength is limited and the bending length is short, which means that the fiber rigidity is low and it is prone to deformation damage due to external forces during weaving and use, and its shape retention is also poor.
[0155] The 5% graphene viscose fiber prepared in Example 2 was subjected to scanning mechanical property and irritation tests. The tensile strength of the 5% graphene viscose fiber was 4.995 MPa (slightly lower than that of pure viscose), the four-point bending strength was 47.663 MPa, and the bending strength was 15.888 MPa. The low proportion of graphene did not form an effective reinforcing network; instead, uneven dispersion led to a slight decrease in fiber mechanical properties, while the increased bending length indicated a slight increase in fiber rigidity. However, the overall mechanical properties were weakened, resulting in poor overall structural stability.
[0156] Scanning mechanical properties and irritation tests were performed on the 12.5% graphene viscose fiber prepared in Example 1. This proportion of graphene viscose fiber exhibited a tensile strength of 13.664 MPa (a 163% increase compared to the 0% proportion), a four-point bending strength of 130.388 MPa (a 164% increase), and a bending strength of 43.463 MPa (a 164% increase). The fiber achieved a balance between rigidity and toughness, with a moderate bending length, resulting in a fabric that possesses both good rigidity to maintain its shape and a certain degree of flexibility. Scanning mechanical properties and irritation tests were also performed on the 25% graphene viscose fiber prepared in Example 1. The 25% graphene viscose fiber showed a tensile strength of only 1.7086 MPa, a four-point bending strength of 18.063 MPa, and a bending strength of 5.1358 MPa. Excessive graphene aggregation led to fiber embrittlement, resulting in a significant decrease in mechanical properties and the longest bending length, indicating that the fabric was too rigid, lacked flexibility, and provided a poor user experience.
[0157] The mechanical properties of viscose fiber were tested, and the results are shown in Table 1.
[0158] Table 1 Mechanical properties of viscose fiber
[0159]
[0160] This table compares the mechanical properties of viscose fibers with different graphene proportions, all prepared using the same method. As shown in Table 1, a 12.5% graphene addition ratio results in a synergistic breakthrough in key mechanical properties such as tensile, bending, and shear strength, significantly outperforming ratios of 0% (pure viscose), 5%, and 25%. Tensile strength: 13.664 MPa at the 12.5% ratio, indicating that graphene can reinforce the viscose fiber matrix at this ratio. Four-point bending strength: 130.388 MPa, 2.64 times that of pure viscose (49.463 MPa), indicating that at the 12.5% ratio, graphene can be uniformly dispersed, significantly improving the fiber's resistance to bending deformation. Low ratio (5%): Due to insufficient graphene dispersion, it is difficult to form an effective reinforcing network, resulting in limited improvement in tensile and bending properties. High ratio (25%): Excessive graphene aggregation leads to deterioration of the fiber matrix structure, significantly reducing tensile, bending, and shear strengths.
[0161] By employing a refined graphene dispersion process, the optimal state of "uniform dispersion-moderate interweaving" of graphene in viscose fibers is achieved, avoiding agglomeration defects while fully leveraging its mechanical reinforcing effect. The strength, deformation, and elongation of the viscose fibers all far exceed conventional requirements.
[0162] Scanning electron microscopy was performed on the blended yarn prepared using Example 1, as shown in the results. Figure 3As shown in the electron microscope image, the distribution of graphene viscose fiber, cotton fiber, and camel hair fiber in the yarn is clearly visible. The different fibers are interwoven and intertwined, with no obvious fiber aggregation or separation. This indicates that, at a ratio of 14g / 21g / 17.7g, the Siro compact spinning process can fully integrate fibers with different properties. This uniform blended structure not only benefits the stability of the yarn's performance during subsequent processing but also ensures that the finished product evenly reflects the advantages of different fibers in all parts.
[0163] Graphene viscose fiber: Its unique structure and properties endow blended yarns with special functions. Electron micrographs show that the surface of graphene viscose fiber is smooth and has a certain degree of regularity, which brings good mechanical properties to the yarn, enhancing its strength and abrasion resistance. At the same time, the presence of graphene also endows the yarn with certain antibacterial and antistatic functions.
[0164] Cotton fiber: Under an electron microscope, the natural form of cotton fiber can be seen. Its natural wrinkles and other structures on the surface increase the moisture absorption and breathability of the yarn, giving the blended yarn the comfortable and skin-friendly characteristics of cotton fiber.
[0165] Camel hair: In electron micrographs, camel hair fibers appear fluffy and soft, providing excellent warmth retention for blended yarns. This gives the yarns a unique advantage in the field of thermal textiles, while their softness also enhances the feel of the yarns.
[0166] Thermogravimetric analysis was performed on the blended yarn of Example 1, and the TG curve of the blended yarn is shown below. Figure 4 As shown in the figure, the thermogravimetric (TG) and differential thermogravimetric (DTG) curves reveal that graphene viscose fibers exhibit excellent thermal stability and unique thermal decomposition behavior.
[0167] Low temperature range (<200℃): The TG curve is flat and the fiber weight loss rate is low, indicating that the material structure is stable under the medium and low temperature environment of conventional processing and use, and is not prone to deterioration due to heat. It is suitable for the heat processing needs of multiple scenarios such as textiles and light industry, and ensures the consistency of product performance.
[0168] Thermal decomposition range (200-400℃): The DTG curve shows a concentrated weight loss peak, indicating that the main fiber components decompose rapidly within a relatively narrow temperature range. This characteristic reflects the regulatory effect of graphene on the thermal response of the viscose matrix.
[0169] High-temperature residue (>600℃): The final residue rate reached 16.19%, which is significantly higher than that of ordinary viscose fiber (pure viscose has almost no residue). This confirms the stabilizing skeletal role of graphene at high temperatures and indicates that the material can retain part of the carbon structure after carbonization, providing a basis for the subsequent derivation of carbon materials.
[0170] The blended yarn prepared in the above embodiments is woven using the following steps:
[0171] (1) Weaving preparation
[0172] The prepared blended yarn is installed on a circular knitting machine, specifically a double-cylinder knitting machine with a 4-way loop-forming system. Based on the structural characteristics of the double-ribbed fabric, the needle configuration is adjusted to ensure the upper and lower cylinder needles are staggered. Simultaneously, the yarn feed tension is set to 3-5 cN to ensure uniform yarn tension during weaving and prevent loose or tight yarn phenomena.
[0173] (2) Weaving process
[0174] Start the knitting machine and set the speed to 18-20 r / min. Weave according to the double-rib structure pattern: the needles of the upper and lower cylinders alternate loops, knitting one row per pass. Through this cycle, a double-rib structure is formed, consisting of two front loops and two back loops alternating. During weaving, monitor the fabric density and appearance quality in real time. Adjust the yarn bend angle and yarn feed to control the warp density at 30-32 rows / 10cm and the weft density at 40-42 rows / 10cm, ensuring a uniform and tight fabric structure.
[0175] (3) Post-processing
[0176] The woven double-ribbed fabric undergoes a softening and setting treatment. A 2% polyurethane softener solution (adjusted to pH 5-6) is prepared with a liquor ratio of 1:20 and treated at 40℃ for 20 minutes to reduce the fabric surface friction coefficient, improve hand smoothness, and decrease the fabric bending stiffness from 2.5 cN·cm to 1.8 cN·cm. To further enhance the fabric's anti-felt shrinkage performance, a 0.5% protease treatment (50℃, 30 minutes) combined with a 1% low-formaldehyde resin finishing can be applied to control the fabric felt shrinkage rate to below 5%, meeting the requirements for machine washing and other uses.
[0177] The fabrics woven using the blended yarns described in the above embodiments were subjected to an itching test, and the test results are shown in Table 2.
[0178] Table 2 Results of Fabric Itching Test
[0179] Bending length (mm) 0% graphene 21.5 5% graphene 23.5 12.5% graphene 22.5 25% graphene 25
[0180] The test data above shows that after adding graphene viscose fiber to blended fabrics, the bending length of the fabric adjusts with the graphene content. Overall, the blended fabric prepared with graphene viscose fiber containing 12.5% graphene has a better itch-relieving effect compared to blended fabrics with other proportions. This is because the blending of viscose fiber and camel hair, through the complementary properties between the fibers (the softness and fluffiness of camel hair alleviates the stiffness of graphene viscose fiber, and the blending process reduces the exposure of fiber ends), suppresses the itch-relieving sensation when the fabric comes into contact with the skin to a certain extent, thus possessing good potential for wearing comfort. When the graphene content is 25% and 5%, the bending length reaches 25mm and 23.5mm respectively, significantly higher than the 21.5mm when no graphene is added (0%). This indicates that at this proportion, the fabric can exhibit a more obvious itch-relieving sensation and is more uncomfortable to wear. In Example 1, when the graphene content was 12.5%, the bending length was 22.5 mm. Due to the increased graphene content, the surface morphology or roughness of the fiber may have changed to some extent. Some testers began to feel a slight itching sensation, but it was still within an acceptable range. This is because the special structure of graphene generates more friction points when in contact with the skin than pure viscose fiber, but the overall impact is not significant.
[0181] Far-infrared tests were conducted on the fabric woven from the blended yarn of Example 1, and the results are shown in Table 3.
[0182] Table 3 Far-infrared test results of the blended yarn fabric from Example 1
[0183] time fabric 0min 24.6℃ 1min 41.4℃ 2min 43.4℃ 3min 45.5℃ 4min 46.8℃ 5min 47.3℃ 6min 47.8℃ 7min 48.5℃ 8min 48.8℃ 9min 49℃ 10min 49℃
[0184] As shown in Table 3, the temperature of the fabric exhibits a stepwise upward trend under far-infrared radiation: the heating rate is rapid from 0 to 3 minutes, then gradually slows down, stabilizing at 49℃ after 10 minutes. This phenomenon indicates that after graphene viscose fiber is blended with camel hair, thanks to the excellent far-infrared emission characteristics of graphene and the heat-insulating structure of camel hair, the fabric can quickly absorb external far-infrared energy and convert it into heat energy, and has good heat retention capacity, verifying the effectiveness of its far-infrared heat storage performance.
[0185] Therefore, the method for preparing Arundo donax graphene viscose fiber, the blended yarn, and the blended yarn preparation method described in this invention can solve the problem of poor performance of Arundo donax graphene viscose fiber and has very good warmth retention.
[0186] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention, and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.
Claims
1. A method for preparing *Arundo donax* graphene viscose fiber, characterized in that, Includes the following steps: S1. Extract cellulose from Reed sphagnum moss, subject Reed sphagnum moss to ozone and chemical treatment to obtain cellulose, and then pulverize the cellulose to obtain cellulose powder. S2. Prepare graphene dispersion by ultrasonically dispersing graphene in a solution containing surfactant to obtain graphene dispersion. S3. Prepare spinning solution by dissolving alfalfa cellulose powder in an alkali / urea solvent, then adding graphene dispersion to the alkali / urea solvent and mixing evenly to obtain spinning solution. S4. Wet spinning: The spinning solution is extruded through the spinneret into the coagulation bath for molding to obtain viscose fiber.
2. The method for preparing *Phyllostachys edulis* graphene viscose fiber according to claim 1, characterized in that, In step S1, the extraction of cellulose from *Arundo donax* includes the following specific steps: S11. Cut the reed into strips, put the strips into deionized water, and introduce ozone into the deionized water to pre-treat the reed. After pre-treatment, wash and dry the reed. S12. The pretreated Reed is placed in a NaOH solution with a mass concentration of 6wt.%-10wt.% for swelling treatment, and ultrasonic treatment is performed during the swelling process; the swelling treatment time is 40min-60min. S13. After the swelling treatment, filter the reed and soak it in an ethanol solution with a solid-liquid ratio of 1:(3-8)g / mL, a soaking temperature of 50℃~80℃, and a treatment time of 1 hour~3 hours. After treatment, wash it clean with deionized water. S14. The washed Reed is placed in a NaClO2 solution with a mass concentration of 6wt.%-10wt.% for treatment. The solid-liquid ratio is 1:5, the treatment temperature is 80℃~100℃, and the treatment time is 1h~3h. After treatment, it is washed with deionized water, filtered, and dried to obtain Reed cellulose. The Reed cellulose is then crushed into Reed cellulose powder with a particle size of 20μm~100μm.
3. The method for preparing *Phyllostachys edulis* graphene viscose fiber according to claim 2, characterized in that: In S11, the ozone concentration is 110 mg / L to 150 mg / L, the liquid coverage rate of reed is 60% to 80%, the treatment time is 15 min to 25 min, and the pH value is 1.5 to 2.
5.
4. The method for preparing *Phyllostachys edulis* graphene viscose fiber according to claim 1, characterized in that: In step S2, the preparation of the graphene dispersion includes the following specific steps: S21. Add graphene oxide powder to deionized water and place it in a magnetic stirrer for pre-dispersion to obtain a pre-dispersion solution. The mass concentration of graphene oxide powder in deionized water is 0.08 g / ml to 0.12 g / ml, the speed of the magnetic stirrer is 500-1000 r / min, and the pre-dispersion time is 5 min to 10 min; wherein, the particle size of graphene oxide is 0.5 μm to 5 μm; S22. Add the surfactant polyethylene glycol to the pre-dispersion liquid and stir for 5 min to 10 min to obtain a mixture; the mass ratio of polyethylene glycol to graphene oxide powder is 1:(3 to 7); S23. Place the mixture into an ultrasonic reactor for intermittent ultrasonic dispersion treatment. The ultrasonic power is 300W-500W and the frequency is 30kHz-50kHz. The ultrasonic treatment time is 30min-120min, with a stop every 15min. After cooling, continue ultrasonic treatment to obtain a graphene dispersion with a sheet diameter of 0.5μm-5μm.
5. The method for preparing *Phyllostachys edulis* graphene viscose fiber according to claim 1, characterized in that: In step S3, the preparation of the spinning solution includes the following specific steps: S31. Prepare an alkali / urea solvent by mixing a 7wt.% to 9wt.% NaOH solution with a 12wt.% to 14wt.% urea solution, wherein the mass ratio of NaOH:urea:water is 7:12:81, and freezing the mixture at -12℃ to -8℃ for 2 to 3 hours to obtain the alkali / urea solvent. S32. Add the cellulose from the reed to the alkali / urea solvent, stir, and then freeze at -12℃ to -8℃. After three cycles of freezing and thawing, centrifuge and take the supernatant. Add the graphene dispersion to the supernatant and mix evenly to obtain the spinning solution.
6. The method for preparing *Phyllostachys edulis* graphene viscose fiber according to claim 1, characterized in that: In S32, the mass ratio of graphene oxide to reed cellulose is 1:19 to 3:
17.
7. The method for preparing *Phyllostachys edulis* graphene viscose fiber according to claim 1, characterized in that: In step S4, wet spinning includes the following specific steps: S41. The spinning solution is metered by a metering pump and then squeezed out of the spinneret to form a fine stream. The fine stream is then coagulated in a coagulation bath to form nascent fibers. The metering pump has a flow rate of 0.5cc / min to 1.0cc / min, the spinneret has an orifice diameter of 0.10mm to 0.20mm, and 30 to 50 orifices. The coagulation bath is an aqueous solution containing 100 to 120g / L sulfuric acid and 150 to 200g / L sodium sulfate, and the bath temperature is 25℃ to 35℃. S42. The nascent fibers are stretched, shaped, wound, and air-dried to obtain viscose fibers; The initial fiber drawing speed is 4m / min to 6m / min, the secondary drawing speed is 12m / min to 15m / min, the drawing temperature is 45℃ to 50℃, the take-up roller linear speed during winding is 12m / min to 15m / min, and the lateral spreading rate is 700m / min to 800m / min.
8. A blended yarn, characterized in that: Including the viscose fiber as described in any one of claims 1-7, wherein the mass ratio of fine cotton, camel hair and viscose fiber is (13-15):(20-22):(17-18).
9. A method for preparing blended yarn as described in claim 8, characterized in that, Includes the following steps: S5. Camel hair impurity removal and degreasing treatment: loosening treatment of camel hair to obtain single-fiber camel hair. Soak in water at 40℃-45℃ for 20-40 minutes, add 0.3%-0.6% nonionic surfactant by weight of camel hair, and stir. Heat to 50℃~60℃, add sodium carbonate solution with a mass ratio of 1%~3% of camel hair, keep warm for 40min-50min; wash with water until neutral, dry at 50℃~70℃ until moisture regain is 12±1%; after treatment with an opening machine, obtain monofibrillated camel hair. S6. The viscose fiber filaments are processed by a cutting machine and then screened by a vibrating screen to obtain viscose short fibers of 35mm to 40mm. S7. Perform static elimination treatment on viscose short fibers and monofibrillated camel hair. S8. Fine cotton, single-fiber camel hair, and viscose staple fiber are processed through drawing, roving, and spinning to obtain blended yarn.
10. The method for preparing blended yarn according to claim 9, characterized in that: In S8, The drawing process includes single-layer drawing, double-layer drawing, and triple-layer drawing. The draft ratio of single-layer drawing / back zone draft ratio is 4.14 / 1.92, the draft ratio of double-layer drawing / back zone draft ratio is 5.57 / 1.51, and the draft ratio of triple-layer drawing / back zone draft ratio is 6.55 / 1.
18. The spacing between single-layer and double-layer drawing is 12mm*20mm, and the spacing between triple-layer drawing is 8*18. The bell mouth diameter is 3.6mm. The roving twist is 6.35 twists / 10m, the roving twist coefficient is 118, the roving evenness CV% is 4.79, the roving roller spacing is 9mm*23mm*35mm, the draft ratio / back zone draft ratio is 8.9 / 1.2, the spindle speed is 750r / min, and the nip is 4mm. The yarn draft ratio / back zone draft ratio is 50.4 / 1.184, the roller spacing is 18mm*40mm, the spindle speed is 10550r / min, the yarn evenness CV% is 13.29, and the yarn twist coefficient is 403.