Antibacterial and anti-mite oyster shell fiber with washable, moisture absorption and moisture release, and antistatic multifunction and preparation method thereof
By pre-treating, activating, and modifying oyster shells, a composite of regenerated oyster micro-powder and active synthetic fiber masterbatch was prepared, which solved the problem of organic matter loss in oyster shells and realized the preparation of multifunctional oyster fiber with antibacterial and anti-mite properties, washability, moisture absorption and wicking, and antistatic properties, thus improving the performance and functional durability of the fiber.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- QINGDAO BANGTE ECOLOGICAL TEXTILE TECH CO LTD
- Filing Date
- 2023-10-20
- Publication Date
- 2026-06-05
AI Technical Summary
In existing technologies, the organic matter in oyster shells is easily damaged during the spinning process, resulting in fibers containing almost no biological activity, severe loss of organic matter, and reduced antibacterial and anti-mite properties, failing to meet multiple functional requirements.
By pretreating, activating, and modifying oyster shells, regenerated oyster micro powder is prepared and then compounded with active synthetic fiber masterbatch to enhance the stability and adhesion of organic matter, thus producing oyster fiber that is antibacterial, anti-mite, washable, moisture-wicking, and antistatic.
It improves the stability and adhesion of organic matter in oyster fiber, enhances the antibacterial, anti-mite, and antistatic properties of the fiber, and improves the moisture absorption and wicking effect, meeting the standards for multi-functional textiles.
Abstract
Description
Technical Field
[0001] This invention relates to the field of functional fiber technology, specifically to a shellfish fiber with multiple functions including antibacterial and anti-mite properties, washability, moisture absorption and wicking, and antistatic properties, and its preparation method. Background Technology
[0002] Oyster shells are abundant, inexpensive, and readily available. They contain not only large amounts of calcium carbonate but also trace elements such as magnesium, potassium, molybdenum, phosphorus, manganese, iron, and zinc, as well as organic matter, making them highly valuable. Processing oyster shells into oyster fiber with antibacterial and anti-mite properties can meet a wider range of needs, while simultaneously turning waste into treasure, thus generating significant social and environmental benefits.
[0003] The patent with patent number "CN202010765516.0" entitled "An Oyster Fiber" describes a method for preparing oyster fiber: using oyster shells as raw material for calcium carbonate, a flexible template in a gel state is constructed using chitosan. Under the control and guidance of the flexible template, aragonite-phase calcium carbonate is synthesized. The use of ω-aminoalkanoic acid effectively transforms the aragonite-phase calcium carbonate into needle-shaped calcium carbonate particles, which are then mixed with polyester chips, granulated, and spun into fibers. However, the organic matter contained in oyster shells is easily damaged during the spinning process, resulting in fibers containing almost no bioactive organic matter. This causes a great waste of biological resources and further reduces the antibacterial and anti-mite properties of the oyster fiber. To obtain multifunctional oyster fiber, technicians can only add various finishing agents, such as antibacterial agents, hygroscopic agents, anti-mite agents, and antistatic agents, but this does not meet modern R&D concepts and consumer demands. Therefore, how to enhance the stability of organic matter in oyster shells during the spinning process has become a technical problem that the textile industry urgently needs to solve. Summary of the Invention
[0004] To address the problems existing in the prior art, this invention provides a multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties, as well as its preparation method, achieving the following objectives:
[0005] 1. Pre-treat and modify oyster shells to enhance the stability of organic matter in the shells and improve their adhesion to the synthetic fiber matrix, thus solving the problem of easy loss of organic matter in oyster shells during the preparation of synthetic fibers;
[0006] 2. The prepared recycled oyster micro powder has a uniform particle size distribution (D90 < 1 μm) and good affinity with the synthetic fiber matrix. Without affecting the mechanical properties of the synthetic fiber itself, it also endows the synthetic fiber with good antibacterial, anti-mite, water-washable, and antistatic properties. At the same time, it also improves the moisture absorption and wicking effect of the synthetic fiber and expands the application range of the synthetic fiber.
[0007] 3. The obtained active synthetic fiber masterbatch has good interaction and affinity with the surface of regenerated shellfish micro powder, which further enhances the adhesion of organic matter in shellfish shells to the fiber masterbatch.
[0008] To solve the above technical problems, the present invention adopts the following technical solution:
[0009] The first aspect of this invention provides a multifunctional shellfish fiber that is antibacterial, anti-mite, washable, moisture-wicking, and antistatic. The raw materials for preparation include the following components by weight: 5-15 parts of regenerated shellfish micro powder and 90-120 parts of active synthetic fiber masterbatch.
[0010] The second aspect of this invention provides a method for preparing multifunctional shellfish fiber that is antibacterial, anti-mite, washable, moisture-wicking, and antistatic, comprising the following steps:
[0011] S1. Preparation of regenerated shellfish micro powder
[0012] S11. Preprocessing
[0013] After drying the recycled shellfish coarse powder to 10μm at 60-90℃ for 10-15h, add 6-10wt% NaOH aqueous solution and ultrasonically disperse for 1.5-2.5h. Then heat and stir at 70-80℃ for 6-8h, adjust the pH to 6.5-7.5, wash, filter and dry, and then grind the dried shellfish coarse powder in a stirred ball mill for 15-20h to obtain pretreated shellfish micro powder.
[0014] S12. Activation
[0015] The pretreated oyster micro powder described in S11 is placed in an ethanol aqueous solution with a volume fraction of 75%, ultrasonically dispersed at 70-80℃ for 1-2 hours, and then cooled to room temperature to obtain an ethanol aqueous solution of activated oyster micro powder.
[0016] S13. Modification
[0017] Add a modifier to the ethanol-water solution of activated oyster shellfish powder, slowly heat to 45-75℃, control the pH at 7-8 at a speed of 900-1500 r / min, stir for 20-40 min, then filter and wash, and keep the filter residue at 45-75℃ for 10-15 h to obtain the regenerated oyster shellfish powder.
[0018] As a preferred technical solution of the present invention, the particle size distribution of the pretreated oyster shell micro powder in S11 is D90 < 1 μm. By strictly controlling the particle size of the recovered coarse oyster shell powder, while ensuring the removal of the outer organic layer of the oyster shell containing various impurities, the organic structure of the innermost layer of the shell is completely preserved, providing a foundation for the multiple functions of oyster shell fibers.
[0019] As a preferred technical solution of the present invention, the mass ratio of the activated oyster micro powder and the modifier in S13 is 90-120:1-3; the heating rate is 1-3℃ / min.
[0020] As a preferred technical solution of the present invention, the modifier mentioned in S13, by weight, is 10-20 parts of polyethylene glycol, 4-6 parts of succinic anhydride, and 1-3 parts of coconut oil amine polyoxyethylene ether; the modifier effectively improves the spatial structure of organic matter in oyster shells, effectively alleviates the autolysis of organic matter, and enhances the stability of organic matter.
[0021] As a more preferred technical solution of the present invention, the polyethylene glycol has a hydroxyl value of 34-42 mgKOH / g and a molecular weight of 2700-3300.
[0022] S2. Preparation of active synthetic fiber masterbatch
[0023] S21. Preparation of active particles
[0024] Talc and polylactic acid-glycolic acid copolymer were placed in dichloromethane and stirred thoroughly at 300-600 r / min for 20-30 min. The mixture was then heated to 50-70℃ and refluxed for 24-48 h. After cooling to room temperature, the mixture was washed 3-4 times with petroleum ether to obtain active particles.
[0025] S22. Granulation
[0026] The active particles described in step S21 are melt-blended with fiber chips for 20-60 minutes, and then extruded and granulated to obtain the active synthetic fiber masterbatch.
[0027] As a preferred embodiment of the present invention, the mass ratio of talc powder and polylactic acid-glycolic acid copolymer in S21 is 1-5:0.2-0.6.
[0028] As a preferred embodiment of the present invention, the mass ratio of the active particles to the fiber chips in S21 is 8-15:100-110.
[0029] As a preferred embodiment of the present invention, the talc powder in S21 has a particle size of 1250 mesh; the polylactic acid-hydroxyacetic acid copolymer has a molecular weight of 5000-15000.
[0030] As a preferred embodiment of the present invention, the fiber chips are any one of polyester chips, polyamide chips, polypropylene chips, and polyurethane chips.
[0031] S3. Preparation of shellfish fiber
[0032] After the recycled shellfish micro powder described in S13 and the active synthetic fiber masterbatch described in S22 are thoroughly stirred at high speed, the composite fiber masterbatch is obtained by extrusion granulation, and after melt spinning, the multifunctional shellfish fiber is obtained.
[0033] As a preferred technical solution of the present invention, the stirring temperature in S3 is 40-60℃ and the stirring speed is 1500-2500r / min.
[0034] By adopting the above technical solution, the technical effect achieved by this invention is as follows:
[0035] 1. This invention employs a triple treatment process of pretreatment, activation, and modification on coarse oyster shell powder, and uses polyethylene glycol, succinic anhydride, and cocoamine polyoxyethylene ether as modifiers to produce regenerated oyster shell micro-powder. This effectively improves the spatial structure of organic matter in the oyster shell, effectively alleviates the autolysis of organic matter, and enhances the stability of organic matter. Testing shows that the organic matter content in the regenerated oyster shell micro-powder can reach 3-4%.
[0036] 2. The active synthetic fiber masterbatch prepared by this invention has good interaction and affinity with the surface of the regenerated oyster shell micro powder in this system, which further enhances the adhesion between the organic matter in the oyster shell and the fiber masterbatch. The test shows that the loss rate of organic matter during the spinning process is less than 1%, and the organic matter content in the oyster fiber is as high as 0.5% or more. While reducing the loss rate of organic matter in this system, it also improves the washability and functional durability of the oyster fiber.
[0037] 3. The oyster fiber prepared by this invention exhibits excellent mechanical properties and retains the active substances in the oyster shell to the greatest extent, ensuring the diversity and durability of the oyster fiber's functions. According to testing in FZ / T 73023-2006, the oyster fiber shows an antibacterial rate of over 99% against Staphylococcus aureus, over 97% against Escherichia coli, and over 96% against Candida albicans. Furthermore, the oyster fiber after 100 washes also meets the AAA grade standard of FZ / T 73023-2006, with antibacterial rates against Staphylococcus aureus, Escherichia coli, and Candida albicans all exceeding 95%. In addition, the oyster fiber washed 100 times has a mit repellency rate of more than 99% (as determined according to GB / T 24253-2009); after washing 5 times, the electrostatic half-life is as low as 1.0s (as determined according to GB.T 12703.1-2008), showing good antibacterial, anti-mite, antistatic and water resistance.
[0038] 4. The oyster fiber prepared by this invention has good moisture absorption and quick-drying properties. The water absorption rate of the oyster fiber is as high as 320%, the water diffusion time is as low as 2.5s, the wicking height is as high as 170.2mm, and the evaporation rate is as high as 0.19g / h (measured according to GB / T21655.1-2008), which meets the national standard for moisture-absorbing and quick-drying textiles. Detailed Implementation
[0039] The present invention will be further illustrated below with reference to specific embodiments.
[0040] Example 1: A multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties, and its preparation method.
[0041] A method for preparing a multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties includes the following steps:
[0042] S1. Preparation of regenerated shellfish micro powder
[0043] S11. Preprocessing
[0044] After drying the recycled oyster shell coarse powder to 10 μm at 75℃ for 13 h, add 8 wt% NaOH aqueous solution and ultrasonically disperse for 2 h. Then heat and stir at 75℃ for 7 h, adjust the pH to 7, and after washing, filtering and drying, place the dried oyster shell coarse powder in a stirred ball mill and grind for 18 h to obtain pretreated oyster shell micro powder.
[0045] The particle size distribution of the pretreated shellfish micro powder is D90 < 1 μm.
[0046] S12. Activation
[0047] The pretreated oyster micro powder described in S11 was placed in an ethanol aqueous solution with a volume fraction of 75%, and ultrasonically dispersed at 75°C for 1.5 h at an ultrasonic frequency of 150 kHz. After cooling to room temperature, an ethanol aqueous solution of activated oyster micro powder was obtained.
[0048] S13. Modification
[0049] Add a modifier to an ethanol-water solution of activated oyster shell powder, slowly heat to 60°C, control the pH at 7.5 at 1200 r / min, stir for 30 min, then filter and wash, and keep the filter residue at 60°C for 13 h to obtain the regenerated oyster shell powder.
[0050] The mass ratio of the activated oyster micro powder to the modifier is 110:2; the heating rate is 2℃ / min.
[0051] The modifier, by weight, comprises 15 parts polyethylene glycol, 5 parts succinic anhydride, and 2 parts cocoamine polyoxyethylene ether. The modifier effectively improves the spatial structure of organic matter in oyster shells, effectively alleviates the autolysis of organic matter, and enhances the stability of organic matter.
[0052] The polyethylene glycol has a hydroxyl value of 38 mg KOH / g and a molecular weight of 3000.
[0053] S2. Preparation of active synthetic fiber masterbatch
[0054] S21. Preparation of active particles
[0055] Talc and polylactic acid-glycolic acid copolymer were placed in dichloromethane and stirred thoroughly at 450 r / min for 25 min. The mixture was then heated to 60 °C and refluxed for 36 h. After cooling to room temperature, the mixture was washed four times with petroleum ether to obtain active particles.
[0056] The mass ratio of talc to polylactic acid-glycolic acid copolymer is 3:0.4.
[0057] S22. Granulation
[0058] The active particles described in step S21 are melt-blended with polyester chips for 40 minutes, and then extruded and granulated to obtain the active synthetic fiber masterbatch.
[0059] The mass ratio of the active particles to the polyester chips is 12:105.
[0060] The talc powder has a particle size of 1250 mesh; the polylactic acid-glycolic acid copolymer has a molecular weight of 10000.
[0061] S3. Preparation of shellfish fiber
[0062] After the recycled shellfish micro powder described in S13 and the active synthetic fiber masterbatch described in S22 are thoroughly stirred at high speed, the composite fiber masterbatch is obtained by extrusion granulation, and after melt spinning, the multifunctional shellfish fiber is obtained.
[0063] The stirring temperature is 50℃ and the rotation speed is 2000 r / min.
[0064] By weight, the recycled shellfish micro powder comprises 10 parts and the active synthetic fiber masterbatch comprises 105 parts.
[0065] The oyster fiber prepared using Example 1 exhibits good mechanical properties, with a breaking strength of 3.8 cN / dtex. It also demonstrates excellent and long-lasting antibacterial properties, showing an inhibition rate of 99.53% against Staphylococcus aureus, 97.82% against Escherichia coli, and 96.43% against Candida albicans. After 100 washes, the oyster fiber maintains inhibition rates of 98.1%, 96.5%, and 95.5% against Staphylococcus aureus, Escherichia coli, and Candida albicans, respectively. The oyster fiber exhibits a 99.5% repellency rate against mites; after 5 washes, its electrostatic half-life is as low as 1.2s, demonstrating excellent antibacterial, anti-mite, antistatic, and water-resistant properties; it also possesses good moisture-wicking and quick-drying properties, with a water absorption rate of 315%, a drip diffusion time of 2.8s, a wicking height of 166.3mm, and an evaporation rate of 0.187g / h, meeting the national standards for moisture-wicking and quick-drying textiles; and the organic matter loss rate during spinning is 0.56%.
[0066] Example 2: A multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties, and its preparation method.
[0067] A method for preparing a multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties includes the following steps:
[0068] S1. Preparation of regenerated shellfish micro powder
[0069] S11. Preprocessing
[0070] After drying the recycled oyster shell coarse powder to 10 μm at 60℃ for 15 h, add 6 wt% NaOH aqueous solution and ultrasonically disperse for 1.5 h. Then heat and stir at 70℃ for 6 h, adjust the pH to 6.5, wash, filter and dry, and then grind the dried oyster shell coarse powder in a stirred ball mill for 15 h to obtain pretreated oyster shell micro powder.
[0071] The particle size distribution of the pretreated shellfish micro powder is D90 < 1 μm.
[0072] S12. Activation
[0073] The pretreated oyster micro powder described in S11 was placed in an ethanol aqueous solution with a volume fraction of 75%, and ultrasonically dispersed at 70°C for 1 hour at an ultrasonic frequency of 120 kHz. After cooling to room temperature, an ethanol aqueous solution of activated oyster micro powder was obtained.
[0074] S13. Modification
[0075] Add a modifier to an ethanol-water solution of activated oyster shell powder, slowly heat to 45°C, control the pH at 7 at a speed of 900 r / min, stir for 20 min, then filter and wash, and keep the filter residue at 45°C for 10 h to obtain the regenerated oyster shell powder.
[0076] The mass ratio of the activated oyster micro powder to the modifier is 90:1; the heating rate is 1℃ / min.
[0077] The modifier, by weight, comprises 10 parts polyethylene glycol, 4 parts succinic anhydride, and 1 part cocoamine polyoxyethylene ether. The modifier effectively improves the spatial structure of organic matter in oyster shells, effectively alleviates the autolysis of organic matter, and enhances the stability of organic matter.
[0078] The polyethylene glycol has a hydroxyl value of 34 mgKOH / g and a molecular weight of 2700.
[0079] S2. Preparation of active synthetic fiber masterbatch
[0080] S21. Preparation of active particles
[0081] Talc and polylactic acid-glycolic acid copolymer were placed in dichloromethane and stirred thoroughly at 300 r / min for 20 min. The mixture was then heated to 50 °C and refluxed for 24 h. After cooling to room temperature, the mixture was washed three times with petroleum ether to obtain active particles.
[0082] The mass ratio of talc to polylactic acid-glycolic acid copolymer is 1:0.2.
[0083] S22. Granulation
[0084] The active particles described in step S21 are melt-blended with polyester chips for 20 minutes, and then extruded and granulated to obtain the active synthetic fiber masterbatch.
[0085] The mass ratio of the active particles to the polyester chips is 8:100.
[0086] The talc powder has a particle size of 1250 mesh; the polylactic acid-glycolic acid copolymer has a molecular weight of 5000.
[0087] S3. Preparation of shellfish fiber
[0088] After the recycled shellfish micro powder described in S13 and the active synthetic fiber masterbatch described in S22 are thoroughly stirred at high speed, the composite fiber masterbatch is obtained by extrusion granulation, and after melt spinning, the multifunctional shellfish fiber is obtained.
[0089] The stirring temperature is 40℃ and the rotation speed is 1500r / min.
[0090] By weight, the recycled shellfish micro powder comprises 5 parts and the active synthetic fiber masterbatch comprises 90 parts.
[0091] The oyster fiber prepared using Example 2 exhibits good mechanical properties, with a breaking strength of 3.37 cN / dtex. It also demonstrates excellent and long-lasting antibacterial properties, showing an inhibition rate of 99.16% against Staphylococcus aureus, 97.2% against Escherichia coli, and 96.18% against Candida albicans. After 100 washes, the oyster fiber showed inhibition rates of 97.88%, 96.1%, and 95.2% against Staphylococcus aureus, Escherichia coli, and Candida albicans, respectively. The oyster fiber also showed a 99.2% repellency rate against mites after 100 washes. After 5 washes, the electrostatic half-life was 1.5 s, demonstrating good antibacterial, anti-mite, antistatic, and water-resistant properties. Furthermore, it exhibits excellent moisture absorption and quick-drying properties. Testing revealed a water absorption rate of 302%, a water droplet diffusion time of 3 s, a wicking height of 161 mm, and an evaporation rate of 0.182 g / h, meeting the national standards for moisture-wicking and quick-drying textiles. Tests showed that the organic matter loss rate during the spinning process was 0.83%.
[0092] Example 3: A multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties, and its preparation method.
[0093] A method for preparing a multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties includes the following steps:
[0094] S1. Preparation of regenerated shellfish micro powder
[0095] S11. Preprocessing
[0096] After drying the recycled oyster shell coarse powder to 10 μm at 90℃ for 10 h, add 10 wt% NaOH aqueous solution and ultrasonically disperse for 2.5 h. Then heat and stir at 80℃ for 8 h, adjust the pH to 7.5, wash, filter and dry, and then grind the dried oyster shell coarse powder in a stirred ball mill for 20 h to obtain pretreated oyster shell micro powder.
[0097] The particle size distribution of the pretreated shellfish micro powder is D90 < 1 μm.
[0098] S12. Activation
[0099] The pretreated oyster micro powder described in S11 was placed in an ethanol aqueous solution with a volume fraction of 75%, and ultrasonically dispersed at 80°C for 2 hours at an ultrasonic frequency of 100 kHz. After cooling to room temperature, an ethanol aqueous solution of activated oyster micro powder was obtained.
[0100] S13. Modification
[0101] Add a modifier to an ethanol-water solution of activated oyster shell powder, slowly heat to 75°C, control the pH at 1500 r / min, stir for 40 min, then filter and wash, and keep the filter residue at 75°C for 15 h to obtain the regenerated oyster shell powder.
[0102] The mass ratio of the activated oyster micro powder to the modifier is 120:3; the heating rate is 3℃ / min.
[0103] The modifier, by weight, comprises 20 parts polyethylene glycol, 6 parts succinic anhydride, and 3 parts cocoaluminum amine polyoxyethylene ether. The modifier effectively improves the spatial structure of organic matter in oyster shells, effectively alleviates the autolysis of organic matter, and enhances the stability of organic matter.
[0104] The polyethylene glycol has a hydroxyl value of 42 mg KOH / g and a molecular weight of 3300.
[0105] S2. Preparation of active synthetic fiber masterbatch
[0106] S21. Preparation of active particles
[0107] Talc and polylactic acid-glycolic acid copolymer were placed in dichloromethane and stirred thoroughly at 600 r / min for 30 min. The mixture was then heated to 70 °C and refluxed for 48 h. After cooling to room temperature, the mixture was washed four times with petroleum ether to obtain active particles.
[0108] The mass ratio of talc to polylactic acid-glycolic acid copolymer is 5:0.6.
[0109] S22. Granulation
[0110] The active particles described in step S21 are melt-blended with polyester chips for 60 minutes, and then extruded and granulated to obtain the active synthetic fiber masterbatch.
[0111] The mass ratio of the active particles to the polyester chips is 15:110.
[0112] The talc powder has a particle size of 1250 mesh; the polylactic acid-glycolic acid copolymer has a molecular weight of 15000.
[0113] S3. Preparation of shellfish fiber
[0114] After the recycled shellfish micro powder described in S13 and the active synthetic fiber masterbatch described in S22 are thoroughly stirred at high speed, the composite fiber masterbatch is obtained by extrusion granulation, and after melt spinning, the multifunctional shellfish fiber is obtained.
[0115] The stirring temperature is 60℃ and the rotation speed is 2500r / min.
[0116] By weight, the recycled shellfish micro powder comprises 15 parts and the active synthetic fiber masterbatch comprises 120 parts.
[0117] The oyster fiber prepared using Example 3 exhibits good mechanical properties, with a breaking strength of 3.62 cN / dtex. It also demonstrates excellent and long-lasting antibacterial properties, showing an inhibition rate of 99.7% against Staphylococcus aureus, 98.15% against Escherichia coli, and 96.9% against Candida albicans. After 100 washes, the oyster fiber showed inhibition rates of 98.55%, 97.23%, and 95.8% against Staphylococcus aureus, Escherichia coli, and Candida albicans, respectively. The oyster fiber also showed a 99.6% repellency rate against mites after 100 washes. After 5 washes, the electrostatic half-life was as low as 1.0 s, demonstrating good antibacterial, anti-mite, antistatic, and water-resistant properties. Furthermore, it exhibits excellent moisture absorption and quick-drying properties. Testing revealed a water absorption rate of 320%, a water droplet diffusion time of 2.5 s, a wicking height of 170.2 mm, and an evaporation rate of 0.19 g / h, meeting the national standards for moisture-wicking and quick-drying textiles. Tests showed that the organic matter loss rate during the spinning process was 0.71%.
[0118] Comparative Example 1
[0119] Example 1, a representative example, was selected. The modification step was removed, and oyster fiber was prepared directly using activated oyster micro powder and active synthetic fiber masterbatch. All other steps were the same as in Example 1. This example serves as Comparative Example 1. In Comparative Example 1, the organic matter loss rate during spinning was 36%, indicating a significant loss of organic matter. The fiber's breaking strength was 3.2 cN / dtex, and its antibacterial rate against Staphylococcus aureus was 92.3%, against Escherichia coli 91.84%, and against Candida albicans 90.62%. After 100 washes, the antibacterial rates against Staphylococcus aureus, Escherichia coli, and Candida albicans were 80.4%, 78.75%, and 77.68%, respectively. The oyster fiber after 100 washes showed an 82% repellency rate against mites. After 5 washes, the electrostatic half-life was 10.8 s, indicating that the organic matter in the modified regenerated oyster micropowder was more stable, had stronger affinity and adhesion to the synthetic fiber matrix, and exhibited better wash resistance and mechanical properties, thus resulting in more durable functionality.
[0120] Comparative Example 2
[0121] Example 1, a representative example, was selected. The step of preparing the active synthetic fiber masterbatch was omitted, and oyster fiber was directly prepared using recycled oyster shell powder and polyester chips. All other steps remained the same as in Example 1. As Comparative Example 2, the organic matter loss rate during spinning in Comparative Example 2 was 12%; the fiber's breaking strength was 2.73 cN / dtex; the inhibition rate against Staphylococcus aureus was 99.46%; against Escherichia coli was 97.9%; and against Candida albicans was 96.35%. The oyster fiber, after 100 washes, showed good resistance to Staphylococcus aureus, Escherichia coli, and... The antibacterial rates of Candida albicans were 92.17%, 91.89%, and 91.28%, respectively; the repellency rate of oyster fiber after 100 washes against mites was 93.1%; and the electrostatic half-life after 5 washes was 5.2 s. This indicates that the active synthetic fiber masterbatch and the surface of the regenerated oyster micropowder in this system have good interaction and affinity, avoiding the impact of the regenerated oyster micropowder on the mechanical properties of the synthetic fiber. This further enhances the adhesion between the organic matter in the oyster shell and the fiber masterbatch, thereby reducing the loss of organic matter, improving the washability of the fiber, and making its functionality more durable.
[0122] Unless otherwise specified, all proportions and percentages mentioned in this invention are mass proportions and mass percentages; all raw materials are commercially available.
[0123] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties, characterized in that: The raw materials for preparing the shellfish fiber include the following components by weight: 5-15 parts of regenerated shellfish micro powder and 90-120 parts of active synthetic fiber masterbatch. The method for preparing the shellfish fiber includes preparing regenerated shellfish micro powder, preparing active synthetic fiber masterbatch, and preparing shellfish fiber. The preparation of the regenerated shellfish micro powder includes pretreatment, activation, and modification; The pretreatment involves drying the recycled oyster shell coarse powder (crushed to 10 μm) at 60-90℃ for 10-15 hours, then adding 6-10 wt% NaOH aqueous solution and ultrasonically dispersing for 1.5-2.5 hours. Immediately afterwards, the powder is heated and stirred at 70-80℃ for 6-8 hours, and the pH is adjusted to 6.5-7.
5. After washing, filtering, and drying, the dried oyster shell coarse powder is ground in a stirred ball mill for 15-20 hours to obtain pretreated oyster shell micro powder. The particle size distribution of the pretreated shellfish micro powder is D90 < 1 μm; The activation process involves placing pretreated shellfish micropowder in a 75% (v / v) ethanol aqueous solution, ultrasonically dispersing it at 70-80°C for 1-2 hours, and then cooling it to room temperature to obtain an ethanol aqueous solution of activated shellfish micropowder. The modification involves adding a modifier to an ethanol-water solution of activated oyster shell powder, slowly heating to 45-75°C, controlling the pH at 7-8 at a speed of 900-1500 r / min, stirring for 20-40 min, then filtering and washing, and keeping the filter residue at 45-75°C for 10-15 h to obtain the regenerated oyster shell powder. The modifier, by weight, is 10-20 parts polyethylene glycol, 4-6 parts succinic anhydride, and 1-3 parts cocoaluminum amine polyoxyethylene ether; The active particles and fiber chips are melt-blended for 20-60 minutes, and then extruded and granulated to obtain the active synthetic fiber masterbatch. The active particles are prepared by placing talc powder and polylactic acid-glycolic acid copolymer in dichloromethane, stirring thoroughly at 300-600 r / min for 20-30 min, heating to 50-70℃, refluxing and stirring for 24-48 h, cooling to room temperature, and washing with petroleum ether 3-4 times to obtain active particles. The mass ratio of talc to polylactic acid-glycolic acid copolymer is 1-5:0.2-0.
6.
2. The multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties according to claim 1, characterized in that, The mass ratio of the activated oyster micro powder to the modifier is 90-120:1-3; the heating rate is 1-3℃ / min.
3. The multifunctional shellfish fiber with antibacterial, anti-mite, washable, moisture-wicking, and antistatic properties according to claim 1, characterized in that, The mass ratio of the active particles to the fiber chips is 8-15:100-110.