Flame-retardant antibacterial colored sea-island fiber and preparation method thereof
By using inorganic dye nano-pretreatment and masterbatch process, the dispersion problem of island fibers in terms of coloring, flame retardancy and antibacterial properties has been solved, realizing uniform coloring, long-lasting flame retardancy and antibacterial properties of island fibers, which are suitable for high-end artificial leather and high-performance fabrics.
Patent Information
- Application Number
- CN202511371656.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-24
- Publication Date
- 2025-12-02
AI Technical Summary
Existing island fibers suffer from problems such as uneven dyeing, poor color fastness, easy loss of functional components, and serious pollution in terms of coloring, flame retardancy, and antibacterial properties, making it difficult to achieve multifunctional uniform dispersion and durability through melt spinning.
By employing inorganic dye nano-pretreatment and masterbatch technology, inorganic dyes, decabromodiphenyl ethane, and polyhexamethylene guanidine are mixed with polyethylene terephthalate chips and melt-extruded and granulated through a twin-screw extruder to form a flame-retardant and antibacterial colored masterbatch. Subsequently, it is combined with island spinning to prepare flame-retardant and antibacterial colored island fiber.
It achieves uniform coloring of fibers, excellent color fastness, long-lasting flame retardant and antibacterial properties, simplifies the production process, reduces energy consumption and pollution, and is suitable for high-grade artificial leather, ultra-high density fabrics and high-performance wiping cloths.
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Figure CN121046989A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of functional chemical fiber preparation technology, and in particular to a multifunctional island fiber that combines long-lasting coloring, high-efficiency flame retardancy and broad-spectrum antibacterial properties, as well as its preparation method. Background Technology
[0002] Island-island fiber is a type of ultrafine fiber produced through composite spinning technology, consisting of "sea" and "island" components. In post-processing, the "sea" component is dissolved, leaving continuous bundles of "island" component ultrafine fibers, giving it an extremely soft feel and high specific surface area. It is widely used in high-end artificial leather, ultra-high-density fabrics, and high-performance wiping cloths.
[0003] Currently, the main problems with island-type fibers on the market are as follows: 1) Most use post-dyeing processes, which result in high water and energy consumption, serious wastewater pollution, uneven dyeing, and poor color fastness (especially rubbing and washing fastness); 2) Some use masterbatch melt dyeing, but inorganic pigments have poor dispersion in polyethylene terephthalate melt, which easily leads to color spots and color differences in the fibers, and seriously affects spinnability, causing breakage and increased fuzz; 3) There is a lack of products that integrate multiple functions. Although flame-retardant or antibacterial island-type fibers have been reported, such as patent CN 120006532 A which mentions that antibacterial suede can be prepared by impregnating gallic acid; and patent CN 120350562 A which obtains flame-retardant microfiber synthetic leather by impregnating a modified polyurethane emulsion coated with fluorinated chain modified melamine as a flame-retardant component. These methods for preparing flame-retardant or antibacterial island fiber synthetic leather mainly rely on post-processing methods such as impregnation, which suffer from significant pollution and poor durability. Achieving coloring, flame retardancy, and antibacterial properties simultaneously through melt spinning, a method with less water pollution, while ensuring uniform dispersion, excellent performance, and long-lasting durability of each functional component, remains a technical challenge.
[0004] Decabromodiphenyl ethane is a highly efficient brominated flame retardant suitable for polyethylene terephthalate (PET); polyhexamethylene guanidine is a safe, broad-spectrum, and wash-resistant polymeric antibacterial agent. However, how to stably and uniformly disperse these functional auxiliaries along with inorganic dyes in high-viscosity PET melts and withstand the harsh island-island spinning process to produce fibers with stable performance remains a pressing technical problem. Summary of the Invention
[0005] To address the problems existing in the prior art, this invention provides a method for preparing flame-retardant and antibacterial colored island fibers. This method solves the problem of uniform dispersion of inorganic dyes, decabromodiphenyl ethane, and polyhexamethylene guanidine in polyethylene terephthalate matrix through inorganic dye nano-pretreatment and masterbatch process.
[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:
[0007] A method for preparing flame-retardant, antibacterial, colored island fiber includes the following steps:
[0008] 1) Inorganic dye pretreatment: Inorganic dye, sodium polyacrylate dispersant and deionized water are mixed and placed in a ball mill for ball milling, then dried and pulverized to obtain nano-inorganic dye;
[0009] (2) Drying of polyethylene terephthalate slices: Dry polyethylene terephthalate slices to a moisture content of less than 0.05% to obtain dried polyethylene terephthalate slices;
[0010] (3) Preparation of flame-retardant and antibacterial colored masterbatch: The nano-inorganic dye obtained in step (1) and the dried polyethylene terephthalate chips obtained in step (2) are mixed with decabromodiphenyl ethane and polyhexamethylene guanidine, and then melt-extruded and granulated by a twin-screw extruder to obtain flame-retardant and antibacterial colored masterbatch.
[0011] (4) Mixing and granulation: The dried polyethylene terephthalate chips obtained in step (2) are mixed with the flame-retardant and antibacterial colored masterbatch obtained in step (3) and then melt-blended and granulated to obtain island component chips.
[0012] (5) Island fiber spinning: The chips obtained in step (4) are used as island components, and soluble polyethylene terephthalate is used as sea components. The chips are melt-spun through an island-type spinning assembly to obtain nascent fibers.
[0013] (6) Post-processing: The nascent fibers obtained in step (5) are stretched and heat-set to obtain the flame-retardant and antibacterial colored island fiber.
[0014] As a preferred technical solution of the present invention, in step (1), the mass ratio of inorganic dye, sodium polyacrylate dispersant and deionized water is 100:(5-20):(100-500), the ball milling time is 4-12 hours, the drying temperature is 100-120℃, and after pulverization, nanoscale inorganic dye with a particle size of 30-200nm is obtained; the inorganic dye is selected from one or more of carbon black, iron oxide red, lead chromium yellow, zinc iron yellow, titanium nickel yellow and cobalt chromium blue.
[0015] As a preferred technical solution of the present invention, the polyethylene terephthalate chips in step (2) are polyethylene terephthalate chips with an intrinsic viscosity of 0.60-0.68 dl / part. The polyethylene terephthalate chips are placed in a vacuum drum drying oven and vacuum dried at 120-140°C for 14-16 hours to make the moisture content of the polyethylene terephthalate chips less than 0.005%.
[0016] As a preferred technical solution of the present invention, in step (3), the mass ratio of nano-inorganic dye, polyethylene terephthalate chips, decabromodiphenyl ethane and polyhexamethylene guanidine is (15-30):(50-70):(10-20):(3-8); the temperature of the twin-screw extruder for melt extrusion granulation is 270-290℃.
[0017] As a preferred technical solution of the present invention, in step (4), the mass ratio of dried polyethylene terephthalate chips to flame-retardant antibacterial colored masterbatch is (70-90):(10-30), and the chips are melt-blended and granulated by a screw extruder at a temperature of 270-290℃.
[0018] As a preferred technical solution of the present invention, in step (5), the mass ratio of island component to sea component is 60:40-80:20, the spinning temperature is 270-290℃, and the spinning speed is 600-1400m / min.
[0019] As a preferred technical solution of the present invention, in step (6), the stretching is carried out in a hot water bath at 85-95°C, the stretching ratio is 1.2-2.5 times, the heat setting temperature is 175-210°C, and the time is 3-5 minutes.
[0020] The present invention also provides a flame-retardant and antibacterial colored island fiber prepared by the above preparation method. This fiber not only has uniform color, high color fastness, and good light and heat resistance, but also has excellent long-lasting flame-retardant and antibacterial properties.
[0021] The island fiber described in this invention has a limiting oxygen index of not less than 28%, an antibacterial rate of not less than 98% against Staphylococcus aureus and Escherichia coli, and color fastness to rubbing and washing of not less than grade 4.
[0022] Compared with the prior art, the present invention has the following significant advantages:
[0023] 1. Excellent and durable coloring performance: This invention prepares nano-sized inorganic dyes by pretreating inorganic dyes. The nano-sized particles allow the dyes to be uniformly dispersed in the fiber matrix, effectively avoiding the uneven dyeing problem caused by traditional post-dyeing methods. At the same time, the nano-inorganic dyes have good compatibility with the polyethylene terephthalate matrix and can be firmly bonded during melt blending, which significantly improves the color fastness of the fibers, making them less prone to fading and providing a long-lasting and stable coloring effect.
[0024] 2. Excellent and long-lasting flame retardant and antibacterial properties: In the preparation of the flame-retardant and antibacterial colored masterbatch, this invention simultaneously adds decabromodiphenyl ethane (flame retardant) and polyhexamethylene guanidine (antibacterial agent). Through melt blending and granulation with nano-inorganic dyes and polyethylene terephthalate chips, a three-functional "flame-retardant and antibacterial colored masterbatch" is designed. This ensures that the flame retardant and antibacterial agent are evenly distributed in the masterbatch, and thus uniformly dispersed in the island components of the island fiber during subsequent island component preparation and spinning. This integrated addition method allows the flame retardant and antibacterial agent to be tightly bonded to the fiber matrix, avoiding the problem of functional components easily detaching due to later coating or impregnation treatments, thereby giving the fiber excellent and long-lasting flame retardant and antibacterial properties.
[0025] 3. Synergistic Effect of Flame Retardants and Antibacterial Agents: While polyhexamethylene guanidine (PHGD) primarily functions as an antibacterial agent, its guanidine groups (-NH-C(=NH)-NH-) decompose at high temperatures, releasing inert gases such as ammonia. This release dilutes the oxygen concentration in the combustion zone, slowing the combustion rate. Furthermore, the nitrogen-containing compounds produced by the decomposition of guanidine groups react with the bromides from the decomposition of decabromodiphenyl ethane (DBD) to generate flame-retardant intermediates such as ammonium bromide, further enhancing the gas-phase flame-retardant effect. DBD, as a flame retardant, decomposes during use to produce trace amounts of bromide ions. These ions can react with active groups such as thiol groups (-SH) within bacterial cells, inhibiting bacterial enzyme activity and assisting PHGD in disrupting bacterial metabolic processes. Therefore, DBD and PHGD exhibit a synergistic effect in both antibacterial and flame-retardant properties.
[0026] 4. High process versatility and environmental friendliness: This method is highly compatible with existing island fiber production lines, requiring no modification to core equipment and facilitating large-scale industrial production. The prepared island fibers do not require subsequent dyeing, coating, or soaking for additional functionalization, simplifying the production process and reducing energy consumption and production costs. Furthermore, the selected raw materials, such as nano-inorganic dyes, decabromodiphenyl ethane, and polyhexamethylene guanidine, all possess good environmental performance, generating no large amounts of harmful pollutants during production, thus meeting environmental protection requirements. Attached Figure Description
[0027] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0028] Figure 1 The image shows colony diagrams of Staphylococcus aureus for antibacterial testing. The right side shows the island fiber substrate prepared in Example 4 of this invention, and the left side shows the ordinary island fiber substrate. Detailed Implementation
[0029] The present invention will be described in detail below through embodiments, but the scope of protection of the present invention is not limited thereto. Unless otherwise specified, all parts referred to below are parts by weight.
[0030] The preparation method of the flame-retardant and antibacterial island fiber of the present invention is as follows:
[0031] (1) Inorganic dye pretreatment: Inorganic dye, sodium polyacrylate dispersant and deionized water are mixed in a mass ratio of 100:(5-20):(100-500) and then placed in a ball mill for ball milling for 4-12 hours. After that, the mixture is dried at a temperature of 100-120℃ and then pulverized to obtain nano-inorganic dye with a particle size of 30-200nm. The inorganic dye is selected from one or more of carbon black, iron oxide red, lead chromium yellow, zinc iron yellow, titanium nickel yellow and cobalt chromium blue.
[0032] (2) Drying of polyethylene terephthalate chips: Select polyethylene terephthalate chips with an intrinsic viscosity of 0.60-0.68 dl / part, place them in a vacuum drum drying oven, and vacuum dry them at 120-140℃ for 14-16 hours to make the moisture content of the polyethylene terephthalate chips less than 0.005%, thus obtaining dried polyethylene terephthalate chips.
[0033] (3) Preparation of flame-retardant and antibacterial colored masterbatch: The nano-inorganic dye obtained in step (1), the dried polyethylene terephthalate chips obtained in step (2), decabromodiphenyl ethane and polyhexamethylene guanidine are mixed in a mass ratio of (15-30):(50-70):(10-20):(3-8). The mixture is fed into a twin-screw extruder for melt extrusion granulation. The temperature of the twin-screw extruder is 270-290℃ to obtain flame-retardant and antibacterial colored masterbatch.
[0034] (4) Mixing and granulation: The dried polyethylene terephthalate chips obtained in step (2) are mixed with the flame-retardant and antibacterial colored masterbatch obtained in step (3) at a mass ratio of (70-90): (10-30). The mixture is added to a screw extruder for melt blending and granulation. The temperature of the screw extruder is controlled at 270-290℃ to obtain island component chips.
[0035] (5) Island fiber spinning: The island component slices obtained in step (4) are used as island components, and soluble polyethylene terephthalate is used as sea components. The mass ratio of island components to sea components is controlled at 60:40-80:20. Melt spinning is carried out through an island-type spinning assembly. The spinning temperature is controlled at 270-290℃ and the spinning speed is controlled at 600-1400m / min to obtain nascent fibers.
[0036] (6) Post-processing: The nascent fibers obtained in step (5) are stretched in a hot water bath at 85-95℃, with the stretching ratio controlled at 1.2-2.5 times. After stretching, they are heat-set at 175-210℃ for 3-5 minutes to obtain the flame-retardant and antibacterial colored island fiber.
[0037] Example 1
[0038] The preparation method of the black flame-retardant and antibacterial island fiber in this embodiment is as follows:
[0039] A method for preparing flame-retardant, antibacterial, colored island fiber, comprising the following specific steps:
[0040] (1) Inorganic dye pretreatment: Carbon black (100 parts), sodium polyacrylate dispersant (5 parts) and deionized water (100 parts) were mixed and placed in a ball mill and ball milled for 4 hours. Then, the mixture was dried at 100°C and pulverized to obtain nano carbon black with a particle size of 150-200 nm.
[0041] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.60 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 120°C for 16 hours. The moisture content of the slices was measured to be 0.004%, and dried polyethylene terephthalate slices were obtained.
[0042] (3) Preparation of flame-retardant and antibacterial colored masterbatch: Mix nano carbon black (15 parts), dried polyethylene terephthalate chips (70 parts), decabromodiphenyl ethane (10 parts) and polyhexamethylene guanidine (3 parts), and put them into a twin-screw extruder. The temperature of the twin-screw extruder is 290℃. Melt extrusion granulation is performed to obtain flame-retardant and antibacterial colored masterbatch.
[0043] (4) Mixing and granulation: Mix dried polyethylene terephthalate chips (90 parts) with flame retardant and antibacterial colored masterbatch (10 parts), add to a screw extruder, and melt blend and granulate at 280°C to obtain island component chips.
[0044] (5) Island-sea fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 60:40, and the fibers are melt-spun through an island-sea type spinning assembly. The spinning temperature is 270℃ and the spinning speed is 600m / min to obtain nascent fibers.
[0045] (6) Post-treatment: The nascent fiber is stretched in a hot water bath at 85°C with a stretching ratio of 1.2 times, and then heat-set at 175°C for 5 minutes to obtain black flame-retardant and antibacterial colored island fiber.
[0046] Example 2
[0047] The preparation method of the red flame-retardant and antibacterial island fiber in this embodiment is as follows:
[0048] (1) Inorganic dye pretreatment: Iron oxide red (100 parts), sodium polyacrylate dispersant (20 parts) and deionized water (400 parts) were mixed and placed in a ball mill and ball milled for 6 hours. Then, the mixture was dried at 120°C and pulverized to obtain nano iron oxide red with a particle size of 80-120 nm.
[0049] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.68 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 140°C for 14 hours. The moisture content of the slices was measured to be 0.003%, and dried polyethylene terephthalate slices were obtained.
[0050] (3) Preparation of flame-retardant and antibacterial colored masterbatch: Mix nano iron oxide red (30 parts), dried polyethylene terephthalate chips (50 parts), decabromodiphenyl ethane (15 parts) and polyhexamethylene guanidine (6 parts), and put them into a twin-screw extruder. The temperature of the twin-screw extruder is 280℃. Melt extrusion granulation is performed to obtain flame-retardant and antibacterial colored masterbatch.
[0051] (4) Mixing and granulation: Mix dried polyethylene terephthalate chips (70 parts) with flame retardant and antibacterial colored masterbatch (30 parts), add to a screw extruder, and melt blend and granulate at 285°C to obtain island component chips.
[0052] (5) Island-sea fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 80:20, and the fibers are melt-spun through an island-sea type spinning assembly. The spinning temperature is 275℃ and the spinning speed is 1200m / min to obtain nascent fibers.
[0053] (6) Post-treatment: The nascent fiber is stretched in a hot water bath at 95°C with a stretching ratio of 2.0 times, and then heat-set at 210°C for 3 minutes to obtain red flame-retardant and antibacterial colored island fiber.
[0054] Example 3
[0055] The preparation method of the yellow flame-retardant and antibacterial island fiber in this embodiment is as follows:
[0056] (1) Inorganic dye pretreatment: Titanium nickel yellow (100 parts), sodium polyacrylate dispersant (15 parts) and deionized water (500 parts) were mixed and placed in a ball mill and ball milled for 12 hours. Then, it was dried at 110°C and pulverized to obtain nano titanium nickel yellow with a particle size of 30-50 nm.
[0057] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.62 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 130°C for 15 hours. The moisture content of the slices was measured to be 0.004%, and dried polyethylene terephthalate slices were obtained.
[0058] (3) Preparation of flame-retardant and antibacterial colored masterbatch: 20 parts of nano titanium nickel yellow, 60 parts of dried polyethylene terephthalate chips, 20 parts of decabromodiphenyl ethane and 4 parts of polyhexamethylene guanidine were mixed and fed into a twin-screw extruder at a temperature of 270°C. The mixture was melt-extruded and granulated to obtain the flame-retardant and antibacterial colored masterbatch.
[0059] (4) Mixing and granulation: Mix dried polyethylene terephthalate chips (80 parts) with flame retardant and antibacterial colored masterbatch (20 parts), add to a screw extruder, and melt blend and granulate at 275°C to obtain island component chips.
[0060] (5) Island-sea fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 70:30, and the fibers are melt-spun through an island-sea type spinning assembly. The spinning temperature is 290℃ and the spinning speed is 1400m / min to obtain nascent fibers.
[0061] (6) Post-treatment: The nascent fibers are stretched in a 90°C hot water bath with a stretching ratio of 2.5 times, and then heat-set at 200°C for 4 minutes to obtain flame-retardant and antibacterial colored island fibers.
[0062] Example 4
[0063] The preparation method of the blue flame-retardant and antibacterial island fiber in this embodiment is as follows:
[0064] (1) Inorganic dye pretreatment: Cobalt chromium blue (100 parts), sodium polyacrylate dispersant (10 parts) and deionized water (300 parts) were mixed and placed in a ball mill and ball milled for 8 hours. Then, the mixture was dried at 105°C and pulverized to obtain nano-titanium nickel yellow with a particle size of 120-160 nm.
[0065] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.65 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 125°C for 14.5 hours. The moisture content of the slices was measured to be 0.003%, and dried polyethylene terephthalate slices were obtained.
[0066] (3) Preparation of flame-retardant and antibacterial colored masterbatch: 18 parts of nano titanium nickel yellow, 65 parts of dried polyethylene terephthalate chips, 12 parts of decabromodiphenyl ethane and 8 parts of polyhexamethylene guanidine were mixed and fed into a twin-screw extruder at a temperature of 275°C. The mixture was melt-extruded and granulated to obtain the flame-retardant and antibacterial colored masterbatch.
[0067] (4) Mixing and granulation: Mix dried polyethylene terephthalate chips (85 parts) with flame retardant and antibacterial colored masterbatch (15 parts), add to a screw extruder, and melt blend and granulate at 270°C to obtain island component chips.
[0068] (5) Island fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 75:25, and the fibers are melt spun through an island type spinning assembly. The spinning temperature is 280℃ and the spinning speed is 800m / min to obtain nascent fibers.
[0069] (6) Post-treatment: The nascent fibers are stretched in a hot water bath at 93°C with a stretching ratio of 1.5 times, and then heat-set at 180°C for 5 minutes to obtain blue flame-retardant and antibacterial colored island fibers.
[0070] Example 5
[0071] The preparation method of the yellow flame-retardant and antibacterial island fiber in this embodiment is as follows:
[0072] (1) Inorganic dye pretreatment: Aluminum iron yellow (50 parts), zinc iron yellow (50 parts), sodium polyacrylate dispersant (13 parts) and deionized water (200 parts) were mixed and placed in a ball mill and ball milled for 5 hours. Then, they were dried at 115°C and pulverized to obtain nano titanium nickel yellow with a particle size of 90-130 nm.
[0073] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.64 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 135°C for 14 hours. The moisture content of the slices was measured to be 0.004%, and dried polyethylene terephthalate slices were obtained.
[0074] (3) Preparation of flame-retardant and antibacterial colored masterbatch: 25 parts of nano titanium nickel yellow, 65 parts of dried polyethylene terephthalate chips, 14 parts of decabromodiphenyl ethane and 5 parts of polyhexamethylene guanidine were mixed and fed into a twin-screw extruder at a temperature of 280°C. The mixture was melt-extruded and granulated to obtain the flame-retardant and antibacterial colored masterbatch.
[0075] (4) Mixing and granulation: Mix dried polyethylene terephthalate chips (75 parts) with flame-retardant and antibacterial colored masterbatch (25 parts), add to a screw extruder, and melt blend and granulate at 290°C to obtain island component chips.
[0076] (5) Island fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 65:35, and the fibers are melt spun through an island type spinning assembly at a spinning temperature of 285℃ and a spinning speed of 1000m / min to obtain nascent fibers.
[0077] (6) Post-treatment: The nascent fibers are stretched in a 90°C hot water bath with a stretching ratio of 2.1 times, and then heat-set at 205°C for 3 minutes to obtain yellow flame-retardant and antibacterial colored island fibers.
[0078] Comparative Example 1
[0079] Based on Example 1, without the inorganic dye nano-pretreatment, the specific steps are as follows:
[0080] (1) Inorganic dye pretreatment: Dry carbon black at 100℃.
[0081] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.60 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 120°C for 16 hours. The moisture content of the slices was measured to be 0.004%, and dried polyethylene terephthalate slices were obtained.
[0082] (3) Preparation of flame-retardant and antibacterial colored masterbatch: Mix nano carbon black (15 parts), dried polyethylene terephthalate chips (70 parts), decabromodiphenyl ethane (10 parts) and polyhexamethylene guanidine (3 parts), and put them into a twin-screw extruder. The temperature of the twin-screw extruder is 290℃. Melt extrusion granulation is performed to obtain flame-retardant and antibacterial colored masterbatch.
[0083] (4) Mixing and granulation: Mix dried polyethylene terephthalate chips (90 parts) with flame retardant and antibacterial colored masterbatch (10 parts), add to a screw extruder, and melt blend and granulate at 280°C to obtain island component chips.
[0084] (5) Island-sea fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 60:40, and the fibers are melt-spun through an island-sea type spinning assembly. The spinning temperature is 270℃ and the spinning speed is 600m / min to obtain nascent fibers.
[0085] (6) Post-treatment: The nascent fiber was stretched in a hot water bath at 85°C with a stretching ratio of 1.2 times, and then heat-set at 175°C for 5 minutes to obtain black flame-retardant and antibacterial colored island fiber, which was designated as control fiber 1.
[0086] The resulting comparative fiber 1 was dull and uneven in color, with a large number of visible black spots. The breakage rate during spinning was as high as 15%, and the flame retardant and antibacterial properties were uneven.
[0087] Comparative Example 2
[0088] The specific steps for preparing colored masterbatch without flame retardant and antibacterial processes are as follows:
[0089] (1) Inorganic dye pretreatment: Carbon black (100 parts), sodium polyacrylate dispersant (5 parts) and deionized water (100 parts) were mixed and placed in a ball mill and ball milled for 4 hours. Then, the mixture was dried at 100°C and pulverized to obtain nano carbon black with a particle size of 150-200 nm.
[0090] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.60 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 120°C for 16 hours. The moisture content of the slices was measured to be 0.004%, and dried polyethylene terephthalate slices were obtained.
[0091] (3) Mixing and granulation: Dry polyethylene terephthalate chips (90 parts) are mixed with carbon black (5 parts), decabromodiphenyl ethane (2 parts) and polyhexamethylene guanidine (3 parts), and added to a screw extruder. The mixture is melt-blended and granulated at 280°C to obtain island component chips.
[0092] (4) Island-sea fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 60:40, and the fibers are melt-spun through an island-sea type spinning assembly. The spinning temperature is 270℃ and the spinning speed is 600m / min to obtain nascent fibers.
[0093] (5) Post-treatment: The nascent fibers were stretched in a hot water bath at 85°C with a stretching ratio of 1.2 times, and then heat-set at 175°C for 5 minutes to obtain the black flame-retardant and antibacterial colored island fiber of Comparison 2.
[0094] Comparative Example 3
[0095] Compared to Example 1, this comparative example does not use flame retardant. The specific preparation method is as follows:
[0096] A method for preparing flame-retardant, antibacterial, colored island fiber, comprising the following specific steps:
[0097] (1) Inorganic dye pretreatment: Carbon black (100 parts), sodium polyacrylate dispersant (5 parts) and deionized water (100 parts) were mixed and placed in a ball mill and ball milled for 4 hours. Then, the mixture was dried at 100°C and pulverized to obtain nano carbon black with a particle size of 150-200 nm.
[0098] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.60 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 120°C for 16 hours. The moisture content of the slices was measured to be 0.004%, and dried polyethylene terephthalate slices were obtained.
[0099] (3) Preparation of flame-retardant and antibacterial colored masterbatch: Nano carbon black (15 parts), dried polyethylene terephthalate chips (70 parts), decabromodiphenyl ethane (0 parts) and polyhexamethylene guanidine (3 parts) are mixed and put into a twin-screw extruder. The temperature of the twin-screw extruder is 290℃. The mixture is melt-extruded and granulated to obtain flame-retardant and antibacterial colored masterbatch.
[0100] (4) Mixing and granulation: Mix dried polyethylene terephthalate chips (90 parts) with flame retardant and antibacterial colored masterbatch (10 parts), add to a screw extruder, and melt blend and granulate at 280°C to obtain island component chips.
[0101] (5) Island-sea fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 60:40, and the fibers are melt-spun through an island-sea type spinning assembly. The spinning temperature is 270℃ and the spinning speed is 600m / min to obtain nascent fibers.
[0102] (6) Post-treatment: The nascent fiber was stretched in a hot water bath at 85°C with a stretching ratio of 1.2 times, and then heat-set at 175°C for 5 minutes to obtain the black flame-retardant and antibacterial colored island fiber of Comparison 3.
[0103] Comparative Example 4
[0104] Compared to Example 1, this comparative example does not use an antibacterial agent. The specific preparation method is as follows:
[0105] A method for preparing flame-retardant, antibacterial, colored island fiber, comprising the following specific steps:
[0106] (1) Inorganic dye pretreatment: Carbon black (100 parts), sodium polyacrylate dispersant (5 parts) and deionized water (100 parts) were mixed and placed in a ball mill and ball milled for 4 hours. Then, the mixture was dried at 100°C and pulverized to obtain nano carbon black with a particle size of 150-200 nm.
[0107] (2) Drying of polyethylene terephthalate slices: Polyethylene terephthalate slices with an intrinsic viscosity of 0.60 dl / part were selected and placed in a vacuum drum drying oven. They were vacuum dried at 120°C for 16 hours. The moisture content of the slices was measured to be 0.004%, and dried polyethylene terephthalate slices were obtained.
[0108] (3) Preparation of flame-retardant and antibacterial colored masterbatch: Nano carbon black (15 parts), dried polyethylene terephthalate chips (70 parts), decabromodiphenyl ethane (10 parts) and polyhexamethylene guanidine (0 parts) are mixed and fed into a twin-screw extruder. The temperature of the twin-screw extruder is 290℃. The mixture is melt-extruded and granulated to obtain flame-retardant and antibacterial colored masterbatch.
[0109] (4) Mixing and granulation: Mix dried polyethylene terephthalate chips (90 parts) with flame retardant and antibacterial colored masterbatch (10 parts), add to a screw extruder, and melt blend and granulate at 280°C to obtain island component chips.
[0110] (5) Island-sea fiber spinning: Island component chips are used as island components, soluble polyethylene terephthalate is used as sea components, the mass ratio of island components to sea components is 60:40, and the fibers are melt-spun through an island-sea type spinning assembly. The spinning temperature is 270℃ and the spinning speed is 600m / min to obtain nascent fibers.
[0111] (6) Post-treatment: The nascent fibers were stretched in a hot water bath at 85°C with a stretching ratio of 1.2 times, and then heat-set at 175°C for 5 minutes to obtain the black flame-retardant and antibacterial colored island fiber of Comparison 4.
[0112] Performance testing
[0113] The fibers obtained in Examples 1-5 and Comparative Examples 1-4 of this invention were subjected to performance tests, and the results are shown in the table below.
[0114]
[0115]
[0116] Test results show that the antibacterial and flame-retardant properties of control fibers 1 and 2, prepared by direct mixing and spinning without inorganic fuel nano-pretreatment (Comparative Example 1) and without flame-retardant and antibacterial colored masterbatch processing (Comparative Example 2), are reduced. The color fastness to rubbing, color fastness to washing, and monofilament strength are all significantly reduced, and the fiber color is dull and uneven with numerous visible black spots, mainly due to uneven mixing of the components. In Comparative Example 3, no flame retardant was added, resulting in a significant reduction in the flame-retardant properties of control fiber 3, although its antibacterial properties also decreased. Similarly, in Comparative Example 4, no antibacterial agent was added, resulting in a significant decrease in the antibacterial properties of control fiber 4, and its flame-retardant properties also decreased significantly. This reveals the synergistic effect of decabromodiphenyl ethane and polyhexamethylene guanidine in the flame-retardant and antibacterial properties of control fiber 4. The fibers prepared by this invention achieve the expected flame-retardant, antibacterial, and color fastness performance indicators, and also exhibit good mechanical properties.
[0117] The foregoing has shown and described the basic principles and main features of the present invention, as well as its advantages. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of this invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing flame-retardant, antibacterial, colored island fiber, characterized in that, Includes the following steps: (1) Inorganic dye pretreatment: Inorganic dye, sodium polyacrylate dispersant and deionized water are mixed and placed in a ball mill for ball milling, then dried and pulverized to obtain nano-inorganic dye; (2) Drying of polyethylene terephthalate slices: The polyethylene terephthalate slices were dried to obtain dried polyethylene terephthalate slices; (3) Preparation of flame-retardant and antibacterial colored masterbatch: The nano-inorganic dye obtained in step (1) and the dried polyethylene terephthalate chips obtained in step (2) are mixed with decabromodiphenyl ethane and polyhexamethylene guanidine, and then melt-extruded and granulated by a twin-screw extruder to obtain flame-retardant and antibacterial colored masterbatch. (4) Mixing and granulation: The dried polyethylene terephthalate chips obtained in step (2) are mixed with the flame-retardant and antibacterial colored masterbatch obtained in step (3) and then melt-blended and granulated to obtain island component chips; (5) Island fiber spinning: The chips obtained in step (4) are used as island components, and soluble polyethylene terephthalate is used as sea components. The chips are melt-spun through an island-type spinning assembly to obtain nascent fibers. (6) Post-processing: The nascent fibers obtained in step (5) are stretched and heat-set to obtain the flame-retardant and antibacterial colored island fiber.
2. The method for preparing flame-retardant, antibacterial, colored island fiber according to claim 1, characterized in that, The inorganic dye is selected from one or more of carbon black, iron oxide red, lead chromium yellow, zinc iron yellow, titanium nickel yellow, and cobalt chromium blue.
3. The method for preparing flame-retardant, antibacterial, colored island fiber according to claim 1, characterized in that, In step (1), the mass ratio of inorganic dye, sodium polyacrylate dispersant and deionized water is 100:(5-20):(100-500), the ball milling time is 4-12 hours, the drying temperature is 100-120℃, and after pulverization, nanoscale inorganic dye with a particle size of 30-200 nm is obtained.
4. The method for preparing flame-retardant, antibacterial, colored island fiber according to claim 1, characterized in that, The polyethylene terephthalate (PET) chips used in step (2) are PET chips with an intrinsic viscosity of 0.60-0.68 dl / part.
5. The method for preparing flame-retardant, antibacterial, colored island fiber according to claim 1, characterized in that, In step (2), polyethylene terephthalate slices are placed in a vacuum drum drying oven and vacuum dried at 120-140°C for 14-16 hours to reduce the moisture content of the polyethylene terephthalate slices to less than 0.005%.
6. The method for preparing flame-retardant, antibacterial, colored island fiber according to claim 1, characterized in that, In step (3), the mass ratio of nano-inorganic dye, polyethylene terephthalate chips, decabromodiphenyl ethane and polyhexamethylene guanidine is (15-30):(50-70):(10-20):(3-8); the temperature range of the twin-screw extruder for melt extrusion granulation is 270-290℃.
7. The method for preparing flame-retardant, antibacterial, colored island fiber according to claim 1, characterized in that, In step (4), the mass ratio of dried polyethylene terephthalate chips to flame-retardant and antibacterial colored masterbatch is (70-90):(10-30). The chips are melt-blended and granulated using a screw extruder at a temperature of 270-290℃.
8. The method for preparing flame-retardant, antibacterial, colored island fiber according to claim 1, characterized in that, In step (5), the mass ratio of island component to sea component is 60:40-80:20, the spinning temperature is 270-290℃, and the spinning speed is 600-1400 m / min.
9. The method for preparing flame-retardant, antibacterial, colored island fiber according to claim 1, characterized in that, In step (6), the stretching is carried out in a hot water bath at 85-95℃, the stretching ratio is 1.2-2.5 times, the heat setting temperature is 175-210℃, and the time is 3-5 minutes.
10. A flame-retardant, antibacterial, colored island fiber, characterized in that, Prepared by the method according to any one of claims 1-9.
Citation Information
Patent Citations
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