Efficient far infrared graphene-nylon 6 composite fiber

Abstract

The invention relates to a high-efficiency far-infrared graphene-nylon 6 composite fiber which is prepared from a high-efficiency graphene far-infrared nano powder material, an auxiliary agent and nylon 6 through a high-speed melt spinning process. The mass ratio of the efficient graphene far infrared nano powder material to the nylon 6 is (0.3-0.5): 100. The high-efficiency graphene is a nano graphene sheet, and the high-efficiency graphene far-infrared nano powder material is prepared by performing wet grinding on hafnium dioxide, albite, quartz, borax and the nano graphite sheet by a sand mill for 1 hour and drying. The auxiliary agent is acetylated calcium lignosulphonate. Products of the efficient far infrared graphene-nylon 6 composite fiber comprise FDY, UDY, POY, HOY and BCF. The far infrared nano powder material modified graphene is compounded with the nylon 6 and the auxiliaries, and the composite fiber is prepared through high-speed melt spinning, so that the performance of the fiber is improved, the product quality is optimized, and the composite fiber has excellent comprehensive performance.

Description

Technical Field

[0001] The invention belongs to the technical field of manufacturing chemical fiber products and relates to a high-efficiency far-infrared graphene-nylon 6 composite fiber. Background Art

[0002] Nylon fiber is one of the earliest industrialized synthetic fibers in the world and one of the most versatile and high-performance synthetic fibers. It possesses numerous excellent properties. In addition to the common synthetic fiber properties of corrosion resistance, mildew resistance, high wet strength, insect resistance, and low moisture absorption, it also offers advantages such as high strength, excellent abrasion resistance, good elasticity, and high fiber elongation recovery. As living standards improve, people are increasingly concerned about the comfort and health benefits of textiles, and the demand for multifunctional fibers is growing. Consequently, the research, development, and production of various functional and differentiated nylon fibers are receiving increasing attention.

[0003] Graphene is based on SP 2 A two-dimensional structure composed of hybridized carbon atoms, in which the carbon atoms are in a hexagonal honeycomb shape. Since graphene is a single layer of carbon atoms, it has a large specific surface area. Theoretical calculations show that the specific surface area of ​​a single layer of graphene is 2630m 2 / g, which is more than twice that of activated carbon. Studies have found that graphene has excellent electrical properties, which mainly depend on the shape and number of graphene layers. Graphene also has excellent thermal conductivity, with a thermal conductivity coefficient of 3000W / (m·K), making it the material with the best thermal conductivity except for metals. Due to its unique nanostructure and excellent properties, graphene can be added to a polymer matrix as an excellent multifunctional filler, giving the matrix excellent properties. At the same time, compared with expensive carbon nanotubes, graphene raw materials are easy to obtain, cheap, and the preparation method is simple and convenient, so it is expected to replace carbon nanotubes as a high-quality filler for polymer-based composites. However, the far-infrared absorption ability of graphene is relatively general. By compounding with far-infrared nanopowders, graphene materials with high efficiency far-infrared absorption are obtained. Summary of the Invention

[0004] The present invention provides a high-efficiency far-infrared graphene-nylon 6 composite fiber, which improves the comprehensive performance of the fiber, optimizes product quality, and enables the graphene-nylon 6 composite fiber to have a wider range of uses.

[0005] The technical solution of this invention is a high-efficiency far-infrared graphene-nylon 6 composite fiber, produced by a high-speed melt spinning process using a high-efficiency graphene far-infrared nanopowder material, additives, and nylon 6. The mass ratio of the high-efficiency graphene far-infrared nanopowder material to nylon 6 is 0.3-0.5:100. Products of the high-efficiency far-infrared graphene-nylon 6 composite fiber include FDY, UDY, POY, HOY, and BCF.

[0006] High-efficiency graphene is nanographene flakes. The high-efficiency graphene far-infrared nanopowder material is made by wet-grinding hafnium dioxide, albite, quartz, borax, and nanographite flakes in a sand mill for 1 hour and then drying. Its composition by mass is: 10-20 parts hafnium dioxide, 5-10 parts albite, 1-10 parts quartz, 2-5 parts borax; and 80-100 parts nanographene flakes. The planar size of the nanographene flakes is 0.03-0.3 μm. 2 The thickness is 0.8-1.5nm. The auxiliary agent is acetylated calcium lignin sulfonate, and the amount of the auxiliary agent used is 0.6-5wt% of the high-efficiency far-infrared graphene-nylon 6 composite fiber.

[0007] The production process conditions of FDY are: spinning temperature of 240-280°C, first godet speed of 4000-4500 m / min, second godet speed of 5000-6000 m / min, stretching ratio of 1.1-1.5 times, cooling air temperature of 15-25°C, wind speed of 0.5-1 m / s, relative humidity of 60%-90%, to obtain fully stretched yarn.

[0008] The production process conditions of UDY are: spinning temperature of 240-280°C, spinning speed of 700-1500m / min, cooling air temperature of 20-30°C, wind speed of 0.3-1m / s, relative humidity of 60%-80%, to obtain unoriented yarn.

[0009] The production process conditions of POY are: spinning temperature of 240-280°C, spinning speed of 4000-4500m / min, cooling air temperature of 15-25°C, wind speed of 0.3-0.6m / s, relative humidity of 60%-80%, to obtain pre-oriented yarn.

[0010] The production process conditions of HOY are: spinning temperature of 240-280°C, spinning speed of 4500-6000m / min, cooling air temperature of 15-20°C, wind speed of 0.3-0.5m / s, relative humidity of 80%-90%, to obtain highly oriented yarn.

[0011] The production process conditions of BCF are: spinning temperature of 240-280℃, cooling air temperature of 20-30℃, wind speed of 0.3-1m / s, relative humidity of 60%-80%, feeding roller temperature of 60-120℃, stretching roller temperature of 100-190℃, feeding speed of 300-1000m / min, stretching speed of 1000-3500m / min, stretching ratio of 3.5-5 times, deformation hot air temperature of 190-230℃, air injection pressure of 196kPa-490kPa, winding speed of 600-3000m / min, and cooling air temperature of 25℃.

[0012] The functions of acetylated calcium lignin sulfonate are: a flow aid for nylon 6 spinning, dispersing graphene and bonding graphene far-infrared nanopowder to nylon 6 chips. Graphene accounts for 0.4-2% of the fiber mass.

[0013] The present invention combines far-infrared nanopowder materials with nylon 6 and additives, and produces high-efficiency far-infrared graphene-nylon 6 composite fibers through high-speed melt spinning. This improves fiber performance, optimizes product quality, and produces composite fibers with excellent overall performance. Because the graphene is evenly dispersed within the composite fibers that comprise the fabric, the product exhibits excellent stability, is immune to UV absorber and screener precipitation, and exhibits UV protection. The present invention can be widely used in the production of protective and shielding products such as sunscreen clothing, parasols, tents, curtains, and swimsuits. The preparation process is suitable for large-scale production and can be well adapted to conventional fabric manufacturing equipment. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 AFM image of nanographene. DETAILED DESCRIPTION

[0015] The present invention is described in detail below with reference to the embodiments. The protection scope of the present invention is not limited to the embodiments, and any changes made by those skilled in the art within the scope defined by the claims also fall within the protection scope of the present invention.

[0016] Example 1

[0017] ⑴ Preparation of acetylated calcium lignin sulfonate: Weigh 20g of acetic anhydride and 30g of choline chloride into a flask, heat at 90°C to dissolve, continue heating for 1h, then add 4g of calcium lignin sulfonate, raise the temperature to 120°C and react for 12h. After the reaction, cool the mixture to room temperature in a cold water bath, pour the mixture into ethanol, filter under reduced pressure and wash thoroughly with ethanol. Finally, dry the product at 60°C for 18h to obtain acetylated calcium lignin sulfonate.

[0018] ⑵ Preparation of high-efficiency graphene far-infrared nanopowder material: According to the mass ratio, hafnium dioxide 10 parts, albite 5 parts, quartz 5 parts, borax 2 parts, nanographene sheet 90 parts, wet-grinded by sand mill for 1 hour, and dried. The AFM image of nanographene is as follows: Figure 1 shown.

[0019] ⑶ Preparation of high-efficiency far-infrared graphene-nylon 6 composite fiber: 0.6% additive, 2% high-efficiency graphene far-infrared nanopowder material (graphene mass accounts for 1.6% of fiber mass ratio) and 97.4% nylon 6 are mixed in a high-speed mixer for 15 minutes until the high-efficiency graphene far-infrared nanopowder material adheres to the nylon 6 slices, and the mixture is subjected to high-speed melt spinning (FDY) to obtain graphene / nylon 6 composite fiber.

[0020] (4) Production of FDY, process parameters: spinning temperature of 240-280 ° C, first godet speed of 4300-4500 m / min, second godet speed of 5500-6000 m / min, stretching ratio of 1.3-1.5 times, cooling air temperature of 20-25 ° C, wind speed of 0.5-7 m / s, relative humidity of 70%-80%, to obtain fully stretched yarn.

[0021] ⑸ Performance test: The obtained high-efficiency far-infrared graphene / nylon 6 composite fiber has an infrared emissivity of ≥86% in the wavelength range of 2-16 at room temperature, a fiber strength of 6.5cN / dtex, an elongation of 18%, and an elastic recovery rate of ≥80% at 18% elongation.

[0022] Example 2:

[0023] ⑴ Preparation of high-efficiency graphene far-infrared nanopowder material: the mass ratio is: 15 parts of hafnium dioxide, 8 parts of albite, 5 parts of quartz, 3 parts of borax, and 95 parts of nanographene sheets, which are wet-milled on a sand mill for 1 hour and dried.

[0024] (2) Preparation of high-efficiency far-infrared graphene / nylon 6 composite fiber: 1% additive, 1% high-efficiency graphene far-infrared nanopowder material (graphene mass proportion 0.75%) and 98% nylon 6 were mixed in a high-speed mixer for 15 minutes until the high-efficiency graphene far-infrared nanopowder material was attached to the nylon 6 slice, and the mixture was subjected to conventional melt spinning (UDY) to obtain graphene / nylon 6 composite fiber. The additive was prepared using acetylated calcium lignin sulfonate prepared in Example 1.

[0025] ⑶ Production of UDY, process parameters: The UDY process is specifically as follows: spinning temperature of 260-275 ° C, spinning speed of 1000-1200 m / min, cooling air temperature of 25-30 ° C, wind speed of 0.5-0.8 m / s, relative humidity of 70%-80%, to obtain unoriented yarn.

[0026] (4) Performance test: the obtained high-efficiency far-infrared graphene / nylon 6 composite fiber has an infrared emissivity of ≥92% in the wavelength range of 2-16 at room temperature, a fiber strength of 6.3cN / dtex, an elongation of 15%, and an elastic recovery rate of ≥82% at 15% elongation.

[0027] Example 3:

[0028] ⑴ Preparation of high-efficiency graphene far-infrared nanopowder material: the mass ratio is: 12 parts of hafnium dioxide, 10 parts of albite, 8 parts of quartz, 5 parts of borax, and 100 parts of nanographene sheets, which are wet-milled on a sand mill for 1 hour and dried.

[0029] (2) Preparation of high-efficiency far-infrared graphene / nylon 6 composite fiber: 3% additive, 4% high-efficiency graphene far-infrared nanopowder material (graphene mass accounts for 3%) and 93% nylon 6 were mixed in a high-speed mixer for 15 minutes until the graphene far-infrared nanopowder adhered to the nylon 6 slices. The mixture was subjected to conventional melt spinning (POY) to obtain graphene / nylon 6 composite fiber. The additive was prepared using acetylated calcium lignin sulfonate prepared in Example 1.

[0030] ⑶ Production of POY, the process parameters are: spinning temperature of 250-260 ° C, spinning speed of 4300-4500 m / min, cooling air temperature of 20-25 ° C, wind speed of 0.4-0.6 m / s, relative humidity of 70%-80%, to obtain pre-oriented yarn.

[0031] (4) Performance test: the obtained high-efficiency far-infrared graphene / nylon 6 composite fiber has an infrared emissivity of ≥90% in the wavelength range of 2-16 at room temperature, a fiber strength of 7.2 cN / dtex, an elongation of 20%, and an elastic recovery rate of ≥88% at 20% elongation.

[0032] Example 4:

[0033] ⑴ Preparation of high-efficiency graphene far-infrared nanopowder material: the mass ratio is: 20 parts of hafnium dioxide, 2 parts of albite, 10 parts of quartz, 5 parts of borax, and 85 parts of nanographene sheets, which are wet-milled on a sand mill for 1 hour and dried.

[0034] (2) Preparation of high-efficiency far-infrared graphene / nylon 6 composite fiber: 5% additive, 3% high-efficiency graphene far-infrared nanopowder material (graphene mass proportion 1.9%) and 92% nylon 6 were mixed in a high-pressure mixer for 15 minutes until the graphene far-infrared nanopowder adhered to the nylon 6 slices. The mixture was subjected to conventional melt pre-orientation spinning (HOY) to obtain graphene / nylon 6 composite fiber. The additive was prepared using acetylated calcium lignin sulfonate prepared in Example 1.

[0035] ⑶ Production of HOY, process parameters: spinning temperature 260-270℃, spinning speed 5500-5800m / min, cooling air temperature 15-20℃, wind speed 0.3-0.5m / s, relative humidity 80%-90%, to obtain highly oriented yarn.

[0036] (4) Performance test: The obtained high-efficiency far-infrared graphene / nylon 6 composite fiber has an infrared emissivity of ≥89% in the wavelength range of 2-16 at room temperature, a fiber strength of 6.8 cN / dtex, an elongation of 18%, and an elastic recovery rate of ≥86% at 18% elongation.

[0037] Example 5:

[0038] ⑴ Preparation of high-efficiency graphene far-infrared nanopowder material: the mass ratio is: 18 parts of hafnium dioxide, 4 parts of albite, 2 parts of quartz, 4 parts of borax, and 80 parts of nanographene sheets, which are wet-milled on a sand mill for 1 hour and dried.

[0039] (2) Preparation of high-efficiency far-infrared graphene / nylon 6 composite fiber: 2% additive, 2% high-efficiency graphene far-infrared nanopowder material (graphene mass proportion 1.5%) and 96% nylon 6 were mixed in a high-speed mixer for 15 minutes until the graphene far-infrared nanopowder adhered to the nylon 6 slices, and the mixture was subjected to conventional melt pre-oriented spinning (BCF) to obtain graphene / nylon 6 composite fiber. The additive was prepared using acetylated calcium lignin sulfonate prepared in Example 1.

[0040] ⑶ To produce BCF, the process parameters are: spinning temperature is 250-280℃, cooling air temperature is 25-30℃, wind speed is 0.5-0.7m / s, relative humidity is 70%-80%, feeding roller temperature is 80-100℃, stretching roller temperature is 150-180℃, feeding speed is 500-700m / min, stretching speed is 2000-2500m / min, stretching ratio is 4.5-5 times, deformation hot air temperature is 190-210℃, air injection pressure is 296kPa-390kPa, winding speed is 1600-2500m / min, and cooling air temperature is 25°.

[0041] (4) Performance test: The obtained high-efficiency far-infrared graphene / nylon 6 composite fiber has an infrared emissivity of ≥85% in the wavelength range of 2-16 at room temperature, a fiber strength of 6.6 cN / dtex, an elongation of 16%, and an elastic recovery rate of ≥85% at an elongation of 18%.

[0042] Example 6 (Compared with Example 1)

[0043] ⑴ Preparation of high-efficiency graphene far-infrared nanopowder material: the mass ratio is: 0 parts of hafnium dioxide, 5 parts of albite, 5 parts of quartz, 2 parts of borax, and 90 parts of nanographene sheets, which are wet-milled on a sand mill for 1 hour and dried.

[0044] (2) Preparation of high-efficiency far-infrared graphene / nylon 6 composite fiber: 0.6% additive, 2% high-efficiency graphene far-infrared nanopowder material (graphene mass accounts for 1.8% of fiber mass ratio) and 97.4% nylon 6 were mixed in a high-speed mixer for 15 minutes until the graphene far-infrared nanopowder adhered to the nylon 6 slice, and the mixture was subjected to high-speed melt spinning (FDY) to obtain graphene / nylon 6 composite fiber. The additive was prepared using acetylated calcium lignin sulfonate prepared in Example 1.

[0045] ⑶ Production of FDY, process parameters: spinning temperature of 240-280℃, first godet speed of 4300-4500m / min, second godet speed of 5500-6000m / min, stretching ratio of 1.3-1.5 times, cooling air temperature of 20-25℃, wind speed of 0.5-7m / s, relative humidity of 70%-80%, to obtain fully stretched yarn.

[0046] (4) Performance test: The obtained high-efficiency far-infrared graphene / nylon 6 composite fiber has an infrared emissivity of ≥75% in the wavelength range of 2-16 at room temperature, a fiber strength of 6.8 cN / dtex, an elongation of 18%, and an elastic recovery rate of ≥85% at 18% elongation.

[0047] Example 7 (Compared with Example 4)

[0048] ⑴ Preparation of high-efficiency graphene far-infrared nanopowder material: the mass ratio is: 20 parts of hafnium dioxide, 2 parts of albite, 10 parts of quartz, 5 parts of borax, and 0 parts of nanographene sheet, which is wet-milled on a sand mill for 1 hour and dried.

[0049] (2) Preparation of high-efficiency far-infrared graphene / nylon 6 composite fiber: 5% additive, 3% high-efficiency graphene far-infrared nanopowder material (graphene mass proportion 0%) and 92% nylon 6 were mixed in a high-speed mixer for 15 minutes until the graphene far-infrared nanopowder adhered to the nylon 6 slices. The mixture was subjected to conventional melt pre-orientation spinning (HOY) to obtain graphene / nylon 6 composite fiber. The additive was prepared using acetylated calcium lignin sulfonate prepared in Example 1.

[0050] ⑶ Production of HOY, process parameters: spinning temperature 260-270℃, spinning speed 5500-5800m / min, cooling air temperature 15-20℃, wind speed 0.3-0.5m / s, relative humidity 80%-90%, to obtain highly oriented yarn

[0051] (4) Performance test: The obtained high-efficiency far-infrared graphene / nylon 6 composite fiber has an infrared emissivity of ≥50% in the wavelength range of 2-16 at room temperature, a fiber strength of 5.8 cN / dtex, an elongation of 12%, and an elastic recovery rate of ≥70% at 12% elongation.

[0052] Examples (Comparative Examples) 6 and 7, which lack nanographene (75%) and hafnium dioxide (50%), respectively, show significant differences in far-infrared emissivity compared to Examples 1 and 4. This comparison demonstrates that far-infrared emissivity is significantly enhanced only when both nanographene and hafnium dioxide are present, demonstrating the synergistic effect of the two materials.

Claims

1. A high-efficiency far-infrared graphene-nylon 6 composite fiber, characterized by: The composite fiber is obtained by a high-efficiency graphene far-infrared nanopowder material, an additive and nylon 6 through a high-speed melt spinning process. The mass ratio of the high-efficiency graphene far-infrared nanopowder material to nylon 6 is 0.3-0.5:

100. The products of the high-efficiency far-infrared graphene-nylon 6 composite fiber include FDY, UDY, POY, HOY and BCF.

2. The high-efficiency far-infrared graphene-nylon 6 composite fiber according to claim 1, characterized in that: The high-efficiency graphene is a nanographene sheet; the high-efficiency graphene far-infrared nanopowder material is prepared by wet-grinding hafnium dioxide, albite, quartz, borax and nanographene sheets with a sand mill for 1 hour and then drying. The composition of the material by mass is: 10 to 20 parts of hafnium dioxide, 5 to 10 parts of albite, 1 to 10 parts of quartz, 2 to 5 parts of borax and 80 to 100 parts of nanographene sheets.

3. The high-efficiency far-infrared graphene-nylon 6 composite fiber according to claim 2, characterized in that: The plane size of the nanographene sheet is 0.03-0.3 μm 2 , thickness 0.8-3nm.

4. The high-efficiency far-infrared graphene-nylon 6 composite fiber according to claim 1, characterized in that: The auxiliary agent is acetylated calcium lignin sulfonate, and the amount of the auxiliary agent used is 0.6-5wt% of the high-efficiency far-infrared graphene-nylon 6 composite fiber.

5. The high-efficiency far-infrared graphene-nylon 6 composite fiber according to claim 1, characterized in that: The production process conditions of the FDY are: a spinning temperature of 240-280°C, a first godet speed of 4000-4500 m / min, a second godet speed of 5000-6000 m / min, a stretching ratio of 1.1-1.5 times, a cooling air temperature of 15-25°C, a wind speed of 0.5-1 m / s, and a relative humidity of 60%-90%.

6. The high-efficiency far-infrared graphene-nylon 6 composite fiber according to claim 1, characterized in that: The production process conditions of the UDY are: spinning temperature of 240-280° C., spinning speed of 700-1500 m / min, cooling air temperature of 20-30° C., wind speed of 0.3-1 m / s, and relative humidity of 60%-80%.

7. The high-efficiency far-infrared graphene-nylon 6 composite fiber according to claim 1, characterized in that: The production process conditions of the POY are: spinning temperature of 240-280° C., spinning speed of 4000-4500 m / min, cooling air temperature of 15-25° C., wind speed of 0.3-0.6 m / s, and relative humidity of 60%-80%.

8. The high-efficiency far-infrared graphene-nylon 6 composite fiber according to claim 1, characterized in that: The production process conditions of the HOY are: spinning temperature of 240-280° C., spinning speed of 4500-6000 m / min, cooling air temperature of 15-20° C., wind speed of 0.3-0.5 m / s, and relative humidity of 80%-90%.

9. The high-efficiency far-infrared graphene-nylon 6 composite fiber according to claim 1, characterized in that: The production process conditions of the BCF are: spinning temperature of 240-280°C, cooling air temperature of 20-30°C, wind speed of 0.3-1m / s, relative humidity of 60%-80%, feeding roller temperature of 60-120°C, stretching roller temperature of 100-190°C, feeding speed of 300-1000m / min, stretching speed of 1000-3500m / min, stretching ratio of 3.5-5 times, deformation hot air temperature of 190-230°C, air injection pressure of 196kPa-490kPa, winding speed of 600-3000m / min, and cooling air temperature of 25°.

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