Inorganic particle embedded spinning method for improving performance of organic fibers

Abstract

The invention discloses an inorganic particle embedded spinning method for improving the performance of organic fibers, and belongs to the technical field of functional fiber preparation. According to the method, inorganic powder particles are embedded into a spinning solution of organic fibers, and the composite fibers with remarkably improved acid and alkali resistance are prepared by utilizing a wet spinning process. The method comprises the following specific steps: mixing an organic fiber raw material and inorganic powder, and stirring at high speed to form a uniform spinning solution; defoaming the spinning solution, then carrying out wet spinning, stretching the extruded fiber, and immersing into a coagulating bath to form the fiber; and finally, carrying out post-treatment to obtain the dried composite fiber. Compared with the prior art, by introducing the ultrasonic vibration device, the heating device and the magnetic stirring device, the layering problem during mixing of inorganic powder and organic fibers is solved, it is ensured that inorganic particles are evenly distributed on the surfaces of the fibers, the acid and alkali resistance of the fibers is remarkably improved, meanwhile, the mechanical property and the dyeing property of the fibers are kept, and the application prospect is wide. Wide application prospects are realized.

Description

Technical Field

[0001] The present invention relates to the technical field of functional fiber preparation, and particularly to an inorganic particle embedded spinning method for improving the properties of organic fibers. Background Art

[0002] Wet spinning is a process widely used in the production of synthetic fibers and modified natural polymer fibers. By dissolving the fiber-forming polymer in an appropriate solvent to form a spinning dope, and then through processes such as mixing, filtering, and degassing, finally spinning into fibers through a wet spinning machine. This process can produce a variety of synthetic fibers (such as polyester fibers, polyacrylonitrile fibers, nylon fibers, etc.) and natural polymer fibers (such as alginate fibers, cellulose fibers, etc.), and has a wide range of applications in the fields of clothing, home textiles, industrial filter materials, medical supplies, etc.

[0003] However, in the traditional wet spinning process, when inorganic powder is mixed with organic fiber raw materials, a series of technical challenges are often faced. The inorganic powder is prone to precipitation in the mixed solution, resulting in the stratification of the mixed solution and making it difficult to achieve uniform dispersion. This stratification phenomenon is particularly obvious when the inorganic powder is mixed with organic fiber raw materials, especially when the inorganic powder is solid particles and the organic fiber is a liquid solution, and solid-liquid separation is likely to occur after mixing.

[0004] In the production of alkali-resistant glass fibers, the addition of zirconia can significantly improve the alkali resistance of the fibers. This is because zirconia can be melted and mixed with the glass fibers at high temperatures to form a uniform composite material. However, this high-temperature treatment is not applicable to the wet spinning of organic fibers because organic fibers are usually spun at low temperatures and cannot achieve uniform mixing like glass fibers through high-temperature melting. Therefore, when zirconia is mixed with organic fibers, the solid form of the inorganic powder will cause the stratification of the mixed solution and it is difficult to be uniformly dispersed inside the fibers.

[0005] In addition, even if the inorganic powder can be uniformly dispersed inside the fibers, it will have a negative impact on the properties of the fibers. The presence of the inorganic powder will interfere with the orientation of the polymer chains inside the organic fibers and destroy the crystal structure of the fibers. The orientation of the polymer chains is a key factor in the mechanical properties of the fibers, and the orderliness of their arrangement directly affects the strength of the fibers. When the inorganic powder is embedded inside the fibers, the continuity and orientation of the polymer chains are destroyed, resulting in a decrease in the strength of the fibers. For example, after adding inorganic powder to alginate fibers, the elongation at break of the fibers decreases, and the breaking strength is also affected.

[0006] To solve the above problems, various methods have been tried in the prior art. For example, chemical modification of inorganic powder and organic fiber raw materials is used to prevent the precipitation of inorganic powder and ensure the uniformity of the mixed solution. However, these methods still cannot completely solve the layering problem when inorganic powder is mixed with organic fiber, nor can they avoid the negative impact of inorganic powder on the fiber strength.

[0007] Therefore, developing a spinning method that can effectively solve the layering problem when inorganic powder is mixed with organic fiber and can improve the acid and alkali resistance of the fiber without reducing the fiber strength is an urgent technical problem to be solved in the current fiber material processing field.

[0008] Chinese invention patent CN115726060A discloses a gel fiber with a wrinkled surface structure, its preparation method and application. The alginate solution and agar solution are thermally mixed, and then the mixed solution is extruded from a spinneret at a certain rate and immersed in a metal cation solution at room temperature; then the fiber is frozen in liquid nitrogen and finally vacuum frozen to obtain a gel fiber with a wrinkled surface structure. The invention uses temperature-sensitive agar and ion-responsive alginate polymers for wet spinning, uses a metal cation solution as a coagulation bath, and the complexation of metal cations can improve the mechanical properties of the gel fiber. By using the methods of pre-condensation and secondary ultra-low temperature freezing, and controlling the extrusion rate and liquid nitrogen freezing time, the microstructure of the fiber is controlled to achieve anisotropic shrinkage and the formation of a wrinkled surface structure, endowing the fiber with strong capillary action; when used for lateral chromatography, it realizes high-throughput, high-precision, and micro-sample detection, overcoming the defects of existing chromatography film carriers. However, the gel fiber prepared by this method still has room for improvement in terms of mechanical properties, dyeing properties, and acid and alkali resistance. Summary of the Invention

[0009] To solve the deficiencies in the prior art, the present invention aims to provide an innovative inorganic particle-embedded spinning method. By optimizing the mixing process and spinning conditions, the uniform embedding of inorganic powder on the surface or inside of the fiber is achieved, significantly improving the acid and alkali resistance of the fiber while maintaining the mechanical properties of the fiber.

[0010] To achieve the above invention purpose, the present invention adopts the following technical solutions:

[0011] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0012] Step 1, Mixing: Weigh the organic fiber raw material and inorganic powder, add the organic fiber raw material and inorganic powder into a beaker, add water to prepare a mixed solution, place the mixed solution on a magnetic stirrer, and stir at high speed for 1 to 3 hours to ensure the uniformity of the mixed solution and obtain a spinning solution;

[0013] Step 2: Spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 1 to 20 hours to remove the air bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; pour the degassed spinning solution into the feed port of a wet spinning machine, turn on the wet spinning machine, extrude the spinning solution, stretch the extruded fibers, and immerse them in a coagulation bath to form fibers, wind the fibers onto a drawing device with a rotational speed of 5 to 30 rpm / min, and collect them using a tube to achieve continuous spinning of fibers;

[0014] Step 3: Post-treatment: Immerse the fiber tube spun in Step 2 in the coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain dry composite filaments.

[0015] Preferably, the inorganic particle embedded spinning method for improving the properties of organic fibers is as follows:

[0016] Step 1: Mixing: Weigh the organic fiber raw material and inorganic powder, add the organic fiber raw material and inorganic powder into a beaker, add water to prepare a mixed solution, place the mixed solution on a magnetic stirrer, and stir at high speed for 1 to 3 hours to ensure the uniformity of the mixed solution and obtain a spinning solution;

[0017] Step 2: Spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 1 to 20 hours to remove the air bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; pour the degassed spinning solution into the feed port of a wet spinning machine. To prevent the precipitation of inorganic powder, add an ultrasonic vibration device to the spinning solution to improve the uniformity of the mixed solution. The ultrasonic power is 200 to 400 W and the ultrasonic frequency is 20 to 60 kHz. Turn on the wet spinning machine, extrude the spinning solution, stretch the extruded fibers, and immerse them in a coagulation bath to form fibers, wind the fibers onto a drawing device with a rotational speed of 5 to 30 rpm / min, and collect them using a tube to achieve continuous spinning of fibers;

[0018] Step 3: Post-treatment: Immerse the fiber tube spun in Step 2 in the coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain dry composite filaments.

[0019] Preferably, the inorganic particle embedded spinning method for improving the properties of organic fibers is as follows:

[0020] Step 1: Mixing: Weigh the organic fiber raw material and inorganic powder, add the organic fiber raw material and inorganic powder into a beaker, add water to prepare a mixed solution, place the mixed solution on a magnetic stirrer, and stir at high speed for 1 to 3 hours to ensure the uniformity of the mixed solution and obtain a spinning solution;

[0021] Step 2: Spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 1 to 20 hours to remove the air bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; pour the degassed spinning solution into the feed inlet of a wet spinning machine, turn on the wet spinning machine, extrude the spinning solution. To prevent precipitation of inorganic powder, an ultrasonic vibration device is added at the spinneret to improve the uniformity of the mixed solution. The ultrasonic power is 200 - 400 W and the ultrasonic frequency is 20 - 60 kHz. The extruded fibers are stretched and immersed in a coagulation bath to form fibers, and the fibers are wound onto a drafting device with a rotational speed of 5 - 30 rpm / min and collected using a tube to achieve continuous spinning of fibers;

[0022] Step 3: Post-treatment: Immerse the fiber tube spun in Step 2 in the coagulation bath for 10 - 50 minutes, take it out and let it stand at room temperature for 5 - 48 hours to obtain dry composite filaments.

[0023] Further preferably, the inorganic particle-embedded spinning method for enhancing the properties of organic fibers is as follows:

[0024] Step 1: Mixing: Weigh the organic fiber raw material and inorganic powder, add the organic fiber raw material and inorganic powder into beakers respectively, add water, and prepare an organic fiber solution and an inorganic powder suspension respectively. Place the organic fiber solution and the inorganic powder suspension in a magnetic stirrer and stir at high speed for 1 - 3 hours to ensure the uniformity of the mixed solution;

[0025] Step 2: Spinning of fibers: Pour the organic fiber solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 1 to 20 hours to remove the air bubbles in the organic fiber solution and ensure the uniformity and stability of the organic fiber solution; pour the degassed organic fiber solution into the feed inlet of a wet spinning machine, turn on the wet spinning machine, extrude the organic fiber solution. The extruded fibers are stretched and immersed in the inorganic powder suspension prepared in Step 1, and then immersed in a coagulation bath to form fibers. The fibers are wound onto a drafting device with a rotational speed of 5 - 30 rpm / min and collected using a tube to achieve continuous spinning of fibers;

[0026] Step 3: Post-treatment: Immerse the fiber tube spun in Step 2 in the coagulation bath for 10 - 50 minutes, take it out and let it stand at room temperature for 5 - 48 hours to obtain dry composite filaments.

[0027] Further preferably, the inorganic particle-embedded spinning method for enhancing the properties of organic fibers is as follows:

[0028] Step 1, Mixing: Weigh the organic fiber raw material and the inorganic powder. Add the organic fiber raw material and the inorganic powder into beakers respectively, add water, and prepare an organic fiber solution and an inorganic powder suspension respectively. Place the organic fiber solution and the inorganic powder suspension in a magnetic stirrer and stir at high speed for 1 - 3 hours to ensure the uniformity of the mixture.

[0029] Step 2, Fiber Spinning: Pour the organic fiber solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 1 - 20 hours to remove the bubbles in the organic fiber solution and ensure the uniformity and stability of the organic fiber solution. Pour the degassed organic fiber solution into the feed inlet of a wet spinning machine, turn on the wet spinning machine, extrude the organic fiber solution, stretch the extruded fiber, immerse it in the inorganic powder suspension prepared in Step 1, add an ultrasonic vibration device to the inorganic powder suspension, with an ultrasonic power of 200 - 400 W and an ultrasonic frequency of 20 - 60 kHz, then immerse it in a coagulation bath to form a fiber, wind the fiber onto a drafting device with a rotational speed of 5 - 30 rpm / min, and collect it using a tube to achieve continuous spinning of the fiber.

[0030] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in the coagulation bath for 10 - 50 minutes, take it out and let it stand at room temperature for 5 - 48 hours to obtain a dry composite filament.

[0031] Further preferably, the inorganic particle embedded spinning method for improving the properties of organic fibers is as follows:

[0032] Step 1, Mixing: Weigh the organic fiber raw material and the inorganic powder. Add the organic fiber raw material and the inorganic powder into beakers respectively, add water, and prepare an organic fiber solution and an inorganic powder suspension respectively. Place the organic fiber solution and the inorganic powder suspension in a magnetic stirrer and stir at high speed for 1 - 3 hours to ensure the uniformity of the mixture.

[0033] Step 2, Fiber Spinning: Pour the organic fiber solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 1 - 20 hours to remove the bubbles in the organic fiber solution and ensure the uniformity and stability of the organic fiber solution. Pour the degassed organic fiber solution into the feed inlet of a wet spinning machine, turn on the wet spinning machine, extrude the organic fiber solution, stretch the extruded fiber, immerse it in the inorganic powder suspension prepared in Step 1, add an ultrasonic vibration device to the inorganic powder suspension, with an ultrasonic power of 200 - 400 W and an ultrasonic frequency of 20 - 60 kHz, and add a heating device to control the temperature of the inorganic powder suspension at 30 - 60 °C, then immerse it in a coagulation bath to form a fiber, wind the fiber onto a drafting device with a rotational speed of 5 - 30 rpm / min, and collect it using a tube to achieve continuous spinning of the fiber.

[0034] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in a coagulation bath for 10 - 50 minutes, take it out and let it stand at room temperature for 5 - 48 hours to obtain dry composite filaments.

[0035] Further preferably, the inorganic particle-embedded spinning method for enhancing the properties of organic fibers is as follows:

[0036] Step 1, Mixing: Weigh the organic fiber raw material and inorganic powder, add the organic fiber raw material and inorganic powder into beakers respectively, add water, and prepare an organic fiber solution and an inorganic powder suspension respectively. Place the organic fiber solution and the inorganic powder suspension in a magnetic stirrer and stir at high speed for 1 - 3 hours to ensure the uniformity of the mixture.

[0037] Step 2, Spinning of fibers: Pour the organic fiber solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 1 - 20 hours to remove the bubbles in the organic fiber solution and ensure the uniformity and stability of the organic fiber solution; pour the degassed organic fiber solution into the feed port of a wet spinning machine, turn on the wet spinning machine, extrude the organic fiber solution, stretch the extruded fibers, and immerse them in the inorganic powder suspension prepared in Step 1. Add an ultrasonic vibration device to the inorganic powder suspension, with an ultrasonic power of 200 - 400 W and an ultrasonic frequency of 20 - 60 kHz, and add a heating device to control the temperature of the inorganic powder suspension at 30 - 60 °C. Further add a magnetic stirring device to control the speed of the magnetic stirring device at 100 - 500 rpm, then immerse it in a coagulation bath to form fibers, wind the fibers onto a drafting device with a rotational speed of 5 - 30 rpm / min, and collect them using a tube to achieve continuous spinning of fibers.

[0038] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in a coagulation bath for 10 - 50 minutes, take it out and let it stand at room temperature for 5 - 48 hours to obtain dry composite filaments.

[0039] The mass fraction of the organic fiber raw material in the mixed solution is 0 - 2 wt%, and the mass fraction of the inorganic powder is 0 - 2 wt%.

[0040] The organic fiber raw material is at least one of sodium alginate, chitosan, wood, and cellulose.

[0041] The inorganic powder is at least one of zirconia, silica, alumina, titanium dioxide, calcium carbonate, magnesium oxide, zinc oxide, talc powder, and kaolin.

[0042] The extrusion speed of the injection pump of the wet spinning machine is 1 mL / min, the pore diameter of the spinneret is 1 mm, and the rotational speed of the drafting device is 20 rpm.

[0043] The coagulation bath is at least one of an aqueous calcium chloride solution, an aqueous ethylene glycol solution, an aqueous N,N-dimethylformamide solution, an aqueous isopropyl alcohol solution, an aqueous dimethyl sulfoxide solution, methanol, and water.

[0044] Preferably, the organic fiber raw material is sodium alginate; the inorganic powder is zirconia.

[0045] In the traditional wet spinning process, when the inorganic powder is mixed with the organic fiber raw material, layering is likely to occur, resulting in poor uniformity of the mixed solution, difficulty in fiber formation during the spinning process, and uneven properties of the final fiber. To solve this problem, the present invention introduces an ultrasonic vibration device during the mixing process. By utilizing its high-frequency vibration and cavitation effect, the agglomeration of the inorganic powder is effectively broken, preventing it from precipitating during the mixing process, thereby ensuring the uniform dispersion of the inorganic powder and the organic fiber raw material. This improvement not only enhances the uniformity and stability of the mixed solution but also optimizes the operability of the spinning process, enabling the fiber to be successfully formed and maintaining good property uniformity. Through the auxiliary action of ultrasonic waves, the present invention realizes the uniform embedding of the inorganic powder in the fiber, significantly improving the acid and alkali resistance of the fiber. At the same time, it avoids the performance fluctuations of the fiber caused by layering, providing an efficient and reliable technical means for the preparation of high-performance composite fibers.

[0046] An ultrasonic vibration device is added at the spinneret to further prevent the inorganic powder from precipitating during the spinning process. The spinneret is a key part for fiber formation. Ultrasonic vibration can ensure that the inorganic powder is still evenly distributed inside the fiber during the extrusion process, avoiding fiber property differences caused by local concentration unevenness, and at the same time improving the acid and alkali resistance and mechanical properties of the fiber.

[0047] In the above wet spinning process, when the inorganic powder is directly mixed with the organic fiber raw material, although the acid and alkali resistance of the fiber can be improved, the uniform dispersion of the inorganic powder inside the fiber often causes interference to the orientation of the polymer chains inside the fiber, thereby reducing the strength of the fiber. To solve this problem, the present invention adopts an innovative strategy: the organic fiber raw material and the inorganic powder are respectively prepared into a solution and a suspension, and then the inorganic powder suspension is embedded on the surface of the organic fiber through a specific process, rather than being directly mixed into the fiber interior. This surface embedding method not only effectively avoids the interference of the inorganic powder to the orientation of the polymer chains inside the fiber but also significantly reduces the negative impact on the fiber strength.

[0048] Although the method of preparing an inorganic powder into a turbid solution and embedding it on the surface of organic fibers can effectively avoid the negative impact on the internal structure and strength of the fibers, there is still a key problem with relying solely on turbid solution treatment: the inorganic powder is prone to agglomeration and sedimentation in the turbid solution, resulting in uneven embedding on the fiber surface, which in turn affects the improvement effect of fiber properties. To address this defect, the present invention further introduces an ultrasonic vibration device, a heating device, and a magnetic stirring device. The ultrasonic vibration can effectively break the agglomeration of the inorganic powder through high-frequency vibration and cavitation effect, keeping it in a good dispersed state; at the same time, the heating device can reduce the viscosity of the turbid solution, further enhancing the dispersibility and fluidity of the inorganic powder. The magnetic stirring ensures the uniform dispersion of the inorganic powder in the zirconia turbid solution, avoiding local agglomeration, while reducing the viscosity of the turbid solution, enhancing the fluidity of the inorganic particles, and enabling them to be more evenly embedded on the fiber surface to form a stable reinforcing layer. The synergistic effect of the three ensures the uniform distribution of the inorganic powder on the fiber surface, thereby significantly improving the acid and alkali resistance of the fiber, while avoiding performance fluctuations caused by uneven dispersion. This improvement not only optimizes the functionality of the fiber but also enhances the stability and reliability of the production process, providing strong technical support for the preparation of high-performance composite fibers.

[0049] In the present invention, sodium alginate is used as the raw material for organic fibers and combined with zirconia inorganic powder, giving full play to the advantages of both. Sodium alginate has good biocompatibility, biodegradability, and fiber-forming properties, making it have broad application prospects in the fields of medicine, food, and environmental protection. However, the acid and alkali resistance of alginate fibers is relatively weak. By introducing zirconia powder, with its excellent acid and alkali resistance, chemical stability, and mechanical strength, the stability of the fiber in an acid-base environment is significantly improved. At the same time, the addition of zirconia does not have a negative impact on the biocompatibility and dyeing properties of sodium alginate fibers. This organic-inorganic composite system not only optimizes the comprehensive properties of the fiber but also expands its application range in the field of high-performance materials, achieving an organic combination of functionality and practicality.

[0050] Through the above improvements, the present invention not only solves the delamination problem when mixing inorganic powder and organic fibers but also significantly improves the acid and alkali resistance, mechanical properties, and dyeing properties of the fibers, while maintaining the original characteristics of the fibers, making them more widely used in industrial and medical fields.

[0051] Compared with the prior art, it has the following beneficial effects:

[0052] 1) By embedding inorganic powder in the organic fiber spinning solution in the present invention, the acid and alkali resistance of the fiber is significantly enhanced. The solubility of the composite fiber modified with inorganic powder in an acid-base environment is greatly reduced, and its acid and alkali resistance is significantly better than that of the unmodified organic fiber, while maintaining the original crystallinity and internal structure of the fiber.

[0053] 2) By introducing an ultrasonic vibration device, a heating device, and a magnetic stirring device, the present invention solves the problem of easy delamination when inorganic powder and organic fiber are mixed, ensuring the uniform distribution of inorganic particles inside or on the surface of the fiber. This uniformity not only improves the overall performance of the fiber but also optimizes the stability and operability of the spinning process, reducing production costs.

[0054] 3) While enhancing the acid and alkali resistance performance, the present invention will not have a negative impact on the mechanical properties, dyeing properties, and flame retardant properties of the fiber. The modified fiber can still maintain good dyeing uniformity in an acid-base environment, and its flame retardant property is not affected, having broader application potential. Brief Description of the Drawings

[0055] Figure 1 Wet spinning equipment model diagram of Step 2 in Example 10;

[0056] Figure 2 Embedded spinning flow chart;

[0057] Figure 3 Physical map and 3D microscope map (surface) of the composite filaments prepared in Examples 1 - 4;

[0058] Figure 4 SEM pictures of the enlarged surface and cross-section of the composite filaments prepared in Examples 1 - 4;

[0059] Figure 5 Comparison of the physical maps of the composite filaments before and after alkali treatment in Example 2 and Example 4;

[0060] Figure 6 Comparison of the 3D microscope surfaces of the composite filaments before and after alkali treatment in Example 2 and Example 4;

[0061] Figure 7 Comparison of the physical maps before and after dyeing of the non-alkali-treated composite filament in Example 2, the composite filament after alkali treatment in Example 2, and the composite filament after alkali treatment in Example 4;

[0062] Figure 8 3D microscope maps before and after dyeing of the non-alkali-treated composite filament in Example 2, the composite filament after alkali treatment in Example 2, and the composite filament after alkali treatment in Example 4; Detailed Embodiments

[0063] To better understand the present invention, the following further clarifies the content of the present invention in combination with examples. However, the present invention is not limited to the following examples. The described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. The specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0064] Main sources of substances:

[0065] Sodium alginate, product number: 9005383, molecular weight: 216.12303 (sugar unit), Henan Anrui Biotechnology Co., Ltd.

[0066] Zirconia, model: ZO-P-0Y, particle size: 0.3 - 50um, specific surface area available range: 3 - 150m 2 / g, Pingxiang Baitian New Materials Co., Ltd.

[0067] The remaining raw materials in the examples and comparative examples of the present invention are all commercially available products.

[0068] The design idea of the present invention is to embed inorganic powder particles in the spinning solution of organic fibers, and use the wet spinning process to prepare composite fibers with significantly improved acid and alkali resistance. During the design process, aiming at the layering problem that easily occurs when inorganic powder is mixed with organic fibers, an ultrasonic vibration device, a heating device and a magnetic stirring device are introduced to ensure the uniform dispersion of inorganic powder, so as to achieve the uniform embedding of inorganic particles inside or on the surface of the fiber. In addition, by optimizing the ratio of organic fiber to inorganic powder, the stirring and degassing process of the spinning solution, and the composition and treatment conditions of the coagulation bath, the comprehensive performance of the fiber is further improved, so that while maintaining the original mechanical properties and dyeing properties, the acid and alkali resistance is significantly enhanced, and its application range in the industrial field is broadened.

[0069] Example 1

[0070] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0071] Step 1, mixing: Weigh sodium alginate, add sodium alginate to a beaker, add water, and configure it into a mixed solution with a mass fraction of 1%. Place the mixed solution in a magnetic stirrer and stir at 500 rpm for 2 hours to ensure the uniformity of the mixed solution and obtain a spinning solution.

[0072] Step 2, spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 12 hours to remove the bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; pour the degassed spinning solution into the feed port of a wet spinning machine, turn on the wet spinning machine, extrude the spinning solution, stretch the extruded fiber, the extrusion speed is 1 mL / min, the pore diameter of the spinneret is 1 mm, the rotation speed of the drafting device is 20 rpm, and immerse it in a calcium chloride aqueous solution with a mass fraction of 3% to form fibers. Wind the fibers onto a drafting device with a rotation speed of 20 rpm / min and collect them using a tube to achieve continuous spinning of the fibers.

[0073] Step 3, post-treatment: Immerse the fiber tube spun in Step 2 in a calcium chloride aqueous solution with a mass fraction of 3% for 30 minutes, take it out and let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0074] Example 2

[0075] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0076] Step 1, Mixing: Weigh sodium alginate, add sodium alginate into a beaker, add water, and prepare a mixed solution with a mass fraction of 2%. Place the mixed solution on a magnetic stirrer and stir at 500 rpm for 2 hours to ensure the uniformity of the mixed solution, obtaining a spinning solution;

[0077] Step 2, Spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 12 hours to remove the bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; Pour the degassed spinning solution into the feed port of a wet spinning machine, turn on the wet spinning machine, extrude the spinning solution, stretch the extruded fibers, with an extrusion speed of 1 mL / min, a spinneret hole diameter of 1 mm, a draw unit rotation speed of 20 rpm, and immerse it in a calcium chloride aqueous solution with a mass fraction of 3% to form fibers. Wind the fibers onto a draw unit with a rotation speed of 20 rpm / min and collect them using a tube to achieve continuous spinning of the fibers;

[0078] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in a calcium chloride aqueous solution with a mass fraction of 3% for 30 minutes, take it out and let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0079] Example 3

[0080] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0081] Step 1, Mixing: Weigh sodium alginate and zirconia, add sodium alginate and zirconia into a beaker, add water, and prepare a mixed solution containing 1% sodium alginate and 1% zirconia by mass. Place the mixed solution on a magnetic stirrer and stir at 500 rpm for 2 hours to ensure the uniformity of the mixed solution, obtaining a spinning solution;

[0082] Step 2, Spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for degassing for 12 hours to remove the bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; Pour the degassed spinning solution into the feed port of a wet spinning machine, turn on the wet spinning machine, extrude the spinning solution, stretch the extruded fibers, with an extrusion speed of 1 mL / min, a spinneret hole diameter of 1 mm, a draw unit rotation speed of 20 rpm, and immerse it in a calcium chloride aqueous solution with a mass fraction of 3% to form fibers. Wind the fibers onto a draw unit with a rotation speed of 20 rpm / min and collect them using a tube to achieve continuous spinning of the fibers;

[0083] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in an aqueous calcium chloride solution with a mass fraction of 3% for 30 minutes, take it out and let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0084] Example 4

[0085] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0086] Step 1, Mixing: Weigh sodium alginate and zirconia, add sodium alginate and zirconia to a beaker, add water to prepare a mixed solution containing 2% sodium alginate and 2% zirconia by mass fraction. Place the mixed solution on a magnetic stirrer and stir at 500 rpm for 2 hours to ensure the uniformity of the mixed solution and obtain a spinning solution.

[0087] Step 2, Spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for defoaming for 12 hours to remove the bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution. Pour the defoamed spinning solution into the feed port of a wet spinning machine, turn on the wet spinning machine, extrude the spinning solution, stretch the extruded fibers, with an extrusion speed of 1 mL / min, a spinneret hole diameter of 1 mm, a draw unit rotation speed of 20 rpm, and immerse it in an aqueous calcium chloride solution with a mass fraction of 3% to form fibers. Wind the fibers onto a draw unit rotating at 20 rpm / min and collect them using a tube to achieve continuous spinning of the fibers.

[0088] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in an aqueous calcium chloride solution with a mass fraction of 3% for 30 minutes, take it out and let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0089] Example 5

[0090] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0091] Step 1, Mixing: Weigh sodium alginate and zirconia, add sodium alginate and zirconia to a beaker, add water to prepare a mixed solution containing 2% sodium alginate and 2% zirconia by mass fraction. Place the mixed solution on a magnetic stirrer and stir at 500 rpm for 2 hours to ensure the uniformity of the mixed solution and obtain a spinning solution.

[0092] Step 2, spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for 12 hours to degas and remove air bubbles in the spinning solution, ensuring the uniformity and stability of the spinning solution; Pour the degassed spinning solution into the feed port of a wet spinning machine, add an ultrasonic vibration device to the spinning solution to improve the uniformity of the mixed solution, with an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, turn on the wet spinning machine, extrude the spinning solution, stretch the extruded fibers, with an extrusion speed of 1 mL / min, a spinneret hole diameter of 1 mm, a draw unit rotation speed of 20 rpm, and immerse them in a 3% calcium chloride aqueous solution to form fibers, wind the fibers onto a draw unit with a rotation speed of 20 rpm / min, and collect them using a tube to achieve continuous spinning of fibers;

[0093] Step 3, post-treatment: Immerse the fiber tube spun in Step 2 in a 3% calcium chloride aqueous solution for 30 minutes, take it out and let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0094] Example 6

[0095] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0096] Step 1, mixing: Weigh sodium alginate and zirconia, add sodium alginate and zirconia to a beaker, add water, and prepare a mixed solution containing 2% sodium alginate and 2% zirconia by mass fraction. Place the mixed solution on a magnetic stirrer and stir at 500 rpm for 2 hours to ensure the uniformity of the mixed solution and obtain a spinning solution;

[0097] Step 2, spinning of fibers: Pour the spinning solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for 12 hours to degas and remove air bubbles in the spinning solution, ensuring the uniformity and stability of the spinning solution; Pour the degassed spinning solution into the feed port of a wet spinning machine, turn on the wet spinning machine, extrude the spinning solution, and to prevent precipitation of inorganic powder, add an ultrasonic vibration device at the spinneret to improve the uniformity of the mixed solution, with an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, stretch the extruded fibers, with an extrusion speed of 1 mL / min, a spinneret hole diameter of 1 mm, a draw unit rotation speed of 20 rpm, and immerse them in a 3% calcium chloride aqueous solution to form fibers, wind the fibers onto a draw unit with a rotation speed of 20 rpm / min, and collect them using a tube to achieve continuous spinning of fibers;

[0098] Step 3, post-treatment: Immerse the fiber tube spun in Step 2 in a 3% calcium chloride aqueous solution for 30 minutes, take it out and let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0099] Example 7

[0100] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0101] Step 1, Mixing: Weigh sodium alginate and zirconia. Add sodium alginate and zirconia into beakers respectively, add water, and prepare a 2% sodium alginate solution and a 2% zirconia suspension with a mass fraction respectively. Place the sodium alginate solution and the zirconia suspension in a magnetic stirrer and stir at a high speed for 2 hours to ensure the uniformity of the mixture.

[0102] Step 2, Spinning of fibers: Pour the sodium alginate solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for defoaming for 12 hours to remove the bubbles in the sodium alginate solution and ensure the uniformity and stability of the sodium alginate solution. Pour the defoamed sodium alginate solution into the feed inlet of a wet spinning machine, turn on the wet spinning machine, extrude the sodium alginate solution, stretch the extruded fibers, the extrusion speed is 1 mL / min, the pore diameter of the spinneret is 1 mm, the rotation speed of the drafting device is 20 rpm, and immerse it in the zirconia suspension prepared in Step 1, and then immerse it in a 3% calcium chloride aqueous solution to form fibers. Wind the fibers onto a drafting device with a rotation speed of 20 rpm / min and collect them using a tube to achieve continuous spinning of the fibers.

[0103] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in a 3% calcium chloride aqueous solution for 30 minutes, take it out and let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0104] Example 8

[0105] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0106] Step 1, Mixing: Weigh sodium alginate and zirconia. Add sodium alginate and zirconia into beakers respectively, add water, and prepare a 2% sodium alginate solution and a 2% zirconia suspension with a mass fraction respectively. Place the sodium alginate solution and the zirconia suspension in a magnetic stirrer and stir at a high speed for 2 hours to ensure the uniformity of the mixture.

[0107] Step 2: Spinning of fibers: Pour the sodium alginate solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for 12 hours to remove the air bubbles in the sodium alginate solution, ensuring the uniformity and stability of the sodium alginate solution; pour the degassed sodium alginate solution into the feed inlet of a wet spinning machine, turn on the wet spinning machine, extrude the sodium alginate solution, stretch the extruded fibers, with an extrusion speed of 1 mL / min, a spinneret aperture of 1 mm, and a draw unit rotation speed of 20 rpm, and immerse them in the zirconia suspension prepared in Step 1, and add an ultrasonic vibration device to the zirconia suspension, with an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, then immerse them in a 3% (by mass) calcium chloride aqueous solution to form fibers, wind the fibers onto a draw unit with a rotation speed of 20 rpm / min, and collect them using a tube to achieve continuous spinning of the fibers;

[0108] Step 3: Post-treatment: Immerse the fiber tube obtained by spinning in Step 2 in a 3% (by mass) calcium chloride aqueous solution for 30 minutes, take it out and let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0109] Example 9

[0110] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0111] Step 1: Mixing: Weigh sodium alginate and zirconia, add sodium alginate and zirconia into beakers respectively, add water, and prepare a 2% (by mass) sodium alginate solution and a 2% (by mass) zirconia suspension respectively. Place the sodium alginate solution and the zirconia suspension on a magnetic stirrer and stir at a high speed for 2 hours to ensure the uniformity of the mixture;

[0112] Step 2: Spinning of fibers: Pour the sodium alginate solution prepared in Step 1 into a spinning cup, place it in a vacuum oven for 12 hours to remove the air bubbles in the sodium alginate solution, ensuring the uniformity and stability of the sodium alginate solution; pour the degassed sodium alginate solution into the feed inlet of a wet spinning machine, turn on the wet spinning machine, extrude the sodium alginate solution, stretch the extruded fibers, with an extrusion speed of 1 mL / min, a spinneret aperture of 1 mm, and a draw unit rotation speed of 20 rpm, and immerse them in the zirconia suspension prepared in Step 1, and add an ultrasonic vibration device to the zirconia suspension, with an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, and add a heating device to control the temperature of the inorganic powder suspension at 40 °C, then immerse them in a 3% (by mass) calcium chloride aqueous solution to form fibers, wind the fibers onto a draw unit with a rotation speed of 20 rpm / min, and collect them using a tube to achieve continuous spinning of the fibers;

[0113] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in an aqueous calcium chloride solution with a mass fraction of 3% for 30 minutes. After taking it out, let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0114] Example 10

[0115] An inorganic particle-embedded spinning method for improving the properties of organic fibers is as follows:

[0116] Step 1, Mixing: Weigh sodium alginate and zirconia. Add sodium alginate and zirconia into beakers respectively, add water, and prepare a sodium alginate solution with a mass fraction of 2% and a zirconia suspension with a mass fraction of 2% respectively. Place the sodium alginate solution and the zirconia suspension in a magnetic stirrer and stir at high speed for 2 hours to ensure the uniformity of the mixture;

[0117] Step 2, Spinning of fibers: Pour the sodium alginate solution prepared in Step 1 into a spinning cup, put it into a vacuum oven for degassing for 12 hours to remove the bubbles in the sodium alginate solution and ensure the uniformity and stability of the sodium alginate solution; Pour the degassed sodium alginate solution into the feed port of a wet spinning machine, turn on the wet spinning machine, extrude the sodium alginate solution, stretch the extruded fibers, the extrusion speed is 1 mL / min, the pore diameter of the spinneret is 1 mm, the rotation speed of the drafting device is 20 rpm, and immerse it in the zirconia suspension prepared in Step 1. Add an ultrasonic vibration device to the zirconia suspension, the ultrasonic power is 300 W, the ultrasonic frequency is 40 kHz, and add a heating device to control the temperature of the inorganic powder suspension at 40°C. Further add a magnetic stirring device to control the speed of the magnetic stirring device at 200 rpm, and then immerse it in an aqueous calcium chloride solution with a mass fraction of 3% to form fibers. Wind the fibers onto a tube with a rotation speed of 20 rpm / min for collection to achieve continuous spinning of fibers;

[0118] Step 3, Post-treatment: Immerse the fiber tube spun in Step 2 in an aqueous calcium chloride solution with a mass fraction of 3% for 30 minutes. After taking it out, let it stand at room temperature for 24 hours to obtain dry composite filaments.

[0119] Test Example 1

[0120] Diameter and linear density test

[0121] Conduct diameter and linear density tests on the composite filaments prepared by the present invention respectively. The specific test data are shown in Table 1.

[0122] Table 1

[0123]

[0124]

[0125] Test Example 2

[0126] Mechanical property test

[0127] The alginate fibers prepared in Examples 3-4 were subjected to mechanical property tests using an Instron 5967 universal testing machine. The tensile speed was 250 mm / min, the gauge length was 5 mm, and each group of samples was tested five times and the average value was taken. The test results are shown in Table 2.

[0128] Table 2

[0129] Experimental scheme Breaking strength (MPa) Elongation at break (%) Example 1 152.97 9.81 Example 2 198.07 25.43 Example 3 148.89 6.32 Example 4 138.56 4.1 Example 5 188.75 4.98 Example 6 194.41 5.45 Example 7 302.94 6.34 Example 8 312.96 6.73 Example 9 328.38 6.77 Example 10 332.65 6.84

[0130] In the present invention, the test results show that with the increase of the alginate concentration (such as in Examples 1 and 2), the mechanical properties of the fibers are significantly improved, which is mainly attributed to the enhanced orientation of polymer chains, the optimization of the internal structure of the fibers, and the increase of the fiber diameter. However, when zirconia powder is doped in the spinning solution (such as in Examples 3 and 4), the breaking strength and elongation at break of the fibers decrease, which is because the embedding of inorganic powder interferes with the orientation of polymer chains, resulting in the influence on the continuity and mechanical properties of the fibers. Further, when an ultrasonic device is introduced during the spinning process (such as in Examples 5 and 6), although the zirconia powder can be more uniformly dispersed in the fibers, the strength of the fibers does not increase significantly, indicating that the mechanical properties of the fibers cannot be fully restored only by ultrasonic treatment. When the fibers enter the zirconia suspension after spinning (such as in Example 7), the fiber strength increases, indicating that through surface treatment, the inorganic powder mainly forms a reinforcing layer on the fiber surface, thereby improving the mechanical properties of the fibers. Finally, when an ultrasonic device and a heating device are simultaneously added to the zirconia suspension (such as in Example 9), the mechanical properties of the fibers are further significantly improved. This is because the high-frequency vibration and cavitation effect of ultrasonic waves can further optimize the dispersion of inorganic powder on the fiber surface, while the heating device reduces the viscosity of the suspension and enhances the fluidity of the inorganic powder, enabling the inorganic particles to be more uniformly embedded on the fiber surface to form a more stable reinforcing layer without affecting the enhancement of polymer chain orientation and the internal structure of the fibers. This synergistic effect not only improves the acid and alkali resistance of the fibers but also significantly improves the mechanical properties of the fibers, achieving a comprehensive improvement of the fiber properties.

[0131] Test Example 3

[0132] Solubility test

[0133] Alkali solubility test method: Cut a small section of the composite filament in Example 2, weigh it to be 0.0071 g, put it into a 1 mol / L sodium hydroxide solution, take it out and dry it after 1 h, weigh it to be 0.0045 g, and calculate the solubility. Cut the composite filament in Example 4 to the same length as in the above step, weigh it to be 0.0197 g, put it into a 1 mol / L sodium hydroxide solution, take it out and dry it after 1 h, weigh it to be 0.0175 g, and calculate the solubility.

[0134] Acid solubility test method: Acid-treat the composite filaments in Example 2 and Example 4 with 1 mol / L hydrochloric acid. Calculate the solubility respectively.

[0135] The solubility test results are shown in Table 3.

[0136] Take a physical picture of the surface of the composite filaments in Examples 1 to 4, as Figure 4 shown; Take physical pictures of the fibers of the composite filaments in Example 2 and Example 4 before and after alkali treatment, as Figure 5 shown.

[0137] Table 3

[0138]

[0139]

[0140] The above results indicate that, compared with Example 2, Example 4 shows less fiber dissolution, indicating that the addition of zirconia powder has improved the alkali resistance of the fiber to a certain extent. The change in solubility indicates that the structure of the fiber has become more complex. Although the addition of zirconia has improved the acid and alkali resistance of the fiber, further, when an ultrasonic device is introduced during the spinning process (such as in Examples 5 and 6), the solubility of the fiber continues to increase, which indicates that ultrasonic treatment can not only evenly disperse the zirconia powder in the fiber, but also further enhance the acid and alkali resistance of the fiber by changing the microstructure of the fiber. The high-frequency vibration and cavitation effect of ultrasonic waves can destroy the microporous structure inside the fiber, making the fiber surface more dense, thereby improving the stability of the fiber in an acid-base environment. When the fiber enters the zirconia suspension after spinning (such as in Example 7), the solubility of the fiber further increases, indicating that through surface treatment, inorganic powder can form a reinforcing layer on the fiber surface, thereby improving the acid and alkali resistance of the fiber. Finally, when an ultrasonic device and a heating device are simultaneously added to the zirconia suspension (such as in Example 9), the solubility of the fiber increases significantly, indicating that the synergistic effect of ultrasonic and heating can further optimize the structure of the fiber. The high-frequency vibration and cavitation effect of ultrasonic waves can further optimize the dispersion of inorganic powder on the fiber surface, while the heating device reduces the viscosity of the suspension and enhances the fluidity of the inorganic powder, enabling inorganic particles to be more evenly embedded on the fiber surface to form a more stable reinforcing layer. This synergistic effect not only improves the acid and alkali resistance of the fiber, but also significantly improves the microstructure of the fiber, further enhancing its stability in an acid-base environment.

[0141] In Example 10 of the present invention, the introduction of a magnetic stirring device further optimizes the performance of the fiber. Through continuous stirring, magnetic stirring ensures the uniform dispersion of inorganic powder in the zirconia suspension, avoids local agglomeration, and at the same time reduces the viscosity of the suspension, enhances the fluidity of inorganic particles, and enables them to be more evenly embedded on the fiber surface to form a stable reinforcing layer. This process, together with the cavitation effect of ultrasonic waves and the synergistic effect of the heating device, further optimizes the microstructure of the fiber, makes the fiber surface more dense, significantly improves the mechanical properties and acid and alkali resistance of the fiber, and realizes the comprehensive improvement of the fiber performance.

[0142] As Figure 5 shown, after alkali treatment, the fiber in Example 2 changed from transparent to yellow, while after alkali treatment in Example 4 with the addition of zirconia powder, its color was not affected.

[0143] From Figure 5 it can be confirmed Figure 4 the color change of the 2% sodium alginate raw filament in

[0144] Comprehensively Figure 4 andFigure 5 The results show that alkali treatment has a negative effect on the morphological structures of both fibers, but the addition of zirconia powder reduces this impact. Thus, it can be proven that zirconia can improve the alkali resistance of sodium alginate fibers.

[0145] The pictures taken show that the color of the 2% sodium alginate raw filaments has changed, but the color of the 2% sodium alginate composite filaments before and after acid treatment has not changed, nor has it affected the particles on the fiber surface. Thus, it can be proven that zirconia can improve the acid resistance of sodium alginate fibers.

[0146] Test Example 4

[0147] Dyeing experiment

[0148] The composite filaments prepared in Examples 2 and 4 and the composite filaments after acid and alkali treatment were subjected to a dyeing experiment.

[0149] The composite filaments were placed in a 1 g / L methylene blue solution and shaken in a water bath at a bath ratio of 1:200 and a temperature of 60 °C for 6 h, and the dyeing degree of the samples was observed.

[0150] Take a physical picture of the dyed sample, as Figure 7 shown.

[0151] As Figure 7 shown, the undyed alkali-treated composite filaments of Example 2, the alkali-treated composite filaments of Example 2, and the alkali-treated composite filaments of Example 4 are all dyed evenly.

[0152] To further observe the dyeing situation of the samples, the surface morphology of the dyed samples was further analyzed using a 3D optical microscope, as Figure 8 shown.

[0153] As Figure 8 shown, the fiber surface is evenly dyed with methylene blue dye, indicating that the dyeing performance of the two fibers after alkali treatment is not significantly affected.

[0154] In the present invention, through experimental tests, it is found that whether it is sodium alginate fibers without doped inorganic powder or composite fibers doped with zirconia, their dyeing performance is not significantly affected. Even after acid and alkali treatment, the dyeing uniformity of the fibers remains good. This shows that the modification method of the present invention not only improves the acid and alkali resistance of the fibers but also successfully retains the dyeing performance of the fibers, ensuring that on the basis of functional improvement, it can still meet the diverse needs in practical applications.

[0155] The above results show that doping zirconia powder in sodium alginate fibers not only does not affect their dyeing performance but also maintains their dyeing performance in an acid and alkali environment.

[0156] Sodium alginate fiber has certain flame retardant properties. In order to explore whether the addition of zirconia will affect its flame retardant properties, thermogravimetric analysis was carried out on the composite filaments of Example 2 and the composite filaments of Example 4.

[0157] The thermogravimetric analysis image shows that the zirconia powder did not show mass loss at 800 °C. The composite filaments of Example 2 and the composite filaments of Example 4 mainly had five stages of mass loss. However, at 800 °C, the mass loss of the composite filaments of Example 4 was only 34.8%, and the residue remaining amount was 65.2%. The results show that the sodium alginate fiber added with zirconia still has good thermal properties.

[0158] Combined with the results of all experiments and characterization tests, the addition of zirconia can not only improve the acid and alkali resistance and dyeing properties of sodium alginate fiber in an acid and alkali environment, but also will not affect the crystallinity and original properties of sodium alginate, and it is a very good modifier. Regarding the dosage of zirconia, after multiple characterization tests of mixing ratios in the present invention, it was found that 2% by mass fraction of zirconia is the most suitable ratio.

Claims

1. An inorganic particle embedded spinning method for improving the performance of organic fibers, characterized in that: Here’s how: Step 1, mixing: weighing an organic fiber raw material and an inorganic powder, adding the organic fiber raw material and the inorganic powder into a beaker, adding water to prepare a mixed solution, placing the mixed solution in a magnetic stirrer, stirring at a high speed for 1 to 3 hours to ensure that the mixed solution is uniform, and obtaining a spinning solution; Step 2, spinning of fibers: pouring the spinning solution prepared in step 1 into a spinning cup, placing it in a vacuum oven for degassing for 1 to 20 hours to remove bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; pouring the degassed spinning solution into the feed port of a wet spinning machine, opening the wet spinning machine, extruding the spinning solution, stretching the extruded fibers, and immersing them in a coagulation bath to form fibers, winding the fibers onto a drafting device with a rotation speed of 5 to 30 rpm / min, and collecting them with a tube to achieve continuous spinning of the fibers; Step 3, post-treatment: soak the fiber tube obtained by spinning in step 2 in a coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain a dry composite yarn.

2. The inorganic particle embedded spinning method for improving the performance of organic fibers according to claim 1, characterized in that: Here’s how: Step 1, mixing: weighing an organic fiber raw material and an inorganic powder, adding the organic fiber raw material and the inorganic powder into a beaker, adding water to prepare a mixed solution, placing the mixed solution in a magnetic stirrer, stirring at a high speed for 1 to 3 hours to ensure that the mixed solution is uniform, and obtaining a spinning solution; Step 2, spinning of fibers: pour the spinning solution prepared in step 1 into a spinning cup, and place it in a vacuum oven for degassing for 1 to 20 hours to remove bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; pour the degassed spinning solution into the feed port of a wet spinning machine, and in order to prevent the precipitation of inorganic powder, add an ultrasonic vibration device to the spinning solution to improve the uniformity of the mixed solution, the ultrasonic power is 200 to 400 W, and the ultrasonic frequency is 20 to 60 kHz, open the wet spinning machine, extrude the spinning solution, stretch the extruded fiber, and immerse it in a coagulation bath to form a fiber, and wind the fiber onto a drafting device with a rotation speed of 5 to 30 rpm / min, and collect it using a tube to achieve continuous spinning of the fiber; Step 3, post-treatment: soak the fiber tube obtained by spinning in step 2 in a coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain a dry composite yarn.

3. The inorganic particle embedded spinning method for improving the performance of organic fibers according to claim 1, characterized in that: Here’s how: Step 1, mixing: weighing an organic fiber raw material and an inorganic powder, adding the organic fiber raw material and the inorganic powder into a beaker, adding water to prepare a mixed solution, placing the mixed solution in a magnetic stirrer, stirring at a high speed for 1 to 3 hours to ensure that the mixed solution is uniform, and obtaining a spinning solution; Step 2, spinning of fibers: pour the spinning solution prepared in step 1 into a spinning cup, and place it in a vacuum oven for degassing for 1 to 20 hours to remove bubbles in the spinning solution and ensure the uniformity and stability of the spinning solution; pour the degassed spinning solution into the feed port of a wet spinning machine, open the wet spinning machine, and extrude the spinning solution. To prevent the precipitation of inorganic powder, an ultrasonic vibration device is added to the spinneret to improve the uniformity of the mixed solution. The ultrasonic power is 200 to 400 W and the ultrasonic frequency is 20 to 60 kHz. The extruded fiber is stretched and immersed in a coagulation bath to form a fiber. The fiber is wound onto a drawing device with a rotation speed of 5 to 30 rpm / min, and collected by a tube to achieve continuous spinning of the fiber; Step 3, post-treatment: soak the fiber tube obtained by spinning in step 2 in a coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain a dry composite yarn.

4. The inorganic particle embedded spinning method for improving the performance of organic fibers according to claim 1, characterized in that: Here’s how: Step 1, mixing: weighing an organic fiber raw material and an inorganic powder, adding the organic fiber raw material and the inorganic powder into a beaker respectively, adding water to prepare an organic fiber solution and an inorganic powder turbid solution respectively, placing the organic fiber solution and the inorganic powder turbid solution in a magnetic stirrer respectively, stirring at high speed for 1 to 3 hours to ensure that the mixed solution is uniform; Step 2, spinning of fibers: pouring the organic fiber solution prepared in step 1 into a spinning cup, placing it in a vacuum oven for degassing for 1 to 20 hours to remove bubbles in the organic fiber solution, and ensuring the uniformity and stability of the organic fiber solution; pouring the degassed organic fiber solution into the feed port of a wet spinning machine, opening the wet spinning machine, extruding the organic fiber solution, stretching the extruded fibers, and immersing them in the inorganic powder turbid solution prepared in step 1, and then immersing them in a coagulation bath to form fibers, winding the fibers onto a drafting device with a rotation speed of 5 to 30 rpm / min, and collecting them with a tube to achieve continuous spinning of the fibers; Step 3, post-treatment: soak the fiber tube obtained by spinning in step 2 in a coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain a dry composite yarn.

5. The inorganic particle embedded spinning method for improving the performance of organic fibers according to claim 1, characterized in that: Here’s how: Step 1, mixing: weighing an organic fiber raw material and an inorganic powder, adding the organic fiber raw material and the inorganic powder into a beaker respectively, adding water to prepare an organic fiber solution and an inorganic powder turbid solution respectively, placing the organic fiber solution and the inorganic powder turbid solution in a magnetic stirrer respectively, stirring at high speed for 1 to 3 hours to ensure that the mixed solution is uniform; Step 2, spinning of fibers: pouring the organic fiber solution prepared in step 1 into a spinning cup, placing it in a vacuum oven for degassing for 1 to 20 hours to remove bubbles in the organic fiber solution, and ensuring the uniformity and stability of the organic fiber solution; pouring the degassed organic fiber solution into the feed port of a wet spinning machine, opening the wet spinning machine, extruding the organic fiber solution, stretching the extruded fibers, and immersing them in the inorganic powder turbid solution prepared in step 1, and adding an ultrasonic vibration device to the inorganic powder turbid solution, with an ultrasonic power of 200 to 400 W and an ultrasonic frequency of 20 to 60 kHz, and then immersing them in a coagulation bath to form fibers, winding the fibers onto a drawing device with a rotation speed of 5 to 30 rpm / min, and collecting them with a tube to achieve continuous spinning of the fibers; Step 3, post-treatment: soak the fiber tube obtained by spinning in step 2 in a coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain a dry composite yarn.

6. The inorganic particle embedded spinning method for improving the performance of organic fibers according to claim 1, characterized in that: Here’s how: Step 1, mixing: weighing an organic fiber raw material and an inorganic powder, adding the organic fiber raw material and the inorganic powder into a beaker respectively, adding water to prepare an organic fiber solution and an inorganic powder turbid solution respectively, placing the organic fiber solution and the inorganic powder turbid solution in a magnetic stirrer respectively, stirring at high speed for 1 to 3 hours to ensure that the mixed solution is uniform; Step 2, spinning of fibers: pouring the organic fiber solution prepared in step 1 into a spinning cup, placing it in a vacuum oven for degassing for 1 to 20 hours to remove bubbles in the organic fiber solution, and ensuring the uniformity and stability of the organic fiber solution; pouring the degassed organic fiber solution into the feed port of a wet spinning machine, opening the wet spinning machine, extruding the organic fiber solution, stretching the extruded fibers, and immersing them in the inorganic powder turbid solution prepared in step 1, and adding an ultrasonic vibration device to the inorganic powder turbid solution, with an ultrasonic power of 200 to 400 W and an ultrasonic frequency of 20 to 60 kHz, and adding a heating device to control the temperature of the inorganic powder turbid solution to 30 to 60° C., and then immersing it in a coagulation bath to form fibers, winding the fibers onto a drawing device with a rotation speed of 5 to 30 rpm / min, and collecting them with a tube to achieve continuous spinning of the fibers; Step 3, post-treatment: soak the fiber tube obtained by spinning in step 2 in a coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain a dry composite yarn.

7. The inorganic particle embedded spinning method for improving the performance of organic fibers according to claim 1, characterized in that: Here’s how: Step 1, mixing: weighing an organic fiber raw material and an inorganic powder, adding the organic fiber raw material and the inorganic powder into a beaker respectively, adding water to prepare an organic fiber solution and an inorganic powder turbid solution respectively, placing the organic fiber solution and the inorganic powder turbid solution in a magnetic stirrer respectively, stirring at high speed for 1 to 3 hours to ensure that the mixed solution is uniform; Step 2, spinning of fibers: pouring the organic fiber solution prepared in step 1 into a spinning cup, placing it in a vacuum oven for degassing for 1 to 20 hours to remove bubbles in the organic fiber solution and ensure the uniformity and stability of the organic fiber solution; pouring the degassed organic fiber solution into the feed port of a wet spinning machine, opening the wet spinning machine, extruding the organic fiber solution, stretching the extruded fibers, and immersing them in the inorganic powder turbid solution prepared in step 1, and adding an ultrasonic vibration device to the inorganic powder turbid solution, with an ultrasonic power of 200 to 400 W and an ultrasonic frequency of 20 to 60 kHz, and adding a heating device to control the temperature of the inorganic powder turbid solution to 30 to 60° C., further adding a magnetic stirring device, controlling the speed of the magnetic stirring device to 100 to 500 rpm, and then immersing it in a coagulation bath to form fibers, winding the fibers onto a drawing device with a rotation speed of 5 to 30 rpm / min, and collecting them with a tube to achieve continuous spinning of the fibers; Step 3, post-treatment: soak the fiber tube obtained by spinning in step 2 in a coagulation bath for 10 to 50 minutes, take it out and let it stand at room temperature for 5 to 48 hours to obtain a dry composite yarn.

8. The inorganic particle embedded spinning method for improving the performance of organic fibers according to any one of claims 1 to 7, characterized in that: The mass fraction of the organic fiber raw material in the mixed solution is 0-2wt%, and the mass fraction of the inorganic powder is 0-2wt%; The organic fiber raw material is at least one of sodium alginate, chitosan, wood, and cellulose; The inorganic powder is at least one of zirconium oxide, silicon dioxide, aluminum oxide, titanium dioxide, calcium carbonate, magnesium oxide, zinc oxide, talc and kaolin.

9. The inorganic particle embedded spinning method for improving the performance of organic fibers according to any one of claims 1 to 7, characterized in that: The wet spinning machine had an injection pump extrusion speed of 1 mL / min, a spinneret aperture of 1 mm, and a drafting device rotation speed of 20 rpm.

10. The inorganic particle embedded spinning method for improving the performance of organic fibers according to any one of claims 1 to 7, characterized in that: The coagulation bath is at least one of a calcium chloride aqueous solution, an ethylene glycol aqueous solution, an N,N-dimethylformamide aqueous solution, an isopropanol aqueous solution, a dimethyl sulfoxide aqueous solution, methanol, and water.

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