A multifunctional diatomaceous earth fiber and its preparation method

Abstract

This invention provides a multifunctional diatomaceous earth fiber and its preparation method. The multifunctional diatomaceous earth fiber uses irregularly shaped polyester-based multifunctional diatomaceous earth fiber filaments as the core and modified ultrafine multifunctional diatomaceous earth fiber filaments as the covering filaments. The core filaments are lightweight, high-strength, and warm. Combined with the synergistic effect of moisture-wicking finishing agents and diatomaceous earth, the moisture absorption and quick-drying properties of the multifunctional diatomaceous earth fiber are effectively improved. The modified ultrafine multifunctional diatomaceous earth fiber filaments exhibit good structural stability and high adsorption capacity. Using the preparation method of this invention, the resulting fiber filaments possess high quality, good antibacterial adsorption properties, and excellent overall performance.

Description

Technical Field

[0001] This invention relates to the field of composite material preparation technology, specifically to a multifunctional diatomaceous earth fiber and its preparation method. Background Technology

[0002] Diatomaceous earth is a siliceous rock, a biogenic siliceous sedimentary rock mainly composed of the remains of ancient diatoms. Its main component is silicate, and its surface has countless micropores that can absorb and decompose odors in the air, providing humidity control and deodorization. Diatomaceous earth possesses characteristics such as ultra-fiber and porousness; its ultra-micropores are 5000 to 6000 times more numerous than those of charcoal, giving it strong adsorption properties. It can automatically regulate indoor humidity; when indoor humidity rises, the ultra-micropores on diatomaceous earth automatically absorb and store moisture from the air. If the indoor air moisture decreases and humidity drops, the diatomaceous earth releases the stored moisture from its micropores. Furthermore, diatomaceous earth wall materials also eliminate odors, acting as a deodorizer and maintaining indoor cleanliness. The absorption and release of moisture by diatomaceous earth wall materials creates a waterfall effect, decomposing water molecules into positive and negative ions. Positive and negative ion clusters float in the air and have bactericidal properties. Given the advantages and benefits of diatomaceous earth, its application in home textile products will have broader value. However, how to prepare more multifunctional diatomaceous earth fibers suitable for home textile products is a question we need to research.

[0003] Patent CN107326466A discloses a method for preparing multifunctional diatomaceous earth fibers. The method involves physically and mechanically pulverizing diatomaceous earth to a fineness of 400-800 mesh (18-38 μm), followed by surface chemical modification. The modified diatomaceous earth powder is then added to the melt spinning process to produce multifunctional diatomaceous earth fibers. However, 400-800 mesh powder is still relatively fine (18-38 μm) for melt spinning solutions; generally, fiber dyes can achieve a fineness of 15-25 μm. Therefore, it tends to agglomerate during melt spinning, easily causing uneven fiber fineness, resulting in uneven fiber strength and making spinning difficult. Furthermore, with the continuous development of the textile industry and the continuous improvement of people's living standards, people have a more urgent desire and higher requirements for comfortable and functional home textile products. Existing conventional multifunctional diatomaceous earth fibers cannot yet meet the further requirements in terms of moisture absorption and perspiration wicking.

[0004] To this end, we have developed a multifunctional diatomaceous earth fiber that is lightweight and high-strength, has good antibacterial and adsorption properties, and excellent moisture absorption and perspiration wicking performance. Summary of the Invention

[0005] This invention addresses the problems of existing multifunctional diatomaceous earth fibers, such as easy aggregation and spinning difficulties during melt spinning, as well as the inability to simultaneously achieve antibacterial, adsorption, and moisture-wicking properties. It proposes a multifunctional diatomaceous earth fiber and its preparation method, which features high-quality finished fiber filaments, good antibacterial and adsorption properties, and excellent comprehensive performance.

[0006] To achieve the above objectives, the present invention proposes the following technical solution: a multifunctional diatomaceous earth fiber, comprising a core and a fixed number of covering filaments, wherein the core comprises a number of polyester-based fiber filaments arranged in parallel;

[0007] The coated filament is a modified ultrafine multifunctional diatomaceous earth fiber, and several of the modified ultrafine multifunctional diatomaceous earth fibers are spirally wound around the outer surface of the filament core.

[0008] Based on the above scheme and as a preferred embodiment of the above scheme, the polyester-based fiber filament is a polyester-based multifunctional diatomaceous earth fiber filament, and the polyester-based multifunctional diatomaceous earth fiber filament is arranged in parallel in three strands; the modified ultrafine multifunctional diatomaceous earth fiber filament is arranged in parallel in four strands.

[0009] Based on the above scheme and as a preferred embodiment of the above scheme, the method for preparing a multifunctional diatomaceous earth fiber includes the following steps:

[0010] 1) Preparation of ultrafine diatomaceous earth

[0011] Diatomaceous earth calcined at 800℃ was selected for fine treatment and ball milling was performed using wet ball milling with deionized water as the dispersion medium and 10% of the diatomaceous earth mass as a mixed dispersant. The ball milling ratio was 7:1. The resulting mixed solution was precipitated for 6 hours, the supernatant was taken, and then precipitated for another 12 hours. The precipitate was then taken, dried, and ground to obtain ultrafine diatomaceous earth.

[0012] 2) Preparation of polyester-based fiber filaments

[0013] Weigh the ultrafine diatomite described in step 1), and blend and melt it with polyester at a mass ratio of 5-30:100 to obtain a spinning solution. The spinning solution is extruded through a screw extruder and then enters a spinneret. The resulting fiber is then subjected to “stretching → washing → spraying with polyether moisture-wicking finishing agent → six-stage baking” to obtain polyester-based multifunctional diatomite fiber filament.

[0014] 3) Preparation of modified ultrafine multifunctional diatomaceous earth fibers

[0015] Place the ultrafine diatomaceous earth from step 1) in deionized water, and add a 20%-50% polyacrylamide solution. Stir the mixture evenly in a water bath at 40℃-70℃. Then, add an appropriate amount of ammonia water dropwise at a rate of 0.5mL / min and continue stirring evenly for 1-5 hours. After soaking for 10-24 hours, dry the precipitate to obtain modified ultrafine diatomaceous earth, and grind it for later use.

[0016] Modified ultrafine diatomaceous earth and polyether moisture-wicking finishing agent are added to polyvinyl alcohol solution and magnetically stirred until uniform. After ultrasonic treatment for 20-50 minutes, the suspension is taken and wet-spun to obtain modified ultrafine multifunctional diatomaceous earth fiber.

[0017] 4) Preparation of composite multifunctional diatomaceous earth fibers

[0018] Polyester-based fiber filaments and multifunctional diatomaceous earth fiber filaments are simultaneously fed into a filament cutter, a first roller, a pre-network, an anti-twist device, a deformation heat box, a cooling plate, a false twister, a second roller, a main networker, a shaping heat box oil wheel, and then wound to obtain the multifunctional diatomaceous earth fiber of the present invention.

[0019] The draw ratio of the second roller to the first roller is 1.015-1.7325, and the winding speed is -3.9% of the winding ratio of the second roller.

[0020] Based on the above scheme and as a preferred scheme, the calcination time of the diatomaceous earth in step 1) is 25-120 min.

[0021] Based on the above scheme and as a preferred embodiment of the above scheme, the mixing dispersant in step 1) is a mixture of acrylate, maleic isool diester and polyvinylpyrrolidone in a mass ratio of 2:1:2.

[0022] Based on the above scheme and as a preferred embodiment of the above scheme, the molecular weight of the polyvinylpyrrolidone in step 1) is 130000 g / mol.

[0023] Based on the above scheme and as a preferred embodiment of the above scheme, the particle size of the ultrafine diatomite in step 1) is 500nm-900nm.

[0024] Based on the above scheme and as a preferred embodiment of the above scheme, the cross-section of the spinneret micro-hole in step 2) is one of a hollow circle, a hollow trilobal shape, or a hollow cross shape.

[0025] Based on the above scheme and as a preferred embodiment of the above scheme, in step 3), the mass fraction concentration of the ultrafine diatomaceous earth is the same as the concentration of polyacrylamide; the concentration of the ammonia solution is 0.5-10M; and the drying temperature of the precipitate is the same as the water bath temperature.

[0026] Based on the above scheme and as a preferred embodiment of the above scheme, the wet spinning step in step 3) is as follows:

[0027] A 15% (w / w) aqueous solution of polyvinyl alcohol was prepared, ultrasonically treated for 20 min, and then magnetically stirred and heated at 85℃-120℃ for 2 h. Modified ultrafine diatomaceous earth and a polyether-based moisture-wicking finishing agent were added to the prepared polyvinyl alcohol solution at a mass ratio of 4:1. The solution was magnetically stirred for 1 h, ultrasonically treated for 30 min, and then allowed to cool to room temperature before emulsion spinning. The wet spinning process parameters were as follows:

[0028] Spinning solution: concentration 16%;

[0029] Metering pump: 0.8 mL / r;

[0030] Rotational speed: 38 r / min;

[0031] Pump flow rate: 30 mL / min;

[0032] Spinneret has 1000 holes; hole diameter: 0.08 mm.

[0033] The coagulation bath length is 1.2m, the coagulation time is 15 seconds, and the fiber generation speed in the coagulation bath is 6m / min.

[0034] Guide wire disc diameter: 80mm;

[0035] Roller speed: 18 r / min; Roller speed: 25 r / min;

[0036] Moist heat stretching temperature: 120-150℃.

[0037] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0038] This invention discloses a multifunctional diatomaceous earth fiber and its preparation method. The multifunctional diatomaceous earth fiber uses irregularly shaped polyester-based multifunctional diatomaceous earth fiber filaments as the core and modified ultrafine multifunctional diatomaceous earth fiber filaments as the covering filaments. The core filaments are lightweight, high-strength, and warm. Combined with the synergistic effect of moisture-wicking finishing agents and diatomaceous earth, the moisture absorption and quick-drying properties of the multifunctional diatomaceous earth fiber are effectively improved. The modified ultrafine multifunctional diatomaceous earth fiber filaments exhibit good structural stability and high adsorption capacity. Using the preparation method of this invention, the resulting fiber filaments possess high quality, good antibacterial adsorption properties, and excellent overall performance.

[0039] It should be understood that all combinations of the foregoing concepts and the additional concepts described in more detail below can be considered part of the subject matter disclosure of the present invention, provided that such concepts do not contradict each other.

[0040] The foregoing and other aspects, embodiments, and features of the teachings of this invention will be more fully understood from the following description. Other additional aspects of the invention, such as features and / or beneficial effects of exemplary embodiments, will become apparent from the following description or may be learned through practice of specific embodiments according to the teachings of this invention. Attached Figure Description

[0041] The above and / or additional aspects and advantages of the present invention will become apparent and readily understood from the description of the embodiments taken in conjunction with the following drawings, in which:

[0042] Figure 1 This is a schematic diagram of the multifunctional diatomaceous earth fiber structure of the present invention;

[0043] Figure 2 Example 1 is the specific surface area test and analysis of ultrafine diatomaceous earth.

[0044] In the diagram, 1 represents polyester-based fiber filaments; 2 represents coated filaments. Detailed Implementation

[0045] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the described embodiments of the present invention without creative effort are within the scope of protection of the present invention. Unless otherwise defined, the technical or scientific terms used herein should have the ordinary meaning understood by those skilled in the art to which this invention pertains.

[0046] The terms "first," "second," and similar words used in the specification and claims of this patent application do not indicate any order, quantity, or importance, but are merely used to distinguish different components. Similarly, unless the context clearly indicates otherwise, the singular forms of "an," "a," or "the," etc., do not indicate a quantity limitation, but rather indicate the presence of at least one. Terms such as "comprising" or "including" mean that the element or object preceding "comprising" encompasses the features, integrals, steps, operations, elements, and / or components listed following "comprising" or "including," and do not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components, and / or collections thereof. Terms such as "upper," "lower," "left," and "right" are used only to indicate relative positional relationships; these relative positional relationships may change accordingly when the absolute position of the described object changes.

[0047] Diatomaceous earth's main component is silicon dioxide, which possesses strong adsorption properties and exhibits negative charge due to the presence of numerous silanol groups on its surface, allowing it to effectively adsorb metals and organic polymers. The varying composition and content of diatomaceous earth result in different appearances and microstructures, with porosities reaching 80%-90%, thus contributing to its good water absorption. Given its advantages, the application of diatomaceous earth in home textile products is a growing trend. However, the current application of multifunctional diatomaceous earth fibers is limited by issues such as uneven fiber strength and easy agglomeration during spinning. Therefore, further research on multifunctional diatomaceous earth fibers is necessary.

[0048] Example 1

[0049] A multifunctional diatomaceous earth fiber includes a core and a fixed number of covering filaments. The core comprises a number of polyester-based fiber filaments arranged in parallel. The covering filaments are modified ultrafine multifunctional diatomaceous earth fiber filaments, and a number of the modified ultrafine multifunctional diatomaceous earth fiber filaments are spirally wound around the outer surface of the core.

[0050] The polyester-based fiber filament is a polyester-based multifunctional diatomaceous earth fiber filament, and three polyester-based multifunctional diatomaceous earth fiber filaments are arranged side by side; four modified ultrafine multifunctional diatomaceous earth fiber filaments are arranged side by side.

[0051] Furthermore, the preparation method of the multifunctional diatomaceous earth fiber includes the following steps:

[0052] 1) Preparation of ultrafine diatomaceous earth

[0053] Diatomaceous earth calcined at 800℃ for 60 min was selected for refining treatment. It was then ball-milled using a wet ball milling method with deionized water as the dispersion medium and a 10% (by weight) mixed dispersant (a ball-to-material ratio of 7:1). The mixed dispersant consisted of acrylate, maleic isool diester, and polyvinylpyrrolidone in a 2:1:2 (by weight) mixture, and the ball milling time was 6 h. The resulting mixed solution was allowed to precipitate for 6 h, the supernatant was collected, and then allowed to precipitate for another 12 h. The precipitate was then dried and ground to obtain ultrafine diatomaceous earth.

[0054] In this embodiment, the molecular weight of the polyvinylpyrrolidone is 130,000 g / mol.

[0055] 2) Preparation of polyester-based fiber filaments

[0056] Weigh the ultrafine diatomaceous earth described in step 1), and blend and melt it with polyester at a mass ratio of 20:100 to obtain a spinning solution. The spinning solution is extruded through a screw extruder and then enters a spinneret. The resulting fiber is then subjected to “stretching → washing → spraying with polyether moisture-wicking finishing agent → six-stage baking” to obtain polyester-based multifunctional diatomaceous earth fiber filament.

[0057] 3) Preparation of modified ultrafine multifunctional diatomaceous earth fibers

[0058] Place the ultrafine diatomaceous earth from step 1) in deionized water and add a 35% polyacrylamide solution. Stir the mixture evenly in a 55°C water bath. Then, add an appropriate amount of ammonia water dropwise at a rate of 0.5 mL / min to adjust the pH to 10. Continue stirring evenly for 3 hours, then soak for 15 hours. Dry the precipitate to obtain modified ultrafine diatomaceous earth, and grind it for later use.

[0059] The concentration of the ultrafine diatomaceous earth is the same as the concentration of polyacrylamide, and the mass ratio of ultrafine diatomaceous earth to polyacrylamide is 3:1; the concentration of the ammonia solution is 2.5M; and the drying temperature of the precipitate is the same as the water bath temperature. Then, the modified ultrafine diatomaceous earth and the moisture-wicking finishing agent are added to a 15% polyvinyl alcohol aqueous solution at a mass ratio of 4:1, and magnetically stirred until homogeneous. After ultrasonic treatment for 30 minutes, the suspension is taken for wet spinning to obtain multifunctional diatomaceous earth fibers.

[0060] Modified ultrafine diatomaceous earth and polyether moisture-wicking finishing agent were added to a polyvinyl alcohol solution and magnetically stirred until homogeneous. After ultrasonic treatment for 30 minutes, the suspension was taken and wet-spun to obtain modified ultrafine multifunctional diatomaceous earth fiber filaments. In this embodiment, the polyether moisture-wicking finishing agent was purchased from Guangzhou Qiantai Chemical Co., Ltd. as moisture-wicking finishing agent QTG-410.

[0061] 4) Preparation of composite multifunctional diatomaceous earth fibers

[0062] Polyester-based fiber filaments and multifunctional diatomaceous earth fiber filaments are simultaneously fed into a filament cutter, a first roller, a pre-network, an anti-twist device, a deformation heat box, a cooling plate, a false twister, a second roller, a main networker, a shaping heat box oil wheel, and then wound to obtain the multifunctional diatomaceous earth fiber of the present invention.

[0063] The draw ratio of the second roller to the first roller is 1.015, and the winding speed of the second roller is -3.9%.

[0064] The ultrafine diatomite in this embodiment has a particle size of 780 nm.

[0065] In step 2), the cross-section of the spinneret's micro-orifices is a hollow trilobal shape. Furthermore, in step 3), the mass fraction concentration of the ultrafine diatomaceous earth is the same as the concentration of polyacrylamide; and the drying temperature of the precipitate is the same as the water bath temperature.

[0066] Furthermore, in step 3) of this embodiment, the wet spinning step is as follows:

[0067] A 15% (w / w) aqueous solution of polyvinyl alcohol was prepared, ultrasonically treated for 20 min, and then magnetically stirred and heated at 90°C for 2 h. Modified ultrafine diatomaceous earth and polyether moisture-wicking finishing agent were added to the prepared polyvinyl alcohol solution at a mass ratio of 4:1. The solution was magnetically stirred for 1 h and ultrasonically treated for 30 min. After the suspension was cooled to room temperature, emulsion spinning was performed. The concentration of the spinning solution increased due to the addition of modified ultrafine diatomaceous earth and polyether moisture-wicking finishing agent.

[0068] The wet spinning process parameters in this embodiment are as follows:

[0069] Spinning solution: concentration 16%;

[0070] Metering pump: 0.8 mL / r;

[0071] Rotational speed: 38 r / min;

[0072] Pump flow rate: 30 mL / min;

[0073] Spinneret has 1000 holes; hole diameter: 0.08 mm.

[0074] The coagulation bath length is 1.2m, the coagulation time is 15 seconds, and the fiber generation speed in the coagulation bath is 6m / min.

[0075] Guide disc diameter: 80mm;

[0076] Roller speed: 18 r / min; Roller speed: 25 r / min;

[0077] Moist heat stretching temperature: 120-150℃.

[0078] Example 2

[0079] Unlike Example 1 above, a method for preparing the multifunctional diatomaceous earth fiber includes the following steps:

[0080] 1) Preparation of ultrafine diatomaceous earth

[0081] Diatomaceous earth calcined at 800℃ for 25 min was selected for refining treatment. It was then ball-milled using a wet ball milling method with deionized water as the dispersion medium and a 10% (by weight) mixed dispersant (a ball-to-material ratio of 7:1). The mixed dispersant consisted of acrylate, maleic isool diester, and polyvinylpyrrolidone in a 2:1:2 (by weight) mixture, and the ball milling time was 6 h. The resulting mixed solution was allowed to precipitate for 6 h, the supernatant was collected, and then allowed to precipitate for another 12 h. The precipitate was then dried and ground to obtain ultrafine diatomaceous earth.

[0082] In this embodiment, the molecular weight of the polyvinylpyrrolidone is 130,000 g / mol.

[0083] 2) Preparation of polyester-based fiber filaments

[0084] Weigh the ultrafine diatomaceous earth described in step 1), and blend and melt it with polyester at a mass ratio of 5:100 to obtain a spinning solution. The spinning solution is extruded through a screw extruder and then enters a spinneret. The resulting fiber is then subjected to “stretching → washing → spraying with polyether moisture-wicking finishing agent → six-stage baking” to obtain polyester-based multifunctional diatomaceous earth fiber filament.

[0085] 3) Preparation of modified ultrafine multifunctional diatomaceous earth fibers

[0086] Place the ultrafine diatomaceous earth from step 1) in deionized water and add a 20% polyacrylamide solution. Stir the mixture evenly in a 40°C water bath. Then, add an appropriate amount of ammonia water dropwise at a rate of 0.5 mL / min and continue stirring evenly for 1 hour. After soaking for 10 hours, dry the precipitate to obtain modified ultrafine diatomaceous earth, and grind it for later use.

[0087] The concentration of the ultrafine diatomaceous earth is the same as the concentration of polyacrylamide; the concentration of the ammonia solution is 0.5 M; and the drying temperature of the precipitate is the same as the water bath temperature. Then, the modified ultrafine diatomaceous earth and polyether-based moisture-wicking finishing agent are added to a 15% polyvinyl alcohol aqueous solution at a mass ratio of 4:1, and magnetically stirred until homogeneous. After ultrasonic treatment for 20 minutes, the suspension is taken and wet-spun to obtain multifunctional diatomaceous earth fibers.

[0088] Modified ultrafine diatomaceous earth and polyether moisture-wicking finishing agent were added to a polyvinyl alcohol solution and magnetically stirred until uniform. After ultrasonic treatment for 30 minutes, the suspension was taken and wet-spun to obtain modified ultrafine multifunctional diatomaceous earth fiber.

[0089] 4) Preparation of composite multifunctional diatomaceous earth fibers

[0090] Polyester-based fiber filaments and multifunctional diatomaceous earth fiber filaments are simultaneously fed into a filament cutter, a first roller, a pre-network, an anti-twist device, a deformation heat box, a cooling plate, a false twister, a second roller, a main networker, a shaping heat box oil wheel, and then wound to obtain the multifunctional diatomaceous earth fiber of the present invention.

[0091] The draw ratio of the second roller to the first roller is 1.015, and the winding speed of the second roller is -3.9%.

[0092] The ultrafine diatomaceous earth in this embodiment has a particle size of 500 nm.

[0093] In step 2), the cross-section of the spinneret's micro-orifices is a hollow trilobal shape. Furthermore, in step 3), the mass fraction concentration of the ultrafine diatomaceous earth is the same as the concentration of polyacrylamide; and the drying temperature of the precipitate is the same as the water bath temperature.

[0094] Furthermore, in step 3) of this embodiment, the wet spinning step is as follows:

[0095] A 15% (w / w) aqueous solution of polyvinyl alcohol was prepared, ultrasonically treated for 20 min, and then magnetically stirred and heated at 85℃ for 2 h. Modified ultrafine diatomaceous earth and a polyether-based moisture-wicking finishing agent were added to the prepared polyvinyl alcohol solution at a mass ratio of 4:1. The solution was magnetically stirred for 1 h, ultrasonically treated for 30 min, and then allowed to cool to room temperature before emulsion spinning. The wet spinning process parameters were as follows:

[0096] Spinning solution: concentration 16%;

[0097] Metering pump: 0.8 mL / r;

[0098] Rotational speed: 38 r / min;

[0099] Pump flow rate: 30 mL / min;

[0100] Spinneret has 1000 holes; hole diameter: 0.08 mm.

[0101] The coagulation bath length is 1.2m, the coagulation time is 15 seconds, and the fiber generation speed in the coagulation bath is 6m / min.

[0102] Guide disc diameter: 80mm;

[0103] Roller speed: 18 r / min; Roller speed: 25 r / min;

[0104] Moist heat stretching temperature: 120-150℃.

[0105] Example 3

[0106] Unlike Example 1 above, a method for preparing the multifunctional diatomaceous earth fiber includes the following steps:

[0107] 1) Preparation of ultrafine diatomaceous earth

[0108] Diatomaceous earth calcined at 800℃ for 120 min was selected for refining treatment. It was then ball-milled using a wet ball milling method with deionized water as the dispersion medium and a 10% (by weight) mixed dispersant (a ball-to-material ratio of 7:1). The mixed dispersant consisted of acrylate, maleic isool diester, and polyvinylpyrrolidone in a 2:1:2 (by weight) mixture, and the ball milling time was 6 h. The resulting mixed solution was allowed to precipitate for 6 h, the supernatant was collected, and then allowed to precipitate for another 12 h. The precipitate was then dried and ground to obtain ultrafine diatomaceous earth.

[0109] In this embodiment, the molecular weight of the polyvinylpyrrolidone is 130,000 g / mol.

[0110] 2) Preparation of polyester-based fiber filaments

[0111] Weigh the ultrafine diatomaceous earth described in step 1), and blend and melt it with polyester at a mass ratio of 30:100 to obtain a spinning solution. The spinning solution is extruded through a screw extruder and then enters a spinneret. The resulting fiber is then subjected to “stretching → washing → spraying with polyether moisture-wicking finishing agent → six-stage baking” to obtain polyester-based multifunctional diatomaceous earth fiber filament.

[0112] 3) Preparation of modified ultrafine multifunctional diatomaceous earth fibers

[0113] Place the ultrafine diatomaceous earth from step 1) in deionized water and add a 50% polyacrylamide solution. Stir the mixture evenly in a 70°C water bath. Then, add an appropriate amount of ammonia water dropwise at a rate of 0.5 mL / min and continue stirring evenly for 5 hours. After soaking for 24 hours, dry the precipitate to obtain modified ultrafine diatomaceous earth, and grind it for later use.

[0114] The concentration of the ultrafine diatomaceous earth is the same as the concentration of polyacrylamide; the concentration of the ammonia solution is 10 M; and the drying temperature of the precipitate is the same as the water bath temperature. Then, the modified ultrafine diatomaceous earth and the moisture-wicking finishing agent are added to a 15% polyvinyl alcohol aqueous solution at a mass ratio of 4:1, and magnetically stirred until homogeneous. After ultrasonic treatment for 50 minutes, the suspension is taken and wet-spun to obtain multifunctional diatomaceous earth fibers.

[0115] Modified ultrafine diatomaceous earth and polyether moisture-wicking finishing agent were added to a polyvinyl alcohol solution and magnetically stirred until uniform. After ultrasonic treatment for 30 minutes, the suspension was taken and wet-spun to obtain modified ultrafine multifunctional diatomaceous earth fiber.

[0116] 4) Preparation of composite multifunctional diatomaceous earth fibers

[0117] Polyester-based fiber filaments and multifunctional diatomaceous earth fiber filaments are simultaneously fed into a filament cutter, a first roller, a pre-network, an anti-twist device, a deformation heat box, a cooling plate, a false twister, a second roller, a main networker, a shaping heat box oil wheel, and then wound to obtain the multifunctional diatomaceous earth fiber of the present invention.

[0118] The draw ratio of the second roller to the first roller is 1.7325, and the winding speed of the second roller is -3.9%.

[0119] The ultrafine diatomite in this embodiment has a particle size of 900 nm.

[0120] In step 2), the cross-section of the spinneret's micro-orifices is a hollow trilobal shape. Furthermore, in step 3), the mass fraction concentration of the ultrafine diatomaceous earth is the same as the concentration of polyacrylamide; and the drying temperature of the precipitate is the same as the water bath temperature.

[0121] Furthermore, in step 3) of this embodiment, the wet spinning step is as follows:

[0122] A 15% (w / w) aqueous solution of polyvinyl alcohol was prepared, ultrasonically treated for 20 min, and then magnetically stirred and heated at 120℃ for 2 h. Modified ultrafine diatomaceous earth and a polyether-based moisture-wicking finishing agent were added to the prepared polyvinyl alcohol solution at a mass ratio of 4:1. The solution was magnetically stirred for 1 h, ultrasonically treated for 30 min, and then allowed to cool to room temperature before emulsion spinning. The wet spinning process parameters were as follows:

[0123] Spinning solution: concentration 16%;

[0124] Metering pump: 0.8 mL / r;

[0125] Rotational speed: 38 r / min;

[0126] Pump flow rate: 30 mL / min;

[0127] Spinneret has 1000 holes; hole diameter: 0.08 mm.

[0128] The coagulation bath length is 1.2m, the coagulation time is 15 seconds, and the fiber generation speed in the coagulation bath is 6m / min.

[0129] Guide disc diameter: 80mm;

[0130] Roller speed: 18 r / min; Roller speed: 25 r / min;

[0131] Moist heat stretching temperature: 120-150℃.

[0132] Comparative Example 1

[0133] Unlike Example 1, the mixing dispersant in step 1) is replaced with an equal mass of polyvinylpyrrolidone, while the other process steps are the same.

[0134] Comparative Example 2

[0135] Unlike Example 1, in step 1), the ball milling time of the diatomaceous earth in the preparation of ultrafine diatomaceous earth is 24 hours, while the other process steps are the same.

[0136] Comparative Example 3

[0137] The difference from Example 1 is that the polyether-based moisture-wicking finishing agent is replaced with moisture-wicking finishing agent LD-9020, while the other process steps are the same.

[0138] Comparative Example 4

[0139] Unlike Example 1, in step 3), the same volume of pure ammonia solution was used to treat the ultrafine diatomaceous earth during the preparation of the modified ultrafine diatomaceous earth, while the other process steps were the same.

[0140] Comparative Example 5

[0141] Unlike Example 1, in step 3), the modified ultrafine diatomaceous earth and polyether moisture-wicking finishing agent are added to the polyethylene terephthalate solution, while the other process steps are the same.

[0142] Performance testing

[0143] Antibacterial

[0144] The antimicrobial properties of fibers against Staphylococcus aureus, Escherichia coli and Candida albicans were tested according to GB / T 20944.3—2008 "Evaluation of antimicrobial properties of textiles - Part 3: Vibration method".

[0145] Moisture-wicking properties

[0146] The finished fibers were woven into wadding sheets of the same specifications, and their moisture absorption and wicking properties were tested. The moisture permeability was measured using the ASTM E96-1995BW standard, with the temperature maintained at 23°C and relative humidity at 50% in a constant temperature and humidity chamber. The moisture permeability of Examples 1-3 and Comparative Examples 1-3 was measured.

[0147] The perspiration performance is tested according to GB / T 21655.1—2008 "Evaluation of the moisture absorption and quick-drying properties of textiles - Part 1: Single combination test method", which measures water absorption rate, water droplet diffusion time and water evaporation rate.

[0148] Adsorption

[0149] The finished fibers are woven into wadding sheets of the same specifications. According to QB / T 2761—2006 "Method for Determining the Purification Effect of Indoor Air Purification Products", a 100g sample of fiber wadding sheets is placed in a 1.5m... 3 The test was conducted inside the test chamber, and the change rate of ammonia gas in the chamber over 24 hours was compared to test the adsorption performance of the fiber.

[0150] Meanwhile, particle size tests were conducted on the ultrafine diatomaceous earth samples from Example 1 and Comparative Examples 1-5. The average diameter of the particles in Comparative Example 2 was significantly larger than that of the other samples, indicating that prolonged ball milling in liquid led to more pronounced powder agglomeration, which is detrimental to the spinnability and dimensional stability of diatomaceous earth.

[0151] Table 1 shows the test results of the finished fiber filaments of Examples 1-3 and Comparative Examples 1-5 according to different performance test requirements. The relevant test results are shown in the table below:

[0152] Table 1. Physical property tests of finished fiber filaments

[0153]

[0154] Based on the above data, and combined with Figure 2 The nitrogen adsorption curve in the specific surface area test analysis of ultrafine diatomaceous earth shows that the diatomaceous earth particles still exhibit adsorption properties after ball milling. Furthermore, during the preparation process of this invention, the particle size of the ultrafine diatomaceous earth ensures that the modified ultrafine multifunctional diatomaceous earth fibers remain within the spinnable fiber range.

[0155] Furthermore, a mixture of acrylate, maleic isool diester, and polyvinylpyrrolidone (PVP) in a mass ratio of 2:1:2 was selected as the dispersant for ball milling. This serves two purposes: firstly, the dispersant effect of PVP enhances the uniformity and dimensional stability of the diatomaceous earth; secondly, the amphiphilic activation effect of the acrylate and maleic isool diester mixture on the diatomaceous earth facilitates its modification, promotes hydrogen bonding between diatomaceous earth particles in aqueous solution, reduces the possibility of diatomaceous earth aggregation, and thus enhances the stability and mechanical properties of the formed fibers. Mechanical property tests were conducted on the fibers from Comparative Example 1 and Example 1. The relevant mechanical properties of Example 1 were significantly better than those of Comparative Example 1.

[0156] Analysis of the adsorption comparison test data of ammonia removal rate shows that the multifunctional diatomaceous earth fiber of the present invention has excellent adsorption performance. Moreover, the multifunctional diatomaceous earth fiber prepared by the present invention has excellent performance in moisture absorption and perspiration, antibacterial properties, etc. The reason for this is that in the preparation process, the polyacrylamide solution system under a weak alkaline atmosphere can not only achieve flocculation, but also accelerate precipitation and active adsorption, and also help polyacrylamide modify diatomaceous earth: (1) Polyacrylamide is a linear polymer. Polyacrylamide can be hydrolyzed in alkaline conditions to undergo methylation and hydroxylation reactions of amines, resulting in hydroxyl groups, which makes the surface properties of diatomaceous earth active; (2) Hydroxyl groups can be adsorbed with charged particles in the solution to maintain charge neutralization, thereby enhancing its active adsorption effect; (3) Especially in the wet spinning process of polyvinyl alcohol, diatomaceous earth with activated hydroxyl groups can accumulate and generate hydrogen bonds, etc., resulting in good stability. Adding polyacrylamide to the modified ultrafine multifunctional diatomaceous earth fiber preparation system can build channel structures between fibers, increasing the contact time and contact area, thereby improving adsorption.

[0157] For polyether-based moisture-wicking finishing agents, the polymer chain structure of polyether-based moisture-wicking finishing agents is highly similar to that of polyester polymers. Therefore, they have extremely high affinity between ultrafine diatomite and polyester in polyester-based fiber filaments, between modified ultrafine diatomite in wet spinning, and between polyether-based moisture-wicking finishing agents. The compound use of polyether-based moisture-wicking finishing agents and diatomite can effectively reduce costs while ensuring moisture-wicking performance. Moreover, diatomite itself has antibacterial adsorption properties, which is conducive to the synergistic effect between moisture-wicking finishing agents and diatomite, effectively improving the moisture absorption and quick-drying properties of multifunctional diatomite fibers.

[0158] The use of polyvinyl alcohol (PVA) involves using stable heating conditions to cause PVA to lose some of its bound water, thereby disrupting intermolecular forces and reducing the impact of excessive hydroxyl groups in the wet spinning system on the stability of the fiber.

[0159] In summary, the preparation method of the multifunctional diatomaceous earth fiber of the present invention is simple to operate, uses inexpensive raw materials, and has the advantages of being green and economical. Moreover, the prepared multifunctional diatomaceous earth fiber has excellent comprehensive performance, which is conducive to its further development and application.

[0160] While the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the invention. Those skilled in the art can make various modifications and refinements without departing from the spirit and scope of the invention. Therefore, the scope of protection of the present invention shall be determined by the claims.

Claims

1. A multifunctional diatomaceous earth fiber, comprising a core and a fixed number of covering filaments, characterized in that: The core is composed of a number of polyester-based fiber filaments arranged in parallel. The coating filament is a modified ultrafine multifunctional diatomaceous earth fiber filament, and several of the modified ultrafine multifunctional diatomaceous earth fiber filaments are spirally wound around the outer surface of the filament core. The polyester-based fiber filament is a polyester-based multifunctional diatomaceous earth fiber filament, and three polyester-based multifunctional diatomaceous earth fiber filaments are arranged side by side; four modified ultrafine multifunctional diatomaceous earth fiber filaments are arranged side by side. The method for preparing multifunctional diatomaceous earth fibers includes the following steps: 1) Preparation of ultrafine diatomaceous earth Diatomaceous earth calcined at 800℃ was selected for fine treatment and ball milling was performed using wet ball milling with deionized water as the dispersion medium and 10% of the diatomaceous earth mass as a mixed dispersant. The ball milling ratio was 7:

1. The resulting mixed solution was precipitated for 6 hours, the supernatant was taken, and then precipitated for another 12 hours. The precipitate was then taken, dried, and ground to obtain ultrafine diatomaceous earth. 2) Preparation of polyester-based fiber filaments Weigh the ultrafine diatomite described in step 1), and blend and melt it with polyester at a mass ratio of 5-30:100 to obtain a spinning solution. The spinning solution is extruded through a screw extruder and then enters a spinneret. The resulting fiber is then subjected to "stretching → washing → spraying with polyether moisture-wicking finishing agent → six-stage baking" to obtain polyester-based multifunctional diatomite fiber filament. 3) Preparation of modified ultrafine multifunctional diatomaceous earth fibers Place the ultrafine diatomaceous earth from step 1) in deionized water, and add a 20%-50% polyacrylamide solution. Stir the mixture evenly in a water bath at 40℃-70℃. Then, add an appropriate amount of ammonia water dropwise at a rate of 0.5mL / min and continue stirring evenly for 1-5 hours. After soaking for 10-24 hours, dry the precipitate to obtain modified ultrafine diatomaceous earth, and grind it for later use. Modified ultrafine diatomaceous earth and polyether moisture-wicking finishing agent are added to polyvinyl alcohol solution and magnetically stirred until uniform. After ultrasonic treatment for 20-50 minutes, the suspension is taken and wet-spun to obtain modified ultrafine multifunctional diatomaceous earth fiber. 4) Preparation of multifunctional diatomaceous earth fibers Polyester-based fiber filaments and multifunctional diatomaceous earth fiber filaments are simultaneously fed into a filament cutter, a first roller, a pre-network, an anti-twist device, a deformation heat box, a cooling plate, a false twister, a second roller, a main networker, a shaping heat box oil wheel, and then wound to obtain multifunctional diatomaceous earth fiber. The draw ratio of the second roller to the first roller is 1.015-1.7325, and the winding speed is -3.9% of the winding ratio of the second roller.

2. The multifunctional diatomaceous earth fiber according to claim 1, characterized in that, The polyester-based fiber filaments are arranged in three parallel rows; the modified ultrafine multifunctional diatomaceous earth fiber filaments are arranged in four parallel rows.

3. The multifunctional diatomaceous earth fiber according to claim 1, characterized in that, Step 1) The calcination time of the diatomaceous earth is 25-120 min.

4. The multifunctional diatomaceous earth fiber according to claim 1, characterized in that, Step 1) The mixed dispersant is a mixture of acrylate, maleic isool diester, and polyvinylpyrrolidone in a mass ratio of 2:1:

2.

5. The multifunctional diatomaceous earth fiber according to claim 1, characterized in that, Step 1) The molecular weight of the polyvinylpyrrolidone is 130,000 g / mol.

6. The multifunctional diatomaceous earth fiber according to claim 1, characterized in that, Step 1) The ultrafine diatomaceous earth has a particle size of 500nm-900nm.

7. The multifunctional diatomaceous earth fiber according to claim 1, characterized in that, Step 2) The cross-section of the spinneret micro-orifice in the spinneret is one of a hollow circle, a hollow trilobal shape, or a hollow cross shape.

8. The multifunctional diatomaceous earth fiber according to claim 1, characterized in that, Step 3) The mass fraction concentration of the ultrafine diatomaceous earth is the same as the concentration of polyacrylamide; the concentration of the ammonia solution is 0.5-10M; the drying temperature of the precipitate is the same as the water bath temperature.

9. The multifunctional diatomaceous earth fiber according to claim 1, characterized in that, Step 3) The wet spinning step is as follows: A 15% (w / w) aqueous solution of polyvinyl alcohol was prepared, ultrasonically treated for 20 min, and then magnetically stirred and heated at 85℃-120℃ for 2 h. Modified ultrafine diatomaceous earth and a polyether-based moisture-wicking finishing agent were added to the prepared polyvinyl alcohol solution at a mass ratio of 4:

1. The solution was magnetically stirred for 1 h, ultrasonically treated for 30 min, and then allowed to cool to room temperature before emulsion spinning. The wet spinning process parameters were as follows: Spinning solution: concentration 16%; Metering pump: 0.8 mL / r; Rotational speed: 38 r / min; Pump flow rate: 30 mL / min; The number of spinneret holes is 1000; Hole diameter: 0.08mm; The coagulation bath length is 1.2m, the coagulation time is 15s, and the fiber generation speed in the coagulation bath is 6m / min. Guide disc diameter: 80mm; Roller speed: 18 r / min; Roller speed: 25 r / min; Moist heat stretching temperature: 120-150℃.

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