Preparation process of high-comfort waterproof and moisture-permeable magnetic health-care fabric

Abstract

The application relates to a preparation process of a high-comfort waterproof and moisture-permeable magnetic health-care fabric. The preparation process of the high-comfort waterproof and moisture-permeable magnetic health-care fabric comprises the following steps: preparation of a silane functionalized graphene dispersion liquid, preparation of magnetic nano Fe3O4 particles, preparation of silane functionalized graphene@Fe3O4 composite nanofibers, and fabric spinning. The spinning mainly comprises the following process steps: roughening, carding, drawing, combing, roving, spinning, warping, harnessing, weaving and the like. The silane functionalized graphene@Fe3O4 composite nanofibers are prepared by using the electrospinning technology, the smaller pore diameter and the interconnected porous characteristics in the micro-pore structure of the nanofibers enable the prepared health-care fabric to prevent liquid water penetration and diffuse a large amount of water vapor or sweat gas emitted by the human body, and the magnetic nano particles contained in the nanofibers enable the high-comfort waterproof and moisture-permeable magnetic health-care fabric prepared by using the method to have excellent magnetic health-care effect, waterproof and moisture-permeable performance and thermal comfort and the like.

Description

Technical Field

[0001] This invention specifically relates to a preparation process for a highly comfortable, waterproof, breathable, and magnetic health care fabric, belonging to the technical field of production processes for comfortable fabric products. Background Technology

[0002] Waterproof and breathable fabrics are textiles that combine waterproofness, comfort, windproofness, and warmth, and are widely used in daily protective clothing, building walls, medical and health care, and water treatment. As people's demands for the comfort, durability, and health benefits of functional protective clothing increase, waterproof, breathable, and health-promoting fabrics are showing huge market demand.

[0003] Magnetic health products, utilizing the magnetic properties of magnetic fibers, offer therapeutic effects on the human body and are gaining increasing popularity. These effects stem from the fact that magnetic fields induce a series of biomagnetic reactions in organisms, such as promoting cell membrane permeability, accelerating the exchange of substances between cells, and increasing nerve excitability and enzyme activity. Magnetic fibers and their fabrics contain permanent magnets that generate stable magnetism around the human body. When these magnetic health fabrics come into contact with the skin, they activate cellular metabolism, promote microcirculation, and achieve health benefits.

[0004] However, the quality of magnetic health care fabrics currently on the market varies greatly. Although they have magnetic health care effects, their waterproof, comfort, and windproof properties are poor, and they do not have good waterproof and breathable effects, which greatly limits the body's heat and moisture permeability. Therefore, the development of comfortable, waterproof, and breathable magnetic health care fabrics has become an increasingly important research topic for scientific researchers. Summary of the Invention

[0005] In order to overcome the above-mentioned technical problems existing in the existing technical field, the purpose of this invention is to provide a preparation process for a highly comfortable, waterproof, breathable, magnetic health care fabric, so as to promote its development and application.

[0006] The present invention provides a preparation process for a highly comfortable, waterproof, breathable, magnetic health care fabric, comprising the following steps:

[0007] Step (1) Preparation of silane-functionalized graphene dispersion

[0008] 1) Add GO solute to a beaker containing DMF solvent, and sonicate the beaker with ultrasound for a period of time to prepare a uniformly dispersed FG dispersion.

[0009] 2) Then, triethylamine catalyst and hexadecyltrimethoxysilane coupling agent were added to the FG dispersion. After stirring on a magnetic stirrer, the mixture was transferred from the beaker to a three-necked flask. An appropriate amount of nitrogen gas was introduced, and the heating temperature of the three-necked flask was set. The mixture was then refluxed under nitrogen protection. Finally, it was washed by centrifugation-washing, and then the product was vacuum dried in an electrically heated constant-temperature drying oven to obtain silane-functionalized graphite.

[0010] 3) Add the prepared silane-functionalized graphene to a beaker containing DMAc and acetone as solvents, and ultrasonically disperse for a period of time to prepare a silane-functionalized graphene dispersion.

[0011] Step (2) Preparation of magnetic Fe3O4 nanoparticles

[0012] NaAc and Fe(NO3)3 were added to a beaker containing ethylene glycol. The beaker was placed on a magnetic stirrer and stirred rapidly until all the reactants were dissolved, yielding Fe. 3+ The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace for a certain period of time. After cooling to room temperature, the reactor lid was opened, and the contents were collected using a magnet. The contents were then washed with deionized water and anhydrous ethanol, respectively. After being placed in a refrigerator and completely frozen, the contents were freeze-dried under vacuum to obtain nano-magnetic Fe3O4 particles.

[0013] Step (3) Preparation of silane-functionalized graphene@Fe3O4 composite nanofibers

[0014] The prepared nano-magnetic Fe3O4 particles were placed in the prepared silane-functionalized graphene dispersion and ultrasonically dispersed. The dispersion was then prepared into a spinning solution by magnetic stirring for a period of time. The solution was then sprayed out through a Taylor cone-shaped nozzle and entered a high-voltage electrostatic field. Finally, the solution was deposited on a receiving roller and drawn and collected to form silane-functionalized graphene@Fe3O4 composite nanofibers.

[0015] Step (4) Spinning and weaving

[0016] The prepared silane-functionalized graphene@Fe3O4 composite nanofibers were processed into a highly comfortable, waterproof, breathable, and magnetic health care fabric through processes such as napping, combing, drawing, combing, roving, spinning, warping, threading, and weaving.

[0017] Preferably, step (1) the preparation of silane-functionalized graphene dispersion includes: 1) adding 150-250 mg of GO solute to a beaker containing 75-150 mL of LDM solvent, and sonicating the beaker with ultrasound for 2-6 hours to prepare a uniformly dispersed FG dispersion; 2) then adding 0.1-0.5 mL of triethylamine catalyst and 2-4 g of hexadecyltrimethoxysilane silane coupling agent to the FG dispersion, stirring on a magnetic stirrer for 20-60 minutes, transferring the mixed solution from the beaker to a three-necked flask, introducing an appropriate amount of nitrogen, setting the heating temperature of the three-necked flask to 100-150 °C, and refluxing the mixture under nitrogen protection for 18-36 hours. Finally, the product was cleaned by centrifugation and washing, and then vacuum dried in an electric thermostatic drying oven at 50~80℃ to obtain silane-functionalized graphene; 3) The prepared silane-functionalized graphene was added to a beaker containing DMAc and acetone as solvents in a mass ratio of 1:(1~3), and ultrasonically dispersed for 2~6h to prepare silane-functionalized graphene dispersion.

[0018] This method uses silane-functionalized graphene to prepare a highly comfortable, waterproof, and breathable magnetic health fabric. Its physical structure exhibits a microscopic "spider web" pore structure, containing numerous tiny pores and interconnected porous features. This not only blocks microorganisms but also allows the prepared fabric to prevent liquid water penetration while simultaneously allowing the diffusion of large amounts of water vapor or perspiration from the human body, significantly improving the fabric's waterproof and breathable properties. During the preparation process, nitrogen is used to reflux the initially prepared mixed solution. This is to remove residual air from the liquid and prevent the reactants from reacting with oxygen in the air during the reaction, thus providing an inert atmosphere protection.

[0019] Preferably, step (2) of preparing magnetic nano-Fe3O4 particles includes adding 4-8g NaAc and 5-9g Fe(NO3)3 into a beaker containing 15-30mL ethylene glycol, placing the beaker on a magnetically heated stirrer, and stirring rapidly until all the reactants are dissolved to obtain Fe 3+ The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace and reacted at 200-250℃ for 10-15 hours. After cooling to room temperature, the reactor lid was opened, and the mixture was collected using a magnet. It was then washed 3-6 times with deionized water and anhydrous ethanol, respectively. After being placed in a -70--85℃ freezer until completely frozen, it was vacuum freeze-dried to obtain nano-magnetic Fe3O4 particles.

[0020] This method employs a hydrothermal reaction to synthesize nano-magnetic Fe3O4 particles because the hydrothermal reaction process is controllable, and the prepared nano-magnetic particles have a uniform particle size. This results in a more uniform structure in the subsequently prepared composite fibers and fabrics, reducing defects caused by uneven particle size and improving fabric comfort. The more uniform the particle size of the nano-magnetic particles, the better it is for maintaining the "spider web" porous structure of silane-functionalized graphene, preserving its excellent waterproof and breathable properties. Magnetic heating and stirring during the reaction process ensures sufficient contact between reactants, accelerating the reaction rate.

[0021] As a preferred embodiment, step (3) of preparing silane-functionalized graphene@Fe3O4 composite nanofibers includes placing 6~10g of nano-magnetic Fe3O4 particles into 15~30mL of silane-functionalized graphene dispersion, ultrasonically dispersing, and preparing a spinning solution by magnetic stirring for 1~2h. The solution is then sprayed out through a Taylor cone-shaped nozzle, enters a high-voltage electrostatic field, and is finally deposited on a receiving roller and drawn and collected to become silane-functionalized graphene@Fe3O4 composite nanofibers. The main parameters are: spinneret specification: SPN1500×0.12mm, spinning speed: 20~40 cm / s, and drawing ratio: 1.0~1.6 times.

[0022] This method utilizes electrospinning technology to prepare silane-functionalized graphene@Fe3O4 composite nanofibers. Because electrospinning produces fibers that are lightweight, soft, and highly comfortable, it significantly enhances the comfort of the resulting highly comfortable, waterproof, breathable, and magnetic health fabric. Furthermore, the preparation process is controllable, simple, and efficient, resulting in relatively low costs for composite fiber preparation using this method.

[0023] Preferably, step (4) spinning and weaving involves processing the prepared silane-functionalized graphene@Fe3O4 composite nanofibers through processes such as beating, combing, drawing, combing, roving, spinning, warping, threading, and weaving to produce a highly comfortable, waterproof, breathable, and magnetic health care fabric. The main parameters in this process are: a blending ratio of 30:30 to 50:50, repeated 3 to 6 times; 3 to 6 yarns combined; and the roving dried in a constant temperature room for 12 to 15 hours.

[0024] Among them, the beating and combing processes during spinning can effectively remove coarse and hard fibers from the fibers, allowing the composite fibers to gradually straighten and become parallel. This results in fabrics with fewer impurities and higher comfort.

[0025] This invention creatively utilizes silane-functionalized graphene with a "spider web" structure, enabling the fabric to prevent liquid water penetration while also allowing the diffusion of large amounts of water vapor or sweat emitted by the human body. It has very high waterproofness and thermal comfort. Furthermore, combined with nano-magnetic particles in the composite material, the fabric not only has high thermal comfort but also magnetic health care functions. Attached Figure Description

[0026] Figure 1 This is a flowchart illustrating the manufacturing process of a highly comfortable, waterproof, breathable, magnetic health care fabric. Detailed Implementation

[0027] Example 1

[0028] The present invention provides a preparation process for a highly comfortable, waterproof, breathable, magnetic health care fabric, comprising the following steps:

[0029] Step (1) Preparation of silane-functionalized graphene dispersion

[0030] 1) Add 150 mg of GO solute to a beaker containing 75 mL of LDM solvent, and sonicate the beaker with ultrasound for 2 hours to prepare a uniformly dispersed FG dispersion.

[0031] 2) Then, 0.1 mL of triethylamine catalyst and 2 g of hexadecyltrimethoxysilane coupling agent were added to the FG dispersion. After stirring on a magnetic stirrer for 20 min, the mixture was transferred from the beaker to a three-necked flask. An appropriate amount of nitrogen gas was introduced, and the heating temperature of the three-necked flask was set to 100 °C. The mixture was then refluxed under nitrogen protection for 18 h. Finally, the mixture was washed by centrifugation and washing, and then the product was vacuum dried in a 50 °C electric thermostatic drying oven to obtain silane-functionalized graphite.

[0032] 3) The prepared silane-functionalized graphene was added to a beaker containing DMAc and acetone in a mass ratio of 1:1 and ultrasonically dispersed for 2 hours to prepare a silane-functionalized graphene dispersion.

[0033] Step (2) Preparation of magnetic Fe3O4 nanoparticles

[0034] Add 4g NaAc and 5g Fe(NO3)3 to a beaker containing 15mL ethylene glycol. Place the beaker on a magnetic stirrer and stir rapidly until all the reactants are dissolved to obtain Fe. 3+ The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace and reacted at 200°C for 10 hours. After cooling to room temperature, the reactor lid was opened, and the mixture was collected using a magnet. It was then washed three times with deionized water and anhydrous ethanol, respectively. After being placed in a -70°C freezer until completely frozen, it was vacuum freeze-dried to obtain nano-magnetic Fe3O4 particles.

[0035] Step (3) Preparation of silane-functionalized graphene@Fe3O4 composite nanofibers

[0036] Six g of nano-magnetic Fe3O4 particles were placed in 15 mL of silane-functionalized graphene dispersion and ultrasonically dispersed. The dispersion was then magnetically stirred for 1 h to prepare a spinning solution. The solution was then ejected through a Taylor cone-shaped nozzle and entered a high-voltage electrostatic field. Finally, the solution was deposited on a receiving roller and drawn and collected to form silane-functionalized graphene@Fe3O4 composite nanofibers. The main parameters are: spinneret specification: SPN1500×0.12 mm, spinning speed: 20 cm / s, and draw ratio: 1.0.

[0037] Step (4) Spinning and weaving

[0038] The prepared silane-functionalized graphene@Fe3O4 composite nanofibers were processed into a highly comfortable, waterproof, breathable, and magnetic health care fabric through processes such as napping, combing, drawing, combing, roving, spinning, warping, threading, and weaving. The main parameters in the process were: a blend ratio of 30:30, repeated 3 times; 3 yarns combined; and the roving was dried in a constant temperature room for 12 hours.

[0039] Example 2

[0040] Step (1) Preparation of silane-functionalized graphene dispersion

[0041] 1) Add 170 mg of GO solute to a beaker containing 85 mL of LDM solvent, and sonicate the beaker with ultrasound for 3 hours to prepare a uniformly dispersed FG dispersion.

[0042] 2) Then, 0.2 mL of triethylamine catalyst and 2.5 g of hexadecyltrimethoxysilane coupling agent were added to the FG dispersion. After stirring on a magnetic stirrer for 30 min, the mixture was transferred from the beaker to a three-necked flask. An appropriate amount of nitrogen gas was introduced, and the heating temperature of the three-necked flask was set to 110 °C. The mixture was then refluxed under nitrogen protection for 22 h. Finally, the mixture was washed by centrifugation and washing, and then the product was vacuum dried in a 60 °C electric thermostatic drying oven to obtain silane-functionalized graphite.

[0043] 3) The prepared silane-functionalized graphene was added to a beaker containing DMAc and acetone in a mass ratio of 1:1.5 as solvents and ultrasonically dispersed for 3 hours to prepare a silane-functionalized graphene dispersion.

[0044] Step (2) Preparation of magnetic Fe3O4 nanoparticles

[0045] Add 5g NaAc and 6g Fe(NO3)3 to a beaker containing 20mL ethylene glycol. Place the beaker on a magnetic stirrer and stir rapidly until all the reactants are dissolved to obtain Fe. 3+The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace and reacted at 220°C for 11 hours. After cooling to room temperature, the reactor lid was opened, and the mixture was collected using a magnet. It was then washed four times with deionized water and anhydrous ethanol, respectively. After being placed in a -75°C freezer until completely frozen, it was vacuum freeze-dried to obtain nano-magnetic Fe3O4 particles.

[0046] Step (3) Preparation of silane-functionalized graphene@Fe3O4 composite nanofibers

[0047] 7g of nano-magnetic Fe3O4 particles were placed in 20mL of silane-functionalized graphene dispersion and ultrasonically dispersed. The dispersion was then magnetically stirred for 1.5h to prepare a spinning solution. The solution was then ejected through a Taylor cone-shaped nozzle and entered a high-voltage electrostatic field. Finally, the solution was deposited on a receiving roller and drawn and collected to form silane-functionalized graphene@Fe3O4 composite nanofibers. The main parameters are: spinneret specification: SPN1500×0.12 mm, spinning speed: 25 cm / s, and draw ratio: 1.2 times.

[0048] Step (4) Spinning and weaving

[0049] The prepared silane-functionalized graphene@Fe3O4 composite nanofibers were processed into a highly comfortable, waterproof, breathable, and magnetic health care fabric through processes such as napping, combing, drawing, combing, roving, spinning, warping, threading, and weaving. The main parameters in the process were: a blend ratio of 35:35, repeated 4 times; 4 yarns combined; and the roving was dried in a constant temperature room for 13 hours.

[0050] Example 3

[0051] Step (1) Preparation of silane-functionalized graphene dispersion

[0052] 1) Add 200 mg of GO solute to a beaker containing 105 mL of LDM solvent, and sonicate the beaker with ultrasound for 4 hours to prepare a uniformly dispersed FG dispersion.

[0053] 2) Then, 0.3 mL of triethylamine catalyst and 3.0 g of hexadecyltrimethoxysilane coupling agent were added to the FG dispersion. After stirring on a magnetic stirrer for 40 min, the mixture was transferred from the beaker to a three-necked flask. An appropriate amount of nitrogen gas was introduced, and the heating temperature of the three-necked flask was set to 120 °C. The mixture was then refluxed under nitrogen protection for 24 h. Finally, the mixture was washed by centrifugation and washing, and then the product was vacuum dried in a 70 °C electric thermostatic drying oven to obtain silane-functionalized graphite.

[0054] 3) The prepared silane-functionalized graphene was added to a beaker containing DMAc and acetone in a mass ratio of 1:2 and ultrasonically dispersed for 3 hours to prepare a silane-functionalized graphene dispersion.

[0055] Step (2) Preparation of magnetic Fe3O4 nanoparticles

[0056] Add 6g NaAc and 7g Fe(NO3)3 to a beaker containing 25mL ethylene glycol. Place the beaker on a magnetic stirrer and stir rapidly until all the reactants are dissolved to obtain Fe. 3+ The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace and reacted at 230°C for 13 hours. After cooling to room temperature, the reactor lid was opened, and the mixture was collected using a magnet. It was then washed five times each with deionized water and anhydrous ethanol. After being placed in a -80°C freezer until completely frozen, it was vacuum freeze-dried to obtain nano-magnetic Fe3O4 particles.

[0057] Step (3) Preparation of silane-functionalized graphene@Fe3O4 composite nanofibers

[0058] 8g of nano-magnetic Fe3O4 particles were placed in 25mL of silane-functionalized graphene dispersion and ultrasonically dispersed. The dispersion was then prepared into a spinning solution by magnetic stirring for 1.5h. The solution was then ejected through a Taylor cone-shaped nozzle and entered a high-voltage electrostatic field. Finally, the solution was deposited on a receiving roller and drawn and collected to form silane-functionalized graphene@Fe3O4 composite nanofibers. The main parameters are: spinneret specification: SPN1500×0.15 mm, spinning speed: 30 cm / s, and draw ratio: 1.4 times.

[0059] Step (4) Spinning and weaving

[0060] The prepared silane-functionalized graphene@Fe3O4 composite nanofibers were processed into a highly comfortable, waterproof, breathable, and magnetic health care fabric through processes such as napping, combing, drawing, combing, roving, spinning, warping, threading, and weaving. The main parameters in the process were: a blend ratio of 40:40, repeated 5 times; 5 yarns combined; and the roving was dried in a constant temperature room for 14 hours.

[0061] Example 4

[0062] Step (1) Preparation of silane-functionalized graphene dispersion

[0063] 1) Add 220 mg of GO solute to a beaker containing 135 mL of LDMF solvent, and sonicate the beaker with ultrasound for 5 hours to prepare a uniformly dispersed FG dispersion.

[0064] 2) Then, 0.4 mL of triethylamine catalyst and 3.5 g of hexadecyltrimethoxysilane coupling agent were added to the FG dispersion. After stirring on a magnetic stirrer for 50 min, the mixture was transferred from the beaker to a three-necked flask. An appropriate amount of nitrogen gas was introduced, and the heating temperature of the three-necked flask was set to 140 °C. The mixture was then refluxed under nitrogen protection for 30 h. Finally, the mixture was washed by centrifugation and washing, and then the product was vacuum dried in a 75 °C electric thermostatic drying oven to obtain silane-functionalized graphite.

[0065] 3) The prepared silane-functionalized graphene was added to a beaker containing DMAc and acetone in a mass ratio of 1:2.5 as solvents and ultrasonically dispersed for 4 hours to prepare a silane-functionalized graphene dispersion.

[0066] Step (2) Preparation of magnetic Fe3O4 nanoparticles

[0067] Add 7g NaAc and 8g Fe(NO3)3 to a beaker containing 30mL ethylene glycol. Place the beaker on a magnetic stirrer and stir rapidly until all the reactants are dissolved to obtain Fe. 3+ The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace and reacted at 240°C for 14 hours. After cooling to room temperature, the reactor lid was opened, and the mixture was collected using a magnet. It was then washed 6 times each with deionized water and anhydrous ethanol. After being placed in a -85°C freezer until completely frozen, it was vacuum freeze-dried to obtain nano-magnetic Fe3O4 particles.

[0068] Step (3) Preparation of silane-functionalized graphene@Fe3O4 composite nanofibers

[0069] Nine g of nano-magnetic Fe3O4 particles were placed in 30 mL of silane-functionalized graphene dispersion and ultrasonically dispersed. The dispersion was then prepared into a spinning solution by magnetic stirring for 2 h. The solution was then ejected through a Taylor cone-shaped nozzle and entered a high-voltage electrostatic field. Finally, the solution was deposited on a receiving roller and drawn and collected to form silane-functionalized graphene@Fe3O4 composite nanofibers. The main parameters are: spinneret specification: SPN1500×0.15 mm, spinning speed: 35 cm / s, and draw ratio: 1.6 times.

[0070] Step (4) Spinning and weaving

[0071] The prepared silane-functionalized graphene@Fe3O4 composite nanofibers were processed into a highly comfortable, waterproof, breathable, and magnetic health care fabric through processes such as napping, combing, drawing, combing, roving, spinning, warping, threading, and weaving. The main parameters in the process were: a blend ratio of 45:45, repeated 6 times; 6 yarns combined; and the roving was dried in a constant temperature room for 15 hours.

[0072] Comparative Example 1

[0073] Step (1) Preparation of silane-functionalized graphene dispersion

[0074] 1) Add 150 mg of GO solute to a beaker containing 75 mL of LMP solvent, and sonicate the beaker with ultrasound for 2 hours to prepare a uniformly dispersed FG dispersion.

[0075] 2) Then, 0.1 mL of triethylamine catalyst and 2 g of hexadecyltrimethoxysilane coupling agent were added to the FG dispersion. After stirring on a magnetic stirrer for 20 min, the mixture was transferred from the beaker to a three-necked flask. An appropriate amount of helium gas was introduced, and the heating temperature of the three-necked flask was set to 100 °C. The mixture was then refluxed under nitrogen protection for 18 h. Finally, the mixture was washed by centrifugation and washing, and then the product was vacuum dried in a 50 °C electric thermostatic drying oven to obtain silane-functionalized graphite.

[0076] 3) Add the prepared silane-functionalized graphene to a beaker containing 10 mL of acetone as solvent and ultrasonically disperse for 2 h to prepare a silane-functionalized graphene dispersion.

[0077] Step (2) Preparation of magnetic Fe3O4 nanoparticles

[0078] Add 4g NaAc and 5g FeCl3 to a beaker containing 15mL ethylene glycol. Place the beaker on a magnetic stirrer and stir rapidly until all the reactants are dissolved to obtain Fe. 3+ The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace and reacted at 200°C for 10 hours. After cooling to room temperature, the reactor lid was opened, and the mixture was collected using a magnet. It was then washed three times with deionized water and anhydrous ethanol, respectively. After being placed in a -70°C freezer until completely frozen, it was vacuum freeze-dried to obtain nano-magnetic Fe3O4 particles.

[0079] Step (3) Preparation of silane-functionalized graphene@Fe3O4 composite nanofibers

[0080] Six g of nano-magnetic Fe3O4 particles were placed in 15 mL of silane-functionalized graphene dispersion and ultrasonically dispersed. The dispersion was then magnetically stirred for 1 h to prepare a spinning solution. The solution was then ejected through a Taylor cone-shaped nozzle and entered a high-voltage electrostatic field. Finally, the solution was deposited on a receiving roller and drawn and collected to form silane-functionalized graphene@Fe3O4 composite nanofibers. The main parameters are: spinneret specification: SPN1500×0.12 mm, spinning speed: 20 cm / s, and draw ratio: 1.0.

[0081] Step (4) Spinning and weaving

[0082] The prepared silane-functionalized graphene@Fe3O4 composite nanofibers were processed into a highly comfortable, waterproof, breathable, and magnetic health care fabric through processes such as napping, combing, drawing, combing, roving, spinning, warping, threading, and weaving. The main parameters in the process were: a blend ratio of 30:30, repeated 3 times; 3 yarns combined; and the roving was dried in a constant temperature room for 12 hours.

[0083] Comparative Example 2

[0084] Step (1) Preparation of silane-functionalized graphene dispersion

[0085] 1) Add 180 mg of GO solute to a beaker containing 90 mL of LMP solvent, and sonicate the beaker with ultrasound for 3 hours to prepare a uniformly dispersed FG dispersion.

[0086] 2) Then, 0.3 mL of triethylamine catalyst and 4 g of hexadecyltrimethoxysilane coupling agent were added to the FG dispersion. After stirring on a magnetic stirrer for 40 min, the mixture was transferred from the beaker to a three-necked flask. An appropriate amount of helium gas was introduced, and the heating temperature of the three-necked flask was set to 120 °C. The mixture was then refluxed under nitrogen protection for 22 h. Finally, the mixture was washed by centrifugation and washing, and then the product was vacuum dried in a 60 °C electric thermostatic drying oven to obtain silane-functionalized graphite.

[0087] 3) The prepared silane-functionalized graphene was added to a beaker containing 15 mL of acetone as solvent and ultrasonically dispersed for 2 h to prepare a silane-functionalized graphene dispersion.

[0088] Step (2) Preparation of magnetic Fe3O4 nanoparticles

[0089] Add 5g NaAc and 6g FeCl3 to a beaker containing 20mL ethylene glycol. Place the beaker on a magnetic stirrer and stir rapidly until all the reactants are dissolved to obtain Fe. 3+ The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace and reacted at 220°C for 12 hours. After cooling to room temperature, the reactor lid was opened, and the mixture was collected using a magnet. It was then washed four times with deionized water and anhydrous ethanol, respectively. After being placed in a -75°C freezer until completely frozen, it was vacuum freeze-dried to obtain nano-magnetic Fe3O4 particles.

[0090] Step (3) Preparation of silane-functionalized graphene@Fe3O4 composite nanofibers

[0091] 8g of nano-magnetic Fe3O4 particles were placed in 25mL of silane-functionalized graphene dispersion and ultrasonically dispersed. The dispersion was then prepared into a spinning solution by magnetic stirring for 2h. The solution was then ejected through a Taylor cone-shaped nozzle and entered a high-voltage electrostatic field. Finally, the solution was deposited on a receiving roller and drawn and collected to form silane-functionalized graphene@Fe3O4 composite nanofibers. The main parameters are: spinneret specification: SPN1500×0.13 mm, spinning speed: 25 cm / s, and draw ratio: 1.2 times.

[0092] Step (4) Spinning and weaving

[0093] The prepared silane-functionalized graphene@Fe3O4 composite nanofibers were processed into a highly comfortable, waterproof, breathable, and magnetic health care fabric through processes such as napping, combing, drawing, combing, roving, spinning, warping, threading, and weaving. The main parameters in the process were: a blend ratio of 40:30, repeated 3 times; 5 yarns combined; and the roving was dried in a constant temperature room for 14 hours.

[0094] The high-comfort, waterproof, breathable, magnetic health care fabric samples prepared in Examples 1 to 4 and Comparative Examples 1 and 2 were subjected to performance tests. The specific testing methods are as follows:

[0095] Tensile fracture performance test

[0096] The mechanical properties (breaking strength - elongation at break) of the samples were determined using an intelligent electronic tensile testing machine (LILY-06ED / PC, Jinan Langguang Electromechanical Co., Ltd.). The prepared fabric was then compared to areas with better uniformity, and cut into 3×80 mm pieces. 2 For long strip samples, the clamping distance was set to 50 mm and the fabric stretching rate was set to 50 mm / min. Multiple tests were conducted on the fabric corresponding to each parameter, and then the average value was calculated.

[0097] Waterproofing test

[0098] The water pressure resistance of the samples was measured using a YG812F water permeability tester. The test was conducted using the pressurization method, with the water flow pressurization rate set at 6 kPa / min. -1 When three water droplets appear on the surface of the sample being tested, record the water pressure resistance value of the corresponding fabric on the display screen at that time. Test each sample 10 times and take the average value.

[0099] Thermal comfort test

[0100] Referring to the testing standard ASTM E96 E96M-16 for waterproof and breathable fabrics, the test method for its fabrics, namely "Test Method for Water Vapor Permeability of Materials," was used. The experiment employed a water vapor transmission rate tester to determine the moisture permeability of the samples. First, the waterproof and breathable fabric was cut into circular pieces with an area of ​​33 cm². 2The size of the fabric is determined, and the cut fabric is placed on a moisture-permeable cup filled with distilled water and secured with rubber rings. The moisture-permeable cups are then placed in a balanced moisture-permeable chamber in sequence (temperature and humidity are 38℃ and 90%, respectively). The relevant parameters are set according to the test operation, and the moisture permeability of the waterproof and breathable fabric is calculated.

[0101] Magnetic durability test

[0102] The surface magnetic induction intensity of each magnetic fabric sample was tested before and after each wash using an LZT-1160 high-Tesla magnetic field strength tester. The specific operation followed GB / T 8629-2001 "Home Washing and Drying Procedures for Textile Testing". Samples were cut into 25cm × 25cm pieces, with six pieces of each fabric type. A 90cm × 90cm piece of pure cotton woven fabric was used as a wash companion. All samples were washed, laid flat, and dried. Multiple tests were conducted, and the average value was recorded.

[0103] Table 1. Tensile fracture property test results

[0104]

[0105] As shown in Table 1, Examples 1 to 4 all exhibit better tensile strength at break than Comparative Examples 1 and 2. This is because the examples used DMF solvent, which has better compatibility with GO solute. Compared with DMP solvent, the polymer molecular chain structure in the prepared fabric is more compact, the fiber is more tough, and the breaking strength at break is greater. Moreover, the silane-functionalized graphene and magnetic nanoparticles are interwoven and combined in the composite fiber, resulting in a very stable composite fiber structure and excellent tensile strength at break.

[0106] Table 2 Waterproofing Test Results

[0107]

[0108] As shown in Table 2, the waterproofing test results indicate that Examples 1 to 4 all exhibit better waterproofing than Comparative Examples 1 and 2. In the comparative examples, the poor compatibility between the DMP solvent and the GO solute resulted in a certain proportion of defects in the prepared composite fibers, leading to lower water pressure resistance and poorer waterproofing performance. In contrast, Examples 1-4, with their increased content of magnetic nanofiber particles and silane-functionalized graphene, improved and strengthened the mechanical properties of the composite fibers. The addition of DMAc solvent during the preparation process also resulted in the formation of a fiber film on the surface of the composite fibers, increasing the contact angle and water pressure resistance of the fabric, thus giving the prepared fabric excellent waterproofing performance.

[0109] Table 3 Thermal comfort test results

[0110]

[0111] As shown in Table 3, the thermal comfort test results indicate that Examples 1 to 4 all exhibit lower moisture permeability and breathability than Comparative Examples 1 and 2, demonstrating better thermal comfort performance. Furthermore, with the increase in the composite fiber content, both moisture permeability and breathability decrease. This is because the increased composite fiber content leads to larger fiber diameters, resulting in a relative increase in internal porosity. More porosity allows sweat generated on the human body surface to be transferred to the external environment more quickly through the gaps between the fibers, preventing discomfort caused by sweat condensation and stickiness, thus improving the fabric's thermal comfort and everyday usability.

[0112] Table 4 Magnetic Durability Test Results

[0113]

[0114] Table 4 shows that all examples and comparative examples exhibit good magnetic durability, with minimal differences in maximum and average values ​​before and after washing. However, the comparative example lacked solvents such as acetone in its preparation of the silane-functionalized graphene dispersion, resulting in lower binding performance with the nano-magnetic particles. Consequently, its overall magnetic properties were lower than those of the examples, and its magnetic health benefits were also relatively lower. The examples, on the other hand, demonstrated good retention of magnetic induction intensity before and after washing, enhancing the magnetic health benefits of the fabric and extending its lifespan.

[0115] This specific embodiment is merely an explanation of the present invention and is not intended to limit the present invention. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but as long as they are within the scope of the claims of the present invention, they are protected by patent law.

Claims

1. A preparation process for a highly comfortable, waterproof, breathable, magnetic health care fabric, characterized in that: Step (1) Preparation of silane-functionalized graphene dispersion 1) Add GO solute to a beaker containing DMF solvent, and sonicate the beaker with ultrasound for a period of time to prepare a uniformly dispersed FG dispersion. 2) Then, triethylamine catalyst and hexadecyltrimethoxysilane coupling agent were added to the FG dispersion. After stirring on a magnetic stirrer, the mixture was transferred from the beaker to a three-necked flask. An appropriate amount of nitrogen was introduced, and the heating temperature of the three-necked flask was set. The mixture was then refluxed under nitrogen protection. Finally, the mixture was washed by centrifugation and washing. The product was then vacuum dried in an electric thermostatic drying oven to obtain silane-functionalized graphene. 3) The prepared silane-functionalized graphene was added to a beaker containing DMAc and acetone as solvents and ultrasonically dispersed for a period of time to prepare a silane-functionalized graphene dispersion. Step (2) Preparation of magnetic Fe3O4 nanoparticles 4-8 g of NaAc and 5-9 g of Fe(NO3)3 were added to a beaker containing 15-30 mL of ethylene glycol. The beaker was placed on a magnetic stirrer and stirred rapidly until all the reactants were dissolved, yielding Fe. 3+ The dispersion was then transferred to a hydrothermal synthesis reactor using a glass rod. The reactor lid was tightened, and the reactor was placed in a muffle furnace and reacted at 200-250℃ for 10-15 hours. After cooling to room temperature, the reactor lid was opened, and the mixture was collected by a magnet and washed 3-6 times with deionized water and anhydrous ethanol, respectively. The mixture was then placed in a -85--70℃ freezer until it was completely frozen and then vacuum freeze-dried to obtain nano-magnetic Fe3O4 particles. Step (3) Preparation of silane-functionalized graphene@Fe3O4 composite nanofibers 6-10g of nano-magnetic Fe3O4 particles are placed in 15-30mL of silane-functionalized graphene dispersion, ultrasonically dispersed, and magnetically stirred for 1-2h to prepare a spinning solution. The solution is then sprayed out through a Taylor cone nozzle, enters a high-voltage electrostatic field, and is finally deposited on a receiving roller and drawn and collected to become silane-functionalized graphene@Fe3O4 composite nanofibers. Step (4) Spinning and weaving The prepared silane-functionalized graphene@Fe3O4 composite nanofibers were processed into a highly comfortable, waterproof, breathable, and magnetic health care fabric through processes such as napping, combing, drawing, combing, roving, spinning, warping, threading, and weaving.

2. The preparation process of a highly comfortable, waterproof, breathable, magnetic health care fabric according to claim 1, characterized in that: Step (1) Preparation of silane-functionalized graphene dispersion includes: 1) Adding 150-250 mg of GO solute to a beaker containing 75-150 mL of LDM solvent, and sonicating the beaker with ultrasound for 2-6 hours to prepare a uniformly dispersed FG dispersion; 2) Then adding 0.1-0.5 mL of triethylamine catalyst and 2-4 g of hexadecyltrimethoxysilane silane coupling agent to the FG dispersion, stirring on a magnetic stirrer for 20-60 minutes, and then transferring the mixture from the beaker to a three-necked flask. After introducing an appropriate amount of nitrogen, the heating temperature of the three-necked flask is set to 100~150℃, and the mixture is refluxed under nitrogen protection for 18~36h; finally, it is washed by centrifugation-washing, and then the product is vacuum dried in an electric thermostatic drying oven at 50~80℃ to obtain silane-functionalized graphene; 3) The prepared silane-functionalized graphene is added to a beaker containing DMAc and acetone as solvents in a mass ratio of 1:(1~3), and ultrasonically dispersed for 2~6h to prepare a silane-functionalized graphene dispersion.

3. The preparation process of a highly comfortable, waterproof, breathable, magnetic health care fabric according to claim 1, characterized in that: Step (4) The main parameters during spinning and weaving are: blending ratio of 30:30 to 50:50, repeated 3 to 6 times; number of yarns combined 3 to 6; and roving dried in a constant temperature room for 12 to 15 hours.

Images