Preparation method of heating type graphene fabric

Abstract

The application discloses a preparation method of a heating type graphene fabric, and steps of the method comprise the following steps: blending cotton fibers and bamboo fibers to obtain a base cloth layer; preparing graphene oxide fibers, performing surface grafting modification treatment on the graphene oxide fibers by using N-aminoethyl-3-aminopropyl methyl dimethoxysilane, performing soaking treatment on the graphene oxide fibers by using a bauhinia championii extract, blending the treated graphene oxide fibers and the cotton fibers to obtain a graphene fiber layer, taking double-layer graphene fiber layers, laying an electric heating wire mesh in the double-layer graphene fiber layers to obtain an electric heating layer; blending polyester fibers, nylon fibers and glass fibers to obtain a heat insulation protective layer; and bonding the base cloth layer, the electric heating layer and the heat insulation protective layer in sequence to obtain the heating type graphene fabric. The prepared fabric can provide stable heating effect, the structure and distribution of graphene are strengthened, the influence of the fabric heat conduction effect in a wearing process is reduced, and the antibacterial effect is outstanding.

Description

Technical Field

[0001] The present invention relates to the technical field of fabric preparation, and in particular to a method for preparing a heated graphene fabric. Background Art

[0002] Graphene is an emerging material that has been widely studied in recent years. It is ultra-thin, has excellent conductivity, super hardness, and is light and soft. It has great application prospects in aerospace, weapons and equipment, major infrastructure, as well as new energy, new energy vehicles, energy conservation and environmental protection, and electronic information.

[0003] Research has shown that graphene materials can be applied to textile fabrics because they also have excellent thermal conductivity and certain antibacterial properties. The high thermal conductivity can enable the fabric to be processed into heating-type fabrics and applied to human protective products used in certain environments, while the antibacterial properties can increase the antibacterial and deodorizing properties of the fabric. However, the development of existing heating-type graphene fabrics with both antibacterial properties has encountered a technical difficulty: the thermal conductivity and antibacterial properties of graphene fabrics will be significantly reduced after repeated wear and use. The reason for this is that the wearing process has a certain impact on the structure and distribution of graphene, thereby reducing its thermal conductivity and antibacterial effects. Summary of the Invention

[0004] The object of the present invention is to provide a method for preparing a heating type graphene fabric, which solves the problem that the thermal conductivity and antibacterial properties of the existing heating type graphene fabric are significantly reduced after being worn and used multiple times.

[0005] The present invention achieves the above-mentioned purpose through the following technical solutions:

[0006] A method for preparing a heated graphene fabric, comprising the following steps:

[0007] S1. Preparing a base fabric layer: blending cotton fiber and bamboo fiber to obtain a base fabric layer;

[0008] S2. Preparation of an electric heating layer: preparing graphene oxide fiber, using N-aminoethyl-3-aminopropylmethyldimethoxysilane to perform surface grafting modification treatment on it, then soaking it with a vine extract, taking the treated graphene oxide fiber and cotton fiber to blend to obtain a graphene fiber layer, then taking a double-layer graphene fiber layer and laying an electric heating wire mesh in the interlayer to obtain an electric heating layer;

[0009] S3, preparing a heat-insulating protective layer: blending polyester fiber, nylon fiber and glass fiber to obtain a heat-insulating protective layer;

[0010] S4. Take the prepared base fabric layer, electric heating layer, and heat-insulating protective layer and bond them in sequence to obtain the heating-type graphene fabric.

[0011] A further improvement is that the mass ratio of cotton fiber to bamboo fiber in the base fabric layer is 1-3:1.

[0012] A further improvement is that the specific operation of preparing graphene oxide fibers is as follows:

[0013] Prepare a spinning solution: take a graphene oxide solution, adjust the pH to 6-10, and obtain a spinning solution;

[0014] Preparation of fibrils: taking the spinning solution through a 0.5-1 mm spinneret and injecting it into a coagulation bath at a speed of 0.2-1 mL / min, and then drying to obtain fibrils;

[0015] Stretching and shaping: placing the raw fibers in a protective atmosphere furnace, controlling the temperature to 200-400°C, and applying tension to the raw fibers to make the fiber length stretching rate reach 28-32%;

[0016] Reduction: Take the original fibers after stretching and shaping, place them in a reducing agent for reduction for 1-5 hours, wash and dry to obtain graphene oxide fibers.

[0017] A further improvement is that the reducing agent is selected from one of hydrazine hydrate, hydrobromic acid, sodium borohydride or hydroiodic acid.

[0018] A further improvement is that the specific operation of the surface grafting modification treatment is: taking N-aminoethyl-3-aminopropylmethyldimethoxysilane and dispersing it in 4-8 times the mass of ethanol to obtain a dispersion, then immersing the graphene oxide fiber in the dispersion, ultrasonically oscillating for 40-60 minutes, taking out the graphene oxide fiber, washing, and drying.

[0019] A further improvement is that the specific operation of the soaking treatment is: take the dried stems of the vine of the Chinese wolfberry, crush them to 120-150 mesh, soak them in 70% ethanol with 15-20 times the mass for 24-48 hours, then stir and extract them at 60-70°C for 100-150 minutes, filter the residue to obtain the extract, immerse the graphene oxide fiber in the extract for 1-3 hours, take out the graphene oxide fiber, wash and dry it.

[0020] A further improvement is that the mass ratio of polyester fiber, nylon fiber and glass fiber in the heat-insulating protective layer is 0.5-4:1-2:1.

[0021] A further improvement is that the base fabric layer, the electric heating layer and the heat-insulating protective layer are bonded together by an adhesive, and the adhesive is selected from one of polyvinyl alcohol, polyacrylate, epoxy resin or carboxymethyl cellulose.

[0022] A further improvement is that the warp density of the base fabric layer is 200-250 threads / 10cm, and the weft density is 160-200 threads / 10cm, the warp density of the graphene fiber layer is 150-180 threads / 10cm, and the weft density is 150-180 threads / 10cm, and the warp density of the thermal insulation protective layer is 180-220 threads / 10cm, and the weft density is 150-180 threads / 10cm.

[0023] The beneficial effects of the present invention are:

[0024] (1) The modified graphene oxide fiber of the present invention has undergone surface grafting modification treatment with N-aminoethyl-3-aminopropylmethyldimethoxysilane, so that the amino group of N-aminoethyl-3-aminopropylmethyldimethoxysilane reacts with the functional groups (such as hydroxyl, carboxyl, etc.) on the fiber surface to form a stable chemical bond. At the same time, the silane group can also form a covalent bond with the carbon atoms on the fiber surface, thereby enhancing the grafting modification effect, significantly improving the fiber's binding ability, chemical stability and biocompatibility, strengthening the structure and distribution of graphene, and reducing the impact of the wearing process on the fabric's thermal conductivity; then the fiber is soaked in a vine extract, so that a large amount of vine bioactive ingredients are infiltrated and locked into the fiber, thereby significantly improving the fiber's antibacterial and antioxidant properties. In this way, the overall antibacterial effect of the fabric can still be effectively maintained after multiple wearing and use;

[0025] (2) The present invention arranges the electric heating wire in the graphene fiber layer, and utilizes its high thermal conductivity to quickly and evenly spread the heat, and transfer it inward from the base fabric layer to provide a stable heating effect. DETAILED DESCRIPTION

[0026] The present application is further described in detail below in conjunction with specific embodiments. It is necessary to point out here that the following specific implementation methods are only used to further illustrate the present application and cannot be understood as limiting the scope of protection of the present application. Technical personnel in this field can make some non-essential improvements and adjustments to the present application based on the above application content.

[0027] 1. Main Materials

[0028] (1) Graphene oxide solution: 100 g of graphite powder and 50 g of sodium nitrate were placed in a glass container, and 2.3 L of concentrated sulfuric acid was slowly added to the container. The mixture was stirred in an ice bath for 2.5 h. 600 g of potassium permanganate was weighed and slowly added to the container. The temperature was maintained at no more than 20 °C and the mixture was stirred for 1 h. The ice bath was then removed and the container was placed in a 35 °C water bath. The mixture was stirred for 2.5 h to obtain a dark brown paste. 4.8 L of hot water was added to the mixture and stirred. After the temperature reached 98 °C, the mixture was quickly transferred to a 98 °C hot water bath and stirred at a constant temperature for 5 min. The hot water bath was then removed and the mixture was transferred to an ordinary water bath and stirred for 30 min. 1.4 L of 50 °C deionized water and 1 L of 30% hydrogen peroxide, the reactant changes from brown to yellow, and after stirring for another 12 minutes, the reactant is taken out and filtered, and the filter cake is washed with 3% hydrochloric acid and centrifuged three times, and then redispersed in deionized water to obtain a brown suspension. After dialysis for 3 days, the graphene oxide solution is obtained.

[0029] (2) N-aminoethyl-3-aminopropylmethyldimethoxysilane: purchased from Nanjing Quanxi New Materials Co., Ltd.

[0030] (3) Dragon's beard vine: purchased from Guangdong Qingping medicinal materials market, identified by the School of Traditional Chinese Medicine of Guangdong Pharmaceutical University as the dried vine stem of Dragon's beard vine of the subgenus Thick disc of the genus Bauhinia in the family Leguminosae.

[0031] (4) Electric heating wire mesh: A mesh structure composed of multiple insulated electric heating wires vertically interwoven. The diameter of the heating wire is 0.5 mm. The mesh is smaller than and connected to a rechargeable power supply.

[0032] 2. Implementation of the Experiment

[0033] Example 1

[0034] A method for preparing a heated graphene fabric, comprising the following steps:

[0035] S1. Preparing a base fabric layer: blending cotton fiber and bamboo fiber to obtain a base fabric layer, wherein the mass ratio of the cotton fiber to the bamboo fiber is 1:1, and the warp density of the base fabric layer is 200 threads / 10 cm, and the weft density is 160 threads / 10 cm.

[0036] S2, prepare electric heating layer: prepare graphene oxide fiber, adopt N-aminoethyl-3-aminopropylmethyldimethoxysilane to carry out surface grafting modification treatment, then adopt sorghum chinense extract to soak it, take treated graphene oxide fiber and cotton fiber blending (blending mass ratio 1: 2) to obtain graphene fiber layer, the warp density of graphene fiber layer is 150 roots / 10cm, and the weft density is 150 roots / 10cm, then take double-layer graphene fiber layer and lay electric heating wire mesh in the interlayer to obtain electric heating layer;

[0037] The specific operations for preparing graphene oxide fibers are as follows: preparing a spinning solution: taking a graphene oxide solution, adjusting the pH to 6, and obtaining a spinning solution; preparing protofibrils: taking the spinning solution, passing it through a 0.5 mm spinneret, and injecting it into a coagulation bath at a speed of 0.2 mL / min, and then drying to obtain protofibrils; stretching and shaping: taking the protofibrils, placing them in a nitrogen protective atmosphere furnace, controlling the temperature to 200° C., and applying tension to the protofibrils so that the fiber length stretching rate is 28%; reducing: taking the protofibrils after stretching and shaping, placing them in a hydrazine hydrate reducing agent for reduction for 1 hour, washing, and drying to obtain graphene oxide fibers.

[0038] The specific operation of the surface grafting modification treatment is as follows: N-aminoethyl-3-aminopropylmethyldimethoxysilane is dispersed in 4 times the mass of ethanol to obtain a dispersion, and then the graphene oxide fiber is immersed in the dispersion (the fiber accounts for 1 / 5 of the mass of the dispersion, the same below), ultrasonically vibrated for 40 minutes, and the graphene oxide fiber is taken out, washed, and dried.

[0039] The specific operation of the soaking treatment is: take the dried stem of the vine of the Chinese wolfberry, crush it to 120 mesh, soak it in 15 times the mass of 70% ethanol for 24 hours, then stir and extract it at 60°C for 150 minutes, filter the residue to obtain the extract, immerse the graphene oxide fiber in the extract for 1 hour (the fiber accounts for 1 / 5 of the mass of the extract, the same below), take out the graphene oxide fiber, wash and dry it.

[0040] S3. Prepare a thermal insulation protective layer: blend polyester fiber, nylon fiber and glass fiber to obtain a thermal insulation protective layer. The mass ratio of polyester fiber, nylon fiber and glass fiber is 0.5:1:1. The warp density of the thermal insulation protective layer is 180 strands / 10 cm, and the weft density is 150 strands / 10 cm.

[0041] S4. Take the prepared base fabric layer, electric heating layer, and heat-insulating protective layer and bond them in sequence to obtain the heating type graphene fabric, and use polyvinyl alcohol as the adhesive.

[0042] Example 2

[0043] A method for preparing a heated graphene fabric, comprising the following steps:

[0044] S1. Preparing a base fabric layer: blending cotton fiber and bamboo fiber to obtain a base fabric layer, wherein the mass ratio of cotton fiber to bamboo fiber is 2:1, and the warp density of the base fabric layer is 220 threads / 10 cm, and the weft density is 180 threads / 10 cm.

[0045] S2, prepare electric heating layer: prepare graphene oxide fiber, adopt N-aminoethyl-3-aminopropylmethyldimethoxysilane to carry out surface grafting modification treatment, then adopt sorghum vine extract to soak it, take treated graphene oxide fiber and cotton fiber blending (blending mass ratio 1: 1) to obtain graphene fiber layer, the warp density of graphene fiber layer is 160 roots / 10cm, and the weft density is 160 roots / 10cm, then take double-layer graphene fiber layer and lay electric heating wire mesh in the interlayer to obtain electric heating layer;

[0046] Among them, the specific operations for preparing graphene oxide fibers are as follows: preparing a spinning solution: taking a graphene oxide solution, adjusting the pH to 8, and obtaining a spinning solution; preparing protofibrils: taking the spinning solution through a 0.7 mm spinneret, and injecting it into a coagulation bath at a speed of 0.6 mL / min, and then drying to obtain protofibrils; stretching and shaping: taking the protofibrils and placing them in a nitrogen protective atmosphere furnace, controlling the temperature to 300° C., and applying tension to the protofibrils so that the fiber length stretching rate is 30%; reducing: taking the stretched and shaped protofibrils, placing them in a sodium borohydride reducing agent for reduction for 3 hours, washing and drying, and thus obtaining graphene oxide fibers.

[0047] The specific operation of the surface grafting modification treatment is as follows: dispersing N-aminoethyl-3-aminopropylmethyldimethoxysilane in 6 times the mass of ethanol to obtain a dispersion, then immersing the graphene oxide fiber in the dispersion, ultrasonically oscillating for 50 minutes, and taking out the graphene oxide fiber, washing, and drying.

[0048] The specific operation of the soaking treatment is: take the dried stem of the vine of the Chinese wolfberry, crush it to 140 mesh, soak it in 70% ethanol with 18 times the mass for 36 hours, then stir and extract it at 65°C for 120 minutes, filter the residue to obtain the extract, immerse the graphene oxide fiber in the extract for 2 hours, take out the graphene oxide fiber, wash it, and dry it.

[0049] S3. Prepare a thermal insulation protective layer: blend polyester fiber, nylon fiber and glass fiber to obtain a thermal insulation protective layer. The mass ratio of polyester fiber, nylon fiber and glass fiber is 2:1.5:1. The warp density of the thermal insulation protective layer is 200 threads / 10 cm, and the weft density is 160 threads / 10 cm.

[0050] S4. Take the prepared base fabric layer, electric heating layer, and heat-insulating protective layer and bond them in sequence to obtain the heating type graphene fabric, and use polyacrylate as the adhesive.

[0051] Example 3

[0052] A method for preparing a heated graphene fabric, comprising the following steps:

[0053] S1. Preparing a base fabric layer: blending cotton fiber and bamboo fiber to obtain a base fabric layer, wherein the mass ratio of cotton fiber to bamboo fiber is 3:1, and the warp density of the base fabric layer is 250 threads / 10 cm, and the weft density is 200 threads / 10 cm.

[0054] S2, prepare electric heating layer: prepare graphene oxide fiber, adopt N-aminoethyl-3-aminopropylmethyldimethoxysilane to carry out surface grafting modification treatment, then adopt sorghum chinense extract to soak it, take treated graphene oxide fiber and cotton fiber blending (blending mass ratio 1: 3) to obtain graphene fiber layer, the warp density of graphene fiber layer is 180 roots / 10cm, and the weft density is 180 roots / 10cm, then take double-layer graphene fiber layer and lay electric heating wire mesh in the interlayer to obtain electric heating layer;

[0055] Among them, the specific operations for preparing graphene oxide fibers are as follows: preparing a spinning solution: taking a graphene oxide solution, adjusting the pH to 10, and obtaining a spinning solution; preparing protofibrils: taking the spinning solution through a 1 mm spinneret, and injecting it into a coagulation bath at a speed of 1 mL / min, and then drying to obtain protofibrils; stretching and shaping: taking the protofibrils and placing them in a nitrogen protective atmosphere furnace, controlling the temperature to 400° C., and applying tension to the protofibrils so that the fiber length stretching rate is 32%; reducing: taking the protofibrils after stretching and shaping, placing them in a hydrobromic acid reducing agent for reduction for 5 hours, washing and drying, and thus obtaining graphene oxide fibers.

[0056] The specific operation of the surface grafting modification treatment is as follows: dispersing N-aminoethyl-3-aminopropylmethyldimethoxysilane in 8 times the mass of ethanol to obtain a dispersion, then immersing the graphene oxide fiber in the dispersion, ultrasonically oscillating for 60 minutes, and taking out the graphene oxide fiber, washing, and drying.

[0057] The specific operation of the soaking treatment is: take the dried stem of the vine of the Chinese wolfberry, crush it into 150 mesh, soak it in 20 times the mass of 70% ethanol for 48 hours, then stir and extract it at 70°C for 100 minutes, filter the residue to obtain the extract, immerse the graphene oxide fiber in the extract for 3 hours, take out the graphene oxide fiber, wash and dry it.

[0058] S3. Prepare a thermal insulation protective layer: blend polyester fiber, nylon fiber and glass fiber to obtain a thermal insulation protective layer. The mass ratio of polyester fiber, nylon fiber and glass fiber is 4:2:1. The warp density of the thermal insulation protective layer is 220 strands / 10 cm, and the weft density is 180 strands / 10 cm.

[0059] S4. Take the prepared base fabric layer, electric heating layer, and heat-insulating protective layer and bond them in sequence to obtain the heating type graphene fabric, and use epoxy resin as the adhesive.

[0060] Comparative Example 1

[0061] A method for preparing a heated graphene fabric, comprising the following steps:

[0062] S1. Preparing a base fabric layer: blending cotton fiber and bamboo fiber to obtain a base fabric layer, wherein the mass ratio of cotton fiber to bamboo fiber is 2:1, and the warp density of the base fabric layer is 220 threads / 10 cm, and the weft density is 180 threads / 10 cm.

[0063] S2, prepare electric heating layer: prepare graphene oxide fiber, adopt elastomeric extract to carry out immersion treatment, get the graphene oxide fiber after treatment and cotton fiber blending (blending mass ratio 1: 1) and obtain graphene fiber layer, the warp density of graphene fiber layer is 160 / 10cm, and the weft density is 160 / 10cm, then get double-layer graphene fiber layer and lay electric heating wire mesh in interlayer, obtain electric heating layer;

[0064] Among them, the specific operations for preparing graphene oxide fibers are as follows: preparing a spinning solution: taking a graphene oxide solution, adjusting the pH to 8, and obtaining a spinning solution; preparing protofibrils: taking the spinning solution through a 0.7 mm spinneret, and injecting it into a coagulation bath at a speed of 0.6 mL / min, and then drying to obtain protofibrils; stretching and shaping: taking the protofibrils and placing them in a nitrogen protective atmosphere furnace, controlling the temperature to 300° C., and applying tension to the protofibrils so that the fiber length stretching rate is 30%; reducing: taking the stretched and shaped protofibrils, placing them in a sodium borohydride reducing agent for reduction for 3 hours, washing and drying, and thus obtaining graphene oxide fibers.

[0065] The specific operation of the soaking treatment is: take the dried stem of the vine of the Chinese wolfberry, crush it to 140 mesh, soak it in 70% ethanol with 18 times the mass for 36 hours, then stir and extract it at 65°C for 120 minutes, filter the residue to obtain the extract, immerse the graphene oxide fiber in the extract for 2 hours, take out the graphene oxide fiber, wash it, and dry it.

[0066] S3. Prepare a thermal insulation protective layer: blend polyester fiber, nylon fiber and glass fiber to obtain a thermal insulation protective layer. The mass ratio of polyester fiber, nylon fiber and glass fiber is 2:1.5:1. The warp density of the thermal insulation protective layer is 200 threads / 10 cm, and the weft density is 160 threads / 10 cm.

[0067] S4. Take the prepared base fabric layer, electric heating layer, and heat-insulating protective layer and bond them in sequence to obtain the heating type graphene fabric, and use polyacrylate as the adhesive.

[0068] Comparative Example 2

[0069] A method for preparing a heated graphene fabric, comprising the following steps:

[0070] S1. Preparing a base fabric layer: blending cotton fiber and bamboo fiber to obtain a base fabric layer, wherein the mass ratio of cotton fiber to bamboo fiber is 2:1, and the warp density of the base fabric layer is 220 threads / 10 cm, and the weft density is 180 threads / 10 cm.

[0071] S2, prepare electric heating layer: prepare graphene oxide fiber, adopt N-aminoethyl-3-aminopropylmethyldimethoxysilane to carry out surface grafting modification treatment, take treated graphene oxide fiber and cotton fiber blending (blending mass ratio 1: 1) to obtain graphene fiber layer, the warp density of graphene fiber layer is 160 roots / 10cm, and the weft density is 160 roots / 10cm, then take double-layer graphene fiber layer and lay electric heating wire mesh in the interlayer to obtain electric heating layer;

[0072] Among them, the specific operations for preparing graphene oxide fibers are as follows: preparing a spinning solution: taking a graphene oxide solution, adjusting the pH to 8, and obtaining a spinning solution; preparing protofibrils: taking the spinning solution through a 0.7 mm spinneret, and injecting it into a coagulation bath at a speed of 0.6 mL / min, and then drying to obtain protofibrils; stretching and shaping: taking the protofibrils and placing them in a nitrogen protective atmosphere furnace, controlling the temperature to 300° C., and applying tension to the protofibrils so that the fiber length stretching rate is 30%; reducing: taking the stretched and shaped protofibrils, placing them in a sodium borohydride reducing agent for reduction for 3 hours, washing and drying, and thus obtaining graphene oxide fibers.

[0073] The specific operation of the surface grafting modification treatment is as follows: dispersing N-aminoethyl-3-aminopropylmethyldimethoxysilane in 6 times the mass of ethanol to obtain a dispersion, then immersing the graphene oxide fiber in the dispersion, ultrasonically oscillating for 50 minutes, and taking out the graphene oxide fiber, washing, and drying.

[0074] S3. Prepare a thermal insulation protective layer: blend polyester fiber, nylon fiber and glass fiber to obtain a thermal insulation protective layer. The mass ratio of polyester fiber, nylon fiber and glass fiber is 2:1.5:1. The warp density of the thermal insulation protective layer is 200 threads / 10 cm, and the weft density is 160 threads / 10 cm.

[0075] S4. Take the prepared base fabric layer, electric heating layer, and heat-insulating protective layer and bond them in sequence to obtain the heating type graphene fabric, and use polyacrylate as the adhesive.

[0076] 3. Performance Testing

[0077] (1) Heating effect:

[0078] The heated graphene fabrics prepared in Examples 1-3 and Comparative Examples 1-2 were taken and cut into 30 cm × 30 cm samples. Five positions were randomly marked on the side of the base fabric layer of each sample as temperature measuring points. After the electric heating screen was connected to the power supply for 10 seconds, the surface temperature values ​​at the five positions were read with a thermometer, and the average temperature value and variance value of the five positions on each sample were calculated. Each sample was first curled (using a cylinder with a diameter of 5 cm, connecting one edge of the sample to the cylinder wall, pulling the other opposite edge of the sample, so that the sample was completely rolled and adhered to the cylinder surface and then unfolded, and the operation was repeated 1000 times), and then extruded (using a pressing plate with the same area as the sample, driving the pressing plate to press it to the fabric surface through a driving device, controlling the pressure to 500 N, and then driving the pressing plate to separate from the fabric, and repeating the operation 1000 times). Then, the average temperature value and variance of each sample were measured and calculated again in the same way. The test results are statistically obtained in the following Tables 1-1 and 1-2.

[0079] (2) Antibacterial properties:

[0080] The heated graphene fabrics prepared in Examples 1-3 and Comparative Examples 1-2 were cut into 10 cm × 10 cm samples, and the antibacterial rate of these fabric samples was tested in accordance with GB / T 20944.2-2007 "Evaluation of Antibacterial Properties of Textiles Part 2: Absorption Method". Each sample was first curled (using a cylinder with a diameter of 5 cm, connecting one edge of the sample to the cylinder wall, pulling the other opposite edge of the sample, so that the sample was completely rolled and adhered to the cylinder surface and then unfolded, and the operation was repeated 1000 times), and then squeezed (using a pressing plate with the same area as the sample, driving the pressing plate to press it to the fabric surface through a driving device, controlling the pressure to 500 N, and then driving the pressing plate to separate from the fabric, and repeating the operation 1000 times). Then, the antibacterial rate of these fabric samples was tested again in the same way, and the test results were statistically obtained in Table 2 below.

[0081] 4. Results Analysis

[0082] Table 1-1: Test results of heating effect before treatment

[0083]

[0084] Table 1-2: Test results of heating effect after curling and extrusion

[0085]

[0086]

[0087] Table 2: Antibacterial rate test results

[0088]

[0089] As can be seen from Tables 1-1, 1-2, and 2 above, the heating-type graphene fabrics produced in Examples 1-3 of the present invention exhibited generally high temperature values ​​at all test points during the heating test, rapid heat conduction, and uniform distribution, resulting in an outstanding heating effect and no significant decline in heat after treatment. In the antibacterial test, Examples 1-3 demonstrated good antibacterial rates against all three bacteria, with no significant decline in heat after treatment. However, in Comparative Example 1, due to the lack of surface modification with N-aminoethyl-3-aminopropylmethyldimethoxysilane grafting, the post-treatment temperature values ​​were generally lower and unevenly distributed, significantly impairing the heating effect and significantly reducing the antibacterial rate. Furthermore, in Comparative Example 2, due to the lack of soaking in a vine extract solution, the antibacterial rate before treatment was also somewhat reduced, and the antibacterial rate further decreased after treatment. This demonstrates that both the surface modification with N-aminoethyl-3-aminopropylmethyldimethoxysilane grafting and soaking in a vine extract solution are essential, working synergistically to reduce the impact of wear and use on the heating and antibacterial effects.

[0090] The above-described embodiments merely illustrate several implementations of the present invention. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, and all such variations and improvements fall within the scope of protection of the present invention.

Claims

1. A method for preparing a heated graphene fabric, characterized in that the steps include: S1. Preparing a base fabric layer: blending cotton fiber and bamboo fiber to obtain a base fabric layer; S2. Preparation of an electric heating layer: preparing graphene oxide fiber, using N-aminoethyl-3-aminopropylmethyldimethoxysilane to perform surface grafting modification treatment on it, then soaking it with a vine extract, taking the treated graphene oxide fiber and cotton fiber to blend to obtain a graphene fiber layer, then taking a double-layer graphene fiber layer and laying an electric heating wire mesh in the interlayer to obtain an electric heating layer; The specific operation of preparing graphene oxide fiber is as follows: Prepare a spinning solution: take a graphene oxide solution, adjust the pH to 6-10, and obtain a spinning solution; Preparation of fibrils: taking the spinning solution through a 0.5-1 mm spinneret and injecting it into a coagulation bath at a speed of 0.2-1 mL / min, and then drying to obtain fibrils; Stretching and shaping: placing the raw fibers in a protective atmosphere furnace, controlling the temperature to 200-400°C, and applying tension to the raw fibers to make the fiber length stretching rate reach 28-32%; Reduction: Take the stretched and shaped original fibers, place them in a reducing agent for reduction for 1-5 hours, wash and dry them to obtain graphene oxide fibers; The specific operation of the surface grafting modification treatment is as follows: dispersing N-aminoethyl-3-aminopropylmethyldimethoxysilane in 4-8 times the mass of ethanol to obtain a dispersion, then immersing the graphene oxide fiber in the dispersion, ultrasonically oscillating for 40-60 minutes, taking out the graphene oxide fiber, washing, and drying; The specific operation of the soaking treatment is as follows: taking the dried stems of the vines of the Chinese truncatum, crushing them into 120-150 mesh, soaking them in 70% ethanol with a mass of 15-20 times the weight for 24-48 hours, then stirring and extracting them at 60-70°C for 100-150 minutes, filtering the residue to obtain an extract, immersing the graphene oxide fiber in the extract for 1-3 hours, taking out the graphene oxide fiber, washing it, and drying it; S3, preparing a heat-insulating protective layer: blending polyester fiber, nylon fiber and glass fiber to obtain a heat-insulating protective layer; S4. Take the prepared base fabric layer, electric heating layer, and heat-insulating protective layer and bond them in sequence to obtain the heating-type graphene fabric.

2. The method for preparing a heated graphene fabric according to claim 1, wherein: The mass ratio of cotton fiber to bamboo fiber in the base fabric layer is 1-3:

1.

3. The method for preparing a heated graphene fabric according to claim 1, wherein: The reducing agent is selected from one of hydrazine hydrate, hydrobromic acid, sodium borohydride or hydroiodic acid.

4. The method for preparing a heated graphene fabric according to claim 1, wherein: The mass ratio of polyester fiber, nylon fiber and glass fiber in the heat insulation protective layer is 0.5-4:1-2:

1.

5. The method for preparing a heated graphene fabric according to claim 1, wherein: The base fabric layer, the electric heating layer and the heat-insulating protective layer are all bonded together by an adhesive, and the adhesive is selected from one of polyvinyl alcohol, polyacrylate, epoxy resin or carboxymethyl cellulose.

6. The method for preparing a heated graphene fabric according to claim 1, wherein: The warp density of the base fabric layer is 200-250 threads / 10cm, and the weft density is 160-200 threads / 10cm. The warp density of the graphene fiber layer is 150-180 threads / 10cm, and the weft density is 150-180 threads / 10cm. The warp density of the thermal insulation protective layer is 180-220 threads / 10cm, and the weft density is 150-180 threads / 10cm.

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