A water-washable self-controlled temperature conductive graphene fabric, its preparation method and application

Abstract

The present invention belongs to the technical field of heat dissipation functional fabrics. The present invention discloses a washable self-controlled temperature conductive graphene fabric, its preparation method and application. The washable self-controlled temperature conductive graphene fabric of the present invention is obtained by weaving high thermal conductivity triacetate fibers prepared from raw materials such as high thermal conductivity graphene additives and high thermal conductivity cellulose fibers prepared from raw materials such as high thermal conductivity graphene additives. The washable self-controlled temperature conductive graphene fabric of the present invention can achieve self-controlled temperature, reduce the body surface temperature, has the characteristics of being washable, high in design degree and comfortable to wear, can solve the problems existing in the existing self-controlled temperature fabrics, and meet the application of higher performance heat dissipation functional fabrics.

Description

Technical Field

[0001] The present invention relates to the technical field of heat-dissipating functional fabrics, and particularly to a water-washable self-controlled temperature-conducting graphene fabric, a preparation method thereof and an application thereof. Background Art

[0002] With the global warming, the outdoor thermal comfort has become increasingly important for improving the health of outdoor personnel. By improving the thermal conductivity coefficient, breathability and hygroscopicity of fabrics to prepare self-controlled temperature fabrics to reduce the body surface temperature of the human body has been increasingly emphasized. At the same time, with the improvement of living standards, people's requirements for clothing have gradually shifted from the initial practicality such as warmth retention and protection to functionality and comfort. In hot summer or during activities with a large amount of exercise, the human body will sweat a lot, and at this time, the clothing is required to have both wearability and the function of moisture absorption and heat dissipation. However, the existing self-controlled temperature fabrics have problems such as inability to significantly reduce the body surface temperature, low wearing comfort, the color of the fabric being black, low designability, and non-water-washable. Therefore, there is an urgent need in this field to develop a heat-dissipating functional fabric that is water-washable, has strong designability, high wearing comfort, and can significantly reduce the body surface temperature. Summary of the Invention

[0003] The purpose of the present invention is to provide a water-washable self-controlled temperature-conducting graphene fabric, a preparation method thereof and an application thereof, so as to solve the problems of the existing self-controlled temperature fabrics, such as inability to significantly reduce the body surface temperature, low wearing comfort, the color of the fabric being black, low designability, and non-water-washable.

[0004] In order to achieve the above purpose, the present invention adopts the following technical solutions:

[0005] The present invention provides a preparation method of a water-washable self-controlled temperature-conducting graphene fabric, comprising the following steps:

[0006] (1) Preparation of a high thermal conductivity graphene additive: Mix graphene, a high thermal conductivity powder, a coupling agent solution and ethanol and react to obtain a high thermal conductivity graphene additive;

[0007] (2) Preparation of a high thermal conductivity triacetate fiber: Mix the high thermal conductivity graphene additive, acetic acid flakes, acetone, a filter aid and water, and obtain a high thermal conductivity triacetate fiber by dry spinning;

[0008] (3) Preparation of a high thermal conductivity cellulose fiber: Dissolve pulp in an aqueous solution of N-methylmorpholine-N-oxide to obtain a cellulose solution, mix the cellulose solution and the high thermal conductivity graphene additive, and obtain a high thermal conductivity cellulose fiber by dry-wet spinning;

[0009] (4) Preparation of a water-washable self-controlled temperature-conducting graphene fabric: Weave the high thermal conductivity triacetate fiber and the high thermal conductivity cellulose fiber to obtain a water-washable self-controlled temperature-conducting graphene fabric.

[0010] Preferably, in step (1), the mass-volume ratio of the graphene, the high thermal conductivity powder, the coupling agent solution, and the ethanol is 1-1.5 g: 55-60 g: 50-60 mL: 150-200 mL; the coupling agent solution is an aqueous solution of a silane coupling agent; the volume fraction of the coupling agent solution is 3-7%; the high thermal conductivity powder is one or more of boron nitride, silicon carbide, aluminum powder, and alumina; the particle size of the high thermal conductivity powder is 60-90 nm.

[0011] Preferably, in step (1), the mixing includes the following steps: mixing the graphene, the high thermal conductivity powder, and the ethanol, and then mixing with the coupling agent solution; the reaction temperature is 30-50 °C, and the reaction time is 2-3 h.

[0012] Preferably, in step (2), the mass ratio of the high thermal conductivity graphene additive, the acetate chip, the acetone, the filter aid, and the water is 6-9: 20-30: 70-80: 0.1-0.5: 20-30; the mass fraction of the combined acid in the acetate chip is 53-56%; the filter aid is one or more of diatomaceous earth, perlite, cellulose, and asbestos; the temperature of the dry spinning is 75-80 °C.

[0013] Preferably, in step (3), the mass fraction of the cellulose solution is 7-9%; the mass ratio of the cellulose solution to the high thermal conductivity graphene additive is 80-100: 0.2-0.3; the mass fraction of the N-methylmorpholine-N-oxide aqueous solution is 86-87%.

[0014] Preferably, in step (3), the vacuum degree of the dissolution is -0.9 to -0.8 bar, the dissolution temperature is 112-120 °C, and the dissolution time is 1-2 h; the mixing time is 10-15 min; in the dry-wet spinning, the flow rate of the spinning solution is 0.5-1.5 m / min, the temperature of the spinneret is 115-120 °C, and the temperature of the aqueous spinning bath is 20-25 °C.

[0015] Preferably, in steps (2) and (3), before dry spinning and dry-wet spinning, the mixtures obtained by respective mixing are sequentially subjected to pressure filtration and filtration.

[0016] Preferably, in step (4), the textile structure includes piqué, plain stitch, horizontal stripe, and pleat structures.

[0017] The present invention also provides a wash-resistant self-controlled temperature conductive graphene fabric prepared by the preparation method of the wash-resistant self-controlled temperature conductive graphene fabric.

[0018] The present invention also provides the application of the wash-resistant self-controlled temperature conductive graphene fabric in a heat dissipation functional fabric.

[0019] As can be seen from the above technical solutions, compared with the prior art, the beneficial effects of the present invention are as follows:

[0020] The washable self-regulating temperature conductive graphene fabric of the present invention can achieve self-regulating temperature, reduce the body surface temperature, has the characteristics of washability, high design degree and comfortable wearing, and can solve the problems existing in the existing self-regulating temperature fabrics. Specific embodiments

[0021] The present invention provides a method for preparing a washable self-regulating temperature conductive graphene fabric, which comprises the following steps:

[0022] (1) Preparation of a highly thermally conductive graphene additive: Graphene, a highly thermally conductive powder, a coupling agent solution and ethanol are mixed and reacted to obtain a highly thermally conductive graphene additive;

[0023] (2) Preparation of highly thermally conductive triacetate fiber: A highly thermally conductive graphene additive, acetic acid flakes, acetone, a filter aid and water are mixed, and dry spinning is carried out to obtain highly thermally conductive triacetate fiber;

[0024] (3) Preparation of highly thermally conductive cellulose fiber: Pulp is dissolved in an aqueous solution of N-methylmorpholine-N-oxide to obtain a cellulose solution. The cellulose solution is mixed with a highly thermally conductive graphene additive, and dry-wet spinning is carried out to obtain highly thermally conductive cellulose fiber;

[0025] (4) Preparation of a washable self-regulating temperature conductive graphene fabric: The highly thermally conductive triacetate fiber and the highly thermally conductive cellulose fiber are woven to obtain a washable self-regulating temperature conductive graphene fabric.

[0026] In step (1), the mass-volume ratio of the graphene, the highly thermally conductive powder, the coupling agent solution and ethanol is preferably 1-1.5 g: 55-60 g: 50-60 mL: 150-200 mL, and more preferably 1.2-1.4 g: 56-58 g: 52-56 mL: 160-180 mL; the coupling agent solution is preferably an aqueous solution of a silane coupling agent; the volume fraction of the coupling agent solution is preferably 3-7%, and more preferably 4-6%; the silane coupling agent is preferably one or more of KH550, KH560, KH570 and Z6040; the highly thermally conductive powder is preferably one or more of boron nitride, silicon carbide, aluminum powder and alumina; the particle size of the highly thermally conductive powder is preferably 60-90 nm, and more preferably 70-80 nm.

[0027] In step (1) of the present invention, the mixing comprises the following steps: Graphene, a highly thermally conductive powder and ethanol are mixed and then mixed with the coupling agent solution;

[0028] Among them, the mixing is preferably ultrasonic mixing. The power of the ultrasonic wave is preferably 300 - 400 W independently, and more preferably 320 - 360 W; the mixing time is preferably 1 - 2 h independently, and more preferably 1.5 h; the reaction temperature is preferably 30 - 50 °C, and more preferably 35 - 45 °C; the reaction time is preferably 2 - 3 h, and more preferably 2.5 h.

[0029] In step (1) of the present invention, the preparation of the graphene includes the following steps: expanding the flake graphite sequentially, intercalating and separating, and freeze-drying to obtain graphene;

[0030] Among them, the particle size of the flake graphite is preferably 100 - 120 μm, and more preferably 105 - 115 μm; the intercalation modifier used for intercalation and separation is preferably sodium dodecylbenzenesulfonate; the temperature of freeze-drying is preferably -20 - -15 °C, and more preferably -18 - -16 °C; the time of freeze-drying is preferably 4 - 6 h, and more preferably 5 h.

[0031] The thermal performance of the high thermal conductivity graphene additive of the present invention can be significantly improved. After the modification treatment with the coupling agent, the dispersion of graphene is well improved, and the generation of thermal resistance is also reduced. The presence of the high thermal conductivity powder promotes the dispersion of graphene on the one hand, improves the thermal conductivity of the fiber, and on the other hand improves the designability of the washable self-controlled temperature thermal conductive graphene fabric.

[0032] In step (2) of the present invention, the mass ratio of the high thermal conductivity graphene additive, acetate chips, acetone, filter aid, and water is preferably 6 - 9:20 - 30:70 - 80:0.1 - 0.5:20 - 30, and more preferably 7 - 8:23 - 29:72 - 75:0.2 - 0.4:21 - 28; the mass fraction of the combined acid in the acetate chips is preferably 53 - 56%, and more preferably 54 - 55%; the filter aid is preferably one or more of diatomaceous earth, perlite, cellulose, and asbestos; the temperature of dry spinning is preferably 75 - 80 °C, and more preferably 76 - 79 °C.

[0033] In step (2) of the present invention, the mixing is preferably stirring mixing, and the stirring rate is preferably 500 - 700 r / min, and more preferably 600 r / min.

[0034] In step (2) of the present invention, during the dry spinning process, the spinning slurry is heated by a preheater, and the heating temperature is preferably 75 - 80 °C. When the filament strand extruded from the spinneret enters the spinning duct, the acetone in the filament strand quickly volatilizes under the action of hot air when passing through the spinning duct, and the filament strand solidifies and forms.

[0035] In step (2) of the present invention, acetone is used to dissolve the acetate chips and is completely recovered later; water serves to reduce the viscosity of the resulting slurry; the filter aid is used for filtering the resulting slurry to remove impurities.

[0036] In step (2) of the present invention, after dry spinning is completed, the obtained product is successively subjected to oiling, drawing, crimping, drying, and winding treatments to obtain high thermal conductivity triacetate fiber; the purpose of oiling is to endow the nascent fiber with good antistatic property, smoothness, and cohesion, and ensure good spinnability during subsequent processing; the purpose of drawing is to perfect the fiber molecular structure and improve fiber strength and structural stability; crimping can enhance the cohesion between fibers; the purpose of drying is to remove the solvent contained in the fiber and has a heat setting effect; the drying temperature is preferably 75-80°C, more preferably 76-78°C; the purpose of winding is for packaging.

[0037] In step (3) of the present invention, the pulp is preferably composed of wood pulp, cotton pulp, bamboo pulp, and grass pulp.

[0038] In step (3) of the present invention, before the pulp is dissolved, the pulp is subjected to ball milling activation treatment; the rotation speed of the ball milling activation treatment is preferably 950-1050 r / min, more preferably 980-1020 r / min; the time of the ball milling activation treatment is preferably 20-50 min, more preferably 30-40 min.

[0039] In step (3) of the present invention, the N-methylmorpholine-N-oxide aqueous solution is selected from the 50% N-methylmorpholine-N-oxide aqueous solution of German Degussa Company, the 50% N-methylmorpholine-N-oxide aqueous solution of German BASF AG Company, the 50% N-methylmorpholine-N-oxide aqueous solution of British Texaco Company, or the 50% N-methylmorpholine-N-oxide aqueous solution of Indian A&P Company; the mass fraction of the cellulose solution is preferably 7-9%, more preferably 7.5-8.5%; the mass ratio of the cellulose solution to the high thermal conductivity graphene additive is preferably 80-100:0.2-0.3, more preferably 85-95:0.25-0.28; the mass fraction of the N-methylmorpholine-N-oxide aqueous solution is preferably 86-87%, more preferably 86.2-86.7%.

[0040] In step (3) of the present invention, the vacuum degree for dissolution is preferably -0.9 to -0.8 bar, more preferably -0.85 bar; the temperature for dissolution is preferably 112 to 120 °C, more preferably 115 to 118 °C; the time for dissolution is preferably 1 to 2 h, more preferably 1.5 h; the time for mixing is preferably 10 to 15 min, more preferably 12 to 14 min; in dry-wet spinning, the flow rate of the spinning solution is preferably 0.5 to 1.5 m / min, more preferably 1 to 1.2 m / min; the temperature of the spinneret is preferably 115 to 120 °C, more preferably 116 to 119 °C; the temperature of the aqueous spinning bath is preferably 20 to 25 °C, more preferably 22 to 24 °C.

[0041] In step (3) of the present invention, after dry-wet spinning is completed, the obtained fibers are successively washed and dried; the reagent used for washing is preferably water; the temperature for drying is preferably 70 to 110 °C, more preferably 80 to 100 °C.

[0042] In steps (2) and (3) of the present invention, before dry spinning and dry-wet spinning, the mixtures obtained by respective mixing are successively pressure-filtered and filtered; the pressure filtration and filtration include the following steps: the mixtures obtained by respective mixing are respectively sent to a multi-stage plate-frame filter press for pressure filtration and quantitatively fed into a candle filter for filtration by a metering pump; the purpose of filtration is to further remove impurities and improve the quality of the slurry.

[0043] In step (4) of the present invention, the textile structure is preferably including piqué, plain stitch, horizontal stripe and pleat.

[0044] The present invention also provides a wash-resistant self-controlled temperature conductive graphene fabric prepared by the preparation method of the wash-resistant self-controlled temperature conductive graphene fabric.

[0045] In the present invention, the high thermal conductivity cellulose fiber is a water-absorbing fiber, while the high thermal conductivity triacetate fiber is a hydrophobic fiber. This hydrophilic-hydrophobic side-by-side structure enables the wash-resistant self-controlled temperature conductive graphene fabric to absorb moisture and expand when encountering sweat, promoting radiative conduction cooling, and when there is no sweat, it can also maintain the breathability of the fabric to promote convective cooling, so as to maximize the efficiency of thermal management; the fabric made of high thermal conductivity triacetate fiber is easy to finish, wrinkle-resistant, dimensionally stable, easy to dry, and maintains a stable shape, so that the wash-resistant self-controlled temperature conductive graphene fabric will not deform after moisture absorption.

[0046] The present invention also provides the application of the wash-resistant self-controlled temperature conductive graphene fabric in a heat dissipation functional fabric.

[0047] In the present invention, the heat dissipation functional fabric includes but is not limited to sunshade and cooling cloth, greenhouse cooling cloth, cooling clothes, cooling sheets and cooling quilt covers.

[0048] The technical solution provided by the present invention will be described in detail below in conjunction with embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0049] The preparation of graphene used hereinafter includes the following steps: Dilute 50 mL of 98 wt% concentrated sulfuric acid to 80 wt% and cool it to room temperature, then mix it with 23 mL of nitric acid to form a mixed acid. Add 10 g of flake graphite and 2.2 g of potassium permanganate under the condition of stirring at 100 r / min. After reacting for 50 min, wash it with water and filter it by suction. Then add hydrogen peroxide with a volume fraction of 30% until no more gas is generated, wash it with water and filter it by suction again. Dry it at 60 °C for 4 h, and then perform an expansion treatment at 900 °C to obtain expanded graphite; Intercalate and separate the expanded graphite under the action of sodium dodecylbenzenesulfonate, and finally perform freeze-drying at -18 °C for 5 h to obtain graphene.

[0050] The pulp used hereinafter is composed of 30 parts of wood pulp, 40 parts of cotton pulp, 15 parts of bamboo pulp and 15 parts of grass pulp.

[0051] Example 1

[0052] (1) Preparation of high thermal conductivity graphene additive: Mix 1.2 g of graphene, 55 g of boron nitride with a particle size of 90 nm and 200 mL of absolute ethanol, and perform ultrasonic dispersion at a power of 360 W for 2 h to obtain a mixed solution. Mix the mixed solution with 60 mL of an aqueous solution of KH550 silane coupling agent with a volume fraction of 5%, and react at 35 °C for 2.5 h to obtain a high thermal conductivity graphene additive;

[0053] (2) Preparation of high thermal conductivity triacetate fiber: Add 7 g of high thermal conductivity graphene additive, 25 g of acetate flakes with a combined acid mass fraction of 54%, 70 g of acetone, 0.3 g of diatomite and 20 g of water to a dissolving device. The dissolving device is equipped with a stirring device. After fully dissolving at a rotation speed of 500 r / min for 50 min, send the obtained slurry to a multi-stage plate and frame filter press, and quantitatively feed it (the addition amount is 2 / 3 of the volume of the candle filter) into the candle filter by a metering pump to further filter out impurities and improve the quality of the slurry; Then heat it to 75 °C through a preheater and extrude it through a spinneret into a spinning channel; The acetone in the filament strand rapidly volatilizes under the action of hot air mixed with water vapor and nitrogen when passing through the spinning channel, and the filament strand is solidified and formed; Then, oiling, stretching, drying at 75 °C and winding are carried out in sequence to obtain high thermal conductivity triacetate fiber;

[0054] (3) Preparation of highly thermally conductive cellulose fiber: The pulp was ball-milled and activated at a rotational speed of 950 r / min for 40 min. The treated pulp and an aqueous solution of N-methyl morpholine-N-oxide with a mass fraction of 86% (obtained by diluting a 50% aqueous solution of N-methyl morpholine-N-oxide from Degussa, Germany with water) were dissolved at -0.9 bar and 112 °C for 1.5 h to obtain a cellulose solution with a mass fraction of 8%. After adding 0.3 g of highly thermally conductive graphene additive to 90 g of the cellulose solution and mixing for 15 min, it was sent to a multi-stage plate-and-frame filter press for pressure filtration, quantitatively fed into a candle filter by a metering pump for filtration to further remove impurities, and then spun by a wet-dry spinning method on a spinning machine equipped with a spinneret with 18 orifices. Then, the obtained fiber was washed with water and dried at 80 °C to obtain highly thermally conductive cellulose fiber; in the wet-dry spinning process, the flow rate of the spinning solution was 1 m / min, the temperature of the spinneret was 115 °C, the temperature of the aqueous spinning bath was 20 °C, and the aqueous spinning bath was water.

[0055] (4) Preparation of wash-resistant self-regulating temperature thermally conductive graphene fabric: Using highly thermally conductive cellulose fiber and highly thermally conductive triacetate fiber, it was woven with 4 kinds of tissues including piqué, plain stitch, horizontal stripe, and pleat to obtain a wash-resistant self-regulating temperature thermally conductive graphene fabric.

[0056] Cover the wash-resistant self-regulating temperature thermally conductive graphene fabric obtained in this example on the simulated skin, suspend it outdoors, the outdoor temperature is 40 °C, hang for 2 h, record the surface temperature of the fabric and the temperature between the fabric and the simulated skin.

[0057] After the wash-resistant self-regulating temperature thermally conductive graphene fabric obtained in this example was washed 200 times in a washing machine (each washing time was 30 min), it was covered on the simulated skin, suspended outdoors, the outdoor temperature was 40 °C, hung for 2 h, and the surface temperature of the fabric was recorded as 41 °C, and the temperature between the fabric and the simulated skin was 31 °C. It shows that washing will not cause the temperature control effect of the wash-resistant self-regulating temperature thermally conductive graphene fabric to decline, and the wash-resistant self-regulating temperature thermally conductive graphene fabric can achieve wash resistance.

[0058] Example 2

[0059] (1) Preparation of highly thermally conductive graphene additive: 1.3 g of graphene, 58 g of aluminum powder with a particle size of 60 nm, and 180 mL of absolute ethanol were mixed and ultrasonically dispersed at a power of 360 W for 1.5 h to obtain a mixed solution. The mixed solution was mixed with 55 mL of an aqueous solution of KH560 silane coupling agent with a volume fraction of 2% and reacted at 40 °C for 3 h to obtain a highly thermally conductive graphene additive;

[0060] (2) Preparation of highly thermally conductive triacetate fiber: Add 9 g of highly thermally conductive graphene additive, 28 g of acetate flakes with a combined acid mass fraction of 53%, 75 g of acetone, 0.5 g of diatomite, and 25 g of water to a dissolving device equipped with a stirring device. After fully dissolving at a rotation speed of 500 r / min for 55 min, send the obtained slurry to a multi-stage plate and frame filter press, and quantitatively feed it (the addition amount is 2 / 3 of the volume of the candle filter) into the candle filter by a metering pump to further filter out impurities and improve the quality of the slurry; then heat it to 75 °C through a preheater and extrude it through a spinneret into a spinning duct; the acetone in the filament rapidly volatilizes under the action of hot air mixed with water vapor and nitrogen when passing through the spinning duct, and the filament solidifies and takes shape; then successively perform oiling, stretching, drying at 80 °C, and winding to obtain highly thermally conductive triacetate fiber;

[0061] (3) Preparation of highly thermally conductive cellulose fiber: Ball mill and activate the pulp at 1000 r / min for 40 min. Dissolve the treated pulp and an aqueous solution of N-methylmorpholine-N-oxide with a mass fraction of 87% (obtained by diluting a 50% aqueous solution of N-methylmorpholine-N-oxide from Texaco, UK, with water) at -0.8 bar and 112 °C for 1.5 h to obtain a cellulose solution with a mass fraction of 8%; after adding 0.2 g of highly thermally conductive graphene additive to 80 g of the cellulose solution and mixing for 15 min, send it to a multi-stage plate and frame filter press for pressure filtration, quantitatively feed it into a candle filter by a metering pump for filtration to further filter out impurities, and then spin it by the dry-wet spinning method on a spinning machine equipped with a spinneret with 18 orifices. Then wash the obtained fiber with water and dry it at 10 °C to obtain highly thermally conductive cellulose fiber; in the dry-wet spinning process, the flow rate of the spinning solution is 1 m / min, the temperature of the spinneret is 118 °C, the temperature of the aqueous spinning bath is 23 °C, and the aqueous spinning bath is water.

[0062] (4) Preparation of washable self-controlled temperature thermally conductive graphene fabric: Use highly thermally conductive cellulose fiber and highly thermally conductive triacetate fiber to weave with 4 kinds of tissues including piqué, plain stitch, horizontal stripe, and pleat to obtain a washable self-controlled temperature thermally conductive graphene fabric.

[0063] Cover the washable self-controlled temperature thermally conductive graphene fabric obtained in this example on a simulated skin, suspend it outdoors, the outdoor temperature is 40 °C, hang it for 2 h, record the surface temperature of the fabric and the temperature between the fabric and the simulated skin.

[0064] Example 3

[0065] (1) Preparation of high thermal conductivity graphene additive: 1.5 g of graphene, 60 g of silicon carbide with a particle size of 80 nm, and 150 mL of absolute ethanol were mixed and ultrasonically dispersed for 1 h at a power of 380 W to obtain a mixed solution. The mixed solution was mixed with 58 mL of an aqueous solution of KH570 silane coupling agent with a volume fraction of 2% and reacted at 45 °C for 3 h to obtain a high thermal conductivity graphene additive;

[0066] (2) Preparation of high thermal conductivity triacetate fiber: 6 g of high thermal conductivity graphene additive, 22 g of acetate flakes with a combined acid mass fraction of 53%, 70 g of acetone, 0.5 g of perlite, and 28 g of water were added to a dissolving device equipped with a stirring device. After being fully dissolved at a rotation speed of 700 r / min for 50 min, the obtained slurry was sent to a multi-stage plate and frame filter press and quantitatively fed (the addition amount was 2 / 3 of the volume of the candle filter) into the candle filter by a metering pump to further filter out impurities and improve the quality of the slurry; then it was heated to 75 °C through a preheater and extruded through a spinneret into a spinning channel; the acetone in the filament bundle quickly volatilized under the action of hot air mixed with water vapor and nitrogen when passing through the spinning channel, and the filament bundle was solidified and formed; then it was oiled, stretched, dried at 78 °C, and wound in sequence to obtain high thermal conductivity triacetate fiber;

[0067] (3) Preparation of high thermal conductivity cellulose fiber: The pulp was ball-milled and activated at 1050 r / min for 20 min. The treated pulp and an aqueous solution of N-methylmorpholine-N-oxide with a mass fraction of 86% (obtained by diluting a 50% aqueous solution of N-methylmorpholine-N-oxide from the British Texaco Company with water) were dissolved at -0.9 bar and 115 °C for 1.5 h to obtain a cellulose solution with a mass fraction of 8%; 0.3 g of high thermal conductivity graphene additive was added to 95 g of cellulose solution and mixed for 12 min, then sent to a multi-stage plate and frame filter press for pressure filtration, quantitatively fed into a candle filter by a metering pump for filtration to further filter out impurities, and then spun by a wet-dry spinning method on a spinning machine with a spinneret having 18 orifices. Then the obtained fiber was washed with water and dried at 90 °C to obtain high thermal conductivity cellulose fiber; in the wet-dry spinning process, the flow rate of the spinning solution was 1 m / min, the temperature of the spinneret was 120 °C, the temperature of the aqueous spinning bath was 25 °C, and the aqueous spinning bath was water.

[0068] (4) Preparation of washable self-controlled temperature conductive graphene fabric: Using high thermal conductivity cellulose fiber and high thermal conductivity triacetate fiber, it was woven with 4 kinds of tissues including piqué, plain stitch, horizontal stripe, and pleat to obtain a washable self-controlled temperature conductive graphene fabric.

[0069] Cover the washable self-controlled temperature conductive graphene fabric obtained in this example on a simulated skin, suspend it outdoors, the outdoor temperature is 40 °C, hang it for 2 h, record the surface temperature of the fabric and the temperature between the fabric and the simulated skin.

[0070] Comparative Example 1

[0071] The high thermal conductivity cellulose fibers and triacetate fibers obtained in Example 1 were woven into a fabric by four types of weaves: piqué, plain stitch, stripe, and pleat

[0072] The fabric obtained in this comparative example was covered on a simulated skin and suspended outdoors. The outdoor temperature was 40°C and it was hung for 2 h. The surface temperature of the fabric and the temperature between the fabric and the simulated skin were recorded.

[0073] Comparative Example 2

[0074] Cotton cloth was covered on a simulated skin and suspended outdoors. The outdoor temperature was 40°C and it was hung for 2 h. The surface temperature of the fabric and the temperature between the fabric and the simulated skin were recorded.

[0075] The test results obtained in Examples 1 to 3 and Comparative Examples 1 to 2 are shown in Table 1.

[0076] Table 1 Test results obtained in Examples 1 to 3 and Comparative Examples 1 to 2

[0077] Test sample Fabric surface temperature / °C Temperature between fabric and simulated skin / °C Example 1 40 31 Example 2 39 35 Example 3 40 32 Comparative example 1 40 38 Comparative example 2 41 42

[0078] As can be seen from Table 1, the washable self-controlled temperature thermal conductive graphene fabric obtained in the present invention can achieve self-controlled temperature, reduce the body surface temperature, and improve the wearing comfort.

[0079] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A preparation method of a water-washable self-controlled temperature conductive graphene fabric, characterized in that It includes the following steps: (1) Preparation of high thermal conductivity graphene additive: Graphene, high thermal conductivity powder, coupling agent solution and ethanol are mixed and reacted to obtain the high thermal conductivity graphene additive; (2) Preparation of high thermal conductivity triacetate fiber: The high thermal conductivity graphene additive, acetate flakes, acetone, filter aid and water are mixed and dry-spun to obtain the high thermal conductivity triacetate fiber; (3) Preparation of high thermal conductivity cellulose fiber: Pulp is dissolved in an aqueous solution of N-methylmorpholine-N-oxide to obtain a cellulose solution. The cellulose solution is mixed with the high thermal conductivity graphene additive and wet-dry spun to obtain the high thermal conductivity cellulose fiber; (4) Preparation of washable self-controlled temperature thermal conductive graphene fabric: The high thermal conductivity triacetate fiber and the high thermal conductivity cellulose fiber are woven to obtain the washable self-controlled temperature thermal conductive graphene fabric; In the step (1), the mixing includes the following steps: Graphene, high thermal conductivity powder and ethanol are mixed and then mixed with the coupling agent solution; In the step (3), the dissolution temperature is 112-120 °C.

2. The preparation method of the washable self-controlled temperature conductive graphene fabric according to claim 1, characterized in that, In step (1), the mass-volume ratio of the graphene, high thermal conductivity powder, coupling agent solution and ethanol is 1-1.5 g:55-60 g:50-60 mL:150-200 mL; the coupling agent solution is an aqueous solution of a silane coupling agent; the volume fraction of the coupling agent solution is 3-7%; the high thermal conductivity powder is one or more of boron nitride, silicon carbide, aluminum powder and alumina; the particle size of the high thermal conductivity powder is 60-90 nm.

3. The preparation method of the washable self-controlled temperature conductive graphene fabric according to claim 2, characterized in that, In step (1), the reaction temperature is 30-50 °C and the reaction time is 2-3 h.

4. The preparation method of the washable self-controlled temperature conductive graphene fabric according to any one of claims 1 to 3, characterized in that, In step (2), the mass ratio of the high thermal conductivity graphene additive, acetate flakes, acetone, filter aid and water is 6-9:20-30:70-80:0.1-0.5:20-30; the mass fraction of the combined acid in the acetate flakes is 53-56%; the filter aid is one or more of diatomite, perlite, cellulose and asbestos; the dry-spinning temperature is 75-80 °C.

5. The preparation method of the washable self-controlled temperature conductive graphene fabric according to claim 4, wherein, In step (3), the mass fraction of the cellulose solution is 7-9%; the mass ratio of the cellulose solution and the high thermal conductivity graphene additive is 80-100:0.2-0.3; the mass fraction of the aqueous solution of N-methylmorpholine-N-oxide is 86-87%.

6. The preparation method of the washable self-controlled temperature conductive graphene fabric according to claim 5, characterized in that, In step (3), the vacuum degree of the dissolution is -0.9 to -0.8 bar and the dissolution time is 1-2 h; the mixing time is 10-15 min; in the wet-dry spinning, the flow rate of the spinning solution is 0.5-1.5 m / min, the temperature of the spinneret is 115-120 °C, and the temperature of the aqueous spinning bath is 20-25 °C.

7. The preparation method of the washable self-controlled temperature conductive graphene fabric according to claim 1, 5 or 6, characterized in that, In steps (2) and (3), before dry-spinning and wet-dry spinning, the mixtures obtained by respective mixing are sequentially pressure-filtered and filtered.

8. The preparation method of the washable self-controlled temperature conductive graphene fabric according to claim 7, characterized in that, In step (4), the woven fabric structure includes piqué, plain stitch, horizontal stripe and pleat structures.

9. A washable self-controlled temperature thermal conductive graphene fabric prepared by the preparation method of the washable self-controlled temperature thermal conductive graphene fabric according to any one of claims 1 to 8.

10. Application of the washable self-controlled temperature thermal conductive graphene fabric according to claim 9 in a heat dissipation functional fabric.