Fabric with electromagnetic shielding function and preparation method thereof

Abstract

This invention discloses a fabric with electromagnetic shielding function and its preparation method, relating to the field of textile materials technology. The electromagnetic shielding fabric prepared by this invention comprises, from the inside out: a fabric base layer and an electromagnetic shielding layer; first, graphene, diethylene glycol, and resin are mixed to prepare a graphene slurry; then, reduced graphene oxide, a thickener, and water are mixed to prepare a reduced graphene oxide slurry; subsequently, the graphene slurry and the reduced graphene oxide slurry are mixed to prepare a graphene / reduced graphene oxide composite slurry; then, the graphene / reduced graphene oxide composite slurry is coated onto the plasma-treated fabric base layer and shaped; wherein, the resin is an epoxy resin obtained by reacting epichlorohydrin and 2,3-dicyanohydroquinone; the thickener is amino-modified aluminum silicate nanofibers; the electromagnetic shielding fabric prepared by this invention exhibits good washability, good abrasion resistance, and good electromagnetic shielding performance.

Description

Technical Field

[0001] This invention relates to the field of textile materials technology, specifically to a fabric with electromagnetic shielding function and its preparation method. Background Technology

[0002] With the continuous development of radar detection technology, radar technology has been widely applied in ground warfare. Advanced ground surveillance radars are readily available on the international arms market, and these devices are characterized by high efficiency, convenience, and a high degree of automation, making them difficult for soldiers to evade on the battlefield. Therefore, there is a need for a fabric with electromagnetic shielding capabilities to manufacture individual radar stealth combat uniforms.

[0003] Existing electromagnetic shielding fabrics typically have a layer of electromagnetic shielding material coated on the fabric base. However, this material is easily peeled off after prolonged washing. Therefore, there is an urgent need for a fabric with both good electromagnetic shielding performance and good washability. Summary of the Invention

[0004] Based on the above background technology, the purpose of this invention is to provide a fabric with electromagnetic shielding function and its preparation method.

[0005] The present invention adopts the following technical solution:

[0006] A fabric with electromagnetic shielding function is obtained by coating a graphene / reduced graphene oxide composite slurry onto a base layer after plasma surface treatment and then shaping it. The graphene / reduced graphene oxide composite slurry is prepared by mixing graphene slurry and reduced graphene oxide slurry. The graphene slurry is prepared by mixing graphene, diethylene glycol, and resin. The reduced graphene oxide slurry is prepared by mixing reduced graphene oxide, thickener, and water.

[0007] Furthermore, the base layer of the fabric is knitted from cotton fiber, polyester fiber, and spandex fiber.

[0008] Furthermore, the resin is an epoxy resin obtained by reacting epichlorohydrin and 2,3-dicyanohydroquinone.

[0009] Furthermore, the thickener is aminated aluminum silicate nanofiber.

[0010] Furthermore, a method for preparing a fabric with electromagnetic shielding function includes the following preparation steps:

[0011] (1) Preparation of graphene slurry: Mix cake graphene and diethylene glycol at a mass ratio of 1:1.8 to 1:2 and stir at 3000 to 4000 r / min for 1 to 3 h. Then add epoxy resin at 0.2 to 0.3 times the mass of cake graphene and stir at 600 to 800 r / min for 20 to 40 min to obtain graphene slurry.

[0012] (2) Preparation of reduced graphene oxide slurry: Reduced graphene oxide and thickener, amino-modified aluminum silicate nanofibers, were mixed at a mass ratio of 1:0.009 to 1:0.011 and stirred at 60 to 80 r / min for 20 to 30 min. Then, 0.2 to 0.4 times the mass of the reduced graphene oxide was added to deionized water and stirred at 1600 to 1800 r / min for 1 to 3 h to obtain the reduced graphene oxide slurry.

[0013] (3) Preparation of graphene / reduced graphene oxide composite slurry: Graphene slurry and reduced graphene oxide slurry are mixed at a mass ratio of 1:0.8 to 1:1.2 and stirred at 600 to 800 r / min for 3 to 5 h to obtain graphene / reduced graphene oxide composite slurry.

[0014] (4) Preparation of fabric with electromagnetic shielding function: A 0.6-1 mm thick graphene / reduced graphene oxide composite slurry is uniformly coated on the surface of the fabric base after plasma surface treatment, and then placed in a high temperature setting machine and set at 110-130℃ at a speed of 10-30 m / min to obtain fabric with electromagnetic shielding function.

[0015] Furthermore, the reduced graphene oxide is prepared by reducing graphene oxide at 150-200℃ for 2-3 hours.

[0016] Further, the preparation method of the epoxy resin in step (1) is as follows: 2,3-dicyanohydroquinone and epichlorohydrin are mixed at a mass ratio of 1:0.4 to 1:0.6, stirred at 100 to 300 r / min for 1 to 3 h, heated to 50 to 70 °C, and then 0.2 to 0.6 times the mass of 2,3-dicyanohydroquinone in a 10% sodium hydroxide solution is added dropwise at 20 to 40 drops / min, and stirring is continued for 1 to 3 h to prepare the epoxy resin.

[0017] Further, the preparation method of the aminated aluminum silicate nanofibers in step (2) is as follows: aluminum silicate nanofibers and concentrated sulfuric acid are mixed at a mass ratio of 1:210 to 1:230, and sonicated at 30 to 40 kHz for 20 to 40 min. Then, concentrated nitric acid with a mass fraction of 68% (55 to 57 times the mass of the aluminum silicate nanofibers) is added, and the mixture is stirred at 1200 to 1400 r / min for 9 to 11 min. The temperature is raised to 58 to 62 °C, and stirring is continued for 1.5 to 2.5 h. Then, deionized water with a mass ratio of 98 to 102 times the mass of the aluminum silicate nanofibers is added for dilution. The mixture is allowed to stand for 3.5 to 4.5 h, and then filtered through a microporous membrane with a pore size of 220 nm. The solution was filtered under vacuum, washed with deionized water until the pH of the filtrate reached 7, then washed 2–4 times with anhydrous ethanol, and dried in an oven at 55–65°C for 40–60 min. The solution was then added to 20–30 times its weight in diethyl ether and sonicated at 30–40 kHz for 20–40 min. γ-aminopropyltriethoxysilane was added in 1–3 times its weight in the aluminum silicate nanofibers, and a 0.1–2% (w / w) ethanol solution was added dropwise at 40–60 drops / min. The mixture was stirred for 1–3 h, filtered, washed 2–4 times with anhydrous ethanol, and dried in an oven at 100–120°C for 40–60 min to obtain amino-modified aluminum silicate nanofibers.

[0018] Furthermore, the preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment for 50-70s under a vacuum of 20-40Pa and 40-80℃, wherein the non-polymerizable gas in the plasma treatment device cavity is oxygen, the applied voltage discharge frequency is 13.75MHz, and the power is 80W, and the fabric base layer after plasma surface treatment is obtained.

[0019] Furthermore, the base layer of the fabric is knitted from 77.76% 20s cotton, 18.45% 150D polyester, and 3.79% 40D spandex by weight; the weight of the base layer is 320 g / m². 2 .

[0020] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0021] The electromagnetic shielding fabric prepared by this invention comprises, from the inside out: a fabric base layer and an electromagnetic shielding layer; firstly, graphene, diethylene glycol, and resin are mixed to prepare a graphene slurry; then, reduced graphene oxide, a thickener, and water are mixed to prepare a reduced graphene oxide slurry; subsequently, the graphene slurry and the reduced graphene oxide slurry are mixed to prepare a graphene / reduced graphene oxide composite slurry; then, the graphene / reduced graphene oxide composite slurry is coated onto the plasma-treated fabric base layer and shaped to obtain the final product; wherein, the resin is an epoxy resin obtained by reacting epichlorohydrin and 2,3-dicyanohydroquinone; and the thickener is amino-modified aluminum silicate nanofibers.

[0022] Combining graphene slurry and reduced graphene oxide slurry has several advantages. First, the numerous defects on the surfaces of both graphene and reduced graphene oxide can induce dipole polarization, generating dielectric loss and attenuating incident electromagnetic waves. Second, the abundant interfaces between graphene and reduced graphene oxide can cause interfacial polarization. Graphene / reduced graphene oxide attenuates electromagnetic waves through dielectric loss and enhances wave absorption performance through interfacial polarization, thereby improving the electromagnetic shielding performance of the graphene / reduced graphene oxide composite slurry.

[0023] On the other hand, the surface of reduced graphene oxide has a large number of pores. The thickener, aminated aluminum silicate nanofibers, embeds itself into the pores of reduced graphene oxide. Subsequently, it absorbs water and swells, firmly embedding the aminated aluminum silicate nanofibers into the reduced graphene oxide, thus enhancing the wear resistance of the fabric with electromagnetic shielding function. A large number of amino groups are formed on the surface of reduced graphene oxide. The phthalonitrile of epoxy resin hydrolyzes to form phthalic acid. The phthalic acid reacts with the amino groups on the surface of reduced graphene oxide to form an imide-containing polymer, which uniformly mixes the graphene slurry and the reduced graphene oxide slurry together, further enhancing the electromagnetic shielding performance of the graphene / reduced graphene oxide composite slurry. At the same time, the epoxy groups on the epoxy resin react with the hydroxyl groups on the fabric base layer after plasma surface treatment, firmly attaching the graphene / reduced graphene oxide composite slurry to the fabric base layer, thus enhancing the wash resistance of the fabric with electromagnetic shielding function. Attached Figure Description

[0024] Figure 1 The image shows the wave absorption performance test results of the fabric with electromagnetic shielding function prepared in Example 2 of this invention. Detailed Implementation

[0025] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0026] To more clearly illustrate the method provided by the present invention, the following embodiments are provided in detail. The testing methods for various indicators of the electromagnetic shielding fabric obtained in the following embodiments are as follows:

[0027] Electromagnetic shielding performance: Fabrics with electromagnetic shielding function prepared by the same mass of the example and comparative examples were tested according to GJB 2038A-2011 to test the reflection loss in the X-band.

[0028] Washability: Take the same mass of the electromagnetic shielding fabric prepared in the example and comparative examples, wash it with water according to GB / T3921 and observe the peeling of the coating on the surface of the fabric after washing.

[0029] In this embodiment, the materials include:

[0030] The disc-shaped graphene was purchased from Suqian Xigu Nanotechnology Co., Ltd.; model NCT-YS2E, with a solid content of 20%, a particle size of less than 15 μm, 1-10 layers, a dispersant content of <0.5%, and deionized water as the solvent.

[0031] Reduced graphene oxide is prepared by reducing graphene oxide at 150-200℃ for 2-3 hours.

[0032] Example 1

[0033] A method for preparing a fabric with electromagnetic shielding function includes the following preparation steps:

[0034] (1) Preparation of graphene slurry: Mix cake graphene and diethylene glycol at a mass ratio of 1:1.8, stir at 3000 r / min for 1 h, then add epoxy resin at 0.2 times the mass of cake graphene, stir at 600 r / min for 20 min to obtain graphene slurry.

[0035] (2) Preparation of reduced graphene oxide slurry: Reduced graphene oxide and thickener aminated aluminum silicate nanofibers were mixed at a mass ratio of 1:0.009 and stirred at 60 r / min for 20 min. Then, 0.2 times the mass of the reduced graphene oxide slurry was added to deionized water and stirred at 1600 r / min for 1 h to obtain the reduced graphene oxide slurry.

[0036] (3) Preparation of graphene / reduced graphene oxide composite slurry: Graphene slurry and reduced graphene oxide slurry were mixed at a mass ratio of 1:0.8 and stirred at 600 r / min for 3 h to obtain graphene / reduced graphene oxide composite slurry.

[0037] (4) Preparation of fabric with electromagnetic shielding function: A 0.6 mm thick graphene / reduced graphene oxide composite slurry is uniformly coated on the surface of the fabric base after plasma surface treatment, and then placed in a high temperature setting machine and set at 10 m / min at 110℃ for 5 min to obtain fabric with electromagnetic shielding function.

[0038] Further, the preparation method of the epoxy resin in step (1) is as follows: 2,3-dicyanohydroquinone and epichlorohydrin are mixed at a mass ratio of 1:0.4, stirred at 100 r / min for 1 h, heated to 50 °C, and then 0.2 times the mass of 2,3-dicyanohydroquinone in a 10% sodium hydroxide solution is added dropwise at 20 drops / min, and stirring is continued for 1 h to prepare the epoxy resin.

[0039] Further, the preparation method of the aminated aluminum silicate nanofibers in step (2) is as follows: aluminum silicate nanofibers and concentrated sulfuric acid are mixed at a mass ratio of 1:210, and sonicated at 30 kHz for 20 min. Then, concentrated nitric acid with a mass fraction of 68% (55 times the mass of the aluminum silicate nanofibers) is added, and the mixture is stirred at 1200 r / min for 9 min. The temperature is raised to 58 ℃, and stirring is continued for 1.5 h. Then, deionized water with a mass fraction of 98 times the mass of the aluminum silicate nanofibers is added for dilution. The mixture is allowed to stand for 3.5 h, and then vacuum filtered through a microporous membrane with a pore size of 220 nm. The solution was filtered, washed with deionized water until the pH of the filtrate reached 7, then washed twice with anhydrous ethanol, and dried in a 55°C oven for 40 min. The solution was then added to 20 times the mass of the aluminosilicate nanofibers in diethyl ether, sonicated at 30 kHz for 20 min, and 1 times the mass of the aluminosilicate nanofibers in γ-aminopropyltriethoxysilane was added. A 0.1% ethanol solution was added dropwise at 40 drops / min, and stirring was continued for 1 h. The solution was filtered, washed twice with anhydrous ethanol, and dried in a 100°C oven for 40 min to obtain aminated aluminosilicate nanofibers.

[0040] Furthermore, the preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment for 50s under a vacuum of 20Pa and 40℃, wherein the non-polymerizable gas in the plasma treatment device cavity is oxygen, the applied voltage discharge frequency is 13.75MHz, and the power is 80W, and the fabric base layer after plasma surface treatment is obtained.

[0041] Furthermore, the base layer of the fabric is knitted from 77.76% 20s cotton, 18.45% 150D polyester, and 3.79% 40D spandex by weight; the weight of the base layer is 320 g / m². 2 .

[0042] Example 2

[0043] A method for preparing a fabric with electromagnetic shielding function includes the following preparation steps:

[0044] (1) Preparation of graphene slurry: Mix cake graphene and diethylene glycol at a mass ratio of 1:1.9 and stir at 3500 r / min for 2 h. Then add epoxy resin with a mass of 0.25 times that of cake graphene and stir at 700 r / min for 30 min to obtain graphene slurry.

[0045] (2) Preparation of reduced graphene oxide slurry: Reduced graphene oxide and thickener aminated aluminum silicate nanofibers were mixed at a mass ratio of 1:0.01 and stirred at 70 r / min for 25 min. Then, 0.3 times the mass of the reduced graphene oxide slurry was added to deionized water and stirred at 1700 r / min for 2 h to obtain the reduced graphene oxide slurry.

[0046] (3) Preparation of graphene / reduced graphene oxide composite slurry: Graphene slurry and reduced graphene oxide slurry were mixed at a mass ratio of 1:1 and stirred at 700 r / min for 4 h to obtain graphene / reduced graphene oxide composite slurry.

[0047] (4) Preparation of fabric with electromagnetic shielding function: A 0.8 mm thick graphene / reduced graphene oxide composite slurry is uniformly coated on the surface of the fabric base after plasma surface treatment, and then placed in a high temperature setting machine and set at 120℃ for 10 min at 20 m / min to obtain fabric with electromagnetic shielding function.

[0048] Further, the preparation method of the epoxy resin in step (1) is as follows: 2,3-dicyanohydroquinone and epichlorohydrin are mixed at a mass ratio of 1:0.5, stirred at 200 r / min for 2 h, heated to 60 °C, and then 0.4 times the mass of 2,3-dicyanohydroquinone in a 10% sodium hydroxide solution is added dropwise at 30 drops / min, and stirring is continued for 2 h to obtain the epoxy resin.

[0049] Further, the preparation method of the aminated aluminum silicate nanofibers in step (2) is as follows: aluminum silicate nanofibers and concentrated sulfuric acid are mixed at a mass ratio of 1:220, and sonicated at 35 kHz for 30 min. Then, concentrated nitric acid with a mass fraction of 68% (56 times the mass of the aluminum silicate nanofibers) is added, and the mixture is stirred at 1300 r / min for 10 min. The temperature is raised to 60 ℃, and stirring is continued for 2 h. Then, deionized water with a mass fraction of 100 times the mass of the aluminum silicate nanofibers is added for dilution. The mixture is allowed to stand for 4 h, and then vacuum filtered through a microporous membrane with a pore size of 220 nm. The solution was filtered, washed with deionized water until the pH of the filtrate was 7, then washed three times with anhydrous ethanol, and dried in a 60°C oven for 50 min. The solution was then added to 25 times the mass of the aluminosilicate nanofibers in diethyl ether, sonicated at 35 kHz for 30 min, and then 2 times the mass of the aluminosilicate nanofibers in γ-aminopropyltriethoxysilane were added. A 1% ethanol solution was added dropwise at 50 drops / min, and stirring was continued for 2 h. The solution was filtered, washed three times with anhydrous ethanol, and dried in a 110°C oven for 50 min to obtain aminated aluminosilicate nanofibers.

[0050] Furthermore, the preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment for 60s under a vacuum of 30Pa and 60℃, wherein the non-polymerizable gas in the plasma treatment device cavity is oxygen, the applied voltage discharge frequency is 13.75MHz, and the power is 80W, and the fabric base layer after plasma surface treatment is obtained.

[0051] Furthermore, the base layer of the fabric is knitted from 77.76% 20s cotton, 18.45% 150D polyester, and 3.79% 40D spandex by weight; the weight of the base layer is 320 g / m². 2 .

[0052] Example 3

[0053] A method for preparing a fabric with electromagnetic shielding function includes the following preparation steps:

[0054] (1) Preparation of graphene slurry: Mix cake graphene and diethylene glycol at a mass ratio of 1:2, stir at 4000 r / min for 3 h, then add epoxy resin at 0.3 times the mass of cake graphene, stir at 800 r / min for 40 min to obtain graphene slurry.

[0055] (2) Preparation of reduced graphene oxide slurry: Reduced graphene oxide and thickener aminated aluminum silicate nanofibers were mixed at a mass ratio of 1:0.011 and stirred at 80 r / min for 30 min. Then, 0.4 times the mass of the reduced graphene oxide slurry was added to deionized water and stirred at 1800 r / min for 3 h to obtain the reduced graphene oxide slurry.

[0056] (3) Preparation of graphene / reduced graphene oxide composite slurry: Graphene slurry and reduced graphene oxide slurry were mixed at a mass ratio of 1:1.2 and stirred at 800 r / min for 5 h to obtain graphene / reduced graphene oxide composite slurry.

[0057] (4) Preparation of fabric with electromagnetic shielding function: A 1 mm thick graphene / reduced graphene oxide composite slurry is uniformly coated on the surface of the fabric base after plasma surface treatment, and then placed in a high temperature setting machine and set at 130℃ for 15 min at 30 m / min to obtain fabric with electromagnetic shielding function.

[0058] Further, the preparation method of the epoxy resin in step (1) is as follows: 2,3-dicyanohydroquinone and epichlorohydrin are mixed at a mass ratio of 1:0.6, stirred at 300 r / min for 3 h, heated to 70 °C, and then 0.6 times the mass of 2,3-dicyanohydroquinone in a 10% sodium hydroxide solution is added dropwise at 40 drops / min, and stirring is continued for 3 h to prepare the epoxy resin.

[0059] Further, the preparation method of the aminated aluminum silicate nanofibers in step (2) is as follows: aluminum silicate nanofibers and concentrated sulfuric acid are mixed at a mass ratio of 1:230, and sonicated at 40 kHz for 40 min. Then, concentrated nitric acid with a mass fraction of 68% (57 times the mass of the aluminum silicate nanofibers) is added, and the mixture is stirred at 1400 r / min for 11 min. The temperature is raised to 62 ℃, and stirring is continued for 2.5 h. Then, deionized water with a mass fraction of 102 times the mass of the aluminum silicate nanofibers is added for dilution. The mixture is allowed to stand for 4.5 h, and then filtered through a microporous membrane with a pore size of 220 nm. Vacuum filtration was performed, and the filtrate was washed with deionized water until the pH of the filtrate reached 7. Then, it was washed four times with anhydrous ethanol and dried in a 65°C oven for 60 min. Subsequently, it was added to 30 times the mass of the aluminosilicate nanofibers in diethyl ether and sonicated at 40 kHz for 40 min. Then, 3 times the mass of the aluminosilicate nanofibers in γ-aminopropyltriethoxysilane was added, and a 2% ethanol solution was added dropwise at 60 drops / min. The mixture was stirred for 3 h, filtered, washed four times with anhydrous ethanol, and dried in a 120°C oven for 60 min to obtain amino-modified aluminosilicate nanofibers.

[0060] Furthermore, the preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment for 70s under a vacuum of 40Pa and 80℃, wherein the non-polymerizable gas in the plasma treatment device cavity is oxygen, the applied voltage discharge frequency is 13.75MHz, and the power is 80W, and the fabric base layer after plasma surface treatment is obtained.

[0061] Furthermore, the base layer of the fabric is knitted from 77.76% 20s cotton, 18.45% 150D polyester, and 3.79% 40D spandex by weight; the weight of the base layer is 320 g / m². 2 .

[0062] Comparative Example 1

[0063] A method for preparing a fabric with electromagnetic shielding function includes the following preparation steps:

[0064] (1) Preparation of graphene slurry: Mix cake graphene and diethylene glycol at a mass ratio of 1:1.9 and stir at 3500 r / min for 2 h to obtain graphene slurry;

[0065] (2) Preparation of reduced graphene oxide slurry: Reduced graphene oxide and thickener aminated aluminum silicate nanofibers were mixed at a mass ratio of 1:0.01 and stirred at 70 r / min for 25 min. Then, 0.3 times the mass of the reduced graphene oxide slurry was added to deionized water and stirred at 1700 r / min for 2 h to obtain the reduced graphene oxide slurry.

[0066] (3) Preparation of graphene / reduced graphene oxide composite slurry: Graphene slurry and reduced graphene oxide slurry were mixed at a mass ratio of 1:1 and stirred at 700 r / min for 4 h to obtain graphene / reduced graphene oxide composite slurry.

[0067] (4) Preparation of fabric with electromagnetic shielding function: A 0.8 mm thick graphene / reduced graphene oxide composite slurry is uniformly coated on the surface of the fabric base after plasma surface treatment, and then placed in a high temperature setting machine and set at 120℃ for 10 min at 20 m / min to obtain fabric with electromagnetic shielding function.

[0068] Further, the preparation method of the aminated aluminum silicate nanofibers in step (2) is as follows: aluminum silicate nanofibers and concentrated sulfuric acid are mixed at a mass ratio of 1:220, and sonicated at 35 kHz for 30 min. Then, concentrated nitric acid with a mass fraction of 68% (56 times the mass of the aluminum silicate nanofibers) is added, and the mixture is stirred at 1300 r / min for 10 min. The temperature is raised to 60 ℃, and stirring is continued for 2 h. Then, deionized water with a mass fraction of 100 times the mass of the aluminum silicate nanofibers is added for dilution. The mixture is allowed to stand for 4 h, and then vacuum filtered through a microporous membrane with a pore size of 220 nm. The solution was filtered, washed with deionized water until the pH of the filtrate was 7, then washed three times with anhydrous ethanol, and dried in a 60°C oven for 50 min. The solution was then added to 25 times the mass of the aluminosilicate nanofibers in diethyl ether, sonicated at 35 kHz for 30 min, and then 2 times the mass of the aluminosilicate nanofibers in γ-aminopropyltriethoxysilane were added. A 1% ethanol solution was added dropwise at 50 drops / min, and stirring was continued for 2 h. The solution was filtered, washed three times with anhydrous ethanol, and dried in a 110°C oven for 50 min to obtain aminated aluminosilicate nanofibers.

[0069] Furthermore, the preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment for 60s under a vacuum of 30Pa and 60℃, wherein the non-polymerizable gas in the plasma treatment device cavity is oxygen, the applied voltage discharge frequency is 13.75MHz, and the power is 80W, and the fabric base layer after plasma surface treatment is obtained.

[0070] Furthermore, the base layer of the fabric is knitted from 77.76% 20s cotton, 18.45% 150D polyester, and 3.79% 40D spandex by weight; the weight of the base layer is 320 g / m². 2 .

[0071] Comparative Example 2

[0072] A method for preparing a fabric with electromagnetic shielding function includes the following preparation steps:

[0073] (1) Preparation of graphene slurry: Mix cake graphene and diethylene glycol at a mass ratio of 1:1.9 and stir at 3500 r / min for 2 h. Then add epoxy resin with a mass of 0.25 times that of cake graphene and stir at 700 r / min for 30 min to obtain graphene slurry.

[0074] (2) Preparation of reduced graphene oxide slurry: Reduced graphene oxide and deionized water were mixed at a mass ratio of 1:0.3 and stirred at 1700 r / min for 2 h to obtain reduced graphene oxide slurry;

[0075] (3) Preparation of graphene / reduced graphene oxide composite slurry: Graphene slurry and reduced graphene oxide slurry were mixed at a mass ratio of 1:1 and stirred at 700 r / min for 4 h to obtain graphene / reduced graphene oxide composite slurry.

[0076] (4) Preparation of fabric with electromagnetic shielding function: A 0.8 mm thick graphene / reduced graphene oxide composite slurry is uniformly coated on the surface of the fabric base after plasma surface treatment, and then placed in a high temperature setting machine and set at 120℃ for 10 min at 20 m / min to obtain fabric with electromagnetic shielding function.

[0077] Further, the preparation method of the epoxy resin in step (1) is as follows: 2,3-dicyanohydroquinone and epichlorohydrin are mixed at a mass ratio of 1:0.5, stirred at 200 r / min for 2 h, heated to 60 °C, and then 0.4 times the mass of 2,3-dicyanohydroquinone in a 10% sodium hydroxide solution is added dropwise at 30 drops / min, and stirring is continued for 2 h to obtain the epoxy resin.

[0078] Furthermore, the preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment for 60s under a vacuum of 30Pa and 60℃, wherein the non-polymerizable gas in the plasma treatment device cavity is oxygen, the applied voltage discharge frequency is 13.75MHz, and the power is 80W, and the fabric base layer after plasma surface treatment is obtained.

[0079] Furthermore, the base layer of the fabric is knitted from 77.76% 20s cotton, 18.45% 150D polyester, and 3.79% 40D spandex by weight; the weight of the base layer is 320 g / m². 2 .

[0080] Comparative Example 3

[0081] A method for preparing a fabric with electromagnetic shielding function includes the following preparation steps:

[0082] (1) Preparation of reduced graphene oxide slurry: Reduced graphene oxide and thickener aminated aluminum silicate nanofibers were mixed at a mass ratio of 1:0.01 and stirred at 70 r / min for 25 min. Then, 0.3 times the mass of the reduced graphene oxide slurry was added to deionized water and stirred at 1700 r / min for 2 h to obtain the reduced graphene oxide slurry.

[0083] (2) Preparation of fabric with electromagnetic shielding function: A 0.8 mm thick reduced graphene oxide slurry is uniformly coated on the surface of the fabric base after plasma surface treatment, and then placed in a high temperature setting machine and set at 150℃ at 20 m / min to obtain fabric with electromagnetic shielding function.

[0084] Further, the preparation method of the aminated aluminum silicate nanofibers in step (1) is as follows: aluminum silicate nanofibers and concentrated sulfuric acid are mixed at a mass ratio of 1:220, and sonicated at 35 kHz for 30 min. Then, concentrated nitric acid with a mass fraction of 68% (56 times the mass of the aluminum silicate nanofibers) is added, and the mixture is stirred at 1300 r / min for 10 min. The temperature is raised to 60 ℃, and stirring is continued for 2 h. Then, deionized water with a mass fraction of 100 times the mass of the aluminum silicate nanofibers is added for dilution. The mixture is allowed to stand for 4 h, and then vacuum filtered through a microporous membrane with a pore size of 220 nm. The solution was filtered, washed with deionized water until the pH of the filtrate was 7, then washed three times with anhydrous ethanol, and dried in a 60°C oven for 50 min. The solution was then added to 25 times the mass of the aluminosilicate nanofibers in diethyl ether, sonicated at 35 kHz for 30 min, and then 2 times the mass of the aluminosilicate nanofibers in γ-aminopropyltriethoxysilane were added. A 1% ethanol solution was added dropwise at 50 drops / min, and stirring was continued for 2 h. The solution was filtered, washed three times with anhydrous ethanol, and dried in a 110°C oven for 50 min to obtain aminated aluminosilicate nanofibers.

[0085] Furthermore, the preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment for 60s under a vacuum of 30Pa and 60℃, wherein the non-polymerizable gas in the plasma treatment device cavity is oxygen, the applied voltage discharge frequency is 13.75MHz, and the power is 80W, and the fabric base layer after plasma surface treatment is obtained.

[0086] Furthermore, the base layer of the fabric is knitted from 77.76% 20s cotton, 18.45% 150D polyester, and 3.79% 40D spandex by weight; the weight of the base layer is 320 g / m². 2 .

[0087] Comparative Example 4

[0088] A method for preparing a fabric with electromagnetic shielding function includes the following preparation steps:

[0089] (1) Preparation of graphene slurry: Mix cake graphene and diethylene glycol at a mass ratio of 1:1.9 and stir at 3500 r / min for 2 h. Then add epoxy resin with a mass of 0.25 times that of cake graphene and stir at 700 r / min for 30 min to obtain graphene slurry.

[0090] (2) Preparation of fabric with electromagnetic shielding function: A 0.8 mm thick graphene paste is uniformly coated on the surface of the fabric base after plasma surface treatment, and then placed in a high temperature setting machine and set at 150℃ at 20 m / min to obtain fabric with electromagnetic shielding function.

[0091] Further, the preparation method of the epoxy resin in step (1) is as follows: 2,3-dicyanohydroquinone and epichlorohydrin are mixed at a mass ratio of 1:0.5, stirred at 200 r / min for 2 h, heated to 60 °C, and then 0.4 times the mass of 2,3-dicyanohydroquinone in a 10% sodium hydroxide solution is added dropwise at 30 drops / min, and stirring is continued for 2 h to obtain the epoxy resin.

[0092] Furthermore, the preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment for 60s under a vacuum of 30Pa and 60℃, wherein the non-polymerizable gas in the plasma treatment device cavity is oxygen, the applied voltage discharge frequency is 13.75MHz, and the power is 80W, and the fabric base layer after plasma surface treatment is obtained.

[0093] Furthermore, the base layer of the fabric is knitted from 77.76% 20s cotton, 18.45% 150D polyester, and 3.79% 40D spandex by weight; the weight of the base layer is 320 g / m². 2 .

[0094] Example of effect

[0095] Table 1 below presents the analysis results of the electromagnetic shielding properties and washability of the fabrics with electromagnetic shielding function prepared using Examples 1 to 3 and Comparative Examples 1 to 4 of the present invention.

[0096] Table 1

[0097]

[0098] Table 1 shows that the electromagnetic shielding fabrics prepared in Examples 1, 2, and 3 have good electromagnetic shielding properties and washability. A comparison of the experimental data from Examples 1, 2, and 3 and Comparative Examples 1 and 3 shows that the fabric prepared using graphene slurry obtained from the reaction of epichlorohydrin and 2,3-dicyanohydroquinone has good electromagnetic shielding properties and washability. The experimental data from Examples 1, 2, and 3 and Comparative Examples 2 and 4 show that the fabric prepared using reduced graphene oxide slurry prepared from amino-modified aluminum silicate nanofibers has good electromagnetic shielding properties. (See Appendix...) Figure 1The electromagnetic shielding fabric prepared in Example 2 has a minimum reflection loss of -17dB in the X-band (8-14GHz) and is below -10dB throughout the entire X-band, meeting the expected performance requirements for electromagnetic shielding fabrics.

[0099] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No markings in the claims should be construed as limiting the scope of the claims.

Claims

1. A fabric having an electromagnetic shielding function, characterized by, The fabric with electromagnetic shielding function is obtained by coating graphene / reduced graphene oxide composite slurry on the fabric base layer after plasma surface treatment and shaping; the graphene / reduced graphene oxide composite slurry is prepared by mixing graphene slurry and reduced graphene oxide slurry; the graphene slurry is prepared by mixing graphene, diethylene glycol and resin; the reduced graphene oxide slurry is prepared by mixing reduced graphene oxide, thickening agent and water; The resin is an epoxy resin obtained by the reaction of epoxy chloropropane and 2,3-dicyano hydroquinone. The thickening agent is amino-silicate-aluminum nanofiber.

2. The fabric with electromagnetic shielding function according to claim 1, characterized in that, The fabric base layer is obtained by knitting cotton fiber, polyester fiber and spandex fiber.

3. A method of manufacturing the fabric having an electromagnetic shielding function according to claim 1, characterized by, The preparation steps include: (1) Preparation of graphene slurry: mix cake-shaped graphene and diethylene glycol at a mass ratio of 1:1.8-1:2, stir at 3000-4000 r / min for 1-3 h, then add epoxy resin with a mass of 0.2-0.3 times that of the cake-shaped graphene, stir at 600-800 r / min for 20-40 min, and prepare the graphene slurry; (2) Preparation of reduced graphene oxide slurry: mix reduced graphene oxide and amino-silicate-aluminum nanofiber thickening agent at a mass ratio of 1:0.009-1:0.011, stir and mix at 60-80 r / min for 20-30 min, then add deionized water with a mass of 0.2-0.4 times that of the reduced graphene oxide, stir at 1600-1800 r / min for 1-3 h, and prepare the reduced graphene oxide slurry; (3) Preparation of graphene / reduced graphene oxide composite slurry: mix graphene slurry and reduced graphene oxide slurry at a mass ratio of 1:0.8-1:1.2, stir at 600-800 r / min for 3-5 h, and prepare the graphene / reduced graphene oxide composite slurry; (4) Preparation of fabric with electromagnetic shielding function: uniformly coat 0.6-1 mm thick graphene / reduced graphene oxide composite slurry on the surface of the fabric base layer after plasma surface treatment, then put it into a high-temperature setting machine, set the temperature at 110-130℃ and the speed at 10-30 m / min, and set for 5-15 min, and prepare the fabric with electromagnetic shielding function.

4. The method of claim 3, wherein the fabric is prepared by coating the fabric with the conductive material. The reduced graphene oxide is prepared by reducing graphene oxide at 150-200℃ for 2-3 hours.

5. The method of claim 3, wherein the fabric having electromagnetic shielding function is prepared by coating a fabric with a conductive material. In step (1), the epoxy resin is prepared as follows: mix 2,3-dicyano hydroquinone and epoxy chloropropane at a mass ratio of 1:0.4-1:0.6, stir at 100-300 r / min for 1-3 h, heat to 50-70℃, then add 2,3-dicyano hydroquinone with a mass of 0.2-0.6 times the mass of the sodium hydroxide solution with a mass fraction of 10%, at a rate of 20-40 drops / min, and continue to stir for 1-3 h to prepare the epoxy resin.

6. The method of claim 3, wherein the fabric having electromagnetic shielding function is prepared by coating a fabric with a conductive material. The preparation method of the amino-silicon-aluminum nanofiber in step (2) is as follows: the silicon-aluminum nanofiber and concentrated sulfuric acid are mixed at a mass ratio of 1:210-1:230, and then ultrasonic treatment is performed at 30-40 kHz for 20-40 min; subsequently, concentrated nitric acid with a mass fraction of 68% is added at a mass ratio of 55-57 times that of the silicon-aluminum nanofiber, and stirring is performed at 1200-1400 r / min for 9-11 min; the temperature is increased to 58-62℃, and stirring is continued for 1.5-2.5 h; deionized water is added at a mass ratio of 98-102 times that of the silicon-aluminum nanofiber for dilution, and the mixture is left to stand for 3.5-4.5 h; then, the mixture is filtered under vacuum using a microporous filter membrane with a pore size of 220 nm; the filtered solution is washed with deionized water until the pH of the solution is 7; then, the mixture is washed with anhydrous ethanol for 2-4 times; the mixture is placed in an oven at 55-65℃ and baked for 40-60 min; then, the mixture is added to ethyl ether at a mass ratio of 20-30 times that of the silicon-aluminum nanofiber, and ultrasonic treatment is performed at 30-40 kHz for 20-40 min; γ-aminopropyltriethoxysilane is added at a mass ratio of 1-3 times that of the silicon-aluminum nanofiber; an ethanol solution with a mass fraction of 0.1-2% is added dropwise at a rate of 40-60 drops / min; stirring is continued for 1-3 h; the mixture is filtered and washed with anhydrous ethanol for 2-4 times; the mixture is placed in an oven at 100-120℃ and baked for 40-60 min; and the amino-silicon-aluminum nanofiber is obtained.

7. The method of claim 3, wherein the fabric having electromagnetic shielding function is prepared by coating a fabric with a conductive material. The preparation method of the fabric base layer after plasma surface treatment in step (4) is as follows: the fabric base layer is subjected to plasma treatment at a vacuum degree of 20-40 Pa and a temperature of 40-80℃ for 50-70 s; the non-polymerizable gas in the cavity of the plasma treatment device is oxygen; the applied voltage discharge frequency is 13.75 MHz; and the power is 80 W; and the fabric base layer after plasma surface treatment is obtained.

8. The method of claim 7, wherein the fabric having electromagnetic shielding function is prepared by coating a fabric with a conductive material. The fabric base layer is obtained by knitting 77.76% of 20s cotton, 18.45% of 150D polyester and 3.79% of 40D spandex by mass fraction; the fabric base layer has a gram weight of 320g / m 2 .

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