CN115652623A - Metal/graphene plated fabric prepared by microwave and preparation method thereof - Google Patents

Metal/graphene plated fabric prepared by microwave and preparation method thereof Download PDF

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CN115652623A
CN115652623A CN202211239469.1A CN202211239469A CN115652623A CN 115652623 A CN115652623 A CN 115652623A CN 202211239469 A CN202211239469 A CN 202211239469A CN 115652623 A CN115652623 A CN 115652623A
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fabric
metal
graphene
solution
microwave
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王毓
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Sichuan Police College
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Sichuan Police College
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Abstract

The invention relates to a metal/graphene plated fabric prepared by microwave and a preparation method thereof, belonging to the technical field of multifunctional textiles. The method for preparing the metal/graphene plated fabric by using the microwave comprises the following steps: a. firstly, dipping a textile fabric in a dopamine solution to obtain a fabric 1; b. soaking the fabric 1 in a graphene oxide solution, performing microwave treatment at 500-1000W for 20min, washing with water, and drying to obtain a fabric 2; c. soaking the fabric 2 in a metal salt solution, performing microwave treatment at 500-1000W for 20min, washing with water, and drying to obtain a metal/graphene plated fabric prepared by microwave; the metal salt solution comprises water, metal salt and a reducing agent, wherein the mass ratio of the water to the metal salt to the reducing agent is 109.55:0.3:0.3 to 30. The metal/graphene plated textile has stable electromagnetic shielding performance, the method is simple to operate, the production efficiency is high, the used reagents are few, and the cost is saved.

Description

Metal/graphene plated fabric prepared by microwave and preparation method thereof
Technical Field
The invention relates to a metal/graphene plated fabric prepared by microwave and a preparation method thereof, belonging to the technical field of multifunctional textiles.
Background
The metal/graphene plated textile refers to plating metal particles and graphene on the surface of the textile by a physical method, a chemical method and the like. The metal particles and the graphene are plated on the surface of the textile, so that the textile has the functions of conductivity, electromagnetic shielding, water resistance and the like, the additional value of the textile is improved, and the application fields of the textile are increased, such as the fields of clothing, household textiles, industrial textiles and the like.
At present, methods for preparing metal/graphene plated textiles mainly comprise a physical deposition method, a chemical deposition method, a supercritical fluid chemical deposition method and the like. However, these methods all have some disadvantages, such as complicated operation, more reagents used, poor diffusion capability, unstable electromagnetic shielding performance of the obtained metal/graphene plated textile, and the like.
How to simplify the process, improve the production efficiency, reduce the usage amount of reagents and reduce the cost, and the preparation of the metal/graphene plated textile with stable electromagnetic shielding performance is a difficult problem in the field.
CN112064341A discloses a graphene-based composite antibacterial material and a preparation method thereof, wherein the antibacterial material comprises a pretreated base cloth, and the upper surface and the lower surface of the pretreated base cloth are both coated with modified graphene oxide layers; the pretreated base fabric is obtained by surface treatment of base fabric and a modifier; the modifier mainly comprises dopamine, sodium alginate, sodium periodate and glycol; the modified graphene oxide layer is mainly prepared from modified graphene oxide, silver nitrate, sodium citrate and sodium borohydride; the modified graphene oxide is ethylene diamine grafted graphene oxide. A preparation method of a graphene-based composite antibacterial material comprises the following steps: 1) Preparing materials; 2) Taking a Tris solution, adjusting the pH value with dilute hydrochloric acid, adding dopamine, sodium alginate and base cloth, stirring for reaction, taking out the base cloth, washing, drying at constant temperature, drying, placing in a sodium periodate solution, reacting in a dark place at 35-40 ℃, soaking in an ethylene glycol aqueous solution, washing with deionized water, and drying to obtain a pretreated base cloth; 3) Taking graphene oxide and deionized water, carrying out ultrasonic dispersion, adding ammonia water in an ultrasonic process until the pH value of the solution is 10, adding ethylenediamine, carrying out stirring reaction, continuously carrying out stirring reaction for 2-2.5 hours in a water bath, carrying out vacuum filtration, alternately washing with ethanol and deionized water, and carrying out vacuum drying to obtain modified graphene oxide; 4) Taking modified graphene oxide and absolute ethyl alcohol, performing ultrasonic dispersion, adding pretreated base cloth, reacting at 40-50 ℃ for 2-4h, washing with deionized water to be neutral after reaction, and drying to obtain modified base cloth; 5) Taking silver nitrate, sodium citrate and hydrogen peroxide, sequentially adding the silver nitrate, the sodium citrate and the hydrogen peroxide into deionized water at 20-30 ℃, stirring for reaction until the mixture is dissolved, adding sodium borohydride and the modified base cloth, stirring for reaction in a dark place, taking out the modified base cloth, washing with the deionized water, drying, then placing the dried modified base cloth into a silver nitrate solution, stirring for reaction for 2-4 hours at 25-40 ℃, washing and drying to obtain a finished product. However, the chemical deposition method is mainly adopted, so that the process steps are complicated, a large number of chemical reagents are used, the cost is high, the antibacterial performance is mainly improved, and the electromagnetic shielding performance is poor.
CN105442306A discloses a nano-silver textile fabric, which comprises raw materials of silver nitrate, a modifier and a textile fabric, wherein the mass ratio of the modifier to the silver nitrate is 1-50, and the mass of the silver nitrate used in each square meter of the textile fabric is 1-50 g. The method adopts dopamine as a modifier to pretreat the textile fabric, prepares the nano-silver by a microwave method and reduces the nano-silver on the surface of the textile fabric in situ, has the characteristics of environmental protection, high production efficiency, high nano-silver binding force, good repeatability and the like, and the obtained nano-silver textile fabric has the functional characteristics of antibiosis, water repellency, electromagnetic shielding and the like. However, the obtained nano-silver textile fabric has no disclosure on how to prepare metal/graphene plated textile with stable electromagnetic shielding performance.
Disclosure of Invention
A first object of the present invention is to provide a novel method for microwave preparation of metal/graphene coated fabrics.
To achieve the first object of the present invention, the method for preparing a metal/graphene coated fabric by microwave comprises:
a. firstly, dipping a textile fabric in a dopamine solution to obtain a fabric 1;
b. soaking the fabric 1 in a graphene oxide solution, performing microwave treatment at 500-1000W for 20-25 min, washing with water, and drying to obtain a fabric 2;
c. soaking the fabric 2 in a metal salt solution, performing microwave treatment at 500-1000W for 20-25 min, washing with water, and drying to obtain a metal/graphene plated fabric prepared by microwave; the metal salt solution comprises water, metal salt and a reducing agent, wherein the mass ratio of the water to the metal salt to the reducing agent is 109.55:0.3:0.3 to 30; the mass ratio of water, metal salt and reducing agent is preferably 109.55:0.3:0.3 to 4.5.
The metal salt solution can be obtained by adding metal salt and reducing agent solution into deionized water and stirring for 5-10 min.
The textile fabric can be at least one of cotton, hemp, wool, bamboo pulp fiber, regenerated fiber, terylene, chinlon or spandex.
In a specific embodiment, the textile fabric is also subjected to pretreatment before being impregnated in the step a, wherein the pretreatment comprises the steps of ultrasonically cleaning the textile fabric in an ethanol solution and an acetone solution for 10-30 min respectively, taking out and drying; the volume ratio of acetone to ethanol is preferably 1 to 1.3.
In a specific embodiment, the impregnation method in the step a is carried out for 24-26 hours at the temperature of 20-25 ℃ under normal pressure.
In a specific embodiment, the concentration of the dopamine solution in the step a is 3 g/L-3.5 g/L, and the pH value is 8.3-8.7; the pH is preferably adjusted with tris.
In a specific embodiment, the graphene oxide solution in the step b is a deionized water solution with a concentration of 1g/L to 1.5 g/L; preferably, the graphene oxide solution is subjected to ultrasonic treatment for 60-70 min to be uniformly dispersed, and the power of the ultrasonic treatment is preferably 200W.
In one embodiment, the metal salt in step c is a silver salt.
The mass of the metal salt used in the step c per square meter of the fabric 2 is preferably 1g to 50g.
In one embodiment, the reducing agent in step c is sodium citrate or sodium borohydride.
In a specific embodiment, the fabric 1 is turned over in the microwave treatment process in the step b, and the turning over is performed every 2-5 min.
In a specific embodiment, the fabric 2 is turned over in the microwave treatment process in the step c, and the turning over is carried out every 2-5 min;
c, preferably, mixing part of water and metal salt to obtain a solution 1, soaking the fabric 2 in the solution 1, and treating for 2-5 min at 500-1000W by using microwaves; and then adding a reducing agent and the rest water into the solution 1 for microwave treatment at 500-1000W for 20-25 min, wherein the concentration of the metal salt in the solution 1 is 3-3.5 g/L.
A second object of the present invention is to provide a microwave-produced metal/graphene plated fabric.
In order to achieve the second object of the present invention, the metal/graphene plated fabric prepared by microwave is prepared by the method for preparing the metal/graphene plated fabric by microwave.
Has the advantages that:
the method can successfully prepare the metal/graphene plated fabric with the functions of electric conduction, electromagnetic shielding and water resistance, the metal/graphene plated layer can be firmly plated on the fabric, and the obtained metal/graphene plated fabric has stable electromagnetic shielding performance.
The method has the advantages of simple operation, high production efficiency, less reagent consumption, cost saving and contribution to popularization and application of the method.
Drawings
Fig. 1 is a scanning electron microscope image of the surface of the nano silver/graphene fabric of example 1 before and after soaping.
Fig. 2 is an electromagnetic shielding diagram of example 1 of the present invention and comparative example 1.
Detailed Description
To achieve the first object of the present invention, the method for preparing a metal/graphene coated fabric by microwave comprises:
a. firstly, dipping a textile fabric in a dopamine solution to obtain a fabric 1;
b. soaking the fabric 1 in a graphene oxide solution, performing microwave treatment at 500-1000W for 20-25 min, washing with water, and drying to obtain a fabric 2;
c. soaking the fabric 2 in a metal salt solution, performing microwave treatment at 500-1000W for 20-25 min, washing with water, and drying to obtain a metal/graphene plated fabric prepared by microwave; the metal salt solution comprises water, metal salt and a reducing agent, wherein the mass ratio of the water to the metal salt to the reducing agent is 109.55:0.3:0.3 to 30; the mass ratio of water, metal salt and reducing agent is preferably 109.55:0.3:0.3 to 4.5.
The metal salt solution can be obtained by adding metal salt and reducing agent solution into deionized water and stirring for 5-10 min.
The textile fabric can be at least one of cotton, hemp, wool, bamboo pulp fiber, regenerated fiber, terylene, chinlon or spandex.
In a specific embodiment, the textile fabric is also subjected to pretreatment before being impregnated in the step a, wherein the pretreatment comprises the steps of ultrasonically cleaning the textile fabric in an ethanol solution and an acetone solution for 10-30 min respectively, taking out and drying; the volume ratio of acetone to ethanol is preferably 1 to 1.3.
In a specific embodiment, the impregnation method in the step a is carried out for 24-26 hours at the temperature of 20-25 ℃ under normal pressure.
In a specific embodiment, the concentration of the dopamine solution in the step a is 3 g/L-3.5 g/L, and the pH value is 8.3-8.7; the pH is preferably adjusted using tris.
In a specific embodiment, the graphene oxide solution in the step b is a deionized water solution with a concentration of 1g/L to 1.5 g/L; preferably, the graphene oxide solution is subjected to ultrasonic treatment for 60-70 min to be uniformly dispersed, and the ultrasonic power is preferably 200W.
In one embodiment, the metal salt in step c is a silver salt.
The mass of the metal salt used in the step c per square meter of the fabric 2 is preferably 1g to 50g.
In one embodiment, the reducing agent in step c is sodium citrate or sodium borohydride.
In a specific embodiment, the fabric 1 is turned over in the microwave treatment process in the step b, and the turning over is performed every 2-5 min.
In a specific embodiment, the fabric 2 is turned over in the microwave treatment process in the step c, and the turning over is carried out every 2-5 min;
c, preferably, mixing part of water and metal salt to obtain a solution 1, soaking the fabric 2 in the solution 1, and treating for 2-5 min at 500-1000W by using microwaves; and then adding a reducing agent and the rest water into the solution 1 for microwave treatment for 20-25 min at the power of 500-1000W, wherein the concentration of the metal salt in the solution 1 is 3-3.5 g/L.
The second purpose of the invention is to provide a metal/graphene coated fabric prepared by microwave.
In order to achieve the second object of the present invention, the metal/graphene plated fabric prepared by microwave is prepared by the method for preparing the metal/graphene plated fabric by microwave.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
Ultrasonically cleaning polyester fiber fabric with the size of 5cm multiplied by 5cm for 30min by using acetone and ethanol respectively, taking out the fabric, and drying the fabric in an oven at 70 ℃; soaking the degreased and cleaned polyester fabric into a dopamine solution, wherein 0.3g of dopamine is weighed and dissolved in 100mL of tris buffer solution, and the pH value is 8.5. Standing for 24h at normal temperature, taking out, washing with water, and air drying;
weighing 0.1g of graphene oxide in 100mL of deionized water, carrying out ultrasonic treatment for 60min, soaking the dopamine-modified polyester fabric in the graphene oxide dispersion liquid, heating for 20min by using microwaves at 700W, turning over every 2min, taking out, washing with water, and airing; 0.3g of AgNO 3 Dissolving in 100mL of deionized water, immersing the prepared GO-loaded dopamine modified polyester fabric into a silver nitrate solution, putting into a microwave oven, and irradiating for 2min at 700W by using microwaves; then, 10mL of 45g/L sodium citrate is added, the mixture is stirred uniformly, heated by microwave 700W for 20min, turned over every 2min, washed by water and dried in an oven at 100 ℃.
The obtained nano-silver/graphene-plated dopamine modified polyester fiber fabric has the following microstructure and macroscopic properties:
fig. 1 is a scanning electron microscope (30000 times magnified) image of the surface of the nano-silver/graphene fabric of example 1 before and after soaping. As can be seen from fig. 1, the polydopamine generated on the surface of the fiber after dopamine modification has adhesiveness, so that the graphene film and silver particles can be fixed on the surface of the fiber, and meanwhile, the graphene film graphene as a substrate can adsorb more silver particles, so that the silver particles are fixed in the fiber and film layers.
Fig. 2 is a nano silver/graphene electromagnetic shield according to example 1 of comparative example 1 of the present invention. As can be seen from fig. 2, the nano silver/graphene fabric without dopamine pretreatment has a small binding force between the plating layer and the fabric, so that the electromagnetic shielding effectiveness before soaping is about 30dB, and the electromagnetic shielding effectiveness after soaping is reduced to zero; the nano silver/graphene fabric of embodiment 1 greatly improves the bonding force between the plating degree and the fabric, and the electromagnetic shielding effectiveness before and after soaping is not reduced much.
Comparative example 1
The other is similar to example 1, except that comparative example 1 does not employ dopamine.

Claims (10)

1. The method for preparing the metal/graphene plated fabric by microwaves is characterized by comprising the following steps of:
a. firstly, dipping a textile fabric in a dopamine solution to obtain a fabric 1;
b. soaking the fabric 1 in a graphene oxide solution, performing microwave treatment at 500-1000W for 20-25 min, washing with water, and drying to obtain a fabric 2;
c. dipping the fabric 2 in a metal salt solution, performing microwave treatment at 500-1000W for 20-25 min, washing with water, and drying to obtain a metal/graphene plated fabric prepared by microwave; the metal salt solution comprises water, metal salt and a reducing agent, wherein the mass ratio of the water to the metal salt to the reducing agent is 109.55:0.3:0.3 to 30; the mass ratio of water, metal salt and reducing agent is preferably 109.55:0.3:0.3 to 4.5.
2. The microwave preparation method of the metal/graphene plated fabric according to claim 1, wherein the textile fabric is subjected to pretreatment before impregnation in the step a, and the pretreatment comprises the steps of ultrasonically cleaning the textile fabric in an ethanol solution and an acetone solution respectively for 10-30 min, taking out, and drying; the volume ratio of acetone to ethanol is preferably 1 to 1.3.
3. The method for preparing a metal/graphene-plated fabric by using microwaves according to claim 1 or 2, wherein the dipping method in the step a is carried out at 20-25 ℃ for 24-26 h under normal pressure.
4. The method for preparing a metal/graphene-plated fabric by using microwaves according to claim 1 or 2, wherein the concentration of the dopamine solution in the step a is 3-3.5 g/L, and the pH value is 8.3-8.7; the pH is preferably adjusted using tris.
5. The method for preparing a metal/graphene-plated fabric by using microwaves according to claim 1 or 2, wherein the graphene oxide solution in the step b is a deionized water solution with the concentration of 1 g/L-1.5 g/L; preferably, the graphene oxide solution is subjected to ultrasonic treatment for 60-70 min to be uniformly dispersed, and the ultrasonic power is preferably 200W.
6. The method of microwave preparation of metal/graphene coated fabric according to claim 1 or 2, wherein the metal salt in step c is silver salt;
the mass of the metal salt used in the step c per square meter of the fabric 2 is preferably 1g to 50g.
7. The method for microwave preparation of metal/graphene coated fabric according to claim 1 or 2, wherein the reducing agent in step c is sodium citrate or sodium borohydride.
8. The method for preparing the metal/graphene plated fabric by using the microwaves according to claim 1 or 2, wherein the fabric 1 is turned over in the microwave treatment process in the step b, and the turning over is carried out every 2-5 min.
9. The method for preparing the metal/graphene plated fabric by using the microwaves according to claim 1 or 2, wherein the fabric 2 is turned over in the microwave treatment process in the step c, and the turning over is carried out every 2-5 min;
preferably, mixing part of water and metal salt to obtain a solution 1, soaking the fabric 2 in the solution 1, and treating for 2-5 min by using microwave at 500-1000W; and then adding a reducing agent and the rest water into the solution 1 for microwave treatment for 20-25 min at the power of 500-1000W, wherein the concentration of the metal salt in the solution 1 is 3-3.5 g/L.
10. The microwave-prepared metal/graphene plated fabric is characterized by being prepared by the method for preparing the metal/graphene plated fabric by microwaves according to any one of claims 1 to 9.
CN202211239469.1A 2022-10-11 2022-10-11 Metal/graphene plated fabric prepared by microwave and preparation method thereof Pending CN115652623A (en)

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Publication number Priority date Publication date Assignee Title
CN105442306A (en) * 2015-11-23 2016-03-30 四川大学 Preparation method of dopamine modified nano-silver textile fabric
CN106854833A (en) * 2016-12-30 2017-06-16 中国科学院宁波材料技术与工程研究所 A kind of antistatic superhigh molecular weight polyethylene fibers of lightweight and preparation method thereof
CN108625158A (en) * 2017-03-21 2018-10-09 上海大学 A kind of antistatic graphene coated fabric and preparation method thereof
CN112144273A (en) * 2020-09-30 2020-12-29 福州大学 Preparation method of multifunctional fabric surface with super-hydrophobic and conductive functions
CN112832020A (en) * 2021-02-08 2021-05-25 四川警察学院 Preparation method of immersion or supercritical fluid pretreatment assisted metal plating textile
CN113152088A (en) * 2021-04-25 2021-07-23 江南大学 Flexible fabric-based strain sensor and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105442306A (en) * 2015-11-23 2016-03-30 四川大学 Preparation method of dopamine modified nano-silver textile fabric
CN106854833A (en) * 2016-12-30 2017-06-16 中国科学院宁波材料技术与工程研究所 A kind of antistatic superhigh molecular weight polyethylene fibers of lightweight and preparation method thereof
CN108625158A (en) * 2017-03-21 2018-10-09 上海大学 A kind of antistatic graphene coated fabric and preparation method thereof
CN112144273A (en) * 2020-09-30 2020-12-29 福州大学 Preparation method of multifunctional fabric surface with super-hydrophobic and conductive functions
CN112832020A (en) * 2021-02-08 2021-05-25 四川警察学院 Preparation method of immersion or supercritical fluid pretreatment assisted metal plating textile
CN113152088A (en) * 2021-04-25 2021-07-23 江南大学 Flexible fabric-based strain sensor and preparation method thereof

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Title
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