阅读说明：本技术 一种石墨烯/尼龙纤维复合材料及其制备方法与应用 (Graphene/nylon fiber composite material and preparation method and application thereof ) 是由 吴敏 黄大勇 黄勇 于 2019-11-21 设计创作，主要内容包括：本发明提供了一种石墨烯/尼龙纤维复合材料及其制备方法与应用,属于复合材料技术领域。本发明使用多糖溶液为溶剂,一是作为石墨烯的分散介质,二是在石墨烯与尼龙粉末之间起到一个“粘结”的作用,使得石墨烯可以均匀包覆在尼龙粉末表面；同时,由于石墨烯具有较薄的片层厚度(2～50nm),使得该复合材料具有优异的抗菌效果,且在红外灯照射下实现快速升温；另外,本发明的制备方法简单、易操作,适合工业化。实施例数据表明：本发明所得石墨烯/尼龙纤维复合材料对大肠杆菌、金黄色葡萄球菌以及肺炎克雷伯氏菌的抑菌率均可达到99％以上；同时,将该复合材料置于100℃的红外灯照射下,样品表面温度可在10s内由25℃升至49℃。(The invention provides a graphene/nylon fiber composite material and a preparation method and application thereof, and belongs to the technical field of composite materials. The preparation method uses polysaccharide solution as a solvent, and the polysaccharide solution is used as a dispersion medium of graphene, and plays a role in bonding between the graphene and nylon powder, so that the graphene can be uniformly coated on the surface of the nylon powder; meanwhile, the graphene has a thin lamellar thickness (2-50 nm), so that the composite material has an excellent antibacterial effect, and rapid temperature rise is realized under the irradiation of an infrared lamp; in addition, the preparation method is simple, easy to operate and suitable for industrialization. The example data shows that: the inhibition rate of the graphene/nylon fiber composite material on escherichia coli, staphylococcus aureus and klebsiella pneumoniae can reach more than 99%; meanwhile, the surface temperature of the sample can be increased from 25 ℃ to 49 ℃ within 10s by placing the composite material under the irradiation of an infrared lamp at 100 ℃.)

1. The preparation method of the graphene/nylon fiber composite material is characterized by comprising the following steps:

dispersing graphene in a polysaccharide solution to obtain a graphene/polysaccharide dispersion solution; the thickness of the graphene sheet layer is 2-50 nm;

mixing the graphene/polysaccharide dispersion liquid with nylon powder to obtain a graphene/nylon dispersion liquid; drying the graphene/nylon dispersion liquid to obtain graphene/nylon powder;

and carrying out melt spinning on the graphene/nylon powder to obtain the graphene/nylon fiber composite material.

2. The method according to claim 1, wherein the graphene is prepared by a reduced oxidation graphite method or a physical mechanical exfoliation method.

3. The method according to claim 1, wherein the polysaccharide in the polysaccharide solution is one or more of carboxymethyl cellulose, hydroxyethyl cellulose, hemicellulose and chitosan.

4. The method according to claim 1 or 3, wherein the concentration of the polysaccharide solution is 0.01 to 5 g/L.

5. The preparation method according to claim 1, wherein the concentration of the graphene in the graphene/polysaccharide dispersion liquid is 0.01-10 g/L.

6. The preparation method according to claim 1, wherein the nylon powder is one or more of nylon-6 powder, nylon-610 powder, nylon-1010 powder and nylon-66 powder.

7. The preparation method according to claim 1 or 6, wherein the concentration of the nylon powder in the graphene/nylon dispersion liquid is 100-2000 g/L.

8. The method according to claim 1, wherein the melt-spinning temperature is 150 to 400 ℃; the drawing speed of the melt spinning is 1000-3000 m/min.

9. The graphene/nylon fiber composite material obtained by the preparation method of any one of claims 1 to 8, wherein the graphene/nylon fiber composite material is prepared by uniformly dispersing graphene flakes in a nylon matrix, and the thickness of the graphene flakes is 2 to 50 nm.

10. Use of the graphene/nylon fiber composite of claim 9 in a warming neck collar area.

Technical Field

The invention belongs to the technical field of composite materials, and particularly relates to a graphene/nylon fiber composite material and a preparation method and application thereof.

Background

Nylon fiber (polyamide fiber) is the first synthetic fiber appearing in the world, namely nylon which we often say. The appearance of nylon is an important milestone of the development of polymer chemistry, so that the appearance of textiles is new. Nylon has the advantages of high strength, high toughness, processability and the like, so that the nylon is widely applied to the fields of engineering plastics, textiles and the like.

Graphene is the thinnest two-dimensional nanomaterial known in the world at present, and has extremely excellent electric conduction and heat conduction properties and extremely high mechanical strength.

The graphene and the nylon fibers are combined together to form the composite material, so that the composite material has the performances of the graphene and the nylon fibers. In the prior art, when a graphene-nylon fiber composite material is prepared, graphene powder and nylon particles are generally mixed and then are obtained by melt blending and extrusion. This preparation method of the prior art is complicated; and the graphene and the nylon are not uniformly mixed, so that the performance of the final composite material is influenced, and the application of the graphene/nylon composite material is limited.

Disclosure of Invention

In view of this, the present invention provides a graphene/nylon fiber composite material, and a preparation method and an application thereof. The preparation method provided by the invention is simple, and the graphene and the nylon can be uniformly dispersed and compounded together, so that the graphene/nylon fiber composite material has a good antibacterial effect, and can realize rapid temperature rise under the irradiation of an infrared lamp.

In order to achieve the above object, the present invention provides the following technical solutions:

the invention provides a preparation method of a graphene/nylon fiber composite material, which comprises the following steps:

dispersing graphene in a polysaccharide solution to obtain a graphene/polysaccharide dispersion solution; the thickness of the graphene sheet layer is 2-50 nm;

mixing the graphene/polysaccharide dispersion liquid with nylon powder to obtain a graphene/nylon dispersion liquid; drying the graphene/nylon dispersion liquid to obtain graphene/nylon powder;

and carrying out melt spinning on the graphene/nylon powder to obtain the graphene/nylon fiber composite material.

Preferably, the graphene is prepared by a reduction oxidation graphite method or a physical mechanical stripping method.

Preferably, the polysaccharide in the polysaccharide solution is one or more of carboxymethyl cellulose, hydroxyethyl cellulose, hemicellulose and chitosan.

Preferably, the concentration of the polysaccharide solution is 0.01-5 g/L.

Preferably, the concentration of the graphene in the graphene/polysaccharide dispersion liquid is 0.01-10 g/L.

Preferably, the nylon powder is one or more of nylon-6 powder, nylon-610 powder, nylon-1010 powder and nylon-66 powder.

Preferably, the concentration of the nylon powder in the graphene/nylon dispersion liquid is 100-2000 g/L.

Preferably, the temperature of the melt spinning is 150-400 ℃; the drawing speed of the melt spinning is 1000-3000 m/min.

The invention further provides the graphene/nylon fiber composite material prepared by the preparation method in the technical scheme, the graphene/nylon fiber composite material is formed by uniformly dispersing graphene sheets in a nylon matrix, and the thickness of the graphene sheets is 2-50 nm.

The invention also provides application of the graphene/nylon fiber composite material in the warm keeping collar domain.

The invention provides a preparation method of a graphene/nylon fiber composite material, which comprises the following steps: dispersing graphene in a polysaccharide solution to obtain a graphene/polysaccharide dispersion solution; the thickness of the graphene sheet layer is 2-50 nm; mixing the graphene/polysaccharide dispersion liquid with nylon powder to obtain a graphene/nylon dispersion liquid; drying the graphene/nylon dispersion liquid to obtain graphene/nylon powder; and carrying out melt spinning on the graphene/nylon powder to obtain the graphene/nylon fiber composite material. The preparation method disclosed by the invention uses the polysaccharide solution as a solvent, and the polysaccharide solution is used as a dispersion medium of graphene, and plays a role in bonding between the graphene and nylon powder, so that the graphene can be uniformly coated on the surface of the nylon powder, and the composite effect of the graphene and nylon is improved; meanwhile, the graphene has a thin sheet thickness, so that the composite material has an excellent antibacterial effect and can realize rapid temperature rise under the irradiation of an infrared lamp; in addition, the preparation method is simple, easy to operate and suitable for industrialization. The data of the examples show that: the graphene/nylon fiber composite material prepared by the preparation method disclosed by the invention has the bacteriostasis rate of over 99% on escherichia coli, staphylococcus aureus and klebsiella pneumoniae, and has a good bacteriostasis effect; meanwhile, the composite material is placed under the irradiation of an infrared lamp at 100 ℃, the surface temperature of a sample can be increased from 25 ℃ to 49 ℃ within 10s, and the composite material is expected to be applied to the field of thermal underwear.

Drawings

Fig. 1 is a Scanning Electron Microscope (SEM) photograph of the graphene/nylon fiber composite obtained in example 1.

Detailed Description

The invention provides a preparation method of a graphene/nylon fiber composite material, which comprises the following steps:

dispersing graphene in a polysaccharide solution to obtain a graphene/polysaccharide dispersion solution;

mixing the graphene/polysaccharide dispersion liquid with nylon powder to obtain a graphene/nylon dispersion liquid; drying the graphene/nylon dispersion liquid to obtain graphene/nylon powder;

and carrying out melt spinning on the graphene/nylon powder to obtain the graphene/nylon fiber composite material.

According to the invention, graphene is dispersed in a polysaccharide solution to obtain a graphene/polysaccharide dispersion solution.

In the invention, the graphene is preferably prepared by a reduction oxidation graphite method or a physical mechanical stripping method; the thickness of the graphene sheet is 2-50 nm, preferably 10-40 nm, and more preferably 20-30 nm. The source of the graphene is not particularly limited, and a commercially available product is adopted. In the invention, the graphene prepared by a reduction oxidation graphite method or a physical mechanical stripping method is in a powder state by macroscopic observation and is easy to disperse in a polysaccharide solution; meanwhile, the graphene prepared by the two methods has fewer layers on the micro scale and thinner thickness, and can exert the advantages of the graphene in the application of infrared heating and antibiosis.

In the present invention, the concentration of the polysaccharide solution is preferably 0.01 to 5g/L, and more preferably 0.1 to 1 g/L. In the present invention, the polysaccharide in the polysaccharide solution is preferably one or more of carboxymethyl cellulose, hydroxyethyl cellulose, hemicellulose and chitosan. In the present invention, the solvent of the polysaccharide solution is preferably water or a weakly acidic aqueous solution; the choice of the solvent in the polysaccharide solution is specifically determined according to the type of polysaccharide, and specifically, when the polysaccharide is carboxymethyl cellulose or hydroxyethyl cellulose, the solvent in the polysaccharide solution is preferably water, and the water is preferably deionized water; when the polysaccharide is hemicellulose, the solvent of the polysaccharide solution is preferably a hydrochloric acid solution with a concentration of 2 wt%; when the polysaccharide is chitosan, the solvent of the polysaccharide solution is preferably an acetic acid solution with a concentration of 1 wt%. In the invention, the concentration of the polysaccharide solution is selected to be 0.01-5 g/L, because the polysaccharide solution with the concentration range can stably disperse graphene; below this concentration range, the interaction force between the polysaccharide molecules and the graphene is too small to completely disperse the graphene; above this concentration range, the polysaccharide solution viscosity is too high for the gel formed to be fluid and thus incapable of dispersing graphene.

In the invention, the dispersing time is preferably 10-30 min, and more preferably 20 min; the dispersion is preferably carried out in an ultrasonic washer or a cell disruptor.

In the present invention, the concentration of the graphene in the graphene/polysaccharide dispersion liquid is preferably 0.01 to 10g/L, and more preferably 0.1 to 1 g/L.

After the graphene/polysaccharide dispersion liquid is obtained, mixing the graphene/polysaccharide dispersion liquid with nylon powder to obtain the graphene/nylon dispersion liquid; and drying the graphene/nylon dispersion liquid to obtain graphene/nylon powder.

In the invention, the average particle size of the nylon powder is preferably 5-50 μm; the nylon powder is preferably one or more of nylon-6 powder, nylon-610 powder, nylon-1010 powder and nylon-66 powder. In the invention, the concentration of the nylon powder in the graphene/nylon dispersion liquid is preferably 010-2000 g/L, and more preferably 500-1500 g/L; according to the invention, the concentration of the nylon powder in the graphene/nylon dispersion liquid is controlled to be 100-2000 g/L, so that the graphene can be completely coated on the surface of the nylon powder, and the composite effect of the graphene and the nylon powder is improved.

In the present invention, the mixing is preferably performed in the following manner: adding the nylon powder into the graphene/polysaccharide dispersion liquid under a stirring state.

In the present invention, the drying is preferably freeze drying or vacuum drying; when the drying mode is freeze drying, the freezing is preferably liquid nitrogen freezing, the drying is preferably carried out on a dryer, the drying temperature is preferably-80 to-60 ℃, and the time is preferably 48 to 96 hours; when the drying mode is vacuum drying, the temperature of the vacuum drying is preferably 40 ℃, and the time is preferably 48 hours, and the vacuum drying is preferably carried out in a vacuum oven.

After the graphene/nylon powder is obtained, the graphene/nylon powder is subjected to melt spinning to obtain the graphene/nylon fiber composite material.

In the invention, the melt spinning temperature is preferably 150-400 ℃, more preferably 200-350 ℃, and more preferably 250-300 ℃; the drawing speed of the melt spinning is preferably 1000 to 3000m/min, more preferably 1500 to 2500m/min, and even more preferably 2000 m/min.

After the graphene/nylon fiber composite material is obtained, the method preferably further comprises the step of spinning the graphene/nylon fiber composite material to obtain the graphene/nylon composite fabric.

The parameters of the spinning are not particularly limited in the present invention, and the spinning parameters known to those skilled in the art can be adopted.

The invention further provides the graphene/nylon fiber composite material prepared by the preparation method in the technical scheme, the graphene/nylon fiber composite material is formed by uniformly dispersing graphene sheets in a nylon matrix, and the thickness of the graphene sheets is 2-50 nm.

According to the graphene/nylon fiber composite material, the graphene is uniformly dispersed in the nylon matrix, so that the composite material can be rapidly heated under the irradiation of an infrared lamp; meanwhile, the graphene nanosheets are very thin, so that the graphene nanosheets have a good antibacterial effect on escherichia coli and staphylococcus aureus.

The invention also provides application of the graphene/nylon fiber composite material in the warm-keeping collar area. The composite material provided by the invention has excellent antibacterial property, and can be rapidly heated under the irradiation of an infrared lamp, so that the composite material is expected to be applied to the field of thermal underwear.

The graphene/nylon fiber composite material and the preparation method and application thereof provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.