CN111172764A - Method for preparing Kevlar nanofiber/carbon nanotube composite reinforced fiber - Google Patents
Method for preparing Kevlar nanofiber/carbon nanotube composite reinforced fiber Download PDFInfo
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- CN111172764A CN111172764A CN202010091264.8A CN202010091264A CN111172764A CN 111172764 A CN111172764 A CN 111172764A CN 202010091264 A CN202010091264 A CN 202010091264A CN 111172764 A CN111172764 A CN 111172764A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/59—Polyamides; Polyimides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
Abstract
A method for compounding and reinforcing fiber by Kevlar nano fiber/carbon nano tube relates to a method for reinforcing fiber. The invention aims to solve the problems that the prior Kevlar fiber has low reactivity and is difficult to further improve the tensile strength by a surface chemical modification method. The method comprises the following steps: firstly, pretreating Kevlar fibers; secondly, preparing a Kevlar nanofiber solution; thirdly, preparing a Kevlar nanofiber/carbon nanotube mixed dispersion liquid; and fourthly, carrying out ultrasonic treatment and drying to obtain the Kevlar nanofiber/carbon nanotube composite reinforced fiber. The preparation process is simple and feasible, the conditions are mild, and particularly the Kevlar fiber is difficult to modify by a chemical method, other chemical reactions or redundant chemical components are not needed, and the carbon nano tube can be stably modified on the surface of the Kevlar fiber by only utilizing the bulk nano fiber, so that the effect of enhancing the Kevlar fiber is achieved. The invention can obtain the Kevlar nanofiber/carbon nanotube composite reinforced fiber.
Description
Technical Field
The present invention relates to a method of reinforcing fibers.
Background
Since ancient times, human life is closely related to fiber, and natural fibers such as cotton and hemp are used worldwide. The development of chemical fiber goes through three stages of artificial fiber, synthetic fiber and chemical fiber, and along with the improvement of fiber production technology, not only fiber products occupy greater and greater specific gravity in the market, but also the application of the fiber is deep in various fields. As an important basic engineering material, the performance of the fiber needs to be higher standard while the chemical industry and the material science develop.
In recent years, the development of composite disciplines and the development of nanocomposites have made tremendous progress, mainly thanks to the increasing development of nanomaterials and nanotechnology. The emergence of nanomaterials with a variety of shapes, sizes and compositions lays a solid foundation for the design, research and development of multifunctional composites. Composite materials composed of nanomaterials such as nanotubes, nanoflakes, nanofibers, etc. may combine two or more of the excellent properties of the raw materials used, such as good mechanical or thermal stability after the inherently unstable materials are compounded with the nanomaterials. When the nano material is used as a reinforcing phase, the matrix material can be endowed with outstanding properties, and some characteristics inherent to the material can be maintained or improved.
Kevlar fiber is a high performance fiber material developed by Dupont, Inc. in the twentieth sixty years. It belongs to para-type aromatic polyamide organic fiber, and has the advantages of high strength, low density, high temperature stability, chemical corrosion resistance, etc. The specific gravity of the Kevlar fiber is only 1.44g/cm3Only 1/5 of steel and 1/2 of glass fiber, but the strength is 5 times of steel and 2 times of glass fiber. These properties are outstanding among known fiber materials, but the tensile strength of kevlar fibers is still not usable in specific applications, and the tensile strength of kevlar fibers needs to be further improved, but the kevlar fibers have low reactivity and are difficult to further improve by a surface chemical modification method.
Disclosure of Invention
The invention aims to solve the problems that the existing Kevlar fiber is low in reaction activity and the tensile strength of the Kevlar fiber is difficult to further improve by a surface chemical modification method, and provides a method for preparing a Kevlar nanofiber/carbon nanotube composite reinforcing fiber.
A method for preparing Kevlar nano fiber/carbon nano tube composite reinforced fiber is completed according to the following steps:
firstly, pretreatment of Kevlar fiber:
immersing Kevlar fibers into N-methyl pyrrolidone for ultrasonic treatment, and immersing the Kevlar fibers subjected to ultrasonic treatment into the N-methyl pyrrolidone again to obtain pretreated Kevlar fibers;
secondly, preparing a Kevlar nanofiber solution:
dissolving KOH into dimethyl sulfoxide to obtain a KOH/dimethyl sulfoxide solution;
②, immersing the pretreated Kevlar fiber into a KOH/dimethyl sulfoxide solution to obtain a Kevlar fiber/KOH/dimethyl sulfoxide mixed solution;
③, stirring and reacting the Kevlar fiber/KOH/dimethyl sulfoxide mixed solution for 5 to 7 days at room temperature to obtain a Kevlar nanofiber solution;
adding carbon nano tubes into the Kevlar nanofiber solution under the stirring condition, and performing ultrasonic treatment to obtain a Kevlar nanofiber/carbon nano tube mixed dispersion liquid;
the mass of the carbon nano tube in the Kevlar nano fiber/carbon nano tube mixed dispersion liquid in the third step accounts for 2-3% of the mass of the Kevlar nano fiber;
and fourthly, firstly, immersing the pretreated Kevlar fiber into the Kevlar nanofiber/carbon nano tube mixed dispersion liquid for treatment, then taking out the Kevlar fiber, and finally drying in an air environment to obtain the Kevlar nanofiber/carbon nano tube composite reinforced fiber.
The principle and the advantages of the invention are as follows:
firstly, the invention combines the Kevlar nano-fiber and the carbon nano-tube into the nano-composite material by utilizing the pi-pi conjugation effect, and then the carbon nano-tube is stably decorated on the surface of the Kevlar fiber by means of the hydrogen bond effect between the Kevlar nano-fiber and the Kevlar fiber. Finally, the Kevlar nano-fiber and the carbon nano-tube can achieve the effect of synergistic enhancement on the Kevlar fiber;
the preparation process is simple and feasible, the conditions are mild, and particularly the Kevlar fiber is difficult to modify by a chemical method, other chemical reactions or redundant chemical components are not needed, and the carbon nano tube can be stably modified on the surface of the Kevlar fiber by only utilizing the body nano fiber, so that the effect of enhancing the Kevlar fiber is achieved;
and thirdly, the tensile strength of the Kevlar nanofiber/carbon nanotube composite reinforced fiber prepared by the method can be improved by 0.33GPa compared with that of the original Kevlar fiber.
The invention can obtain the Kevlar nanofiber/carbon nanotube composite reinforced fiber.
Detailed Description
The first embodiment is as follows: the embodiment is a method for preparing Kevlar nano fiber/carbon nano tube composite reinforced fiber, which is completed according to the following steps:
firstly, pretreatment of Kevlar fiber:
immersing Kevlar fibers into N-methyl pyrrolidone for ultrasonic treatment, and immersing the Kevlar fibers subjected to ultrasonic treatment into the N-methyl pyrrolidone again to obtain pretreated Kevlar fibers;
secondly, preparing a Kevlar nanofiber solution:
dissolving KOH into dimethyl sulfoxide to obtain a KOH/dimethyl sulfoxide solution;
②, immersing the pretreated Kevlar fiber into a KOH/dimethyl sulfoxide solution to obtain a Kevlar fiber/KOH/dimethyl sulfoxide mixed solution;
③, stirring and reacting the Kevlar fiber/KOH/dimethyl sulfoxide mixed solution for 5 to 7 days at room temperature to obtain a Kevlar nanofiber solution;
adding carbon nano tubes into the Kevlar nanofiber solution under the stirring condition, and performing ultrasonic treatment to obtain a Kevlar nanofiber/carbon nano tube mixed dispersion liquid;
the mass of the carbon nano tube in the Kevlar nano fiber/carbon nano tube mixed dispersion liquid in the third step accounts for 2-3% of the mass of the Kevlar nano fiber;
and fourthly, firstly, immersing the pretreated Kevlar fiber into the Kevlar nanofiber/carbon nano tube mixed dispersion liquid for treatment, then taking out the Kevlar fiber, and finally drying in an air environment to obtain the Kevlar nanofiber/carbon nano tube composite reinforced fiber.
The principle and advantages of the embodiment are as follows:
firstly, the embodiment combines the Kevlar nanofiber and the carbon nanotube into a nano composite material by utilizing the pi-pi conjugation effect, then the carbon nanotube is stably modified on the surface of the Kevlar fiber by virtue of the hydrogen bond effect between the Kevlar nanofiber and the Kevlar fiber, and finally, the Kevlar nanofiber and the carbon nanotube can achieve the synergistic enhancement effect on the Kevlar fiber;
the preparation process is simple and feasible, the conditions are mild, and particularly the Kevlar fiber is difficult to modify by a chemical method, other chemical reactions or redundant chemical components are not needed, and the carbon nano tube can be stably modified on the surface of the Kevlar fiber by only utilizing the body nano fiber, so that the effect of enhancing the Kevlar fiber is achieved;
thirdly, the tensile strength of the Kevlar nanofiber/carbon nanotube composite reinforcing fiber prepared by the embodiment can be improved by 0.33GPa compared with the tensile strength of the original Kevlar fiber.
The embodiment can obtain the Kevlar nanofiber/carbon nanotube composite reinforced fiber.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: in the first step, the Kevlar fiber is immersed into N-methyl pyrrolidone for ultrasonic treatment for 20-40 min, and the ultrasonic power is 200-400W. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and the Kevlar fiber after ultrasonic treatment in the step one is immersed in the N-methyl pyrrolidone again for 10 to 14 hours. The other steps are the same as in the first or second embodiment.
fourth embodiment the difference between this embodiment and the first to third embodiments is that the concentration of the KOH/dimethyl sulfoxide solution in the second step ① is 3 mg/mL-5 mg/mL, and the other steps are the same as in the first to third embodiments.
fifth embodiment A difference between the first to fourth embodiments is that the concentration of the Kevlar fiber in the Kevlar fiber/KOH/dimethyl sulfoxide mixed solution in the second step is 2 to 8mg/mL, and the other steps are the same as in the first to fourth embodiments.
sixth embodiment a sixth embodiment is different from the first to fifth embodiments in that the second step and the third step are performed at a stirring speed of 200r/min to 1500r/min, and the other steps are the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the stirring speed in the third step is 500 r/min-2000 r/min. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the ultrasonic treatment power in the step three is 200W-400W, and the ultrasonic time is 20 min-40 min. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: in the fourth step, the pretreated Kevlar fiber is firstly immersed into the Kevlar nano fiber/carbon nano tube mixed dispersion liquid for treatment for 10 s-30 min. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: the drying temperature in the fourth step is 85-120 ℃, and the drying time is 4-6 h. The other steps are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: a method for preparing Kevlar nano fiber/carbon nano tube composite reinforced fiber is completed according to the following steps:
firstly, pretreatment of Kevlar fiber:
immersing Kevlar fiber (Kevlar-29) into N-methyl pyrrolidone for ultrasonic treatment for 30min, and immersing the Kevlar fiber subjected to ultrasonic treatment into the N-methyl pyrrolidone for 12h again to obtain pretreated Kevlar fiber;
in the first step, the Kevlar fiber is immersed into N-methyl pyrrolidone, and the ultrasonic power of ultrasonic treatment is 400W;
secondly, preparing a Kevlar nanofiber solution:
dissolving KOH into dimethyl sulfoxide to obtain a KOH/dimethyl sulfoxide solution;
the concentration of the KOH/dimethyl sulfoxide solution in the second step ① is 4 mg/mL;
②, immersing the pretreated Kevlar fiber into a KOH/dimethyl sulfoxide solution to obtain a Kevlar fiber/KOH/dimethyl sulfoxide mixed solution;
the concentration of the Kevlar fiber in the Kevlar fiber/KOH/dimethyl sulfoxide mixed solution in the second step ② is 2 mg/mL;
stirring and reacting the Kevlar fiber/KOH/dimethyl sulfoxide mixed solution for 6 days at room temperature to obtain a Kevlar nanofiber solution;
the stirring speed is 1500 r/min;
adding carbon nano tubes into the Kevlar nanofiber solution under the condition that the stirring speed is 1500r/min, and carrying out ultrasonic treatment for 30min to obtain a Kevlar nanofiber/carbon nano tube mixed dispersion liquid;
the power of ultrasonic treatment in the third step is 400W;
the mass of the carbon nano tube in the Kevlar nano fiber/carbon nano tube mixed dispersion liquid in the third step accounts for 2.5 percent of the mass of the Kevlar nano fiber;
soaking the pretreated Kevlar fiber into the Kevlar nanofiber/carbon nanotube mixed dispersion liquid for treatment, then taking out the Kevlar fiber, and finally drying in an air environment to obtain the Kevlar nanofiber/carbon nanotube composite reinforced fiber;
in the fourth step, firstly, the pretreated Kevlar fiber is immersed into the Kevlar nano fiber/carbon nano tube mixed dispersion liquid for treatment for 10 s;
the drying temperature in the fourth step is 100 ℃, and the drying time is 5 hours.
Determination of tensile Strength: the tensile strength of the Kevlar nanofibers and the Kevlar nanofiber/carbon nanotube composite reinforcing fibers prepared in example one was measured using an electronic universal tester at a test speed of 5 mm/min. The results are as follows: the original Kevlar fiber tensile strength is 3.08GPa, and the Kevlar nanofiber/carbon nanotube composite reinforcing fiber prepared by using the Kevlar nanofiber solution with the concentration of 2mg/mL in the first embodiment has the tensile strength of 3.41 GPa.
Example two: a method for preparing Kevlar nano fiber/carbon nano tube composite reinforced fiber is completed according to the following steps:
firstly, pretreatment of Kevlar fiber:
immersing Kevlar fibers into N-methyl pyrrolidone for ultrasonic treatment for 30min, and immersing the Kevlar fibers subjected to ultrasonic treatment into the N-methyl pyrrolidone for 12h again to obtain pretreated Kevlar fibers;
in the first step, the Kevlar fiber is immersed into N-methyl pyrrolidone, and the ultrasonic power of ultrasonic treatment is 400W;
secondly, preparing a Kevlar nanofiber solution:
dissolving KOH into dimethyl sulfoxide to obtain a KOH/dimethyl sulfoxide solution;
the concentration of the KOH/dimethyl sulfoxide solution in the second step ① is 4 mg/mL;
②, immersing the pretreated Kevlar fiber into a KOH/dimethyl sulfoxide solution to obtain a Kevlar fiber/KOH/dimethyl sulfoxide mixed solution;
the concentration of the Kevlar fiber in the Kevlar fiber/KOH/dimethyl sulfoxide mixed solution in the second step ② is 6 mg/mL;
stirring and reacting the Kevlar fiber/KOH/dimethyl sulfoxide mixed solution for 7 days at room temperature to obtain a Kevlar nanofiber solution;
the stirring speed is 1500 r/min;
adding carbon nano tubes into the Kevlar nanofiber solution under the condition that the stirring speed is 1500r/min, and then carrying out ultrasonic treatment for 30min to obtain a Kevlar nanofiber/carbon nano tube mixed dispersion liquid;
the power of ultrasonic treatment in the third step is 400W;
the mass of the carbon nano tube in the Kevlar nano fiber/carbon nano tube mixed dispersion liquid in the third step accounts for 2.5 percent of the mass of the Kevlar nano fiber;
soaking the pretreated Kevlar fiber into the Kevlar nanofiber/carbon nanotube mixed dispersion liquid for treatment for 10s, taking out the Kevlar fiber, and finally drying in an air environment to obtain the Kevlar nanofiber/carbon nanotube composite reinforced fiber;
the drying temperature in the fourth step is 100 ℃, and the drying time is 5 hours.
Determination of tensile Strength: the tensile strength of the Kevlar nanofiber and the Kevlar nanofiber/carbon nanotube composite reinforcing fiber prepared in example two was measured using an electronic universal tester at a test speed of 5 mm/min. The results are as follows: the original Kevlar fiber tensile strength is 3.08GPa, and the Kevlar nanofiber/carbon nanotube composite reinforcing fiber prepared by the Kevlar nanofiber solution with the concentration of 6mg/mL in the second embodiment has the tensile strength of 3.25 GPa.
Claims (10)
1. A method for preparing Kevlar nano fiber/carbon nano tube composite reinforced fiber is characterized in that the method for preparing the Kevlar nano fiber/carbon nano tube composite reinforced fiber is completed according to the following steps:
firstly, pretreatment of Kevlar fiber:
immersing Kevlar fibers into N-methyl pyrrolidone for ultrasonic treatment, and immersing the Kevlar fibers subjected to ultrasonic treatment into the N-methyl pyrrolidone again to obtain pretreated Kevlar fibers;
secondly, preparing a Kevlar nanofiber solution:
dissolving KOH into dimethyl sulfoxide to obtain a KOH/dimethyl sulfoxide solution;
②, immersing the pretreated Kevlar fiber into a KOH/dimethyl sulfoxide solution to obtain a Kevlar fiber/KOH/dimethyl sulfoxide mixed solution;
③, stirring and reacting the Kevlar fiber/KOH/dimethyl sulfoxide mixed solution for 5 to 7 days at room temperature to obtain a Kevlar nanofiber solution;
adding carbon nano tubes into the Kevlar nanofiber solution under the stirring condition, and performing ultrasonic treatment to obtain a Kevlar nanofiber/carbon nano tube mixed dispersion liquid;
the mass of the carbon nano tube in the Kevlar nano fiber/carbon nano tube mixed dispersion liquid in the third step accounts for 2-3% of the mass of the Kevlar nano fiber;
and fourthly, firstly, immersing the pretreated Kevlar fiber into the Kevlar nanofiber/carbon nano tube mixed dispersion liquid for treatment, then taking out the Kevlar fiber, and finally drying in an air environment to obtain the Kevlar nanofiber/carbon nano tube composite reinforced fiber.
2. The method of claim 1, wherein the Kevlar fiber is immersed in N-methyl pyrrolidone for ultrasonic treatment for 20-40 min at 200-400W in the first step.
3. The method of claim 1, wherein the time for immersing the Kevlar fiber subjected to the ultrasonic treatment in the N-methylpyrrolidone again is 10-14 h.
4. the method of claim 1, wherein the concentration of the KOH/DMSO solution in the second step is 3 mg/mL-5 mg/mL.
5. the method of claim 1, wherein the concentration of the Kevlar fiber in the Kevlar fiber/KOH/dimethyl sulfoxide mixture in the second step is 2mg/mL to 8 mg/mL.
6. the method of claim 1, wherein the stirring speed in the second step is 200-1500 r/min.
7. The method of claim 1, wherein the stirring speed in step three is 500r/min to 2000 r/min.
8. The method of claim 1, wherein the power of the ultrasonic treatment in step three is 200W-400W, and the ultrasonic time is 20 min-40 min.
9. The method of claim 1, wherein the step four comprises immersing the pretreated Kevlar fiber in the Kevlar nanofiber/carbon nanotube mixed dispersion for 10 s-30 min.
10. The method of claim 1, wherein the drying temperature is 85-120 ℃ and the drying time is 4-6 h.
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| US20230134231A1 (en) * | 2021-11-01 | 2023-05-04 | Wisconsin Alumni Research Foundation | Carbon-based composite materials with enhanced dynamic performance |
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