CN111593555A - Method for modifying aramid fiber by combining plasma with dopamine - Google Patents
Method for modifying aramid fiber by combining plasma with dopamine Download PDFInfo
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- CN111593555A CN111593555A CN202010602028.8A CN202010602028A CN111593555A CN 111593555 A CN111593555 A CN 111593555A CN 202010602028 A CN202010602028 A CN 202010602028A CN 111593555 A CN111593555 A CN 111593555A
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- 229920006231 aramid fiber Polymers 0.000 title claims abstract description 41
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229960003638 dopamine Drugs 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000000835 fiber Substances 0.000 claims abstract description 45
- 238000001035 drying Methods 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 238000009832 plasma treatment Methods 0.000 claims abstract 2
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims 1
- 239000003822 epoxy resin Substances 0.000 abstract description 12
- 229920000647 polyepoxide Polymers 0.000 abstract description 12
- 239000002131 composite material Substances 0.000 abstract description 10
- 229920001690 polydopamine Polymers 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 abstract 1
- 238000002715 modification method Methods 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- 229920005989 resin Polymers 0.000 description 11
- 239000011347 resin Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 238000002791 soaking Methods 0.000 description 9
- 239000007983 Tris buffer Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 6
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 229960001149 dopamine hydrochloride Drugs 0.000 description 5
- 238000012681 fiber drawing Methods 0.000 description 5
- 238000007586 pull-out test Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000004760 aramid Substances 0.000 description 3
- 229920003235 aromatic polyamide Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/368—Hydroxyalkylamines; Derivatives thereof, e.g. Kritchevsky bases
-
- 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
-
- 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
The invention provides a method for modifying aramid fiber by combining plasma with dopamine, aiming at the problem of poor interfacial adhesion of aramid fiber and epoxy resin. The plasma pretreatment time is 2 minutes, and the concentration of the dopamine solution is 2 g/L. Removing impurities on the surface of the aramid fiber by using absolute ethyl alcohol and then drying; carrying out plasma treatment on the fiber; and (3) dipping the treated aramid fiber in a dopamine solution to form a polydopamine coating on the surface. The strength of the modified aramid fiber prepared by the method is enhanced by 1.4%, and the shearing strength of the fiber interface is improved by 20.6% in an epoxy resin composite material drawing experiment. The fiber treated by the modification method effectively improves the mechanical property of the composite material prepared by the fiber, and has wide application prospect in various fields such as military, building industry and the like.
Description
Technical Field
The invention relates to a method for improving the interfacial adhesion of modified aramid fiber and epoxy resin, provides a theoretical basis for the subsequent mechanical property research of aramid fiber composite materials, and belongs to the technical field of aramid fiber composite material science.
Background
Among various varieties of aramid fibers, para-aramid (aramid 1414) has the most excellent comprehensive performance, and the aramid has excellent performances of high strength, high modulus, high temperature resistance, chemical corrosion resistance and the like due to a rigid macromolecular structure, is often used as a composite material reinforcement and is widely applied to the fields of aerospace, military, traffic, protective articles and the like.
Due to the conjugation effect between the molecular connecting segments of the aramid fiber and the steric effect of the benzene ring, the activity of the surface group is low, the molecular chain is in a rigid extended state, the structural characteristic leads the fiber surface to be smooth, the aramid fiber is not easy to combine with a matrix in the preparation process of the composite material, the interface performance of the fiber influences the overall performance of the composite material, and the exertion of the excellent performance of the aramid fiber is limited. Therefore, aramid fiber surface modification is of great importance.
Dopamine molecules contain catechol groups and amino groups with high activity, and the dopamine molecules can be oxidized and polymerized at normal temperature, so that a thin polydopamine coating can be deposited on the surface of a fiber and serves as a bridge between the fiber and a matrix. The poly dopamine layer contains a large number of active hydrophilic groups, amino groups and hydroxyl groups in molecules, so that the surface performance of the base material can be improved, and the poly dopamine layer can be used as a transition layer and further grafted with other functional groups to functionalize the material.
The invention adopts the methods of plasma pretreatment and dopamine coating modification to roughen the surface of the fiber and increase the surface groups so as to increase the surface energy and further improve the surface adhesion of the fiber and the epoxy resin. After fiber stretching and contact angle tests and fiber drawing tests, the method is proved to have great improvement on the binding force of aramid fiber and epoxy resin under the condition that the strength of the aramid fiber is not reduced greatly, and the method can be used for simply realizing the reinforcement of the composite material and can also be used for carrying out subsequent analysis research on the basis of the mechanical property of the composite material.
Disclosure of Invention
The invention provides a method for improving the interfacial adhesion between aramid fiber and epoxy resin by modifying the aramid fiber, aiming at the problem of poor adhesion between the aramid fiber and the epoxy resin. In order to achieve the purpose of the present invention, the inventor finally obtains the following technical scheme through a great amount of experimental research and continuous exploration:
a method for modifying aramid fiber by combining plasma with dopamine comprises the following steps:
(1) pretreating aramid fiber in an absolute ethyl alcohol solution to remove impurities on the surface of the fiber, repeatedly cleaning the fiber with deionized water, and drying the fiber for 1 hour at 30 ℃ for later use;
(2) plasma pretreatment: and (3) putting the cleaned aramid fiber into a plasma degumming machine, and respectively processing for 0, 1, 2 and 3 minutes in an oxygen environment at the pressure of 40Pa and the power of 50W.
(3) A2 g/l dopamine hydrochloride solution was prepared and the pH of the solution was adjusted to 8.5 with Tris (Tris buffer). And then putting the aramid fiber pretreated by the plasma into a dopamine solution, soaking for 24h, taking out, washing for 3-5 times by using deionized water, and drying for 2h at 60 ℃.
(4) The strength of the modified fiber, the contact angle of the fiber surface and the drawing force of the modified fiber in the resin were tested.
The preferred plasma pretreatment time is 2 minutes.
During plasma pretreatment, the pressure is 40Pa and the power is 50W under the oxygen environment.
The concentration of the dopamine solution is 2 g/L.
The oven drying temperature was 60 ℃ for 2 hours.
The resin is epoxy resin GCC-135, and the curing agent is GCC-137 curing agent.
Compared with the unmodified aramid fiber, the aramid fiber of the invention has the advantages that the strength of the fiber is improved by 1.4 percent, the interfacial shear strength is improved by 20.6 percent, the interfacial cohesiveness between the fiber and the resin is effectively improved, and the performance of the subsequent composite material is better.
Drawings
Fig. 1 is SEM images of dopamine modified fiber at different plasma pretreatment times, fig. 2 is a contact angle of the modified fiber, fig. 3 is a tensile property parameter of the modified fiber, and fig. 4 is a drawing property parameter of the modified fiber.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
(1) Fiber modification treatment
Soaking aramid fiber in absolute ethyl alcohol for 4 hours, repeatedly cleaning with deionized water, drying in a drying oven at 60 ℃, and sealing for later use. And (3) putting the cleaned aramid fiber into a plasma degumming machine, and treating for 0 minute in an oxygen environment at the pressure of 40Pa and the power of 50W. Preparing 2g/L dopamine hydrochloride solution, adjusting the pH value of the solution to 8.5 by using a TRIS buffer, putting the aramid fiber pretreated by the plasma into the dopamine solution, soaking for 24 hours, then washing for 3-5 times by using deionized water, and drying in an oven at 60 ℃ for 2 hours.
(2) Fiber pull-out test in resin
The resin was prepared according to the ratio of epoxy resin GCC-135 to curing agent GCC-137 of 100: 30, and injected into a fiber drawing apparatus to test the drawing force.
(3) Fiber strength test
The strength of the fibers was measured using a single fiber strength tester and 5 groups were averaged.
Example 2
(1) Fiber modification treatment
Soaking aramid fiber in absolute ethyl alcohol for 4 hours, repeatedly cleaning with deionized water, drying in a drying oven at 60 ℃, and sealing for later use. And (3) putting the cleaned aramid fiber into a plasma degumming machine, and treating for 1 minute in an oxygen environment at the pressure of 40Pa and the power of 50W. Preparing 2g/L dopamine hydrochloride solution, adjusting the pH value of the solution to 8.5 by using a TRIS buffer, putting the aramid fiber pretreated by the plasma into the dopamine solution, soaking for 24 hours, then washing for 3-5 times by using deionized water, and drying in an oven at 60 ℃ for 2 hours.
(3) Fiber pull-out test in resin
The resin was prepared according to the ratio of epoxy resin GCC-135 to curing agent GCC-137 of 100: 30, and injected into a fiber drawing apparatus to test the drawing force.
(3) Fiber strength test
The strength of the fibers was measured using a single fiber strength tester and 5 groups were averaged.
Example 3
(1) Fiber modification treatment
Soaking aramid fiber in absolute ethyl alcohol for 4 hours, repeatedly cleaning with deionized water, drying in a drying oven at 60 ℃, and sealing for later use. And (3) putting the cleaned aramid fiber into a plasma degumming machine, and treating for 2 minutes in an oxygen environment at the pressure of 40Pa and the power of 50W. Preparing 2g/L dopamine hydrochloride solution, adjusting the pH value of the solution to 8.5 by using a TRIS buffer, putting the aramid fiber pretreated by the plasma into the dopamine solution, soaking for 24 hours, then washing for 3-5 times by using deionized water, and drying in an oven at 60 ℃ for 2 hours.
(2) Fiber pull-out test in resin
The resin was prepared according to the ratio of epoxy resin GCC-135 to curing agent GCC-137 of 100: 30, and injected into a fiber drawing apparatus to test the drawing force.
(3) Fiber strength test
The strength of the fibers was measured using a single fiber strength tester and 5 groups were averaged.
Example 4
(1) Fiber modification treatment
Soaking aramid fiber in absolute ethyl alcohol for 4 hours, repeatedly cleaning with deionized water, drying in a drying oven at 60 ℃, and sealing for later use. And (3) putting the cleaned aramid fiber into a plasma degumming machine, and treating for 3 minutes in an oxygen environment at the pressure of 40Pa and the power of 50W. Preparing 2g/L dopamine hydrochloride solution, adjusting the pH value of the solution to 8.5 by using a TRIS buffer, putting the aramid fiber pretreated by the plasma into the dopamine solution, soaking for 24 hours, then washing for 3-5 times by using deionized water, and drying in an oven at 60 ℃ for 2 hours.
(2) Fiber pull-out test in resin
The resin was prepared according to the ratio of epoxy resin GCC-135 to curing agent GCC-137 of 100: 30, and injected into a fiber drawing apparatus to test the drawing force.
(3) Fiber strength test
The strength of the fibers was measured using a single fiber strength tester and 5 groups were averaged.
TABLE 1 fiber Performance test
Claims (4)
1. Removing impurities on the surface of the aramid fiber by using absolute ethyl alcohol, drying, and treating the fiber for 2min in a plasma degumming machine under the oxygen environment, the pressure of 40Pa and the power of 50W. Preparing 2g/L dopamine solution with the pH value of 8.5, putting the aramid fiber pretreated by the plasma into the modified solution, oxidizing and self-polymerizing for 24 hours at room temperature, then washing with deionized water, and drying for 2 hours at 30 ℃.
2. The method of claim 1, wherein the plasma pretreatment time is 2 minutes.
3. The method of claim 1, wherein the plasma treatment conditions are an oxygen environment, a pressure of 40Pa and a power of 50W.
4. The method for modifying aramid fiber by combining dopamine according to claim 1, wherein the drying temperature of a vacuum oven is 60 ℃ and the drying time is 2 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010602028.8A CN111593555A (en) | 2020-06-29 | 2020-06-29 | Method for modifying aramid fiber by combining plasma with dopamine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010602028.8A CN111593555A (en) | 2020-06-29 | 2020-06-29 | Method for modifying aramid fiber by combining plasma with dopamine |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114496349A (en) * | 2022-02-09 | 2022-05-13 | 浙江荣泰电工器材股份有限公司 | Ultra-long high-temperature-resistant mica tape and preparation method thereof |
| CN114523741A (en) * | 2022-04-19 | 2022-05-24 | 浙江荣泰电工器材股份有限公司 | High-strength high-tensile high-modulus mica plate for thermal runaway management of new energy automobile and preparation method thereof |
| CN114874471A (en) * | 2022-05-11 | 2022-08-09 | 江苏领瑞新材料科技有限公司 | Preparation method of aramid fiber multi-layer composite UD cloth |
| CN115819921A (en) * | 2022-11-14 | 2023-03-21 | 华北电力大学 | Preparation method and application of interface modified aramid fiber/epoxy resin composite material |
-
2020
- 2020-06-29 CN CN202010602028.8A patent/CN111593555A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114496349A (en) * | 2022-02-09 | 2022-05-13 | 浙江荣泰电工器材股份有限公司 | Ultra-long high-temperature-resistant mica tape and preparation method thereof |
| CN114496349B (en) * | 2022-02-09 | 2023-09-26 | 浙江荣泰电工器材股份有限公司 | Ultra-long high-temperature-resistant mica tape and preparation method thereof |
| CN114523741A (en) * | 2022-04-19 | 2022-05-24 | 浙江荣泰电工器材股份有限公司 | High-strength high-tensile high-modulus mica plate for thermal runaway management of new energy automobile and preparation method thereof |
| CN114523741B (en) * | 2022-04-19 | 2022-07-29 | 浙江荣泰电工器材股份有限公司 | High-strength high-tensile high-modulus mica plate for thermal runaway management of new energy automobile |
| CN114874471A (en) * | 2022-05-11 | 2022-08-09 | 江苏领瑞新材料科技有限公司 | Preparation method of aramid fiber multi-layer composite UD cloth |
| CN115819921A (en) * | 2022-11-14 | 2023-03-21 | 华北电力大学 | Preparation method and application of interface modified aramid fiber/epoxy resin composite material |
| CN115819921B (en) * | 2022-11-14 | 2024-03-08 | 华北电力大学 | Preparation method and application of interface modified aramid fiber/epoxy resin composite material |
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