CN111118896A - Modified aramid fiber and modified aramid fiber composite material - Google Patents
Modified aramid fiber and modified aramid fiber composite material Download PDFInfo
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- CN111118896A CN111118896A CN201911397141.0A CN201911397141A CN111118896A CN 111118896 A CN111118896 A CN 111118896A CN 201911397141 A CN201911397141 A CN 201911397141A CN 111118896 A CN111118896 A CN 111118896A
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- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
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- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
Abstract
The invention discloses a modified aramid fiber and a modified aramid fiber composite material. The modified aramid fiber is prepared by performing steps including pretreatment, plasma treatment, dopamine modification and silane coupling agent modification on aramid fabric. The modified aramid composite material is prepared by soaking modified aramid in a resin composition and drying to obtain prepregs, and then laminating at least one prepreg and hot-pressing. The modified aramid composite material has the advantages of good associativity, high tensile strength and the like.
Description
Technical Field
The invention belongs to the technical field of polymer fibers, and particularly relates to a modified aramid fiber and a modified aramid fiber composite material.
Background
The aromatic polyamide fiber is a synthetic high-performance fiber, which is abbreviated as aramid fiber. It is an alternating linear high molecular polymer formed by benzene rings and amide bonds. The U.S. Federal trade Commission defines at least 85% of amide bonds directly attached to two benzene rings and names them as Aramid fibers. The research on the application of aramid fiber is early in foreign countries, and the aramid fiber is firstly used as a special fiber in the industrial field, is applied to products needing special properties and special requirements, is not large in dosage generally, and is basically used as an auxiliary modified material. Du pont (DuPont) is a pioneer in the development and commercialization of aramid fibers in the united states, and du pont was successful in the development and commercialization of meta-aramid fibers in the 60's of the 20 th century under the trade name Nomex. Then, dupont successfully developed and commercialized para-aramid fiber under the trade name Kevlar. 85% of aramid fibers used in the current market are para-aramid fibers.
With the development and continuous research of scientific technology, the unique physical and chemical properties of aramid fibers attract the attention of researchers more and more, and the aramid fibers are called as all-round fibers due to the characteristics of high strength, high modulus, high temperature resistance, chemical corrosion resistance, wear resistance and the like, and can be used in various fields.
Due to the higher crystallinity and the steric hindrance of a benzene ring, the aramid fiber has limited application of smooth fiber surface, few active functional groups and low reactivity. Therefore, it has poor adhesion to most polymer matrices, and thus the application of aramid fibers is limited. Therefore, it is necessary to modify the surface of aramid fiber to improve the interfacial interaction between aramid fiber and the matrix material and to fully develop the excellent mechanical properties of aramid fiber.
Plasma treatment can modify aramid fiber, and certain changes can occur to the surface property of the treated fiber, so that the reactivity is improved, the surface energy is improved, new reactive groups are generated, the fiber can react with a polymer matrix, covalent chemical bond connection is formed, the interface action between the fiber and the matrix is improved, the surface etching is serious, the roughness is increased, and the interface bonding degree between the aramid fiber and the matrix can be greatly improved due to the changes. However, grooves and cracks with different degrees appear on the surface of the aramid fiber after plasma treatment, and the positions are relatively fragile, so that the tensile strength of the aramid fiber is reduced, the tensile strength of the aramid composite material is further influenced, and the mechanical property and reliability of the product are reduced.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a modified aramid fiber and a modified aramid fiber composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the modified aramid fiber is prepared by performing steps including pretreatment, plasma treatment, dopamine modification and silane coupling agent modification on aramid fabric.
Further, the pretreatment step is as follows: soaking aramid fabric in an organic solvent for a certain time, and then sequentially baking the soaked aramid fabric at low temperature and high temperature. The volatilization of the organic solvent can be accelerated by low-temperature baking, the oily impurities of the aramid fabric can be further removed by high-temperature baking, and the subsequent plasma treatment, dopamine modification and silane coupling agent modification effects can be improved by the soaking and baking steps.
Preferably, the aramid fabric is woven by aramid yarns with the thickness of 50-500 deniers.
Preferably, the organic solvent is one or more selected from acetone, butanone, methanol and ethanol, and the soaking time is 20-30 hours; more preferably, the organic solvent is prepared by mixing acetone and ethanol according to the mass ratio of 1:1, and the soaking time is 24 hours.
Preferably, the low-temperature baking temperature is 60-80 ℃, and the baking time is 8-12 hours; the high-temperature baking temperature is 180-220 ℃, and the baking time is 2-3 hours.
More preferably, the low-temperature baking temperature is 80 ℃, and the baking time is 10 hours; the high-temperature baking temperature is 200 ℃, and the baking time is 3 hours.
Further, the plasma processing comprises the following steps: and carrying out plasma treatment on the pretreated aramid fiber cloth, wherein helium is used as a gas, the vacuum degree is 20-100 pa, the power is 50-300 w, the gas flow is 10-30 ml per minute, and the treatment time is 5-30 minutes.
Preferably, the vacuum degree is 20pa, the power is 100w, the gas flow rate is 20ml per minute, and the treatment time is 15 minutes.
Further, the dopamine modification step is as follows: soaking the aramid fiber cloth subjected to plasma treatment in the treatment liquid A while ultrasonically stirring, and then cleaning and drying by using deionized water; the treating fluid A is prepared by dissolving tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine in deionized water, and ultrasonically stirring for 30 minutes to uniformly disperse the three components.
Preferably, the mass ratio of the treatment liquid A to the aramid cloth is 5:1, the soaking time is 2-6 hours, and the drying temperature is 60-80 ℃.
Preferably, the treatment liquid A contains 0.5-1% by mass of tris (hydroxymethyl) aminomethane, 0.2-0.4% by mass of hydrochloric acid and 0.5-1% by mass of dopamine; more preferably, the treatment liquid a contains 0.8% by mass of tris (hydroxymethyl) aminomethane, 0.3% by mass of hydrochloric acid, and 0.8% by mass of dopamine. The tris (hydroxymethyl) aminomethane in the treatment fluid can further maintain the stability of the solution, so that the treatment fluid A can fully react with the dopamine in the aramid fabric modification process, and the dopamine modification effect is improved.
Further, the silane coupling agent is modified by the following steps: soaking the dopamine-modified aramid fiber cloth in the treatment liquid B while ultrasonically stirring, and then washing and drying by using deionized water; the treatment liquid B consists of a silane coupling agent, an alcohol solvent and deionized water, and is uniformly dispersed by ultrasonic stirring for 30 minutes.
Preferably, the alcohol solvent is one or more of methanol, ethanol and ethylene glycol.
Preferably, the silane coupling agent is one or more of KH550, KH560, KH570, A1100, A174 and A187.
Preferably, the mass fraction of the deionized water in the treatment liquid B is 5-10%, the mass fraction of the silane coupling agent is 5-30%, and the balance is an alcohol solvent.
More preferably, the mass fraction of the deionized water is 5%, and the mass fraction of the coupling agent A174 is 20%. The alcohol solvent is ethanol.
Preferably, the mass ratio of the treating fluid B to the aramid fabric is 5:1, the soaking time is 5-30 minutes, and the drying temperature is 60-80 ℃.
The modified aramid composite material is prepared by soaking the modified aramid in a resin composition and drying to obtain a prepreg, and then laminating at least one prepreg and performing hot pressing.
Preferably, the resin composition comprises 80-120 parts of epoxy resin, 0.5-3 parts of curing agent, 0.05-0.5 part of accelerator and 20-60 parts of solvent; more preferably, the resin composition comprises 100 parts of epoxy resin, 2 parts of curing agent, 0.1 part of accelerator and 50 parts of solvent.
Preferably, the epoxy resin is selected from one or more of bisphenol A epoxy resin, brominated epoxy resin, phosphorus-containing epoxy resin, bifunctional epoxy resin and polyfunctional epoxy resin; the curing agent is selected from one or more than two of electronic grade dicyandiamide, 4-diamino diphenyl sulfone, ethylenediamine, hexanediamine, diethylenetriamine, maleic anhydride, phthalic anhydride, boron trifluoride ethylamine complex and phenolic resin; the accelerant is one or more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, DMP-30, triethanolamine, N-dimethylbenzylamine and boron trifluoride monoethylamine; the solvent is one or more selected from acetone, butanone, propylene glycol methyl ether acetate, N-dimethylformamide and toluene.
Preferably, ultrasonic stirring is carried out simultaneously in the dipping process for 5-10 minutes, the drying temperature is 120-180 ℃, and the fluidity of the prepreg is 5-20%.
Preferably, the hot pressing temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The invention has the following technical characteristics:
1. according to the invention, through sequentially carrying out plasma treatment, dopamine modification and silane coupling agent modification on aramid fibers, the effect of improving the aramid fiber reactivity by the plasma treatment is retained, and the side effect of reducing the tensile strength of aramid fibers after the plasma treatment is avoided, so that the modified aramid fiber composite material with good binding property and high tensile strength is prepared.
2. The sequence of the modification steps of the invention can not be changed at will, and the tensile property and the bonding property of the modified aramid fiber composite material can be improved to the maximum extent only by sequentially carrying out the modification steps.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
The plasma treatment time, the composition ratio of the treatment liquid A and the treatment liquid B in examples 1 to 4 of the present invention and comparative examples 1 to 13 are shown in Table 1.
Examples 1 to 3
The modified aramid composite material is realized by the following steps:
step one, the aramid fabric selected is woven by aramid yarn with the thickness of 300 deniers, and the aramid fabric is pretreated according to the following steps:
1.1 soaking aramid fabric in a mixture of acetone and ethanol in a mass ratio of 1:1 for 24 hours.
1.2 taking out the soaked aramid fiber cloth, and baking the aramid fiber cloth in an oven at the temperature of 80 ℃ for 10 hours
And 1.3, putting the baked aramid fiber cloth into a high-temperature oven, and baking for 3 hours at a high temperature of 200 ℃.
And step two, sequentially adding tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine into deionized water according to the proportion shown in the table 1, and ultrasonically stirring for 30 minutes to uniformly disperse the materials to obtain a treatment solution A.
And step three, sequentially adding deionized water and a silane coupling agent A174 into absolute ethyl alcohol according to the proportion shown in the table 1, and uniformly dispersing the mixture by ultrasonic stirring for 30 minutes to prepare a treatment solution B.
And step four, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
And fifthly, performing plasma treatment on the aramid fiber cloth pretreated in the first step for 15 minutes by using helium as gas, wherein the vacuum degree is 20pa, the power is 100w, and the gas flow is 20ml per minute.
And step six, soaking the aramid fiber cloth subjected to the plasma treatment in the treatment liquid A according to the table 1, stirring for 4 hours by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in a 60-DEG C drying oven.
And step seven, soaking the dried aramid fiber cloth in the treatment liquid B according to the table 1, stirring for 20 minutes by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in an oven at 60 ℃.
And step eight, soaking the treated aramid fiber cloth in the epoxy resin adhesive prepared in the step four, ultrasonically stirring for 10 minutes, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step nine, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The bonding performance of the modified aramid composite material is determined by a thermal shock test, the molded modified aramid composite material is immersed in a tin furnace at 300 ℃, the molded modified aramid composite material is taken out after being layered and cracked, the recording time is recorded, and the longer the thermal shock time is, the stronger the bonding performance of the modified aramid composite material is.
The tensile strength and the tensile modulus of the modified aramid composite material are determined according to GB/T1447-.
The test results are shown in Table 2.
Example 4
The modified aramid composite material can be realized by the following steps:
step one, the aramid fabric selected is woven by aramid yarn with the thickness of 300 deniers, and the aramid fabric is pretreated according to the following steps:
1.1 soaking aramid fabric in methanol for 24 hr.
1.2 taking out the soaked aramid fiber cloth, and baking the aramid fiber cloth in an oven at the temperature of 80 ℃ for 10 hours
And 1.3, putting the baked aramid fiber cloth into a high-temperature oven, and baking for 3 hours at a high temperature of 200 ℃.
And step two, sequentially adding tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine into deionized water according to the proportion shown in the table 1, and ultrasonically stirring for 30 minutes to uniformly disperse the materials to obtain a treatment solution A.
And step three, sequentially adding deionized water and a silane coupling agent A174 into absolute ethyl alcohol according to the proportion shown in the table 1, and uniformly dispersing the mixture by ultrasonic stirring for 30 minutes to prepare a treatment solution B.
And step four, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
And fifthly, performing plasma treatment on the aramid fiber cloth pretreated in the first step for 15 minutes by using helium as gas, wherein the vacuum degree is 20pa, the power is 100w, and the gas flow is 20ml per minute.
And step six, soaking the aramid fiber cloth subjected to the plasma treatment in the treatment liquid A according to the table 1, stirring for 4 hours by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in a 60-DEG C drying oven.
And step seven, soaking the dried aramid fiber cloth in the treatment liquid B according to the table 1, stirring for 20 minutes by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in an oven at 60 ℃.
And step eight, soaking the treated aramid fiber cloth in the epoxy resin adhesive prepared in the step four, stirring for 10 minutes by using ultrasonic waves, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step nine, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The test methods were as above, and the results are shown in Table 2.
Comparative examples 1 to 5, comparative examples 12 to 13
The modified aramid fiber and the composite material thereof which are not soaked in the treatment solution under different plasma treatment time can be realized by the following steps:
step one, the aramid fabric selected is woven by aramid yarn with the thickness of 300 deniers, and the aramid fabric is pretreated according to the following steps:
1.1 soaking aramid fabric in a mixture of acetone and ethanol in a mass ratio of 1:1 for 24 hours.
1.2 taking out the soaked aramid fiber cloth, and baking the aramid fiber cloth in an oven at the temperature of 80 ℃ for 10 hours
And 1.3, putting the baked aramid fiber cloth into a high-temperature oven, and baking for 3 hours at a high temperature of 200 ℃.
And step two, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
And step three, carrying out plasma treatment on the aramid fiber cloth pretreated in the step one, wherein helium is used as gas, the vacuum degree is 20pa, the power is 100w, the gas flow is 20ml per minute, and the plasma treatment is carried out correspondingly according to the table 1.
And step four, soaking the treated aramid fiber cloth in the epoxy resin adhesive prepared in the step two, stirring for 10 minutes by using ultrasonic waves, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step five, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The test methods were as above, and the results are shown in Table 2.
Comparative example 6
The aramid fiber modified by only soaking treatment liquid A and the composite material thereof can be realized by the following steps:
step one, the aramid fabric selected is woven by aramid yarn with the thickness of 300 deniers, and the aramid fabric is pretreated according to the following steps:
1.1 soaking aramid fabric in a mixture of acetone and ethanol in a mass ratio of 1:1 for 24 hours.
1.2 taking out the soaked aramid fiber cloth, and baking the aramid fiber cloth in an oven at the temperature of 80 ℃ for 10 hours
And 1.3, putting the baked aramid fiber cloth into a high-temperature oven, and baking for 3 hours at a high temperature of 200 ℃.
And step two, sequentially adding tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine into deionized water according to the proportion shown in the table 1, and ultrasonically stirring for 30 minutes to uniformly disperse the materials to obtain a treatment solution A.
And step three, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
And step four, carrying out plasma treatment on the aramid fiber cloth pretreated in the step one, wherein helium is used as gas, the vacuum degree is 20pa, the power is 100w, the gas flow is 20ml per minute, and the treatment time is 15 minutes.
And step five, soaking the aramid fiber cloth subjected to the plasma treatment in the treatment liquid A according to the table 1, stirring for 4 hours by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in a 60-DEG C drying oven.
And step six, soaking the treated aramid fiber cloth in the epoxy resin adhesive prepared in the step three, stirring for 10 minutes by using ultrasonic waves, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step seven, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The test methods were as above, and the results are shown in Table 2.
Comparative example 7
The aramid fiber modified by only soaking treatment liquid B and the composite material thereof can be realized by the following steps:
step one, the aramid fabric selected is woven by aramid yarn with the thickness of 300 deniers, and the aramid fabric is pretreated according to the following steps:
1.1 soaking aramid fabric in a mixture of acetone and ethanol in a mass ratio of 1:1 for 24 hours.
1.2 taking out the soaked aramid fiber cloth, and baking the aramid fiber cloth in an oven at the temperature of 80 ℃ for 10 hours
And 1.3, putting the baked aramid fiber cloth into a high-temperature oven, and baking for 3 hours at a high temperature of 200 ℃.
And step two, sequentially adding deionized water and a silane coupling agent A174 into absolute ethyl alcohol according to the proportion shown in the table 1, and uniformly dispersing the mixture by ultrasonic stirring for 30 minutes to prepare a treatment solution B.
And step three, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
And step four, carrying out plasma treatment on the aramid fiber cloth pretreated in the step one, wherein helium is used as gas, the vacuum degree is 20pa, the power is 100w, the gas flow is 20ml per minute, and the treatment time is 15 minutes.
And step five, soaking the dried aramid fiber cloth in the treatment liquid B according to the table 1, stirring for 20 minutes by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in an oven at 60 ℃.
And step six, soaking the treated aramid fiber cloth in the epoxy resin adhesive prepared in the step three, stirring for 10 minutes by using ultrasonic waves, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step seven, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The test methods were as above, and the results are shown in Table 2.
Comparative example 8
The sequential modification of aramid fiber and composite material thereof by replacing soaking treatment liquid can be realized by the following steps:
step one, the aramid fabric selected is woven by aramid yarn with the thickness of 300 deniers, and the aramid fabric is pretreated according to the following steps:
1.1 soaking aramid fabric in a mixture of acetone and ethanol in a mass ratio of 1:1 for 24 hours.
1.2 taking out the soaked aramid fiber cloth, and baking the aramid fiber cloth in an oven at the temperature of 80 ℃ for 10 hours
And 1.3, putting the baked aramid fiber cloth into a high-temperature oven, and baking for 3 hours at a high temperature of 200 ℃.
And step two, sequentially adding tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine into deionized water according to the proportion shown in the table 1, and ultrasonically stirring for 30 minutes to uniformly disperse the materials to obtain a treatment solution A.
And step three, sequentially adding deionized water and a silane coupling agent A174 into absolute ethyl alcohol according to the proportion shown in the table 1, and uniformly dispersing the mixture by ultrasonic stirring for 30 minutes to prepare a treatment solution B.
And step four, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
And fifthly, performing plasma treatment on the aramid fiber cloth pretreated in the first step for 15 minutes by using helium as gas, wherein the vacuum degree is 20pa, the power is 100w, and the gas flow is 20ml per minute.
And step six, soaking the dried aramid fiber cloth in the treatment liquid B according to the table 1, stirring for 20 minutes by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in an oven at 60 ℃.
And step seven, soaking the aramid fiber cloth subjected to the plasma treatment in the treatment liquid A according to the table 1, stirring for 4 hours by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in a 60-DEG C drying oven.
And step eight, soaking the treated aramid fiber cloth in the epoxy resin adhesive prepared in the step four, stirring for 10 minutes by using ultrasonic waves, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step nine, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The test methods were as above, and the results are shown in Table 2.
Comparative example 9
The pretreatment-free modified aramid fiber and the composite material thereof can be realized by the following steps:
step one, sequentially adding tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine into deionized water according to the proportion shown in table 1, and ultrasonically stirring for 30 minutes to uniformly disperse the three to obtain a treatment solution A.
And step two, sequentially adding deionized water and a silane coupling agent A174 into absolute ethyl alcohol according to the proportion shown in the table 1, and uniformly dispersing the mixture by ultrasonic stirring for 30 minutes to prepare a treatment solution B.
And step three, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
Soaking the aramid fiber cloth subjected to the plasma treatment in the treatment liquid A according to the table 1, stirring for 4 hours by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in an oven at 60 ℃.
And step five, the selected aramid cloth is woven by aramid yarns with the thickness of 300 deniers, the dried aramid cloth is soaked in the treatment liquid B according to the table 1 and is ultrasonically stirred for 20 minutes, and the aramid cloth is taken out and is washed by deionized water and is dried in an oven at the temperature of 60 ℃.
And step six, performing plasma treatment on the aramid fiber cloth for 15 minutes, wherein helium is used as gas, the vacuum degree is 20pa, the power is 100w, and the gas flow is 20ml per minute.
And step seven, soaking the treated aramid cloth in the epoxy resin adhesive prepared in the step three, stirring for 10 minutes by using ultrasonic waves, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step eight, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The test methods were as above, and the results are shown in Table 2.
Comparative example 10
The modified aramid fiber and the composite material thereof can be realized by the following steps:
step one, the aramid fabric selected is woven by aramid yarn with the thickness of 300 deniers, and the aramid fabric is pretreated according to the following steps:
1.1 soaking aramid fabric in a mixture of acetone and ethanol in a mass ratio of 1:1 for 10 hours.
1.2 taking out the soaked aramid fiber cloth, and baking the aramid fiber cloth in an oven at the temperature of 80 ℃ for 10 hours
And 1.3, putting the baked aramid fiber cloth into a high-temperature oven, and baking for 3 hours at a high temperature of 200 ℃.
And step two, sequentially adding tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine into deionized water according to the proportion shown in the table 1, and ultrasonically stirring for 30 minutes to uniformly disperse the materials to obtain a treatment solution A.
And step three, sequentially adding deionized water and a silane coupling agent A174 into absolute ethyl alcohol according to the proportion shown in the table 1, and uniformly dispersing the mixture by ultrasonic stirring for 30 minutes to prepare a treatment solution B.
And step four, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
And fifthly, performing plasma treatment on the aramid fiber cloth pretreated in the first step for 15 minutes by using helium as gas, wherein the vacuum degree is 20pa, the power is 100w, and the gas flow is 20ml per minute.
And step six, soaking the aramid fiber cloth subjected to the plasma treatment in the treatment liquid A according to the table 1, stirring for 4 hours by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in a 60-DEG C drying oven.
And step seven, soaking the dried aramid fiber cloth in the treatment liquid B according to the table 1, stirring for 20 minutes by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in an oven at 60 ℃.
And step eight, soaking the treated aramid fiber cloth in the epoxy resin adhesive prepared in the step four, stirring for 10 minutes by using ultrasonic waves, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step nine, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The test methods were as above, and the results are shown in Table 2.
Comparative example 11
The modified aramid fiber and the composite material thereof can be realized by the following steps:
step one, the aramid fabric selected is woven by aramid yarn with the thickness of 300 deniers, and the aramid fabric is pretreated according to the following steps:
1.1 soaking aramid fabric in a mixture of acetone and ethanol in a mass ratio of 1:1 for 24 hours.
1.2 taking out the soaked aramid fiber cloth, and baking the aramid fiber cloth in an oven at the temperature of 80 ℃ for 10 hours
And 1.3, putting the baked aramid fiber cloth into a high-temperature oven, and baking for 1 hour at the high temperature of 200 ℃.
And step two, sequentially adding tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine into deionized water according to the proportion shown in the table 1, and ultrasonically stirring for 30 minutes to uniformly disperse the materials to obtain a treatment solution A.
And step three, sequentially adding deionized water and a silane coupling agent A174 into absolute ethyl alcohol according to the proportion shown in the table 1, and uniformly dispersing the mixture by ultrasonic stirring for 30 minutes to prepare a treatment solution B.
And step four, uniformly mixing 100 parts of bisphenol A epoxy resin, 2 parts of electronic grade dicyandiamide, 0.1 part of 2-ethyl-4-methylimidazole and 50 parts of butanone into a mixed solution according to the weight components.
And fifthly, performing plasma treatment on the aramid fiber cloth pretreated in the first step for 15 minutes by using helium as gas, wherein the vacuum degree is 20pa, the power is 100w, and the gas flow is 20ml per minute.
And step six, soaking the aramid fiber cloth subjected to the plasma treatment in the treatment liquid A according to the table 1, stirring for 4 hours by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in a 60-DEG C drying oven.
And step seven, soaking the dried aramid fiber cloth in the treatment liquid B according to the table 1, stirring for 20 minutes by using ultrasonic waves, taking out, cleaning by using deionized water, and drying in an oven at 60 ℃.
And step eight, soaking the treated aramid fiber cloth in the epoxy resin adhesive prepared in the step four, stirring for 10 minutes by using ultrasonic waves, taking out, and drying at 120-180 ℃ to obtain a prepreg with the fluidity of 5-20%.
And step nine, overlapping more than one prepreg, and then molding the prepreg in a hot press at high temperature and high pressure to obtain the modified aramid composite material. The temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
The test methods were as above, and the results are shown in Table 2.
TABLE 1
TABLE 2
| Test results | Thermal shock time(s) | Tensile Strength ((N/mm2)) | Tensile modulus (GPa) |
| Example 1 | 27 | 392 | 21.2 |
| Example 2 | 21 | 371 | 20.1 |
| Example 3 | 30 | 380 | 20.7 |
| Example 4 | 17 | 369 | 19.8 |
| Comparative example 1 | 1 | 341 | 16.7 |
| Comparative example 2 | 2 | 337 | 16.4 |
| Comparative example 3 | 5 | 323 | 15.8 |
| Comparative example 4 | 10 | 304 | 14.4 |
| Comparative example 5 | 14 | 293 | 13.6 |
| Comparative example 6 | 7 | 339 | 16.8 |
| Comparative example 7 | 12 | 348 | 17.1 |
| Comparative example 8 | 13 | 352 | 17.7 |
| Comparative example 9 | 8 | 332 | 16.4 |
| Comparative example 10 | 15 | 361 | 18.9 |
| Comparative example 11 | 19 | 370 | 20.0 |
| Comparative example 12 | 25 | 377 | 20.6 |
| Comparative example 13 | 16 | 364 | 19.1 |
As can be seen from Table 2:
by comparing comparative examples 1-5, it can be found that the longer the plasma treatment time is, the stronger the bonding performance of the modified aramid composite material is, but the tensile property of the material is continuously reduced, and the plasma treatment for 15 minutes in comparative example 3 is a more appropriate treatment time.
By comparing examples 1-3 with comparative example 3, it can be found that the bonding property and tensile strength of the modified aramid composite material prepared by treating the plasma-treated aramid with the treatment liquid A and the treatment liquid B are both significantly improved, and the modified aramid composite material with good bonding property and tensile property is prepared.
By comparing examples 1-3 with example 4, the combination property of the modified aramid composite material is affected by changing the type and proportion of the pretreatment solvent.
Compared with the examples 1-3 and the comparative example 6, the modified aramid composite material prepared by the treatment lacking the treatment liquid B has obviously reduced bonding performance and tensile property.
By comparing examples 1-3 with comparative example 7, the bonding performance and tensile property of the modified aramid composite material prepared by the treatment lacking the treatment liquid A are obviously reduced.
By comparing examples 1-3 with comparative example 8, the bonding performance and tensile property of the modified aramid composite material prepared by replacing the treatment sequence of the treatment solution A and the treatment solution B are obviously reduced.
By comparing examples 1-3 with comparative example 9, the bonding performance and tensile property of the modified aramid composite material prepared without pretreatment and by changing the plasma treatment sequence are obviously reduced.
Compared with the examples 1-3 and the comparative example 10, the bonding performance and the tensile property of the modified aramid composite material prepared by the pretreatment soaking time are reduced to a certain extent.
By comparing examples 1-3 with comparative example 11, the bonding performance and tensile property of the modified aramid composite material prepared by pretreating the aramid composite material with insufficient high-temperature baking time are reduced to a certain extent.
By comparing examples 1-3 with comparative example 12, the tensile property of the modified aramid composite material prepared by the component A of the treating fluid is reduced to a certain extent.
By comparing examples 1-3 with comparative example 13, the bonding performance and tensile property of the modified aramid composite material prepared by the treatment fluid B component exceeding the range are reduced to a certain extent.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core ideas. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (10)
1. The modified aramid fiber is characterized by being prepared by carrying out steps including pretreatment, plasma treatment, dopamine modification and silane coupling agent modification on aramid fabric.
2. The modified aramid fiber of claim 1, characterized in that the step of pre-treating is: soaking aramid fabric in an organic solvent for a certain time, and then sequentially baking the soaked aramid fabric at low temperature and high temperature.
3. The modified aramid fiber of claim 2, wherein the organic solvent is one or more selected from acetone, butanone, methanol and ethanol, and the soaking time is 20-30 hours; the low-temperature baking temperature is 60-80 ℃, the baking time is 8-12 hours, the high-temperature baking temperature is 180-220 ℃, and the baking time is 2-3 hours.
4. The modified aramid fiber of claim 1, characterized in that the plasma treatment step is: and carrying out plasma treatment on the pretreated aramid fiber cloth, wherein helium is used as a gas, the vacuum degree is 20-100 pa, the power is 50-300 w, the gas flow is 10-30 ml per minute, and the treatment time is 5-30 minutes.
5. The modified aramid fiber of claim 1, wherein the dopamine is modified by: soaking the aramid fiber cloth subjected to plasma treatment in the treatment liquid A while ultrasonically stirring, and then cleaning and drying by using deionized water; the treating fluid A is prepared by dissolving tris (hydroxymethyl) aminomethane, concentrated hydrochloric acid and dopamine in deionized water and performing ultrasonic dispersion uniformly.
6. The modified aramid fiber as claimed in claim 5, wherein the treating liquid A contains 0.5 to 1% by mass of tris (hydroxymethyl) aminomethane, 0.2 to 0.4% by mass of hydrochloric acid, and 0.5 to 1% by mass of dopamine; more preferably, the treatment liquid a contains 0.8% by mass of tris (hydroxymethyl) aminomethane, 0.3% by mass of hydrochloric acid, and 0.8% by mass of dopamine.
7. The modified aramid fiber of claim 1, wherein the silane coupling agent is modified by the steps of: soaking the dopamine-modified aramid fiber cloth in the treatment liquid B while ultrasonically stirring, and then washing and drying by using deionized water; and the treatment liquid B consists of a silane coupling agent, an alcohol solvent and deionized water.
8. The modified aramid fiber of claim 7 wherein the alcoholic solvent is one or more of methanol, ethanol, ethylene glycol; the silane coupling agent adopts one or more of KH550, KH560, KH570, A1100, A174 and A187.
9. A modified aramid composite material is characterized in that the modified aramid composite material is prepared by soaking the modified aramid of claims 1-8 in a resin composition, drying to obtain a prepreg, and then laminating at least one prepreg and hot-pressing.
10. The modified aramid composite material of claim 9, wherein ultrasonic stirring is performed simultaneously in the dipping process for 5-10 minutes, the drying temperature is 120-180 ℃, and the fluidity of the prepreg is 5-20%; the hot pressing temperature is 100-200 ℃, and the pressure is 10-20 Mpa.
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