CN105113260A - Method for performing amino functionalizing on carbon fiber surface - Google Patents
Method for performing amino functionalizing on carbon fiber surface Download PDFInfo
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- CN105113260A CN105113260A CN201510512182.5A CN201510512182A CN105113260A CN 105113260 A CN105113260 A CN 105113260A CN 201510512182 A CN201510512182 A CN 201510512182A CN 105113260 A CN105113260 A CN 105113260A
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Abstract
The invention relates to a method for performing amino functionalizing on a carbon fiber surface. The method comprises the steps that the fiber surface is coated with a copolymer coating containing a large amount of active amino by utilizing a Michael addition and Schiff base reaction of dopamine and poly-amino molecules through a one-step solution dipping method. Compared with the prior art, the method is simple in technology and mild in condition, does not damage a fiber body structure and can effectively increase active groups of the carbon fiber surface, and therefore the interface bonding property between fiber and resin is improved.
Description
Technical field
The invention belongs to material with carbon element modification field, especially relate to a kind of method of carbon fiber surface modification.
Background technology
Carbon fiber (CF) is as high-performance fiber of new generation, there is specific strength high, specific modulus is high, creep-resistant property is good, density is low, heat endurance and chemical stability good, the performance of a series of excellences such as low and the hot and electrical conductivity of thermal coefficient of expansion is high, its composite has been widely used in the fields such as Aero-Space, military project, communications and transportation, medical treatment and sports goods.
The performance of carbon fibre reinforced composite is jointly determined by the own performance of CF and matrix and interfacial combined function between the two.Interface phase is very important microstructure in composite, as " bridge " that be connected between reinforcement CF with matrix, has very important impact to every mechanical performance of composite.
Due to CF smooth surface and chemical inertness, lack activated functional group, cause fiber and matrix phase capacitive not good enough, interface adhesion is poor, have impact on the mechanical property of composite, thus greatly hinders the process of composite material high performance.Therefore, suitable method must be adopted to carry out surface modification to CF, to improve its surface-activity and roughness, strengthen Chemical bonding and the physics inlay resultant force of itself and resin, and then improve wettability and the caking property of itself and matrix, just can give full play to the humidification of CF, obtain the composite of excellent combination property.
The more CF surface treatment method of current use mainly contains gaseous oxidation, liquid phase oxidation, electrochemical oxidation (CN104562631A), Cement Composite Treated by Plasma, vapour deposition, electrochemical deposition, coupling agent coating, polymer coating (CN104018355A, CN103015163A), surface aggregate and grafting (CN104195835A, CN103850124A) etc.These methods improve interface cohesion situation to a certain extent, but often have that treatment process is more loaded down with trivial details, cost is high, easily cause damage to fiber bodies and the shortcoming such as interface binding power is more weak.
Dopamine causes extensive concern as a kind of novel material modified recent years.Dopamine is easy to oxidized in alkaline aqueous solution, then causes from poly-cross-linking reaction, forms the poly-DOPA amine layer of close attachment at almost any one solid material surface.Solid material to be modified only need be put into the dopamine solution of fresh configuration by this method of modifying, takes out, can obtain surface attachment and gather the material modified of dopamine coating after soaking a period of time.Whole modifying process completes in aqueous, and reaction condition is gentle, avoids with an organic solvent pollution on the environment, and settles at one go the modification of material surface, and operating procedure is simple, and reaction condition and modifying process are easy to control.Chinese patent CN103572591A uses the method to carry out surface modification to carbon fiber, but dopamine is in course of reaction, and a large amount of amido is consumed, and causes residual amine less.But in the poly-dopamine coating that material surface generates, there is the adjacent benzene diquinone group that abundant catechol and catechol be oxidized to, they can by Michael addition and schiff base reaction and the effect of the group such as amido, sulfydryl.Therefore, this can be utilized to react, in dopamine system, introduce the molecule of other amino-containeds, to improve the amine groups content of fiber surface, be conducive to fiber and be combined with the surface chemistry of resin, thus improve the macro property of composite.
Summary of the invention
Object of the present invention is exactly providing to overcome defect that above-mentioned prior art exists that a kind of technique is simple, mild condition, not damaging fiber bodies structure, effectively can increase the active group of carbon fiber surface, thus improve the method for the carbon fiber surface functional amido of fiber and interlaminar resin interfacial combined function, the method only needs a step solution impregnation to realize.
Object of the present invention can be achieved through the following technical solutions:
A method for carbon fiber surface functional amido, the method by a step solution dipping method, coated copolymer coated containing a large amount of active amine of fiber surface, comprises the following steps:
(1) Tris buffer solution is configured: take a certain amount of tri methylol amino methane (Tris) in volumetric flask, add deionized water dissolving, obtain the Tris solution of 10mmol/L, add concentrated hydrochloric acid number and drip, pH is adjusted to about 8.5, namely obtains Tris buffer solution;
(2) surface treatment of carbon fiber: take mass ratio for (0.1 ~ 10): the polyamines base molecule of 1 and dopamine, be dissolved in the Tris buffer solution that step (1) configures, by impregnated carbon fiber in reaction system, at room temperature stir process 2 ~ 48h, after process terminates, fully wash with deionized water, put into the dry 12 ~ 24h of vacuum drying oven of 50 ~ 70 DEG C, namely obtain the carbon fiber of surface amine groups functionalization.
, for dopamine component with polyamines base molecule is disposable joins in cushioning liquid, there is the copolymerization of bi-component in the solution in a described step solution dipping method.In the auto polymerization process of dopamine, amino in polymine can participate in Michael addition or schiff base reaction, simultaneously can further with the phenolic hydroxyl group on base material and quinonyl unit generation cross-linking reaction, thus to adhere on fiber surface together with poly-dopamine.Wherein, the amino of polyethyleneimine: amine component both take part in copolymer coated formation, also for fiber surface provides enough amino.
Described polyamines base molecule is one or more in ethylenediamine, hexamethylene diamine, polyethylene polyamine, polymine, dendritic interphase or shitosan, preferably polyethylene imines, it is water soluble polymer, and degree of branching is high, containing a large amount of amido, there is higher reactivity.
The molecular weight of described polymine is 600 ~ 100000, and preferred molecular weight is 5000 ~ 20000.The molecular weight of polymine lower than 600 time, the crosslinking copolymers density of formation is too high, causes coating too crisp, lacking toughness, easily produces interfacial stress and concentrates.Polymine higher than 100000 time, the motility of molecule is poor, is unfavorable for being penetrated into matrix resin inside.
Described polymine and the mass ratio of dopamine are (0.1 ~ 10): 1, and preferred mass is than being 0.5:1 ~ 2:1.In copolymerization composition, the ratio of polymine and dopamine is lower than 0.1:1, and in reaction, dopamine can consume the amino on polymine in a large number, causes the free amino group amount being finally incorporated into fiber surface less.When the ratio of polymine and dopamine is higher than 10:1, the molecular dimension growth of polymerization initial stage can be caused too fast, and the poly-dopamine of impact is in effective adhesion of fiber surface.
Described dopamine concentration is 0.1mg/ml ~ 10mg/ml (namely adding 0.1mg ~ 10mg dopamine in every milliliter of Tris buffer solution), and preferred concentration is 0.5mg/ml ~ 4mg/ml.When the concentration of dopamine is lower than 0.1mg/ml, copolymer is difficult to be coated on fiber surface completely, causes interface cohesion uneven.When the concentration of dopamine is higher than 10mg/ml, fiber surface copolymer coated too thick, the boundary layer formed is corresponding also partially thick, the thickness of interface phase is usually between tens to a hundreds of nm, thickness exceedes to a certain degree, the interactions such as the interfacial diffusion between fiber and resin can be affected, on the contrary can the overall performance of attacking material.
Described carbon fiber comprises polyacrylonitrile-based carbon fibre, asphalt base carbon fiber or viscose-based carbon fiber.
Compared with prior art, the present invention has the following advantages:
1, the present invention directly can carry out modification to business-like CF, and CF does not need the preliminary treatment such as extracting, oxidation, thus can not destroy the body construction of CF, remains the high-strength and high-modulus characteristic of CF itself;
2, in the present invention, the introducing of polymine, considerably increases the amine groups content of fiber surface;
3, carbon fiber modifying process control of the present invention is better, by regulating the process conditions such as ratio, concentration, time of the molecular weight of polymine, polymine and dopamine, the controlledization process of CF surface amine groups quantity can be realized, thus obtain dissimilar interface;
4, the present invention adopts a step solution dipping method and reacts and carry out in room temperature and the aqueous solution, simple and fast, mild condition, environmental protection;
5, the invention is not restricted to improve the interface performance that CF strengthens thermosetting resin, as epoxy resin, phenolic resins, two Malaya amide resin, CF is strengthened to the thermoplastic resin of polarity, as acid modified polyolefin, polyester, polyamide, polyimides, also have interface humidification.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of modified carbon fiber obtained in embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of unmodified carbon fiber.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Raw material used in embodiment and comparative example and method of testing as follows:
Carbon fiber is the T700 of toray, and density is 1.8g/cm
3, stretch modulus is 230GPa, and TENSILE STRENGTH is 4.9GPa.The E51 that epoxy resin (EP) is Wuxi blue star petrochemical industry, viscosity 2500mPas (40 DEG C), epoxide number 0.48-0.54eq/100g, curing agent is methyl tetrahydro phthalic anhydride, and the mass ratio of epoxy resin and curing agent is 100:70.The liter that maleic anhydride inoculated polypropylene (MPP) is Shanghai day is produced, and wherein the percent grafting of maleic anhydride is 1wt%.The CM1017 that nylon 6 (PA6) is toray, density is 1.13g/cm
3, TENSILE STRENGTH is 85MPa, and bending strength is 120MPa.Use Japanese Dong Rong Co., Ltd. HM410 type composite material interface evaluating apparatus, the interface shear strength (IFSS) adopting micro-unsticking method to test monofilament and interlaminar resin directly can weigh the interfacial bond property of material.Wherein, CF and the EP of long time without surface modification, the IFSS between MPP, PA6 are respectively 30.5MPa, 10.2MPa, 22.4MPa.
Embodiment 1
Take 100mg molecular weight be 10000 polymine and 200mg dopamine (mass ratio is 0.5:1, the concentration of dopamine is 2mg/ml), being dissolved in 100mlpH is in the Tris buffer solution of 8.5, is immersed in reaction system by 5gCF thereupon, stirs 24h at room temperature environment lower magnetic force.After process terminates, fully wash with deionized water, put into the dry 24h of vacuum drying oven of 60 DEG C.The stereoscan photograph of CF prepared by the present embodiment as shown in Figure 1, as shown in Figure 2, can find out by the stereoscan photograph of unmodified CF, and modified CF Surface coating has uniform polymer coating.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 72.8MPa, 32.3MPa, 47.5MPa, are the CF of non-modified and 238.7%, 316.7%, 212.1% of above-mentioned three kinds of interlaminar resin IFSS, and interface strengthens Be very effective.
Embodiment 2
The polymine molecular weight that the present embodiment uses as different from Example 1 is 15000, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 65.3MPa, 29.7MPa, 42.7MPa, are the CF of non-modified and 214.1%, 291.2%, 190.6% of above-mentioned three kinds of interlaminar resin IFSS, and interface strengthens Be very effective.
Embodiment 3
The mass ratio of the polymine that the present embodiment uses as different from Example 1 and dopamine is 2:1, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 70.2MPa, 35.6MPa, 48.6MPa, are the CF of non-modified and 230.2%, 291.2%, 217.0% of above-mentioned three kinds of interlaminar resin IFSS, and interface strengthens Be very effective.
Embodiment 4
The concentration of the dopamine that the present embodiment uses as different from Example 1 is 4mg/ml, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 60.1MPa, 26.0MPa, 40.3MPa, it is the CF of preparation and 160.7%, 144.4%, 136.6% of above-mentioned three kinds of interlaminar resin IFSS in comparative example 1, be the CF of non-modified and 197.0%, 254.9%, 179.9% of above-mentioned three kinds of interlaminar resin IFSS, interface strengthens Be very effective.
Embodiment 5
The polyamines base molecule that the present embodiment uses as different from Example 1 is hexamethylene diamine, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 42.6MPa, 21.5MPa, 34.4MPa, it is the CF of non-modified and 139.7%, 210.8%, 153.6% of above-mentioned three kinds of interlaminar resin IFSS, it is better that interface strengthens effect, but the CF using polymine to prepare not as embodiment 1-4.
Comparative example 1
The molecular weight of the polymine that this comparative example uses as different from Example 1 is 200, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 31.3MPa, 11.5MPa, 21.0MPa, and be the CF of non-modified and 102.6%, 112.7%, 93.8% of above-mentioned three kinds of interlaminar resin IFSS, boundary strength there is not change substantially.
Comparative example 2
The molecular weight of the polymine that this comparative example uses as different from Example 1 is 200000, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 28.6MPa, 8.9MPa, 20.7MPa, and be the CF of non-modified and 93.8%, 87.3%, 92.4% of above-mentioned three kinds of interlaminar resin IFSS, boundary strength declines on the contrary.
Comparative example 3
The mass ratio of the polymine that this comparative example uses as different from Example 1 and dopamine is 0.05:1, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 39.0MPa, 13.5MPa, 27.2MPa, and be the CF of non-modified and 127.9%, 132.4%, 121.4% of above-mentioned three kinds of interlaminar resin IFSS, boundary strength slightly improves.
Comparative example 4
The mass ratio of the polymine that this comparative example uses as different from Example 1 and dopamine is 20:1, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 34.8MPa, 12.9MPa, 25.7MPa, and be the CF of non-modified and 114.1%, 126.5%, 114.7% of above-mentioned three kinds of interlaminar resin IFSS, boundary strength increase rate is little.
Comparative example 5
The concentration of the dopamine that this comparative example uses as different from Example 1 is 0.05mg/ml, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 26.3MPa, 9.1MPa, 20.5MPa, and be the CF of non-modified and 86.2%, 89.2%, 91.5% of above-mentioned three kinds of interlaminar resin IFSS, boundary strength slightly declines.
Comparative example 6
The concentration of the dopamine that this comparative example uses as different from Example 1 is 20mg/ml, and other are identical with embodiment 1.CF and EP prepared by the present embodiment, the IFSS between MPP, PA6 are respectively 22.0MPa, 7.3MPa, 17.2MPa, and be the CF of non-modified and 72.1%, 71.6%, 76.8% of above-mentioned three kinds of interlaminar resin IFSS, boundary strength has decline to a certain degree.
Table 1
From table 1, the result of embodiment 1-5 is known, the CF that the present invention obtains and resin have better boundary strength, because CF surface polar groups prepared by the present invention increases, stronger chemical action can be formed with interlaminar resin, make to reach good interface cohesion between matrix resin and CF, thus boundary strength is greatly enhanced.The interface shear strength result of comparative example 1-6 shows, in one-step method solution impregnation process, the molecular weight of polymine, the mass ratio of polymine and dopamine, the concentration of dopamine will control within certain scope, otherwise it is general to improve effect to interface performance, even can damage boundary strength.
Embodiment 6
Take 100mg molecular weight be 100000 polymine and 10mg dopamine (mass ratio is 10:1, the concentration of dopamine is 0.1mg/ml), being dissolved in 100mlpH is in the Tris buffer solution of 8.5, is immersed in reaction system by 5gCF thereupon, stirs 24h at room temperature environment lower magnetic force.After process terminates, fully wash with deionized water, put into the dry 24h of vacuum drying oven of 50 DEG C.Modified CF Surface coating has uniform polymer coating.The interface of CF and EP prepared by the present embodiment, MPP, PA6 strengthens Be very effective.
Embodiment 7
Take 100mg molecular weight be 600 polymine and 1000mg dopamine (mass ratio is 0.1:1, the concentration of dopamine is 10mg/ml), being dissolved in 100mlpH is in the Tris buffer solution of 8.5, is immersed in reaction system by 5gCF thereupon, stirs 2h at room temperature environment lower magnetic force.After process terminates, fully wash with deionized water, put into the dry 12h of vacuum drying oven of 70 DEG C.Modified CF Surface coating has uniform polymer coating.The interface of CF and EP prepared by the present embodiment, MPP, PA6 strengthens Be very effective.
Embodiment 8
(mass ratio is 0.5:1 to take 100mg ethylenediamine and 200mg dopamine, the concentration of dopamine is 2mg/ml), being dissolved in 100mlpH is in the Tris buffer solution of 8.5, is immersed in reaction system by 5g polyacrylonitrile-based carbon fibre thereupon, stirs 24h at room temperature environment lower magnetic force.After process terminates, fully wash with deionized water, put into the dry 24h of vacuum drying oven of 60 DEG C.Modified CF Surface coating has uniform polymer coating.Interface strengthens Be very effective.
Embodiment 9
The present embodiment is substantially the same manner as Example 8, and difference is, polyamines base molecule is hexamethylene diamine and ethylenediamine (mol ratio is 1:1), and carbon fiber is asphalt base carbon fiber.Modified CF Surface coating has uniform polymer coating.The interface of CF and EP prepared by the present embodiment, MPP, PA6 strengthens Be very effective.
Embodiment 10
The present embodiment is substantially the same manner as Example 8, and difference is, polyamines base molecule is polyethylene polyamine, and carbon fiber is viscose-based carbon fiber.Modified CF Surface coating has uniform polymer coating.The interface of CF and EP prepared by the present embodiment, MPP, PA6 strengthens Be very effective.
Embodiment 11
The present embodiment is substantially the same manner as Example 8, and difference is, polyamines base molecule is dendritic interphase.Modified CF Surface coating has uniform polymer coating.The interface of CF and EP prepared by the present embodiment, MPP, PA6 strengthens Be very effective.
Embodiment 12
The present embodiment is substantially the same manner as Example 8, and difference is, polyamines base molecule is shitosan.Modified CF Surface coating has uniform polymer coating.The interface of CF and EP prepared by the present embodiment, MPP, PA6 strengthens Be very effective.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It is noted that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple modification of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. the method for a carbon fiber surface functional amido, it is characterized in that, the method is by a step solution dipping method, coated copolymer coated containing a large amount of active amine of fiber surface, specifically comprise the following steps: take mass ratio for (0.1 ~ 10): the polyamines base molecule of 1 and dopamine, be dissolved in Tris buffer solution, forming reactions system, by impregnated carbon fiber in reaction system, at room temperature stir process 2 ~ 48h, then wash, dry, namely obtain the carbon fiber of surface amine groups functionalization.
2. the method for a kind of carbon fiber surface functional amido according to claim 1, it is characterized in that, described polyamines base molecule is selected from one or more in ethylenediamine, hexamethylene diamine, polyethylene polyamine, polymine, dendritic interphase or shitosan.
3. the method for a kind of carbon fiber surface functional amido according to claim 1 and 2, is characterized in that, described polyamines base molecule is polymine, and the molecular weight of polymine is 600 ~ 100000.
4. the method for a kind of carbon fiber surface functional amido according to claim 3, is characterized in that, described polymine molecular weight is 5000 ~ 20000.
5. the method for a kind of carbon fiber surface functional amido according to claim 1, is characterized in that, the concentration of described dopamine is 0.1mg/ml ~ 10mg/ml.
6. the method for a kind of carbon fiber surface functional amido according to claim 1 or 5, it is characterized in that, the concentration of described dopamine is 0.5mg/ml ~ 4mg/ml.
7. the method for a kind of carbon fiber surface functional amido according to claim 1, is characterized in that, described polyamines base molecule and the mass ratio of dopamine are 0.5:1 ~ 2:1.
8. the method for a kind of carbon fiber surface functional amido according to claim 1, is characterized in that, the pH of described Tris buffer solution is 8.5.
9. the method for a kind of carbon fiber surface functional amido according to claim 1, it is characterized in that, described carbon fiber comprises polyacrylonitrile-based carbon fibre, asphalt base carbon fiber or viscose-based carbon fiber.
10. the method for a kind of carbon fiber surface functional amido according to claim 1, is characterized in that, described oven dry is dry 12 ~ 24h in the vacuum drying oven of 50 ~ 70 DEG C.
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