CN114773785B - Polyaniline nano whisker modified epoxy resin composite material and preparation method thereof - Google Patents
Polyaniline nano whisker modified epoxy resin composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a synthesis method of polyaniline nanowhiskers, which comprises the following steps: through a chemical oxidation process, phytic acid, aniline and ammonium persulfate react according to a certain proportion, and polyaniline nanowhiskers with whisker-like morphology, diameter of 60-100nm and length-diameter ratio of 4-8 are prepared after centrifugation, washing and drying; the invention also discloses a preparation method of the polyaniline nano whisker modified epoxy resin composite material, which comprises the following raw materials in percentage by weight: 1-7% of polyaniline nano whisker, 74-78% of epoxy resin and 18-22% of 4, 4-diaminodiphenyl methane. The polyaniline nanowhisker disclosed by the invention has the advantages of uniform size, regular morphology and strong dispersing capability in epoxy resin, the mechanical property of the epoxy resin is obviously improved, the wear rate of the material is greatly reduced, the excellent wear resistance is obtained, and the polyaniline nanowhisker can be used for reinforcing and wear-resisting integrated construction of epoxy resin composite materials.
Description
Technical Field
The invention relates to the field of modified epoxy resin composite materials, in particular to a polyaniline nano whisker modified epoxy resin composite material and a preparation method thereof.
Background
Epoxy resin is a thermosetting polymer with very wide application, has good chemical corrosion resistance, bonding strength, dielectric property and the like, is favored in various fields such as aerospace, national defense and military, transportation engineering, petrochemical industry and the like, and the research and development of related materials and products are concerned by academic circles and industry at home and abroad. However, epoxy resin can form a three-dimensional crosslinked network structure in the curing process, the molecular chain has poor movement capability and relatively large brittleness, the surface layer material is easy to peel off when the external load is impacted, and particularly, the surface layer material is extremely easy to severely abrade when the surface layer material is subjected to sliding dry friction, so that the service life of related products is severely reduced, and therefore, the application of the surface layer material is greatly limited in many occasions, particularly in the fields with high requirements on mechanical strength and wear resistance.
The tribological property of epoxy resin is closely related to its mechanical strength and hardness, so that researchers at home and abroad can use hard inorganic filler to improve the strength and hardness of epoxy resin and simultaneously endow the epoxy resin with good anti-wear capability by introducing different inorganic filler such as nano particles, fibers and the like into an epoxy matrix. However, there is a significant polarity difference between the hydrophilic inorganic filler and the lipophilic epoxy resin, so that it is often difficult to obtain good interface bonding, which is not beneficial to improving the mechanical strength and the abrasion resistance of the epoxy resin; in addition, inorganic nanoparticles are easy to form a large amount of aggregation due to van der Waals force existing among the particles, so that the performance of the epoxy resin composite material is difficult to be deteriorated due to the fact that the inorganic nanoparticles are difficult to uniformly disperse in an epoxy matrix, and fibers with larger length-diameter ratio are entangled with each other when the filling amount is higher, so that the inorganic nanoparticles are also difficult to disperse, and the epoxy resin composite material with high filling amount is not favorable to be obtained. Therefore, the development of a novel organic rigid wear-resistant modifier with high interfacial compatibility with epoxy resin is particularly important and necessary for improving the friction and wear properties of the epoxy resin.
Disclosure of Invention
Aiming at the technical problems in the background technology, the application provides a polyaniline nano whisker modified epoxy resin composite material and a preparation method thereof. The invention utilizes a chemical oxidation method with simple operation and mild condition to obtain polyaniline nanowhiskers on the basis of optimizing synthesis process parameters, then introduces the polyaniline nanowhiskers into epoxy resin to serve as functional filler, and prepares the epoxy resin composite material with uniform dispersion of the polyaniline nanowhiskers in a matrix, greatly improved mechanical properties and obviously reduced wear rate through a solution blending method.
The technical content is as follows:
a polyaniline nano whisker modified epoxy resin composite material is characterized in that: the main material is epoxy resin, and the filler is polyaniline nano whisker; wherein the consumption of the polyaniline nano whisker is 1-7% of the mass of the epoxy resin.
The preparation method of the polyaniline nano whisker modified epoxy resin composite material comprises the following steps:
weighing a certain amount of polyaniline nanowhiskers, adding the polyaniline nanowhiskers into 20mL of acetone solution, treating the polyaniline nanowhiskers for 1h by using an ultrasonic cell grinder to perform pre-dispersion, slowly dripping the polyaniline nanowhiskers into epoxy resin solution preheated for 20-50min at 50-90 ℃ and strongly stirring the polyaniline nanowhiskers for 2-6h, so that the polyaniline nanowhiskers and the epoxy resin solution are fully mixed; under the condition of continuous strong stirring, rapidly adding the curing agent which is melted at 90-120 ℃ in advance into the mixed system, and continuously and strongly stirring for 1-3 hours; then pouring the mixture into a silica gel mold preheated at 40-80 ℃ in advance, vacuum degassing the mixture at 40-100 ℃ for 20-40min, and curing and forming the mixture at high temperature to obtain the polyaniline nano whisker modified epoxy resin composite material.
Preferably, the epoxy resin solution is preheated at 70 ℃ for 30min;
preferably, the curing agent is heated to a liquid state at 105 ℃;
preferably, vacuum degassing is carried out at 60℃for 30min;
preferably, the high temperature cure is at 100 ℃ for 2 hours and 150 ℃ for 2 hours;
preferably, the curing agent is 4, 4-diaminodiphenyl methane, and the mass ratio of the curing agent to the epoxy resin is 26.5:100.
the synthesis method of the polyaniline nano whisker comprises the following steps:
s1, dissolving phytic acid and aniline in 20mL of deionized water at room temperature, and strongly stirring for 5min to obtain a uniform orange-yellow solution A; dissolving ammonium persulfate in 10mL of deionized water and strongly stirring for 5min to obtain a uniform colorless transparent solution B;
s2, slowly adding the solution B into the solution A under the continuous strong stirring action to obtain a dark green solution, immediately stopping stirring, standing for reaction for 24 hours, and drying in vacuum at 60 ℃ to constant weight after repeated centrifugation and washing to obtain the polyaniline nanowhisker.
Preferably, in S1, the amount of phytic acid is 0.002 to 0.05mol, preferably 0.01mol;
preferably, in S1, the aniline is used in an amount of 0.01 to 0.25mol, preferably 0.05mol;
preferably, in S1, the ammonium persulfate is used in an amount of 0.0025 to 0.0625mol, preferably 0.0125mol;
preferably, in S2, the reaction temperature is from 0 to 10℃and preferably 4 ℃.
Drawings
FIG. 1 is an SEM image of polyaniline nanowhiskers described in example 3;
FIG. 2 is a TEM image of polyaniline nanowhiskers described in example 3;
FIG. 3 is an optical image of the worn area of the neat epoxy resin described in comparative example 1
FIG. 4 is a wear scar contour line of the worn area of the virgin epoxy described in comparative example 1;
FIG. 5 is an optical photograph of the worn area of the polyaniline nanowhisker modified epoxy resin composite described in example 3
Fig. 6 is a wear scar contour line of the wear zone of the polyaniline nanowhisker modified epoxy resin composite described in example 3.
From fig. 1 and fig. 2, it can be seen that the prepared polyaniline nanowhiskers have a diameter of about 60-100nm and an aspect ratio of 4-8, and exhibit a typical whisker-like morphology, indicating that the polyaniline nanowhiskers were successfully synthesized.
As can be seen from fig. 3 and 4, the pure epoxy resin exhibited a large area of wear zone, with a wear scar width of up to about 6.6mm; in contrast, fig. 5 and 6 show that the abrasion zone of the polyaniline nanowhisker modified epoxy resin composite material is significantly narrowed, and the abrasion mark width is only 2.5mm. Obviously, the polyaniline nano whisker modified epoxy resin composite material has higher wear resistance.
Detailed Description
In order to make the purposes, technical schemes and advantages of the embodiments of the present invention more clear, the technical schemes in the embodiments of the present invention are clearly and completely described. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The epoxy resins used in the examples and comparative examples herein were technical grade, E51, bisphenol A, and epoxy values of 0.48 to 0.53.
Example 1:
s1, dissolving 0.01mol of phytic acid and 0.05mol of aniline in 20mL of deionized water at room temperature, and strongly stirring for 5min to obtain a uniform orange-yellow solution A; dissolving 0.0125mol of ammonium persulfate in 10mL of deionized water and strongly stirring for 5min to obtain a uniform colorless transparent solution B;
s2, slowly adding the solution B into the solution A under the continuous strong stirring action to obtain a dark green solution, immediately stopping stirring, standing at the temperature of 4 ℃ for reaction for 24 hours, and drying in vacuum at the temperature of 60 ℃ to constant weight after repeated centrifugation and washing to obtain the polyaniline nanowhisker.
S3, weighing 0.16g of polyaniline nanowhiskers, adding the polyaniline nanowhiskers into 20mL of acetone solution, treating the polyaniline nanowhiskers for 1h by using an ultrasonic cell grinder to perform pre-dispersion, slowly dripping the polyaniline nanowhiskers into 15.69g of epoxy resin solution preheated for 30min at 70 ℃ and strongly stirring the polyaniline nanowhiskers for 4h, so that the polyaniline nanowhiskers and the epoxy resin solution are fully mixed; under the condition of continuous strong stirring, 4.15g of 4, 4-diaminodiphenyl methane which is melted in advance at 105 ℃ is rapidly added into the mixed system, and the strong stirring is continued for 1h; then pouring the mixture into a silica gel mold preheated at 60 ℃ in advance, vacuum degassing at 60 ℃ for 30min, curing at 100 ℃ for 2h, and curing at 150 ℃ for 2h to obtain the polyaniline nano whisker modified epoxy resin composite material.
Example 2:
s1 and S2 were the same as in example 1, except that the amount of polyaniline nanowhiskers in S3 was 0.46g, the amount of epoxy resin was 15.45g, and the amount of 4, 4-diaminodiphenylmethane was 4.09g.
Example 3:
s1 and S2 were the same as in example 1, except that the amount of polyaniline nanowhiskers in S3 was 0.76g, the amount of epoxy resin was 15.21g, and the amount of 4, 4-diaminodiphenylmethane was 4.03g.
Example 4:
s1 and S2 were the same as in example 1, except that the amount of polyaniline nanowhiskers in S3 was 1.05g, the amount of epoxy resin was 14.99g, and the amount of 4, 4-diaminodiphenylmethane was 3.97g.
Comparative example 1:
15.82g of epoxy resin are preheated at 70 ℃ for 30min, 4.18g of 4, 4-diaminodiphenylmethane which is melted in advance at 105 ℃ are added, and the mixture is strongly stirred for 1h; then pouring the epoxy resin into a silica gel mold preheated at 60 ℃ in advance, vacuum degassing at 60 ℃ for 30min, curing at 100 ℃ for 2h, and curing at 150 ℃ for 2h to obtain the pure epoxy resin.
Comparative example 2:
s1, dissolving 0.025mol of phytic acid and 0.05mol of aniline in 20mL of deionized water at room temperature, and strongly stirring for 5min to obtain a uniform orange-yellow solution A; dissolving 0.005mol of ammonium persulfate in 10mL of deionized water and strongly stirring for 5min to obtain a uniform colorless transparent solution B;
s2, slowly adding the solution B into the solution A under the continuous strong stirring action to obtain a dark green solution, immediately stopping stirring, standing at the temperature of 4 ℃ for reaction for 24 hours, and drying in vacuum at the temperature of 60 ℃ to constant weight after repeated centrifugation and washing to obtain the polyaniline nanowhisker.
S3, weighing 0.76g of polyaniline nanowhiskers prepared in S1, adding the polyaniline nanowhiskers into 20mL of acetone solution, treating the mixture for 1h by using an ultrasonic cell grinder to perform pre-dispersion, slowly dripping the mixture into 15.21g of epoxy resin solution preheated at 70 ℃ for 30min, and strongly stirring the mixture for 4h to fully mix the mixture; under the condition of continuous strong stirring, 4.03g of 4, 4-diaminodiphenyl methane which is melted in advance at 105 ℃ is rapidly added into the mixed system, and the strong stirring is continued for 1h; then pouring the mixture into a silica gel mold preheated at 60 ℃ in advance, vacuum degassing at 60 ℃ for 30min, curing at 100 ℃ for 2h, and curing at 150 ℃ for 2h to obtain the polyaniline nano whisker modified epoxy resin composite nano whisker.
Comparative example 3:
s1, dissolving 0.05mol of phytic acid and 0.05mol of aniline in 20mL of deionized water at room temperature, and strongly stirring for 5min to obtain a uniform orange-yellow solution A; dissolving 0.0125mol of ammonium persulfate in 10mL of deionized water and strongly stirring for 5min to obtain a uniform colorless transparent solution B;
s2, slowly adding the solution B into the solution A under the continuous strong stirring action to obtain a dark green solution, immediately stopping stirring, standing at the temperature of 4 ℃ for reaction for 24 hours, and drying in vacuum at the temperature of 60 ℃ to constant weight after repeated centrifugation and washing to obtain the polyaniline nanowhisker.
S3, weighing 0.76g of polyaniline nanowhiskers prepared in S1, adding the polyaniline nanowhiskers into 20mL of acetone solution, treating the mixture for 1h by using an ultrasonic cell grinder to perform pre-dispersion, slowly dripping the mixture into 15.21g of epoxy resin solution preheated at 70 ℃ for 30min, and strongly stirring the mixture for 4h to fully mix the mixture; under the condition of continuous strong stirring, 4.03g of 4, 4-diaminodiphenyl methane which is melted in advance at 105 ℃ is rapidly added into the mixed system, and the strong stirring is continued for 1h; then pouring the mixture into a silica gel mold preheated at 60 ℃ in advance, vacuum degassing at 60 ℃ for 30min, curing at 100 ℃ for 2h, and curing at 150 ℃ for 2h to obtain the polyaniline nano whisker modified epoxy resin composite material.
Comparative example 4:
s1, dissolving 0.005mol of phytic acid and 0.05mol of aniline in 20mL of deionized water at room temperature, and strongly stirring for 5min to obtain a uniform orange-yellow solution A; dissolving 0.0125mol of ammonium persulfate in 10mL of deionized water and strongly stirring for 5min to obtain a uniform colorless transparent solution B;
s2, slowly adding the solution B into the solution A under the continuous strong stirring action to obtain a dark green solution, immediately stopping stirring, standing at the temperature of 4 ℃ for reaction for 24 hours, and drying in vacuum at the temperature of 60 ℃ to constant weight after repeated centrifugation and washing to obtain the polyaniline nanofiber.
S3, weighing 0.76g of polyaniline nanofiber prepared in S1, adding the polyaniline nanofiber into 20mL of acetone solution, treating the polyaniline nanofiber with an ultrasonic cell grinder for 1h to perform pre-dispersion, slowly dripping the polyaniline nanofiber into 15.21g of epoxy resin solution preheated at 70 ℃ for 30min, and strongly stirring the polyaniline nanofiber for 4h to fully mix the polyaniline nanofiber and the epoxy resin solution; under the condition of continuous strong stirring, 4.03g of 4, 4-diaminodiphenyl methane which is melted in advance at 105 ℃ is rapidly added into the mixed system, and the strong stirring is continued for 1h; then pouring the mixture into a silica gel mold preheated at 60 ℃ in advance, vacuum degassing at 60 ℃ for 30min, curing at 100 ℃ for 2h, and curing at 150 ℃ for 2h to obtain the polyaniline nano whisker modified epoxy resin composite material.
The performance tests were carried out on examples 1-4 and comparative examples 1-4 using the following methods:
the sliding dry friction test is carried out according to national standard GB/T3960-2016, and the size of the sample is 30 multiplied by 6 multiplied by 7mm 3 The test specimen was conditioned at a prescribed room temperature (23.+ -.5) and relative humidity (50.+ -.5)% for 24 hours before the test, and then tested at the same temperature and under a moderate condition, the applied load was 12kg, the rotational speed of the friction pair was 100rpm, and the friction time was 1 hour.
The single tensile property test is carried out according to national standard GB/T1040-2006, the test sample is in a 1BA dumbbell shape, the test speed is 2mm/min, and the test process is carried out until the test sample breaks.
Test example 1: the performance data for comparative examples 1-4 and example 3 are shown in Table 1:
table 1:
as can be seen from the data described in table 1, the polyaniline nanowhisker-modified epoxy resin composite material prepared according to example 3 exhibited better overall properties with the same amount of addition and a mass ratio of 5%, and the tensile strength, elastic modulus and wear rate were significantly higher than those of the pure epoxy resin prepared according to comparative example 1, the polyaniline nanowhisker-modified epoxy resin composites prepared according to comparative examples 2 to 3, and the polyaniline nanofiber-modified polyaniline composite material prepared according to comparative example 4. However, the mechanical properties and abrasion resistance of the modified epoxy resin composites prepared according to comparative example 2, comparative example 3 and example 3 are significantly higher than those of the pure epoxy resin obtained according to comparative example 1, showing that the combination properties of the epoxy resin composites can be improved both with polyaniline nanowhiskers and polyaniline nanofibers.
The possible reasons for the above results are that the polyaniline nanowhiskers synthesized according to the method described in example 3 have the best morphology, the best dispersibility and the proper aspect ratio, and can be uniformly dispersed in the epoxy matrix to achieve the best reinforcing effect. Compared with the polyaniline nanofibers synthesized according to the methods described in comparative examples 2 and 3, the polyaniline nanofibers have the advantages of obvious coarsening structure, low length-diameter ratio and obvious agglomeration phenomenon, and more agglomeration is easy to form in the epoxy resin matrix; the polyaniline synthesized according to the method described in comparative example 4 is fibrous, and the length-diameter ratio is far higher than that of polyaniline whisker, but the polyaniline is more difficult to disperse in the process of compounding the polyaniline and the epoxy matrix, and as a result, the mechanical property of the polyaniline is not improved, and the abrasion rate is reduced, so that the abrasion resistance of the epoxy resin is not improved.
Test example 2: the performance data for examples 1-4 are shown in Table 2:
table 2:
from the data reported in table 2, the incorporation of polyaniline nanowhiskers synthesized according to examples 1-4 into epoxy resins significantly improved the mechanical and tribological properties of the epoxy resin composites. As the addition amount of polyaniline nanofiber is increased from 1% to 7%, the tensile strength of the epoxy resin composite material shows a change trend of firstly increasing and then slightly decreasing, and reaches the maximum value when the mass fraction is 5%, and is greatly increased by 42.6% compared with the pure epoxy resin prepared in comparative example 1; the modulus of elasticity is steadily increased, while the elongation at break is slightly increased and then gradually decreased. This shows that the introduction of polyaniline nanowhiskers can greatly improve the mechanical strength and rigidity of epoxy resin composites, but easily results in a decrease in toughness, i.e., an increase in brittleness of the material to some extent.
In addition, the abrasion rate of the epoxy resin composite material shows a trend of sharply decreasing due to the introduction of polyaniline nanofiber, the lowest value of the abrasion rate is 70% lower than that of pure epoxy resin, and the area is gentle within the range of 3-7% of the addition amount, so that the optimal abrasion resistance effect is achieved; in contrast, epoxy composites have higher average coefficients of friction than pure epoxy, indicating that such materials may be useful in applications requiring slip resistance and wear resistance.
In summary, the application of the invention shows that the addition amount of the polyaniline nano whisker is within the range of 1% -7%, preferably within the range of 3% -7%, and the mechanical property and tribological property of the epoxy resin can be obviously improved, and the prepared polyaniline nano whisker modified epoxy resin composite material has the obvious advantages of high strength, high modulus and high abrasion resistance compared with pure epoxy resin, and when the addition amount of the polyaniline nano whisker is 5%, the comprehensive performance is optimal.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to apply equivalents and modifications to the technical solution and the inventive concept thereof within the scope of the present invention.
Claims (7)
1. A polyaniline nano whisker modified epoxy composite material is characterized in that: the main material is epoxy resin, and the filler is polyaniline nano whisker; wherein the consumption of the polyaniline nano whisker is 1% -7%, the epoxy resin is 74% -78% and the curing agent is 18% -22%; the synthesis method of the polyaniline nano whisker comprises the following steps:
s1, dissolving phytic acid and aniline in 20mL of deionized water at room temperature, and strongly stirring for 5min to obtain a uniform orange-yellow solution A; ammonium persulfate is dissolved in 10mL of deionized water and is strongly stirred for 5min to obtain colorless transparent solution B;
s2, slowly adding the solution B into the solution A under the continuous strong stirring action to obtain a dark green solution, immediately stopping stirring, standing at 0-10 ℃ for reaction for 24 hours, and carrying out repeated centrifugation and washing, and then carrying out vacuum drying at 60 ℃ until the weight is constant, thus obtaining the polyaniline nanowhisker.
2. The polyaniline nanowhisker modified epoxy composite according to claim 1, wherein: in S1, the dosage of the phytic acid is 0.002-0.05 mol, the dosage of the aniline is 0.01-0.25 mol, and the dosage of the ammonium persulfate is 0.0025-0.0625 mol.
3. A method for preparing the polyaniline nanowhisker modified epoxy resin composite material according to claim 1, comprising the steps of:
s1, weighing a certain amount of polyaniline nanowhiskers, adding the polyaniline nanowhiskers into 20mL of acetone solution, treating the polyaniline nanowhiskers for 1h by using an ultrasonic cell grinder to perform pre-dispersion, slowly dripping the polyaniline nanowhiskers into an epoxy resin solution, and strongly stirring the polyaniline nanowhiskers for 2-6h to fully mix the polyaniline nanowhiskers and the epoxy resin solution;
s2, under the condition of continuous strong stirring, rapidly adding the curing agent into the mixed system, and continuously and strongly stirring for 1-3 hours; then pouring the mixture into a silica gel mold, vacuum degassing at 40-100 ℃ for 20-40min, and curing and forming at high temperature to obtain the polyaniline nano whisker modified epoxy resin composite material.
4. The method for preparing a polyaniline nanowhisker modified epoxy resin composite according to claim 3, wherein the curing agent is 4, 4-diaminodiphenylmethane.
5. The method for preparing the polyaniline nanowhisker modified epoxy resin composite material according to claim 3, wherein the mass ratio of the curing agent to the epoxy resin is 26.5:100.
6. the method for preparing a polyaniline nanowhisker modified epoxy resin composite material according to claim 3, wherein the epoxy resin solution is preheated at 50-90 ℃ for 20-50min, the curing agent is heated to a molten state at 90-120 ℃, and the silica gel mold is preheated at 40-80 ℃ for 20-40min.
7. The method for preparing the polyaniline nano whisker modified epoxy resin composite material according to claim 3, wherein the high temperature curing is performed at 100 ℃ for 2 hours and 150 ℃ for 2 hours.
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| 聚苯胺纳米纤维的合成及应用进展;蒋柳等;《化工新型材料》;第49卷(第06期);第47-50页 * |
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