CN115873272A - Carbon nano tube resin matrix composite material and preparation method thereof - Google Patents
Carbon nano tube resin matrix composite material and preparation method thereof Download PDFInfo
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- CN115873272A CN115873272A CN202211656289.3A CN202211656289A CN115873272A CN 115873272 A CN115873272 A CN 115873272A CN 202211656289 A CN202211656289 A CN 202211656289A CN 115873272 A CN115873272 A CN 115873272A
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Abstract
The invention discloses a carbon nano tube resin matrix composite material and a preparation method thereof. The preparation method comprises the following steps: uniformly mixing the carbon nano tube, the organic dispersant with the curing function, the resin and the solvent to form a carbon nano tube dispersion liquid; and then removing the solvent to obtain the carbon nano tube resin matrix composite material, wherein the organic dispersing agent contains amino. The method prepares the carbon nanotube resin-based composite material in situ, the selected dispersing agent is an organic dispersing agent, the dispersing agent contains amino, the resin can be cured while the dispersing effect is achieved, the interface combination between the carbon nanotube and the resin matrix can be enhanced, the problem that the resin in the carbon nanotube film is difficult to uniformly infiltrate in the traditional process is solved, the carbon nanotube resin-based composite material with excellent mechanical property is prepared, and the problems that the mechanical property of the composite material can be reduced by the dispersing agent in the traditional process, the process for removing the dispersing agent is complex and the effect is not ideal are solved.
Description
Technical Field
The invention relates to a carbon nano tube resin matrix composite material and a preparation method thereof, belonging to the technical field of nano composite materials.
Background
Carbon Nanotubes (CNTs) have high aspect ratios and excellent mechanical and electrical properties, and are considered to be ideal reinforcements for making high composite materials. The huge specific surface area of the carbon nano tube can enhance the interaction between the carbon nano tube and a resin matrix, so that higher stress transfer and energy dissipation are generated, and the strength and the toughness of the composite material are obviously improved.
The preparation method of the carbon nano tube resin matrix composite material mainly comprises a blending method and an impregnation method. The blending method is to directly disperse carbon nanotube powder in a resin matrix, and the method is simple to operate, low in process cost and capable of realizing large-scale production, but the prepared composite material is poor in performance due to the fact that the carbon nanotubes are poor in dispersibility and orientation in the matrix, and the problems of solvent residue and low content of the carbon nanotubes exist. The impregnation method can prepare the high-content carbon nanotube composite material with a certain degree of orientation, but the problems that resin is difficult to enter between carbon nanotube tubes, the content of the resin in the inner layer and the outer layer of an impregnation structure is inconsistent, the impregnation process is complex and the like exist in the preparation process. The carbon nanotube composite material prepared by the blending method and the dipping method has poor mechanical properties, and cannot give full play to the excellent mechanical properties of the carbon nanotube.
In addition, some researchers have dispersed carbon nanotubes in water by an aqueous dispersant to prepare carbon nanotube film products from an aqueous carbon nanotube dispersion. The prepared film has small porosity, contains a large amount of residual dispersant inside, and seriously influences the performance of the finally prepared composite material; although the dispersant is removed by a subsequent process method, the dispersant is difficult to completely remove, and the intrinsic structure of the carbon nanotube is damaged.
Moreover, when the composite material is further prepared, the carbon nanotube film needs to be impregnated with resin, so that the wet-process carbon nanotube film prepared in the industry at present has low porosity, the bulk density of the carbon nanotubes is high, the resin is often enriched on the surface of the film, and the infiltration of the internal resin is poor, so that the mechanical property of the film is not ideal.
Disclosure of Invention
The invention mainly aims to provide a carbon nanotube resin-based composite material (namely carbon nanotube film prepreg) and a preparation method thereof, so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of a carbon nano tube resin matrix composite material, which comprises the following steps:
uniformly mixing the carbon nano tube, the organic dispersant with the curing function, the resin and the solvent to form a carbon nano tube dispersion liquid;
and then removing the solvent to obtain the carbon nano tube resin matrix composite material, wherein the organic dispersing agent contains amino.
In some embodiments, the organic dispersant comprises any one or more of a combination of an unsaturated polyamine amide, an unsaturated polycarboxylic acid polymer and polysiloxane copolymer, an alkyl ammonium salt solution of an acidic copolymer containing hydroxyl functional groups, and an amine-based polymer containing pyrene structures.
The embodiment of the invention also provides the carbon nano tube resin matrix composite material prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
the method provided by the invention prepares the carbon nanotube resin-based composite material in situ, the selected dispersing agent is an organic dispersing agent, the dispersing agent contains amino, the resin can be cured while the dispersing effect is achieved, the interface combination between the carbon nanotube and the resin matrix can be enhanced, the problem that the resin in the carbon nanotube film is difficult to uniformly infiltrate in the traditional process is solved, the carbon nanotube resin-based composite material with excellent mechanical property is prepared, and the problems that the mechanical property of the composite material can be reduced by the dispersing agent in the traditional process, the process for removing the dispersing agent is complex and the effect is not ideal are solved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a graph showing the mechanical test of the product obtained in example 1 of the present invention.
Detailed Description
In view of the defects of the traditional technical scheme, the inventor of the present invention provides the technical scheme of the present invention through long-term research and a great deal of practice, wherein the technical scheme is mainly that the carbon nano tube is uniformly dispersed in a resin solution by using a modified dispersing agent/curing agent with dispersing and curing functions, the carbon nano tube is oriented by the shearing force of pipeline extrusion, and the oriented carbon nano tube prepreg product is obtained through the process steps of continuous suction filtration, drying, rolling and the like. The technical solution, its implementation and principles, etc. will be further explained as follows.
One aspect of the embodiments of the present invention provides a method for preparing a carbon nanotube resin-based composite material, including:
uniformly mixing the carbon nano tube, the organic dispersant with the curing function, the resin and the solvent to form a carbon nano tube dispersion liquid;
and then removing the solvent to obtain the carbon nano tube resin matrix composite material, wherein the organic dispersing agent contains amino.
In some embodiments, the organic dispersant preferably includes a compound of any one or more of an unsaturated polyamine amide, a low molecular weight unsaturated polycarboxylic acid polymer and polysiloxane copolymer, an alkyl ammonium salt solution of an acidic copolymer having a hydroxyl functional group, an amine-based polymer having a pyrene structure, and the like, but is not limited thereto. The dispersant selected by the invention is an organic dispersant with a curing function, contains an amino group, can cure resin while having a dispersing function, can enhance the interface bonding between the carbon nano tube and the resin matrix, solves the problems that the mechanical property of a composite material is reduced by the dispersant in the traditional process, the process for removing the dispersant is complex and the effect is not ideal, and simultaneously solves the problem that the resin in the carbon nano tube film is difficult to uniformly infiltrate.
In the invention, the organic dispersing agent containing amino is selected, the finally prepared composite material has better performance, and the amino mainly plays a role in improving the performance of the product.
In some embodiments, the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, multi-walled carbon nanotubes, and the like, or a combination thereof, but are not limited thereto. Wherein, the single component or the compound of the two components in any proportion can be used for preparing the carbon nano tube film prepreg, and the mechanical properties of the final product are different.
In some embodiments, the selection of the resin type includes a formulation of either or both of difunctional epoxy resins, trifunctional epoxy resins, and the like, with a pre-reaction of cyanamide. The bifunctionality or trifunctional epoxy resin can be compounded according to any proportion, the mass ratio of the compounded functionality a resin component to dicyandiamide is 100.
Further, the solvent includes any one or a combination of two or more of ethanol, isopropanol, DMF, NMP, xylene, isobutanol, and the like, but is not limited thereto.
In some embodiments, the mass ratio of the carbon nanotubes, the organic dispersant, the resin and the solvent is 1 to 8:1 to 50:10 to 40:100.
wherein the content ratio of the carbon nano tube is 1-8, which can reduce the production efficiency if the content ratio is lower, and can influence the dispersion effect if the content ratio is higher; the content ratio of the organic dispersant is 1-50, the dispersion effect is poor when the content ratio is lower, and the mechanical property is reduced when the content ratio is higher; the content ratio of the resin is 10-40, which can be adjusted, and the mechanical property can be influenced when the content ratio is lower, and the dispersion effect can be influenced when the content ratio is higher; the content ratio of the solvent is 100, and the dispersion effect is affected by the continuous reduction, and the production efficiency is reduced if the content ratio is higher.
In some embodiments, the mixing means includes any one or a combination of two or more of mechanical stirring, ultrasound, high pressure homogenization, microfluidization, and the like, but is not limited thereto.
Further, the parameter setting of the mechanical stirring can be calculated according to the rotating speed and the time. Specifically, the stirring speed is 100-500 rpm, the time is 10-60 min, and the optimal stirring speed is 20min by magnetic force.
Further, the parameter settings of the ultrasound may be calculated in terms of frequency, power, time. Specifically, the ultrasonic frequency is 10-50 kHz, the power is 20-200W, and the time is 10-60 min.
Further, the parameter setting of the high-pressure homogenization can be calculated according to the set pressure, time and processing amount. Specifically, the pressure is 100-400 Bar, the time and the treatment amount are 5-20 min/100mL, and the optimal pressure is 200bar homogeneity 5min/100mL.
Further, the parameter setting of the micro-jet can be calculated according to the set pressure and times. Specifically, the pressure is 600-1000 Bar, the times are 6-10 times, and the optimal time is 1000bar 6 times of micro-jet.
In some embodiments, the method of making comprises: and (3) performing suction filtration to remove the solvent at least by adopting a filter paper and suction filtration device, and then packaging to obtain the carbon nanotube resin-based composite material. In the invention, the carbon nano tube resin matrix composite material is prepared by suction filtration, and the solvent can be recycled.
Further, the preparation method comprises the following steps: sequentially carrying out suction filtration, drying and rolling to obtain the carbon nano tube resin matrix composite material with orientation.
In conclusion, the carbon nanotube resin-based composite material with excellent mechanical properties is successfully prepared by dispersing the carbon nanotube powder in the organic resin solution through the organic dispersing/curing agent and preparing the carbon nanotube film containing the resin in situ.
In another aspect, the embodiment of the invention also provides a high-carbon nanotube resin-based composite material prepared by the preparation method.
Further, the carbon nanotube resin-based composite material comprises a resin matrix and a continuous belt-shaped prepreg formed by carbon nanotubes uniformly dispersed in the resin matrix, wherein the carbon nanotubes are arranged in an orientation manner.
Further, the tensile strength of the carbon nano tube resin matrix composite material is 1.5-3 GPa.
In summary, in the above technical solutions, the carbon nanotube resin-based composite material is prepared in situ, the selected dispersant is an organic dispersant, and the dispersant contains an amine group, so that the resin can be cured while having a dispersing effect, the interfacial bonding between the carbon nanotube and the resin matrix can be enhanced, the problem that the resin in the carbon nanotube film is difficult to uniformly infiltrate in the conventional process is solved, the carbon nanotube prepreg with excellent mechanical properties is prepared, and the problems that the mechanical properties of the composite material can be reduced by the dispersant in the conventional process, the process for removing the dispersant is complicated, and the effect is not ideal are also solved.
Hereinafter, embodiments of the present invention will be described in detail. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided to explain the principles of the invention and the practical application, thereby enabling others skilled in the art to better understand the invention for various embodiments and with various modifications as are suited to the particular use contemplated.
Unless otherwise specified, various raw materials, production equipment, test equipment, and the like used in the following examples are commercially available. The test methods employed therein are also known in the art.
Example 1
Selecting trifunctional epoxy resin TDE85 and difunctional epoxy resin E51 according to a mass ratio of 3:2, compounding, namely mixing the compounded resin with dicyandiamide according to the mass ratio of 100: and 13, mixing by using a three-roll grinder for later use.
In the embodiment, the single-walled carbon nanotube is selected for dispersion treatment, the amine-based polymer containing a pyrene structure is used as a dispersing agent, the resin component prepared in the process is used as a matrix phase, and DMF is used as a solvent. The mass ratio of the carbon nano tube to the dispersant to the resin to the solvent is 4:8:20:100, and dispersing the carbon nano tube by a high-pressure homogenization method under the dispersion process condition of 200bar and 5min/100mL to obtain a stable carbon nano tube dispersion liquid after the dispersion is finished.
Extruding the carbon nanotube dispersion liquid to the surface of the translational filter paper through the flat needle, keeping the vacuum filtration state below the filter paper, and rolling the carbon nanotube film after the carbon nanotube film enters a drying area and is heated and dried. The orientation of the carbon nano-tube is realized by the shearing action in the needle head, and the solvent in the filter flask can be recycled (containing resin and dispersant). The prepared carbon nano tube resin-based composite material needs to be sealed and frozen at the temperature of 20 ℃.
According to the preparation requirement of a test sample, after thawing, cutting the carbon nano tube resin matrix composite material into 3cm × 1cm size, and after hot pressing and curing at 150 ℃/2h, measuring the tensile strength of the carbon nano tube resin matrix composite material, wherein the measured value is 2.5-3 GPa.
Example 2
Selecting trifunctional epoxy resin TDE85 and bifunctional epoxy resin E51 according to the mass ratio of 3:2, compounding, namely mixing the compounded resin with dicyandiamide according to the mass ratio of 100: and 13, mixing by using a three-roll grinder for later use.
In this example, the single-walled carbon nanotube is dispersed, an alkyl ammonium salt solution of an acidic copolymer containing a hydroxyl functional group is used as a dispersant, a resin component prepared in the above process is used as a matrix phase, and NMP is used as a solvent. The mass ratio of the carbon nano tube to the dispersant to the resin to the solvent is 1:1:10:100, and dispersing the carbon nano tube by a high-pressure homogenization method under the dispersion process condition of 100bar 15min/100mL to obtain a stable carbon nano tube dispersion liquid after the dispersion is finished.
Extruding the carbon nano tube dispersion liquid to the surface of the translational filter paper through the flat needle, keeping the vacuum filtration state below the filter paper, and rolling the carbon nano tube film which finishes the filtration process after the carbon nano tube film enters a drying area and is heated and dried. The orientation of the carbon nano-tube is realized by the shearing action in the needle head, and the solvent in the filter flask can be recycled (containing resin and dispersant). The prepared carbon nano tube film prepreg needs to be sealed and frozen at the temperature of 20 ℃.
And (3) thawing the carbon nano tube resin matrix composite material according to the preparation requirement of a test sample, cutting the thawed carbon nano tube resin matrix composite material into 3cm x 1cm, and measuring the tensile strength of the carbon nano tube resin matrix composite material after hot-pressing curing at the temperature of 150 ℃/2h, wherein the measured value is 1.5-1.8 GPa.
Example 3
Selecting trifunctional epoxy resin TDE85 and bifunctional epoxy resin E51 according to the mass ratio of 3:2, compounding, namely mixing the compounded resin with dicyandiamide according to the mass ratio of 100: and 13, mixing by using a three-roll grinder for later use.
In the embodiment, the single-walled carbon nanotube is selected for dispersion treatment, the unsaturated polycarboxylic acid polymer and the polysiloxane copolymer are used as dispersing agents, the resin component prepared in the process is used as a matrix phase, and isopropanol is used as a solvent. The mass ratio of the carbon nano tube to the dispersant to the resin to the solvent is 8:50:40:100, and dispersing the carbon nano tube by a high-pressure homogenization method under the dispersion process condition of 400bar 20min/100mL to obtain stable carbon nano tube dispersion liquid after the dispersion is finished.
Extruding the carbon nanotube dispersion liquid to the surface of the translational filter paper through the flat needle, keeping the vacuum filtration state below the filter paper, and rolling the carbon nanotube film after the carbon nanotube film enters a drying area and is heated and dried. The orientation of the carbon nano-tube is realized by the shearing action in the needle head, and the solvent in the filter flask can be recycled (containing resin and dispersant). The prepared carbon nano tube film prepreg needs to be sealed and frozen at the temperature of 20 ℃.
According to the preparation requirement of a test sample, after thawing, cutting the carbon nano tube resin matrix composite material into 3cm × 1cm size, and after hot pressing and curing at 150 ℃/2h, measuring the tensile strength of the carbon nano tube resin matrix composite material, wherein the measured value is 1.6-1.8 GPa.
Example 4
This example is different from example 1 in that: the carbon nano tube is a multi-wall carbon nano tube, the organic dispersing agent is unsaturated polyamine amide, and the solvent is dimethylbenzene and isobutanol. The mixing mode adopts micro-jet flow, the pressure is 1000Bar, and the times are 6.
And (3) thawing the carbon nano tube resin matrix composite material according to the preparation requirement of a test sample, cutting the thawed carbon nano tube resin matrix composite material into 3cm x 1cm, and measuring the tensile strength after hot-pressing curing at the temperature of 150 ℃/2h, wherein the measured value is 2.1-2.3 GPa.
Example 5
This example is different from example 1 in that: the solvent is ethanol. The mixing method adopts micro-jet flow, the pressure is 600Bar, and the times are 10 times.
And (3) thawing the carbon nano tube resin matrix composite material according to the preparation requirement of a test sample, cutting the thawed carbon nano tube resin matrix composite material into 3cm x 1cm, and measuring the tensile strength after hot-pressing curing at the temperature of 150 ℃/2h, wherein the measured value is 2.0-2.1 GPa.
Example 6
This example is different from example 1 in that: the mixing mode adopts mechanical stirring, the rotating speed is 100-500 rpm, and the time is 10-60 min.
According to the preparation requirement of a test sample, after thawing, cutting the carbon nano tube resin matrix composite material into 3cm × 1cm size, and after hot pressing and curing at 150 ℃/2h, measuring the tensile strength of the carbon nano tube resin matrix composite material, wherein the measured value is 1.6-2.3 GPa.
Example 7
This example is different from example 1 in that: the mixing mode adopts ultrasound, the frequency of the ultrasound is 10-50 kHz, the power is 20-200W, and the time is 10-60 min.
According to the preparation requirement of a test sample, after thawing, cutting the carbon nano tube resin matrix composite material into 3cm × 1cm size, and after hot pressing and curing at 150 ℃/2h, measuring the tensile strength of the carbon nano tube resin matrix composite material, wherein the measured value is 1.8-2.4 GPa.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
Comparative example 1
The comparative example differs from example 1 in that: the dispersants used do not contain amine groups.
According to the preparation requirement of a test sample, after thawing, cutting the carbon nano tube resin matrix composite material into 3cm × 1cm size, and after hot pressing and curing at 150 ℃/2h, measuring the tensile strength of the carbon nano tube resin matrix composite material, wherein the measured value is 0.5-0.8 GPa.
Comparative example 2
Compared with the embodiment 1, the comparative example is characterized in that the mass ratio of the carbon nano tube, the dispersant, the resin and the solvent is 1:1:10:200 are mixed.
A continuously formed carbon nanotube ribbon cannot be obtained when the carbon nanotube dispersion is extruded through a flat needle.
Comparative example 3
Compared with the embodiment 1, the comparison example is characterized in that the mass ratio of the carbon nano tube, the dispersant, the resin and the solvent is 8:50:40:50, and mixing.
After dispersion treatment, the dispersion liquid has obvious agglomeration state, and stable carbon nano tube dispersion liquid cannot be obtained.
Although the present invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (10)
1. A preparation method of a carbon nano tube resin matrix composite material is characterized by comprising the following steps:
uniformly mixing the carbon nano tube, the organic dispersant with the curing function, the resin and the solvent to form a carbon nano tube dispersion liquid;
and then removing the solvent to obtain the carbon nano tube resin matrix composite material, wherein the organic dispersing agent contains amino.
2. The production method according to claim 1, characterized in that: the organic dispersing agent comprises any one or a compound of more than two of unsaturated polyamine amide, unsaturated polycarboxylic acid polymer and polysiloxane copolymer, alkyl ammonium salt solution of acidic copolymer containing hydroxyl functional groups and amine polymer containing pyrene structures.
3. The production method according to claim 1, characterized in that: the carbon nanotube comprises any one or a compound of a single-walled carbon nanotube and a multi-walled carbon nanotube.
4. The method of claim 1, wherein: the resin comprises any one or a compound of two of bifunctional epoxy resin and trifunctional epoxy resin.
5. The method of claim 1, wherein: the solvent comprises any one or the combination of more than two of ethanol, isopropanol, DMF, NMP, xylene and isobutanol.
6. The method of claim 1, wherein: the mass ratio of the carbon nano tube, the organic dispersant, the resin and the solvent is 1-8: 1 to 50:10 to 40:100.
7. the method of claim 1, wherein: the mixing mode comprises any one or the combination of more than two of mechanical stirring, ultrasound, high-pressure homogenization and micro-jet.
8. The production method according to claim 1, characterized in that: the rotation speed of the mechanical stirring is 100-500 rpm, and the time is 10-60 min; and/or the ultrasonic frequency is 10-50 kHz, the power is 20-200W, and the time is 10-60 min; and/or the pressure of the high-pressure homogenization is 100-400 Bar, and the time and the treatment capacity are 5-20 min/100mL; and/or the pressure of the micro-jet is 600-1000 Bar, and the times are 6-10.
9. The method of claim 1, comprising: performing suction filtration to remove the solvent at least by adopting a filter paper and suction filtration mode; and/or, the preparation method comprises the following steps: sequentially carrying out suction filtration, drying and rolling to obtain the carbon nano tube resin matrix composite material with orientation.
10. A carbon nanotube resin-based composite material produced by the production method according to any one of claims 1 to 9;
the carbon nano tube resin matrix composite material comprises a resin matrix and a continuous belt-shaped prepreg formed by carbon nano tubes uniformly dispersed in the resin matrix, wherein the carbon nano tubes are arranged in an orientation manner;
preferably, the tensile strength of the carbon nanotube resin-based composite material is 1.5-3 GPa.
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