CN113150502A - Electrically-driven glass polymer material and preparation method thereof - Google Patents
Electrically-driven glass polymer material and preparation method thereof Download PDFInfo
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- CN113150502A CN113150502A CN202110366567.0A CN202110366567A CN113150502A CN 113150502 A CN113150502 A CN 113150502A CN 202110366567 A CN202110366567 A CN 202110366567A CN 113150502 A CN113150502 A CN 113150502A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
Abstract
The invention provides an electrically-driven glass polymer material, which comprises an epoxy resin cross-linked network containing dynamic ester bonds, a Carbon Nano Tube (CNT) and carbon fibers, wherein E-51 resin, sebacic acid and phthalic anhydride are used as monomers, and the epoxy resin glass polymer material containing the dynamic ester bonds is synthesized under the action of a catalyst 1,5, 7-triazabicyclo [4,4,0] dec-5-ene (TBD); the cross-linked network can be rearranged through ester exchange reaction, so that the material can be remolded, welded, repaired and recycled at high temperature, and can be used for preparing devices with complex shapes; has properties similar to those of conventional thermosetting resins at low temperatures. The material has higher glass transition temperature, and the doping of the carbon nano tube and the carbon fiber ensures that the material has good electric drive performance and mechanical property, and can be widely applied to the field of functional materials as a drive material, such as the field of aerospace and the like.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to an electrically-driven glass high polymer material and a preparation method thereof.
Background
The development of a space variable structure is an important research direction in the field of aerospace nowadays. The expansion of the structures such as the antenna and the solar panel after the spacecraft is in orbit, the profile compensation and the posture adjustment after the expansion all depend on the allosteric function. Therefore, the method improves the variable structure capability of the space structure, and plays an important role in improving the working efficiency of equipment such as satellites and antennas and enhancing the flexibility and maneuverability of the equipment. The unfolding and the transformation of the traditional space structure are mainly realized by mechanical modes such as spring lock nets, mechanical pull ropes, motor drive and the like. However, the mechanical structure has the limitations of heavy structure, poor flexibility, complex control, high cost and the like, and thus the development requirements of large-scale, light-weight and intelligent novel space equipment in the future cannot be met gradually. The intelligent material is applied to aerospace manufacturing, the device structure is expected to be simplified, the structure weight is reduced, the manufacturing cost is reduced, a new implementation way is provided for functions of large-size expansion, programmable expansion, reflection profile regulation, mass center regulation and the like of a space structure, and a new function is provided for a spacecraft.
Due to the extreme environment of high vacuum, high radiation and strong temperature difference (low orbit +/-100 ℃ and high orbit +/-200 ℃) of the outer space and the ultrahigh instantaneous acceleration existing in the rocket launching process, the aerospace device needs to have higher mechanical strength and thermal stability, so that the application of a large amount of intelligent materials such as gel and the like is limited. In addition, in the space environment, the electric energy possesses the advantage of acquireing easily, be convenient for store, response is rapid, the controllability is strong, compares other energy forms, is applicable to spatial structure's control more. Therefore, the electrically-driven intelligent material which can meet the use requirements of space environment and has light weight, high thermal stability and high mechanical strength has greater development potential in the future.
The inventor already applies for the invention with patent application number 202010693858.6, named as conductive glass polymer material and a preparation method thereof, uses bisphenol A diglycidyl ether and sebacic acid as reaction raw materials, uses TBD as a catalyst, and adds silver-coated glass fiber and CNT. Although the obtained material has good conductivity and toughness, the material cannot reach the aerospace application standard at the glass transition temperature and strength.
Disclosure of Invention
Therefore, the invention provides an electrically-driven glass polymer material and a preparation method thereof, and the electrically-driven composite material, the structure and the device which can be subjected to three-dimensional shaping, can generate three-dimensional deformation, can realize reciprocating driving and have high thermal stability and mechanical stability are obtained by combining the properties of the glass polymer with the shape memory polymer material. Therefore, the method provides support for the development of an electric drive device with a three-dimensional variable structure in space, and fills the blank of the field of glass-like polymers in the aspects of space application and electric response property research.
The invention provides an electrically-driven glass polymer material, which comprises an epoxy resin cross-linked network containing dynamic ester bonds, Carbon Nano Tubes (CNT) and carbon fibers, wherein E-51 resin, sebacic acid and phthalic anhydride are used as monomers, and the epoxy resin glass polymer material containing the dynamic ester bonds is synthesized under the action of a catalyst 1,5, 7-triazabicyclo [4,4,0] dec-5-ene (TBD).
Preferably, the E-51 resin, sebacic acid, and phthalic anhydride are present in a ratio of 4:0.93: 1.66: 0.55: 0.68, melting at 120-130 ℃, adding a catalyst TBD accounting for 7-10% of the E51 resin, and carrying out pre-crosslinking reaction.
Preferably, the epoxy resin crosslinked network containing dynamic ester bonds is subjected to a rapid ester exchange reaction at the temperature of 180-230 ℃, and the ester bonds in the epoxy resin crosslinked network are rearranged.
Preferably, the CNT is added in an amount of 7-10 wt%, and the carbon fiber is added in an amount of 13-20 wt%.
Preferably, the glass transition temperature of the electrically-driven glass polymer material is 110 ℃, the tensile strength is 80MPa, the tensile modulus is 1.2GPa, the bending strength is 120MPa, and the bending modulus is 8.5 GPa.
The invention also provides a preparation method of the electrically-driven glass polymer material, which comprises the following steps: mixing the reaction raw material E-51 resin and sebacic acid, heating to 120-130 ℃ to melt the resin, then adding phthalic anhydride, continuously heating to keep the temperature at 120-130 ℃ until the phthalic anhydride is completely melted, then adding a catalyst TBD, CNT and carbon fibers into the molten mixture, and rapidly stirring to obtain a mixture.
Preferably, the method further comprises a pressing process, wherein the pressing process comprises the following steps: and placing the obtained mixture into a template, sequentially covering the upper surface and the lower surface of the template with a polytetrafluoroethylene film and an aluminum plate, tabletting by using a powder tablet press, wherein the hot pressing temperature is 180-200 ℃, the pressure is 2-4 MPa, the time is 2-4 h, and the thickness of the template is 0.2-2 mm.
The invention also provides application of the electrically-driven glass polymer material in preparation of a three-dimensional deformation structure.
Preferably, the deformation structure is a pod rod structure or a four-arm structure.
The invention also provides an application of the electrically-driven glass polymer material in preparing a three-dimensional allosteric device.
The electrically-driven glass polymer material is prepared by crosslinking an epoxy resin crosslinking network containing dynamic ester bonds by using E-51 resin, sebacic acid and phthalic anhydride as monomers under the action of a catalyst TBD. By optimizing the chemical composition, the high glass transition temperature of the material is realized. In the presence of a catalyst TBD, a rapid ester exchange reaction can occur in the crosslinked network at a certain temperature, and the crosslinked network can be rearranged to embody the characteristic of dynamic chemical bonds, so that the electrically-driven glass high polymer material has good heavy plasticity, self-repairability and weldability, and has tensile property.
The invention can adjust the mechanical and electrical properties of the electrically-driven glass macromolecule by doping the CNT and the carbon fiber. When the carbon nano tube is singly doped, the material has electric drive property but limited mechanical strength; through the composite carbon fiber, the breaking strength and modulus of the material are remarkably improved.
The electric-driven glass polymer material doped with the carbon nano tubes and the carbon fibers can form a film through pressing, and tests show that the film has remarkably enhanced mechanical toughness, and more importantly, the film has excellent electric-driven characteristics, such as the electric-driven glass polymer material doped with 10 wt% of CNT and 15 wt% of carbon fibers. By means of dynamic covalent bond, the polymer film can be self-repaired, further welded and shaped into different structures.
In addition, the elastic modulus of the electrically-driven glass polymer material can be regulated and controlled by regulating and controlling the proportion of sebacic acid and phthalic anhydride in the raw materials. Within a certain range, the higher the proportion of sebacic acid is, the better the flexibility of the material is; conversely, the higher the proportion of phthalic anhydride, the greater the stiffness of the material. In addition, the strength and modulus of the material can be regulated by regulating the amount of the carbon fibers, the strength of the material is increased along with the increase of the content of the carbon fibers in a certain range, and then the strength of the material is kept unchanged after the content of the carbon fibers is increased. As the doping of the carbon nano tubes and the carbon fibers and the proportion of the sebacic acid and the phthalic anhydride can be adjusted, various physical and chemical properties of the film can be adjusted.
Therefore, the novel material has good electric drive characteristics, has the characteristics of three-dimensional deformation, remolding, welding and repairability, can be spliced into a specific three-dimensional structure from a simple shape, has high mechanical strength, high glass transition temperature and high stable temperature, and has high application value.
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.
FIG. 1a is a schematic view of a pod rod structure made of electrically driven glass-like polymer material according to the present invention;
FIG. 1b is a photograph showing the structure of the pod rod made of the electrically driven glass-like polymer material according to the present invention;
FIG. 2a is a schematic view of a four-arm structure made of an electrically-driven glass polymer material according to the present invention;
FIG. 2b is a photograph showing a four-arm structure prepared from the electrically-driven glass polymer material according to the present invention;
FIG. 3a is a plot of modulus versus temperature for an electrically driven glass polymer material in accordance with the present invention;
FIG. 3b is a DSC chart of the electrically driven glass polymer material of the present invention;
FIG. 4a is a graph showing the results of a tensile test of an electrically-driven glass polymer material according to the present invention;
FIG. 4b is a graph showing the bending test result of the electrically-driven glass polymer material according to the present invention;
FIG. 5 is a test of the electrically driven deployment performance of the pod rod configuration of the present invention;
fig. 6 is a test of the electrically driven retraction performance of the four arm structure of the present invention.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The reagents and raw materials used in this specification are all commercially available products except for special instructions.
Example 1
This example provides an electrically-driven glass polymer material, which comprises a crosslinked network of epoxy resin containing dynamic ester bonds, wherein the crosslinked network uses E-51 resin, sebacic acid, and phthalic anhydride as reaction raw materials, uses 1,5, 7-triazabicyclo [4,4,0] dec-5-ene (TBD) as a catalyst, and the chemical formula of the catalyst TBD is shown in chemical formula 1, and the chemical reaction process is shown in synthetic chemical reaction 1.
Chemical formula 1:
synthetic chemistry reaction 1:
the preparation process of the electrically-driven glass polymer material in the embodiment is as follows: 4g of epoxy resin E-51 and 0.93g of sebacic acid are placed in a heating jacket and heated to 130 ℃ to melt the raw materials, phthalic anhydride is added into the mixture, the mixture is continuously heated until all phthalic anhydride is melted, 0.284g of 1,5, 7-triazabicyclo [4,4,0] dec-5-ene and 0.55g of carbon nano tube are added into the melted mixture, after rapid stirring is carried out for 50s, the obtained mixture is pressed for 4h under the environment of 4MPa and 180 ℃, and the electrically-driven glass-transition-temperature-like glass polymer material is obtained.
Example 2
The electrically-driven glass polymer material provided in this example is different from example 1 in that: weighing 4g of epoxy resin E-51 and 0.93g of sebacic acid, placing the epoxy resin E-51 and 0.93g of sebacic acid in a heating jacket, heating to 130 ℃ to melt the raw materials, then adding phthalic anhydride into the mixture, continuously heating until all phthalic anhydride is melted, adding 0.284g of 1,5, 7-triazabicyclo [4,4,0] dec-5-ene, 0.55g of carbon nano tube and 0.68g of carbon fiber powder (200um) into the molten mixture, rapidly stirring for 50s, and pressing the obtained mixture for 4h under the environment of 4MPa and 180 ℃ to obtain the carbon fiber reinforced electric-driven high glass transition temperature glass-like polymer material.
Example 3
This example provides an electrically driven glass polymer material, which is prepared by placing 4.58g of the pre-crosslinked product obtained in example 2 in a 5cm × 5cm × 1mm template, covering the template with a polytetrafluoroethylene film and an aluminum plate, and tabletting the coated product with a powder tabletting machine at 180 ℃ under 4MPa for 4 hours.
Example 4
This example provides an electrically driven glass polymer material, which is prepared by placing 3.44g of the pre-crosslinked product obtained in example 2 in a 7.5cm × 5cm × 0.5mm mold, covering with a polytetrafluoroethylene film and an aluminum plate, and tabletting with a powder tablet press at 180 ℃ under 4MPa for about 4 hours.
Example 5
This example provides an electrically driven glass polymer material, which is prepared by placing 30.5g of the pre-crosslinked product obtained in example 2 in a 9.5cm × 25cm × 0.7mm mold, covering with a polytetrafluoroethylene film and an aluminum plate, and tabletting with a powder tablet press at 180 ℃ under 2MPa for 2 hours.
Example 6
This example provides an electrically driven pod rod structure, as shown in fig. 1a and 1b, by placing the films from examples 3, 4, and 5 in a custom mold and shaping at 200 ℃ for 10 min.
Example 7
This example provides an electrically driven four-wall unfolding and folding structure, as shown in fig. 2a and 2b, the films obtained in examples 3, 4 and 5 were placed in a custom mold and shaped at 200 ℃ for 10min to obtain a four-arm unfolding structure.
Examples of the experiments
Firstly, testing the glass transition temperature:
the glass transition temperature of the materials obtained in examples 3, 4 and 5 was measured by dynamic thermomechanical analysis to be about 110 c, as shown in figure 3 a. FIG. 3b shows DSC curves of materials with different ratios of sebacic acid to phthalic anhydride measured by differential scanning calorimetry, and it can be seen that as the content of phthalic anhydride increases, the final glass transition temperature can reach more than 110 ℃, which meets the use requirements of low-orbit space environment.
II, mechanical testing:
mechanical property tests including tensile test and bending test were performed on the materials obtained in examples 3, 4 and 5 by a dynamic thermomechanical analyzer, and fig. 4a shows the tensile test results and fig. 4b shows the bending test results. The test result shows that the tensile breaking strength of the material is improved to 80MPa, the tensile modulus is 1.2GPa, the bending strength is improved to 120MPa, and the bending modulus is 8 GPa.
Thirdly, driving test:
the pod rod samples prepared in example 6 were subjected to an electrical test and the structures were found to unfold at 20V over 100s, as shown in figure 5.
The four-arm sample prepared in example 7 was subjected to an energization test, and it was found that the structure was developed at a voltage of 25V over 100 seconds, as shown in FIG. 6.
Experiments show that the structure of the electrically-driven glass polymer material based on the invention has electrically-driven three-dimensional deformation capability.
The electrically-driven glass polymer material provided by the invention not only has excellent electrically-driven characteristics, but also has the properties of being electrically driven, remoldable, three-dimensional deformable and the like, so that the possibility that the material is applied to a functional material device with a complex geometric shape is greatly improved; the electrically-driven glass material can be widely applied to the fields of aerospace grippers, electrically-driven unfolding trusses and the like.
It is obvious that the above examples are only examples for clearly illustrating, but limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. An electrically-driven glass polymer material is characterized by comprising an epoxy resin cross-linked network containing dynamic ester bonds, Carbon Nano Tubes (CNT) and carbon fibers, wherein E-51 resin, sebacic acid and phthalic anhydride are used as monomers, and the epoxy resin glass polymer material containing the dynamic ester bonds is synthesized under the action of a catalyst 1,5, 7-triazabicyclo [4,4,0] dec-5-ene (TBD).
2. The electrically-driven glass polymer material according to claim 1, wherein the E-51 resin, sebacic acid and phthalic anhydride are mixed in a ratio of 4:0.93: 1.66: 0.55: 0.68, melting at 120-130 ℃, adding a catalyst TBD accounting for 7-10% of the E51 resin, and carrying out pre-crosslinking reaction.
3. The electrically driven glass polymer material according to claim 2, wherein the epoxy resin crosslinked network containing dynamic ester bonds undergoes a rapid transesterification reaction at a temperature of 180 ℃ to 230 ℃, and the ester bonds inside the epoxy resin crosslinked network are rearranged.
4. The electrically-driven glass polymer material according to claim 3, wherein the CNT is added in an amount of 7 to 10 wt%, and the carbon fiber is added in an amount of 13 to 20 wt%.
5. The electrically-driven glass polymer material according to claim 4, wherein the glass transition temperature of the electrically-driven glass polymer material is 110 ℃, the tensile strength is 80MPa, the tensile modulus is 1.2GPa, the bending strength is 120MPa, and the bending modulus is 8.5 GPa.
6. The process for producing an electrically driven glass polymer material according to any one of claims 1 to 5, comprising the steps of: mixing the reaction raw material E-51 resin and sebacic acid, heating to 120-130 ℃ to melt the resin, then adding phthalic anhydride, continuously heating to keep the temperature at 120-130 ℃ until the phthalic anhydride is completely melted, then adding a catalyst TBD, CNT and carbon fibers into the molten mixture, and rapidly stirring to obtain a mixture.
7. The method for preparing an electrically-driven glass polymer material according to claim 6, further comprising a pressing process, wherein the pressing process comprises: and placing the obtained mixture into a template, sequentially covering the upper surface and the lower surface of the template with a polytetrafluoroethylene film and an aluminum plate, tabletting by using a powder tablet press, wherein the hot pressing temperature is 180-200 ℃, the pressure is 2-4 MPa, the time is 2-4 h, and the thickness of the template is 0.2-2 mm.
8. The electric-driven glass polymer material is applied to preparing a three-dimensional deformation structure.
9. Use of an electrically driven glass-like polymer material according to claim 8, wherein the deformation structure is a pod rod structure or a four-arm structure.
10. The application of the electrically-driven glass polymer material in preparing a three-dimensional allosteric device.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116041910A (en) * | 2023-02-24 | 2023-05-02 | 华中科技大学 | High-rigidity high-damping self-healing composite material based on epoxy resin and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116041910A (en) * | 2023-02-24 | 2023-05-02 | 华中科技大学 | High-rigidity high-damping self-healing composite material based on epoxy resin and preparation method thereof |
| CN116041910B (en) * | 2023-02-24 | 2024-02-02 | 华中科技大学 | High-rigidity high-damping self-healing composite material based on epoxy resin and preparation method thereof |
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