CN112852109A - Preparation method of high-temperature self-repairing hot-mix epoxy asphalt material - Google Patents
Preparation method of high-temperature self-repairing hot-mix epoxy asphalt material Download PDFInfo
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- CN112852109A CN112852109A CN202110049177.0A CN202110049177A CN112852109A CN 112852109 A CN112852109 A CN 112852109A CN 202110049177 A CN202110049177 A CN 202110049177A CN 112852109 A CN112852109 A CN 112852109A
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3462—Six-membered rings
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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
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/22—Di-epoxy compounds
- C08G59/24—Di-epoxy compounds carbocyclic
- C08G59/245—Di-epoxy compounds carbocyclic aromatic
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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
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4207—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aliphatic
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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
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4223—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aromatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- Epoxy Resins (AREA)
Abstract
The invention discloses a preparation method of a high-temperature self-repairing hot-mix epoxy asphalt material, which consists of a component A, a component B and a component C, wherein the component A and the component B are hot-pressed at high temperature to form the epoxy asphalt material, the component C is introduced and uniformly mixed, and a hot press is used for applying a certain pressure to cure at high temperature to obtain the hot-mix epoxy asphalt material with self repairing.
Description
Technical Field
The invention relates to the field of bridge deck pavement repair materials, in particular to a preparation method of a high-temperature self-repairing hot-mix epoxy asphalt material.
Background
The steel bridge deck pavement structure layer has the main function of protecting a steel bridge deck, and according to the experience of a general vehicle for many years, the steel bridge deck pavement structure layer material is promoted to be converted into an upper layer epoxy asphalt concrete and a lower layer epoxy asphalt concrete structure from initial pouring type asphalt concrete in the face of huge economic loss caused by various maintenance problems (such as cracks, cracking, bulge damage, delamination between pavement layers, slippage and the like), and finally, the steel bridge deck pavement structure layer material is converted into a double-layer epoxy asphalt concrete structure with better performance. But the method is far from enough, still can cause lower floor's steel bridge deck plate to rust because of disease such as fracture, leads to the great reduction of life.
At present, most of solutions for the problem of pathological changes and diseases of epoxy asphalt pavement layer structures are carried out by adopting a repairing technology, namely, the large-scale diseases are filled by manually adding epoxy asphalt or asphalt materials again, but the method cannot solve the disadvantages of the performance of base materials, so the appearance is not beautiful after repairing, the using effect is not good, the base materials are easy to be damaged again due to external influence, and the other solution and maintenance method for the pathological changes of the steel bridge deck pavement layer is reconstruction, but the construction period of the method is longer, a large amount of manpower and material resources are generally consumed, in the maintenance period, the maintenance place is required to be interrupted, the traffic is delayed to a great extent, and the maintenance cost is overhigh,
in the prior art, the research on the epoxy asphalt pavement material capable of self-repairing at high temperature is basically absent, so that the discovery of a hot-mix epoxy asphalt material capable of generating repairing performance by simple heating assistance per se as a structural material of a pavement layer of a steel bridge deck is urgent, and the hot-mix epoxy asphalt material has great application value and economic benefit.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a high-temperature self-repairing hot-mix epoxy asphalt material, which solves the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-temperature self-repairing hot-mix epoxy asphalt material comprises the following steps of preparing a component A, a component B and a component C; the component A is an epoxy resin compound, the component B is a curing agent, and the component C is a transesterification catalyst; the preparation method of the epoxy asphalt material comprises the following specific steps:
s1, placing the component A and the component B with the molar ratio of 1-1.5:1-1.5 in a container for mechanical stirring or ultrasonic sound, and mixing to obtain a uniform mixture Y1;
s2, introducing the component C into the mixture Y1 and manually stirring for 10min until the mixture is uniform to obtain a viscous mixture Y2;
s3, finally, placing the sticky mixture Y2 between two glass slides covered by polytetrafluoroethylene template tapes, and applying pressure to the glass slides by a hot press at high temperature for curing to obtain the self-repairing hot-mixed epoxy asphalt material.
Preferably, the epoxy resin compound is bisphenol a type epoxy resin, diglycidyl ether of 4,4 '-dihydroxybiphenyl, or 4,4' -dihydroxy-a-methylstyrene diglycidyl ether.
Preferably, the curing agent is oxalic acid, sebacic acid, glutaric acid, pripol 1040 (a mixture of two or three acids), citric acid trihydrate, suberic acid, phthalic anhydride, succinic anhydride, glutaric anhydride or methyltetrahydrophthalic anhydride.
Preferably, the transesterification catalyst is zinc acetate, stannous octoate, 1,5, 7-triazabicyclo [4.4.0] dec-5-ene or zinc acetylacetonate.
Preferably, the molar ratio of the component A to the component B in the step S1 is 1:1.
Preferably, the stirring or ultrasonic treatment time in step S1 is 20 min.
Preferably, the component C introduced in the step S2 accounts for 1-5% of the mole fraction of the mixture Y1.
Preferably, the component C introduced in the step S2 accounts for 5% of the mole fraction of the mixture Y1.
Preferably, the specific parameters of the hot press for applying pressure at high temperature in step S3 are: the temperature is 180 ℃, the pressure is 4-6Mpa, and the curing time is 6 h.
The invention has the beneficial effects that:
1. the epoxy glass body prepared by the invention has accelerated ester exchange reaction at the temperature above the Tv temperature, so that the material has the ability of stress relaxation and self-healing, has the properties of cycle reprocessing and self-healing, and can automatically heal scratches and crack breakage parts in a short time under the heating condition.
2. According to the invention, the epoxy glass polymer material containing the dynamic covalent bond is introduced into the hot-mix asphalt steel bridge deck pavement material, so that the overall mechanical property of the asphalt material is improved, and the asphalt material is endowed with the high-temperature self-repairing capability, thereby being beneficial to the close protection of a steel bridge pavement structure layer on a lower layer steel bridge deck to a greater extent, reducing the manpower and capital invested in daily maintenance and repair, and greatly prolonging the service life of the steel bridge deck.
3. Substances with photoresponse performance (such as azobenzene, CNT, GO, aniline, AgNW and the like) can be added into the system, so that the repairing is carried out by means of light driving, under the condition that the external temperature is lower in winter, cracks and defects can be repaired through illumination without heating, the healing function is achieved, and the repairing efficiency is greatly improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Placing epoxy material bisphenol A epoxy resin DGEBA (component A) and curing agent sebacic acid (component B) with a molar ratio of 1:1 in a suitable container, mechanically stirring or ultrasonically stirring for 20min to mix the two into a uniform mixture, then introducing a transesterification catalyst 1,5, 7-triazabicyclo [4.4.0] -5-decene (5 mol% of the amount relative to the carboxyl-COOH molar content) (component C) into the mixture, stirring the mixture by using an instrument for 10min until the mixture is uniform, finally placing the uniformly mixed viscous mixture between two glass slides covered by polytetrafluoroethylene membrane plate adhesive tapes, applying 6MPa pressure at high temperature of 180 ℃ by using a hot press, and curing for 6 hours, wherein the thickness of the film can be controlled by placing a gasket between the two plates.
The epoxy glass body prepared in the embodiment 1 has the repairing performance of more than 93 percent at the high temperature of 180 ℃ and the mechanical strength of 3.1MPa, and the repairing time is 20 min.
Example 2
Placing diglycidyl ether of 4,4' -dihydroxybiphenyl (component A) and glutaric acid (component B) as curing agent at a molar ratio of 1:1.2 in a suitable container, mechanically stirring or ultrasonically stirring for 20min to obtain a uniform mixture, adding 1,5, 7-triazabicyclo [4.4.0] -5-decene (5 mol% of the amount of carboxyl-COOH) as a transesterification catalyst into the mixture (component C), stirring with an instrument for 10min until the mixture is uniform, placing the uniformly mixed viscous mixture between two glass slides covered with a polytetrafluoroethylene film tape, applying 4MPa pressure at 180 ℃ with a hot press, and curing for 6 hours, wherein the thickness of the film can be controlled by placing a gasket between the two plates.
The epoxy glass body prepared in the embodiment 2 has the repairing performance of more than 86% and the mechanical strength of 2.6MPa at the high temperature of 180 ℃, and the repairing time is 25 min.
Example 3
4,4' -dihydroxy-a-methyl styrene diglycidyl ether (component A) and curing agent phthalic anhydride (component B) with a molar ratio of 1:1.5 are placed in a suitable container and mechanically stirred or ultrasonically treated for 20min to mix the two into a uniform mixture, then introducing a transesterification catalyst 1,5, 7-triazabicyclo [4.4.0] -5-decene (in an amount of 2.5 mol% relative to the molar content of carboxyl-COOH) (component C) into the mixture, stirring the mixture for 10min by using an instrument until the mixture is uniform, finally placing the uniformly mixed sticky mixture between two glass slides covered by polytetrafluoroethylene membrane plate adhesive tapes, applying 5Mpa pressure at high temperature of 180 ℃ by using a hot press, and curing for 6 hours, wherein the thickness of the film can be controlled by placing a gasket between the two plates.
The epoxy glass body prepared in the embodiment 3 has the repairing performance of more than 75% and the mechanical strength of 2.3Mpa at the high temperature of 180 ℃, and the repairing time is 28 min.
Example 4
Placing epoxy material bisphenol A epoxy resin DGEBA (component A) and curing agent sebacic acid (component B) with a molar ratio of 1.2:1 in a suitable container, mechanically stirring or ultrasonically stirring for 20min to mix the two into a uniform mixture, then introducing a transesterification catalyst 1,5, 7-triazabicyclo [4.4.0] -5-decene (5 mol% of the amount relative to the molar content of carboxyl-COOH) (component C) into the mixture, stirring for 10min by using an instrument until the mixture is uniform, finally placing the uniformly mixed viscous mixture between two glass slides covered by polytetrafluoroethylene membrane tape, applying 6MPa pressure at high temperature of 180 ℃ by using a hot press, and curing for 6 hours, wherein the thickness of the film can be controlled by placing a gasket between the two plates.
The epoxy glass body prepared in the embodiment 4 has the repairing performance of more than 84 percent and the mechanical strength of 2.9MPa at the high temperature of 180 ℃, and the repairing time is 20 min.
Example 5
4,4' -dihydroxy-a-methyl styrene diglycidyl ether (component A) and curing agent glutaric anhydride (component B) in a molar ratio of 1.5:1 are placed in a suitable container and mechanically stirred or ultrasonically treated for 20min to mix the two into a uniform mixture, then introducing a transesterification catalyst 1,5, 7-triazabicyclo [4.4.0] -5-decene (in an amount of 1 mol% relative to the molar content of carboxyl-COOH) (component C), stirring the mixture for 10min by using an instrument until the mixture is uniform, finally placing the uniformly mixed sticky mixture between two glass slides covered by polytetrafluoroethylene membrane plate adhesive tapes, applying 5Mpa pressure at high temperature of 180 ℃ by using a hot press, and curing for 6 hours, wherein the thickness of the film can be controlled by placing a gasket between the two plates.
The epoxy glass body prepared in the embodiment 5 has over 73 percent of repairing performance and 2.5MPa of mechanical strength at the high temperature of 180 ℃, and the repairing time is 28 min.
Example 6
By adopting the raw materials and the proportion in the embodiment 1, the carbon nano tube with good dispersion is introduced into the mixture finally mixed uniformly in the embodiment 1, the raw materials and the proportion are subjected to ultrasonic treatment for 1 hour, the solvent in the mixture is heated and removed, then the mixture is placed into a film, a hot press is used for applying the pressure of 6Mpa at the temperature of 180 ℃, and the film is cured for 6 hours, so that the film can be formed.
The epoxy glass body prepared by the method has a photo-thermal conversion agent CNT, so that the epoxy glass body does not need to be heated, can reach more than 93 percent of healing capacity under the condition of greatly shortening the repairing time by irradiating infrared light (0.84 watt/square centimeter), has the mechanical strength of 3.0Mpa, takes 5min for repairing by irradiating the IR light, and can repair cracks and defects by irradiating without heating under the condition of low external temperature in winter to achieve the healing function.
Comparative example
296g of Pripol 2040 (component B) trimer acid and 6.96g of 1,5, 7-triazabicyclo [4.4.0] -5-decene (component C) transesterification catalyst are added into a suitable container, heated and mixed uniformly, then added with epoxy material bisphenol a type epoxy resin DGEBA (component a), stirred rapidly to ensure complete mixing, and finally poured into a film, cured for 6 hours under 6Mpa pressure at high temperature of 180 ℃ by a hot press to obtain the product.
The epoxy glass body prepared by the method can obtain 86% of repairing performance only at the temperature of more than 200 ℃, has too high strength (6.2MPa) and exceeds the implementation temperature of a hot-mixing type, so that the material is not considered to be used as a material of a hot-mixing epoxy glass body base asphalt steel bridge deck pavement structure layer.
It can be seen from the comparison of examples 1-6 and the comparative example that the transesterification reaction is accelerated above the Tv temperature, so that the material has the ability of stress relaxation and self-healing, and has the ability of cycle reprocessing and self-healing, and can automatically heal the scratch and crack damage in a short time under the heating condition, and a substance with light response property (such as azobenzene, CNT, GO, aniline, AgNW, etc.) can be added into the system, so as to repair the scratch and crack damage by light driving, and under the condition of low external temperature in winter, the crack and defect can be repaired by light without heating, so that the healing function is achieved, and the repairing efficiency is greatly improved.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (9)
1. A preparation method of a high-temperature self-repairing hot-mix epoxy asphalt material is characterized in that the epoxy asphalt material consists of a component A, a component B and a component C; the component A is an epoxy resin compound, the component B is a curing agent, and the component C is a transesterification catalyst; the preparation method of the epoxy asphalt material comprises the following specific steps:
s1, placing the component A and the component B with the molar ratio of 1-1.5:1-1.5 in a container for mechanical stirring or ultrasonic sound, and mixing to obtain a uniform mixture Y1;
s2, introducing the component C into the mixture Y1 and manually stirring for 10min until the mixture is uniform to obtain a viscous mixture Y2;
s3, finally, placing the sticky mixture Y2 between two glass slides covered by polytetrafluoroethylene template tapes, and applying pressure to the glass slides by a hot press at high temperature for curing to obtain the self-repairing hot-mixed epoxy asphalt material.
2. The preparation method of the high-temperature self-repairing hot-mix epoxy asphalt material according to claim 1, characterized by comprising the following steps: the epoxy resin compound is bisphenol A epoxy resin, diglycidyl ether of 4,4 '-dihydroxybiphenyl or 4,4' -dihydroxy-a-methyl styrene diglycidyl ether.
3. The preparation method of the high-temperature self-repairing hot-mix epoxy asphalt material according to claim 1, characterized by comprising the following steps: the curing agent is oxalic acid, sebacic acid, glutaric acid, pripol 1040, citric acid trihydrate, suberic acid, phthalic anhydride, succinic anhydride, glutaric anhydride or methyl tetrahydrophthalic anhydride.
4. The preparation method of the high-temperature self-repairing hot-mix epoxy asphalt material according to claim 1, characterized by comprising the following steps: the ester exchange catalyst is zinc acetate, stannous octoate, 1,5, 7-triazabicyclo [4.4.0] dec-5-ene or zinc acetylacetonate.
5. The preparation method of the high-temperature self-repairing hot-mix epoxy asphalt material according to claim 1, characterized by comprising the following steps: the molar ratio of component A to component B in step S1 was 1:1.
6. The preparation method of the high-temperature self-repairing hot-mix epoxy asphalt material according to claim 1, characterized by comprising the following steps: the stirring or ultrasonic treatment time in the step S1 is 20 min.
7. The preparation method of the high-temperature self-repairing hot-mix epoxy asphalt material according to claim 1, characterized by comprising the following steps: the component C introduced in the step S2 accounts for 1-5% of the mole fraction of the mixture Y1.
8. The preparation method of the high-temperature self-repairing hot-mix epoxy asphalt material according to claim 7, characterized by comprising the following steps: the component C introduced in the step S2 accounts for 5 percent of the mole fraction of the mixture Y1.
9. The preparation method of the high-temperature self-repairing hot-mix epoxy asphalt material according to claim 1, characterized by comprising the following steps: the specific parameters of the hot press for applying pressure at high temperature in the step S3 are as follows: the temperature is 180 ℃, the pressure is 4-6Mpa, and the curing time is 6 h.
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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 |
| CN116376225A (en) * | 2023-03-30 | 2023-07-04 | 华中科技大学 | Light high-rigidity high-damping material with self-healing function and application thereof |
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| CN115304926A (en) * | 2022-07-25 | 2022-11-08 | 章丘市黄河水利水电工程有限公司 | Modified asphalt and asphalt concrete |
| 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 |
| CN116376225A (en) * | 2023-03-30 | 2023-07-04 | 华中科技大学 | Light high-rigidity high-damping material with self-healing function and application thereof |
| CN116376225B (en) * | 2023-03-30 | 2024-06-14 | 华中科技大学 | Light high-rigidity high-damping material with self-healing function and application thereof |
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