CN111635617A - Preparation method for improving conductivity of composite material epoxy resin matrix - Google Patents
Preparation method for improving conductivity of composite material epoxy resin matrix Download PDFInfo
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- CN111635617A CN111635617A CN202010572924.4A CN202010572924A CN111635617A CN 111635617 A CN111635617 A CN 111635617A CN 202010572924 A CN202010572924 A CN 202010572924A CN 111635617 A CN111635617 A CN 111635617A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 92
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 92
- 239000011159 matrix material Substances 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 71
- 239000004917 carbon fiber Substances 0.000 claims abstract description 71
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000000843 powder Substances 0.000 claims abstract description 67
- 239000002184 metal Substances 0.000 claims abstract description 47
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims abstract description 26
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000001291 vacuum drying Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000000465 moulding Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000004073 vulcanization Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010285 flame spraying Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/10—Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/56—Coatings, e.g. enameled or galvanised; Releasing, lubricating or separating agents
- B29C33/58—Applying the releasing agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/02—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/22—Component parts, details or accessories; Auxiliary operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/22—Component parts, details or accessories; Auxiliary operations
- B29C39/24—Feeding the material into the mould
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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
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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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
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- Reinforced Plastic Materials (AREA)
Abstract
The invention relates to a preparation method for improving the conductivity of a composite material epoxy resin matrix, which specifically comprises the following steps: s1, weighing the raw materials in proportion; s2, putting the carbon fiber powder into nitric acid, washing the carbon fiber powder with pure water to remove the nitric acid, and then putting the carbon fiber powder into a vacuum drying oven for drying; s3, placing epoxy resin and a methyl tetrahydrophthalic anhydride curing agent into a flask, stirring, adding DMP-30 into the flask after stirring, S4 treating the surface of a metal mold with alcohol, then placing the metal mold into a vacuum drying oven for drying, spraying a release agent on the surface of the metal mold, and placing the metal mold into the vacuum drying oven again for vulcanization; s5, adding the mixed liquid of the carbon fiber powder and the epoxy resin matrix into a ball mill for fully mixing, introducing the fully mixed liquid into a vulcanized metal mold for waiting for molding, and demolding after molding to obtain the modified epoxy resin matrix.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a preparation method for improving the conductivity of an epoxy resin matrix of a composite material.
Background
The carbon fiber composite material is widely used for manufacturing airplane parts, the use amount of the composite material in the fuselage, wings, empennage and the like of an airplane accounts for more than 50% of the self weight of the airplane, and the weight of the airplane can be reduced by more than 25% by using the composite material. Thunder is a violent gas discharge phenomenon, lightning current above 200kA can be generated at most in the discharge process, and the airplane can be struck by lightning every 3000 hours of flying according to statistics. The carbon fiber composite material has lower electrical conductivity than metal, and the material can be seriously damaged by lightning striking the composite material, so that the electrical conductivity of the carbon fiber composite material is very important to be improved. For lightning protection of composite materials, the main method is to improve the overall conductivity of the materials, and currently, researchers have proposed many methods for enhancing the conductivity of the materials. The surface of the composite material can be protected by flame spraying conductive paint or metal nets, and the protection method has the advantages of improving the conductivity of the surface of the material, but greatly increasing the mass of the airplane and causing cost increase. The carbon nano tube coated on the surface of the material can also effectively enhance the overall conductivity of the material, but the carbon nano tube is expensive and is not suitable for large-area coating on the surface of an airplane. The patent thus proposes a method for reinforcing the electrical conductivity of epoxy resins with carbon fiber powder, which has the advantage of avoiding expensive production costs and also allows a relatively small increase in the mass of the composite material.
Therefore, there is a need to develop a preparation method for improving the conductivity of the composite material epoxy resin matrix.
Disclosure of Invention
The invention aims to provide a preparation method for improving the conductivity of a composite material epoxy resin matrix.
In order to solve the technical problems, the technical scheme adopted by the invention is that the preparation method for improving the conductivity of the composite material epoxy resin matrix specifically comprises the following steps:
s1 preparation at the early stage: weighing carbon fiber powder, epoxy resin, a methyltetrahydrophthalic anhydride curing agent, a DMP-30 accelerator and nitric acid according to a proportion;
s2 treatment of carbon fiber powder: putting carbon fiber powder into nitric acid, and treating for 4-6 h in a water bath at 50-70 ℃; washing the carbon fiber powder with pure water to remove nitric acid, and drying in a vacuum drying oven for later use;
preparation of S3 epoxy resin matrix: putting epoxy resin and a methyltetrahydrophthalic anhydride curing agent into a flask, putting the flask into a magnetic stirrer, vacuumizing and stirring, carrying out water bath treatment at 50-70 ℃, adding a DMP-30 promoter into the flask after stirring for 5-15 min, and stirring again for 3-8 min to obtain an epoxy resin matrix;
s4 treatment of the metal mold: treating the surface of the metal mold with alcohol to ensure the surface to be clean and free from dirt; then putting the metal mold into a vacuum drying oven for drying treatment, taking out the metal mold, spraying a release agent on the surface of the metal mold, and then putting the metal mold into the vacuum drying oven again for vulcanization treatment;
s5 mixing treatment of carbon fiber powder and epoxy resin matrix: adding the carbon fiber powder dried in the step S2 into the epoxy resin matrix in the step S3, adding a mixed solution of the carbon fiber powder and the epoxy resin matrix into a ball mill for fully mixing, introducing the fully mixed solution into the vulcanized metal mold for waiting for molding, and demolding the metal mold after molding to obtain the modified epoxy resin matrix.
As a preferred technical scheme of the invention, the carbon fiber powder, the epoxy resin, the methyltetrahydrophthalic anhydride curing agent, the DMP-30 accelerator and the nitric acid are prepared from the following components in parts by weight: 15-20 parts of carbon fiber powder, 40-50 parts of epoxy resin, 30-40 parts of methyl tetrahydrophthalic anhydride curing agent, 0.5-2 parts of DMP-30 accelerator and 40-70 parts of nitric acid. Wherein the type of the carbon fiber powder is T700, and the type of the epoxy resin is Yueyangpetrochemical E-51.
As a preferred technical scheme of the invention, the carbon content in the carbon fiber powder is more than 95%, and the particle diameter is less than 8 μm; the concentration of the nitric acid is 60%.
As a preferable technical scheme of the invention, the drying treatment in the step S2 is performed at 100 ℃ for 5-7 h; the drying treatment in the step S4 is carried out at the temperature of 130 ℃ for 10-20 min; the temperature of the vulcanization treatment in the step S4 is 170 ℃, and the treatment time is 15 min.
As a preferable technical scheme of the invention, the volume ratio of the carbon fiber powder and the nitric acid in the step S2 is 1: 5; the mass ratio of the epoxy resin to the methyltetrahydrophthalic anhydride curing agent in the step S3 is 100: 85 parts by weight; the mass fraction of the DMP-30 accelerator added in the step S3 accounts for 2% of the mass fraction of the epoxy resin.
As a preferred embodiment of the present invention, the mixing time in the step S5 using a ball mill is 10 min; the time for waiting for forming is 5 h.
In a preferred embodiment of the present invention, the water bath treatment temperature in each of the steps S2 and S3 is 60 ℃.
By adopting the technical scheme of the invention, the beneficial effects are as follows: the preparation method for improving the conductivity of the epoxy resin matrix of the composite material improves the conductivity of the epoxy resin matrix by adding the carbon fiber, and simultaneously keeps the high performance of the epoxy resin matrix composite material, thereby being more beneficial to wide application.
Drawings
In order that the present invention may be more readily and clearly understood, reference is now made to the following detailed description of the invention taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a process flow diagram of a method of the present invention for improving the conductivity of a composite epoxy resin matrix;
FIG. 2 is a flowchart of step S3 of the method for improving the conductivity of the composite epoxy resin matrix of example 1;
FIG. 3 is a flowchart of step S4 of the method for improving the conductivity of the composite epoxy resin matrix of example 1;
fig. 4 is a flowchart of step S5 of the preparation method for improving the conductivity of the composite epoxy resin matrix in example 1 of the present invention.
Detailed Description
Example 1: the preparation method for improving the conductivity of the composite material epoxy resin matrix specifically comprises the following steps:
s1 preparation at the early stage: weighing carbon fiber powder, epoxy resin, a methyltetrahydrophthalic anhydride curing agent, a DMP-30 accelerator and nitric acid according to a proportion; the carbon fiber powder, the epoxy resin, the methyl tetrahydrophthalic anhydride curing agent, the DMP-30 accelerant and the nitric acid are as follows in parts by weight: 17.6 parts of carbon fiber powder, 44.1 parts of epoxy resin, 37.4 parts of methyl tetrahydrophthalic anhydride curing agent, 0.9 part of DMP-30 accelerator and 50 parts of nitric acid; wherein the carbon content in the carbon fiber powder is more than 95 percent, and the particle diameter is less than 8 mu m; the concentration of the nitric acid is 60 percent; wherein the type of the carbon fiber powder is T700, the density is 1.76, and the type of the epoxy resin is Yueyangpetrochemical E-51;
s2 treatment of carbon fiber powder: putting carbon fiber powder into nitric acid, wherein the volume ratio of the carbon fiber powder to the nitric acid in the step S2 is 1: 5; treating in water bath at 60 deg.C for 5 hr; washing the carbon fiber powder with pure water to remove nitric acid, and then putting the carbon fiber powder into a vacuum drying oven for drying treatment at the temperature of 100 ℃ for 5 hours for later use;
preparation of S3 epoxy resin matrix: putting epoxy resin and a methyltetrahydrophthalic anhydride curing agent into a flask, wherein the mass ratio of the epoxy resin to the methyltetrahydrophthalic anhydride curing agent is 100: 85 parts by weight; putting a flask into a magnetic stirrer, vacuumizing and stirring, performing water bath treatment at 60 ℃, and adding a DMP-30 accelerator into the flask after stirring for 10min, wherein the mass fraction of the DMP-30 accelerator accounts for 2% of that of the epoxy resin; stirring for 5min again to obtain an epoxy resin matrix;
s4 treatment of the metal mold: treating the surface of the metal mold with alcohol to ensure the surface to be clean and free from dirt; then, putting the metal mold into a vacuum drying oven for drying treatment, wherein the temperature of the drying treatment is 130 ℃, and the drying time is 15 min; drying, taking out the metal mold, spraying a release agent on the surface of the metal mold, and then putting the metal mold into a vacuum drying oven again for vulcanization treatment at the temperature of 170 ℃ for 15 min;
s5 mixing treatment of carbon fiber powder and epoxy resin matrix: adding the carbon fiber powder dried in the step S2 into the epoxy resin matrix in the step S3, and adding the mixed liquid of the carbon fiber powder and the epoxy resin matrix into a ball mill for fully mixing for 10 min; then introducing the fully mixed solution into the vulcanized metal mold for molding, wherein the molding waiting time is 5 hours; and (3) demolding the metal mold after molding to obtain a modified epoxy resin matrix, wherein the demolding agent is Jiadan JD-909A produced by Jiadan lubricating oil Co.
Example 2: the preparation method for improving the conductivity of the composite material epoxy resin matrix specifically comprises the following steps:
s1 preparation at the early stage: weighing carbon fiber powder, epoxy resin, a methyltetrahydrophthalic anhydride curing agent, a DMP-30 accelerator and nitric acid according to a proportion; the carbon fiber powder, the epoxy resin, the methyl tetrahydrophthalic anhydride curing agent, the DMP-30 accelerant and the nitric acid are as follows in parts by weight: 15 parts of carbon fiber powder, 40 parts of epoxy resin, 30 parts of methyl tetrahydrophthalic anhydride curing agent, 0.5 part of DMP-30 accelerator and 42.6 parts of nitric acid; wherein the carbon content in the carbon fiber powder is more than 95 percent, and the particle diameter is less than 8 mu m; the concentration of the nitric acid is 60 percent; wherein the type of the carbon fiber powder is T700, the density is 1.76, and the type of the epoxy resin is Yueyangpetrochemical E-51;
s2 treatment of carbon fiber powder: putting carbon fiber powder into nitric acid, wherein the volume ratio of the carbon fiber powder to the nitric acid in the step S2 is 1: 5; treating in water bath at 50 deg.C for 6 h; washing the carbon fiber powder with pure water to remove nitric acid, and then putting the carbon fiber powder into a vacuum drying oven for drying treatment at the temperature of 100 ℃ for 5 hours for later use;
preparation of S3 epoxy resin matrix: putting epoxy resin and a methyltetrahydrophthalic anhydride curing agent into a flask, wherein the mass ratio of the epoxy resin to the methyltetrahydrophthalic anhydride curing agent is 100: 85 parts by weight; putting a flask into a magnetic stirrer, vacuumizing and stirring, performing water bath treatment at 50 ℃, and adding a DMP-30 accelerator into the flask after stirring for 15min, wherein the mass fraction of the DMP-30 accelerator accounts for 2% of that of the epoxy resin; stirring for 8min again to obtain an epoxy resin matrix;
s4 treatment of the metal mold: treating the surface of the metal mold with alcohol to ensure the surface to be clean and free from dirt; then, putting the metal mold into a vacuum drying oven for drying treatment, wherein the temperature of the drying treatment is 130 ℃, and the drying time is 10 min; drying, taking out the metal mold, spraying a release agent on the surface of the metal mold, and then putting the metal mold into a vacuum drying oven again for vulcanization treatment at the temperature of 170 ℃ for 15 min;
s5 mixing treatment of carbon fiber powder and epoxy resin matrix: adding the carbon fiber powder dried in the step S2 into the epoxy resin matrix in the step S3, and adding the mixed liquid of the carbon fiber powder and the epoxy resin matrix into a ball mill for fully mixing for 10 min; then introducing the fully mixed solution into the vulcanized metal mold for molding, wherein the molding waiting time is 5 hours; and (3) demolding the metal mold after molding to obtain a modified epoxy resin matrix, wherein the demolding agent is Jiadan JD-909A produced by Jiadan lubricating oil Co.
Example 3: the preparation method for improving the conductivity of the composite material epoxy resin matrix specifically comprises the following steps:
s1 preparation at the early stage: weighing carbon fiber powder, epoxy resin, a methyltetrahydrophthalic anhydride curing agent, a DMP-30 accelerator and nitric acid according to a proportion; the carbon fiber powder, the epoxy resin, the methyl tetrahydrophthalic anhydride curing agent, the DMP-30 accelerant and the nitric acid are as follows in parts by weight: 20 parts of carbon fiber powder, 50 parts of epoxy resin, 40 parts of methyl tetrahydrophthalic anhydride curing agent, 1.5 parts of DMP-30 accelerator and 56.8 parts of nitric acid; wherein the carbon content in the carbon fiber powder is more than 95 percent, and the particle diameter is less than 8 mu m; the concentration of the nitric acid is 60 percent; wherein the type of the carbon fiber powder is T700, the density is 1.76, and the type of the epoxy resin is Yueyangpetrochemical E-51;
s2 treatment of carbon fiber powder: putting carbon fiber powder into nitric acid, wherein the volume ratio of the carbon fiber powder to the nitric acid in the step S2 is 1: 5; treating in water bath at 70 deg.C for 4 hr; washing the carbon fiber powder with pure water to remove nitric acid, and then putting the carbon fiber powder into a vacuum drying oven for drying treatment at the temperature of 100 ℃ for 7 hours for later use;
preparation of S3 epoxy resin matrix: putting epoxy resin and a methyltetrahydrophthalic anhydride curing agent into a flask, wherein the mass ratio of the epoxy resin to the methyltetrahydrophthalic anhydride curing agent is 100: 85 parts by weight; putting a flask into a magnetic stirrer, vacuumizing and stirring, performing 70 ℃ water bath treatment, stirring for 5min, and then adding a DMP-30 accelerator into the flask, wherein the mass fraction of the DMP-30 accelerator accounts for 2% of that of the epoxy resin; stirring for 8min again to obtain an epoxy resin matrix;
s4 treatment of the metal mold: treating the surface of the metal mold with alcohol to ensure the surface to be clean and free from dirt; then, putting the metal mold into a vacuum drying oven for drying treatment, wherein the temperature of the drying treatment is 130 ℃, and the drying time is 20 min; drying, taking out the metal mold, spraying a release agent on the surface of the metal mold, and then putting the metal mold into a vacuum drying oven again for vulcanization treatment at the temperature of 170 ℃ for 15 min;
s5 mixing treatment of carbon fiber powder and epoxy resin matrix: adding the carbon fiber powder dried in the step S2 into the epoxy resin matrix in the step S3, and adding the mixed liquid of the carbon fiber powder and the epoxy resin matrix into a ball mill for fully mixing for 10 min; then introducing the fully mixed solution into the vulcanized metal mold for molding, wherein the molding waiting time is 5 hours; and (3) demolding the metal mold after molding to obtain a modified epoxy resin matrix, wherein the demolding agent is Jiadan JD-909A produced by Jiadan lubricating oil Co.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (7)
1. A preparation method for improving the conductivity of a composite material epoxy resin matrix is characterized by comprising the following steps:
s1 preparation at the early stage: weighing carbon fiber powder, epoxy resin, a methyltetrahydrophthalic anhydride curing agent, a DMP-30 accelerator and nitric acid according to a proportion;
s2 treatment of carbon fiber powder: putting carbon fiber powder into nitric acid, and treating for 4-6 h in a water bath at 50-70 ℃; washing the carbon fiber powder with pure water to remove nitric acid, and drying in a vacuum drying oven for later use;
preparation of S3 epoxy resin matrix: putting epoxy resin and a methyltetrahydrophthalic anhydride curing agent into a flask, putting the flask into a magnetic stirrer, vacuumizing and stirring, carrying out water bath treatment at 50-70 ℃, adding a DMP-30 promoter into the flask after stirring for 5-15 min, and stirring again for 3-8 min to obtain an epoxy resin matrix;
s4 treatment of the metal mold: treating the surface of the metal mold with alcohol to ensure the surface to be clean and free from dirt; then putting the metal mold into a vacuum drying oven for drying treatment, taking out the metal mold, spraying a release agent on the surface of the metal mold, and then putting the metal mold into the vacuum drying oven again for vulcanization treatment;
s5 mixing treatment of carbon fiber powder and epoxy resin matrix: adding the carbon fiber powder dried in the step S2 into the epoxy resin matrix in the step S3, adding a mixed solution of the carbon fiber powder and the epoxy resin matrix into a ball mill for fully mixing, introducing the fully mixed solution into the vulcanized metal mold for waiting for molding, and demolding the metal mold after molding to obtain the modified epoxy resin matrix.
2. The preparation method for improving the conductivity of the composite material epoxy resin matrix according to claim 1, wherein the carbon fiber powder, the epoxy resin, the methyltetrahydrophthalic anhydride curing agent, the DMP-30 accelerator and the nitric acid are prepared from the following components in parts by weight: 15-20 parts of carbon fiber powder, 40-50 parts of epoxy resin, 30-40 parts of methyl tetrahydrophthalic anhydride curing agent, 0.5-2 parts of DMP-30 accelerator and 40-70 parts of nitric acid.
3. The preparation method for improving the conductivity of the composite material epoxy resin matrix according to claim 2, wherein the carbon content in the carbon fiber powder is more than 95%, and the particle diameter is less than 8 μm; the concentration of the nitric acid is 60%.
4. The preparation method for improving the conductivity of the composite material epoxy resin matrix according to claim 2, wherein the drying treatment in the step S2 is carried out at 100 ℃ for 5-7 h; the drying treatment in the step S4 is carried out at the temperature of 130 ℃ for 10-20 min; the temperature of the vulcanization treatment in the step S4 is 170 ℃, and the treatment time is 15 min.
5. The preparation method for improving the conductivity of the composite material epoxy resin matrix according to claim 3, wherein the volume ratio of the carbon fiber powder to the nitric acid in the step S2 is 1: 5; the mass ratio of the epoxy resin to the methyltetrahydrophthalic anhydride curing agent in the step S3 is 100: 85 parts by weight; the mass fraction of the DMP-30 accelerator added in the step S3 accounts for 2% of the mass fraction of the epoxy resin.
6. The preparation method for improving the conductivity of the composite material epoxy resin matrix according to claim 4, wherein the mixing time in the step S5 by using a ball mill is 10 min; the time for waiting for forming is 5 h.
7. The preparation method for improving the conductivity of the composite material epoxy resin matrix according to claim 4, wherein the water bath treatment temperature in the steps S2 and S3 is 60 ℃.
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| CN113214726A (en) * | 2021-05-06 | 2021-08-06 | 合肥工业大学 | Lightning protection coating for radome and preparation method thereof |
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