CN113387713A - Method for preparing flexible graphite grounding conductor material by in-situ polymerization method - Google Patents
Method for preparing flexible graphite grounding conductor material by in-situ polymerization method Download PDFInfo
- Publication number
- CN113387713A CN113387713A CN202110504988.5A CN202110504988A CN113387713A CN 113387713 A CN113387713 A CN 113387713A CN 202110504988 A CN202110504988 A CN 202110504988A CN 113387713 A CN113387713 A CN 113387713A
- Authority
- CN
- China
- Prior art keywords
- carbon
- resin
- graphite
- flexible graphite
- grounding conductor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R4/00—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation
- H01R4/58—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation characterised by the form or material of the contacting members
- H01R4/66—Connections with the terrestrial mass, e.g. earth plate, earth pin
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- 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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- 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
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
-
- 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
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- 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
-
- 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 a preparation method of a flexible graphite grounding conductor material, which comprises the following steps: mixing resin, a carbon forming agent and a conductive material in a preset ratio, and stirring to form carbon forming resin; impregnating a carbon skeleton material with the carbon forming resin; laying and stacking the impregnated carbon skeleton material according to a preset laying mode, and curing the carbon skeleton material into a carbon skeleton composite material under a heating condition; carbonizing the cured carbon skeleton composite material at high temperature, and hot-pressing into an enhanced graphite belt; and preparing the reinforced graphite belt into the flexible graphite grounding material by further cutting, weaving, twisting or rolling. According to the invention, the carbon forming resin is impregnated with the carbon framework material and then is cured and carbonized, so that the graphite carbon layer is directly generated on the surface of the carbon framework material, the interface bonding force of graphite and the carbon framework material is improved, and the carbon forming rate and the compactness of the resin are improved by introducing the PSF carbon forming agent.
Description
Technical Field
The invention relates to the technical field of grounding materials of power systems, in particular to a method for preparing a flexible graphite grounding conductor material by an in-situ polymerization method.
Background
The corrosion problem of the grounding engineering seriously threatens the grounding safety of the line and causes huge economic loss, and the most effective method for solving the corrosion problem of the grounding material in the ground is to adopt a polymer composite conductive material to replace a metal material. At present, most of composite grounding material products adopt a thermoplastic roll forming process to prepare expanded graphite and synthetic fibers into graphite wires, and then are woven and formed through various wire layer structures. In order to ensure the structural compactness and the mechanical property of the grounding material, the fiber material and the expanded graphite need to be bonded by using a conductive adhesive in the preparation process of the product. Once a large fault current is passed through the material, the resulting temperature rise can cause some degradation and failure of the adhesive, which can seriously affect the stability of the grounding material.
Disclosure of Invention
In view of this, the invention provides a preparation method of a flexible graphite grounding conductor material, and aims to solve the problem that the existing grounding material is poor in structural stability.
The invention provides a preparation method of a flexible graphite grounding conductor material, which comprises the following steps:
and 5, preparing the reinforced graphite belt into the flexible graphite grounding material by further cutting, weaving, twisting or rolling.
Further, in the preparation method of the flexible graphite grounding conductor material, in the step 1, the dosage ratio of each raw material is as follows: 30-40 parts of resin, 5-10 parts of carbon forming agent and 50-60 parts of conductive material.
Further, in the above method for preparing a flexible graphite ground conductor material, the resin in step 1 includes at least one of cyanate ester resin, epoxy resin, and phenolic resin.
Further, in the above method for preparing a flexible graphite ground conductor material, the char-forming agent in step 1 is a schiff base compound having a phosphorus-containing group, a furan group, and a phenolic hydroxyl group, wherein: the phosphorus-containing group comprises a DOPO phosphaphenanthrene group, a diethyl phosphate group or a diphenyl phosphate group; the phenolic hydroxyl group includes a ortho-phenolic hydroxyl group or a para-phenolic hydroxyl group.
Further, in the above method for preparing a flexible graphite grounding conductor material, the conductive material is at least one selected from the group consisting of vermicular graphite, flexible graphite, carbon fiber, graphene and metal powder.
Further, in the above method for preparing a flexible graphite grounding conductor material, the carbon skeleton material in step 2 is selected from at least one of carbon fiber yarn, carbon fiber cloth, carbon fiber sleeve, flexible graphite, and blended fabric of carbon fiber and glass fiber.
Further, in the above method for preparing the flexible graphite ground conductor material, the fibrous carbon skeleton material in step 2 is washed with acetone in advance and blown with hot air to remove the sizing agent on the surface, so as to disperse the fiber yarn bundle.
Further, in the preparation method of the flexible graphite grounding conductor material, the layering mode in the step 3 includes stacking, rolling, twisting, bundling or winding, and the curing temperature is 120-.
Further, in the preparation method of the flexible graphite grounding conductor material, the carbonization temperature in the step 4 is 800-.
Further, in the above preparation method of the flexible graphite grounding conductor material, in the step 5, the graphite sheet is cut into narrow strips with a width of 1-5mm, and then the flexible graphite grounding conductor material is prepared by subsequent weaving processing.
According to the preparation method of the flexible graphite grounding conductor material, the resin, the carbon forming agent and the conductive material are compounded to prepare the prepreg tape, the prepreg tape is impregnated with the carbon skeleton material and then is cured at a certain temperature to form an enhanced graphite precursor, the enhanced graphite precursor is carbonized at a high temperature and then is pressed into a graphite tape, and then the graphite tape is woven to form the grounding material; the process is simple, no adhesive is required to be added, and the prepared flexible graphite grounding conductor material has strong structural stability and excellent conductivity.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a flexible graphite grounding conductor material according to the present invention;
FIG. 2 is an infrared spectrum of a char-forming agent PSF employed in the present invention;
FIG. 3 is a nuclear magnetic resonance hydrogen spectrum of a char-forming agent PSF employed in the present invention;
FIG. 4 is a NMR phosphorus spectrum of a char-forming agent PSF and DOPO used in the present invention;
FIG. 5 is an SEM image of vermicular graphite employed in the present invention;
FIG. 6 is an SEM image of a cross section parallel to the fiber direction of a flexible graphite grounding conductor material prepared by the present invention;
fig. 7 is an SEM image of a cross-section perpendicular to the direction of the fibers of the flexible graphite ground conductor material prepared in accordance with the present invention.
Detailed Description
While the preferred embodiments of the present invention are described below, it should be understood that various changes and modifications can be made by one skilled in the art without departing from the principles of the invention, and such changes and modifications are also considered to be within the scope of the invention.
The preparation method of the flexible graphite grounding conductor material provided by the embodiment of the invention comprises the following steps:
specifically, the dosage ratio of each raw material is as follows: 130 parts of resin 110-. The dosage ratio of the raw materials is preferably as follows: 130 parts of resin, 25 parts of carbon forming agent and 150 parts of conductive material.
The resin comprises at least one of cyanate ester resin, epoxy resin and phenolic resin, the cyanate ester resin and the phenolic resin have high carbon forming rate, the epoxy resin can react with the cyanate ester resin and the phenolic resin, the fluidity is good, and the manufacturability of the resin is improved.
The char-forming agent is a Schiff base compound with phosphorus-containing groups, furan groups and phenolic hydroxyl groups, and has the following general formula:
In this embodiment, the char-forming agent is preferably PSF, which has the following chemical formula:
the charring agent has a DOPO phosphine phenanthrene group and can promote organic matters to form carbon at high temperature; the carbon has furan groups, and can be graphitized at high temperature to improve the carbon formation rate; the phenolic hydroxyl groups are contained, so that the phenolic hydroxyl groups can participate in the curing reaction of the resin, the surface migration at high temperature is avoided, and the carbon forming uniformity of the resin is improved.
The preparation process of the char forming agent (PSF) in the embodiment of the present invention is as follows: 40ml of ethanol, furfuryl amine (9.7g, 0.1mol), salicylaldehyde (12.2g, 0.1mol) and DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide 21.6g, 0.1mol) were added to a three-necked flask, and stirred at normal temperature for 24 hours to obtain a light yellow crude product. The crude product was filtered and washed twice with methanol, which was dried under reduced pressure in a vacuum oven at 60 ℃ to give a white product with a yield of 86%. The reaction equation is as follows:
with reference to fig. 2-4, the invention adopts infrared spectroscopy analysis and nuclear magnetic resonance hydrogen and phosphorus element spectrograms to analyze the chemical structure characteristics of the PSF; wherein the infrared spectrogram of PSF is as shown in FIG. 2, and is 1485cm-1And 1596cm-1The stretching vibration peak of P-Ph appears at 925cm-1The stretching vibration peak of P-O-Ph appears at 1197cm-1And a P ═ O stretching vibration peak appears, and the characteristic vibration peak indicates that a DOPO structure exists in the PSF. And 3430cm-1Is located at 1276cm and is a characteristic peak of N-H-1Is characterized by an N-C characteristic peak at 2943cm-1Is characterized by C-H characteristic peak, threeThe characteristic peak shows that the nucleophilic addition of DOPO and the N ═ C bond of the Schiff base occurs to form the structure of-NH-CH-P. The infrared absorption peak is 1409cm because furfuryl amine with furan ring is used in synthesizing Schiff base-1And 1083cm-1The C-C characteristic peak and the C-O-C characteristic peak appear at 3157cm-1The peak is a phenolic hydroxyl group.
From FIG. 3, it can be seen that the chemical shift of the phenolic hydroxyl group in PSF is 9.86ppm, and the chemical shifts of the three hydrogen atoms on the furan ring are respectively H1 at 7.58, H2 at 7.05 and H3 at 6.99. Chemical shifts at 4.12-4.15ppm are-CH attached to the furan ring2-group and chemical shifts of the benzene ring hydrogen at 6.7-8.3ppm, including 12 total hydrogen atoms of the benzene ring in DOPO and the benzene ring in salicylaldehyde. Because of nucleophilic addition of DOPO with-N ═ C-bond in schiff base, two new H chemical shifts of-NH-CH-were formed, respectively-NH-5.95 ppm and-CH-5.45 ppm. By integrating the chemical shifts and calculating the ratios, the ratios of the individual hydrogen atoms in the PSF were found to be consistent with the ratios in the designed molecule. As shown in FIG. 3, the chemical shift of the phosphorus atom of PSF is 28.1ppm, which is a single peak, indicating that only phosphorus atoms of one chemical structure are present, and the chemical shift of the phosphorus atom of DOPO is 13.0-17.5ppm, indicating that the phosphorus element is newly generated by the chemical reaction.
With reference to fig. 3 and 4, i.e., by nmr hydrogen and phosphorus spectra, it is further demonstrated that the PSF and chemical structure are consistent with the designed chemical structure, while the elemental content analysis shows C, H, N element content as: c:69.11(69.06), H:4.78(4.80), N:3.31(3.36) (calculated in parentheses). The test value is close to the calculated value, and the synthesized product is the PSF.
The conductive material is selected from at least one of vermicular graphite, flexible graphite, carbon fiber, graphene and metal powder, preferably vermicular graphite, the microstructure characteristics of the vermicular graphite are shown in figure 5, the vermicular graphite is of a multilayer spring structure and can be mutually embedded in the compression process, the compactness of a carbon layer is improved, and the price is low.
The reaction mechanism of the carbon formation in the invention is as follows:
PSF is decomposed to form a phosphaphenanthrene group, a nitrogen-containing free radical inhibitor and a furan group, the phosphaphenanthrene group and the nitrogen-containing free radical inhibitor promote resin to form carbon, and the furan group is gradually crosslinked, dehydrated and carbonized under the action of the phosphaphenanthrene group and the nitrogen-containing free radical inhibitor to finally form a graphitized structure, wherein the reaction formula is as follows:
and 2, impregnating a carbon framework material with the carbon forming resin to form a prepreg tape.
Specifically, the carbon skeleton material is selected from at least one of carbon fiber yarn, carbon fiber cloth, carbon fiber sleeve, flexible graphite and blended fabric of carbon fiber and glass fiber. During impregnation, one or more layers of carbon skeleton material may be impregnated with a carbon-forming resin to form a prepreg tape.
In practice, when selecting the fiber-based carbon skeleton material, the fiber-based carbon skeleton material is washed by acetone in advance and blown by hot air to remove the sizing agent on the surface and disperse fiber yarn bundles, so that the fiber bundles are dispersed into fiber monofilaments, the contact area of the fibers, graphite powder and resin is increased, and the dispersibility is improved.
The impregnation process is specifically that the fiber passes through an impregnation glue tank in which the carbon forming resin is placed, and then the redundant carbon forming resin is extruded by a double roller, wherein the carbon forming resin plays the role of glue solution.
And 3, laying and stacking the prepreg tapes according to a preset laying mode, and curing the prepreg tapes into the carbon skeleton composite material under a heating condition, wherein the carbon skeleton composite material can be used as a precursor.
Specifically, the layering mode comprises stacking, rolling, twisting, bundling or winding, and the curing temperature is 120-300 ℃. In the embodiment, a stepwise temperature rise mode is selected for curing, for example, the temperature is maintained at 120 ℃ for 1 hour, the temperature is maintained at 150 ℃ for 1 hour, the temperature is maintained at 180 ℃ for 1 hour, the temperature is maintained at 220 ℃ for 1 hour, and the temperature is maintained at 300 ℃ for 1 hour, so that the stepwise temperature rise can ensure that the resin is fully cured, and meanwhile, internal defects such as crack pores and the like cannot be formed in the resin, so that the compactness of the subsequent carbonization process is influenced.
And 4, carbonizing the cured carbon skeleton composite material at high temperature, and hot-pressing the carbonized carbon skeleton composite material into the reinforced graphite belt.
Specifically, the carbonization temperature in the step 4 is 800-.
And 5, preparing the reinforced graphite belt into the flexible graphite grounding material by further cutting, weaving, twisting or rolling.
Specifically, the graphite sheet is cut into narrow strips with the width of 1-5mm, and then the flexible graphite grounding conductor material is prepared by subsequent weaving processing. The fabric forms formed by the weaving process include, but are not limited to, twisting into a thread, rolling into a tube, weaving into a cloth or sleeve, and combinations thereof.
Fig. 6 and 7 show the structure of the flexible graphite grounding conductor material prepared by the present invention, and the figure shows that the upper and lower surfaces of the expanded graphite/carbon fiber composite material are covered with expanded graphite, and the whole body presents a sandwich structure, i.e. expanded graphite-carbon fiber-expanded graphite. Observation of the carbon fiber layer revealed that there was a small amount of expanded graphite bonded to the fibers from fiber to fiber. The grounding material prepared by in-situ polymerization has the following advantages: 1) the combination of the carbon fiber and the graphite is tight, the graphite is not easy to fall off, and the contact resistance of the carbon fiber and the graphite is reduced. 2) The polymer resin is converted into a graphite carbon structure with more stable chemical properties, and performance attenuation caused by chemical aging of the polymer under high temperature and high pressure is avoided.
According to the invention, the carbon forming resin is impregnated into the carbon framework material and then is cured and carbonized, so that the graphite carbon layer is directly generated on the surface of the carbon framework material, the interface bonding force between graphite and the carbon framework material is improved, and the carbon forming agent is introduced, so that the carbon forming rate and the compactness of the resin are improved.
The invention is described in detail below in terms of several specific examples.
Example 1
Stirring 100g of cyanate ester resin, 30g of epoxy resin, 25g of carbon forming agent PSF and 150g of vermicular graphite to form carbon forming resin;
impregnating a layer of carbon fiber unidirectional cloth with the carbon forming resin to prepare a carbon fiber prepreg;
the carbon fiber prepreg is laid in one direction, heated to 180 ℃, kept warm for 3 hours, heated to 220 ℃, kept warm for 1 hour and cured to prepare a carbon fiber reinforced resin plate;
carbonizing the fiber reinforced resin plate at the high temperature of 1000 ℃, and hot-pressing the fiber reinforced resin plate into a fiber reinforced graphite belt under the conditions of 15kN and 600 ℃;
the fiber reinforced graphite tape is further cut into strips with the width of 3mm to be rolled to prepare the flexible graphite grounding material, the tensile strength of the graphite grounding material is more than 80MPa, and the carbon yield is more than 40%.
Example 2
Stirring 100g of phenolic resin, 10g of epoxy resin, 5g of charring agent PSF and 120g of vermicular graphite to form high-carbon-forming resin;
impregnating a plurality of layers of carbon fiber unidirectional cloth with high carbon forming resin to prepare a carbon fiber prepreg;
rolling the carbon fiber prepreg into a tubular shape, heating to 120 ℃, preserving heat for 3h, heating to 150 ℃, preserving heat for 1h, and curing to prepare a carbon fiber reinforced resin plate;
carbonizing the fiber reinforced resin plate at the high temperature of 800 ℃, and hot-pressing the fiber reinforced resin plate into a fiber reinforced graphite belt under the conditions of 15kN and 800 ℃;
the fiber reinforced graphite tape is further cut into strips with the width of 5mm, and the flexible graphite grounding material is prepared in a braided sleeve mode, wherein the tensile strength of the graphite grounding material is more than 85MPa, and the carbon forming rate is more than 60%.
Example 3
Stirring 50g of cyanate ester, 50g of phenolic resin, 20g of epoxy resin, 15g of carbon forming agent PSF and 140g of vermicular graphite to form high carbon forming resin;
impregnating carbon fiber roving with high carbon forming resin to prepare a carbon fiber prepreg tape;
weaving the carbon fiber prepreg tape into a sleeve, heating to 120 ℃, preserving heat for 3h, heating to 250 ℃, preserving heat for 1h, and curing to prepare a carbon fiber reinforced resin sleeve;
the fiber reinforced resin plate is carbonized at high temperature of 800 ℃, and is hot-pressed into the flexible graphite grounding material under the conditions of 10kN and 800 ℃, the tensile strength of the graphite grounding material is more than 75MPa, and the carbon forming rate is more than 50%.
In conclusion, the carbon forming agent is introduced, so that the carbon forming rate of the resin is improved to 40-60%, and the yield of graphite carbon formed by resin carbonization is high; meanwhile, the bonding force of graphite and carbon fibers is improved by carbonizing resin on the surfaces of the carbon fibers, and in addition, all polymer structures are converted into carbon structure materials due to chemical change in the carbonization process, so that the product almost does not contain polymer components, and adverse consequences of structural stability and performance reduction of the graphite grounding material caused by aging of the polymer in the later period are avoided.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a flexible graphite grounding conductor material is characterized by comprising the following steps:
step 1, mixing resin, a char-forming agent and a conductive material in a preset ratio, and stirring to form a char-forming resin;
step 2, impregnating a carbon framework material with the carbon forming resin to form a prepreg tape;
step 3, laying and stacking the prepreg tapes according to a preset laying mode, and curing the prepreg tapes into the carbon skeleton composite material under the heating condition;
step 4, carbonizing the cured carbon skeleton composite material at high temperature, and hot-pressing the carbonized carbon skeleton composite material into an enhanced graphite belt;
and 5, preparing the reinforced graphite belt into the flexible graphite grounding material by further cutting, weaving, twisting or rolling.
2. The method for preparing the flexible graphite grounding conductor material according to claim 1, wherein in the step 1, the dosage ratio of each raw material is as follows: 130 parts of resin 110-.
3. The method for preparing a flexible graphite grounding conductor material according to claim 1, wherein the resin in step 1 comprises at least one of cyanate ester resin, epoxy resin and phenolic resin.
4. The method for preparing a flexible graphite grounding conductor material according to claim 1, wherein the char-forming agent in step 1 is a schiff base compound having phosphorus-containing groups, furan groups, and phenolic hydroxyl groups, wherein: the phosphorus-containing group comprises a DOPO phosphaphenanthrene group, a diethyl phosphate group or a diphenyl phosphate group; the phenolic hydroxyl group includes a ortho-phenolic hydroxyl group or a para-phenolic hydroxyl group.
5. The method of claim 1, wherein the conductive material is selected from at least one of vermicular graphite, flexible graphite, carbon fiber, graphene, and metal powder.
6. The method for preparing the flexible graphite grounding conductor material according to claim 1, wherein the carbon skeleton material in the step 2 is selected from at least one of carbon fiber yarn, carbon fiber cloth, carbon fiber sleeve, flexible graphite and blended fabric of carbon fiber and glass fiber.
7. The method as claimed in claim 1, wherein the fibrous carbon skeleton material in step 2 is washed with acetone and blown with hot air to remove the surface sizing agent, so as to disperse the fiber yarn bundle.
8. The method as claimed in claim 1, wherein the step 3 of laying comprises stacking, rolling, twisting, bundling or winding, and the curing temperature is 120-300 ℃.
9. The method as claimed in claim 1, wherein the carbonization temperature in step 4 is 800-.
10. The method for preparing a flexible graphite grounding conductor material according to claim 1, wherein in the step 5, the graphite sheet is cut into narrow strips with the width of 1-5mm, and then the flexible graphite grounding conductor material is prepared by subsequent weaving processing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110504988.5A CN113387713B (en) | 2021-05-10 | 2021-05-10 | Method for preparing flexible graphite grounding conductor material by in-situ polymerization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110504988.5A CN113387713B (en) | 2021-05-10 | 2021-05-10 | Method for preparing flexible graphite grounding conductor material by in-situ polymerization method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113387713A true CN113387713A (en) | 2021-09-14 |
| CN113387713B CN113387713B (en) | 2023-01-31 |
Family
ID=77616856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110504988.5A Active CN113387713B (en) | 2021-05-10 | 2021-05-10 | Method for preparing flexible graphite grounding conductor material by in-situ polymerization method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113387713B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115594507A (en) * | 2022-10-12 | 2023-01-13 | 郑州格瑞特高温材料有限公司（Cn） | Low-density microporous silicon nitride combined silicon carbide material and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5437821A (en) * | 1992-09-30 | 1995-08-01 | The United States Of America As Represented By The Secretary Of The Navy | Process for making carbon-carbon composites by using acetylene terminated conjugated Schiff's base monomers |
| CN101391893A (en) * | 2008-11-05 | 2009-03-25 | 北京玻钢院复合材料有限公司 | Carbon/carbon composite material and preparation method thereof |
| WO2015058668A1 (en) * | 2013-10-23 | 2015-04-30 | 武汉大学 | Graphite composite grounding material and preparation method thereof |
| CN108046821A (en) * | 2018-01-24 | 2018-05-18 | 航天睿特碳材料有限公司 | A kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon carbon lid plate |
| CN108794745A (en) * | 2018-05-11 | 2018-11-13 | 顺德职业技术学院 | Schiff bases carbon forming agent containing triazine ring and its synthetic method |
| CN109111570A (en) * | 2018-07-13 | 2019-01-01 | 顺德职业技术学院 | Linear phosphorous schiff bases carbon forming agent and its synthetic method |
| CN110498685A (en) * | 2019-08-02 | 2019-11-26 | 中国航发北京航空材料研究院 | A kind of carbon fibre reinforced ceramics based composites preparation method |
| CN111584151A (en) * | 2020-05-26 | 2020-08-25 | 杭州幄肯新材料科技有限公司 | Carbon fiber/carbon/graphite composite carbon felt and method for enhancing heat conduction and electric conduction performance of polymer composite material |
| WO2020182353A1 (en) * | 2019-03-08 | 2020-09-17 | Gurit (Uk) Ltd | Fire-retardant composite materials |
-
2021
- 2021-05-10 CN CN202110504988.5A patent/CN113387713B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5437821A (en) * | 1992-09-30 | 1995-08-01 | The United States Of America As Represented By The Secretary Of The Navy | Process for making carbon-carbon composites by using acetylene terminated conjugated Schiff's base monomers |
| CN101391893A (en) * | 2008-11-05 | 2009-03-25 | 北京玻钢院复合材料有限公司 | Carbon/carbon composite material and preparation method thereof |
| WO2015058668A1 (en) * | 2013-10-23 | 2015-04-30 | 武汉大学 | Graphite composite grounding material and preparation method thereof |
| CN108046821A (en) * | 2018-01-24 | 2018-05-18 | 航天睿特碳材料有限公司 | A kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon carbon lid plate |
| CN108794745A (en) * | 2018-05-11 | 2018-11-13 | 顺德职业技术学院 | Schiff bases carbon forming agent containing triazine ring and its synthetic method |
| CN109111570A (en) * | 2018-07-13 | 2019-01-01 | 顺德职业技术学院 | Linear phosphorous schiff bases carbon forming agent and its synthetic method |
| WO2020182353A1 (en) * | 2019-03-08 | 2020-09-17 | Gurit (Uk) Ltd | Fire-retardant composite materials |
| CN110498685A (en) * | 2019-08-02 | 2019-11-26 | 中国航发北京航空材料研究院 | A kind of carbon fibre reinforced ceramics based composites preparation method |
| CN111584151A (en) * | 2020-05-26 | 2020-08-25 | 杭州幄肯新材料科技有限公司 | Carbon fiber/carbon/graphite composite carbon felt and method for enhancing heat conduction and electric conduction performance of polymer composite material |
Non-Patent Citations (1)
| Title |
|---|
| 雷毅等: "碳/碳复合材料用基体先驱体研究进展", 《宇航材料工艺》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115594507A (en) * | 2022-10-12 | 2023-01-13 | 郑州格瑞特高温材料有限公司（Cn） | Low-density microporous silicon nitride combined silicon carbide material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113387713B (en) | 2023-01-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11027503B2 (en) | Fiber reinforced polymer composite material and preparation method thereof | |
| DE2338857C3 (en) | Laminate for electrical insulation | |
| EP0287517B1 (en) | Communication or control cable with a supporting element | |
| KR101472850B1 (en) | High-temperature-resistant composite | |
| CN113387713B (en) | Method for preparing flexible graphite grounding conductor material by in-situ polymerization method | |
| DE3027363C2 (en) | Process for making a carbon fiber reinforced carbon friction material | |
| DE2456669A1 (en) | HIGH TEMPERATURE RESISTANT FABRIC | |
| KR102041989B1 (en) | Fiber-reinforced composite material and process for producing fiber-reinforced composite material | |
| DE2504931A1 (en) | METHOD OF MANUFACTURING A FRICTION PART | |
| DE2510796C2 (en) | Laminate and process for its manufacture | |
| EP2740321A2 (en) | Electrically conductive material and radiator comprising electrically conductive material and also process for the production thereof | |
| CN105481413A (en) | Preparation method of metal-type C/C composite material carbon slide strips | |
| US4101354A (en) | Coating for fibrous carbon material in boron containing composites | |
| DE112015005492T5 (en) | Superconducting cable and cable core for conductive cable | |
| DE112012000867B4 (en) | Shielded cable | |
| EP3988692A1 (en) | Current-collecting sliding material and method for producing same | |
| EP0231787B1 (en) | Method of manufacturing an impervious carbon or graphite article | |
| CN115810442A (en) | Outdoor military soft wear-resistant reel power cable | |
| KR101675336B1 (en) | Eletrod collector of fiber type for secondary battery and Manufacturing method thereof | |
| CN113846489B (en) | Conductive modified basalt fiber cloth, low-insulativity basalt fiber reinforced polymer composite material and preparation method thereof | |
| WO2018003043A1 (en) | Coil for rotating electrical machine, method for producing coil for rotating electrical machine, mica tape, method for producing mica tape, cured product of mica tape, and insulating material | |
| DE112015002016T5 (en) | Cylindrical heat insulating material and process for its production | |
| CN103236292A (en) | Mica tape | |
| EP0466962B1 (en) | Process for making carbon-fibre-reinforced carbon composite bodies. | |
| JPS6136329B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |