CN110105714B - Preparation method of carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material - Google Patents
Preparation method of carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material Download PDFInfo
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- CN110105714B CN110105714B CN201910464687.7A CN201910464687A CN110105714B CN 110105714 B CN110105714 B CN 110105714B CN 201910464687 A CN201910464687 A CN 201910464687A CN 110105714 B CN110105714 B CN 110105714B
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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
- C08G59/50—Amines
- C08G59/5033—Amines 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
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/042—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
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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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- 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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/16—Ethene-propene or ethene-propene-diene copolymers
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- 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
- C08K3/06—Sulfur
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- 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
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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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
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
Abstract
The invention discloses a preparation method of a carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material, which comprises the following steps: step one, preparing a carbon fiber/epoxy resin prepreg; mixing ethylene propylene diene monomer; thirdly, placing the carbon fiber/epoxy resin prepreg in a mold to be paved, then placing the mixed ethylene propylene diene monomer rubber above the epoxy resin prepreg to be paved, closing the mold, and placing the mold in a mold press to be cured to obtain a co-curing system of the ethylene propylene diene monomer rubber and the epoxy group composite material; and step four, placing the co-curing system of the ethylene propylene diene monomer and the epoxy composite material at room temperature to obtain the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material. The carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material which can be applied to the shell of the solid rocket engine is prepared in a co-curing mode, and the bonding performance of the two phases is ensured.
Description
Technical Field
The invention relates to a method for preparing a carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material in a co-curing mode.
Background
In recent years, with the great development of national important strategies of aviation, aerospace, weaponry and the like in China, the research and development of the composite material are extremely wide. The resin-based composite material is of great interest, and is widely applied to the field of aerospace due to the characteristics of low density, high specific strength and high specific modulus. In the field of aerospace, a solid rocket engine shell is mostly prepared from carbon fiber reinforced epoxy resin matrix composite materials. However, due to the limited heat resistance of epoxy resin-based composites, a thermal insulation layer, typically nitrile rubber, silicone rubber, and ethylene propylene diene monomer, is present in the interior of the solid rocket motor case in the area directly contacting the grain. Ethylene propylene diene monomer, which is commonly used as a third monomer, is dicyclopentadiene and bornylene, has gained increasing use in recent years, and is obtained by solvent polymerization of ethylene, propylene and the third monomer under catalytic conditions. The ethylene propylene diene monomer is a saturated rubber, only unsaturated bonds exist on side groups, and the unsaturated coefficient is low, so that the ethylene propylene diene monomer has excellent aging resistance and chemical stability. Ethylene propylene diene monomer may be used as the thermal insulation layer, however, because of its extremely low thermal conductivity and high carbon formation rate after combustion.
However, due to the saturated skeleton structure, extremely low unsaturation degree and non-polarity characteristics of the ethylene propylene diene monomer, the bonding of the ethylene propylene diene monomer with the resin matrix composite and the aluminum matrix composite for aerospace becomes difficult. The ethylene propylene diene monomer rubber is in direct contact with the explosive column in the combustion chamber, when the solid rocket engine works, the internal working condition is very bad, the temperature can reach 2600-2800 ℃, and the instantaneous pressure can reach 15MPa, so that higher requirements are provided for the bonding of rubber and a shell material, otherwise, once the internal ethylene propylene diene monomer rubber fails in the working condition, the consequences cannot be imagined. Therefore, in order to meet the higher requirements of the shell of the solid rocket engine of the new generation, a new preparation method is urgently needed, so that the problem of bonding ethylene propylene diene monomer rubber and the shell is solved efficiently, and the overall performance is improved.
Disclosure of Invention
The invention provides a preparation method of a carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material, which is more efficient and energy-saving, in order to solve the problem of bonding ethylene propylene diene monomer and a shell and maintain the advantages of the carbon fiber reinforced epoxy resin matrix composite material and the ethylene propylene diene monomer. The carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material is prepared by a co-curing method, and the possibility of being applied to a solid rocket engine shell is realized on the premise of ensuring the two-phase bonding performance.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material comprises the following steps:
step one, preparing a carbon fiber/epoxy resin prepreg: using epoxy resin, a curing agent and carbon fibers as raw materials, and impregnating the carbon fibers into a mixed solution of the epoxy resin and the curing agent to obtain a carbon fiber/epoxy resin prepreg, wherein: the curing agent is arylamine curing agent metaphenylene diamine (MPD); in the mixed liquid of the epoxy resin and the curing agent, the mass ratio of the epoxy resin to the curing agent is 10: 1.4-1.7; the type of the epoxy resin is E-51;
step two, mixing ethylene propylene diene monomer: the ethylene propylene diene monomer solution is milled on a double-roller mill, after the ethylene propylene diene monomer solution is coated on rollers, a vulcanizing agent and an auxiliary agent are added, the mixture is uniformly mixed, a left cutter and a right cutter are used for three times, triangular coating is performed for thin passing, and sheets are taken for standby application, wherein: the vulcanizing agent is dicumyl peroxide (DCP); the mass ratio of the ethylene propylene diene monomer to the vulcanizing agent is about 100: 2.5 to 3.5; the auxiliary agent is a crosslinking inhibitor or a crosslinking accelerator, the crosslinking inhibitor is sulfur (S), and the crosslinking accelerator is triacrylate isocyanurate (TAIC), and the dosage of the auxiliary agent is determined according to the type of the auxiliary agent: if the crosslinking accelerator added is triacrylate isocyanurate (TAIC), the mass ratio of ethylene propylene diene monomer to triacrylate isocyanurate (TAIC) is about 100: 4.0 to 6.0; if the crosslinking inhibitor added is sulfur (S), the mass ratio of ethylene propylene diene monomer to sulfur (S) is approximately 100: 0.3-0.5, and finally obtaining the mixed ethylene propylene diene monomer raw rubber;
step three, firstly, placing the carbon fiber/epoxy resin prepreg prepared in the step one in a mould to be paved, then placing the ethylene propylene diene monomer rubber mixed in the step two above the epoxy resin prepreg to be paved, closing the mould, and placing the mould in a mould press to be cured to obtain a co-curing system of the ethylene propylene diene monomer rubber and the epoxy group composite material, wherein: the curing temperature is 80-180 ℃, and the curing time is 5-6 hours;
step four, placing the co-curing system of the ethylene propylene diene monomer and epoxy group composite material obtained in the step three at room temperature for 24-48 h to obtain the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material, wherein: the carbon fiber accounts for 60-65% of the total volume of the resin matrix composite, and the ethylene propylene diene monomer accounts for 60-90% of the total volume of the composite.
Compared with the prior art, the invention has the following advantages:
the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material which can be applied to the shell of the solid rocket engine is prepared in a co-curing mode, and the bonding performance of the two phases is ensured.
Drawings
FIG. 1 is a curing schedule of the curing agent used in example 1;
FIG. 2 is a graph showing the vulcanization of ethylene-propylene-diene monomer rubber of example 1;
FIG. 3 is a digital photograph of an interface load of a co-cured sample of example 1;
FIG. 4 is a digital photograph of an interface of a co-cured sample of example 1 when subjected to an external force;
FIG. 5 is a digital photograph of the sample cured step by step in example 1 when subjected to an external force.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
the embodiment provides a co-curing method of an epoxy-based composite material and ethylene propylene diene monomer rubber by taking m-phenylenediamine (MPD) as a curing agent, which comprises the following specific steps:
firstly weighing 15g E-51 epoxy resin, putting the epoxy resin in a vacuum oven at 50 ℃ for heating, then weighing 1.7g of solid m-phenylenediamine (MPD) and putting the MPD in glass (or enamel), then putting the glass (or enamel) in a common blast constant-temperature drying oven, and heating to 115 ℃ to melt the MPD; and (4) preserving the temperature for 15min when the temperature of the melt reaches 115 ℃, taking out the melt, and naturally cooling the melt to room temperature to obtain the product. The heated epoxy resin and MPD were mixed thoroughly and ready for use.
Selecting T800 type carbon fiber filaments produced by Toray corporation, preparing short carbon fiber tows with the length of 25cm and the number of turns of 25 turns by a chopping machine, completely soaking the carbon fiber tows in a mixed solution of epoxy resin and phenylenediamine (MPD), and uniformly mixing to obtain the carbon fiber/epoxy resin-based prepreg.
Weighing 10g of ethylene propylene diene monomer rubber, placing the ethylene propylene diene monomer rubber in a two-roll open mill for open milling, after the ethylene propylene diene monomer rubber is coated on a roll, sequentially adding 0.4g of dicumyl peroxide (DCP) serving as a vulcanizing agent and 0.1g of sulfur (S) serving as a crosslinking inhibitor, fully and uniformly mixing, then cutting the mixture for three times, wrapping the mixture in a triangular mode, thinly passing the mixture, taking the mixture out, and placing the mixed ethylene propylene diene monomer rubber for 24 hours at room temperature for later use.
Weighing 3.5g of vulcanized ethylene propylene diene monomer, flatly paving in a mold with the thickness of 2cm, placing on a molding press for mold pressing, and finally pressing into a long strip with the thickness of 1-2 cm for later use.
And then, under the condition of room temperature, placing the carbon fiber/epoxy resin matrix composite material and vulcanized ethylene propylene diene monomer rubber in a mold, heating and vulcanizing on a flat vulcanizing machine, wherein the curing system is 80 ℃/2h, 130 ℃/2h, 150 ℃/1h and 160 ℃/1h, and placing the prepared co-curing system of the ethylene propylene diene monomer rubber and the epoxy matrix composite material for 24h at room temperature to obtain the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer rubber composite material.
Fig. 1 and 2 provide the necessary theoretical basis for the curing regime during co-curing, and fig. 3 and 4 demonstrate that the interface of the co-curing system has good bonding strength: namely, the sample does not split phase under external force and can bear a heavy object with certain mass, and the phase splitting phenomenon is serious under the external force condition of the step-by-step solidified sample shown in figure 5, which proves that no good bonding performance exists between two phases of the step-by-step solidified sample.
Example 2:
firstly weighing 15g E-51 epoxy resin, putting the epoxy resin in a vacuum oven at 50 ℃ for heating, then weighing 1.7g of solid m-phenylenediamine (MPD) and putting the MPD in glass (or enamel), then putting the glass (or enamel) in a common blast constant-temperature drying oven, and heating to 115 ℃ to melt the MPD; and (4) preserving the temperature for 15min when the temperature of the melt reaches 115 ℃, taking out the melt, and naturally cooling the melt to room temperature to obtain the product. The heated epoxy resin and MPD were mixed thoroughly and ready for use.
Selecting T800 type carbon fiber filaments produced by Toray corporation, preparing short carbon fiber tows with the length of 25cm and the number of turns of 25 turns by a chopping machine, completely soaking the carbon fiber tows in a mixed solution of epoxy resin and phenylenediamine (MPD), and uniformly mixing to obtain the carbon fiber/epoxy resin-based prepreg.
Weighing 10g of ethylene propylene diene monomer rubber, placing the ethylene propylene diene monomer rubber in a two-roll open mill for open milling, after the ethylene propylene diene monomer rubber is coated on a roll, sequentially adding 0.4g of dicumyl peroxide (DCP) serving as a vulcanizing agent and 0.5g of Triallylisocyanurate (TAIC) serving as a crosslinking accelerator, fully and uniformly mixing, then cutting the mixture for three times from left to right, wrapping the mixture in a triangular mode for thinning, discharging the sheet, and placing the mixed ethylene propylene diene monomer rubber for 24 hours at room temperature for later use.
Weighing 3.5g of vulcanized ethylene propylene diene monomer, flatly paving in a mold with the thickness of 2cm, placing on a molding press for mold pressing, and finally pressing into a long strip with the thickness of 1-2 cm for later use.
And then, under the condition of room temperature, placing the carbon fiber/epoxy resin matrix composite material and vulcanized ethylene propylene diene monomer rubber in a mold, heating and vulcanizing on a flat vulcanizing machine, wherein the curing system is 80 ℃/2h, 130 ℃/2h, 150 ℃/1h and 160 ℃/1h, and placing the prepared co-curing system of the ethylene propylene diene monomer rubber and the epoxy matrix composite material for 48h at room temperature to obtain the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer rubber composite material.
Claims (10)
1. A preparation method of a carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material is characterized by comprising the following steps:
step one, preparing a carbon fiber/epoxy resin prepreg: taking epoxy resin, a curing agent and carbon fibers as raw materials, and soaking the carbon fibers into a mixed solution of the epoxy resin and the curing agent to obtain a carbon fiber/epoxy resin prepreg;
step two, mixing ethylene propylene diene monomer: the ethylene propylene diene monomer solution is milled on a double-roll mill, after the ethylene propylene diene monomer solution is coated on a roll, a vulcanizing agent and an auxiliary agent are added, the mixture is uniformly mixed, a left cutter and a right cutter are used for three times, triangular coating is carried out for thin passing, and sheet discharging is carried out, so that the mixed ethylene propylene diene monomer raw rubber is obtained;
thirdly, placing the carbon fiber/epoxy resin prepreg in a mold to be paved, then placing the mixed ethylene propylene diene monomer rubber above the epoxy resin prepreg to be paved, closing the mold, and placing the mold in a mold press to be cured to obtain a co-curing system of the ethylene propylene diene monomer rubber and the epoxy group composite material;
step four, placing the co-curing system of the ethylene propylene diene monomer and the epoxy composite material at room temperature to obtain the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material, wherein: the carbon fiber accounts for 60-65% of the total volume of the resin matrix composite, and the ethylene propylene diene monomer accounts for 60-90% of the total volume of the composite.
2. The method for preparing a carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 1, wherein the curing agent is m-phenylenediamine.
3. The preparation method of the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 1 or 2, wherein the mass ratio of the epoxy resin to the curing agent in the mixed solution of the epoxy resin and the curing agent is 10: 1.4-1.7.
4. The method for preparing the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 1, wherein the vulcanizing agent is dicumyl peroxide.
5. The preparation method of the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 1 or 4, wherein the mass ratio of the ethylene propylene diene monomer to the vulcanizing agent is 100: 2.5 to 3.5.
6. The method for preparing the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 1, wherein the auxiliary agent is a crosslinking inhibitor or a crosslinking accelerator.
7. The method for preparing the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 6, wherein the crosslinking accelerator is triacrylate isocyanurate, and the mass ratio of the ethylene propylene diene monomer to the triacrylate isocyanurate is 100: 4.0 to 6.0.
8. The preparation method of the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 6, wherein the crosslinking inhibitor is sulfur, and the mass ratio of the ethylene propylene diene monomer to the sulfur is 100: 0.3 to 0.5.
9. The preparation method of the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 1, wherein the curing temperature is 80-180 ℃ and the curing time is 5-6 hours.
10. The preparation method of the carbon fiber reinforced epoxy resin and ethylene propylene diene monomer composite material according to claim 1, wherein the co-curing system of the ethylene propylene diene monomer and epoxy composite material is placed at room temperature for 24-48 h.
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| CN114957741B (en) * | 2021-12-29 | 2024-01-02 | 江苏志纤复能科技有限公司 | Low-temperature co-cured high-damping composite material and preparation method thereof |
| CN114410019B (en) * | 2022-03-08 | 2023-12-26 | 内蒙古工业大学 | Carbon fiber/resin/rubber ternary composite material and preparation method and application thereof |
| CN114571744B (en) * | 2022-04-21 | 2024-04-26 | 内蒙古工业大学 | Fiber preform reinforced resin rubber ternary composite material and preparation method and application thereof |
| CN115595100A (en) * | 2022-10-24 | 2023-01-13 | 湖北三江航天江北机械工程有限公司（Cn） | High-strength adhesive for metal and various composite materials and bonding method |
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| JP2010120191A (en) * | 2008-11-17 | 2010-06-03 | Sri Sports Ltd | Tube and method for producing the same |
| CN101786356A (en) * | 2010-01-25 | 2010-07-28 | 张博明 | Preparation method of a co-cured high damping composite material |
| CN102009509A (en) * | 2010-05-10 | 2011-04-13 | 梁森 | Manufacturing technology of embedded co-curing high-damping composite and laminate material structure |
| CN102146196A (en) * | 2011-01-27 | 2011-08-10 | 北京玻钢院复合材料有限公司 | Preparation method of high damping epoxy resin composite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010120191A (en) * | 2008-11-17 | 2010-06-03 | Sri Sports Ltd | Tube and method for producing the same |
| CN101786356A (en) * | 2010-01-25 | 2010-07-28 | 张博明 | Preparation method of a co-cured high damping composite material |
| CN102009509A (en) * | 2010-05-10 | 2011-04-13 | 梁森 | Manufacturing technology of embedded co-curing high-damping composite and laminate material structure |
| CN102146196A (en) * | 2011-01-27 | 2011-08-10 | 北京玻钢院复合材料有限公司 | Preparation method of high damping epoxy resin composite |
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