CN110105714A - The preparation method of carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material - Google Patents
The preparation method of carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material Download PDFInfo
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- CN110105714A CN110105714A CN201910464687.7A CN201910464687A CN110105714A CN 110105714 A CN110105714 A CN 110105714A CN 201910464687 A CN201910464687 A CN 201910464687A CN 110105714 A CN110105714 A CN 110105714A
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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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- 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
- C08K3/06—Sulfur
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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
- C08K5/04—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 the preparation methods of a kind of carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material, and described method includes following steps: Step 1: the preparation of carbon fiber/epoxy resin prepreg;Step 2: the mixing of ethylene propylene diene rubber;It is paved Step 3: first carbon fiber/epoxy resin prepreg is placed in mold, then it will be molded after the ethylene propylene diene rubber of mixing is placed on and paves above epoxy prepreg, it is placed in moulding press and solidifies, obtain the co-curing system of ethylene propylene diene rubber and epoxy matrix composite;Step 4: the co-curing system of ethylene propylene diene rubber and epoxy matrix composite is placed at room temperature, carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material are obtained.The present invention prepares the carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material that can be applied in solid rocket motor case by the way of co-curing, and ensure that the adhesive property of two-phase.
Description
Technical field
The present invention relates to a kind of, and that carbon-fibre reinforced epoxy resin and ethylene propylene diene rubber are prepared by way of co-curing is multiple
The method of condensation material.
Background technique
In recent years, as China greatly develops the national Major Strategic such as Aeronautics and Astronautics, weaponry, composite material is ground
Study carefully the extremely extensive of development.Wherein polymer matrix composites have obtained great concern, since its density is low, high specific strength, height
The characteristic of specific modulus is widely used in aerospace field.In aerospace field, solid rocket motor case is adopted more
It is prepared with carbon fiber reinforced epoxy resin-based composite.But since epoxy resin-base composite material heat resistance has
Limit, so in the region that directly contacts of inside and powder column of solid rocket motor case there are one layer of heat insulation layer, usually fourth
Nitrile rubber, silicon rubber and ethylene propylene diene rubber.Ethylene propylene diene rubber obtained more and more applications, ethylene-propylene-diene monomer in recent years
Glue is obtained under catalytic condition by solvent polymeric by ethylene, propylene and Third monomer, and conventionally used Third monomer is
Dicyclopentadiene and bornylene.Ethylene propylene diene rubber be saturation glue only in side group there are unsaturated bond, unsaturated coefficient compared with
It is low, so ethylene propylene diene rubber has excellent ageing-resistant performance and chemical stability.However ethylene propylene diene rubber can be used as
Heat insulation layer is because of its extremely low thermal conductivity coefficient and the higher carbon forming rate after burned.
But due to the saturated-backbone structure, extremely low degree of unsaturation and nonpolar feature of ethylene propylene diene rubber, so that
Ethylene propylene diene rubber becomes more difficult with polymer matrix composites and the bonding of space flight aluminum matrix composite.Ethylene-propylene-diene monomer
Glue is directly contacted with powder column in the combustion chamber, and in solid propellant rocket work, internal operating condition is very severe, and temperature is reachable
To 2600 ~ 2800 DEG C, instantaneous pressure is up to 15MPa, so this just proposes higher want to the bonding of rubber and case material
It asks, otherwise once being failed in the case where work, consequence will not can be envisaged internal ethylene propylene diene rubber.Therefore, it faces
The requirements at the higher level that solid rocket motor case of new generation proposes, there is an urgent need to a kind of new preparation methods to high efficiency for we
Solve the problems, such as that ethylene propylene diene rubber is bonding with shell and then be improved overall performance.
Summary of the invention
The present invention is keeping carbon-fibre reinforced epoxy resin to solve the problems, such as that ethylene propylene diene rubber is bonding with shell
On the basis of based composites and ethylene propylene diene rubber own advantages, a kind of more efficient, energy-efficient fibre reinforced is provided
The preparation method of epoxy resin and ternary ethlene propyene rubbercompound material.This method prepares fibre reinforced by the method for co-curing
Epoxy resin and ternary ethlene propyene rubbercompound material have it applied to solid fire under the premise of guaranteeing two-phase adhesive property
The possibility of arrow motor body.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material, includes the following steps:
Step 1: the preparation of carbon fiber/epoxy resin prepreg: using epoxy resin, curing agent and carbon fiber as raw material, by carbon fiber
Dimension is impregnated into the mixed liquor of epoxy resin and curing agent, obtains carbon fiber/epoxy resin prepreg, in which: curing agent is virtue
Amine curing agent m-phenylene diamine (MPD) (MPD);In the mixed liquor of epoxy resin and curing agent, the mass ratio of epoxy resin and curing agent is
10:1.4~1.7;The model E-51 of epoxy resin;
Step 2: the mixing of ethylene propylene diene rubber: by ethylene-propylene-diene monomer sol solution mill on the double roll mill, to its packet roller
Afterwards, vulcanizing agent and auxiliary agent is added, is uniformly mixed, left and right cutter three times, beats that triangle bag is thin to lead to, and bottom sheet is spare, in which: vulcanizing agent
For cumyl peroxide (DCP);The mass ratio of ethylene propylene diene rubber and vulcanizing agent is about 100:2.5 ~ 3.5;Auxiliary agent is to hand over
Joining inhibitor or crosslinking accelerator, cross-linked inhibitor is sulphur (S), three acrylic isocyanuric acid ester (TAIC) of crosslinking accelerator,
Dosage is depending on adjuvant used type: if the crosslinking accelerator being added is three acrylic isocyanuric acid esters (TAIC), ternary second
The mass ratio of third rubber and three acrylic isocyanuric acid esters (TAIC) is about 100:4.0 ~ 6.0;If the cross-linked inhibitor being added
For sulphur (S), then the mass ratio of ethylene propylene diene rubber and sulphur (S) are about 100:0.3 ~ 0.5, can finally obtain three by mixing
First the third raw rubber of second;
It is paved Step 3: first the carbon fiber/epoxy resin prepreg prepared in step 1 is placed in mold, then by step 2
It is middle to be molded after the ethylene propylene diene rubber of mixing is placed on and paves above epoxy prepreg, it is placed in moulding press and solidifies,
Obtain the co-curing system of ethylene propylene diene rubber and epoxy matrix composite, in which: solidification temperature is 80 ~ 180 DEG C, curing time
It is 5 ~ 6 hours;
Step 4: the co-curing system of the ethylene propylene diene rubber obtained in step 3 and epoxy matrix composite is put at room temperature
24 ~ 48h is set, carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material are obtained, in which: it is compound that carbon fiber accounts for resin base
The 60 ~ 65% of material total volume, ethylene propylene diene rubber account for the 60 ~ 90% of total composite volume.
Compared with the prior art, the present invention has the advantage that
The present invention prepares the fibre reinforced epoxy that can be applied in solid rocket motor case by the way of co-curing
Resin and ternary ethlene propyene rubbercompound material, and ensure that the adhesive property of two-phase.
Detailed description of the invention
Fig. 1 is the curing cycle figure of curing agent used in embodiment 1;
Fig. 2 is 1 ethylene propylene diene rubber curing curve figure of embodiment;
Fig. 3 is the digital photograph in kind that 1 co-curing example interface of embodiment bears weight;
Fig. 4 be 1 co-curing example interface of embodiment by external force when digital photograph in kind;
Fig. 5 be 1 step curing sample of embodiment by external force when digital photograph in kind.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained
Lid is within the protection scope of the present invention.
Embodiment 1:
It present embodiments provides a kind of total for the epoxy matrix composite and ethylene propylene diene rubber of curing agent with m-phenylene diamine (MPD) (MPD)
Curing method, the specific steps are as follows:
15g E-51 epoxy resin is weighed first be placed in 50 DEG C of vacuum drying oven and heat, then weigh 1.7g solid m-phenylene diamine (MPD)
(MPD) it is placed in glass (or enamel), then places it in common air blast thermostatic drying chamber, being heated to 115 DEG C keeps MPD molten
Change;15min is kept the temperature when melt temperature reaches 115 DEG C, takes out simultaneously cooled to room temperature, that is, ponderable quantity.By the epoxy after heating
Resin and MPD are sufficiently mixed, are spare.
It chooses Dongli Ltd. and produces T800 type carbon fiber filament, be prepared into that length is 25cm, the number of turns is by chopping machine
This carbon fibre tow is completely infused in the mixed solution of epoxy resin and phenylenediamine (MPD) by the chopped carbon fiber tow of 25 circles
In, carbon fiber/epoxy resin base prepreg is obtained after mixing.
It weighs 10g ethylene propylene diene rubber and is placed on two-roll mill mill, after its packet roller, sequentially add vulcanizing agent peroxidating
Diisopropylbenzene (DIPB) (DCP) 0.4g, cross-linked inhibitor sulphur (S) 0.1g, left and right cutter three times, it is thin to beat triangle bag after being sufficiently mixed uniformly
Logical, bottom sheet will place at room temperature for 24 hours by the ethylene propylene diene rubber being kneaded, spare.
Ethylene propylene diene rubber 3.5g after weighing vulcanization, is laid in the mold of 2cm thickness, is placed on moulding press and is molded, most
It is pressed into the strip of 1 ~ 2cm thickness afterwards, it is spare.
Then, at room temperature, by the ethylene-propylene-diene monomer after above-mentioned carbon fiber/epoxy resin based composites and vulcanization
Glue is put in a mold, and vulcanization is heated on vulcanizing press, and curing cycle is 80 DEG C/2h, and 130 DEG C/2h, 150 DEG C/1h, 160
DEG C/1h, the co-curing system of the ethylene propylene diene rubber of preparation and epoxy matrix composite is placed for 24 hours at room temperature, obtains carbon
Fiber reinforced epoxy resin and ternary ethlene propyene rubbercompound material.
Fig. 1, Fig. 2 provide necessary theoretical basis for the curing cycle during co-curing, and Fig. 3, Fig. 4 demonstrate solid altogether
The interface of change system has good adhesive strength: split-phase and can not born the weight of certain mass by external force, Fig. 5 is then
The sample of step curing, noted phase separation phenomena is serious in the case where by external force, it was demonstrated that not good between step curing sample two-phase
Adhesive property.
Embodiment 2:
15g E-51 epoxy resin is weighed first be placed in 50 DEG C of vacuum drying oven and heat, then weigh 1.7g solid m-phenylene diamine (MPD)
(MPD) it is placed in glass (or enamel), then places it in common air blast thermostatic drying chamber, being heated to 115 DEG C keeps MPD molten
Change;15min is kept the temperature when melt temperature reaches 115 DEG C, takes out simultaneously cooled to room temperature, that is, ponderable quantity.By the epoxy after heating
Resin and MPD are sufficiently mixed, are spare.
It chooses Dongli Ltd. and produces T800 type carbon fiber filament, be prepared into that length is 25cm, the number of turns is by chopping machine
This carbon fibre tow is completely infused in the mixed solution of epoxy resin and phenylenediamine (MPD) by the chopped carbon fiber tow of 25 circles
In, carbon fiber/epoxy resin base prepreg is obtained after mixing.
It weighs 10g ethylene propylene diene rubber and is placed on two-roll mill mill, after its packet roller, sequentially add vulcanizing agent peroxidating
Diisopropylbenzene (DIPB) (DCP) 0.4g, crosslinking accelerator three acrylic isocyanuric acid ester (TAIC) 0.5g, left and right is cut after being sufficiently mixed uniformly
Knife three times, beats that triangle bag is thin logical, and bottom sheet will place at room temperature for 24 hours by the ethylene propylene diene rubber being kneaded, spare.
Ethylene propylene diene rubber 3.5g after weighing vulcanization, is laid in the mold of 2cm thickness, is placed on moulding press and is molded, most
It is pressed into the strip of 1 ~ 2cm thickness afterwards, it is spare.
Then, at room temperature, by the ethylene-propylene-diene monomer after above-mentioned carbon fiber/epoxy resin based composites and vulcanization
Glue is put in a mold, and vulcanization is heated on vulcanizing press, and curing cycle is 80 DEG C/2h, and 130 DEG C/2h, 150 DEG C/1h, 160
DEG C/1h, the co-curing system of the ethylene propylene diene rubber of preparation and epoxy matrix composite is placed into 48h at room temperature, obtains carbon
Fiber reinforced epoxy resin and ternary ethlene propyene rubbercompound material.
Claims (10)
1. the preparation method of a kind of carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material, it is characterised in that the side
Method includes the following steps:
Step 1: the preparation of carbon fiber/epoxy resin prepreg: using epoxy resin, curing agent and carbon fiber as raw material, by carbon fiber
Dimension is impregnated into the mixed liquor of epoxy resin and curing agent, obtains carbon fiber/epoxy resin prepreg;
Step 2: the mixing of ethylene propylene diene rubber: by ethylene-propylene-diene monomer sol solution mill on the double roll mill, to its packet roller
Afterwards, vulcanizing agent and auxiliary agent is added, is uniformly mixed, left and right cutter three times, beats that triangle bag is thin to lead to, and bottom sheet obtains three by mixing
First the third raw rubber of second;
It is paved Step 3: first carbon fiber/epoxy resin prepreg is placed in mold, then by the ethylene-propylene-diene monomer by being kneaded
Glue is placed on paved above epoxy prepreg after mold, be placed in moulding press and solidify, obtain ethylene propylene diene rubber and epoxy
The co-curing system of based composites;
Step 4: the co-curing system of ethylene propylene diene rubber and epoxy matrix composite is placed at room temperature, carbon fiber is obtained
Reinforced epoxy and ternary ethlene propyene rubbercompound material, in which: carbon fiber accounts for the 60 ~ 65% of polymer matrix composites total volume,
Ethylene propylene diene rubber accounts for the 60 ~ 90% of total composite volume.
2. the preparation method of carbon-fibre reinforced epoxy resin according to claim 1 and ternary ethlene propyene rubbercompound material,
It is characterized in that the curing agent is m-phenylene diamine (MPD).
3. the preparation side of carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material according to claim 1 or 2
Method, it is characterised in that in the mixed liquor of the epoxy resin and curing agent, the mass ratio of epoxy resin and curing agent be 10:1.4 ~
1.7。
4. the preparation method of carbon-fibre reinforced epoxy resin according to claim 1 and ternary ethlene propyene rubbercompound material,
It is characterized in that the vulcanizing agent is cumyl peroxide.
5. the preparation side of carbon-fibre reinforced epoxy resin and ternary ethlene propyene rubbercompound material according to claim 1 or 4
Method, it is characterised in that the mass ratio of the ethylene propylene diene rubber and vulcanizing agent is 100:2.5 ~ 3.5.
6. the preparation method of carbon-fibre reinforced epoxy resin according to claim 1 and ternary ethlene propyene rubbercompound material,
It is characterized in that the auxiliary agent is cross-linked inhibitor or crosslinking accelerator.
7. the preparation method of carbon-fibre reinforced epoxy resin according to claim 6 and ternary ethlene propyene rubbercompound material,
It is characterized in that the crosslinking accelerator is three acrylic isocyanuric acid esters, ethylene propylene diene rubber and three acrylic isocyanuric acid esters
Mass ratio be 100:4.0 ~ 6.0.
8. the preparation method of carbon-fibre reinforced epoxy resin according to claim 6 and ternary ethlene propyene rubbercompound material,
It is characterized in that the cross-linked inhibitor is sulphur, the mass ratio of ethylene propylene diene rubber and sulphur is 100:0.3 ~ 0.5.
9. the preparation method of carbon-fibre reinforced epoxy resin according to claim 1 and ternary ethlene propyene rubbercompound material,
It is characterized in that the solidification temperature is 80 ~ 180 DEG C, curing time is 5 ~ 6 hours.
10. the preparation method of carbon-fibre reinforced epoxy resin according to claim 1 and ternary ethlene propyene rubbercompound material,
It is characterized in that time for placing at room temperature of the co-curing system of the ethylene propylene diene rubber and epoxy matrix composite be 24 ~
48h。
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CN114571744A (en) * | 2022-04-21 | 2022-06-03 | 内蒙古工业大学 | Fiber preform reinforced resin rubber ternary composite material and preparation method and application thereof |
CN114957741A (en) * | 2021-12-29 | 2022-08-30 | 江苏志纤复能科技有限公司 | Novel low-temperature co-curing high-damping composite material and preparation method 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 |
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 |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN114957741A (en) * | 2021-12-29 | 2022-08-30 | 江苏志纤复能科技有限公司 | Novel low-temperature co-curing high-damping composite material and preparation method thereof |
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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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