CN109897375A - A kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape-memory material and preparation method thereof - Google Patents
A kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape-memory material and preparation method thereof Download PDFInfo
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- CN109897375A CN109897375A CN201910248346.6A CN201910248346A CN109897375A CN 109897375 A CN109897375 A CN 109897375A CN 201910248346 A CN201910248346 A CN 201910248346A CN 109897375 A CN109897375 A CN 109897375A
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- cyanate ester
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Abstract
The invention discloses a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape-memory materials and preparation method thereof, the composite material of shape memory is using cyanate ester resin as matrix resin, carboxyl-terminated liguid nitrile rubber and flexible-epoxy are toughener, carbon fibre material is reinforced phase, is solidified by heating in vacuum.It is good that toughening type cyanate ester resin pours building body working life length, being coated with property, pass through existing moulding process composite molding with carbon fiber, gained flexible-epoxy modified cyanic acid ester resin/carbon fiber composite shape-memory material surfacing, no significant defect has many advantages, such as that tensile strength is high, stretch modulus is high, shear strength is high, bending strength is high.
Description
Technical field
The present invention relates to a kind of cyanate ester resin/carbon fiber compound shape memory materials, especially relate to one kind by carboxyl end group liquid
The composite material of shape memory that body nitrile rubber and the common toughening cyanate ester resin of flexible-epoxy and carbon fiber are combined,
The compound shape memory material has many advantages, such as excellent shape-memory properties, high tensile, bending strength, shear strength,
It can be applied to the foldable structures such as satellite line, truss, belong to aerospace material technical field.
Background technique
Continually developing and utilizing with space resources, research aerospace device in need larger room device or
Structure, the huge volume of air equipment, which is increased, transports the difficulty into space environment from earth surface for it.How efficiently benefit
It is Important Problems urgently to be solved in space cause with carrying space and reduction delivery volume.Shape-memory material can be on ground
On folded, it is effective to reduce delivery volume, into space after accurately expansion reach scheduled shape.Shape memory polymers
Object is a kind of novel intelligent material with broad prospect of application.The shape-memory polymer mainly studied at present mainly has poly- ammonia
Ester, polynorbornene, styrene-butadiene copolymer etc..Studying the thermoplasticity shape-memory polymer used at present has power
Learn the defects such as performance is poor, receiving load is small, glass transition temperature is low.Simple shape-memory polymer can only realize that shape is remembered
Recall function, is difficult to meet the requirement of the strength and stiffness of structure.The defects of in order to solve shape-memory polymer poor mechanical property,
The research of polymer/carbon fiber composite shape-memory material is of great significance.
Polymer/carbon fiber composite shape memory material has many advantages, such as that density is low, intensity is high, shape-memory properties are good,
It is noticeable new material in current aerospace field application.Compared with pure resin shape-memory material, polymer/carbon
The advantages that fiber composite type shape-memory material deformation recovery power output with higher, high rigidity, high intensity.Due to carbon fiber
Modulus is high, is to form matrix in resin surface to split first when effect of the Cyanate Ester/carbon Fiber Composite by external force
Line, resin matrix and fiber interface unsticking, fiber is primarily subjected to load until fibrous fracture after resin fracture.It is polymerizeing simultaneously
Carbon fiber occurs to force tensile deformation in object/carbon fiber-based shape-memory material deformation process, and the internal stress of material increases, shape
Recovery rate is accelerated.
Summary of the invention
For current shape memory polymer material there are the mechanical properties such as intensity, rigidity poor, deformation recovery rate compared with
Slow problem, the first purpose of this invention are to be to provide one kind with deformation quantity is big, recovery rate is fast, density is low, high-tensile strength
Flexible-epoxy modified cyanic acid ester resin/carbon fiber composite the shape-memory material for the advantages that learning performance.
Another object of the present invention be to provide a kind of flexible-epoxy modified cyanic acid ester resin/carbon fiber it is compound
The preparation method of type shape-memory material, this method is simple, at low cost, is conducive to industrialized production.
In order to achieve the above technical purposes, the present invention provides a kind of high-strength flexible epoxy resin modification cyanate resins
Rouge/carbon fiber composite shape-memory material, is combined by carbon fibre material reinforced phase and modified cyanic acid ester resin matrix；
The modified cyanic acid ester resin matrix includes following mass component: 2~4 parts of carboxyl-terminated liguid nitrile rubber；Flexible-epoxy 2
~5 parts；8~12 parts of cyanate ester resin.
Preferred scheme, the cyanate ester resin include bisphenol E-type cyanate resin and/or bisphenol A cyanate ester resin.
Most preferred cyanate ester resin is bisphenol E-type cyanate resin, is in a liquid state at room temperature, viscosity: 30~150mpa.s/25
DEG C, it can purchase in Hubei Ju Sheng Science and Technology Ltd..
Preferred scheme, the molecular weight of the carboxyl-terminated liguid nitrile rubber are 2000~5000.Molecular weight is bigger, material
Viscosity it is bigger, the functional group reacted under equal quality is fewer, and carboxyl-terminated liguid nitrile rubber agglomerates into resin matrix
Rubber phase particle may be bigger, will affect the mechanical property of material, it is compound in preferred molecular weight ranges to obtain
Preferable comprehensive performance.
Preferred scheme, the flexible-epoxy include at least one of Jef-0211, Jew-0114, Jef-0213.
Most preferred flexible-epoxy is Jef-0211 flexible-epoxy, is in a liquid state at room temperature, viscosity 200~
300mpa.s/25 DEG C, epoxide number 0.35~0.40.
The carbon fibre material account for cyanate ester resin/carbon fiber composite shape-memory material gross mass 40%~
60%.
Preferred scheme, the carbon fibre material are T300 carbon fiber plain cloth (T300 carbon fiber plain cloth density
About 92g/m2), NIMKT carbon fibre fabric or SKO carbon fibre fabric.Carbon fibre material should be thin as far as possible, to guarantee resin prepreg
Material adequately penetrates between carbon fiber.
The present invention also provides a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape notes
Recall the preparation method of material, this method is to stir the heating of cyanate ester resin, carboxyl-terminated liguid nitrile rubber and flexible-epoxy
Carry out prepolymerization is mixed, obtains pouring building body；Gained pours building body coated in behind carbon fibre material surface, carries out vacuum heat cure,
To obtain the final product.
Preferred scheme, the temperature of the prepolymerization are 90~100 DEG C, and the time is 1~2 hour.
Preferred scheme, the thermosetting turn to temperature programming solidification: at 120~125 DEG C, keeping the temperature 3~4h；150~155
DEG C, keep the temperature 1~2h；At 170~175 DEG C, 1~2h is kept the temperature.
Flexible-epoxy modified cyanic acid ester resin/carbon fiber composite shape-memory material of the invention is with carboxyl end group liquid
The cyanate ester resin of body nitrile rubber and flexible-epoxy composite toughening is that base shape remembers resin material, is had longer
Working life and being coated with property, there is good processing performance, and use carbon fiber for reinforced phase, it is compound after formation with excellent
Shape-memory properties, flexible-epoxy modified cyanic acid ester tree the advantages that high tensile, bending strength, shear strength
Rouge/carbon fiber composite shape-memory material.
Key of the invention is the compound resin matrix for being to obtain a kind of excellent shape memory performance.For the prior art
Middle cyanate ester resin have excellent mechanics, heat-resisting, environmental resistance, but solidify after generate triazine ring rigid structure make it is proper
It is the disadvantages of crystallinity is high, solidfied material is more crisp, toughness is poor, the toughness reguirements for making it be difficult to meet distressed structure material.Meanwhile
The curing process of cyanate ester resin mainly passes through addition transition metal complex catalyst, therefore obtained resin pours building body
Trial period is shorter, is unable to satisfy the particular/special requirement of certain applications technique.And technical solution of the present invention using liquid nitrile rubber and
Flexible-epoxy improves the toughness of cyanate ester resin as composite toughing agent, and liquid nitrile rubber is as a kind of toughening performance
Preferable toughener introduces, and can be obviously improved the toughness of resin system using the flexible structure in main chain, but the fine rubber of fourth
Glue and cyanate ester resin compatibility are relatively poor, and there are obvious laminations, and resin not only can be improved in flexible-epoxy
The toughness of system also adds the compatibility between liquid nitrile rubber and cyanate ester resin, reduces the viscosity of resin system,
Reduce the difficulty of processing of resin system.Therefore liquid nitrile rubber, flexible-epoxy and cyanic acid in compound shape memory material
The excellent composite performance of ester resin obtains comprehensive embodiment, and the shape-memory material of acquisition has very excellent shape-memory properties,
Higher intensity, toughness and storage stability and processing performance simultaneously.
The compound of cyanate ester resin and carbon fibre material of the invention can be compound using conventional method.
Cyanate ester resin of the invention pours building body modest viscosity, is coated with performance and longer working life with good,
After solidifying with carbon fibre material, obtains cyanate ester resin/carbon fiber composite material of shape memory surfacing, lacked without obvious
It falls into.
High-intensitive flexible-epoxy modified cyanic acid ester resin/carbon fiber composite shape-memory material of the invention
Specific preparation method, is illustrated using carbon cloth as reinforced phase；Pass through carboxyl-terminated liguid nitrile rubber, flexible-epoxy
Resin is prepared to cyanate ester resin progress toughening modifying and pours building body (performed polymer), building body will be then poured and uniformly brush in carbon
Fiber cloth surface, subsequent cutting, laying, encapsulate, vacuumize be heating and curing to get.
Carbon cloth is cut according to [0/90 °], [+45 °/- 45 °] direction, size is each about 240mm × 200mm.[0/
90 °] 20 layers of paving, it is used for Mechanics Performance Testing；[+45 °/- 45 °] spread 10 layers, test for shape-memory properties.The carbon that will be completed
The encapsulation of fiber cloth vacuum bag method is vacuumized and is heating and curing, and Cyanate Ester/carbon Fiber Composite plate is made.
High-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape-memory material of the invention, with
Bis-phenol E/A type cyanate ester resin is as matrix resin, using carboxyl-terminated liguid nitrile rubber and flexible-epoxy as toughener, with
Carbon fibre material is reinforced phase.Pass through carboxyl-terminated liguid nitrile rubber and flexible-epoxy toughening cyanate ester resin, abundant body
The compound advantage of cyanate ester resin, carboxyl-terminated liguid nitrile rubber, flexible-epoxy is showed, such as intensity with higher, tough
Property and storage stability and processing performance, it is then that toughening type cyanate ester resin and carbon fiber is compound, resin base can be shown
The outstanding shape-memory properties of body, and the excellent mechanical property of carbon fiber is shown, gained cyanate ester resin/carbon fiber shape note
Composite material is recalled with high tensile, bending strength, shear strength and excellent shape-memory properties, meets application requirement.
The present invention most preferably prepares high-intensitive flexible-epoxy modified cyanic acid ester resin/carbon fiber composite shape
The method of memory material: by carboxyl-terminated liguid nitrile rubber 30g, Jef-0211 flexible-epoxy 20g, bisphenol E-type cyanate
Resin 100g is stirred to react 2h after being heated to 100 DEG C.Resulting prepreg is uniformly brushed in T300 carbon fiber plain cloth
On.Carbon cloth is cut into prescribed level, subsequent laying encapsulates, vacuumizes and be heating and curing.Curing process is 120 DEG C/4h+
150℃/2h+170℃/2h。
Compared with the prior art, technical solution of the present invention bring the utility model has the advantages that
1) flexible-epoxy of the invention modified cyanic acid ester resin/carbon fiber composite shape-memory material cyanate resin
Rouge pours that building body working life is long, being coated with property is good, and prepared Cyanate Ester/carbon Fiber Composite plate surface is smooth, without bright
Aobvious defect.
2) flexible-epoxy of the invention modified cyanic acid ester resin/carbon fiber composite shape-memory material can be used existing
Some composite material process plannings, moulding process are mature, easy to operate.
3) flexible-epoxy of the invention modified cyanic acid ester/carbon fiber composite shape-memory material has deformation quantity
Greatly, the advantages that recovery rate is fast, density is low, strong mechanical performance.
4) flexible-epoxy of the invention modified cyanic acid ester/carbon fiber composite shape-memory material has high stretch by force
Degree, bending strength, shear strength.
5) flexible-epoxy of the invention modified cyanic acid ester resin/carbon fiber composite shape-memory material preparation side
Method is simple, at low cost, is conducive to industrialized production.
Detailed description of the invention
[Fig. 1] is carboxyl-terminated liguid nitrile rubber, flexible-epoxy toughening ester cyanate system in the embodiment of the present invention
System solidifies front and back infrared spectrogram, and a is before solidifying, and b is after solidifying.
[Fig. 2] is cyanate ester resin/carbon fiber composite material of shape memory SEM picture in the embodiment of the present invention.
[Fig. 3] is the stress-strain curve diagram of the embodiment of the present invention, comparative examples.
[Fig. 4] is cyanate ester resin/carbon-fiber composite material shape-memory properties test record figure in the embodiment of the present invention, a
For 0s, b 12s, c 20s, d 24s, the deformed state of material when e is 35s.
Specific embodiment
Below in conjunction with Figure of description and specific preferred example, the invention will be further described, but is not so limited this
The content of invention.
Equipment and instrument employed in implementing below are commercially available.
Shape-memory material is made of following mass component raw material in following embodiment: carboxyl-terminated liguid nitrile rubber 2~4
Part；2~5 parts of flexible-epoxy；8~12 parts of cyanate ester resin；Carbon cloth accounts for composite material of shape memory gross mass
40%~60%.
Following implement in, carboxyl-terminated liguid nitrile rubber come from Jingjiang City Tong Gao Chemical Co., Ltd., molecular weight 3000,
Model: FS260.Bisphenol E-type cyanate comes from Hubei Ju Sheng Science and Technology Ltd.；Jef-0211 flexible-epoxy comes from Changshu
Jia Fa Chemical Co., Ltd., epoxide number are 0.35~0.40.
Embodiment 1
High-intensitive flexible-epoxy modified cyanic acid ester resin/carbon fiber composite shape-memory material preparation method
Are as follows: carboxyl-terminated liguid nitrile rubber 30g, Jef-0211 flexible-epoxy 30g, bisphenol E-type are weighed according to above-mentioned mass fraction
Cyanate ester resin 100g is stirred to react 2h after being heated to 100 DEG C.It is then uniform to brush in about 1m2T300 carbon fiber plain weave
On fabric, carbon fiber plain cloth is then cut into prescribed level by [0/90 °] and [+45 °/- 45 °] direction.With later layer
One layer of alignment is completed, and the carbon cloth that [0/90 °] direction is cut spreads 20 layers, the carbon cloth paving that [+45 °/- 45 °] direction is cut
10 layers.It is encapsulated by vacuum bag method, vacuumizes and be heating and curing to obtain cyanate ester resin/carbon fiber composite material of shape memory plate
Material.Curing process is 120 DEG C/4h+150 DEG C/2h+170 DEG C/2h.
Carboxyl in carboxyl-terminated liguid nitrile rubber, the epoxy group in Jef-0211 flexible-epoxy and bisphenol E-type
Cyanate group reaction solidification in cyanate ester resin obtains cyanate ester resin system.It will be seen from figure 1 that 1737cm-1Place pair
Answer the characteristic absorption peak of CTBN carboxyl, 2238cm-1Place is the absorption peak of cyano (- CN).In the infrared spectrogram of cyanate, it is located at
1735cm-1The epoxy group absorption peak at place is located at 2270cm-1And 2238cm-1The strong absworption peak at place is cyanic acid ester group (- OCN) respectively
With the absorption peak of cyano (- CN), fade away with curing reaction, while in 1570cm-1、1370cm-1Place occurs new
Peak, respectively correspond C-N the and C=N structure in triazine ring.Positioned at 1735cm-1The carboxyl absorption peak at place fades away, explanation
CTBN, Jef-0211 flexible-epoxy are reacted with bisphenol E-type cyanate resin, in addition, sample infrared light after solidification
Spectrogram is in 1210cm-1Ester group characteristic absorption peak is generated with place.Figure it is seen that between cyanate ester resin matrix and carbon fiber
It is tightly combined, CTBN is also precipitated from cyanate ester resin matrix, is evenly distributed in cyanate ester resin matrix with island structure.
Cyanate ester resin obtained/carbon fiber composite material of shape memory carbon cloth content through the invention is about
50%~56%.The glass transition temperature of material is 150 DEG C, and material has preferable good mechanical property and excellent shape
Shape memory performance.Tensile strength about 579MPa, Young's modulus about 36.7GPa, bending strength 711MPa, bending modulus are
44.7GPa, interlaminar shear strength 44MPa, shape fixed rate about 97%, about 98% elongation at break of shape recovery rate are
2.06%.Figure 4, it is seen that cyanate ester resin/shape note of carbon fiber composite material of shape memory completion one time is made to obtain
Recall recovery and takes around 35s.
Comparative examples
High-intensitive flexible-epoxy modified cyanic acid ester resin/carbon fiber composite shape-memory material preparation method
Are as follows: carboxyl-terminated liguid nitrile rubber 30g, bisphenol E-type cyanate 100g are weighed according to above-mentioned mass fraction, after being heated to 100 DEG C
It is stirred to react 2h.It is then uniform to brush in about 1m2T300 carbon fiber plain cloth on, then carbon fiber plain cloth is pressed
[0/90 °] and [+45 °/- 45 °] direction is cut into prescribed level.Then alignment is completed in layer, what [0/90 °] direction was cut
Carbon cloth spreads 20 layers, and the carbon cloth that [+45 °/- 45 °] direction is cut spreads 10 layers.It is encapsulated by vacuum bag method, vacuumizes and add
Heat cure obtains cyanate ester resin/carbon fiber composite material of shape memory plate.Curing process is 120 DEG C/4h+150 DEG C/2h+
170℃/2h。
Cyanate ester resin obtained/carbon fiber composite material of shape memory carbon cloth content through the invention is about
40%~60%.The glass transition temperature of material is 180 DEG C, and material has preferable good mechanical property and excellent shape
Shape memory performance.Tensile strength about 541MPa, Young's modulus about 34.2GPa, bending strength 601MPa, bending modulus are
40.1GPa, interlaminar shear strength 48MPa, shape fixed rate about 97%, shape recovery rate about 98%, elongation at break are
2.35%.
Claims (9)
1. a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape-memory material, feature exist
In: it is combined by carbon fibre material reinforced phase and modified cyanic acid ester resin matrix；
The modified cyanic acid ester resin matrix includes following mass component:
2~4 parts of carboxyl-terminated liguid nitrile rubber；
2~5 parts of flexible-epoxy；
8~12 parts of cyanate ester resin.
2. a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape according to claim 1
Shape memory material, it is characterised in that: the cyanate ester resin includes bisphenol E-type cyanate resin and/or bisphenol A cyanate ester tree
Rouge.
3. a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape according to claim 1
Shape memory material, it is characterised in that: the molecular weight of the carboxyl-terminated liguid nitrile rubber is 2000~5000.
4. a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape according to claim 1
Shape memory material, it is characterised in that: the flexible-epoxy includes at least one in Jef-0211, Jew-0114, Jef-0213
Kind.
5. a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape according to claim 1
Shape memory material, it is characterised in that: the carbon fibre material accounts for cyanate ester resin/total matter of carbon fiber composite shape-memory material
The 40%~60% of amount.
6. a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape according to claim 5
Shape memory material, it is characterised in that: the carbon fibre material is T300 carbon fiber plain cloth, NIMKT carbon fibre fabric or SKO
Carbon fibre fabric.
7. a kind of described in any item high-strength flexible cyanate ester modified with epoxy resin/carbon fibers of claim 1~6 are compound
The preparation method of type shape-memory material, it is characterised in that: by cyanate ester resin, carboxyl-terminated liguid nitrile rubber and flexible epoxy
Resin heating stirring carries out prepolymerization, obtains pouring building body；It is true coated in carrying out behind carbon fibre material surface that gained pours building body
Empty heat cure to get.
8. a kind of high-strength flexible cyanate ester modified with epoxy resin/carbon fiber composite shape according to claim 7
The preparation method of shape memory material, it is characterised in that: the temperature of the prepolymerization is 90~100 DEG C, and the time is 1~2 small
When.
9. a kind of flexible-epoxy modified cyanic acid ester resin/carbon fiber composite of high intensity according to claim 7
The preparation method of shape-memory material, it is characterised in that: the thermosetting turns to temperature programming solidification: at 120~125 DEG C, heat preservation 3
~4h；At 150~155 DEG C, 1~2h is kept the temperature；At 170~175 DEG C, 1~2h is kept the temperature.
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| CN113087852A (en) * | 2021-04-26 | 2021-07-09 | 中国科学院兰州化学物理研究所 | Cyanate ester shape memory polymer material capable of being printed in 4D mode, preparation method of cyanate ester shape memory polymer material, cyanate ester shape memory polymer device and application of cyanate ester shape memory polymer device |
| JP2022170112A (en) * | 2021-04-28 | 2022-11-10 | 株式会社イノアックコーポレーション | Fiber-reinforced molding, method for manufacturing fiber-reinforced molding, and resin sheet |
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| JP2022170112A (en) * | 2021-04-28 | 2022-11-10 | 株式会社イノアックコーポレーション | Fiber-reinforced molding, method for manufacturing fiber-reinforced molding, and resin sheet |
| JP7419291B2 (en) | 2021-04-28 | 2024-01-22 | 株式会社イノアックコーポレーション | Method for manufacturing fiber-reinforced molded body, resin sheet, and method for manufacturing resin sheet |
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