CN103980666B - A kind of high-toughness epoxy resin compositions suitable in RTM technique and preparation method - Google Patents
A kind of high-toughness epoxy resin compositions suitable in RTM technique and preparation method Download PDFInfo
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Abstract
The present invention provides a kind of RTM of being not only suitable for technique to have again the composition epoxy resin of high tenacity and higher-strength.The preparation method that the present invention also provides for above-mentioned composition epoxy resin.It at room temperature by diethyl toluene diamine and polyetheramine D-230 mix homogeneously, is configured to the B component liquid curing-agent that the D-230 mass fraction containing polyetheramine is 20%～90%；Then by component A epoxy resin and B component liquid curing-agent vacuum removal bubble at 30 DEG C～40 DEG C；Adopt RTM injector by component A: the quality of B component=100:25～50, than mix homogeneously, is re-introduced into mould temperature and solidifies in the RTM mold of 30 DEG C～40 DEG C, can obtain the epoxy resin cured product of high tenacity.RTM operating procedure window at the composition epoxy resin of the present invention 30～45 DEG C, more than 138min, is suitable to RTM technological forming；Composition epoxy resin viscosity is low, it is not necessary to use diluent, defoamer etc.；The cured product of composition epoxy resin has high tenacity.
Description
Technical field
The present invention relates to a kind of high-toughness epoxy resin composition and method of making the same suitable in RTM technique, specifically, the present invention relates to and a kind of there is under process operation temperatures relatively low initial viscosity and longer RTM process window, and there is the composition epoxy resin of high tenacity and higher-strength and preparation method thereof.
Background technology
Resin transfer moulding, it is infuse resin into the composite material process planning method of infiltration reinforcing material curing molding in Guan Bi mould also referred to as RTM technique, have that surface size precision height, product entirety dead size molding, porosity be low, shaping efficiency advantages of higher, be widely used in the fields such as Aero-Space, boats and ships, automobile.Fiber is only had a step impregnation process by the resin in RTM technique, therefore it is required that resin has relatively low viscosity at the working temperature (generally answers < 1Pa s, ideally < 0.5Pa s) and longer process window, to meet resin flowing mold filling and the infiltration to fiber.It is also required that resin has higher mechanical property.
Epoxy resin due to after solidifying the weakness such as matter is crisp, impact resistance is poor, easy cracking seriously constrain its application in high tenacity occasion.Come toughness reinforcing typically via adding the method such as elastomer, thermoplastic granulates in epoxy resin-base, but adopt this type of method to there are problems in RTM technique, because fiber preform act as filter, filtered out these granules when resin flows into fibre bundle.Meanwhile, the granule of interpolation causes that resin viscosity significantly increases, and will substantially suppress the resin infiltration to fiber.Therefore the low viscosity technological requirement of RTM so that the toughness reinforcing of RTM epoxy resin encounters more challenge.
RTM epoxy resin toughness conventional both at home and abroad at present is generally poor, and its fracture elongation is little, and impact flexibility is low.Fracture elongation only 1.9% such as the RTM epoxy-resin systems PR500 of 3M company exploitation.The fracture elongation of the RTM epoxy-resin systems RTM6 that Hexcel releases is 3.4%[Crewe Ken Bahe, Pei Dun；Aero-Space composite material structural member resin transfer molding technology, Beijing: 2009.12].Beijing Research Inst. of Aeronautic Material uses the firming agent of long-chain and the bisphenol A epoxide resin toughening modifying TDE-85/ methyl hexahydrophthalic anhydride system of long-chain simultaneously, and its fracture elongation modified only brings up to 1.95%[Zhao Sheng dragon, Li Hongyun, Zheng Ruiqi from 0.92%；Material engineering, 2001:111-117]；Adopt good 830 epoxy resin of toughness and long chain type toughening agent modified after, its fracture elongation also only increases to 2.5%[Zhao Sheng dragon, Li Hongyun, Zheng Ruiqi；NCCM-13:498-503].After Northwestern Polytechnical University adopts BMI/diallyl phenyl compound toughening modifying TDE-85/MNA anhydride system, its impact flexibility only 11.3KJ/m2[Gu beautiful woman is beautiful, Liang Guozheng, Lan Liwen；Polymer material science and engineering, 1996 (2): 43-47].After Aviation Industry of China Jinan unique construction institute adopts linear bisphenol-A Toughening Epoxy Resin TDE-90 epoxy resin, its impact flexibility is only by 8.25KJ/m2Bring up to 9.82KJ/m2[Tang Qiming；Fibrous composite, 2001 (3): 13-14].The fracture elongation of modified bisphenol A epoxy/modified amine system that Beijing glass steel institute compound Materials Co., Ltd prepares by common bisphenol A epoxide resin carries out toughening modifying is up to 5.7%, but its intensity, modulus and glass transition temperature [Lv Jinyan, Wang Lei, bavin Fructus Mume on the low side；About Frp/cm, 2008 (4): 16-18].The fracture elongation that Zhuzhou Times new materials Science Co., Ltd carries out, by CYD-128 epoxy resin and high-performance epoxy resin, the modified CYD-128/ liquid amine system that Blending Toughening Modification prepares reaches 5.3%, but its intensity, modulus and glass transition temperature relatively low [CN101880443A].
In summary, the toughness of the RTM epoxy resin of current toughening modifying improves limited, but even if or toughness improve its intensity more, modulus and glass transition temperature etc. and reduce more, it is difficult to meet the field such as Aero-Space, cryogenic engineering to RTM epoxy resin in the requirement being maintained with higher-strength, modulus and glass transition temperature obtaining high tenacity.
Summary of the invention
Present invention aim at the composition epoxy resin providing a kind of RTM of being not only suitable for technique to have again high tenacity and higher-strength.Another object of the present invention is in that the preparation method providing above-mentioned composition epoxy resin.
A kind of high-toughness epoxy resin compositions suitable in RTM technique of the present invention, it is characterised in that: this composition epoxy resin is made up of two components of A and B, and the mass ratio of component A and B component is 100:25～50；
Described component A is the one in 830 epoxy resin, AFG-90 epoxy resin, TDE-85 epoxy resin or its combination；
Described B component is liquid curing-agent；This firming agent is made up of diethyl toluene diamine and polyetheramine D-230, and wherein polyetheramine D-230 accounts for firming agent mass percent is 20%～90%.
A kind of high-toughness epoxy resin compositions suitable in RTM technique as above, its described AFG-90 epoxy resin is triglycidyl group para-aminophenol epoxy resin.
A kind of high-toughness epoxy resin compositions suitable in RTM technique as above, its described TDE-85 epoxy resin is the epoxy resin having alicyclic epoxy and (+)-2,3-Epoxy-1-propanol epoxy-type epoxy double characteristic concurrently.
A kind of high-toughness epoxy resin compositions suitable in RTM technique as above, its described diethyl toluene diamine is the aromatic amine curing agent that contained two amidos are all directly connected with aromatic radical.
The preparation method of a kind of high-toughness epoxy resin compositions suitable in RTM technique of the present invention, it comprises the steps:
(1) at room temperature by diethyl toluene diamine and polyetheramine D-230 mix homogeneously, it is configured to the B component liquid curing-agent that the D-230 mass fraction containing polyetheramine is 20%～90%；
(2) then at 30 DEG C～40 DEG C by component A epoxy resin and B component liquid curing-agent vacuum removal bubble；
(3) adopt RTM injector by component A: the quality of B component=100:25～50 compares mix homogeneously, it is re-introduced into mould temperature to solidify in the RTM mold of 30 DEG C～40 DEG C, can obtaining the epoxy resin cured product of high tenacity, described high tenacity refers to that fracture elongation is 5～8.5%.
The preparation method of a kind of high-toughness epoxy resin compositions suitable in RTM technique as above, in its step (3), curing process is for being first warming up to 80 DEG C of insulation 1h, then heats to 100 DEG C of insulation 2h, is finally warming up to 130 DEG C of insulation 2h.
Effect of the invention is that: the present invention utilizes the mixed curing agent that the diethyl toluene diamine containing phenyl ring and the D-230 containing flexible polyether segments form to react with epoxy resin, generate not only containing rigid chain segment but also the curable epoxide thing containing soft segment, in conjunction with appropriate solidification temperature so that it is be maintained with higher intensity, modulus and glass transition temperature toughness reinforcing.Diethyl toluene diamine viscosity is relatively big simultaneously, and the addition of low viscous polyetheramine D-230 can make this epoxy-resin systems have relatively low viscosity and longer process window, thus meeting the requirement of RTM technique.
Composition epoxy resin provided by the present invention and preparation method thereof has the advantage that the RTM operating procedure window at the composition epoxy resin 30～45 DEG C of (1) present invention is more than 138min, is suitable to RTM technological forming；(2) the composition epoxy resin viscosity of the present invention is low, it is not necessary to use diluent, defoamer etc.；(3) cured product of the composition epoxy resin of the present invention has high tenacity (5.0%～8.5%, impact flexibility is 31KJ/m to its fracture elongation2～55KJ/m2)；(4) cured product of the composition epoxy resin of the present invention has higher intensity (its hot strength reaches 76MPa～85MPa), modulus (stretch modulus >=3.0GPa) and glass transition temperature (Tg is at 85 DEG C～115 DEG C).
Detailed description of the invention
A kind of high-toughness epoxy resin compositions suitable in RTM technique of the present invention and preparation method is further illustrated below by specific embodiment and comparative example.
Embodiment 1
At room temperature by 19 parts of diethyl toluene diamines and 10 parts of polyetheramine D-230 stirrings, it is uniformly mixed into the B component liquid curing-agent that the D-230 mass fraction containing polyetheramine is 34%；
Then by component A 830 epoxy resin and B component liquid curing-agent vacuum removal bubble at 40 DEG C；
Adopt RTM injector by component A: the quality of B component=100:29, than mix homogeneously, reinjects in the RTM mold that mould temperature is 35 DEG C, solidify by 80 DEG C/1h+100 DEG C/2h+130 DEG C/2h, epoxy resin cured product can be obtained.
RTM operating procedure window at this embodiment epoxy resin compositions 35 DEG C is 148min (viscosity < 1Pa s).The fracture elongation of this epoxy resin-cured product is 5.0%, and impact flexibility is 53.8KJ/m2, its hot strength is 77.6MPa simultaneously, and stretch modulus is 3.1GPa, and glass ring transition temperature Tg is 89 DEG C.Other performance data is in Table one.
Embodiment 2
At room temperature 15 parts of diethyl toluene diamines and 15 parts of polyetheramine D-230 are stirred, be mixed into containing the B component liquid curing-agent that D-230 mass fraction is 50%；
Then by component A 830 epoxy resin and B component liquid curing-agent vacuum removal bubble at 35 DEG C；
Adopt RTM injector by component A: the quality of B component=100:30, than mix homogeneously, reinjects in the RTM mold that mould temperature is 38 DEG C, solidify by 80 DEG C/1h+100 DEG C/2h+130 DEG C/2h, epoxy resin cured product can be obtained.
This embodiment epoxy resin compositions RTM operating procedure window at 35 DEG C is 140min (viscosity < 1Pa s).The fracture elongation of this epoxy resin-cured product is 8.3%, and impact flexibility is 41.5KJ/m2, its hot strength is 76.2MPa simultaneously, and stretch modulus is 3.0GPa, and glass ring transition temperature Tg is 85 DEG C.Other performance data is in Table one.
Embodiment 3
At room temperature 11 parts of diethyl toluene diamines and 20.5 parts of polyetheramine D-230 are stirred, be mixed into containing the B component liquid curing-agent that D-230 mass fraction is 65%；
Then by component A 830 epoxy resin and B component liquid curing-agent vacuum removal bubble at 30 DEG C；
Adopt RTM injector by component A: the quality of B component=100:31.5, than mix homogeneously, reinjects in the RTM mold that mould temperature is 35 DEG C, solidify by 80 DEG C/1h+100 DEG C/2h+130 DEG C/2h, epoxy resin cured product can be obtained.
This embodiment epoxy resin compositions RTM operating procedure window at 35 DEG C is 139min (viscosity < 1Pa s).The fracture elongation of this epoxy resin-cured product is 5.8%, and impact flexibility is 31.3KJ/m2, its hot strength is 79.3MPa simultaneously, and stretch modulus is 3.1GPa, and glass ring transition temperature Tg is 89 DEG C.Other performance data is in Table one.
Embodiment 4
At room temperature 16.8 parts of diethyl toluene diamines and 30 parts of polyetheramine D-230 are stirred, be mixed into containing the B component liquid curing-agent that D-230 mass fraction is 64%；
Then by component A AFG-90 epoxy resin and B component liquid curing-agent vacuum removal bubble at 40 DEG C；
Adopt RTM injector by component A: the quality of B component=100:46.8, than mix homogeneously, reinjects in the RTM mold that mould temperature is 38 DEG C, solidify by 80 DEG C/1h+100 DEG C/2h+130 DEG C/2h, epoxy resin cured product can be obtained.
This embodiment epoxy resin compositions RTM operating procedure window at 35 DEG C is 142min (viscosity < 1Pa s).The fracture elongation of this epoxy resin-cured product is 5.6%, and impact flexibility is 33.9KJ/m2, its hot strength is 82.8MPa simultaneously, and stretch modulus is 3.3GPa, and glass ring transition temperature Tg is 112 DEG C.Other performance data is in Table one.
Embodiment 5
At room temperature 8.9 parts of diethyl toluene diamines and 40 parts of polyetheramine D-230 are stirred, be mixed into containing the B component liquid curing-agent that D-230 mass fraction is 82%；
Then by component A AFG-90 epoxy resin and B component liquid curing-agent vacuum removal bubble at 40 DEG C；
Adopt RTM injector by component A: the quality of B component=100:48.9, than mix homogeneously, reinjects in the RTM mold that mould temperature is 35 DEG C, solidify by 80 DEG C/1h+100 DEG C/2h+130 DEG C/2h, epoxy resin cured product can be obtained.
RTM operating procedure window at this embodiment epoxy resin compositions 35 DEG C is 140min (viscosity < 1Pa s).The fracture elongation of this epoxy resin-cured product is 5.6%, and impact flexibility is 36.8KJ/m2, its hot strength is 79.1MPa simultaneously, and stretch modulus is 3.2GPa, and glass ring transition temperature Tg is 103 DEG C.Other performance data is in Table one.
Embodiment 6
At room temperature 21.2 parts of diethyl toluene diamines and 21.2 parts of polyetheramine D-230 are stirred, be mixed into containing the B component liquid curing-agent that D-230 mass fraction is 50%；
60 parts of TDE-85 epoxy resin and 40 part of 830 epoxy resin are uniformly mixed into component A epoxy resin；
Then by component A epoxy resin and B component liquid curing-agent vacuum removal bubble at 35 DEG C；
Adopt RTM injector by component A: the quality of B component=100:42.4, than mix homogeneously, is re-introduced in the RTM mold that mould temperature is 30 DEG C, solidify by 80 DEG C/1h+100 DEG C/2h+130 DEG C/2h, epoxy resin cured product can be obtained.
RTM operating procedure window at this embodiment epoxy resin compositions 35 DEG C is 145min (viscosity < 1Pa s).The fracture elongation of this epoxy resin-cured product is up to 5.6%, and impact flexibility is up to 31.6KJ/m2, its hot strength is 82.2MPa simultaneously, and stretch modulus is 3.3GPa, and glass ring transition temperature Tg is 108 DEG C.Other performance data is in Table one.
Comparative example
We, by inquiring about document, choose the good RTM epoxy resin of toughening effect and contrast.The impact flexibility only 11.3KJ/m of the TDE-85/MNA anhydride system after Northwestern Polytechnical University is toughness reinforcing2；The impact flexibility of the TDE-90 epoxy-resin systems after Aviation Industry of China Jinan unique construction institute is toughness reinforcing only increases to 9.82KJ/m2；All significantly lower than the notched bar impact strength of six embodiments of the present invention.The fracture elongation of the modified bisphenol A after Beijing glass steel institute compound Materials Co., Ltd's toughening modifying/modified amine system is higher (5.7%)；But its hot strength (70.3MPa), modulus (2.8GPa) and Tg (76 DEG C) are relatively low, are below the analog value of six embodiments of the present invention, as shown in Table 1.The fracture elongation higher (5.3%) of the modified CYD-128/ liquid amine system of Zhuzhou Times new materials Science Co., Ltd；But its hot strength (68MPa) and bending strength (99MPa) are relatively low, Tg only about 61 DEG C, all significantly lower than the analog value of six embodiments of the present invention, as shown in Table 1.
The performance comparison of each embodiment of table one and comparative example
The above, be only the specific embodiment of the present invention, it is impossible to the present invention is defined to the content described by description.The present invention, in the technical scope that the invention discloses, is carried out the various change readily occurred in or change, should be encompassed within protection scope of the present invention by any those familiar with the art.
Claims (6)
1. the high-toughness epoxy resin compositions being applicable to RTM technique, it is characterised in that: this composition epoxy resin is made up of two components of A and B, and the mass ratio of component A and B component is 100:25～50；
Described component A is the one in 830 epoxy resin, AFG-90 epoxy resin, TDE-85 epoxy resin or its combination；
Described B component is liquid curing-agent；This firming agent is made up of diethyl toluene diamine and polyetheramine D-230, and wherein polyetheramine D-230 accounts for firming agent mass percent is 20%～90%.
2. a kind of high-toughness epoxy resin compositions suitable in RTM technique according to claim 1, it is characterised in that: described AFG-90 epoxy resin is triglycidyl group para-aminophenol epoxy resin.
3. a kind of high-toughness epoxy resin compositions suitable in RTM technique according to claim 1, it is characterised in that: described TDE-85 epoxy resin is the epoxy resin having alicyclic epoxy and glycidyl ester type epoxy double characteristic concurrently.
4. a kind of high-toughness epoxy resin compositions suitable in RTM technique according to claim 1, it is characterised in that: described diethyl toluene diamine is the aromatic amine curing agent that contained two amidos are all directly connected with aromatic radical.
5. the preparation method of the high-toughness epoxy resin compositions being applicable to RTM technique described in a Claims 1-4 any one, it is characterised in that: the method comprises the steps:
(1) at room temperature by diethyl toluene diamine and polyetheramine D-230 mix homogeneously, it is configured to the B component liquid curing-agent that the D-230 mass fraction containing polyetheramine is 20%～90%；
(2) then at 30 DEG C～40 DEG C by component A epoxy resin and B component liquid curing-agent vacuum removal bubble；
(3) adopt RTM injector by component A: the quality of B component=100:25～50 compares mix homogeneously, it is re-introduced into mould temperature to solidify in the RTM mold of 30 DEG C～40 DEG C, can obtaining the epoxy resin cured product of high tenacity, described high tenacity refers to that fracture elongation is 5～8.5%.
6. the preparation method of a kind of high-toughness epoxy resin compositions suitable in RTM technique according to claim 5, it is characterized in that: in step (3), curing process is for being first warming up to 80 DEG C of insulation 1h, then heat to 100 DEG C of insulation 2h, be finally warming up to 130 DEG C of insulation 2h.
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| CN106751819A (en) * | 2016-11-23 | 2017-05-31 | 江苏恒神股份有限公司 | A kind of RTM techniques cyanate resin composition and preparation method |
| CN108753100B (en) * | 2018-05-03 | 2020-05-05 | 东南大学 | Water-based epoxy concrete repairing interface agent and preparation method thereof |
| CN112143339A (en) * | 2020-09-29 | 2020-12-29 | 中国科学院长春应用化学研究所 | Epoxy resin coating for shipboard aircraft and preparation method thereof |
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