CN105219046A - Intermediate temperature setting is wound around resin and preparation method thereof, gained is wound around one-way slabs - Google Patents
Intermediate temperature setting is wound around resin and preparation method thereof, gained is wound around one-way slabs Download PDFInfo
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- CN105219046A CN105219046A CN201510561304.XA CN201510561304A CN105219046A CN 105219046 A CN105219046 A CN 105219046A CN 201510561304 A CN201510561304 A CN 201510561304A CN 105219046 A CN105219046 A CN 105219046A
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Abstract
The invention provides a kind of intermediate temperature setting and be wound around resin and preparation method thereof, gained winding one-way slabs, this intermediate temperature setting is wound around resin and comprises resin portion, toughner part and curing agent part, the massfraction of resin portion is 30 ~ 60%, the massfraction of toughner part is 3 ~ 10%, and the massfraction of curing agent part is 40 ~ 70%; The glass transition temperature Tg of prepared intermediate temperature setting winding resin is higher, can reach 240 DEG C, thus solves in aviation field and be wound around product to the resistant to elevated temperatures requirement of resin, and the modest viscosity of this resin, is applicable to winding process simultaneously; In addition this resin has sufficiently long working life, and the adaptive phase under technological temperature reaches 7 ~ 18h, adds technique fault-tolerant.This resin is solidification value 70 ~ 100 DEG C just, and after after fixing, product heat resistance is good.
Description
Technical field
The present invention relates to a kind of intermediate temperature setting and be wound around resin and preparation method thereof, gained winding one-way slabs.
Background technology
Filament-wound Machine is the processing method that resin matrix composite material product molding is conventional.This method is designed by the mechanics of materials, can give full play to the characteristic that tensile strength of fiber is high.Have the advantages such as specific tenacity is high, corrosion-resistant, cost is low, steady quality due to Filament-wound Machine goods, and be easy to realize mechanize, automatization, production efficiency is high, because application is very extensive.At present at the winding product that aerospace field makes, by the restriction of solidification value, heatproof level is general lower, causes and much requires that strict product cannot use winding process to make to heatproof.
Therefore, need now to develop a kind of intermediate temperature setting resistant to elevated temperatures, be applicable to the resin material of winding process product.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of intermediate temperature setting, and heat resistance is excellent, product long service life, is applicable to resin of winding process use and preparation method thereof, obtained ring-wound testpieces.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of intermediate temperature setting is wound around resin, comprise resin portion, toughner part and curing agent part, the massfraction of described resin portion is 30 ~ 60%, and the massfraction of described toughner part is 3 ~ 10%, and the massfraction of described curing agent part is 40 ~ 70%;
Described resin portion is one or more in polyester vinyl ester resin, bimaleimide resin, epoxy resin, unsaturated polyester, resol, cyanate ester resin;
The component of described toughner part is one or more in mineral filler, synthetic rubber, thermoplastic resin, flexible chain solidifying agent;
The component of described curing agent part is one or more in amine, anhydrides, imidazoles, metallic salt, linear resin oligopolymer class or their derivative.
Further, the massfraction of described resin portion is 40 ~ 60%, and the massfraction of described toughner part is 5 ~ 10%, and the massfraction of described curing agent part is 40 ~ 60%.
Further, the glass transition temperature Tg that resin Composition adopts differentia scanning calorimetry DSC to record is 170 ~ 280 DEG C, and the glass transition temperature Tg adopting dynamic properties analytical method DMA to record after solidification is 170 ~ 250 DEG C.
Further, following steps preparation is adopted:
Step 1: at normal temperatures, takes resin portion and toughner part by weight ratio, dissolves rear and abundant stirring and makes it mix;
Step 2: at 70 ~ 90 DEG C of temperature, constantly stirs 30 ~ 60min by the hybrid resin in step 1, and being cooled to normal temperature acquisition resin viscosity is 300 ~ 800Cps;
Step 3: at normal temperatures, takes described curing agent part by weight ratio, and is fully uniformly mixed;
Step 4: at normal temperatures, takes the resin portion of step 2 and the curing agent part of step 3 by weight ratio, is fully uniformly mixed, and can obtain the resistant to elevated temperatures winding resin system of intermediate temperature setting.
Adopt technique scheme, the resin obtained has higher second-order transition temperature, and its Tg can reach 170 ~ 280 DEG C, thus solves aviation field product to the resistant to elevated temperatures requirement of resin, and its modest viscosity, can be used for winding process; Resin sufficiently long working life, adds technique fault-tolerant simultaneously.
Resin portion is one or more the mixture in polyester vinyl ester resin, bimaleimide resin, epoxy resin, unsaturated polyester, resol, cyanate ester resin.Wherein, processing characteristics and the epoxy resin of cyanate ester resin are close, cyanate ester resin and the copolymerization such as epoxy resin, unsaturated polyester can be improved thermotolerance and the mechanical property of material; Resol has good high thermal resistance, and the resol after crosslinked can resist the decomposition of any chemical substance, resol and other resin copolymerization can be improved thermotolerance and the chemical resistance of material.
The component of toughner part is one or more the mixture in mineral filler, synthetic rubber, thermoplastic resin, flexible chain solidifying agent.Mineral filler, rubber, thermoplastic resin can form two phase structure with epoxy resin and reach toughness reinforcing object; Thermoplastics can also form semi-interpenetrating network type polymkeric substance continuously and come toughness reinforcing in epoxy networks; Introduce flexible chain, the chemical structure composition of cross-linked network can be changed, to improve the mobility of cross-linked network.
The component of curing agent part is one or more the mixture in amine, anhydrides, imidazoles, metallic salt, linear resin oligopolymer class or their derivative.The mechanical property, thermotolerance, water tolerance, erosion resistance etc. of selection to the resin obtained after crosslinking reaction of curing agent part kind all have a significant impact.Epoxy resin uses the solidifying agent such as aliphatic amide, alicyclic hydrocarbon and polymeric amide can obtain good thermotolerance often in middle low-temperature curing; Aliphatic polyamine solidifying agent cementability and alkaline-resisting, water tolerance is all excellent.Aromatic polyamine is also excellent in resistance to chemical reagents.Because the nitrogen element of amino and metal form hydrogen bond, thus there is excellent rust-proof effect.Amine mass concentration is higher, and rust-proof effect better; Anhydride curing agent and epoxy resin can form ester bond, improve resin to the resistibility of organic acid and mineral acid and electric property.
The second-order transition temperature (Tg) that resin Composition adopts differentia scanning calorimetry (DSC) to record is 170 ~ 280 DEG C, and the second-order transition temperature (Tg) adopting dynamic properties analytical method (DMA) to record after solidification is 170 ~ 250 DEG C.
A preparation method for intermediate temperature setting winding resin, concrete steps are as follows:
Step 1: at normal temperatures, with the massfraction of resin portion be 30 ~ 60%, the massfraction of toughner part is 3 ~ 10% take resin portion and toughner part, fully stir and make it mix after dissolving;
Step 2: at 70 ~ 90 DEG C of temperature, constantly stirs 30 ~ 60min by the hybrid resin in step 1, and being cooled to normal temperature acquisition resin viscosity is 300 ~ 800Cps;
Step 3: at normal temperatures, is 40 ~ 70% take described curing agent part with the massfraction of curing agent part, and is fully uniformly mixed;
Step 4: at normal temperatures, takes the resin portion of step 2 and the curing agent part of step 3 by weight ratio, is fully uniformly mixed, and can obtain the resistant to elevated temperatures winding resin system of intermediate temperature setting.
The method gained resin viscosity is moderate; After post curing treatment, effectively can eliminate internal stress; Prepared middle temperature is wound around resin, and the working life under technological temperature reaches 7 ~ 18h.
Further, described resin portion is one or more in polyester vinyl ester resin, bimaleimide resin, epoxy resin, unsaturated polyester, resol, cyanate ester resin;
The component of described toughner part is one or more in mineral filler, synthetic rubber, thermoplastic resin, flexible chain solidifying agent;
The component of described curing agent part is one or more in amine, anhydrides, imidazoles, metallic salt, linear resin oligopolymer class or their derivative.
Further, the glass transition temperature Tg that resin Composition adopts differentia scanning calorimetry DSC to record is 170 ~ 280 DEG C, and the glass transition temperature Tg adopting dynamic properties analytical method DMA to record after solidification is 170 ~ 250 DEG C.
A kind of winding one-way slabs, adopt above-mentioned intermediate temperature setting to be wound around resin and adopt winding process to obtain, this one-way slabs is after post curing treatment, and glass transition temperature Tg is 150 ~ 250 DEG C; Interlaminar shear strength is at 50MPa-150MPa, and tensile strength is at 1000MPa-3000MPa, and tensile modulus is at 70GPa-170GPa.
Further, one-way slabs is after post curing treatment, and glass transition temperature Tg is 180 ~ 240 DEG C; Interlaminar shear strength is at 60Mpa-120MPa, and tensile strength is at 1800MPa-2800MPa, and tensile modulus is at 100GPa-170GPa.
Adopt technical scheme of the present invention, its beneficial effect produced is: the glass transition temperature Tg of prepared intermediate temperature setting winding resin is higher, 240 DEG C can be reached, thus solve in aviation field and be wound around product to the resistant to elevated temperatures requirement of resin, the modest viscosity of this resin, is applicable to winding process simultaneously; In addition this resin has sufficiently long working life, and the adaptive phase under technological temperature reaches 7 ~ 18h, adds technique fault-tolerant.This resin is solidification value 70 ~ 100 DEG C just, and after after fixing, product heat resistance is good.
Accompanying drawing explanation
Fig. 1 is the DSC phenogram of embodiment of the present invention intermediate temperature setting winding resin.
Embodiment
The preferred embodiments of the present invention are described in detail below in conjunction with accompanying drawing.
Embodiment resin is after intermediate temperature setting, and glass transition temperature Tg is higher, can reach 170 ~ 280 DEG C, and as Fig. 1, thus solve in aviation field that product is to the resistant to elevated temperatures requirement of resin, the modest viscosity of this resin, is applicable to winding process simultaneously; In addition this intermediate temperature setting winding resin has sufficiently long working life, adds technique fault-tolerant; This intermediate temperature setting winding resin is solidification value 70 ~ 100 DEG C just, and after after fixing, product heat resistance is good.
Comparative example
The resin portion selected is multifunction group epoxy mixture, and its massfraction accounting for total system is 48%, and the curing agent part selected is the mixture of acid anhydrides and Tertiary amine accelerators, and its massfraction accounting for total system is respectively 50.8% and 1.2%; Concrete preparation process is as follows:
Step 1: at normal temperatures, takes resin portion by weight ratio and fully stirs and make it mix.
Step 2: at normal temperatures, takes curing agent part by weight ratio, and is fully uniformly mixed;
Step 3: at normal temperatures, takes the resin portion of step 1 and the curing agent part of step 2 by weight ratio, is fully uniformly mixed.
Select T700S fiber and this resin system, adopt winding process to make one-way slabs.
Embodiment 1
The resin portion selected is multifunction group epoxy mixture, its massfraction accounting for total system is 47%, the toughner part selected is synthetic rubber class, its massfraction accounting for total system is 3%, the curing agent part selected is the mixture of acid anhydrides and imidazoles, and its massfraction accounting for total system is respectively 49.45% and 0.55%; Concrete preparation process is as follows:
Step 1: at normal temperatures, takes resin portion and toughner part by weight ratio, dissolves rear and abundant stirring and makes it mix.
Step 2: at 70 ~ 90 DEG C of temperature, by step: the hybrid resin in 1 constantly stirs 30 ~ 60min, being cooled to normal temperature acquisition resin viscosity is 300 ~ 800Cps.
Step 3: at normal temperatures, takes curing agent part by weight ratio, and is fully uniformly mixed;
Step 4: at normal temperatures, takes the resin portion of step 2 and the curing agent part of step 3 by weight ratio, is fully uniformly mixed, and can obtain the resistant to elevated temperatures winding resin system of intermediate temperature setting.
Select T700S fiber and this resin system, adopt winding process to make one-way slabs.
Embodiment 2
The resin portion selected is multifunction group epoxy mixture, its massfraction accounting for total system is 45%, the toughner part selected is synthetic rubber class, its massfraction accounting for total system is 8%, the curing agent part selected is the mixture of acid anhydrides and imidazoles, and its massfraction accounting for total system is respectively 46.49% and 0.51%
Concrete preparation process is as follows:
Step 1: at normal temperatures, takes resin portion and toughner part by weight ratio, dissolves rear and abundant stirring and makes it mix;
Step 2: at 70 ~ 90 DEG C of temperature, constantly stirs 30 ~ 60min by the hybrid resin in step 1, and being cooled to normal temperature acquisition resin viscosity is 300 ~ 800Cps;
Step 3: at normal temperatures, takes curing agent part by weight ratio, and is fully uniformly mixed;
Step 4: at normal temperatures, takes the resin portion of step 2 and the curing agent part of step 3 by weight ratio, is fully uniformly mixed, and can obtain the resistant to elevated temperatures winding resin system of intermediate temperature setting.
Select T700S fiber and this resin system, adopt winding process to make one-way slabs.
Embodiment 3
The resin portion selected is multifunction group epoxy mixture, its massfraction accounting for total system is 46%, the toughner part selected is synthetic rubber class, its massfraction accounting for total system is 5%, the curing agent part selected is the mixture of acid anhydrides and imidazoles, and its massfraction accounting for total system is respectively 48.47% and 0.53%
Concrete preparation process is as follows:
Step 1: at normal temperatures, takes resin portion and toughner part by weight ratio, dissolves rear and abundant stirring and makes it mix;
Step 2: at 70 ~ 90 DEG C of temperature, constantly stirs 30 ~ 60min by the hybrid resin in step 1, and being cooled to normal temperature acquisition resin viscosity is 300 ~ 800Cps;
Step 3: at normal temperatures, takes curing agent part by weight ratio, and is fully uniformly mixed;
Step 4: at normal temperatures, takes the resin portion of step 2 and the curing agent part of step 3 by weight ratio, is fully uniformly mixed, and can obtain the resistant to elevated temperatures winding resin system of intermediate temperature setting.
Select T700S fiber and this resin system, adopt winding process to make one-way slabs.
Through experiment, test comparison data are as following table:
This intermediate temperature setting winding resin can improve temperature tolerance and the manufacturability of resin system, expands resin system range of application, can be applied in small-sized and large mould and product making, be applicable to the every field of commercial market to military markets.
Finally, it is also to be noted that what enumerate above is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (9)
1. an intermediate temperature setting is wound around resin, it is characterized in that: comprise resin portion, toughner part and curing agent part, the massfraction of described resin portion is 30 ~ 60%, and the massfraction of described toughner part is 3 ~ 10%, and the massfraction of described curing agent part is 40 ~ 70%;
Described resin portion is one or more in polyester vinyl ester resin, bimaleimide resin, epoxy resin, unsaturated polyester, resol, cyanate ester resin;
The component of described toughner part is one or more in mineral filler, synthetic rubber, thermoplastic resin, flexible chain solidifying agent;
The component of described curing agent part is one or more in amine, anhydrides, imidazoles, metallic salt, linear resin oligopolymer class or their derivative.
2. intermediate temperature setting as claimed in claim 1 is wound around resin, and it is characterized in that: the massfraction of described resin portion is 40 ~ 60%, the massfraction of described toughner part is 5 ~ 10%, and the massfraction of described curing agent part is 40 ~ 60%.
3. intermediate temperature setting as claimed in claim 1 or 2 is wound around resin, it is characterized in that, the glass transition temperature Tg that resin Composition adopts differentia scanning calorimetry DSC to record is 170 ~ 280 DEG C, and the glass transition temperature Tg adopting dynamic properties analytical method DMA to record after solidification is 170 ~ 250 DEG C.
4. intermediate temperature setting as claimed in claim 1 or 2 is wound around resin, it is characterized in that, adopts following steps preparation:
Step 1: at normal temperatures, takes resin portion and toughner part by weight ratio, dissolves rear and abundant stirring and makes it mix;
Step 2: at 70 ~ 90 DEG C of temperature, constantly stirs 30 ~ 60min by the hybrid resin in step 1, and being cooled to normal temperature acquisition resin viscosity is 300 ~ 800Cps;
Step 3: at normal temperatures, takes described curing agent part by weight ratio, and is fully uniformly mixed;
Step 4: at normal temperatures, takes the resin portion of step 2 and the curing agent part of step 3 by weight ratio, is fully uniformly mixed, and can obtain the resistant to elevated temperatures winding resin system of intermediate temperature setting.
5. a preparation method for intermediate temperature setting winding resin described in any one of claim 1-4, is characterized in that: concrete steps are as follows:
Step 1: at normal temperatures, with the massfraction of resin portion be 30 ~ 60%, the massfraction of toughner part is 3 ~ 10% take resin portion and toughner part, fully stir and make it mix after dissolving;
Step 2: at 70 ~ 90 DEG C of temperature, constantly stirs 30 ~ 60min by the hybrid resin in step 1, and being cooled to normal temperature acquisition resin viscosity is 300 ~ 800Cps;
Step 3: at normal temperatures, is 40 ~ 70% take described curing agent part with the massfraction of curing agent part, and is fully uniformly mixed;
Step 4: at normal temperatures, takes the resin portion of step 2 and the curing agent part of step 3 by weight ratio, is fully uniformly mixed, and can obtain the resistant to elevated temperatures winding resin system of intermediate temperature setting.
6. the preparation method of intermediate temperature setting winding resin as claimed in claim 5, is characterized in that: described resin portion is one or more in polyester vinyl ester resin, bimaleimide resin, epoxy resin, unsaturated polyester, resol, cyanate ester resin;
The component of described toughner part is one or more in mineral filler, synthetic rubber, thermoplastic resin, flexible chain solidifying agent;
The component of described curing agent part is one or more in amine, anhydrides, imidazoles, metallic salt, linear resin oligopolymer class or their derivative.
7. intermediate temperature setting as claimed in claim 6 is wound around resin, it is characterized in that, the glass transition temperature Tg that resin Composition adopts differentia scanning calorimetry DSC to record is 170 ~ 280 DEG C, and the glass transition temperature Tg adopting dynamic properties analytical method DMA to record after solidification is 170 ~ 250 DEG C.
8. the winding one-way slabs that obtains of any one of a claim 1-4 resin-made, it is characterized in that: adopt the intermediate temperature setting of any one of claim 1-4 to be wound around resin and adopt winding process to obtain, this one-way slabs is after post curing treatment, and glass transition temperature Tg is 150 ~ 250 DEG C; Interlaminar shear strength is at 50MPa-150MPa, and tensile strength is at 1000MPa-3000MPa, and tensile modulus is at 70GPa-170GPa.
9. intermediate temperature setting as claimed in claim 8 is wound around resin, and it is characterized in that, one-way slabs is after post curing treatment, and glass transition temperature Tg is 180 ~ 240 DEG C; Interlaminar shear strength is at 60Mpa-120MPa, and tensile strength is at 1800MPa-2800MPa, and tensile modulus is at 100GPa-170GPa.
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Application publication date: 20160106 |