CN107868400A - Intermediate temperature setting prepreg resin matrix and preparation method thereof - Google Patents
Intermediate temperature setting prepreg resin matrix and preparation method thereof Download PDFInfo
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- CN107868400A CN107868400A CN201610850794.XA CN201610850794A CN107868400A CN 107868400 A CN107868400 A CN 107868400A CN 201610850794 A CN201610850794 A CN 201610850794A CN 107868400 A CN107868400 A CN 107868400A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/53—Core-shell polymer
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The present invention relates to a kind of intermediate temperature setting prepreg resin matrix and preparation method thereof, mainly solves the existing intermediate temperature setting prepreg resin matrix technical problem that heat resistance declines while toughness is improved.By using in terms of mass fraction, including 100 parts of epoxy resin compositions, 1~15 part of curing agent, 0.5~10 part of accelerator, 1~30 part of nucleocapsid type rubber particle toughening agent；The technical scheme for the intermediate temperature setting prepreg resin matrix that its epoxy resin mixture is mixed in terms of mass fraction by 30~70 parts of liquid-state epoxy resins and 70~30 parts of solid epoxy resins, preferably solve problem above, there is provided epoxy resin-base toughness T while significantly improvegBe held essentially constant, and at 120 DEG C hardening time be less than 1 hour, and pot life at room temperature exceedes January, available for fields such as Leisure Sport articles for use, automobile, yachts.
Description
Technical field
The invention belongs to prepreg manufacturing technology field, more particularly to a kind of intermediate temperature setting prepreg resin matrix and its system
Preparation Method.
Background technology
Prepreg be under conditions of the strict control after the resin matrix impregnating continuous fibres or fabric made of resin base
The composition of body and reinforcing fiber, it is the intermediate materials for producing high-performance composite materials.According to the difference of solidification temperature, hot melt
Epoxy prepreg be broadly divided into intermediate temperature setting prepreg (solidification temperature is between 80~150 DEG C) and hot setting prepreg (Gu
Change temperature more than 180 DEG C).Hot setting prepreg is mainly for the production of the field such as space flight and aviation, military project main force support structure
Part and some other resistant to elevated temperatures structural member of needs, and intermediate temperature setting prepreg is mainly for the production of space flight and aviation, military project etc.
Structural member of the field in the civilian industry such as secondary structure part or Leisure Sport articles for use, automobile, yacht.Hot setting can obtain resistance to
The excellent cured product of hot property.But because solidification temperature is higher, material expand with heat and contract with cold will cause to exist inside product it is larger
Internal stress, dimension control is influenceed, product premature degradation can be caused when serious.It can also be brought into addition, solidification temperature is higher
The problems such as pattern tool selection range is narrow, manufacturing process is complicated and power consumption is high, is unfavorable for the reduction of production cost.Comparatively, in
Temperature solidification requires low advantage with short molding cycle, to mould and former.In addition, reducing forming temperature can be reduced again
Condensation material internal stress caused by expanding with heat and contract with cold and resulting buckling deformation, are advantageously ensured that outside the design of large-scale component
Shape, it is to make low cost, the first choice of high-performance composite materials.
In recent years, with the decline of carbon fiber price, carbon fibre composite is in civilian industries such as automobile, high ferro, steamers
In demand rise year by year, but because matrix resin is in the high crosslink density formed in the curing process, cause resin to resist
Impact difference is low with fracture toughness, constrains its further application.Therefore in order to improve the toughness of composite, more using bullet
Property body, rubber, nano-particle or thermoplastic resin are added in resin matrix as toughener.
CN201310032354.X provides a kind of method of dimer acid modified epoxy resin roughening carbon fiber prepreg, it
Dimer acid modified epoxy resin is employed as toughener, a kind of carbon fibre composite of toughness reinforcing has been obtained, has improved compound
The interlaminar shear strength of material.But as the addition of dimer acid modified epoxy resin, the Tg of the resin system solidfied material are gradual
Reduce, constrain further applying for the system.
CN201310031083.6 provides a kind of improvement prepreg using polyurethane modified epoxy resin as toughener
Toughness method, the epoxy-resin systems utilize polyurethane modified epoxy resin high bond strength and impact resistance, assign
The high interlaminar shear strength of prepreg, improve the toughness of composite.But the addition of polyurethane modified epoxy significantly reduces
The heat resistance of epoxy-resin systems, make the T of its solidfied materialgIt is decreased obviously.
The content of the invention
One of technical problems to be solved by the invention are existing intermediate temperature setting prepreg resin matrix toughness and heat resistance
It is difficult to the technical problem synchronously improved, by adding a kind of nano-rubber particle with core shell structure in resin matrix, carries
A kind of intermediate temperature setting prepreg resin matrix is supplied, the resin matrix has than prior art while high impact is kept
The higher glass transition temperature of toughened system.
The two of the technical problems to be solved by the invention are to provide a kind of intermediate temperature setting solved described in one of technical problem
The preparation method of prepreg resin matrix, the preparation method is easy to operate, significantly shortens material and melts, mixes, the time of deaeration.
To solve one of above technical problem, the technical solution adopted by the present invention is as follows：A kind of intermediate temperature setting prepreg tree
Aliphatic radical body, in terms of mass fraction, including 100 parts of epoxy resin compositions, 1~15 part of curing agent, 0.5~10 part of accelerator, 3~
30 parts of nucleocapsid type rubber particle toughening agent；Its epoxy resin mixture is in terms of mass fraction by 30~70 parts of liquid-state epoxy resins
Mixed with 70~30 parts of solid epoxy resins.
In above-mentioned technical proposal, preferable technical scheme：The liquid-state epoxy resin is bisphenol A type epoxy resin, Bisphenol F
Combination more than one or both of type epoxy resin, novolac epoxy resin, glycidyl amine epoxy resin.
In above-mentioned technical proposal, preferable technical scheme：The solid epoxy resin is bisphenol A type epoxy resin, Bisphenol F
Combination more than one or both of type epoxy resin, bisphenol-s epoxy resin, novolac epoxy resin.
In above-mentioned technical proposal, preferable technical scheme：The curing agent is dicyandiamide, and the particle diameter D90 of dicyandiamide does not surpass
Cross 25 μm.
In above-mentioned technical proposal, preferable technical scheme：The accelerator is substituted urea, and the particle diameter D90 of substituted urea does not surpass
Cross 25 μm.
In above-mentioned technical proposal, preferable technical scheme：The toughener is nucleocapsid type rubber particle toughening agent, and its core is excellent
It is butadiene and styrol copolymer to elect core as, and shell is acrylic polymer.
To solve the two of above technical problem, the technical solution adopted by the present invention is as follows：A kind of intermediate temperature setting prepreg tree
The preparation method of aliphatic radical body, using mixing apparatus of the rotation-revolution de-airing mixer as composition epoxy resin, including it is following
Step：
A, solid epoxy resin is broken for particle of the diameter less than 15mm；
B, above-mentioned solid epoxy resin, liquid-state epoxy resin, toughness reinforcing are added in the container of rotation-revolution de-airing mixer
Agent and curing agent；
C, set the stirring condition of rotation-revolution mixer as：500~2000 revs/min of mixing speed, vacuum
0.2kPa~normal pressure, mixing time 1~30 minute, after whipping procedure is automatically performed, obtain deaeration it is complete and well mixed in
Temperature solidification prepreg resin matrix.
In above-mentioned technical proposal, preferable technical scheme, solid epoxy resin is broken for diameter in step a and is less than 5mm
Particle, organic and inorganic or high polymer material solid particle is added in the container of rotation-revolution de-airing mixer in step b
As abrasive media, a diameter of 0.5~10mm of abrasive media.
The experimental raw that the present invention selects mainly includes：
Liquid bisphenol A epoxy resin：331, Dow Chemical；
Solid-state bisphenol A epoxide resin：671, Dow Chemical；
Bisphenol F epoxy resin：354, Dow Chemical；
Novolac epoxy resin：438, Dow Chemical；
Nitrile rubber toughener：F201, Dow Chemical；
Polyurethane modified epoxy resin toughener：ESR-133, many departments in Shanghai；
Trifunctional glycidyl amine epoxy resin：MY0510, Huntsman company；
Tetrafunctional glycidyl amine epoxy resin：XB9721, Huntsman company；
Dicyandiamide：100S, Evonik Degussa Corp.；
Substituted urea：UR-500, Evonik Degussa Corp.；
Nucleocapsid type rubber particle：MX-154, core are butadiene and styrol copolymer, and shell is acrylic polymer,
Japanese Kaneka Corp..
Prepreg resin matrix and its Solidified enzyme method of testing are with execution standard：
1) impact property of solidfied material：GB/T2567- is pressed on the CEAST6957 type Charpy impact testers of Italy
The requirement of 2008 standards is tested；
2) tensile property of solidfied material：Marked on the universal testing machine of Instron companies of the U.S. by GB/T 2567-2008
Alignment request is carried out, rate of extension 5mm/min；
3) T of solidfied materialg：Carried out on U.S. TA companies Q800 type dynamic mechanical analyzers, under selection G ' starts
T of the curve near tangent temperature as solidfied material during dropg。
Intermediate temperature setting prepreg resin matrix provided by the invention and preparation method thereof, the advantage is that：
1) by using toughener of the nano-rubber particle of core shell structure as resin system, resinite is not only increased
The impact property of system, and keep the heat resistance of resin system not decline.2) the rotation-revolution vacuum that is blended in of resin matrix is stirred
Mix and carried out on machine, the melting of material, the scattered, step of deaeration three-procedure one are completed, when simplifying technological process and shortening mixing
Between, so as to shorten the thermal history of material, be advantageous to extend the Storage period of epoxy composite.
Using technical scheme, by using toughness reinforcing of the nano-rubber particle of core shell structure as resin system
Agent, the impact property of resin system is not only increased, and keep the heat resistance of resin system not decline, impact strength is reachable
69kJ/m2, glass transition temperature achieves preferable technique effect up to 142 DEG C.
The present invention is further elaborated below by embodiment.
Embodiment
【Embodiment 1】
Resin matrix formula is formed by mass fraction：
Liquid bisphenol A epoxy resin 331：50 parts；
Solid-state bisphenol A epoxide resin 671：50 parts；
Dicyandiamide 100S：6 parts；
Substituted urea UR-500：5 parts；
Nucleocapsid type rubber particle MX-154：10 parts.
The preparation method of resin matrix：Solid epoxy is broken for particle of the diameter less than 5mm, then matched somebody with somebody by above-mentioned
Each component is added in the container of mixer by side.First 3 are stirred under conditions of vacuum is 30kPa, rotating speed is 2000rpm
Minute, then stirred 8 minutes under conditions of vacuum is 0.3kPa, rotating speed is 2000rpm, stirring finishes to obtain epoxy resin group
Compound.
The preparation method of standard batten：Standard batten mould is put into forced air oven, protected after temperature rises to 120 DEG C
Temperature 1 hour, composition epoxy resin is cast in mould, isothermal curing 1 hour, then naturally cools to room temperature.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
【Embodiment 2】
Resin matrix formula is formed by mass fraction：
Liquid bisphenol A epoxy resin 331：50 parts；
Solid-state bisphenol A epoxide resin 671：50 parts；
Dicyandiamide 100S：6 parts；
Substituted urea UR-500：5 parts；
Nucleocapsid type rubber particle MX-154：20 parts.
The preparation method of resin matrix and standard batten is the same as embodiment 1.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
【Embodiment 3】
Resin matrix formula is formed by mass fraction：
Liquid glycidyl amine epoxy resin MY0510：40 parts；
Solid-state bisphenol A epoxide resin 671：60 parts；
Dicyandiamide 100S：4 parts；
Substituted urea UR-500：3 parts；
Nucleocapsid type rubber particle MA-154：20 parts.
The preparation method of resin matrix and standard batten is the same as embodiment 1.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
【Embodiment 4】
Resin matrix formula is formed by mass fraction：
Liquid glycidyl amine epoxy resin MY-0510：40 parts；
Solid-state bisphenol A epoxide resin 671：60 parts；
Dicyandiamide 100S：4 parts；
Substituted urea UR-500：3 parts；
Nucleocapsid type rubber particle MX-154：10 parts.
The preparation method of resin matrix and standard batten is the same as embodiment 1.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
【Embodiment 5】
Resin matrix formula is formed by mass fraction：
Liquid bisphenol F types epoxy resin 354：30 parts；
Solid-state bisphenol A epoxide resin 671：70 parts；
Dicyandiamide 100S：6 parts；
Substituted urea UR-500：5 parts；
Nucleocapsid type rubber particle MX-154：5 parts.
The preparation method of resin matrix and standard batten is the same as embodiment 1.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
【Embodiment 6】
Resin matrix formula is formed by mass fraction：
Liquid bisphenol F types epoxy resin 354：30 parts；
Solid-state bisphenol A epoxide resin 671：70 parts；
Dicyandiamide 100S：6 parts；
Substituted urea UR-500：5 parts；
Nucleocapsid type rubber particle MX-154：15 parts.
The preparation method of resin matrix and standard batten is the same as embodiment 1.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
【Embodiment 7】
Resin matrix formula is formed by mass fraction：
Liquid novolac epoxy resin 438：40 parts；
Solid-state bisphenol A type epoxy resin fat 671：60 parts；
Dicyandiamide 100S：4 parts；
Substituted urea UR-500：3 parts；
Nucleocapsid type rubber particle MX-154：30 parts.
The preparation method of resin matrix and standard batten is the same as embodiment 1.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
【Embodiment 8】
Resin matrix formula is formed by mass fraction：
Liquid novolac epoxy resin 438：30 parts；
Solid-state bisphenol A type epoxy resin fat 671：70 parts；
Dicyandiamide 100S：4 parts；
Substituted urea UR-500：3 parts；
Nucleocapsid type rubber particle MX-154：10 parts.
The preparation method of resin matrix and standard batten is the same as embodiment 1.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
【Comparative example 1】
Resin matrix formula is formed by mass fraction：
Liquid bisphenol A epoxy resin 331：50 parts；
Solid-state bisphenol A epoxide resin 671：50 parts；
Dicyandiamide 100S：6 parts；
Substituted urea UR-500：5 parts；
Nitrile rubber toughener F201：20 parts.
The preparation method of resin matrix：First, liquid-state epoxy resin 331 and the solidification of equivalent are added in homogenizer
System powder (dicyandiamide:Substituted urea=6:5), high-speed stirred 30~45 minutes at room temperature, vacuumized in whipping process with de-
Except mixed air in system, finely dispersed solidification masterbatch is obtained, discharge simultaneously clears up mixer.Then, in high-speed stirred
Solid epoxy resin 671 and remaining liquid-state epoxy resin 331 are added in machine, stirs and is warming up to 80~120 DEG C, treat that 671 is complete
60~70 DEG C are cooled to after fine melt solution, adds nitrile rubber toughener and appropriate solidification masterbatch, 5~30 points of high-speed stirred
Clock, vacuumize with mixed air in removing system in whipping process, obtain prepreg resin matrix.
The preparation method of standard batten：Resin matrix is cast to while hot in the stainless steel mould for having been preheated with 120 DEG C,
Isothermal curing 1 hour, then naturally cools to room temperature.
The test result of composition epoxy resin and its solidfied material is shown in Table 1.
Table 1
Claims (8)
1. a kind of intermediate temperature setting prepreg resin matrix, in terms of mass fraction, including 100 parts of epoxy resin compositions, 1~15 part
Curing agent, 0.5~10 part of accelerator, 1~30 part of nucleocapsid type rubber particle toughening agent；Its epoxy resin mixture is with mass parts
Number meter is mixed by 30~70 parts of liquid-state epoxy resins and 70~30 parts of solid epoxy resins.
2. intermediate temperature setting prepreg resin matrix according to claim 1, it is characterised in that the liquid-state epoxy resin is
One or both of bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy resin, glycidyl amine epoxy resin
Combination above.
3. intermediate temperature setting prepreg resin matrix according to claim 1, it is characterised in that the solid epoxy resin is
One or both of bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, novolac epoxy resin with
On combination.
4. intermediate temperature setting prepreg resin matrix according to claim 1, it is characterised in that the curing agent is dicyandiamide,
The particle diameter D90 of dicyandiamide is no more than 25 μm.
5. intermediate temperature setting prepreg resin matrix according to claim 1, it is characterised in that the accelerator is substituted urea,
The particle diameter D90 of substituted urea is no more than 25 μm.
6. intermediate temperature setting prepreg resin matrix according to claim 1, it is characterised in that the nucleocapsid type rubber particle
Core in toughener is butadiene and styrol copolymer, and shell is acrylic polymer.
7. according to the preparation method of any described intermediate temperature setting prepreg resin matrix of claim 1~6, it is characterised in that adopt
By the use of rotation-revolution de-airing mixer as the mixing apparatus of composition epoxy resin, comprise the following steps：
A, the solid epoxy resin is broken for particle of the diameter less than 15mm；
B, the desired amount of solid epoxy resin, liquid-state epoxy resin, toughness reinforcing are added in the container of rotation-revolution de-airing mixer
Agent and curing agent；
C, set the stirring condition of rotation-revolution mixer as：500~2000 revs/min of mixing speed, vacuum 0.2kPa~
Normal pressure, mixing time 1~30 minute, after whipping procedure is automatically performed, it is pre- to obtain the complete and well mixed intermediate temperature setting of deaeration
Leaching material resin matrix.
8. the preparation method of the intermediate temperature setting prepreg resin matrix according to claims 7, it is characterised in that in step a
Solid epoxy resin is broken for particle of the diameter less than 5mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111087895A (en) * | 2019-12-20 | 2020-05-01 | 天津经纬正能电气设备有限公司 | Reactor encapsulation slurry and preparation method thereof |
| CN115141466A (en) * | 2022-06-30 | 2022-10-04 | 武汉联影医疗科技有限公司 | Acoustic matching layer material, acoustic matching layer, ultrasonic transducer, ultrasonic probe, ultrasonic imaging device and preparation method |
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