CN106633645B - A kind of fibre reinforced high-strength lightweight composite material and preparation method thereof - Google Patents
A kind of fibre reinforced high-strength lightweight composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of fibre reinforced high-strength lightweight composite materials and preparation method thereof, the composite material, consists of the following parts by weight: 100 parts of epoxy resin, 30-100 parts of curing agent, 10-30 parts of reactive diluent, 30-150 parts of hollow glass micropearl, epoxy are grafted carbon fiber 5-30 parts.Preparation method of the present invention, carbon fiber is grafted by being prepared for epoxy in the method for carbon fiber surface grafted epoxy group, and it is added to epoxy resin, curing agent, reactive diluent, in hollow glass micropearl composite system, prepares high-strength light composite buoyancy material.The compatibility and dispersibility that carbon fiber and epoxy resin are improved by surface grafting epoxy group, improve the intensity of composite buoyancy material, while keeping lower density.Fibre reinforced high-strength lightweight composite material prepared by the present invention can be applied to oil, feed channel field of thermal insulation and deep sea equipment buoyant material field.
Description
Technical field
The present invention relates to high-strength lightweight composite material technical fields, and in particular to a kind of fibre reinforced high-strength light is compound
Material and preparation method thereof.
Background technique
High-strength lightweight composite material can be applied not only to oil, feed channel field of thermal insulation, can also be in ocean development
Various equipments provide buoyancy.High-strength lightweight composite material belongs to field of new materials.But in application process, it is desirable that high-strength light
Composite material itself has lower density and higher incompressible intensity.But traditional high-strength lightweight composite material is applied to float
When power Material Field, when especially epoxy/hollow glass micropearl composite material is applied to ocean development buoyant material, due to sky
The introducing of heart glass microballoon, which can generate some defects, leads to the decline of mechanical property.Composite material is often opened under compression
It splits or breakoff phenomenon, although hollow glass micropearl has the effect of sprawling of cracking in certain prevention composite material, effect
Less；If adding a kind of substance that small cracking can be prevented to continue sprawling in the composite, can mention significantly
The mechanical strength of high composite material.
Fibrous material such as carbon fibre material is a kind of relatively good substance for enhancing high molecular material in engineer application field,
But carbon fibre material, due to itself being carbon material, the polarity spectrum of polarity and epoxy resin is very big, the compatibility of the two and point
Scattered property will appear problem.One side carbon fiber in other words chopped carbon fiber material be easy to reunite be difficult and epoxy resin mixing
Uniformly；The associativity of still further aspect carbon fiber and epoxy resin is very poor, and the two has apparent interface, is easy to produce after mixing
Raw defect, can reduce the mechanical property of composite material.
Carbon fiber during the preparation process, although sizing agent can be introduced, to improve its associativity with resin, its starching
Agent is poor with the associativity of carbon fiber ontology after all, is unable to satisfy the effect of composite buoyancy material enhancing.Therefore improve carbon fiber
Surface property, so as to improve its dispersibility and interfacial bonding property just become one comparison of reinforced epoxy composite buoyancy material urgently
It solves the problems, such as.
Application publication number is that the Chinese invention patent application of CN 104479297A (application No. is 201410810065.2) is public
A kind of method for improving epoxy resin carbon fiber composite material interface toughness is opened, comprising: step 1: being located in advance to carbon fiber
Reason；Step 2: synthesis tetra functional organosilicon epoxy resin, in organic solvent by the dissolution of tetra functional organosilicon epoxy resin,
Then carbon fiber is immersed in aforementioned lysate；Step 3: with epoxy resin-matrix body fluid to the carbon fiber obtained in step 2 into
Row infiltration, is then solidified.In the technical solution, joined tetra functional in epoxy resin carbon fiber composite material interface has
Machine epoxy silicone can effectively improve the interfacial toughness of epoxy resin carbon fiber composite material.So that organic with tetra functional
The composite impact toughness on epoxy silicone Treatment of Carbon surface improves 20%, but it passes through simple compound, power
It is limited to learn performance raising.
Application publication number is that the Chinese invention patent application of CN 103214792A (application No. is 201310125726.3) is public
A kind of carbon fiber/epoxy resin composite material and preparation method thereof is opened, which includes: to be crosslinked by liquid-state epoxy resin
The solid epoxy resin that is formed after solidification, the curing agent for making liquid-state epoxy resin crosslinking curing, organic phosphates fire retardant, carbon fiber
Dimension.The organic phosphates fire retardant includes one of phosphate, condensed phosphoric esters, phosphine oxide and phosphorous heterocylic compound or several
Kind mixture.The carbon fiber includes the plain weave or twill carbon cloth or unidirectional carbon fiber of 3K, 6K, 12K, 24K, 48K
Any one in laminated cloth.In the technical solution, carbon fiber and epoxy resin interface associativity are poor, and overall performance is not
It is good.
Summary of the invention
For overcome the deficiencies in the prior art, it is multiple that the object of the present invention is to provide a kind of fibre reinforced high-strength lights
Condensation material and preparation method thereof, by using the method for specific surface grafting epoxy group, in chopped carbon fiber surface grafting
Epoxy group, and the epoxy of acquisition grafting carbon fiber is added in epoxy resin composite material system, improve epoxy composite material
The intensity of Material system improves the compatibility and dispersibility of carbon fiber in the epoxy, to meet high-strength light epoxy composite material
Expect the demand of application field.
The technical solution adopted by the present invention is as described below:
A kind of fibre reinforced high-strength lightweight composite material, consists of the following parts by weight:
Further preferably, the fibre reinforced high-strength lightweight composite material, consists of the following parts by weight:
Still more preferably, the fibre reinforced high-strength lightweight composite material, consists of the following parts by weight:
The present invention by the method for grafting in chopped carbon fiber surface grafting epoxy resin group, and then improve carbon fiber with
The interfacial bonding property of epoxy resin, while improving the dispersibility of carbon fiber in the epoxy, to prepare a kind of carbon fiber
Enhance high-strength lightweight composite material.
Epoxy resin used in the present invention includes glycidyl type epoxy resin (E-51, FarBond LY of such as bisphenol A-type
1564, TDE-85 etc.), epoxidation of olefins based epoxy resin (such as D-17), heterocyclic type and mixed type epoxy resin (such as cyanuric acid
Three-glycidyl epoxy resin).I.e. the epoxy resin is glycidyl type epoxy resin, epoxidation of olefins class asphalt mixtures modified by epoxy resin
One or more of rouge, heterocycle mixed type epoxy resin.
Curing agent used in the present invention is the system to match with epoxy resin, and type includes acid anhydride type curing agent and polyamine
Class curing agent, the 3486 of polynary amine curing agent such as amine, acid anhydride type curing agent for example phthalic anhydride, maleic anhydride,
Methyl tetrahydro phthalic anhydride.I.e. the curing agent is acid anhydride type curing agent or polynary amine curing agent.
Diluent used in the present invention is for reducing system viscosity, in order to which epoxy is grafted carbon fiber and hollow glass micropearl
It can be well dispersed in epoxy resin-base, selected diluent includes butyl glycidyl ether, 1,4-butanediol two
Glycidol ether, ethylene glycol diglycidylether, phenyl glycidyl ether, polypropylene glycol diglycidyl ether, C12-14 fat
Glycidol ether, benzyl glycidyl ether, 1,6- hexanediol diglycidyl ether, propylene oxide o-cresyl ether, neopentyl glycol
Diglycidyl ether.I.e. the diluent is butyl glycidyl ether, 1,4- butanediol diglycidyl ether, the contracting of ethylene glycol two
Water glycerin ether, phenyl glycidyl ether, polypropylene glycol diglycidyl ether, C12-14 fatty glycidyl ether, benzyl shrink sweet
Oily ether, 1,6- hexanediol diglycidyl ether, propylene oxide o-cresyl ether, at least one in neopentylglycol diglycidyl ether
Kind.
Hollow glass micropearl used in the present invention is the hollow glass micropearl that compression strength is greater than 20MPa, including 3M company
The hollow glass micropearl of S35, K37, S38, S38HS, K46 trade mark, diameter are 10 μm -120 μm.That is the hollow glass micropearl
Diameter be 10 μm -120 μm.
The preparation of the described epoxy grafting carbon fiber the following steps are included:
(1) hydroxylating of carbon fiber: chopped carbon fiber tow is immersed in hydrogen peroxide, reflow treatment obtains surface hydroxyl
The carbon fiber of change；
(2) carbon fiber is vinylated: the carbon fiber of surface hydroxylation is put into vinyl silicane coupling agent ethanol solution
Middle reflux obtains vinylated carbon fiber；
(3) epoxy is grafted carbon fiber: it is molten that vinylated carbon fiber being put into 1,2- epoxy -4- vinyl cyclohexane acetone
In liquid, mixed liquor is obtained；Then mixed liquor is irradiated under oxygen-free environment, the vinyl in irradiation process in carbon fiber and 1,2-
Vinyl in epoxy -4- vinyl cyclohexane carries out cross-linking reaction, post-treated to obtain epoxy grafting carbon fiber.
In step (1), the condition of the reflow treatment are as follows: reflow treatment 6~10 hours, further preferably at 100 DEG C
Lower reflow treatment 8 hours.
The chopped carbon fiber tow selects T300 carbon fiber, the source as chopped carbon fiber tow.
The chopped carbon fiber tow, it is specific to select draw ratio for (7-15): 1 acrylonitrile base carbon fiber, carbon fiber
Diameter is 7-8 μm.
In step (2), vinyl silicane coupling agent ethanol solution is mixed by vinyl silicane coupling agent and ethyl alcohol, second
The mass percent of alkenyl silanes coupling agent ethanol solution medium vinyl silane coupling agent is 5%-20%, the vinyl silicon
Alkane coupling agent selects vinyltriethoxysilane (A-151).
The time of the reflux is 1~3 hour, is further 2 hours.
Coupling agent selects vinyl silicane coupling agent, and the vinyl groups of introducing is conducive to as follows with the functional group of vinyl
One step vinyl epoxy carries out irradiation grafting reaction, and the vinyl silanes of introducing can be vinyltriethoxysilane A-151.
In step (3), 1, the 2- epoxy -4- vinyl cyclohexane, for flowering structure:
1,2- epoxy -4- vinyl cyclohexane the acetone soln is by 1,2- epoxy -4- vinyl cyclohexane and acetone
It mixes.The quality of 1,2- epoxy -4- vinyl cyclohexane in the 1,2- epoxy -4- vinyl cyclohexane acetone soln
Percentage is 5%-20%.
The mass ratio of the vinylated carbon fiber and 1,2- epoxy -4- vinyl cyclohexane acetone soln is 1:
0.5~1.5.Further preferably, the vinylated carbon fiber and 1,2- epoxy -4- vinyl cyclohexane acetone soln
Mass ratio is 1:1.
The mixed liquor irradiates under oxygen-free environment, specifically includes:
Mixed liquor is put into polyethylene plastic packaging bag, rushes nitrogen 3~8 minutes and catches up with except the oxygen in solution, plastic packaging is put in electricity
Sub- accelerator underdrive irradiation, while being cooled down with fan, irradiation dose 5-30kGy, beam energy is 1.5~
2.5MeV, 8~12mA, the vinyl and 1 in irradiation process in carbon fiber, the vinyl in 2- epoxy -4- vinyl cyclohexane
Carry out cross-linking reaction.
Further preferably, mixed liquor is put into polyethylene plastic packaging bag, rushes and catches up within nitrogen 5 minutes except the oxygen in solution, modeling
Envelope is put in the irradiation of electron accelerator underdrive, while being cooled down with fan, irradiation dose 5-30kGy, and beam energy is
2MeV, 10mA, the vinyl and 1 in irradiation process in carbon fiber, the vinyl in 2- epoxy -4- vinyl cyclohexane are handed over
Connection reaction.
The post-processing；Reactant after irradiation is grafted through filtering, acetone washing, filtering, the dry epoxy that can be obtained
Carbon fiber.
1,2- epoxy -4- vinyl cyclohexane in above-mentioned steps (3), vinyl can be with step (2) medium vinyls
Carbon fiber vinyl carry out graft reaction, the present invention select 1,2- epoxy -4- vinyl cyclohexane as graft；By 1,
2- epoxy -4- vinyl cyclohexane is put into acetone solvent, forms 1,2- epoxy -4- vinyl cyclohexane acetone soln, concentration
For 5-20%, then ethylene base carbon fibre is put into mixed solution；The quality and 1,2- epoxy -4- of vinylated carbon fiber
Mass ratio in vinyl cyclohexane acetone soln is 1:1；The mixed liquor of above-mentioned three is put into polyethylene plastic packaging bag, nitrogen is rushed
It catches up with except the oxygen in solution within gas 5 minutes, thoroughly removes interference of the oxygen for graft reaction；In addition irradiation sample has to put
In polyethylene plastic packaging bag, the infiltration of oxygen in irradiation process is prevented, while being driven irradiation and guaranteeing heat dissipation in time, irradiation dose
It controls, irradiation dose is selected as 5-30kGy, controls irradiation grafting degree.
A kind of preparation method of fibre reinforced high-strength lightweight composite material, comprising the following steps:
Epoxy resin is added in reactive diluent, epoxy grafting carbon fiber is then sequentially added, curing agent, finally adds
Enter hollow glass micropearl, then mixing, deaeration in rotation deaeration machine after mixed liquor ultrasonic disperse pour the mixture into mold
Solidified, is demoulded up to fibre reinforced high-strength lightweight composite material.
Fibre reinforced high-strength lightweight composite material of the present invention, excellent in mechanical performance, while lower density is kept, it is light
Material can be used for oil, feed channel field of thermal insulation and deep sea equipment buoyant material field.
Compared with prior art, the present invention has the advantage that
Fibre reinforced high-strength lightweight composite material of the present invention and preparation method thereof.By in carbon fiber surface grafted epoxy
The method of group is prepared for epoxy grafting carbon fiber, and is added to epoxy resin, curing agent, reactive diluent, hollow glass
In glass microballon composite system, high-strength light composite buoyancy material is prepared.Carbon is improved by surface grafting epoxy group
The compatibility and dispersibility of fiber and epoxy resin, improve the intensity of composite buoyancy material, while keeping lower density.It is high
The density of high strength light composite material is 0.60g/cm3, incompressible intensity can achieve 58MPa.Carbon fiber prepared by the present invention increases
Strong high-strength lightweight composite material can be applied to oil, feed channel field of thermal insulation and deep sea equipment buoyant material field.
Specific embodiment
Preferred embodiment of the invention is given below, these embodiments not limit the contents of the present invention.
Embodiment 1 (preparation of epoxy grafting carbon fiber)
Epoxy be grafted carbon fiber preparation the following steps are included:
(1) hydroxylating of carbon fiber: selecting T300 carbon fiber as chopped carbon fiber source, and chopped carbon fiber is draw ratio
For (7-15): 1 acrylonitrile base carbon fiber, carbon fiber diameter are 7-8 μm；Chopped carbon fiber tow is immersed in hydrogen peroxide,
Reflow treatment 8 hours at 100 DEG C, obtain the carbon fiber of surface hydroxylation；
(2) carbon fiber is vinylated: the carbon fiber of surface hydroxylation is put into vinyl silicane coupling agent ethanol solution
Middle reflux obtains vinylated carbon fiber for 2 hours, vinyl silicane coupling agent ethanol solution by vinyl silicane coupling agent and
Ethyl alcohol mixes, wherein the mass percent of vinyl silicane coupling agent ethanol solution medium vinyl silane coupling agent is
12%, vinyl silicane coupling agent selects vinyltriethoxysilane A-151；
(3) epoxy is grafted carbon fiber: 1,2- epoxy -4- vinyl cyclohexane being dissolved in acetone, 1,2- epoxy -4- is formed
Vinyl cyclohexane acetone soln, 1,2- epoxy -4- vinyl cyclohexane in 1,2- epoxy -4- vinyl cyclohexane acetone soln
Mass percentage concentration be 10%, it is molten that vinylated carbon fiber is then put into 1,2- epoxy -4- vinyl cyclohexane acetone
In liquid, mixed liquor, the quality of vinylated carbon fiber and the quality of 1,2- epoxy -4- vinyl cyclohexane acetone soln are obtained
Than above-mentioned mixed liquor being put into polyethylene plastic packaging bag, rushes nitrogen 5 minutes and catches up with except the oxygen in solution, plastic packaging is put in for 1:1
The irradiation of electron accelerator underdrive, while being cooled down with fan, irradiation dose 20kGy, beam energy 2MeV,
10mA, the vinyl and 1 in irradiation process in carbon fiber, the vinyl in 2- epoxy -4- vinyl cyclohexane be crosslinked anti-
It answers；Reactant after irradiation is through filtering, acetone washing, filtering, dry that epoxy grafting carbon fiber can be obtained.
Embodiment 2
It takes bisphenol A type epoxy resin E51 40g and ethylene glycol diglycidylether 10g to be stirred, is then added and implements
Epoxy prepared by example 1 is grafted carbon fiber 5g, curing agent methyl tetrahydro phthalic anhydride 25g, and after mixed liquor ultrasonic disperse, it is empty that 3M company is added
Heart glass microballoon (S32, diameter are 10 μm -120 μm, and compression strength is greater than 20MPa) 45g, mixed in high speed rotation deaeration machine,
Deaeration 10min, mixture pours into steel die to be solidified according to certain curing cycle, and curing cycle is 80 DEG C of * 1h+120
DEG C * 2h+160 DEG C * 2h first solidifies 1 hour at 80 DEG C, then solidify at 120 DEG C DEG C 2 hours, small in 160 DEG C of solidifications 2 again later
When, it demoulds up to fiber reinforced high-strength light composite material.The density of composite material is 0.58g/cm3, incompressible intensity can be with
Reach 40MPa.
Embodiment 3
1564 40g of bisphenol A type epoxy resin FarBond LY is taken to be mixed into 10g 1, in 6- hexanediol diglycidyl ether,
Epoxy prepared by embodiment 1 is grafted carbon fiber 10g, curing agent FarBond LY (acid anhydride type curing agent) 3486 17g, and 3M is added
Company's hollow glass micropearl (S38HS, diameter be 10 μm -120 μm) 60g, in high speed rotation deaeration machine after mixed liquor ultrasonic disperse
Middle mixing, deaeration 10min, then mixture pours into steel die and is solidified according to certain curing cycle, and curing cycle is
80 DEG C of * 1h+100 DEG C * 1h first solidify 1 hour at 80 DEG C, then solidify 1 hour at 100 DEG C DEG C, demould high up to fiber reinforcement
High strength light composite material.The density of composite material is 0.6g/cm3, incompressible intensity can achieve 58MPa.
Comparative example 1
With the epoxy grafted carbon in chopped carbon fiber 5g and 1,2- epoxy -4- vinyl cyclohexane 0.5g alternate embodiment 2
Fiber 5g, other are the same as embodiment 2.The density for obtaining composite material is 0.58g/cm3, incompressible intensity can achieve 30MPa.
Comparative example 2
Carbon fiber is grafted with the epoxy in chopped carbon fiber 10g and 1,2- epoxy -4- vinyl cyclohexane 1g alternate embodiment 3
10g is tieed up, other are the same as embodiment 3.The density of composite material is 0.6g/cm3, incompressible intensity can achieve 43MPa.
Comparative example 1 and comparative example 2 use common blending and modifying carbon fiber, and the composite materials property finally obtained is wanted
Significantly lower than embodiment 2 and 3.
There are many concrete application approach of the present invention, the above is only a preferred embodiment of the present invention, it is noted that for
For those skilled in the art, without departing from the principle of the present invention, several improvement can also be made, this
A little improve also should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of fibre reinforced high-strength lightweight composite material, which comprises the following steps:
Epoxy resin is added in reactive diluent, epoxy grafting carbon fiber is then sequentially added, curing agent, is eventually adding sky
Heart glass microballoon, mixing, deaeration in rotation deaeration machine, then pour the mixture into mold and carry out after mixed liquor ultrasonic disperse
Solidification demoulds up to fibre reinforced high-strength lightweight composite material；
The preparation of the epoxy grafting carbon fiber, comprising the following steps:
(1) chopped carbon fiber tow is immersed in hydrogen peroxide, reflow treatment obtains the carbon fiber of surface hydroxylation；
(2) carbon fiber of surface hydroxylation is put into reflux in vinyl silicane coupling agent ethanol solution and obtains vinylated carbon
Fiber；
(3) vinylated carbon fiber is put into 1,2- epoxy -4- vinyl cyclohexane acetone soln, obtains mixed liquor；So
Mixed liquor is irradiated under oxygen-free environment afterwards, the vinyl in irradiation process in carbon fiber and 1,2- epoxy -4- vinyl cyclohexyl
Vinyl in alkane carries out cross-linking reaction, post-treated after the reaction was completed to obtain epoxy grafting carbon fiber；
The fibre reinforced high-strength lightweight composite material, consists of the following parts by weight:
2. preparation method according to claim 1, which is characterized in that the fibre reinforced high-strength lightweight composite material,
It consists of the following parts by weight:
3. preparation method according to claim 1, which is characterized in that the diluent be butyl glycidyl ether, 1,
4- butanediol diglycidyl ether, ethylene glycol diglycidylether, phenyl glycidyl ether, polypropylene glycol diglycidyl ether,
C12-14 fatty glycidyl ether, benzyl glycidyl ether, 1,6- hexanediol diglycidyl ether, propylene oxide o-tolyl
At least one of ether, neopentylglycol diglycidyl ether.
4. preparation method according to claim 1, which is characterized in that the diameter of the hollow glass micropearl be 10 μm-
120μm。
5. preparation method according to claim 1, which is characterized in that in step (1), the condition of the reflow treatment
Are as follows: reflow treatment 6~10 hours.
6. preparation method according to claim 1, which is characterized in that in step (1), the chopped carbon fiber tow choosing
It is (7-15): 1 acrylonitrile base carbon fiber with draw ratio, carbon fiber diameter is 7-8 μm.
7. preparation method according to claim 1, which is characterized in that in step (2), vinyl silicane coupling agent ethyl alcohol is molten
Liquid is mixed by vinyl silicane coupling agent and ethyl alcohol, vinyl silicane coupling agent ethanol solution medium vinyl silane coupling agent
Mass percent be 5%-20%；
The time of the reflux is 1~3 hour.
8. preparation method according to claim 1, which is characterized in that in step (3), 1, the 2- epoxy -4- ethylene
Butylcyclohexane acetone soln is mixed by 1,2- epoxy -4- vinyl cyclohexane and acetone, 1, the 2- epoxy -4- ethylene
The mass percent of 1,2- epoxy -4- vinyl cyclohexane is 5%-20% in butylcyclohexane acetone soln；
The mass ratio of the vinylated carbon fiber and 1,2- epoxy -4- vinyl cyclohexane acetone soln be 1:0.5~
1.5。
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| CN108587070A (en) * | 2018-05-25 | 2018-09-28 | 潘荣强 | A kind of lightweight buoyancy material and preparation method thereof |
| CN108997717A (en) * | 2018-09-10 | 2018-12-14 | 迦南(福建)新材料科技有限公司 | A kind of High-performance solid buoyancy material and its preparation process |
| CN109577007B (en) * | 2018-11-15 | 2021-04-09 | 南昌航空大学 | Preparation method of hyperbranched polyester grafted carbon fiber |
| CN109651928A (en) * | 2018-12-30 | 2019-04-19 | 青岛海洋新材料科技有限公司 | A kind of low-density high-modulus epoxy resin restraint layer plate and preparation method thereof |
| CN112029457A (en) * | 2020-08-03 | 2020-12-04 | 河北天启通宇航空器材科技发展有限公司 | Light bonding material and preparation method thereof |
| CN112266604A (en) * | 2020-11-10 | 2021-01-26 | 北京中超伟业信息安全技术股份有限公司 | Carbon fiber composite material for reinforcing notebook computer shell and preparation method thereof |
| CN113277868B (en) * | 2021-05-25 | 2022-04-22 | 杭州幄肯新材料科技有限公司 | Light carbon fiber/carbon composite thermal field material and preparation method thereof |
| CN114182533A (en) * | 2021-12-07 | 2022-03-15 | 陈宗良 | Carbon fiber sizing agent and preparation method thereof, and carbon fiber composite material and preparation method thereof |
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