CN109943022A - A kind of basalt fibre reinforced epoxy composite material and preparation method - Google Patents
A kind of basalt fibre reinforced epoxy composite material and preparation method Download PDFInfo
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- CN109943022A CN109943022A CN201910247374.6A CN201910247374A CN109943022A CN 109943022 A CN109943022 A CN 109943022A CN 201910247374 A CN201910247374 A CN 201910247374A CN 109943022 A CN109943022 A CN 109943022A
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- graphene
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Abstract
The invention belongs to resin material technical fields, and in particular to a kind of basalt fibre reinforced epoxy composite material and preparation method.The present invention provides a kind of preparation methods of basalt fibre reinforced epoxy composite material, the present invention improves the heat resistance of basalt fibre reinforced epoxy composite material using graphene base-material, by adding graphene base-material in the epoxy, graphene base-material and epoxy resin-base are generated and new are stably connected with key, in the case where not changing epoxy resin density substantially, so that the mechanical property of epoxy resin is improved.In addition, heat dissipation is uniformly quick since graphene base-material has preferable thermal conductivity, and the chemical bond stability formed is good, can also be improved the heat resistance for the basalt fibre reinforced epoxy composite material being finally prepared.
Description
Technical field
The invention belongs to resin material technical fields, and in particular to a kind of basalt fibre reinforced epoxy composite material
And preparation method thereof.
Background technique
Epoxy resin is that have good heat resistance by artificial synthesized a kind of high molecular polymer, and cost of material is low, because
This is used widely.But the intensity of pure epoxy resin material is poor, needs to be modified it.
Method of modifying common at present are as follows: phenolic resin is modified using epoxy resin, to improve phenolic resin
Intensity.But phenolic resin intensity prepared by the above method is still lower, is unable to satisfy people's requirement, limits phenolic aldehyde
The application range of resin.
Summary of the invention
The purpose of the present invention is to provide a kind of basalt fibre reinforced epoxy composite material and preparation methods, originally
The epoxy resin composite material intensity with higher provided is provided, and there is excellent heat resistance, it is multiple to expand epoxy
The application range of condensation material.
To achieve the goals above, the present invention provides a kind of preparations of basalt fibre reinforced epoxy composite material
Method, comprising the following steps:
(1) by graphene base-material dispersion liquid and epoxy resin-base heating mixing, graphene epoxy resin complex liquid is obtained；
(2) the graphene epoxy resin complex liquid that the step (1) obtains is mixed with basalt fibre, is poured
Material；
(3) castable that the step (2) obtains successively is poured, solidified and is cured, obtain basalt fibre increasing
Strong epoxy resin composite material.
Preferably, the mass ratio of the graphene base-material in the graphene base-material dispersion liquid and epoxy resin-base is 0.2
~0.4: 1.
Preferably, the graphene base-material dispersion liquid includes modified graphene dispersion liquid or graphene oxide dispersion；Institute
Modified graphene in modified graphene dispersion liquid is stated to be obtained by graphene through organosilane-modified；The graphene oxide dispersion
Middle graphene oxide is prepared by graphene through Hummers method.
Preferably, when the graphene base-material dispersion liquid is modified graphene dispersion liquid, the epoxy resin-base is
Epoxy resin.
Preferably, when the graphene base-material dispersion liquid is graphene oxide dispersion, the epoxy resin-base is
Epoxy resin latex, the preparation method of the epoxy resin latex the following steps are included:
(a) after mixing epoxy resin and propylene glycol monomethyl ether, 70~90 DEG C are heated to, then adds diethanol amine progress
Reaction, obtains reaction solution；
(b) after the reaction solution that the step (a) obtains being cooled to 55~65 DEG C, acetum is added dropwise, then adds
Water obtains epoxy resin latex.
Preferably, in the step (2) mass ratio of graphene epoxy resin complex liquid and basalt fibre be 1: 0.3~
0.5。
Preferably, the cured time is 12~15h in the step (3)；The time of the curing is 10 days or more.
The present invention also provides the basalt fibre reinforced epoxy trees that preparation method described in above-mentioned technical proposal is prepared
Resin composite material.
The present invention provides a kind of preparation methods of basalt fibre reinforced epoxy composite material, including following step
It is rapid: graphene base-material dispersion liquid and epoxy resin-base being mixed, graphene epoxy resin complex liquid is obtained；By graphene epoxy
Resin compounded liquid is mixed with basalt fibre, obtains pouring material；Castable is successively poured, solidified and cured, is obtained profound
Military rock fibre reinforced epoxy resin composite.The present invention is compound to basalt fibre reinforced epoxy using graphene base-material
The heat resistance of material is improved, and since graphene base-material has preferable thermal conductivity, heat dissipation is uniformly quick, and formed
Chemical bond stability is good, can also be improved the heat-resisting of the basalt fibre reinforced epoxy composite material being finally prepared
Property, while by adding graphene base-material in the epoxy, graphene base-material is generated with epoxy resin-base new
Be stably connected with key, in the case where not improving epoxy resin density substantially, so that the mechanical property of epoxy resin is improved.
In addition, the addition of basalt fibre, is conducive to the intensity for further increasing composite material and heat resistance.
Specific embodiment
The present invention provides a kind of preparation methods of basalt fibre reinforced epoxy composite material, including following step
It is rapid:
(1) by graphene base-material dispersion liquid and epoxy resin-base heating mixing, graphene epoxy resin complex liquid is obtained；
(2) the graphene epoxy resin complex liquid that the step (1) obtains is mixed with basalt fibre, is poured
Material；
(3) castable that the step (2) obtains successively is poured, solidified and is cured, obtain basalt fibre increasing
Strong epoxy resin composite material.
The present invention mixes graphene base-material dispersion liquid and epoxy resin-base, obtains graphene epoxy resin complex liquid.
In the present invention, the solvent of the graphene base-material dispersion liquid preferably includes acetone or water；The graphene base-material
The concentration of dispersion liquid is preferably 0.8~1.2g/L, further preferably 1.0~1.2g/L.In the present invention, described graphene-based
The mass ratio for expecting graphene base-material and epoxy resin-base in dispersion liquid is preferably 0.2~0.4: 1, and further preferably 0.3:
1.In the present invention, the graphene base-material dispersion liquid preferably includes modified graphene dispersion liquid and graphene oxide dispersion.
In the present invention, modified graphene is preferably organic by the way that graphene to be immersed in the modified graphene dispersion liquid
Modification obtains in solution of silane；The organosilan is preferably Silane coupling agent KH550；The quality of the organosilane solution is dense
Degree preferably 0.75%；The solvent of the organosilane solution is preferably that the mixing of dehydrated alcohol and water that volume ratio is 1: 1 is molten
Agent.In the present invention, the time of the immersion is preferably 25~35min, further preferably 30min.In the present invention, described
The ratio of graphene and organosilane solution is preferably 3g: 10mL；2 μm of the preferred < of the diameter of the graphene, thickness are preferably 1
~5nm, specific surface area are preferably 500m2/ g, density are preferably 2~2.25g/cm3, the preferred > 3000w/mK of thermal coefficient leads
Electrically preferably > 107S/m。
After obtaining modified graphene, present invention preferably employs the modes of ultrasonic disperse, and modified graphene is dispersed in acetone
In, obtain modified graphene dispersion liquid.
In the present invention, graphene oxide is prepared by graphene through Hummers method in the graphene oxide dispersion
It arrives；The preparation method of the graphene oxide preferably includes following steps:
Graphene, sodium nitrate and the concentrated sulfuric acid are mixed, potassium permanganate is then added at a temperature of ice-water bath and is reacted；So
Heated after water is added in backward reaction system, obtains reaction solution；
Aqueous hydrogen peroxide solution is added in above-mentioned reaction solution, is filtered while hot, then filter cake salt acid elution is dried, obtained
To graphene oxide.
In the present invention, the amount ratio of the graphene, sodium nitrate, the concentrated sulfuric acid and potassium permanganate is preferably 2~4g: 0.5
~1.5g: 65~70mL: 11~13g, further preferably 3g: 1g: 69mL: 12g.In the present invention, after potassium permanganate being added
Reaction preferably include two stages, first stage is preferably 10 DEG C or less reaction 0.5~1.5h, further preferably 8~
10 DEG C of reaction 1h；Second stage is preferably 1.8~2.2h of reaction at 30~40 DEG C, reacts 2h at further preferably 35 DEG C.
In the present invention, the temperature of the heat treatment is preferably 90~100 DEG C, and further preferably 95 DEG C, the time is preferably 25~
35min, further preferably 30min.In the present invention, the mass concentration of the aqueous hydrogen peroxide solution be preferably 25%~
35%, further preferably 30%.When aqueous hydrogen peroxide solution is added in reaction solution by the present invention, bubble is generated, peroxide is worked as
When changing aqueous solution of hydrogen addition to a certain extent, no longer generation bubble, the present invention are preferred by whether generating bubble to control peroxide
The additional amount for changing aqueous solution of hydrogen when no longer generating bubble stops that aqueous hydrogen peroxide solution is added.In the present invention, washing filter
The volume fraction of the hydrochloric acid of cake is preferably 8%~12%, and further preferably 10%.The present invention preferably passes through washing removal filter cake
In sulfate ion.The present invention does not specially require dry specific implementation method, ripe using those skilled in the art institute
The drying mode known.
After obtaining graphene oxide, present invention preferably employs the modes of ultrasonic disperse to be dispersed in water graphene oxide,
Obtain graphene oxide dispersion.
After obtaining graphene base-material dispersion liquid, the present invention mixes graphene base-material dispersion liquid and epoxy resin-base, obtains
To graphene epoxy resin complex liquid.
In the present invention, when the graphene base-material dispersion liquid is preferably modified graphene dispersion liquid, the graphene
Epoxy resin complex liquid is preferably modified graphene-epoxy resin complex liquid；The epoxy resin-base is preferably epoxy resin.
In the present invention, the epoxy resin preferably includes bisphenol A type epoxy resin, and the free phenol content of the epoxy resin is preferably small
In the solid content of 1.5%, epoxy resin be preferably 45%~55%, further preferably 50%, the room temperature viscosity of epoxy resin
Preferably 290~310Pa.s, further preferably 300Pa.s.In the present invention, the epoxide number of the epoxy resin is preferably
0.5eq/100g~0.7eq/100g, further preferably 0.6eq/100g.
Epoxy resin-base is preferably heated to 80 DEG C or more, further preferably 80~90 DEG C by the present invention, makes asphalt mixtures modified by epoxy resin
Aliphatic radical body is in flow regime, then by epoxy resin-base and graphene base-material dispersion liquid ultrasonic mixing, obtains modified graphite
Alkene-epoxy resin complex liquid.The present invention is conducive to improve composite material by mixing epoxy resin-base with modified graphene
Intensity, heat resistance and wear-resisting property.
In the present invention, when the graphene base-material dispersion liquid is preferably graphene oxide dispersion, the graphene
Epoxy resin complex liquid is preferably graphene oxide-epoxy resin complex liquid, and the epoxy resin-base is epoxy resin latex,
The preparation method of the epoxy resin latex preferably includes following steps:
(a) after mixing epoxy resin and propylene glycol monomethyl ether, 70~90 DEG C are heated to, then adds diethanol amine progress
Reaction, obtains reaction solution；
(b) after the reaction solution that the step (a) obtains being cooled to 55~65 DEG C, acetum is added dropwise, then adds
Water obtains epoxy resin latex.
After the present invention mixes epoxy resin and propylene glycol monomethyl ether, 70~90 DEG C are heated to, diethanol amine is then added
It is reacted, obtains reaction solution.
In the present invention, the mass ratio of the epoxy resin and propylene glycol monomethyl ether preferably 1.5~2.5: 1, further preferably
It is 2: 1.Epoxy resin and propylene glycol monomethyl ether are preferably heated to 70~90 DEG C, further preferably 80 DEG C by the present invention.The present invention
It is preferred that diethanol amine is added into the solution after epoxy resin and propylene glycol monomethyl ether heating, reacted.In the present invention, described
The mass ratio of epoxy resin and diethanol amine is preferably 4.5~5.5: 1, further preferably 5: 1.In the present invention, described anti-
The temperature answered is preferably 70~90 DEG C, and further preferably 80 DEG C, the time is preferably 2~2.5h.
After obtaining reaction solution, after reaction solution is cooled to 55~65 DEG C by the present invention, acetum, heat preservation a period of time is added dropwise
Afterwards, water is added, epoxy resin-base is obtained.
Reaction solution is preferably cooled to 60 DEG C by the present invention, and acetum is then added dropwise.In the present invention, the acetum
Mass fraction be preferably 15%~25%, further preferably 20%.The present invention be added acetum after, preferably keep the temperature 25~
35min, further preferably 30min.
After obtaining epoxy resin-base, the present invention mixes graphene oxide dispersion with epoxy resin-base, obtains oxygen
Graphite alkene-epoxy resin complex liquid；The mixing is preferably ultrasonic mixing, specific implementation of the present invention to the ultrasonic mixing
Mode does not have particular/special requirement, to be able to achieve the uniform mixing of graphene oxide dispersion and epoxy resin-base.The present invention
By mixing epoxy resin-base with graphene oxide dispersion, be conducive to improve the intensity of composite material, heat resistance and resistance to
Grind performance.
After obtaining graphene epoxy resin complex liquid, the present invention mixes graphene epoxy resin complex liquid with basalt fibre
It closes, obtains pouring material.
In the present invention, the mass ratio of the graphene epoxy resin complex liquid and basalt fibre be preferably 1: 0.3~
0.5, further preferably 1: 0.4.The present invention does not specially require basalt fibre, using commercially available basalt fibre.
The specific embodiment that the present invention mixes graphene epoxy resin complex liquid with basalt fibre does not have particular/special requirement, can make profound
Military rock fiber comes into full contact with graphene epoxy resin complex liquid, obtains the uniform pouring material of component.In the present invention, institute
State intensity, heat resistance and wear-resisting property that basalt fibre is conducive to improve composite material.
After obtaining castable, the castable is successively poured, solidified and cured by the present invention, obtains basalt fibre
Reinforced epoxy composite material.
In the present invention, the temperature of the casting is preferably 60~65 DEG C, and more preferably 60~63 DEG C.When pouring, this hair
It is bright that preferably the castable poured to mold is vibrated, the gas in castable is discharged, improve epoxy resin composite wood
Expect the uniformity of mechanical property.The present invention does not have particular/special requirement to the mode for pouring and vibrating, using those skilled in the art
Known to member.The present invention does not have particular/special requirement with mold to described pour, and according to actual needs, selects the mould of suitable dimension
Tool.In embodiments of the present invention, the test sample is preferably dimensioned to be outer diameter 10cm, wall thickness 1cm, the pipe of length 50cm
Shape material.
After pouring, the present invention preferably solidifies the material after pouring, it is described solidify preferably include successively to carry out it is solidifying
Glue and two stages of solidification.The present invention is in gel phase, the mixing of the basalt fibre and graphene epoxy resin complex liquid
Object is still liquid, and can be applied in suitable working environment；In order to guarantee reliably to be bonded, work is all constructed and positioned
Work should be carried out in gel phase.After gel, gel masses enter solidification stages, and the present invention is in solidification stages, the Black Warrior
Rock fiber and the mixture of graphene epoxy resin complex liquid initially enter solidification phase, at this moment the mixture start solidification or
" mutation "；In this stage any interference cannot be carried out to the mixture；The mixture will become soft solidifying as hard rubber
Glue object.In the present invention, the cured time is preferably 12~15h, further preferably 13~14h.
After the completion of solidification, material is carried out maturation process by the present invention, obtains basalt fibre reinforced epoxy composite wood
Material.
In the present invention, the temperature of the curing is preferably room temperature；The time of the curing is preferably 10~25 days, more excellent
It is selected as 15~21 days.
The present invention preferably after the completion of curing, is demoulded, and basalt fibre reinforced epoxy composite material is obtained.This
The specific embodiment of demoulding is not particularly limited in invention, using stripping means well-known to those skilled in the art.
In the present invention, in the above specific embodiment, unless otherwise specified, the reagent is those skilled in the art
Well known commercial product.
The basalt fibre reinforced epoxy obtained the present invention also provides preparation method described in above-mentioned technical proposal is multiple
Condensation material.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.
Embodiment 1
(1) graphene is immersed in the Silane coupling agent KH550 solution that mass concentration is 0.75% (solvent is second alcohol and water
The mixed solvent that volume ratio is 1: 1) in, drying is taken out after impregnating 30min at room temperature, obtains modified graphene powder；
(2) modified graphene powder is added in acetone, is then placed it in Ultrasound Instrument to mixed solution ultrasound
Reason, is prepared into finely dispersed modified graphene dispersion liquid；
(3) bisphenol A epoxide resin is heated to 80 DEG C of softening temperature, is at melt-flow state, be then added and change
Property graphene dispersing solution, after being mixed slowly using blender again quickly stirring to be uniformly mixed, formed modified graphene-asphalt mixtures modified by epoxy resin
Rouge complex liquid；Wherein the mass ratio of the quality of modified graphene and epoxy resin is 0.3: 1 in modified graphene dispersion liquid；
(4) basalt fibre is put into modified graphene-epoxy resin complex liquid and is sufficiently infiltrated, obtain pouring liquid,
The weight of middle basalt fibre accounts for modified graphene-epoxy resin complex liquid weight 30%；
(5) liquid that pours in step (4) is poured into mold, bubble is discharged using vibratory drilling method, until reaching design thickness, according to
It is secondary by gel, solidification and curing three phases after, one demould, obtain basalt fibre reinforced epoxy composite material.
Embodiment 2
(1) graphene oxide is prepared using improvement Hummers method: 3g graphite powder and 1g sodium nitrate is added dense equipped with 69mL
In the three-necked flask of sulfuric acid, it is slowly added to 12g potassium permanganate under stirring in ice-water bath, in 10 DEG C or less reaction 1h；It is warming up to 35
DEG C or so, continue to stir 2h；It is slowly added to 120mL deionized water, system temperature is made to be increased to 95 DEG C or so, 30min is maintained, adds
Enter a large amount of distilled water dilutions, pouring into mass concentration is 30%H2O2It generates to no bubble, filters while hot, and with HCl (volume ratio
It is 1: 10) washs filter cake, until without SO in filtrate4 2-(BaCl2Detection), it is dried to obtain graphene oxide；Graphite oxide is dissolved in
In water, ultrasound is allowed to be completely dispersed, and obtains graphene oxide dispersion；
(2) 50g epoxy resin and 25g propylene glycol monomethyl ether are added in three-necked flask, are warming up to 80 DEG C, it is slow under stirring
10.5g diethanol amine is added dropwise, reacts 2h；Then 60 DEG C are cooled to, the acetum that mass concentration is 20% is added dropwise and reacts
30min is then slowly added into the quick stirring and emulsifying of distilled water and obtains epoxy resin-base；
(3) graphene oxide dispersion is added in epoxy resin-base, wherein modified stone in modified graphene dispersion liquid
The quality of black alkene and the mass ratio of epoxy resin-base are 0.3: 1；Ultrasound 1h is stirred, 3h is kept the temperature at 60 DEG C, then proceedes to surpass
Sound 30min, filtering, obtains graphene oxide-epoxy resin complex liquid；
(4) basalt fibre is put into graphene oxide-epoxy resin complex liquid and is sufficiently infiltrated, obtain pouring liquid,
The weight of middle basalt fibre accounts for graphene oxide-epoxy resin complex liquid weight 50%；
(5) liquid that pours in step (4) is poured into mold, bubble is discharged using vibratory drilling method, until reaching design thickness, according to
It is secondary by gel, solidification and curing three phases after, one demould, obtain basalt fibre reinforced epoxy composite material.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of basalt fibre reinforced epoxy composite material, comprising the following steps:
(1) by graphene base-material dispersion liquid and epoxy resin-base heating mixing, graphene epoxy resin complex liquid is obtained；
(2) the graphene epoxy resin complex liquid that the step (1) obtains is mixed with basalt fibre, obtains pouring material；
(3) castable that the step (2) obtains successively is poured, solidified and is cured, obtain basalt fibre enhancing ring
Epoxy resin composite material.
2. preparation method according to claim 1, which is characterized in that graphene-based in the graphene base-material dispersion liquid
The mass ratio of material and epoxy resin-base is 0.2~0.4: 1.
3. preparation method according to claim 1, which is characterized in that the graphene base-material dispersion liquid includes modified graphite
Alkene dispersion liquid or graphene oxide dispersion；Modified graphene is by graphene through organosilan in the modified graphene dispersion liquid
Modification obtains；Graphene oxide is prepared by graphene through Hummers method in the graphene oxide dispersion.
4. described in any item preparation methods according to claim 1~3, which is characterized in that when the graphene base-material dispersion liquid
When for modified graphene dispersion liquid, the epoxy resin-base is epoxy resin.
5. described in any item preparation methods according to claim 1~3, which is characterized in that when the graphene base-material dispersion liquid
When for graphene oxide dispersion, the epoxy resin-base is epoxy resin latex, the preparation side of the epoxy resin latex
Method the following steps are included:
(a) after mixing epoxy resin and propylene glycol monomethyl ether, 70~90 DEG C are heated to, diethanol amine is then added and carries out instead
It answers, obtains reaction solution；
(b) after the reaction solution that the step (a) obtains being cooled to 55~65 DEG C, acetum is added dropwise, then adds water, obtains
To epoxy resin latex.
6. preparation method according to claim 1, which is characterized in that graphene epoxy resin is compound in the step (2)
The mass ratio of liquid and basalt fibre is 1: 0.3~0.5.
7. preparation method according to claim 1, which is characterized in that in the step (3) the cured time be 12~
15h；The time of the curing is 10 days or more.
8. the basalt fibre reinforced epoxy composite material that any one of claim 1~7 preparation method is prepared.
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Cited By (3)
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| CN113845756A (en) * | 2021-11-04 | 2021-12-28 | 西南石油大学 | Preparation method of basalt fiber composite material |
| CN114193687A (en) * | 2021-12-01 | 2022-03-18 | 重庆智笃新材料科技有限公司 | Fiber insulation ribbon and preparation process thereof |
| CN117304648A (en) * | 2023-08-25 | 2023-12-29 | 长春盛达化工制品有限公司 | Preparation method of main insulating plate of super-hydrophobic circuit breaker |
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| KR20180042978A (en) * | 2016-10-19 | 2018-04-27 | 인하대학교 산학협력단 | Graphene oxide synthesized from pitch-based carbon fiber and manufacturing method thereof |
| CN108676326A (en) * | 2018-05-08 | 2018-10-19 | 黄河科技学院 | Graphene based on epoxy resin and glass fiber reinforcement plank |
| CN109265917A (en) * | 2018-07-20 | 2019-01-25 | 黄河科技学院 | Basalt fibre reinforced epoxy board making and stress measuring method |
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| KR20180042978A (en) * | 2016-10-19 | 2018-04-27 | 인하대학교 산학협력단 | Graphene oxide synthesized from pitch-based carbon fiber and manufacturing method thereof |
| CN107892792A (en) * | 2017-11-01 | 2018-04-10 | 成都天府轨谷科技有限公司 | A kind of basalt fiber composite material containing epoxy resin and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114193687A (en) * | 2021-12-01 | 2022-03-18 | 重庆智笃新材料科技有限公司 | Fiber insulation ribbon and preparation process thereof |
| CN117304648A (en) * | 2023-08-25 | 2023-12-29 | 长春盛达化工制品有限公司 | Preparation method of main insulating plate of super-hydrophobic circuit breaker |
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