CN106189092B - A kind of fiber reinforcement flame-retarded light high-strength composite material and preparation method thereof - Google Patents
A kind of fiber reinforcement flame-retarded light high-strength composite material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5317—Phosphonic compounds, e.g. R—P(:O)(OR')2
- C08K5/5333—Esters of phosphonic acids
- C08K5/5357—Esters of phosphonic acids cyclic
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses a kind of fiber reinforcement flame-retarded light high-strength composite materials and preparation method thereof, which is made of the raw material of following mass percent：Epoxy resin 23~36%, curing agent 5~20%, diluent 10~24%, hollow glass micropearl 16~36%, phosphonium flame retardant modified carbon fiber 8~20%, the phosphonium flame retardant modified carbon fiber uses chopped carbon fiber surface grafting phosphonium flame retardant, a diameter of 7 12 μm of the chopped carbon fiber, draw ratio are 7 15：1.In the present invention, the phosphonium flame retardant modified carbon fiber is added in composite material, the mechanical property of composite material can not only be improved, and, ensure the flame retardant property of composite material, take into account flame retardant property and mechanical property, while use phosphonium flame retardant modified carbon fiber, it reduces the influence to composite density to the greatest extent, prepares a kind of high-strength lightweight composite material.
Description
Technical field
The present invention relates to light composite material fields, and in particular to a kind of fiber reinforcement flame-retarded light high-strength composite material and
Preparation method.
Background technology
Lightweight high-strength 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.Lightweight high-strength composite material belongs to field of new materials.But in application process, it is desirable that high-strength light
Composite material has relatively low density and higher incompressible intensity in itself, while has certain anti-flammability.Halogen containing flame-retardant
Although flame retarding efficiency is high, the poisonous smoke of releasing has been replaced at this stage by halogen-free flame retardants gradually in flame retardant area.It passes
Halogen-free flame retardants (aluminium hydroxide, magnesium hydroxide) additive amount of uniting is high, increases the density of material, is not suitable for applied to light material
It is fire-retardant, although and the addition of halogen-free expanded flame-retardant agent can improve the flame retardant property of material, the addition of fire retardant is to a certain degree
On can increase material density and reduce material mechanical property, so take into account flame retardant property and mechanical property just become a urgency
It need to solve the problems, such as.
It is hindered as patent of invention " a kind of Flame retardant solid buoyancy material and preparation method thereof " (CN201110118095.3) is open
Combustion solid buoyancy material contains the component in terms of mass parts as follows：100 parts of epoxy resin；15~30 parts of halogen containing flame-retardant；It is inorganic
7~15 parts of fire retardant；12~20 parts of active flame-proof diluent；1~4 part of foaming agent；0.15~0.3 part of wetting dispersing agent；Promote
0.5~1 part of agent；90~130 parts of curing agent；20~150 parts of hollow glass micropearl.The technical solution used halogen containing flame-retardant and
The fire-retardant mode that inorganic combustion inhibitor and halogen diluent are combined carries out fire-retardant, but this flame resistant method is had ignored to compound
The influence of density of material and mechanical property.
Patent of invention " a kind of halogen-free flameproof solid buoyancy material and preparation method thereof " (CN201410049812.5) is open
Halogen-free flameproof solid buoyancy material contains the component of following parts by weight meter：100 parts of epoxy resin, hollow glass micropearl 25~100
Part, 10~20 parts of diluent, 50~80 parts of curing agent, 0.1~3 part of catalyst, poly- phosphamide flame-proof modifier 5~30%.Its
Described in poly- phosphamide flame-proof modifier be by surface cause polycondensation reaction, grafted on hollow glass micropearl table
Face because of its phosphorus and nitrogen with high-content, makes hollow glass micropearl have superior flame retardant property；In addition, its end is also contained
One amino when being mixed with epoxy resin, can cure together with matrix, enhance between hollow glass micropearl and epoxy matrix
Interface cohesion reduces material internal defect.The technical solution is grafted the method for halogen-free flame retardants to multiple on hollow glass micropearl
Condensation material progress is fire-retardant, although preferable flame retardant effect can be obtained, the hollow glass micropearl density after grafting rises, together
When mechanical property can also be affected.
So flame retardant property and mechanical property are taken into account, while the influence reduced to the greatest extent to composite density just becomes one
Urgent problem.And fibrous material can increase the mechanical property of composite material, but flame retardant property does not reach requirement, institute
A kind of fibrous material of expanding fire retardant cladding is prepared with the present invention, by application and light composite material, expanding fire retardant
The mechanical property of material, the mechanics enhancing of binding fiber material and the flame retardant property of expanding fire retardant can be increased, prepare one
Kind high-strength lightweight composite material.
Invention content
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of fiber reinforcement flame-retarded light is high-strength multiple
Condensation material and preparation method thereof, by chopped carbon fiber surface grafting phosphonium flame retardant, and by the flame retardant type carbon fiber of acquisition
It is added in epoxy resin composite material system, improves the intensity of epoxy composite material system, and improves the flame retardant property of material,
To meet the needs of high-strength light epoxy composite material application field.
The technical solution adopted by the present invention is as described below.
A kind of fiber reinforcement flame-retarded light high-strength composite material, is made of the raw material of following mass percent：
The phosphonium flame retardant modified carbon fiber uses chopped carbon fiber surface grafting phosphonium flame retardant, and described is chopped
A diameter of 7-12 μm of carbon fiber, draw ratio 7-15：1.
In the present invention, using chopped carbon fiber surface grafting phosphonium flame retardant, the undulation degree coated using expanding fire retardant
Material not only improves the mechanical property of composite material, moreover, ensureing the flame retardant property of composite material, takes into account flame retardant property and mechanics
Performance, while phosphonium flame retardant modified carbon fiber is used, it reduces the influence to composite density to the greatest extent, prepares a kind of high-strength
Light composite material.
It is used as the preferred technical solution of the present invention below：
Epoxy resin used in the present invention includes glycidyl type epoxy resin (E-51, FarBond LY of such as bisphenol A-type
1564th, 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).The i.e. described epoxy resin is glycidyl type epoxy resin, epoxidation of olefins class asphalt mixtures modified by epoxy resin
One or more of fat, heterocyclic type and mixed type epoxy resin (including two kinds).
The curing agent is the system to match with epoxy resin, and type includes anhydride and polynary amine such as amine
3486, phthalic anhydride, maleic anhydride, the methyl tetrahydro phthalic anhydride of anhydride.
Diluent used in the present invention is for reducing system viscosity, in order to which high heat conducting nano particle can disperse well
In epoxy resin-base, reactive diluent and non-activated thinner, the present invention used in be non-activated thinner third
Ketone, it is the reaction rate in order to improve anhydride curing system to add in accelerating agent.The diluent is acetone.
A diameter of 10 μm -120 μm of the hollow glass micropearl, preferably compression strength are more than the hollow glass of 20MPa
Microballon.
The chopped carbon fiber uses acrylonitrile base carbon fiber.
The phosphonium flame retardant is the miscellaneous -10- phospho hetero phenanthrenes -10- oxides of 9,10- dihydro-9-oxies.
The fiber reinforcement flame-retarded light high-strength composite material, is made of the raw material of following mass percent：
The phosphonium flame retardant modified carbon fiber uses chopped carbon fiber surface grafting phosphonium flame retardant, and described is chopped
A diameter of 7-12 μm of carbon fiber, draw ratio 7-15：1.
The preparation of the phosphonium flame retardant modified carbon fiber includes：
(1) surface hydroxylation of chopped carbon fiber：Chopped carbon fiber is added in the concentrated sulfuric acid, then ultrasonic disperse heats
Reflux, mixture then filtered and be washed with deionized, and vacuum drying obtains the hydroxylating carbon fibre material containing hydroxyl.
The mass percent of the concentrated sulfuric acid is 70%~99%.
The chopped carbon fiber and the mass ratio of the concentrated sulfuric acid are 1：5~15, further preferably 1：10.
The time of the ultrasonic disperse is 5~15min, further preferably 10min.
The condition being heated to reflux is：Flow back 1~3h at 120~140 DEG C, further preferably, in 130 DEG C of reflux
2h。
(2) silane-modified phosphonium flame retardant：It is separately added into 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide,
The item of vinyl methyl dimethoxysilane and solvent chloroform and initiator azodiisobutyronitrile, mechanical agitation and nitrogen protection
Under part, heating maintains the reflux for 10~16h, filters, dry, obtains silicone-modified phosphonium flame retardant；
Miscellaneous -10- phospho hetero phenanthrenes -10- the oxides of the 9,10- dihydro-9-oxies, vinyl methyl dimethoxysilane and idol
The mass ratio of nitrogen bis-isobutyronitrile is 49~59：28~38：0.5~1.5, further preferably 54：33：1, solvent chloroform is in right amount
Can, solute can be dissolved by being subject to.
The temperature maintained the reflux for is 60~64 DEG C, further preferably 62 DEG C, the about boiling point of chloroform.
(3) preparation of phosphonium flame retardant modified carbon fiber：Hydroxylating carbon fibre material containing hydroxyl and ethyl alcohol are mixed,
Silicone-modified phosphonium flame retardant is added in again, is gradually heated to reflux under nitrogen protection and stirring condition, is finally taken
Go out filtering, and washed with ethyl alcohol, vacuum drying obtains phosphonium flame retardant modified carbon fiber.
The mass ratio of the hydroxylating carbon fibre material containing hydroxyl and silicone-modified phosphonium flame retardant is 10：
5~20, further preferably 10：10.
Described to be heated to reflux as the 8~12h that flow back at 70 DEG C~90 DEG C, further preferably flow back 10h at 80 DEG C.
A kind of preparation process of fiber reinforcement flame-retarded light high-strength composite material of the present invention is as follows：First by suitable ring
Oxygen resin is added in organic solvent-acetone, then sequentially adds the reagents such as flame-retardant modified carbon fiber, diluent, curing agent, most
After add in hollow glass micropearl.Deaeration is mixed in high speed rotation deaeration machine after mixed liquor ultrasonic disperse, removes organic solvent
Mixture is poured into steel die to be cured according to certain curing cycle, is demoulded up to fiber reinforcement flame-retarded light high-strength compound
Material.The composite material of acquisition carries out oxygen index (OI) test and incompressible strength test.
A kind of preparation method of fiber reinforcement flame-retarded light high-strength composite material, includes the following steps：
Extracting epoxy resin is mixed into acetone, then adds in phosphonium flame retardant modified carbon fiber and curing agent, forms mixed liquor,
After ultrasonic disperse, hollow glass micropearl is added in, mixes deaeration in deaeration machine is rotated, the mixture for removing organic solvent pours into
Cure in mold, demould up to fiber reinforcement flame-retarded light high-strength composite material.
Mix deaeration 5min~15min, preferably 10min.
Compared with prior art, the invention has the advantages that：
In the present invention, using chopped carbon fiber surface grafting phosphonium flame retardant, phosphonium flame retardant modified carbon fiber is obtained, and
The phosphonium flame retardant modified carbon fiber is added in composite material, can not only improve the mechanical property of composite material, moreover,
Ensure the flame retardant property of composite material, take into account flame retardant property and mechanical property, while use phosphonium flame retardant modified carbon fiber, to the greatest extent
Amount reduces the influence to composite density, prepares a kind of high-strength lightweight composite material.Composite material of the present invention it is comprehensive
Can be excellent, it is easy to market-oriented utilization and extention, has wide application prospect.
Specific embodiment
The preferred embodiment of the present invention is given below, these embodiments not limit present disclosure.
Embodiment 1
The preparation process of phosphonium flame retardant modified carbon fiber includes the following steps：
(1) surface hydroxylation of chopped carbon fiber：Chopped carbon fiber is added to containing the concentrated sulfuric acid (chopped carbon fiber use
Acrylonitrile base carbon fiber, a diameter of 7-12 μm of chopped carbon fiber, draw ratio 7-15：1, carbon fiber is with concentrated sulfuric acid mass ratio
1：10, the mass percent of the concentrated sulfuric acid is in three-necked flask 85%), ultrasonic disperse 10min is then slowly heated to 130 DEG C
Flow back 2h, then filters mixture and is washed with deionized repeatedly, it is fine that vacuum drying obtains the hydroxylating carbon containing hydroxyl
Tie up material.
(2) silane-modified phosphonium flame retardant：9,10- dihydro-9-oxies are separately added into the three neck round bottom flask of 500ml
Miscellaneous -10- phospho hetero phenanthrenes -10- oxides (54g), vinyl methyl dimethoxysilane (33g) and solvent chloroform (200ml) and
Under conditions of 1g initiator azodiisobutyronitriles, mechanical agitation and nitrogen protection, it is gradually warming up to 62 DEG C of (about boilings of chloroform
Point), 12h is maintained the reflux for, is filtered, it is dry, you can to obtain silicone-modified phosphonium flame retardant.
(3) phosphonium flame retardant modified carbon fiber：By the hydroxylating carbon fibre material containing hydroxyl of 10g and the nothing of 200ml
Water-ethanol is added in 500ml three-necked flasks, then phosphonium flame retardant silicone-modified 10g is added in mixed system, in nitrogen
80 DEG C of reflux 10h are gradually heated under gas shielded and stirring condition, are finally drawn off filtering, and washed 3 times with absolute ethyl alcohol,
Vacuum drying obtains phosphonium flame retardant modified carbon fiber.
Embodiment 2
Take bisphenol A type epoxy resin E51 (average epoxy value 51/100=0.51, epoxide number N/100 are 0.48-0.54)
50g dissolves in 30g and is mixed into acetone, adds the phosphonium flame retardant modified carbon fiber 20g of the preparation of embodiment 1, curing agent methyl four
Hydrogen phthalic anhydride 25g, after mixed liquor ultrasonic disperse, adding in 3M companies hollow glass micropearl, (S32, the diameter of hollow glass micropearl is in 80 μ
Within m) 36g, deaeration 10min is mixed in high speed rotation deaeration machine, the mixture for removing organic solvent is poured into steel die
Cured according to certain curing cycle, condition of cure is 80 DEG C of * 1h+120 DEG C * 2h+140 DEG C * 4h, is demoulded up to fiber reinforcement
Flame-retarded light high-strength composite material.
The oxygen index (OI) of composite material can reach 26, density 0.64g/cm3, incompressible intensity can reach 35MPa.
Comparative example 1
Take bisphenol A type epoxy resin E51 (average epoxy value 51/100=0.51, epoxide number N/100 are 0.48-0.54)
50g dissolves in 30g and is mixed into acetone, adds chopped carbon fiber 10g and the miscellaneous -10- phospho hetero phenanthrenes -10- oxidations of 9,10- dihydro-9-oxy
Object 10g, curing agent methyl tetrahydro phthalic anhydride 25g, after mixed liquor ultrasonic disperse, add in 3M companies hollow glass micropearl (S32, it is hollow
The diameter of glass microballoon is within 80 μm) 36g, deaeration 10min is mixed in high speed rotation deaeration machine, removes the mixed of organic solvent
It closes object and pours into steel die and cured according to certain curing cycle, condition of cure is 80 DEG C of * 1h+120 DEG C * 2h+140 DEG C *
4h is demoulded up to fiber reinforcement flame-retarded light high-strength composite material.
The oxygen index (OI) of composite material can reach 24, density 0.71g/cm3, incompressible intensity can reach 28MPa.
Embodiment 3
1564 50g of bisphenol A type epoxy resin FarBond LY is taken to be mixed into 30g to be dissolved in acetone, embodiment 1 is added and makes
Standby 3486 17g of phosphonium flame retardant modified carbon fiber 30g, curing agent FarBond LY add in 3M companies hollow glass micropearl
(S38, the diameter of hollow glass micropearl is within 85 μm) 55g is mixed in high speed rotation deaeration machine after mixed liquor ultrasonic disperse
Deaeration 10min, the mixture for removing organic solvent are poured into steel die and are cured according to certain curing cycle, curing cycle
For 100 DEG C of * 1h, demould up to fiber reinforcement flame-retarded light high-strength composite material.
The oxygen index (OI) of composite material can reach 28, density 0.65g/cm3, incompressible intensity can reach 55MPa.
Comparative example 2
1564 50g of bisphenol A type epoxy resin FarBond LY is taken to be mixed into 30g to be dissolved in acetone, it is fine to add chopped carbon
15g and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide 15g, 3486 17g of curing agent FarBond LY are tieed up, is added in
3M companies hollow glass micropearl (S38, the diameter of hollow glass micropearl is within 85 μm) 55g, in height after mixed liquor ultrasonic disperse
Deaeration 10min is mixed in fast rotation deaeration machine, the mixture for removing organic solvent is poured into steel die according to certain curing system
Degree is cured, and curing cycle is 100 DEG C of * 1h, is demoulded up to fiber reinforcement flame-retarded light high-strength composite material.
The oxygen index (OI) of composite material can reach 26, density 0.72g/cm3, incompressible intensity can reach 45MPa.
The phosphonium flame retardant modified carbon fiber that embodiment 2 uses, comparative example 1 use non-grafted chopped carbon fiber and 9,
Miscellaneous -10- phospho hetero phenanthrenes -10- the oxides of 10- dihydro-9-oxies, the oxygen index (OI) of 2 composite material of embodiment is 26, and the oxygen of comparative example 1 refers to
Number is 24, although the flame retardant property of embodiment 2 is slightly better than comparative example 1, the two is not much different, and the density of comparative example 1 is opposite
There is apparent increase in embodiment 2, the incompressible intensity of embodiment 2 will be substantially better than comparative example 1.
The phosphonium flame retardant modified carbon fiber that embodiment 3 uses, comparative example 2 use non-grafted chopped carbon fiber and 9,
Miscellaneous -10- phospho hetero phenanthrenes -10- the oxides of 10- dihydro-9-oxies, the oxygen index (OI) of 3 composite material of embodiment is 28, and the oxygen of comparative example 1 refers to
Number is 26, although the flame retardant property of embodiment 3 is slightly better than comparative example 2, the two is not much different, and the density of comparative example 2 is opposite
There is apparent increase in embodiment 3, the incompressible intensity of embodiment 3 will be substantially better than comparative example 2.
As it can be seen that using chopped carbon fiber surface grafting phosphonium flame retardant, phosphonium flame retardant modified carbon fiber is obtained, and should
Phosphonium flame retardant modified carbon fiber is added in composite material, can not only improve the mechanical property of composite material, moreover, ensureing
The flame retardant property of composite material takes into account flame retardant property and mechanical property, while uses phosphonium flame retardant modified carbon fiber, subtracts as possible
A kind of high-strength lightweight composite material is prepared in few influence to composite density.
There are many concrete application approach of the present invention, and the above is only the 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 fiber reinforcement flame-retarded light high-strength composite material, which is characterized in that be made of the raw material of following mass percent：
The phosphonium flame retardant modified carbon fiber uses chopped carbon fiber surface grafting phosphonium flame retardant, and the chopped carbon is fine
A diameter of 7-12 μm of dimension, draw ratio 7-15：1；
The preparation of the phosphonium flame retardant modified carbon fiber includes：
(1) chopped carbon fiber is added in the concentrated sulfuric acid, then ultrasonic disperse is heated to reflux, then mixture is filtered and spent
Ion water washing, vacuum drying obtain the hydroxylating carbon fibre material containing hydroxyl；
(2) be separately added into the miscellaneous -10- phospho hetero phenanthrenes -10- oxides of 9,10- dihydro-9-oxies, vinyl methyl dimethoxysilane and
Under conditions of solvent chloroform and initiator azodiisobutyronitrile, mechanical agitation and nitrogen protection, heating maintains the reflux for 10~
16h is filtered, dry, obtains silicone-modified phosphonium flame retardant；
(3) the hydroxylating carbon fibre material containing hydroxyl and ethyl alcohol are mixed, then silicone-modified phosphonium flame retardant are added in,
It is gradually heated to reflux under nitrogen protection and stirring condition, is finally drawn off filtering, and washed with ethyl alcohol, be dried in vacuo to obtain the final product
To phosphonium flame retardant modified carbon fiber；
The chopped carbon fiber uses acrylonitrile base carbon fiber.
2. fiber reinforcement flame-retarded light high-strength composite material according to claim 1, which is characterized in that the diluent
For acetone.
3. fiber reinforcement flame-retarded light high-strength composite material according to claim 1, which is characterized in that the hollow glass
A diameter of 10 μm -120 μm of glass microballon.
4. fiber reinforcement flame-retarded light high-strength composite material according to claim 1, which is characterized in that in step (1), institute
The mass percent for the concentrated sulfuric acid stated is 70%~99%；
The chopped carbon fiber and the mass ratio of the concentrated sulfuric acid are 1：5~15；
The time of the ultrasonic disperse is 5~15min；
The condition being heated to reflux is：Flow back 1~3h at 120~140 DEG C.
5. fiber reinforcement flame-retarded light high-strength composite material according to claim 1, which is characterized in that in step (2), institute
Miscellaneous -10- phospho hetero phenanthrenes -10- the oxides of 9,10- dihydro-9-oxies, vinyl methyl dimethoxysilane and the azodiisobutyronitrile stated
Mass ratio be 49~59：28~38：0.5~1.5.
6. fiber reinforcement flame-retarded light high-strength composite material according to claim 1, which is characterized in that in step (3), institute
The mass ratio of the hydroxylating carbon fibre material containing hydroxyl stated and silicone-modified phosphonium flame retardant is 10：5~20.
7. fiber reinforcement flame-retarded light high-strength composite material according to claim 1, which is characterized in that in step (3), institute
That states is heated to reflux as the 8~12h that flows back at 70 DEG C~90 DEG C.
It is 8. special according to the preparation method of claims 1 to 3 any one of them fiber reinforcement flame-retarded light high-strength composite material
Sign is, includes the following steps：
Extracting epoxy resin is mixed into acetone, then adds in phosphonium flame retardant modified carbon fiber and curing agent, forms mixed liquor, through super
After sound dispersion, hollow glass micropearl is added in, mixes deaeration in deaeration machine is rotated, the mixture for removing organic solvent pours into mold
Middle curing is demoulded up to fiber reinforcement flame-retarded light high-strength composite material.
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| CN107501856B (en) * | 2017-09-30 | 2020-04-24 | 南京林业大学 | Preparation method of flame-retardant modified wood fiber composite phenolic foam |
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