CN109181231A - A kind of preparation method of modified carbon fiber-epoxy resin composite material - Google Patents
A kind of preparation method of modified carbon fiber-epoxy resin composite material Download PDFInfo
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- CN109181231A CN109181231A CN201811046853.3A CN201811046853A CN109181231A CN 109181231 A CN109181231 A CN 109181231A CN 201811046853 A CN201811046853 A CN 201811046853A CN 109181231 A CN109181231 A CN 109181231A
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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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K9/00—Use of pretreated ingredients
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- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0856—Iron
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of preparation methods of modified carbon fiber-epoxy resin composite material, belong to technical field of polymer materials.The present invention mixes carbon fiber with sodium hydroxide solution, impregnates, filtering, and Freezing smashing washs, dry, obtains single treatment carbon fiber；By supernatant, single treatment carbon fiber, saccharomycete, deionized water mixed fermentation, then dropwise addition iron nitrate solution is stirred, and is filtered, and is washed, dry, isothermal holding, and cooling obtains secondary treatment carbon fiber；It is dry by secondary treatment carbon fiber water steam treatment, obtain modified carbon fiber；By epoxy resin, diluent, modified carbon fiber, curing agent, nanometer iron powder is stirred, and applies magnetic field, injection molding, compression moulding demoulds to get modified carbon fiber-epoxy resin composite material.Modified carbon fiber-epoxy resin composite material provided by the invention has excellent electromagnetic shielding performance and mechanical property.
Description
Technical field
The invention discloses a kind of preparation methods of modified carbon fiber-epoxy resin composite material, belong to high molecular material
Technical field.
Background technique
Modern times require to favor conductive polymer material more and more to the lighting of computer and electronic device.
The advantages that conductive polymer material shell is due to its low-density, high specific strength and good electromagnetic compatibility characteristic and gradually replace original
The metal shell come, is widely applied in computer and electronic device.High molecular material and conductive particle, conductive fiber etc. are led
Electric filler progress is compound, is a kind of important method for preparing conductive polymer material.Conductive filler is diversified, carbon fiber
The advantages that due to its high specific strength, low-density, corrosion-resistant, high temperature resistant, strong environment resistant ability and in conductive polymer material field
Widely paid close attention to.It is intrinsic due to itself but when carbon fiber is used as the conductive filler of conductive polymeric composite
Resistivity is relatively high and process in be easily broken, keep the resistivity of composite material relatively high.After carbon fiber surface metallization
It can solve these problems.Compared with carbon fiber, nickel-coated carbon fibers have higher electric conductivity, therefore the addition of nickel-coated carbon fibers
The shield effectiveness of composite material can more greatly be improved.
Chemical plating is an important method of carbon fiber surface nickel plating, and researcher also has been devoted to carbon fiber surface chemistry
The research of nickel plating and its composite material electromagnetic performance, but the research of the influence factor to the composite material screening ability of different frequency range
It is also rarely found.At present traditional modified carbon fiber-epoxy resin composite material there is also electromagnetic shielding performance and mechanical properties not
Good problem also needs to study it.
Summary of the invention
The present invention solves the technical problem of: for traditional modified carbon fiber-epoxy resin composite material electromagnetic screen
Performance and the bad problem of mechanical property are covered, a kind of preparation method of modified carbon fiber-epoxy resin composite material is provided.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) according to parts by weight, by 10~20 parts of albumen powders, 1~2 part of alkali protease, 30~40 parts of water termostat stir process,
Heat up enzyme deactivation, and sodium hydroxide solution is then added dropwise and adjusts pH, centrifuge separation obtains supernatant；
(2) carbon fiber is mixed with sodium hydroxide solution 1:10~1:20 in mass ratio, is impregnated, filtering, Freezing smashing, washing,
It is dry, obtain single treatment carbon fiber；
(3) according to parts by weight, by 10~20 parts of supernatants, 20~30 parts of single treatment carbon fibers, 10~20 parts of saccharomycete,
30~50 parts of deionized water mixed fermentations are then added dropwise iron nitrate solution and are stirred, filter, wash, dry, filling with inert gas
Isothermal holding, cooling, obtains secondary treatment carbon fiber；
(4) secondary treatment carbon fiber is handled by high-temperature water vapor, it is dry, obtain modified carbon fiber；
(5) according to parts by weight, by 40~60 parts of epoxy resin, 20~30 parts of diluents, 15~20 parts of modified carbon fibers, 5~8
Part curing agent, 10~20 parts of nanometer iron powders are stirred, and apply external magnetic field in mixed process, injection molding, compression moulding, are taken off
Mould is to get modified carbon fiber-epoxy resin composite material.
Step (1) albumen powder is soyabean protein powder, any one in albumen powder or PURE WHEY.
Step (3) inert gas is nitrogen, any one in argon gas or neon.
Step (5) epoxy resin is any one in bisphenol-A liquid epoxy resin or bisphenol-f type liquid epoxies
Kind.
Step (5) diluent is dimethylbenzene, any one in acetone or alcohol.
Step (5) curing agent is vinyl triamine, any one in ethylenediamine or ethylenediamine tetra-acetic acid.
Step (5) the application external magnetic field strength is 40~50T.
The beneficial effects of the present invention are:
The present invention is by addition modified carbon fiber, during the preparation process, firstly, the protein in system is by alkali protease
Processing, is hydrolyzed into polypeptide, and then, carbon fiber is impregnated by sodium hydroxide solution, using freezing ball milling, so that carbon fiber surface
There is defect and then during the fermentation, using Absorption Growth of the saccharomycete in Carbon fibe bowl configurations, utilizes saccharomycete
The active group on surface, the polypeptide that adhesion protein powder is hydrolyzed into, then by addition ferric nitrate, polypeptide can be in complex system
Iron ion, then, in heat preservation carbonization process, the organic matter on modified carbon fiber surface is carbonized, while generating tar, with temperature
Raising, iron ion is reduced into fe in system, then passes through high-temperature water vapor processing, and fe is anti-with high-temperature water vapor
It answers, the magnetic ferroso-ferric oxide of the tool of generation, in use, the ferroso-ferric oxide of modified carbon fiber surface deposition can
Nanometer iron powder in absorption system, so that the interface resistance between modified carbon fiber and epoxy resin reduces, so that the conduction of system
Performance gets a promotion, so that the electromagnetic shielding performance of system is improved, meanwhile, adsorption capacity makes in the carbonaceous of modified fibre surface
Tar exudation, so that the interface bond strength between modified carbon fiber and epoxy resin gets a promotion, so that system
Mechanical property gets a promotion.
Specific embodiment
According to parts by weight, by 10~20 parts of albumen powders, 1~2 part of alkali protease, 30~40 parts of water are placed in No. 1 beaker
In, and No. 1 beaker is placed in digital display and is tested the speed in constant temperature blender with magnetic force, it is 32 DEG C in temperature, revolving speed is 200~300r/min item
Under part, constant temperature 40~60min of stir process is then warming up to 80~90 DEG C, and the hydrogen-oxygen that mass fraction is 20~26% is then added dropwise
Change sodium solution and adjust pH to 7.6~7.9, obtains enzymatic treatment liquid, enzymatic treatment liquid is then placed in a centrifuge centrifuge separation, is discarded down
Layer precipitating, obtains supernatant；Sodium hydroxide solution 1:10~the 1:20 in mass ratio for being 30~35% by carbon fiber and mass fraction
It is placed in mixing kettle, is 50~60 DEG C in temperature, under the conditions of revolving speed is 400~600r/min, is stirred 3~5h of immersion, obtains
Soak, then soak is filtered, filter residue is obtained, then filter residue is placed in liquid nitrogen and is freezed, obtains filter residue block, then sets filter residue block
40~60min of ball milling in ball mill obtains filter residue powder, and it is neutral for then being washed filter residue powder to cleaning solution with glacial acetic acid, then
Filter residue powder after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 105~110 DEG C, obtain single treatment carbon fiber
Dimension；According to parts by weight, by 10~20 parts of supernatants, 20~30 parts of single treatment carbon fibers, 10~20 parts of saccharomycete, 30~
50 parts of deionized waters are placed in fermentation cauldron, are 28~32 DEG C in temperature, under the conditions of revolving speed is 200~300r/min, are stirred
Fermentation 3~5 days, then into fermentation cauldron be added dropwise mass fraction be 10~20% iron nitrate solution, in revolving speed be 400~600r/
Under the conditions of min, it is stirred 40~60min, obtains mixed serum, is refiltered, filter cake is obtained, then with deionized water by Washing of Filter Cake
3~5 times, then the filter cake after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 105~110 DEG C, it obtains dry
Dry cake, is then placed in Muffle furnace by dry filter cake, and filling with inert gas is filled with into furnace with 60~90mL/min rate, in
Under the conditions of temperature is 1150 DEG C, after 1~2h of isothermal holding, it is down to room temperature with furnace, obtains secondary treatment carbon fiber；By secondary treatment carbon
Fiber is placed in reaction kettle, and high-temperature water vapor is then passed through into reaction kettle, under the conditions of temperature is 240~280 DEG C, processing 1
~2h obtains Treatment of Carbon three times, Treatment of Carbon will then be placed in baking oven three times, in temperature be 105~110 DEG C of conditions
Under, it is dry to constant weight, obtain modified carbon fiber；According to parts by weight, by 40~60 parts of epoxy resin, 20~30 parts of diluents, 15
~20 parts of modified carbon fibers, 5~8 parts of curing agent, 10~20 parts of nanometer iron powders are placed in batch mixer, in revolving speed be 600~800r/
Under the conditions of min, it is stirred 40~60min, the external magnetic field that intensity is 40~50T is applied to material in batch mixer, obtains mixing slurry
Material then sprays methyl-silicone oil to die surface, then injects in mold mixed slurry, then mold is placed in molding,
It is 150~165 DEG C in temperature, under the conditions of pressure is 2~3MPa, after compression moulding, demoulds to get modified carbon fiber-asphalt mixtures modified by epoxy resin
Resin composite material.The albumen powder is soyabean protein powder, any one in albumen powder or PURE WHEY.The inertia
Gas is nitrogen, any one in argon gas or neon.The epoxy resin is bisphenol-A liquid epoxy resin or bisphenol-f type
Any one in liquid epoxies.The diluent is dimethylbenzene, any one in acetone or alcohol.The curing agent is
Any one in vinyl triamine, ethylenediamine or ethylenediamine tetra-acetic acid.
According to parts by weight, by 20 parts of albumen powders, 2 parts of alkali proteases, 40 parts of water are placed in No. 1 beaker, and No. 1 is burnt
Cup is placed in digital display and tests the speed in constant temperature blender with magnetic force, in temperature be 32 DEG C, under the conditions of revolving speed is 300r/min, constant temperature stir process
60min is then warming up to 90 DEG C, and the sodium hydroxide solution that mass fraction is 26% is then added dropwise and adjusts pH to 7.9, obtains enzymatic treatment
Enzymatic treatment liquid is then placed in a centrifuge centrifuge separation, discards lower sediment, obtains supernatant by liquid；By carbon fiber and quality
The sodium hydroxide solution 1:20 in mass ratio that score is 35% is placed in mixing kettle, is 60 DEG C in temperature, revolving speed is 600r/min item
Under part, it is stirred and impregnates 5h, obtain soak, then soak is filtered, obtain filter residue, then filter residue is placed in liquid nitrogen and is freezed,
Filter residue block is obtained, filter residue block is then placed in ball milling 60min in ball mill, obtains filter residue powder, is then washed filter residue powder with glacial acetic acid
It is neutrality to cleaning solution, then the filter residue powder after washing is placed in baking oven, under the conditions of temperature is 110 DEG C, drying to constant weight,
Obtain single treatment carbon fiber；According to parts by weight, by 20 parts of supernatants, 30 parts of single treatment carbon fibers, 20 parts of saccharomycete, 50
Part deionized water is placed in fermentation cauldron, is 32 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred fermentation 5 days, then
The iron nitrate solution that mass fraction is 20% is added dropwise into fermentation cauldron, under the conditions of revolving speed is 600r/min, is stirred 60min,
Mixed serum is obtained, refilters, obtains filter cake, the filter cake after washing is then then placed in baking by Washing of Filter Cake 5 times with deionized water
In case, under the conditions of temperature is 110 DEG C, drying to constant weight obtains dry cake, then dry cake is placed in Muffle furnace, and
It is filled with filling with inert gas into furnace with 90mL/min rate, under the conditions of temperature is 1150 DEG C, after isothermal holding 2h, is down to furnace
Room temperature obtains secondary treatment carbon fiber；Secondary treatment carbon fiber is placed in reaction kettle, high-temperature water steaming is then passed through into reaction kettle
Vapour handles 2h, obtains Treatment of Carbon three times, then Treatment of Carbon will be placed in baking oven three times under the conditions of temperature is 280 DEG C
In, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain modified carbon fiber；According to parts by weight, by 60 parts of epoxy resin, 30
Part diluent, 20 parts of modified carbon fibers, 8 parts of curing agent, 20 parts of nanometer iron powders are placed in batch mixer, in revolving speed be 800r/min item
Under part, it is stirred 60min, the external magnetic field that intensity is 50T is applied to material in batch mixer, mixed slurry is obtained, then to mold
Surface spray methyl-silicone oil, then by mixed slurry inject mold in, then mold is placed in molding, in temperature be 165 DEG C,
Under the conditions of pressure is 3MPa, after compression moulding, demould to get modified carbon fiber-epoxy resin composite material.The albumen powder is
Soyabean protein powder.The inert gas is nitrogen.The epoxy resin is bisphenol-A liquid epoxy resin.The diluent is
Dimethylbenzene.The curing agent is vinyl triamine.
According to parts by weight, by 20 parts of albumen powders, 2 parts of alkali proteases, 40 parts of water are placed in No. 1 beaker, and No. 1 is burnt
Cup is placed in digital display and tests the speed in constant temperature blender with magnetic force, in temperature be 32 DEG C, under the conditions of revolving speed is 300r/min, constant temperature stir process
60min is then warming up to 90 DEG C, and the sodium hydroxide solution that mass fraction is 26% is then added dropwise and adjusts pH to 7.9, obtains enzymatic treatment
Enzymatic treatment liquid is then placed in a centrifuge centrifuge separation, discards lower sediment, obtains supernatant by liquid；According to parts by weight, will
20 parts of supernatants, 30 parts of carbon fibers, 20 parts of saccharomycete, 50 parts of deionized waters are placed in fermentation cauldron, in temperature be 32 DEG C, revolving speed
Under the conditions of 300r/min, it is stirred fermentation 5 days, the iron nitrate solution that mass fraction is 20% is then added dropwise into fermentation cauldron,
Under the conditions of revolving speed is 600r/min, it is stirred 60min, obtains mixed serum, is refiltered, filter cake is obtained, then uses deionized water
By Washing of Filter Cake 5 times, then the filter cake after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, it obtains
Dry cake is then placed in Muffle furnace by dry cake, and filling with inert gas, Yu Wen are filled with into furnace with 90mL/min rate
Under the conditions of degree is 1150 DEG C, after isothermal holding 2h, it is down to room temperature with furnace, obtains secondary treatment carbon fiber；By secondary treatment carbon fiber
It is placed in reaction kettle, high-temperature water vapor is then passed through into reaction kettle, under the conditions of temperature is 280 DEG C, handles 2h, obtain and locate three times
Carbon fiber is managed, Treatment of Carbon will be then placed in baking oven three times, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain modification
Carbon fiber；According to parts by weight, by 60 parts of epoxy resin, 30 parts of diluents, 20 parts of modified carbon fibers, 8 parts of curing agent, 20 parts are received
Rice iron powder is placed in batch mixer, under the conditions of revolving speed is 800r/min, is stirred 60min, is applied to material in batch mixer strong
Degree is the external magnetic field of 50T, obtains mixed slurry, then sprays methyl-silicone oil to die surface, mixed slurry is then injected mold
In, then mold is placed in molding, is 165 DEG C in temperature, under the conditions of pressure is 3MPa, after compression moulding, demoulds to get changing
Property carbon fiber epoxy resin composite material.The albumen powder is soyabean protein powder.The inert gas is nitrogen.The epoxy
Resin is bisphenol-A liquid epoxy resin.The diluent is dimethylbenzene.The curing agent is vinyl triamine.
According to parts by weight, by 20 parts of albumen powders, 2 parts of alkali proteases, 40 parts of water are placed in No. 1 beaker, and No. 1 is burnt
Cup is placed in digital display and tests the speed in constant temperature blender with magnetic force, in temperature be 32 DEG C, under the conditions of revolving speed is 300r/min, constant temperature stir process
60min is then warming up to 90 DEG C, and the sodium hydroxide solution that mass fraction is 26% is then added dropwise and adjusts pH to 7.9, obtains enzymatic treatment
Enzymatic treatment liquid is then placed in a centrifuge centrifuge separation, discards lower sediment, obtains supernatant by liquid；By carbon fiber and quality
The sodium hydroxide solution 1:20 in mass ratio that score is 35% is placed in mixing kettle, is 60 DEG C in temperature, revolving speed is 600r/min item
Under part, it is stirred and impregnates 5h, obtain soak, then soak is filtered, obtain filter residue, then filter residue is placed in liquid nitrogen and is freezed,
Filter residue block is obtained, filter residue block is then placed in ball milling 60min in ball mill, obtains filter residue powder, is then washed filter residue powder with glacial acetic acid
It is neutrality to cleaning solution, then the filter residue powder after washing is placed in baking oven, under the conditions of temperature is 110 DEG C, drying to constant weight,
Obtain single treatment carbon fiber；Single treatment carbon fiber is placed in reaction kettle, high-temperature water vapor is then passed through into reaction kettle, in
Under the conditions of temperature is 280 DEG C, 2h is handled, Treatment of Carbon three times is obtained, Treatment of Carbon will then be placed in baking oven three times, Yu Wen
It is dry to constant weight under the conditions of degree is 110 DEG C, obtain modified carbon fiber；According to parts by weight, by 60 parts of epoxy resin, 30 parts of dilutions
Agent, 20 parts of modified carbon fibers, 8 parts of curing agent, 20 parts of nanometer iron powders are placed in batch mixer, under the conditions of revolving speed is 800r/min,
It is stirred 60min, the external magnetic field that intensity is 50T is applied to material in batch mixer, mixed slurry is obtained, is then sprayed to die surface
Methyl-silicone oil is spilt, then mixed slurry is injected in mold, then mold is placed in molding, is 165 DEG C in temperature, pressure is
Under the conditions of 3MPa, after compression moulding, demould to get modified carbon fiber-epoxy resin composite material.The albumen powder is soybean egg
White powder.The inert gas is nitrogen.The epoxy resin is bisphenol-A liquid epoxy resin.The diluent is dimethylbenzene.
The curing agent is vinyl triamine.
According to parts by weight, by 20 parts of albumen powders, 2 parts of alkali proteases, 40 parts of water are placed in No. 1 beaker, and No. 1 is burnt
Cup is placed in digital display and tests the speed in constant temperature blender with magnetic force, in temperature be 32 DEG C, under the conditions of revolving speed is 300r/min, constant temperature stir process
60min is then warming up to 90 DEG C, and the sodium hydroxide solution that mass fraction is 26% is then added dropwise and adjusts pH to 7.9, obtains enzymatic treatment
Enzymatic treatment liquid is then placed in a centrifuge centrifuge separation, discards lower sediment, obtains supernatant by liquid；By carbon fiber and quality
The sodium hydroxide solution 1:20 in mass ratio that score is 35% is placed in mixing kettle, is 60 DEG C in temperature, revolving speed is 600r/min item
Under part, it is stirred and impregnates 5h, obtain soak, then soak is filtered, obtain filter residue, then filter residue is placed in liquid nitrogen and is freezed,
Filter residue block is obtained, filter residue block is then placed in ball milling 60min in ball mill, obtains filter residue powder, is then washed filter residue powder with glacial acetic acid
It is neutrality to cleaning solution, then the filter residue powder after washing is placed in baking oven, under the conditions of temperature is 110 DEG C, drying to constant weight,
Obtain single treatment carbon fiber；According to parts by weight, by 20 parts of supernatants, 30 parts of single treatment carbon fibers, 20 parts of saccharomycete, 50
Part deionized water is placed in fermentation cauldron, is 32 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred fermentation 5 days, then
The iron nitrate solution that mass fraction is 20% is added dropwise into fermentation cauldron, under the conditions of revolving speed is 600r/min, is stirred 60min,
Mixed serum is obtained, refilters, obtains filter cake, the filter cake after washing is then then placed in baking by Washing of Filter Cake 5 times with deionized water
In case, under the conditions of temperature is 110 DEG C, drying to constant weight obtains dry cake, then dry cake is placed in Muffle furnace, and
It is filled with filling with inert gas into furnace with 90mL/min rate, under the conditions of temperature is 1150 DEG C, after isothermal holding 2h, is down to furnace
Room temperature obtains modified carbon fiber；According to parts by weight, by 60 parts of epoxy resin, 30 parts of diluents, 20 parts of modified carbon fibers, 8 parts solid
Agent, 20 parts of nanometer iron powders are placed in batch mixer, under the conditions of revolving speed is 800r/min, 60min are stirred, in batch mixer
Material applies the external magnetic field that intensity is 50T, obtains mixed slurry, then methyl-silicone oil is sprayed to die surface, then by mixing slurry
Material injection mold in, then mold is placed in molding, in temperature be 165 DEG C, pressure be 3MPa under the conditions of, after compression moulding,
Demoulding is to get modified carbon fiber-epoxy resin composite material.The albumen powder is soyabean protein powder.The inert gas is nitrogen
Gas.The epoxy resin is bisphenol-A liquid epoxy resin.The diluent is dimethylbenzene.The curing agent is vinyl three
Amine.
According to parts by weight, by 20 parts of albumen powders, 2 parts of alkali proteases, 40 parts of water are placed in No. 1 beaker, and No. 1 is burnt
Cup is placed in digital display and tests the speed in constant temperature blender with magnetic force, in temperature be 32 DEG C, under the conditions of revolving speed is 300r/min, constant temperature stir process
60min is then warming up to 90 DEG C, and the sodium hydroxide solution that mass fraction is 26% is then added dropwise and adjusts pH to 7.9, obtains enzymatic treatment
Enzymatic treatment liquid is then placed in a centrifuge centrifuge separation, discards lower sediment, obtains supernatant by liquid；By carbon fiber and quality
The sodium hydroxide solution 1:20 in mass ratio that score is 35% is placed in mixing kettle, is 60 DEG C in temperature, revolving speed is 600r/min item
Under part, it is stirred and impregnates 5h, obtain soak, then soak is filtered, obtain filter residue, then filter residue is placed in liquid nitrogen and is freezed,
Filter residue block is obtained, filter residue block is then placed in ball milling 60min in ball mill, obtains filter residue powder, is then washed filter residue powder with glacial acetic acid
It is neutrality to cleaning solution, then the filter residue powder after washing is placed in baking oven, under the conditions of temperature is 110 DEG C, drying to constant weight,
Obtain single treatment carbon fiber；According to parts by weight, by 20 parts of supernatants, 30 parts of single treatment carbon fibers, 20 parts of saccharomycete, 50
Part deionized water is placed in fermentation cauldron, is 32 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred fermentation 5 days, then
The iron nitrate solution that mass fraction is 20% is added dropwise into fermentation cauldron, under the conditions of revolving speed is 600r/min, is stirred 60min,
Mixed serum is obtained, refilters, obtains filter cake, the filter cake after washing is then then placed in baking by Washing of Filter Cake 5 times with deionized water
In case, under the conditions of temperature is 110 DEG C, drying to constant weight obtains dry cake, then dry cake is placed in Muffle furnace, and
It is filled with filling with inert gas into furnace with 90mL/min rate, under the conditions of temperature is 1150 DEG C, after isothermal holding 2h, is down to furnace
Room temperature obtains secondary treatment carbon fiber；Secondary treatment carbon fiber is placed in reaction kettle, high-temperature water steaming is then passed through into reaction kettle
Vapour handles 2h, obtains Treatment of Carbon three times, then Treatment of Carbon will be placed in baking oven three times under the conditions of temperature is 280 DEG C
In, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain modified carbon fiber；According to parts by weight, by 60 parts of epoxy resin, 30
Part diluent, 20 parts of modified carbon fibers, 8 parts of curing agent are placed in batch mixer, under the conditions of revolving speed is 800r/min, are stirred
60min applies the external magnetic field that intensity is 50T to material in batch mixer, obtains mixed slurry, then spray methyl silicon to die surface
Mixed slurry is then injected in mold, then mold is placed in molding by oil, is 165 DEG C in temperature, pressure is 3MPa condition
Under, after compression moulding, demould to get modified carbon fiber-epoxy resin composite material.The albumen powder is soyabean protein powder.Institute
Stating inert gas is nitrogen.The epoxy resin is bisphenol-A liquid epoxy resin.The diluent is dimethylbenzene.It is described solid
Agent is vinyl triamine.
According to parts by weight, by 20 parts of albumen powders, 2 parts of alkali proteases, 40 parts of water are placed in No. 1 beaker, and No. 1 is burnt
Cup is placed in digital display and tests the speed in constant temperature blender with magnetic force, in temperature be 32 DEG C, under the conditions of revolving speed is 300r/min, constant temperature stir process
60min is then warming up to 90 DEG C, and the sodium hydroxide solution that mass fraction is 26% is then added dropwise and adjusts pH to 7.9, obtains enzymatic treatment
Enzymatic treatment liquid is then placed in a centrifuge centrifuge separation, discards lower sediment, obtains supernatant by liquid；By carbon fiber and quality
The sodium hydroxide solution 1:20 in mass ratio that score is 35% is placed in mixing kettle, is 60 DEG C in temperature, revolving speed is 600r/min item
Under part, it is stirred and impregnates 5h, obtain soak, then soak is filtered, obtain filter residue, then filter residue is placed in liquid nitrogen and is freezed,
Filter residue block is obtained, filter residue block is then placed in ball milling 60min in ball mill, obtains filter residue powder, is then washed filter residue powder with glacial acetic acid
It is neutrality to cleaning solution, then the filter residue powder after washing is placed in baking oven, under the conditions of temperature is 110 DEG C, drying to constant weight,
Obtain single treatment carbon fiber；According to parts by weight, by 20 parts of supernatants, 30 parts of single treatment carbon fibers, 20 parts of saccharomycete, 50
Part deionized water is placed in fermentation cauldron, is 32 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred fermentation 5 days, then
The iron nitrate solution that mass fraction is 20% is added dropwise into fermentation cauldron, under the conditions of revolving speed is 600r/min, is stirred 60min,
Mixed serum is obtained, refilters, obtains filter cake, the filter cake after washing is then then placed in baking by Washing of Filter Cake 5 times with deionized water
In case, under the conditions of temperature is 110 DEG C, drying to constant weight obtains dry cake, then dry cake is placed in Muffle furnace, and
It is filled with filling with inert gas into furnace with 90mL/min rate, under the conditions of temperature is 1150 DEG C, after isothermal holding 2h, is down to furnace
Room temperature obtains secondary treatment carbon fiber；Secondary treatment carbon fiber is placed in reaction kettle, high-temperature water steaming is then passed through into reaction kettle
Vapour handles 2h, obtains Treatment of Carbon three times, then Treatment of Carbon will be placed in baking oven three times under the conditions of temperature is 280 DEG C
In, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain modified carbon fiber；According to parts by weight, by 60 parts of epoxy resin, 30
Part diluent, 20 parts of modified carbon fibers, 8 parts of curing agent, 20 parts of nanometer iron powders are placed in batch mixer, in revolving speed be 800r/min item
Under part, it is stirred 60min, obtains mixed slurry, then methyl-silicone oil is sprayed to die surface, mixed slurry is then injected into mould
In tool, then mold is placed in molding, in temperature be 165 DEG C, pressure be 3MPa under the conditions of, after compression moulding, demoulding to get
Modified carbon fiber-epoxy resin composite material.The albumen powder is soyabean protein powder.The inert gas is nitrogen.The ring
Oxygen resin is bisphenol-A liquid epoxy resin.The diluent is dimethylbenzene.The curing agent is vinyl triamine.
Comparative example: the epoxy resin composite material of Shanghai new material Co., Ltd production.
1 to 6 gained epoxy resin composite material of example and comparative example product are subjected to performance detection, specific detection method is such as
Under:
Above-mentioned modified carbon fiber-epoxy resin composite material is pressed into 300mm × 300mm × 4mm square plate to test
Shield effectiveness.
The interface shear strength of above-mentioned composite material is tested using CMT4204 type microcomputer controlled electronic universal tester.
Specific testing result is as shown in table 1:
Table 1: performance detection table
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example |
| Shield effectiveness/dB | 56 | 38 | 41 | 40 | 42 | 41 | 27 |
| Interface shear strength/MPa | 84.8 | 60.4 | 56.8 | 57.2 | 63.4 | 57.6 | 39.2 |
By 1 testing result of table it is found that present invention gained modified carbon fiber-epoxy resin composite material has excellent electromagnetic shielding
Performance and mechanical property.
Claims (7)
1. a kind of preparation method of modified carbon fiber-epoxy resin composite material, it is characterised in that specific preparation process is as follows:
(1) according to parts by weight, by 10~20 parts of albumen powders, 1~2 part of alkali protease, 30~40 parts of water termostat stir process,
Heat up enzyme deactivation, and sodium hydroxide solution is then added dropwise and adjusts pH, centrifuge separation obtains supernatant；
(2) carbon fiber is mixed with sodium hydroxide solution 1:10~1:20 in mass ratio, is impregnated, filtering, Freezing smashing, washing,
It is dry, obtain single treatment carbon fiber；
(3) according to parts by weight, by 10~20 parts of supernatants, 20~30 parts of single treatment carbon fibers, 10~20 parts of saccharomycete,
30~50 parts of deionized water mixed fermentations are then added dropwise iron nitrate solution and are stirred, filter, wash, dry, filling with inert gas
Isothermal holding, cooling, obtains secondary treatment carbon fiber；
(4) secondary treatment carbon fiber is handled by high-temperature water vapor, it is dry, obtain modified carbon fiber；
(5) according to parts by weight, by 40~60 parts of epoxy resin, 20~30 parts of diluents, 15~20 parts of modified carbon fibers, 5~8
Part curing agent, 10~20 parts of nanometer iron powders are stirred, and apply external magnetic field in mixed process, injection molding, compression moulding, are taken off
Mould is to get modified carbon fiber-epoxy resin composite material.
2. a kind of preparation method of modified carbon fiber-epoxy resin composite material according to claim 1, it is characterised in that:
Step (1) albumen powder is soyabean protein powder, any one in albumen powder or PURE WHEY.
3. a kind of preparation method of modified carbon fiber-epoxy resin composite material according to claim 1, it is characterised in that:
Step (3) inert gas is nitrogen, any one in argon gas or neon.
4. a kind of preparation method of modified carbon fiber-epoxy resin composite material according to claim 1, it is characterised in that:
Step (5) epoxy resin is any one in bisphenol-A liquid epoxy resin or bisphenol-f type liquid epoxies.
5. a kind of preparation method of modified carbon fiber-epoxy resin composite material according to claim 1, it is characterised in that:
Step (5) diluent is dimethylbenzene, any one in acetone or alcohol.
6. a kind of preparation method of modified carbon fiber-epoxy resin composite material according to claim 1, it is characterised in that:
Step (5) curing agent is vinyl triamine, any one in ethylenediamine or ethylenediamine tetra-acetic acid.
7. a kind of preparation method of modified carbon fiber-epoxy resin composite material according to claim 1, it is characterised in that:
Step (5) the application external magnetic field strength is 40~50T.
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| CN109929235A (en) * | 2019-03-03 | 2019-06-25 | 姜丽丽 | A kind of electric-conductivity heat-conductivity high carbon nano-complex and preparation method thereof |
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| CN110373003A (en) * | 2019-06-12 | 2019-10-25 | 何治华 | A kind of preparation method of the short fine composite plate of enhanced carbon fiber |
| CN111876045A (en) * | 2020-08-17 | 2020-11-03 | 李法雷 | High-temperature-resistant environment-friendly anticorrosive paint and preparation method thereof |
| CN113429743A (en) * | 2021-07-13 | 2021-09-24 | 郑州佛光发电设备有限公司 | Electromagnetic shielding material and preparation method thereof |
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| CN109929235A (en) * | 2019-03-03 | 2019-06-25 | 姜丽丽 | A kind of electric-conductivity heat-conductivity high carbon nano-complex and preparation method thereof |
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| CN110272612A (en) * | 2019-05-20 | 2019-09-24 | 华中科技大学 | Protein-carbon nano-fiber/epoxy resin composite material and preparation method thereof |
| CN110373003A (en) * | 2019-06-12 | 2019-10-25 | 何治华 | A kind of preparation method of the short fine composite plate of enhanced carbon fiber |
| CN111876045A (en) * | 2020-08-17 | 2020-11-03 | 李法雷 | High-temperature-resistant environment-friendly anticorrosive paint and preparation method thereof |
| CN113429743A (en) * | 2021-07-13 | 2021-09-24 | 郑州佛光发电设备有限公司 | Electromagnetic shielding material and preparation method thereof |
| CN114573949A (en) * | 2022-03-21 | 2022-06-03 | 嘉兴学院 | Bending-resistant carbon fiber epoxy composite material and preparation method thereof |
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Application publication date: 20190111 |