CN109206840A - The production and stress measuring method of glass fibre-reinforced phenolic resin plate - Google Patents
The production and stress measuring method of glass fibre-reinforced phenolic resin plate Download PDFInfo
- Publication number
- CN109206840A CN109206840A CN201810738409.1A CN201810738409A CN109206840A CN 109206840 A CN109206840 A CN 109206840A CN 201810738409 A CN201810738409 A CN 201810738409A CN 109206840 A CN109206840 A CN 109206840A
- Authority
- CN
- China
- Prior art keywords
- graphene
- phenolic resin
- glass fibre
- phenolic
- plate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- 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
- C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L25/00—Testing or calibrating of apparatus for measuring force, torque, work, mechanical power, or mechanical efficiency
-
- 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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- 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
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- 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
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2471/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- 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
- C08K7/14—Glass
-
- 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
Abstract
The production and stress measuring method of glass fibre-reinforced phenolic resin plate, comprising the following steps: weigh graphene powder and be added in acetone soln, be prepared into suspension；Poly(aryl ether ketone), epoxy resin, phenolic resin are mixed and heated to be added in suspension after melting according to the weight of 1:1:8 and form graphene phenolic-resin complex liquid；Pretreated glass fibre is put into graphene phenolic-resin complex liquid sufficiently infiltration and forms slurry；Slurry is poured into board making mold；Plate is formed after gel, solidification and curing three phases；Loading force and change in resistance curve are measured using digital resistance instrument, completes plate pressure sensing calibration measurement.The present invention using graphene change in resistance under pressure characteristic, produce can with electrified regulation, it is sensitive to pressure change and can real-time monitoring glass fibre-reinforced phenolic resin plate.The plate made keep its density it is small, intensity is high under the premise of, modulus is bigger, and wearability is stronger.
Description
Technical field
The invention belongs to polymer-based nanos and glass-fibre technology field, and in particular to one kind has heating and stress sense
Know the production and stress measuring method of the glass fibre-reinforced phenolic resin plate of function.
Background technique
Glass fibre is dosage maximum, most widely used inorganic non-metallic material in reinforced substrate of composite material.With multiple
Condensation material develops to high-performance and multifunction, and the high performance glass fibre such as S glass fibre is constantly released, it has higher power
Learn performance, stronger corrosion resistance, higher heat resistance.
Phenolic resin is by artificial synthesized a kind of high molecular polymer.Urea formaldehyde is strangled in the processing and forming of product, by
In its good heat resistance, cost of material is low, there is preferable economic benefit compared with other raw materials.After epoxy-modified, phenol
The performance of urea formaldehyde further increases.
Glass fibre-reinforced phenolic resin composite board is one of current most widely used composite material, is had close
The advantages that small, intensity is high is spent, it is to be widely used in state that in addition its raw material sources is extensive, machine-shaping is easy, designability is strong
The important composite board of one of people's economy and national defense construction.But the composite panel conduction is bad, is unable to electrified regulation,
Using being subject to certain restrictions in cold climate.The load that plate is subject to cannot be from perceiving, and there are hidden danger for safety under specific condition.
Graphene is as a kind of nano-carbon material, and the electron mobility of graphene is more than 15000 cm at normal temperature2/ (V
S), resistivity about 10-6Cm is the smallest material of current resistivity；Graphene has excellent thermal conductivity,
Thermal coefficient may be up to 5300W/mK, be much higher than carbon nanotube and diamond.Graphene had both had high-intensitive, high-elastic mould and strong
The mechanical properties such as toughness, and there are the functional performances such as excellent thermally conductive, conductive, electromagnetism and assign the increasing of phenolic resin base glass fibre
Strong composite material function/intelligent behaviour.With the sharp fall of graphene price, graphene is applied to field of compound material
Undoubtedly there is major application prospect.
Summary of the invention
The present invention provides a kind of keeping before its density is small, intensity is high to solve shortcoming in the prior art
Put, can electrified regulation, perceive plate pressure change glass fibre-reinforced phenolic resin plate production and stress measurement
Method.
In order to solve the above technical problems, the present invention adopts the following technical scheme: glass fibre-reinforced phenolic resin plate
Production and stress measuring method, comprising the following steps:
(1), graphene is formed into graphene powder after machine is hydride modified；
(2), the graphene powder for weighing constant weight is added portionwise in acetone soln, then places it in Ultrasound Instrument to mixed
Solution ultrasonic treatment is closed, finely dispersed suspension is prepared into；
(3), poly(aryl ether ketone), epoxy resin, phenolic resin are weighed according to the weight ratio of 1:1:8 spare；
(4) load weighted poly(aryl ether ketone) is uniformly mixed with epoxy resin, mixture is melted to obtain to performed polymer at a certain temperature,
Then performed polymer is put into pulverizer and breaks into powder, and pass through the dusting cover of 80 mesh；By performed polymer powder and load weighted phenolic aldehyde
Resin is added in blender and is stirred, and softening temperature or more is heated in mixed process, is at melt-flow state；
(5), the phenolic resin of melting is added in the suspension of step (2) preparation, after being mixed slowly using blender again quickly
Stirring forms graphene phenolic-resin complex liquid to being uniformly mixed；
(6), glass fibre is followed the steps below pretreatment: the acetone for being put into the 50 m L 40% that temperature is 30 DEG C is molten
After impregnating 20 min in liquid, oil removing wash with distilled water；It is 40 g/L that glass fabric after oil removing, which is soaked in 50 mL concentration,
Sodium hydroxide roughening solution in clean after 30 min, temperature maintains 60 DEG C；By the glass fabric being roughened at 35 DEG C
It is put into the sensitizing solution SnCl of 50 m L, 30 g/L2In after 20 min, cleaning；Glass fabric after sensitization is put into 50
The activating solution Pd Cl of 0.1 g/L of mL2In solution, 20 min are kept in 30 DEG C, finally wash with distilled water；
(7), pretreated glass fibre is put into graphene phenolic-resin complex liquid and sufficiently infiltrates；
(8), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(9) the graphene phenolic-resin complex liquid in step (5) is poured into board making mold, gas is discharged using vibratory drilling method
Bubble, until reaching design thickness；
(10), slurry successively forms plate, positive electrode after gel, solidification and curing three phases in board making mold
It adheres on plate with negative electrode and is integrally demoulded with plate；
(11), after a certain period of time by the cooling placement of plate, according to certain method for supporting, plate is carried out using center loaded method
On-load pressure, positive electrode and negative electrode connect digital resistance instrument, and digital resistance instrument measures loading force and change in resistance curve,
Complete plate pressure sensing calibration measurement.
The weight of graphene powder in step (2) is the 0.3% of the phenolic resin weight melted in step (3).
Using method addition graphene is first mixed in step (1), graphene uses multi-layer graphene, the rule of multi-layer graphene raw material
Lattice are diameter < 2 μm, with a thickness of 1-5nm, specific surface area 500m2/ g, density 2-2.25g/ml, thermal coefficient > 3000w/m
K, electric conductivity > 107S/m。
The softening point of the phenolic resin of melting is at 70 °C and following.
Graphene phenolic-resin complex liquid in step (5) can also be prepared with reduction method；
Reduction method prepares graphene phenolic-resin complex liquid process are as follows:
Graphene oxide is prepared using Hummers method is improved；3g graphite powder and 1g sodium nitrate are added equipped with the 69 mL concentrated sulfuric acids
In three-necked flask, it is slowly added to 12g potassium permanganate under stirring in ice-water bath, in 10 DEG C or less reaction 1h；35 DEG C are warming up to, is continued
2h is stirred, 120 mL deionized waters are slowly added to, system temperature is made to be increased to 95 DEG C, 30 min is maintained, a large amount of distilled water is added
Dilution, pours into 30%H2O2To no bubble generate, filter while hot, and with volume ratio for 1: 10 HCl solution wash it is filtered
Filter cake, using BaCl2Detection, until without SO in filtrate4, filtration cakes torrefaction obtains graphite oxide；Graphite oxide is soluble in water, surpass
Sound is allowed to be completely dispersed；Obtain graphene oxide；
50g phenolic resin and 25g propylene glycol monomethyl ether are added in three-necked flask, 80 DEG C is warming up to, is slowly added dropwise under stirring
10.5g diethanol amine reacts 2h；Then 60 DEG C are cooled to, 20% acetum reaction 30min is added dropwise, is then slowly added into steaming
The quick stirring and emulsifying of distilled water obtains cationic phenolic aldehyde emulsion；
It adds graphene oxide into Phenolic resin emulsion, stirs ultrasound 1h, keep the temperature 3h at 60 DEG C, then proceed to ultrasound
30min, filtering, obtains graphene oxide phenolic resin complex liquid.
The weight for the glass fibre being added in step (6) accounts for 30%-the 50% of graphene phenolic-resin complex liquid weight, glass
In glass fiber according to weight ratio contain 55% silica, 20% aluminum oxide and 12% magnesia.
Gel, solidification and the detailed process of curing in step (10) are as follows:
Gel: gel time is a part of curing time, and after mixing, resin/curing agent mixture is still liquid and can
To work and be suitble to application；In order to guarantee reliably to be bonded, all construction and positioning work should be done within the curing operation time
It is good；Solidification: mixture initially enters solidification phase, and at this moment it starts gel or " mutation "；At this moment phenolic aldehyde does not have prolonged work
It may make, will also lose viscosity；In this stage any interference cannot be carried out to it；It will become soft gel as hard rubber
Object, you with thumb will press it is dynamic it；
Curing: cure stage mixture is local solidification, the phenolic resin newly used still can with its chemical bonds, therefore should
Untreated surface still can be bonded or be reacted；Anyway, close to cured mixture, these abilities are reducing；Phenol
Aldehyde mixture reaches solidification and becomes solids stages, at this moment can be sanded and integer；At this moment with thumb pressed it is motionless it, at this moment phenol
There are about 90% end reaction intensity for urea formaldehyde, therefore can remove fixed clip, place it and maintain several angels at room temperature
It continues to solidify.
Center loaded method in step (11) specifically: multistage loadings are carried out to practical maximum to plate plane position of form center
Load；By sheet material measurement under by different load actions the variation of voltage and current calculate resistivity, utilize digital resistance instrument survey
It measures loading force and change in resistance curve calculates actual loading, while the security situation of plate is monitored.
The epoxide number of epoxy resin is 0.5 in step (3), the technical parameter of phenolic resin are as follows: free phenol is less than
1.5%, solid content about 50%, amount of flow 60mm, room temperature viscosity 300Pa.s.
By adopting the above technical scheme, method for supporting is set according to the actual support condition of test plate, different practical branch
Stay part uses different method for supporting.Such as: simply supported on four sides, opposite side freely-supported, arbitrary loading, opposite side are clamped.
Since graphene partial size is very small and is powder, the present invention is added multi-layer graphene using method is first mixed, is not easy in this way
It is adsorbed on stirring vessel and stirring blade and causes damages.The present invention improves phenolic resin base glass using a certain amount of graphene is added
Glass fibrous plate conduction and voltage-dependent characteristic, adapt to plate heating requirements under specified conditions, while can pass through real-time measurement resistance
Rate variation perception plate stress condition.
Although glass fibre additional amount is bigger, composite material strength is higher, and glass fibre additional amount is bigger, composite wood
The brittleness of material is also bigger.The effect of glass fibre: glass fibre is a kind of inorganic non-metallic material haveing excellent performance, heat resistance
By force, corrosion resistance is good, high mechanical strength, tensile strength are big.Tensile strength is 6.3~6.9g/d in normal conditions, moistens shape
5.4~5.8g/d of state, density 2.54g/cm3, glass fibre is in the composite material as reinforcing material.
Production method of the present invention is simple and easy, using the characteristic of graphene change in resistance under pressure, produces
Can with electrified regulation, it is sensitive to pressure change and can real-time monitoring glass fibre-reinforced phenolic resin plate.It makes
Plate keep its density it is small, intensity is high under the premise of, modulus is bigger, and wearability is stronger.After tested, based on the stone of phenolic resin
Black alkene+glass fiber compound material heating declines 80 times with the resistance of force sensing function plate is answered.Thermal coefficient improves 40%, pressure
Quick coefficient reaches 100 or more.
Specific embodiment
The production and stress measuring method of glass fibre-reinforced phenolic resin plate of the invention, comprising the following steps:
(1), graphene is formed into graphene powder after machine is hydride modified；
(2), the graphene powder for weighing constant weight is added portionwise in acetone soln, then places it in Ultrasound Instrument to mixed
Solution ultrasonic treatment is closed, finely dispersed suspension is prepared into；
(3), poly(aryl ether ketone), epoxy resin, phenolic resin are weighed according to the weight ratio of 1:1:8 spare；
(4) load weighted poly(aryl ether ketone) is uniformly mixed with epoxy resin, mixture is melted to obtain to performed polymer at a certain temperature,
Then performed polymer is put into pulverizer and breaks into powder, and pass through the dusting cover of 80 mesh；By performed polymer powder and load weighted phenolic aldehyde
Resin is added in blender and is stirred, and softening temperature or more is heated in mixed process, is at melt-flow state；
(5), the phenolic resin of melting is added in the suspension of step (2) preparation, after being mixed slowly using blender again quickly
Stirring forms graphene phenolic-resin complex liquid to being uniformly mixed；
(6), glass fibre is followed the steps below pretreatment: the acetone for being put into the 50 m L 40% that temperature is 30 DEG C is molten
After impregnating 20 min in liquid, oil removing wash with distilled water；It is 40 g/L that glass fabric after oil removing, which is soaked in 50 mL concentration,
Sodium hydroxide roughening solution in clean after 30 min, temperature maintains 60 DEG C；By the glass fabric being roughened at 35 DEG C
It is put into the sensitizing solution SnCl of 50 m L, 30 g/L2In after 20 min, cleaning；Glass fabric after sensitization is put into 50
The activating solution Pd Cl of 0.1 g/L of mL2In solution, 20 min are kept in 30 DEG C, finally wash with distilled water；
(7), pretreated glass fibre is put into graphene phenolic-resin complex liquid and sufficiently infiltrates；
(8), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(9) the graphene phenolic-resin complex liquid in step (5) is poured into board making mold, gas is discharged using vibratory drilling method
Bubble, until reaching design thickness；
(10), slurry successively forms plate, positive electrode after gel, solidification and curing three phases in board making mold
It adheres on plate with negative electrode and is integrally demoulded with plate；
(11), after a certain period of time by the cooling placement of plate, according to certain method for supporting, plate is carried out using center loaded method
On-load pressure, positive electrode and negative electrode connect digital resistance instrument, and digital resistance instrument measures loading force and change in resistance curve,
Complete plate pressure sensing calibration measurement.
The weight of graphene powder in step (2) is the 0.3% of the phenolic resin weight melted in step (3).
Using method addition graphene is first mixed in step (1), graphene uses multi-layer graphene, the rule of multi-layer graphene raw material
Lattice are diameter < 2 μm, with a thickness of 1-5nm, specific surface area 500m2/ g, density 2-2.25g/ml, thermal coefficient > 3000w/m
K, electric conductivity > 107S/m。
The softening point of the phenolic resin of melting is at 70 °C and following.
Graphene phenolic-resin complex liquid in step (5) can also be prepared with reduction method；
Reduction method prepares graphene phenolic-resin complex liquid process are as follows:
Graphene oxide is prepared using Hummers method is improved；3g graphite powder and 1g sodium nitrate are added equipped with the 69 mL concentrated sulfuric acids
In three-necked flask, it is slowly added to 12g potassium permanganate under stirring in ice-water bath, in 10 DEG C or less reaction 1h；35 DEG C are warming up to, is continued
2h is stirred, 120 mL deionized waters are slowly added to, system temperature is made to be increased to 95 DEG C, 30 min is maintained, a large amount of distilled water is added
Dilution, pours into 30%H2O2To no bubble generate, filter while hot, and with volume ratio for 1: 10 HCl solution wash it is filtered
Filter cake, using BaCl2Detection, until without SO in filtrate4, filtration cakes torrefaction obtains graphite oxide；Graphite oxide is soluble in water, surpass
Sound is allowed to be completely dispersed；Obtain graphene oxide；
50g phenolic resin and 25g propylene glycol monomethyl ether are added in three-necked flask, 80 DEG C is warming up to, is slowly added dropwise under stirring
10.5g diethanol amine reacts 2h；Then 60 DEG C are cooled to, 20% acetum reaction 30min is added dropwise, is then slowly added into steaming
The quick stirring and emulsifying of distilled water obtains cationic phenolic aldehyde emulsion；
It adds graphene oxide into Phenolic resin emulsion, stirs ultrasound 1h, keep the temperature 3h at 60 DEG C, then proceed to ultrasound
30min, filtering, obtains graphene oxide phenolic resin complex liquid.
The weight for the glass fibre being added in step (6) accounts for 30%-the 50% of graphene phenolic-resin complex liquid weight, glass
In glass fiber according to weight ratio contain 55% silica, 20% aluminum oxide and 12% magnesia.
Gel, solidification and the detailed process of curing in step (10) are as follows:
Gel: gel time is a part of curing time, and after mixing, resin/curing agent mixture is still liquid and can
To work and be suitble to application；In order to guarantee reliably to be bonded, all construction and positioning work should be done within the curing operation time
It is good；Solidification: mixture initially enters solidification phase, and at this moment it starts gel or " mutation "；At this moment phenolic aldehyde does not have prolonged work
It may make, will also lose viscosity；In this stage any interference cannot be carried out to it；It will become soft gel as hard rubber
Object, you with thumb will press it is dynamic it；
Curing: cure stage mixture is local solidification, the phenolic resin newly used still can with its chemical bonds, therefore should
Untreated surface still can be bonded or be reacted；Anyway, close to cured mixture, these abilities are reducing；Phenol
Aldehyde mixture reaches solidification and becomes solids stages, at this moment can be sanded and integer；At this moment with thumb pressed it is motionless it, at this moment phenol
There are about 90% end reaction intensity for urea formaldehyde, therefore can remove fixed clip, place it and maintain several angels at room temperature
It continues to solidify.
Center loaded method in step (11) specifically: multistage loadings are carried out to practical maximum to plate plane position of form center
Load；By sheet material measurement under by different load actions the variation of voltage and current calculate resistivity, utilize digital resistance instrument survey
It measures loading force and change in resistance curve calculates actual loading, while the security situation of plate is monitored.
The epoxide number of epoxy resin is 0.5 in step (3), the technical parameter of phenolic resin are as follows: free phenol is less than
1.5%, solid content about 50%, amount of flow 60mm, room temperature viscosity 300Pa.s.
The present invention carries out pressure sensing calibration measurement to plate while board making is completed, and by positive electrode and negative electricity
It is extremely left on plate in advance, positive electrode can be connected connection digital resistance by user with negative electrode in use process after plate factory
Instrument is monitored the stress moment of plate, it is ensured that the security reliability of plate.
The present embodiment not makes any form of restriction shape of the invention, material, structure etc., all according to this hair
Bright technical spirit any simple modification, equivalent change and modification to the above embodiments, belong to the technology of the present invention side
The protection scope of case.
Claims (9)
1. the production and stress measuring method of glass fibre-reinforced phenolic resin plate, it is characterised in that: the following steps are included:
(1), graphene is formed into graphene powder after machine is hydride modified；
(2), the graphene powder for weighing constant weight is added portionwise in acetone soln, then places it in Ultrasound Instrument to mixed
Solution ultrasonic treatment is closed, finely dispersed suspension is prepared into；
(3), poly(aryl ether ketone), epoxy resin, phenolic resin are weighed according to the weight ratio of 1:1:8 spare；
(4) load weighted poly(aryl ether ketone) is uniformly mixed with epoxy resin, mixture is melted to obtain to performed polymer at a certain temperature,
Then performed polymer is put into pulverizer and breaks into powder, and pass through the dusting cover of 80 mesh；By performed polymer powder and load weighted phenolic aldehyde
Resin is added in blender and is stirred, and softening temperature or more is heated in mixed process, is at melt-flow state；
(5), the phenolic resin of melting is added in the suspension of step (2) preparation, after being mixed slowly using blender again quickly
Stirring forms graphene phenolic-resin complex liquid to being uniformly mixed；
(6), glass fibre is followed the steps below pretreatment: the acetone for being put into the 50 m L 40% that temperature is 30 DEG C is molten
After impregnating 20 min in liquid, oil removing wash with distilled water；It is 40 g/L that glass fabric after oil removing, which is soaked in 50 mL concentration,
Sodium hydroxide roughening solution in clean after 30 min, temperature maintains 60 DEG C；By the glass fabric being roughened at 35 DEG C
It is put into the sensitizing solution SnCl of 50 m L, 30 g/L2In after 20 min, cleaning；Glass fabric after sensitization is put into 50
The activating solution Pd Cl of 0.1 g/L of mL2In solution, 20 min are kept in 30 DEG C, finally wash with distilled water；
(7), pretreated glass fibre is put into graphene phenolic-resin complex liquid and sufficiently infiltrates；
(8), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(9) the graphene phenolic-resin complex liquid in step (5) is poured into board making mold, gas is discharged using vibratory drilling method
Bubble, until reaching design thickness；
(10), slurry successively forms plate, positive electrode after gel, solidification and curing three phases in board making mold
It adheres on plate with negative electrode and is integrally demoulded with plate；
(11), after a certain period of time by the cooling placement of plate, according to certain method for supporting, plate is carried out using center loaded method
On-load pressure, positive electrode and negative electrode connect digital resistance instrument, and digital resistance instrument measures loading force and change in resistance curve,
Complete plate pressure sensing calibration measurement.
2. the production and stress measuring method of glass fibre-reinforced phenolic resin plate according to claim 1, feature
Be: the weight of the graphene powder in step (2) is the 0.3% of the phenolic resin weight melted in step (3).
3. the production and stress measuring method of glass fibre-reinforced phenolic resin plate according to claim 1, feature
Be: using method addition graphene is first mixed in step (1), graphene uses multi-layer graphene, the specification of multi-layer graphene raw material
For diameter < 2 μm, with a thickness of 1-5nm, specific surface area 500m2/ g, density 2-2.25g/ml, thermal coefficient > 3000w/mK,
Electric conductivity > 107S/m。
4. the production and stress measuring method of glass fibre-reinforced phenolic resin plate according to claim 2, feature
Be: the softening point of the phenolic resin of melting is at 70 °C and following.
5. the production and stress measuring method of glass fibre-reinforced phenolic resin plate according to claim 1, feature
Be: the graphene phenolic-resin complex liquid in step (5) can also be prepared with reduction method；
Reduction method prepares graphene phenolic-resin complex liquid process are as follows:
Graphene oxide is prepared using Hummers method is improved；3g graphite powder and 1g sodium nitrate are added equipped with the 69 mL concentrated sulfuric acids
In three-necked flask, it is slowly added to 12g potassium permanganate under stirring in ice-water bath, in 10 DEG C or less reaction 1h；35 DEG C are warming up to, is continued
2h is stirred, 120 mL deionized waters are slowly added to, system temperature is made to be increased to 95 DEG C, 30 min is maintained, a large amount of distilled water is added
Dilution, pours into 30%H2O2To no bubble generate, filter while hot, and with volume ratio for 1: 10 HCl solution wash it is filtered
Filter cake, using BaCl2Detection, until without SO in filtrate4, filtration cakes torrefaction obtains graphite oxide；Graphite oxide is soluble in water, surpass
Sound is allowed to be completely dispersed；Obtain graphene oxide；
50g phenolic resin and 25g propylene glycol monomethyl ether are added in three-necked flask, 80 DEG C is warming up to, is slowly added dropwise under stirring
10.5g diethanol amine reacts 2h；Then 60 DEG C are cooled to, 20% acetum reaction 30min is added dropwise, is then slowly added into steaming
The quick stirring and emulsifying of distilled water obtains cationic phenolic aldehyde emulsion；
It adds graphene oxide into Phenolic resin emulsion, stirs ultrasound 1h, keep the temperature 3h at 60 DEG C, then proceed to ultrasound
30min, filtering, obtains graphene oxide phenolic resin complex liquid.
6. the production and stress measuring method of glass fibre-reinforced phenolic resin plate according to claim 1, feature
Be: the weight for the glass fibre being added in step (6) accounts for 30%-the 50% of graphene phenolic-resin complex liquid weight, glass fibers
In dimension according to weight ratio contain 55% silica, 20% aluminum oxide and 12% magnesia.
7. the production and stress measuring method of glass fibre-reinforced phenolic resin plate according to claim 1, feature
It is: gel, solidification and the detailed process of curing in step (10) are as follows:
Gel: gel time is a part of curing time, and after mixing, resin/curing agent mixture is still liquid and can
To work and be suitble to application；In order to guarantee reliably to be bonded, all construction and positioning work should be done within the curing operation time
It is good；Solidification: mixture initially enters solidification phase, and at this moment it starts gel or " mutation "；At this moment phenolic aldehyde does not have prolonged work
It may make, will also lose viscosity；In this stage any interference cannot be carried out to it；It will become soft gel as hard rubber
Object, you with thumb will press it is dynamic it；
Curing: cure stage mixture is local solidification, the phenolic resin newly used still can with its chemical bonds, therefore should
Untreated surface still can be bonded or be reacted；Anyway, close to cured mixture, these abilities are reducing；Phenol
Aldehyde mixture reaches solidification and becomes solids stages, at this moment can be sanded and integer；At this moment with thumb pressed it is motionless it, at this moment phenol
There are about 90% end reaction intensity for urea formaldehyde, therefore can remove fixed clip, place it and maintain several angels at room temperature
It continues to solidify.
8. the production and stress measuring method of glass fibre-reinforced phenolic resin plate according to claim 1, feature
It is: the center loaded method in step (11) specifically: multistage loadings are carried out to practical maximum lotus to plate plane position of form center
It carries；By sheet material measurement under by different load actions the variation of voltage and current calculate resistivity, utilize digital resistance instrument measurement
Loading force and change in resistance curve calculate actual loading out, while being monitored to the security situation of plate.
9. the production and stress measuring method of glass fibre-reinforced phenolic resin plate according to claim 1, feature
Be: the epoxide number of epoxy resin is 0.5 in step (3), the technical parameter of phenolic resin are as follows: free phenol less than 1.5%,
Solid content about 50%, amount of flow 60mm, room temperature viscosity 300Pa.s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810738409.1A CN109206840A (en) | 2018-07-06 | 2018-07-06 | The production and stress measuring method of glass fibre-reinforced phenolic resin plate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810738409.1A CN109206840A (en) | 2018-07-06 | 2018-07-06 | The production and stress measuring method of glass fibre-reinforced phenolic resin plate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109206840A true CN109206840A (en) | 2019-01-15 |
Family
ID=64990279
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810738409.1A Pending CN109206840A (en) | 2018-07-06 | 2018-07-06 | The production and stress measuring method of glass fibre-reinforced phenolic resin plate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109206840A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971119A (en) * | 2019-03-29 | 2019-07-05 | 河北纳格新材料科技有限公司 | A kind of glass fibre-reinforced phenolic resin composite material and preparation method |
| CN113248747A (en) * | 2021-07-10 | 2021-08-13 | 山东墨匠新材料科技有限公司 | Preparation method of modified glass fiber resin composite material |
| CN113911382A (en) * | 2021-11-02 | 2022-01-11 | 中国商用飞机有限责任公司 | Air cavity shelf, method for manufacturing air cavity shelf and electronic equipment shelf |
| IT202000026621A1 (en) * | 2020-11-09 | 2022-05-09 | Idea & Sviluppo Srl | COMPOSITE MATERIALS BASED ON LIGHT-CURING EPOXY RESIN WITH GRAPHENE OXIDE DERIVATIVES AND RELATED PRODUCTION METHOD. |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107081916A (en) * | 2017-04-18 | 2017-08-22 | 中北大学 | The preparation method of nickel coated glass fibres fabric/epoxy resin electromagnetic shielding composite material |
| CN107418032A (en) * | 2017-06-16 | 2017-12-01 | 东台晨霞新材料科技有限公司 | A kind of graphene-containing/fibre reinforced composites and preparation method thereof |
-
2018
- 2018-07-06 CN CN201810738409.1A patent/CN109206840A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107081916A (en) * | 2017-04-18 | 2017-08-22 | 中北大学 | The preparation method of nickel coated glass fibres fabric/epoxy resin electromagnetic shielding composite material |
| CN107418032A (en) * | 2017-06-16 | 2017-12-01 | 东台晨霞新材料科技有限公司 | A kind of graphene-containing/fibre reinforced composites and preparation method thereof |
Non-Patent Citations (5)
| Title |
|---|
| 任冬燕: "《玻璃钢制品手糊及模压成型》", 30 June 2011, 武汉理工大学出版社 * |
| 李登新等: "《NOx催化氧化吸收技术与系统》", 30 November 2017, 中国环境出版社 * |
| 赵方冉等: "《土木工程材料》", 31 July 2004, 上海：同济大学出版社 * |
| 邢丽英: "《结构功能一体化复合材料技术》", 31 July 2017, 航空工业出版社 * |
| 陈建剑等: ""石墨烯改性环氧树脂/碳纤维复丝拉伸性能的影响"", 《合成纤维工业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971119A (en) * | 2019-03-29 | 2019-07-05 | 河北纳格新材料科技有限公司 | A kind of glass fibre-reinforced phenolic resin composite material and preparation method |
| IT202000026621A1 (en) * | 2020-11-09 | 2022-05-09 | Idea & Sviluppo Srl | COMPOSITE MATERIALS BASED ON LIGHT-CURING EPOXY RESIN WITH GRAPHENE OXIDE DERIVATIVES AND RELATED PRODUCTION METHOD. |
| CN113248747A (en) * | 2021-07-10 | 2021-08-13 | 山东墨匠新材料科技有限公司 | Preparation method of modified glass fiber resin composite material |
| CN113911382A (en) * | 2021-11-02 | 2022-01-11 | 中国商用飞机有限责任公司 | Air cavity shelf, method for manufacturing air cavity shelf and electronic equipment shelf |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109206840A (en) | The production and stress measuring method of glass fibre-reinforced phenolic resin plate | |
| CN109111694A (en) | The production and stress measuring method of glass fiber reinforced epoxy resin plate | |
| CN108676326A (en) | Graphene based on epoxy resin and glass fiber reinforcement plank | |
| CN109265909A (en) | The board making and stress determination method of basalt fibre enhancing phenolic resin | |
| CN109265917A (en) | Basalt fibre reinforced epoxy board making and stress measuring method | |
| CN109203500A (en) | The plate forming and stress determination method of carbon-fibre reinforced epoxy resin | |
| CN107057283B (en) | A kind of carbon fiber enhancement resin base composite material and preparation method thereof | |
| CN108914681A (en) | A kind of preparation method of carbon fiber paper | |
| CN109228076A (en) | The plate forming and stress determination method of carbon fiber reinforced phenol formaldehyde resin | |
| CN105566857B (en) | A kind of lightweight epoxy resin composite material and preparation method thereof | |
| CN109111695A (en) | The production method of graphene and aramid fiber mixing reinforced epoxy plate | |
| CN106968128A (en) | A kind of soft graphite alkenyl extrusion coating paper and its preparation method and application | |
| CN104530653A (en) | Preparation method of epoxy resin/graphene/nano copper composite material | |
| CN106118003A (en) | A kind of modified reinforced polyester glass-reinforced plastic material and preparation method thereof | |
| Varma et al. | Coir fibres II: evaluation as a reinforcement in unsaturated polyester resin composites | |
| CN109181210A (en) | The plate forming and stress determination method of boron fibre enhancing phenolic resin | |
| CN108997708A (en) | Para-aramid fiber enhances phenolic resin board making and stress measuring method | |
| CN110126368A (en) | A kind of electric heating rubber and preparation method thereof | |
| CN109262924A (en) | The board making and stress determination method of basalt fibre enhancing unsaturated-resin | |
| CN109016577A (en) | The production and stress measuring method of glass fiber reinforcement unsaturated-resin plate | |
| CN109161157A (en) | Para-aramid fiber reinforced epoxy board making and stress measuring method | |
| CN108707310A (en) | With heating and making and the stress assay method of answering force sensing function plank | |
| CN103923462A (en) | Preparation method of modified PBO [poly(p-phenylene benzobisoxazole)] fiber prepreg | |
| CN109135169A (en) | The production method of graphene and aramid fiber mixing enhancing phenolic resin plate | |
| CN108081691A (en) | A kind of carbon fiber prepreg of aramid fiber short fibre enhancing, preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190115 |
|
| RJ01 | Rejection of invention patent application after publication |