CN109265917A - Basalt fibre reinforced epoxy board making and stress measuring method - Google Patents
Basalt fibre reinforced epoxy board making and stress measuring method Download PDFInfo
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- CN109265917A CN109265917A CN201810799831.8A CN201810799831A CN109265917A CN 109265917 A CN109265917 A CN 109265917A CN 201810799831 A CN201810799831 A CN 201810799831A CN 109265917 A CN109265917 A CN 109265917A
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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
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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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
- 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
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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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
- C08K7/10—Silicon-containing compounds
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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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Abstract
Basalt fibre reinforced epoxy board making and stress measuring method, comprising the following steps: weighing graphene powder, which is added in acetone soln, is prepared into suspension；Epoxy resin and polyamide are mixed to form the epoxy resin melt of melting；Epoxy resin melt is added in graphene epoxy resin complex liquid；It will be put into infiltration in graphene epoxy resin complex liquid after a series of processing of basalt fibre and form slurry, slurry is poured into board making mold；Successively 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 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 basalt fibre technical field, and in particular to one kind has heating and stress
The basalt fibre reinforced epoxy board making and stress measuring method of perceptional function.
Background technique
Basalt fibre is the continuous fibre made of platinum-rhodium alloy bushing using natural basalt ore as raw material
Dimension has preferable tensile property, resistance to heavy corrosion and chemical stability, high temperature resistant, high heat insulation performance, good insulating.
Epoxy resin is by artificial synthesized a kind of high molecular polymer.For thick liquid or the solid that can soften is heated,
Usually there is the temperature range of melting or softening when heated, can be under external force Plastic Flow state, produce synthetic resin
Raw material sources are abundant.Synthetic resin has very strong cohesive force, and molecular structure is fine and close, due to containing vivaciously not in molecular structure
Saturated group crosslinks them with a plurality of types of curing agent and reacts and being formed insoluble has three-way grid structure
High polymer.Synthetic resin after solidification has good physics, chemical property, it has the surface of metal and nonmetallic materials
There is excellent adhesion strength, dielectric properties are good, and set shrinking percentage is small, and product size stability is good, and hardness is high, and flexibility is good.
Basalt fibre reinforced epoxy composite board is one of current most widely used composite material, is had
The advantages that density is small, intensity is high, in addition its raw material sources is extensive, machine-shaping is easy, high production efficiency, and designability is strong,
It is to be widely used in the important composite board of one of national economy and national defense construction.It is somebody's turn to do but the composite panel insulate not
Conduction is unable to electrified regulation, using being subject to certain restrictions in cold climate.The load that plate is subject to cannot be from perception, special item
There are hidden danger for safety under part.
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 epoxy resin-matrix basalt fibre
Enhance composite material function/intelligent behaviour.With the sharp fall of graphene price, graphene is led applied to composite material
Domain undoubtedly has 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
It puts, it being capable of electrified regulation, the basalt fibre reinforced epoxy board making of perception plate pressure change and stress measurement
Method.
In order to solve the above technical problems, the present invention adopts the following technical scheme: basalt fibre reinforced epoxy 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), the epoxy resin of constant weight is weighed, the epoxide number of epoxy resin is 0.60eq/100g, and heating epoxy resin is to soft
Change temperature or more, is at the epoxy resin melt that melt-flow state forms melting；
(4), the epoxy resin melt of melting is added in the suspension of step (2) preparation, after being mixed slowly using blender again
Quickly stirring forms graphene epoxy resin complex liquid to being uniformly mixed；
(5), a certain amount of basalt fibre is weighed, the line density of basalt fibre is 400tex, and basalt fibre is cut into
Size identical with board making mold size shape, with five to six hours of soaked in absolute ethyl alcohol；Being then placed in medium is third
Vibration washing half an hour in the supersonic wave cleaning machine of ketone；It finally dries or is dried up with hair dryer spare；
It (6), is 1:1 ratio dehydrated alcohol and deionized water mixing for standby use with volume ratio, with volumetric flask silane coupling agent
KH550 matches the solution as concentration 0.75%, and after mixing evenly, hydrolysis is poured into plastic tub for five minutes；According still further to three to ten bath
It is put into plastic tub than the basalt fibre product after drying, impregnates three and ten minutes later take out basalt fibre product；Most
After be laid in naturally dry on testing stand, place into 110 DEG C of air dry ovens dry, taken out after a hour, use preservative film
It wraps, is placed on after shady place is fully cooled, is finally putting into graphene phenolic-resin complex liquid sufficiently infiltration and forms slurry；
(7), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(8), the slurry in step (6) is poured into board making mold, bubble is discharged using vibratory drilling method, it is thick until reaching design
Degree；
(9), 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；
(10), plate is placed after a certain period of time, according to certain method for supporting, plate is loaded using center loaded method
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；
(11), plate is packaged.
The weight of graphene powder in step (2) is the 0.3% of the epoxy resin melt weight melted in step (4).
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 epoxy resin melt of melting is at 70 °C and following.
Graphene epoxy resin complex liquid in step (4) can also be prepared with reduction method；
Reduction method prepares graphene epoxy 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 or so are warming up to,
Continue to stir 2h；120 mL deionized waters are slowly added to, system temperature is made to be increased to 95 DEG C or so, maintain 30 min, are added big
Distilled water dilution is measured, 30%H is poured into2O2It generates to no bubble, filters while hot, and washed with the HCl solution that volume ratio is 1: 10
Filter cake, using BaCl2Detection, until without SO in filtrate4, it is dried to obtain graphite oxide；Graphite oxide is soluble in water, and ultrasound makes
Be completely dispersed；Obtain graphene oxide；
50 epoxy 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 unsaturation lotion；
It adds graphene oxide into epoxy resin latex, stirs ultrasound 1h, keep the temperature 3h at 60 DEG C, then proceed to ultrasound
30min, filtering, obtains graphene oxide/epoxy blend dispersion liquid.
The weight for the basalt fibre being added in step (6) accounts for 30%-the 50% of graphene epoxy resin complex liquid weight.
Gel, solidification and the detailed process of curing in step (8) 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 unsaturation is not prolonged
Work is possible, will also lose viscosity；In this stage any interference cannot be carried out to it；It will become soft gel as hard rubber
Object, with thumb will press it is dynamic it；
Curing: cure stage mixture is local solidification, the epoxy 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；No
Saturated 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
There are about 90% end reaction intensity for epoxy resin, therefore can remove fixed clip, place it and maintain several days at room temperature
It is set to continue to solidify.
Center loaded method in step (10) 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 technical parameter of epoxy resin in step (3) 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 is profound using a certain amount of graphene improvement epoxy resin-matrix is added
Military rock fibrous plate conduction and voltage-dependent characteristic adapt to plate heating requirements under specified conditions, while can pass through real-time measurement electricity
Resistance rate variation perception plate stress condition.
Although basalt fibre additional amount is bigger, composite material strength is higher, and basalt fibre additional amount is bigger, multiple
The brittleness of condensation material is also bigger.The effect of basalt fibre: basalt fibre is a kind of inorganic non-metallic material haveing excellent performance,
Heat resistance is strong, corrosion resistance is good, high mechanical strength, tensile strength are big.Tensile strength is 6.3~6.9g/d in normal conditions,
5.4~5.8g/d of moisture state, density 2.54g/cm3, basalt fibre are used as a kind of reinforcing material in the composite 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 basalt fibre reinforced epoxy 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 epoxy resin
Graphene+basalt fiber composite material heating declines 80 times with the resistance of force sensing function plate is answered.Thermal coefficient improves
40%, pressure-sensitive coefficient reaches 100 or more.
Specific embodiment
Basalt fibre reinforced epoxy board making and stress measuring method 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), the epoxy resin of constant weight is weighed, the epoxide number of epoxy resin is 0.60eq/100g, and heating epoxy resin is to soft
Change temperature or more, is at the epoxy resin melt that melt-flow state forms melting；
(4), the epoxy resin melt of melting is added in the suspension of step (2) preparation, after being mixed slowly using blender again
Quickly stirring forms graphene epoxy resin complex liquid to being uniformly mixed；
(5), a certain amount of basalt fibre is weighed, the line density of basalt fibre is 400tex, and basalt fibre is cut into
Size identical with board making mold size shape, with five to six hours of soaked in absolute ethyl alcohol；Being then placed in medium is third
Vibration washing half an hour in the supersonic wave cleaning machine of ketone；It finally dries or is dried up with hair dryer spare；
It (6), is 1:1 ratio dehydrated alcohol and deionized water mixing for standby use with volume ratio, with volumetric flask silane coupling agent
KH550 matches the solution as concentration 0.75%, and after mixing evenly, hydrolysis is poured into plastic tub for five minutes；According still further to three to ten bath
It is put into plastic tub than the basalt fibre product after drying, impregnates three and ten minutes later take out basalt fibre product；Most
After be laid in naturally dry on testing stand, place into 110 DEG C of air dry ovens dry, taken out after a hour, use preservative film
It wraps, is placed on after shady place is fully cooled, is finally putting into graphene phenolic-resin complex liquid sufficiently infiltration and forms slurry；
(7), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(8), the slurry in step (6) is poured into board making mold, bubble is discharged using vibratory drilling method, it is thick until reaching design
Degree；
(9), 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；
(10), plate is placed after a certain period of time, according to certain method for supporting, plate is loaded using center loaded method
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；
(11), plate is packaged.
The weight of graphene powder in step (2) is the 0.3% of the epoxy resin melt weight melted in step (4).
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 epoxy resin melt of melting is at 70 °C and following.
Graphene epoxy resin complex liquid in step (4) can also be prepared with reduction method；
Reduction method prepares graphene epoxy 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 or so are warming up to,
Continue to stir 2h；120 mL deionized waters are slowly added to, system temperature is made to be increased to 95 DEG C or so, maintain 30 min, are added big
Distilled water dilution is measured, 30%H is poured into2O2It generates to no bubble, filters while hot, and washed with the HCl solution that volume ratio is 1: 10
Filter cake, using BaCl2Detection, until without SO in filtrate4, it is dried to obtain graphite oxide；Graphite oxide is soluble in water, and ultrasound makes
Be completely dispersed；Obtain graphene oxide；
50 epoxy 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 unsaturation lotion；
It adds graphene oxide into epoxy resin latex, stirs ultrasound 1h, keep the temperature 3h at 60 DEG C, then proceed to ultrasound
30min, filtering, obtains graphene oxide/epoxy blend dispersion liquid.
The weight for the basalt fibre being added in step (6) accounts for 30%-the 50% of graphene epoxy resin complex liquid weight.
Gel, solidification and the detailed process of curing in step (8) 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 unsaturation is not prolonged
Work is possible, will also lose viscosity；In this stage any interference cannot be carried out to it；It will become soft gel as hard rubber
Object, with thumb will press it is dynamic it；
Curing: cure stage mixture is local solidification, the epoxy 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；No
Saturated 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
There are about 90% end reaction intensity for epoxy resin, therefore can remove fixed clip, place it and maintain several days at room temperature
It is set to continue to solidify.
Center loaded method in step (10) 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 technical parameter of epoxy resin in step (3) 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 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. basalt fibre reinforced epoxy board making and stress measuring method, 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), the epoxy resin of constant weight is weighed, the epoxide number of epoxy resin is 0.60eq/100g, and heating epoxy resin is to soft
Change temperature or more, is at the epoxy resin melt that melt-flow state forms melting；
(4), the epoxy resin melt of melting is added in the suspension of step (2) preparation, after being mixed slowly using blender again
Quickly stirring forms graphene epoxy resin complex liquid to being uniformly mixed；
(5), a certain amount of basalt fibre is weighed, the line density of basalt fibre is 400tex, and basalt fibre is cut into
Size identical with board making mold size shape, with five to six hours of soaked in absolute ethyl alcohol；Being then placed in medium is third
Vibration washing half an hour in the supersonic wave cleaning machine of ketone；It finally dries or is dried up with hair dryer spare；
It (6), is 1:1 ratio dehydrated alcohol and deionized water mixing for standby use with volume ratio, with volumetric flask silane coupling agent
KH550 matches the solution as concentration 0.75%, and after mixing evenly, hydrolysis is poured into plastic tub for five minutes；According still further to three to ten bath
It is put into plastic tub than the basalt fibre product after drying, impregnates three and ten minutes later take out basalt fibre product；Most
After be laid in naturally dry on testing stand, place into 110 DEG C of air dry ovens dry, taken out after a hour, use preservative film
It wraps, is placed on after shady place is fully cooled, is finally putting into graphene phenolic-resin complex liquid sufficiently infiltration and forms slurry；
(7), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(8), the slurry in step (6) is poured into board making mold, bubble is discharged using vibratory drilling method, it is thick until reaching design
Degree；
(9), 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；
(10), plate is placed after a certain period of time, according to certain method for supporting, plate is loaded using center loaded method
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；
(11), plate is packaged.
2. basalt fibre reinforced epoxy board making according to claim 1 and stress measuring method, feature
Be: the weight of the graphene powder in step (2) is the 0.3% of the epoxy resin melt weight melted in step (4).
3. basalt fibre reinforced epoxy board making according to claim 1 and stress measuring method, 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. basalt fibre reinforced epoxy board making according to claim 2 and stress measuring method, feature
Be: the softening point of the epoxy resin melt of melting is at 70 °C and following.
5. basalt fibre reinforced epoxy board making according to claim 1 and stress measuring method, feature
Be: the graphene epoxy resin complex liquid in step (4) can also be prepared with reduction method；
Reduction method prepares graphene epoxy 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 or so are warming up to,
Continue to stir 2h；120 mL deionized waters are slowly added to, system temperature is made to be increased to 95 DEG C or so, maintain 30 min, are added big
Distilled water dilution is measured, 30%H is poured into2O2It generates to no bubble, filters while hot, and washed with the HCl solution that volume ratio is 1: 10
Filter cake, using BaCl2Detection, until without SO in filtrate4, it is dried to obtain graphite oxide；Graphite oxide is soluble in water, and ultrasound makes
Be completely dispersed；Obtain graphene oxide；
50 epoxy 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 unsaturation lotion；
It adds graphene oxide into epoxy resin latex, stirs ultrasound 1h, keep the temperature 3h at 60 DEG C, then proceed to ultrasound
30min, filtering, obtains graphene oxide/epoxy blend dispersion liquid.
6. basalt fibre reinforced epoxy board making according to claim 1 and stress measuring method, feature
Be: the weight for the basalt fibre being added in step (6) accounts for 30%-the 50% of graphene epoxy resin complex liquid weight.
7. basalt fibre reinforced epoxy board making according to claim 1 and stress measuring method, feature
It is: gel, solidification and the detailed process of curing in step (8) 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 unsaturation is not prolonged
Work is possible, will also lose viscosity；In this stage any interference cannot be carried out to it；It will become soft gel as hard rubber
Object, with thumb will press it is dynamic it；
Curing: cure stage mixture is local solidification, the epoxy 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；No
Saturated 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
There are about 90% end reaction intensity for epoxy resin, therefore can remove fixed clip, place it and maintain several days at room temperature
It is set to continue to solidify.
8. basalt fibre reinforced epoxy board making according to claim 1 and stress measuring method, feature
It is: the center loaded method in step (10) 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. basalt fibre reinforced epoxy board making according to claim 1 and stress measuring method, feature
Be: the technical parameter of epoxy resin in step (3) 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 |
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| CN116001189A (en) * | 2023-03-24 | 2023-04-25 | 达州增美玄武岩纤维科技有限公司 | Injection molding process of basalt fiber composite material |
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| CN116001189A (en) * | 2023-03-24 | 2023-04-25 | 达州增美玄武岩纤维科技有限公司 | Injection molding process of basalt fiber composite material |
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