CN109161157A - Para-aramid fiber reinforced epoxy board making and stress measuring method - Google Patents
Para-aramid fiber reinforced epoxy board making and stress measuring method Download PDFInfo
- Publication number
- CN109161157A CN109161157A CN201810743077.6A CN201810743077A CN109161157A CN 109161157 A CN109161157 A CN 109161157A CN 201810743077 A CN201810743077 A CN 201810743077A CN 109161157 A CN109161157 A CN 109161157A
- Authority
- CN
- China
- Prior art keywords
- graphene
- epoxy resin
- para
- aramid fiber
- board making
- 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
- 238000000034 method Methods 0.000 title claims abstract description 53
- 239000000835 fiber Substances 0.000 title claims abstract description 35
- 229920003235 aromatic polyamide Polymers 0.000 title claims abstract description 34
- 239000004593 Epoxy Substances 0.000 title claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 73
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 63
- 239000003822 epoxy resin Substances 0.000 claims abstract description 46
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000007711 solidification Methods 0.000 claims abstract description 20
- 230000008023 solidification Effects 0.000 claims abstract description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000008859 change Effects 0.000 claims abstract description 14
- 238000011068 loading method Methods 0.000 claims abstract description 14
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 239000004952 Polyamide Substances 0.000 claims abstract description 10
- 229920002647 polyamide Polymers 0.000 claims abstract description 10
- 229920005989 resin Polymers 0.000 claims abstract description 10
- 239000011347 resin Substances 0.000 claims abstract description 10
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 230000008595 infiltration Effects 0.000 claims abstract description 4
- 238000001764 infiltration Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 18
- 238000002604 ultrasonography Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- 210000003813 thumb Anatomy 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 3
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 229920001875 Ebonite Polymers 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 241000270708 Testudinidae Species 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 229910001626 barium chloride Inorganic materials 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 125000002091 cationic group Chemical group 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 229940043237 diethanolamine Drugs 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000005553 drilling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000001804 emulsifying effect Effects 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 150000004678 hydrides Chemical group 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 239000004816 latex Substances 0.000 claims description 3
- 229920000126 latex Polymers 0.000 claims description 3
- 239000006210 lotion Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000035772 mutation Effects 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 230000002035 prolonged effect Effects 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 abstract description 4
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 239000003365 glass fiber Substances 0.000 abstract 1
- 230000002787 reinforcement Effects 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 9
- 229920000642 polymer Polymers 0.000 description 4
- 229920006231 aramid fiber Polymers 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920003002 synthetic resin Polymers 0.000 description 3
- 239000000057 synthetic resin Substances 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 241000549556 Nanos Species 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0019—Compressive
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0617—Electrical or magnetic indicating, recording or sensing means
- G01N2203/0623—Electrical or magnetic indicating, recording or sensing means using piezoelectric gauges
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Para-aramid fiber 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 is put into infiltration in graphene epoxy resin complex liquid after para-aramid fiber is handled and forms 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 glass fiber reinforcement unsaturated-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 para-aramid fiber technical field, and in particular to one kind has heating and answers
The para-aramid fiber reinforced epoxy board making and stress measuring method of force sensing function.
Background technique
P-aramid fiber belongs to high rigidity polymer, and molecular structure has the symmetry and regularity of height, macromolecular chain
Between form very strong hydrogen bond, therefore there is high intensity, high-modulus, high temperature resistant, low-density, heat-shrinkable is small, dimensional stability
The advantages that good.
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.
Para-aramid fiber reinforced epoxy composite board is one of current most widely used composite material, tool
Have the advantages that density is small, intensity is high, in addition its raw material sources is extensive, machine-shaping is easy, designability is strong, is to be widely applied
In key areas such as aerospace, security protection, backbone equipment, communications and transportation, automobile manufacture and structure enhancings.But the composite wood
Flitch electric conductivity is poor, is unable to electrified regulation, using being subject to certain restrictions in cold climate.The load that plate is subject to is unable to self-induction
Know, 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 epoxy resin-matrix p-aramid fiber fibre
Dimension enhancing composite material function/intelligent behaviour.With the sharp fall of graphene price, graphene is applied to composite material
Field 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 para-aramid fiber reinforced epoxy board making of perception plate pressure change and stress survey
Determine method.
In order to solve the above technical problems, the present invention adopts the following technical scheme: para-aramid fiber reinforced epoxy plate
Material 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), epoxy resin and polyamide are weighed and are mixed according to mass ratio 5:3, preheat 20min at 50 DEG C,
To viscosity drop as low as postposition to a certain degree in a vacuum drying oven, vacuumize 40min under the conditions of 50 DEG C, removal epoxy resin and
Bubble present in polyamide；Then the acetone and mass fraction 20% of mass fraction 10% are sequentially added in the epoxy
Dibutyl phthalate, will guarantee to be uniformly mixed after being added each time, then pour into carbon fiber in batches, be eventually adding
Curing agent polyamide, stirs, and 30min is vibrated in ultrasonic cleaner, finally puts in a vacuum drying oven
40min is vacuumized at a temperature of 50 DEG C, to remove the epoxy resin melt for forming melting in whipping process after mixed bubble；
(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 resin compounded liquid to being uniformly mixed；
(5), para-aramid fiber is immersed in dichloroethanes, heating is boiled and then immersed in dehydrated alcohol again, and heating is boiled, and is removed
The inorganic agent for going to para-aramid fiber surface, it is dry in the hot constant temperature blast drying oven of tortoise after the completion of processing, stone is put into after dry
Sufficiently infiltration forms slurry in black alkene epoxy resin complex liquid；
(6), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(7) slurry in step (5) is poured into board making mold, bubble is discharged using vibratory drilling method, it is thick until reaching design
Degree；
(8), 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；
(9), 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；
(10), positive electrode and negative electrode are removed, 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；
50g 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 para-aramid fiber being added in step (6) accounts for 30%-the 50% of graphene resin compounded 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, you 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.
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 epoxy resin-matrix pair using a certain amount of graphene is added
Position aramid fiber plate conduction and voltage-dependent characteristic, adapt to plate heating requirements under specified conditions, while can pass through real-time measurement
Change in resistance perceives plate stress condition.
Although para-aramid fiber additional amount is bigger, composite material strength is higher, and para-aramid fiber additional amount is got over
Greatly, the brittleness of composite material is also bigger.The effect of para-aramid fiber: para-aramid fiber be it is a kind of have excellent performance it is inorganic non-
Metal material, heat resistance is strong, corrosion resistance is good, high mechanical strength, tensile strength are big.Tensile strength is 6.3 in normal conditions
~6.9g/d, 5.4~5.8g/d of moisture state, density 2.54g/cm3, para-aramid fiber is in the composite material as one kind
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 para-aramid fiber reinforced epoxy plate.It produces
Come plate keep its density it is small, intensity is high under the premise of, modulus is bigger, and wearability is stronger.After tested, it is based on epoxy resin
Graphene+para-aramid fiber composite material heating with answer force sensing function plate resistance decline 80 times.Thermal coefficient mentions
High by 40%, pressure-sensitive coefficient reaches 100 or more.
Specific embodiment
Para-aramid fiber reinforced epoxy board making 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), epoxy resin and polyamide are weighed and are mixed according to mass ratio 5:3, preheat 20min at 50 DEG C,
To viscosity drop as low as postposition to a certain degree in a vacuum drying oven, vacuumize 40min under the conditions of 50 DEG C, removal epoxy resin and
Bubble present in polyamide；Then the acetone and mass fraction 20% of mass fraction 10% are sequentially added in the epoxy
Dibutyl phthalate, will guarantee to be uniformly mixed after being added each time, then pour into carbon fiber in batches, be eventually adding
Curing agent polyamide, stirs, and 30min is vibrated in ultrasonic cleaner, finally puts in a vacuum drying oven
40min is vacuumized at a temperature of 50 DEG C, to remove the epoxy resin melt for forming melting in whipping process after mixed bubble；
(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 resin compounded liquid to being uniformly mixed；
(5), para-aramid fiber is immersed in dichloroethanes, heating is boiled and then immersed in dehydrated alcohol again, and heating is boiled, and is removed
The inorganic agent for going to para-aramid fiber surface, it is dry in the hot constant temperature blast drying oven of tortoise after the completion of processing, stone is put into after dry
Sufficiently infiltration forms slurry in black alkene epoxy resin complex liquid；
(6), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(7) slurry in step (5) is poured into board making mold, bubble is discharged using vibratory drilling method, it is thick until reaching design
Degree；
(8), 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；
(9), 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；
(10), positive electrode and negative electrode are removed, 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；
50g 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 para-aramid fiber being added in step (6) accounts for 30%-the 50% of graphene resin compounded 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, you 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 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 (8)
1. para-aramid fiber 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), epoxy resin and polyamide are weighed and are mixed according to mass ratio 5:3, preheat 20min at 50 DEG C,
To viscosity drop as low as postposition to a certain degree in a vacuum drying oven, vacuumize 40min under the conditions of 50 DEG C, removal epoxy resin and
Bubble present in polyamide；Then the acetone and mass fraction 20% of mass fraction 10% are sequentially added in the epoxy
Dibutyl phthalate, will guarantee to be uniformly mixed after being added each time, then pour into carbon fiber in batches, be eventually adding
Curing agent polyamide, stirs, and 30min is vibrated in ultrasonic cleaner, finally puts in a vacuum drying oven
40min is vacuumized at a temperature of 50 DEG C, to remove the epoxy resin melt for forming melting in whipping process after mixed bubble；
(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 resin compounded liquid to being uniformly mixed；
(5), para-aramid fiber is immersed in dichloroethanes, heating is boiled and then immersed in dehydrated alcohol again, and heating is boiled, and is removed
The inorganic agent for going to para-aramid fiber surface, it is dry in the hot constant temperature blast drying oven of tortoise after the completion of processing, stone is put into after dry
Sufficiently infiltration forms slurry in black alkene epoxy resin complex liquid；
(6), positive electrode and negative electrode are embedded in the diagonal position of board making die inside wall respectively, reserve connecting terminal；
(7) slurry in step (5) is poured into board making mold, bubble is discharged using vibratory drilling method, it is thick until reaching design
Degree；
(8), 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；
(9), 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；
(10), positive electrode and negative electrode are removed, plate is packaged.
2. para-aramid fiber reinforced epoxy board making according to claim 1 and stress measuring method, special
Sign is: the weight of the graphene powder in step (2) is the 0.3% of the epoxy resin melt weight melted in step (4).
3. para-aramid fiber reinforced epoxy board making according to claim 1 and stress measuring method, special
Sign is: 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。
4. para-aramid fiber reinforced epoxy board making according to claim 2 and stress measuring method, special
Sign is: the softening point of the epoxy resin melt of melting is at 70 °C and following.
5. para-aramid fiber reinforced epoxy board making according to claim 1 and stress measuring method, special
Sign is: 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；
50g 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. para-aramid fiber reinforced epoxy board making according to claim 1 and stress measuring method, special
Sign is: the weight for the para-aramid fiber being added in step (6) accounts for 30%-the 50% of graphene resin compounded liquid weight.
7. para-aramid fiber reinforced epoxy board making according to claim 1 and stress measuring method, special
Sign 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, you 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. para-aramid fiber reinforced epoxy board making according to claim 1 and stress measuring method, special
Sign is: the center loaded method in step (10) specifically: carries out multistage loadings 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810743077.6A CN109161157A (en) | 2018-07-09 | 2018-07-09 | Para-aramid fiber reinforced epoxy board making and stress measuring method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810743077.6A CN109161157A (en) | 2018-07-09 | 2018-07-09 | Para-aramid fiber reinforced epoxy board making and stress measuring method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109161157A true CN109161157A (en) | 2019-01-08 |
Family
ID=64897503
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810743077.6A Pending CN109161157A (en) | 2018-07-09 | 2018-07-09 | Para-aramid fiber reinforced epoxy board making and stress measuring method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109161157A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971126A (en) * | 2019-03-29 | 2019-07-05 | 河北纳格新材料科技有限公司 | A kind of aramid fiber reinforced epoxy composite material and preparation method |
| CN111463417A (en) * | 2020-04-17 | 2020-07-28 | 贵州梅岭电源有限公司 | Method for doping conductive agent into positive electrode material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554530A (en) * | 2013-10-11 | 2014-02-05 | 中国航空工业集团公司北京航空材料研究院 | Electric conductive continuous fiber-reinforced fabric or prepreg and electric conductive treatment method |
| CN108997708A (en) * | 2018-07-09 | 2018-12-14 | 黄河科技学院 | Para-aramid fiber enhances phenolic resin board making and stress measuring method |
-
2018
- 2018-07-09 CN CN201810743077.6A patent/CN109161157A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554530A (en) * | 2013-10-11 | 2014-02-05 | 中国航空工业集团公司北京航空材料研究院 | Electric conductive continuous fiber-reinforced fabric or prepreg and electric conductive treatment method |
| CN108997708A (en) * | 2018-07-09 | 2018-12-14 | 黄河科技学院 | Para-aramid fiber enhances phenolic resin board making and stress measuring method |
Non-Patent Citations (3)
| Title |
|---|
| 国家电网公司武汉高压研究所: "《电力检测与故障诊断技术全书 （一）GIS、开关卷（下）》", 30 September 2005 * |
| 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 * |
| 陈建剑 等: "石墨烯改性对环氧树脂／碳纤维复丝拉伸性能的影响", 《合成纤维工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971126A (en) * | 2019-03-29 | 2019-07-05 | 河北纳格新材料科技有限公司 | A kind of aramid fiber reinforced epoxy composite material and preparation method |
| CN111463417A (en) * | 2020-04-17 | 2020-07-28 | 贵州梅岭电源有限公司 | Method for doping conductive agent into positive electrode material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108676326A (en) | Graphene based on epoxy resin and glass fiber reinforcement plank | |
| Guadagno et al. | Self-healing epoxy nanocomposites via reversible hydrogen bonding | |
| CN107057283B (en) | Carbon fiber reinforced resin matrix composite material and preparation method thereof | |
| 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 | |
| CN106832774B (en) | A kind of 3D graphene/epoxy resin composite material and its preparation method and application of aramid fiber enhancing | |
| CN109111694A (en) | The production and stress measuring method of glass fiber reinforced epoxy resin plate | |
| Huang et al. | Cryogenic properties of SiO2/epoxy nanocomposites | |
| CN109265909A (en) | The board making and stress determination method of basalt fibre enhancing phenolic resin | |
| CN109206840A (en) | The production and stress measuring method of glass fibre-reinforced phenolic resin plate | |
| CN105968717A (en) | Preparation of carbon fiber/graphene/carbon nanotube/epoxy resin prepreg and carbon fiber composite material | |
| CN109111695A (en) | The production method of graphene and aramid fiber mixing reinforced epoxy plate | |
| CN109161157A (en) | Para-aramid fiber reinforced epoxy board making and stress measuring method | |
| CN109228076A (en) | The plate forming and stress determination method of carbon fiber reinforced phenol formaldehyde resin | |
| WO2011064707A3 (en) | Fiber reinforced polymeric composites with tailorable electrical resistivities and process for preparing the same | |
| CN107815122B (en) | High-strength tear-resistant silicone rubber foam material and preparation method thereof | |
| CN106009677A (en) | Nanometer conductive rubber sensing unit and method for preparing same | |
| CN106007508B (en) | A kind of graphene fiber enhancing inorganic polymer grinding disc substrate and preparation method thereof | |
| CN107418213A (en) | A kind of method that the highly conductive flexible composite of low sizing content is prepared based on swelling osmosis | |
| CN110408083A (en) | It is a kind of using bacteria cellulose as high-heat-conductive composite material of matrix and preparation method thereof | |
| CN104231624A (en) | Modified cyanate ester resin heat-conducting composite material and preparation method thereof | |
| CN109206905A (en) | A kind of graphene bismaleimide resin composite material and preparation method thereof | |
| CN111574906A (en) | High-strength modified epoxy resin insulating and heat-conducting composite coating and preparation method thereof | |
| CN108997708A (en) | Para-aramid fiber enhances phenolic resin board making and stress measuring method | |
| CN103923462A (en) | Preparation method of modified PBO [poly(p-phenylene benzobisoxazole)] fiber prepreg |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190108 |