CN108318302A - A kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament - Google Patents
A kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament Download PDFInfo
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- CN108318302A CN108318302A CN201810047065.XA CN201810047065A CN108318302A CN 108318302 A CN108318302 A CN 108318302A CN 201810047065 A CN201810047065 A CN 201810047065A CN 108318302 A CN108318302 A CN 108318302A
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- multifilament
- carbon fiber
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- glue
- test
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 64
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 64
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000010426 asphalt Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000012360 testing method Methods 0.000 title claims abstract description 33
- 239000003292 glue Substances 0.000 claims abstract description 60
- 238000005470 impregnation Methods 0.000 claims abstract description 24
- 238000005452 bending Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000004804 winding Methods 0.000 claims abstract description 9
- 238000009736 wetting Methods 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000003822 epoxy resin Substances 0.000 claims description 14
- 229920000647 polyepoxide Polymers 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 13
- 238000007711 solidification Methods 0.000 claims description 11
- 230000008023 solidification Effects 0.000 claims description 11
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- MUTGBJKUEZFXGO-UHFFFAOYSA-N hexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21 MUTGBJKUEZFXGO-UHFFFAOYSA-N 0.000 claims description 6
- -1 phthalate anhydride Chemical class 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 5
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 4
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 4
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 claims description 3
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 41
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 2
- 230000005484 gravity Effects 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 description 15
- 239000011347 resin Substances 0.000 description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- 239000000853 adhesive Substances 0.000 description 13
- 230000001070 adhesive effect Effects 0.000 description 13
- 239000007788 liquid Substances 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 12
- 230000008595 infiltration Effects 0.000 description 6
- 238000001764 infiltration Methods 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 3
- 239000011302 mesophase pitch Substances 0.000 description 3
- 239000011295 pitch Substances 0.000 description 3
- 206010044565 Tremor Diseases 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 1
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy
Abstract
The present invention relates to a kind of method for making sample of asphalt base carbon fiber tensile property of multi-filament test, belong to material properties test technical field.The method includes：Apply tension carbon fiber multifilament is wound on frame, fixed material is used in combination to fix the bending part of the multifilament on said frame；So that the frame for winding multifilament is placed vertically along multifilament extending direction, glue is added dropwise from the frame upper end, so that the glue of dropwise addition is flowed from the multifilament upper end to lower end along the multifilament, until multifilament described in complete wetting, obtains impregnation multifilament frame；The impregnation multifilament frame is cured, multifilament is cut, stickup papery reinforced sheet obtains tensile sample.The invention avoids the damages of fiber in operating process, improve sample preparation efficiency, also avoiding glue surface tension and glue and multifilament its own gravity leads to fibre single thread brittle failure problem, ensure fiber multifilament maximum Developed fiber strength, the accuracy for greatly improving tensile strength test value reduces tensile strength coefficient of dispersion.
Description
Technical field
The invention belongs to material properties test technical fields, and in particular to one kind being used for asphalt base carbon fiber multifilament draftability
The method for making sample that can be tested.
Background technology
Mesophase pitch-based carbon fibers are a kind of high-performance carbon fibres, due to its molecular structure it is height-oriented and in modulus and
Heat conductivility etc. shows superiority, mesophase pitch-based carbon fibers generally with raw material selected from coal tar pitch and petroleum asphalt or other
Pitch is raw material, is made by optically anisotropic mesophase pitch.1975, U.S. combinating carbide company disclosed in use
Between asphalt phase manufacture high modulus carbon fiber " Thornel P " method, and put into commodity production soon.From this, asphaltic base carbon fiber
Dimension enters the fast traffic lane of development, becomes the second largest raw material route production carbon fiber after polyacrylonitrile-based carbon fibre.Currently,
The unit of foreign study asphalt base carbon fiber is more, but the unit that can manufacture high-performance carbon fibre only has U.S.'s cyanogen special public
Department, Mitsubishi chemistry and Japanese graphite fibre company.And the unit of China's research high-performance asphalt base carbon fiber is less, experiment
Room fiber key performance reaches external peer-level, but so far not yet can batch steady production.
Relative to polyacrylonitrile-based carbon fibre, high heat conduction asphalt base carbon fiber have higher thermal conductivity and stretch modulus,
The composite material of the lower negative coefficient of thermal expansion of room temperature, enhancing is handed in high heat conduction structural panel, high rigidity structural member, temperature
Changing environment zero thermal expansion coefficient component, high heat conduction resistance to oxidation heat of ablation structural member etc. have irreplaceable role, are satellites
Irreplaceable core material on agent structure, functional structure, safeguard structure and supplementary structure.
Standard GB/T/T3362-2005 carbon fiber tensile property of multi-filament test methods treat the manual impregnation side of carbon determination fiber
Method has more specific regulation and description, frame winding-craft impregnation-dry solidification.Specifically, one root long of first clip is multiple
Silk, applies certain tension and multifilament is wound on frame, so that multifilament is laterally stretched and tighten, frame both ends are held by frame with hand
Level immerses round trip or for several times in glue, or is reintroduced after impregnating a few minutes；The multifilament of dipped glue shrugs off extra glue
Liquid dries at room temperature；The frame of fixed multifilament is placed in forced air drying and is cured, multifilament, adhesive paper are then cut
Matter reinforced sheet obtains tensile sample.Due to high (such as U.S. Qing Te companies asphalt base carbon fiber of asphalt base carbon fiber stretch modulus
The stretch modulus of K1100 reaches 965GPa, is the 95% of theoretical stretch modulus 1020GPa), brittleness is very big, using GB/T3362-
Manual impregnation in 2005 standards, which trembles glue easily, makes the pitch fibers monofilament brittle failure of part ultra high modulus, significantly reduces mechanical property
Energy.
Invention content
The purpose of the present invention is to provide a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament, should
Method for making sample can effectively solve tensile strength caused by fibre damage during asphalt base carbon fiber multifilament tensile sample and test
It is worth relatively low, the discrete technical problems such as bigger than normal, the tensile bars appearance of preparation is smooth, and extension test result is stablized, and is suitable for a variety of
Asphalt base carbon fiber.The impregnation method for making sample has important in road asphalt base carbon fibre and its composite material development and production
Popularizing application prospect.
What the above-mentioned purpose of the present invention was mainly achieved by following technical solution：
A kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament, which is characterized in that including following step
Suddenly：
Carbon fiber multifilament is wound on frame by step 1, application tension, is used in combination fixed material by the bending part of the multifilament
Position is fixed on said frame；
Step 2 makes the frame for winding multifilament be placed vertically along multifilament extending direction, and glue is added dropwise from the frame upper end
Liquid makes the glue of dropwise addition be flowed from the multifilament upper end to lower end along the multifilament, until multifilament described in complete wetting, obtains
Impregnation multifilament frame make the glue of dropwise addition from the bending part of the multifilament upper end along the multifilament to the curved of corresponding lower end
Folding part bit flow, until multifilament described in complete wetting, obtains impregnation multifilament frame；
Step 3, the impregnation multifilament frame is cured, cut multifilament, paste papery reinforced sheet obtain tensile sample.
In an alternative embodiment, the carbon fiber multifilament be stretch modulus not less than 600GPa, strand specification be 0.5~
The asphalt base carbon fiber of 6K.
In an alternative embodiment, the tension is 1~5N.
In an alternative embodiment, glue is added dropwise with the drop glue rate of 1~5mL/min in step 2.
It is 0.1~2 minute/section that the glue time is dripped in an alternative embodiment, in step 2.
In an alternative embodiment, the glue includes the component of following mass fraction：100 parts of epoxy resin, curing agent
60~120 parts, 0.5~3 part of accelerating agent, 60~120 parts of solvent.
In an alternative embodiment, the epoxy resin is 4,4 '-diaminodiphenylmethane, triglycidyl group to amino
At least one of phenol or 1,2- 7-oxa-bicyclo[4.1.0 4,5- dicarboxylic acid diglycidyl esters.
In an alternative embodiment, the curing agent is hexahydrophthalic acid anhydride, methyl hexahydrophthalic acid anhydride or methyl
At least one of tetrahydrochysene phthalate anhydride.
In an alternative embodiment, the accelerating agent is N, N dimethyl aniline, diethylaminopropylamine or 2- ethyl -4- first
At least one of base imidazoles；The solvent is at least one of acetone, toluene or dimethylbenzene.
In an alternative embodiment, solidification temperature is 100~200 DEG C in step 3, hardening time is 2~6 hours.
The present invention has the advantages that compared with prior art：
(1) present invention fixes multifilament and frame by using fixed material, avoids multifilament in winding and immersing glue process
Fracture so that the glue of dropwise addition is flowed from the multifilament upper end edge multifilament to lower end by the way that glue is added dropwise above frame and realize
Infiltration to multifilament takes frame, trembles the manual operationss such as glue or rubber, so as to avoid behaviour when avoiding horizontal impregnation in the prior art
The damage of fiber during work, improves sample preparation efficiency；Meanwhile this method also avoids glue surface tension and glue and multifilament
Its own gravity, to fibre single thread brittle failure problem caused by multifilament applied force, ensures fiber multifilament most from perpendicular to multifilament extending direction
Big Developed fiber strength greatly improves the accuracy of tensile strength test value, reduces tensile strength coefficient of dispersion；Further
Ground, compared with traditional dipping method, the present invention is greatly reduced with glue amount, has saved testing cost；
(2) present invention reduces fiber and impregnation resin system surface by solvent adjustment impregnation resin system viscosity
Power slowly drips glue, fibre single thread fracture is reduced while ensureing fully infiltration, while using polyfunctional epoxy resin and acid
Anhydride curing agent increases asphalt base carbon fiber and resin boundary surface binding force as impregnation system, can be avoided after sample preparation due to
The problem of caused by fiber surface inertia with resin unsticking, to ensure giving full play to for fibre strength performance, be conducive to multifilament
Tensile property is tested.
(3) present invention prepares asphalt-based carbon fiber mechanical stretch sample using epoxy method, and impregnation epoxy resin is greatly reduced
Dosage reduces carbon fiber mechanical property sample preparation testing cost.The tensile sample smooth in appearance prepared simultaneously is uniform, can be used for more
The tensile property sample preparation of kind asphalt base carbon fiber.Extension test result energy objective evaluation fibrous mechanical property, centrifugal pump are smaller.
Description of the drawings
Fig. 1 is method for making sample schematic diagram provided in an embodiment of the present invention；
Specific implementation mode
Illustrate below by specific embodiment, but the present invention is not limited to following embodiment.
An embodiment of the present invention provides a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament, including
Following steps：
Carbon fiber multifilament is wound on frame by step 1, application tension, is used in combination fixed material by the bending part of the multifilament
Position is fixed on said frame；
Specifically, in the embodiment of the present invention, carbon fiber multifilament preferred tensile modulus is not less than 600GPa, strand specification
The asphalt base carbon fiber of 0.5~6K；
The fixed material can either provide cohesive force for High temperature-resistanadhesive adhesive tape, adhesive tape, glued membrane etc. makes multifilament bending part
Position cements with frame and is resistant to the material of solidification high temperature；As shown in Figure 1, in one embodiment, passing through High temperature-resistanadhesive adhesive tape 5
The bending part outer surface of multifilament 4 is coated on to be fixed with frame 3；
Specifically, the preferred 1N~5N of the tension both can guarantee that smoothly winding was tightened in multifilament when tension is 1~5N
It on frame, and is avoided that fibre damage caused by overtension, further ensures test accuracy.
Step 2 makes the frame for winding multifilament be placed vertically along multifilament extending direction, and glue is added dropwise from the frame upper end
Liquid, make the glue of dropwise addition from the multifilament upper end along the multifilament to lower end flowing multifilament described in the complete wetting, obtain
Impregnation multifilament frame；
Specifically, referring to Fig. 1, in the embodiment of the present invention, to the damage of fibre bundle caused by avoid overturning adjustment frame
Evil places frame 3 vertically when winding, and vertically winds multifilament 4 from top to bottom or from bottom to top, twines on the frame 3
When around multifilament 4, multifilament 4 forms multistage between descending two frame sides on the frame 3；After winding directly by dropper 1 it is equal be added dropwise device from
Infiltration glue 2 is added dropwise in 3 top of frame paragraph by paragraph；It is preferred that glue is added dropwise with the drop glue rate of 1~5mL/min, both ensured glue to multiple
The abundant infiltration of each fibre bundle in silk further reduces the damage to fibre bundle such as glue tension and dead weight；When dripping glue
Between preferably 0.1~2 minute/section, not only ensured abundant infiltration of the glue to each fibre bundle in multifilament, but avoid impregnation tow suction
Tide influences glue resin property；
In the embodiment of the present invention, the glue includes the component of following mass fraction：100 parts of epoxy resin, curing agent 60
~120 parts, 0.5~3 part of accelerating agent, 60~120 parts of solvent；The epoxy resin preferably 4,4 '-diaminodiphenylmethane, three contractings
At least one of water glyceryl para-aminophenol or 1,2- 7-oxa-bicyclo[4.1.0 4,5- dicarboxylic acid diglycidyl esters；The solidification
At least one of the preferred hexahydrophthalic acid anhydride of agent, methyl hexahydrophthalic acid anhydride or methyl tetrahydrochysene phthalate anhydride；It is described
The preferred N of accelerating agent, at least one of N dimethyl aniline, diethylaminopropylamine or 2-ethyl-4-methylimidazole；The solvent
It is preferred that at least one of acetone, toluene or dimethylbenzene；The present invention reduces fibre by solvent adjustment impregnation resin system viscosity
Dimension and impregnation resin system surface tension, slowly drip glue, and fibre single thread fracture is reduced while ensureing fully infiltration, is adopted simultaneously
It uses polyfunctional epoxy resin and acid anhydride type curing agent as impregnation system, increases asphalt base carbon fiber and combined with resin boundary surface
Power, can be avoided the problem that after sample preparation due to caused by fiber surface inertia with resin unsticking, to ensure fibre strength performance
Give full play to, be conducive to tensile property of multi-filament test.
Step 3, the impregnation multifilament frame is cured, cut multifilament, paste papery reinforced sheet obtain tensile sample.
Specifically, solidification temperature is 100~200 DEG C in the present embodiment, hardening time is 2~6 hours.
It is below several specific embodiments of the present invention, raw materials used and reagent is commercial product in each embodiment.
Embodiment 1
Wind the XN-90 asphalt base carbon fiber multifilament of 6K specifications on iron frame using 5N tension, blend compounds band is by institute
The bending part for stating multifilament is fixed on said frame；100 mass parts 1,2- 7-oxa-bicyclo[4.1.0s are sequentially added in 500mL measuring cups
Then 4,5- dicarboxylic acid diglycidyl esters, 60 mass parts hexahydrophthalic acid anhydrides and 0.5 mass parts N, N dimethyl aniline add
Enter 120 parts of acetone and be sufficiently stirred 5 minutes to obtain resin adhesive liquid；Epoxy resin adhesive liquid is sucked from frame upper end edge fiber using dropper
Glue is added dropwise in multifilament bundled, and drop glue rate is 5mL/min, and the drop glue time is 0.1 minute/section；Impregnation multifilament frame is placed in air blast
Baking oven for drying solidification, curing process condition are (80 DEG C/1h)+(140 DEG C/2h)+(200 DEG C/3h), cut multifilament after cooling, glue
Paster matter reinforced sheet obtains tensile sample.Asphalt base carbon fiber tensile property of multi-filament is shown in Table 1.
Embodiment 2
Wind the P-120 asphalt base carbon fiber multifilament of 2K specifications on iron frame using 1N tension, blend compounds band is by institute
The bending part for stating multifilament is fixed on said frame；100 4,4 '-diamino of mass parts two are sequentially added in 500mL measuring cups
Then phenylmethane, 100 mass parts methyl hexahydrophthalic acid anhydrides and 1.5 mass parts diethylaminopropylamines are added 100 parts of toluene and fill
Stirring is divided to obtain resin adhesive liquid in 5 minutes；It is slowly dripped from frame upper end edge fiber multifilament bundled using dropper sucking epoxy resin adhesive liquid
It is 4mL/min to add glue, drop glue rate, and the drop glue time is 1 minute/section；The merging convection oven drying of impregnation multifilament frame is solid
Change, curing process condition is (140 DEG C/1h)+(200 DEG C/1h), and multifilament is cut after cooling, pastes papery reinforced sheet and is stretched
Sample.Asphalt base carbon fiber tensile property of multi-filament is shown in Table 1.
Embodiment 3
The K13D asphalt base carbon fiber multifilament of 2K specifications is wound on iron frame using 1N tension, blend compounds band will be described
The bending part of multifilament is fixed on said frame；100 mass parts 4,4 '-diamino hexichol are sequentially added in 500mL measuring cups
Then 60 parts of dimethylbenzene are added in methane, 80 mass parts methyl tetrahydrochysene phthalate anhydrides and 3 mass parts 2-ethyl-4-methylimidazoles
It is sufficiently stirred 5 minutes and obtains resin adhesive liquid；It is slow from frame upper end edge fiber multifilament bundled using dropper sucking epoxy resin adhesive liquid
Glue is added dropwise, drop glue rate is 3mL/min, and the drop glue time is 2 minutes/section；Multifilament frame after drop glue is placed in convection oven
Dry solidification, curing process condition are (80 DEG C/1h)+(140 DEG C/1h)+(200 DEG C/2h), and multifilament, adhesive paper are cut after cooling
Matter reinforced sheet obtains tensile sample.Asphalt base carbon fiber tensile property of multi-filament is shown in Table 1.
Embodiment 4
Wind the K1100 asphalt base carbon fiber multifilament of 2K specifications on iron frame using 1N tension, blend compounds band is by institute
The bending part for stating multifilament is fixed on said frame, and 100 mass parts triglycidyl groups pair are sequentially added in 500mL measuring cups
Then amino-phenol, 80 mass parts hexahydrophthalic acid anhydrides and 2 mass parts 2-ethyl-4-methylimidazoles are added 100 parts of acetone and fill
Stirring is divided to obtain resin adhesive liquid in 5 minutes；It is slowly dripped from frame upper end edge fiber multifilament bundled using dropper sucking epoxy resin adhesive liquid
It is 2mL/min to add glue, drop glue rate, and the drop glue time is 0.1 minute/section；Multifilament frame after drop glue is placed in convection oven
Dry solidification, curing process condition are (80 DEG C/2h)+(140 DEG C/2h)+(200 DEG C/2h), and multifilament, adhesive paper are cut after cooling
Matter reinforced sheet obtains tensile sample.Asphalt base carbon fiber tensile property of multi-filament is shown in Table 1.
Embodiment 5
Wind the road asphalt base carbon fibre multifilament of 0.5K specifications on iron frame using 1N tension, blend compounds band is by institute
The bending part for stating multifilament is fixed on said frame；100 mass parts 1,2- 7-oxa-bicyclo[4.1.0s are sequentially added in 500mL measuring cups
Then 4,5- dicarboxylic acid diglycidyl esters, 120 mass parts hexahydrophthalic acid anhydrides and 0.5 mass parts N, N dimethyl aniline add
Enter 120 parts of acetone and be sufficiently stirred 5 minutes to obtain resin adhesive liquid；Epoxy resin adhesive liquid is sucked from frame upper end edge fiber using dropper
Glue is added dropwise in multifilament bundled, and drop glue rate is 1mL/min, and the drop glue time is 0.1 minute/section；After impregnation multifilament frame is dripped glue
Multifilament frame is placed in convection oven dry solidification, and curing process condition is (80 DEG C/1h)+(140 DEG C/2h)+(200 DEG C/3h), cold
But multifilament is cut afterwards, is pasted papery reinforced sheet and is obtained tensile sample.Asphalt base carbon fiber tensile property of multi-filament is shown in Table 1 institute.
Comparative example 1
Japanese Graphite Company XN-90 asphalt base carbon fiber tensile property of multi-filament manufacture report value is shown in Table 1.
Comparative example 2
U.S.'s Qing Te companies P-120 carbon fiber tensile property of multi-filament manufacture report value is shown in Table 1.
Comparative example 3
Mitsubishi Corporation of Japan K13D asphalt base carbon fiber tensile property of multi-filament manufacture report value is shown in Table 1.
Comparative example 4
U.S.'s Qing Te companies K1100 asphalt base carbon fiber tensile property of multi-filament manufacture report value is shown in Table 1.
Comparative example 5
Certain road asphalt base carbon fibre tensile property of multi-filament producer laboratory value is shown in Table 1.
Comparative example 6
The XN-90 asphalt base carbon fiber multifilament for winding 6K specifications on iron frame using 5N tension, using GB/T3362-
2005 method sample preparations, obtain tensile sample.
Comparative example 7
Method for making sample is identical as comparative example 6, unique the difference is that the resin system and solidification work for using embodiment 1 to provide
Skill.
Examples 1 to 5 and comparative example 1~7 are tested for the property according to test method as defined in GB/T3362-2005,
Test result is referring to table 1：
1 asphalt base carbon fiber tensile property of multi-filament of table
aStretch modulus is tested using contact extensometer
bElongation at break=tensile strength/stretch modulus
It can be seen that from the comparison of embodiment 1 and comparative example 1,6,7 and asphaltic base carbon fiber prepared using method for making sample of the present invention
The tensile strength, stretch modulus and elongation at break for tieing up XN-90 multifilament samples are suitable with factory-said value, the test knot of embodiment 1
Fruit is substantially better than comparative example 6 and 7.It can be seen that from the comparison of embodiment 2 and comparative example 2 and prepared using method for making sample of the present invention
The tensile strength test value of asphalt base carbon fiber P-120 multifilament samples slightly above manufacture reported values, stretch modulus and extension at break
Rate is suitable with factory-said value.It can be seen that from the comparison of embodiment 3 and comparative example 3 and asphaltic base prepared using method for making sample of the present invention
Tensile strength, stretch modulus and the elongation at break test value of carbon fiber K13D multifilament samples are suitable with manufacture reported values.From
The comparison of embodiment 4 and comparative example 4 can be seen for preparing the examination of asphalt base carbon fiber K1100 multifilament using method for making sample of the present invention
The tensile strength of sample slightly above manufacture reported values, stretch modulus and elongation at break are suitable with factory-said value.From embodiment 5 and comparison
The comparison of example 5 is as can be seen that the tensile property for preparing road asphalt base carbon fibre multifilament sample using method for making sample of the present invention is bright
The aobvious test value that GB/T 2262-2005 method for making sample is used higher than producer laboratory, can more objective reaction domestic carbon fibre mechanics
Performance can be used for instructing road asphalt base carbon fibre batch to develop.In addition, the external pitch prepared using method for making sample of the present invention
All tensile properties test centrifugal pump of base carbon fibre multifilament sample is respectively less than 6%, has absolutely proved the effect of the present invention.
The above, best specific implementation mode only of the invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.
The content that description in the present invention is not described in detail belongs to the known technology of professional and technical personnel in the field.
Claims (10)
1. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament, which is characterized in that include the following steps：
Carbon fiber multifilament is wound on frame by step 1, application tension, and fixed material is used in combination to consolidate the bending part of the multifilament
Determine on said frame；
Step 2 makes the frame for winding multifilament be placed vertically along multifilament extending direction, and glue is added dropwise from the frame upper end, makes
The glue of dropwise addition is flowed along the multifilament to lower end from the multifilament upper end, until multifilament described in complete wetting, obtains impregnation
Multifilament frame；
Step 3, the impregnation multifilament frame is cured, cut multifilament, paste papery reinforced sheet obtain tensile sample.
2. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament according to claim 1, special
Sign is：The carbon fiber multifilament is stretch modulus not less than the asphalt base carbon fiber that 600GPa, strand specification are 0.5~6K.
3. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament according to claim 1, special
Sign is：The tension is 1~5N.
4. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament according to claim 1, special
Sign is：Glue is added dropwise with the drop glue rate of 1~5mL/min in step 2.
5. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament according to claim 4, special
Sign is：It is 0.1~2 minute/section that the glue time is dripped in step 2.
6. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament according to claim 1, special
Sign is：The glue includes the component of following mass fraction：
100 parts of epoxy resin, 60~120 parts of curing agent, 0.5~3 part of accelerating agent, 60~120 parts of solvent.
7. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament according to claim 6, special
Sign is：The epoxy resin is 4,4 '-diaminodiphenylmethane, triglycidyl group para-aminophenol or 1,2- epoxy hexamethylenes
At least one of alkane 4,5- dicarboxylic acid diglycidyl esters.
8. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament according to claim 6, special
Sign is：The curing agent is in hexahydrophthalic acid anhydride, methyl hexahydrophthalic acid anhydride or methyl tetrahydrochysene phthalate anhydride
It is at least one.
9. a kind of method for making sample for the test of asphalt base carbon fiber tensile property of multi-filament according to claim 6, special
Sign is：The accelerating agent is N, at least one of N dimethyl aniline, diethylaminopropylamine or 2-ethyl-4-methylimidazole；
The solvent is at least one of acetone, toluene or dimethylbenzene.
10. a kind of method for making sample of asphalt base carbon fiber tensile property of multi-filament test according to claim 1, feature exist
In：Solidification temperature is 100~200 DEG C in step 3, hardening time is 2~6 hours.
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| CN112444445A (en) * | 2020-10-20 | 2021-03-05 | 航天材料及工艺研究所 | Method for preparing silicon carbide fiber bundle mechanical sample by using solvent-free glue solution |
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