CN107217491A - The method that polyaniline-coated is modified chopped carbon fiber - Google Patents
The method that polyaniline-coated is modified chopped carbon fiber Download PDFInfo
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- CN107217491A CN107217491A CN201710605310.XA CN201710605310A CN107217491A CN 107217491 A CN107217491 A CN 107217491A CN 201710605310 A CN201710605310 A CN 201710605310A CN 107217491 A CN107217491 A CN 107217491A
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- carbon fiber
- chopped carbon
- ammonium persulfate
- polyaniline
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 47
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 17
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 24
- 239000000725 suspension Substances 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000004048 modification Effects 0.000 claims abstract description 11
- 238000012986 modification Methods 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 10
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 10
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- MMCPOSDMTGQNKG-UHFFFAOYSA-N anilinium chloride Chemical compound Cl.NC1=CC=CC=C1 MMCPOSDMTGQNKG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000011010 flushing procedure Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 20
- 230000003647 oxidation Effects 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 4
- MMCPOSDMTGQNKG-UJZMCJRSSA-N aniline;hydrochloride Chemical compound Cl.N[14C]1=[14CH][14CH]=[14CH][14CH]=[14CH]1 MMCPOSDMTGQNKG-UJZMCJRSSA-N 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 16
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000002604 ultrasonography Methods 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 238000006056 electrooxidation reaction Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/61—Polyamines polyimines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- 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
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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
- C08K9/02—Ingredients treated with inorganic substances
-
- 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
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention belongs to the modification field of chopped carbon fiber, a kind of method that polyaniline-coated is modified chopped carbon fiber is disclosed.（1）, chopped carbon fiber is soaked in the ammonium persulfate aqueous solution that concentration is 30 ~ 50g/L, ultrasonically treated 1 ~ 4h, the chopped carbon fiber suspension pre-oxidized；In the step, 8 ~ 15g of chopped carbon fiber is added in every 1L ammonium persulfate aqueous solutions；（2）, under stirring state, first add aniline hydrochloride into above-mentioned suspension, add ammonium persulfate and ferrous sulfate, then temperature control reacts 10 ~ 16h at 5 ~ 10 DEG C；In the step, 0.1 ~ 0.5moL of aniline hydrochloride, the moL of ammonium persulfate 0.1 ~ 0.5,0.002 ~ 0.01moL of ferrous sulfate are separately added into every 1L suspension；（3）, hydrochloric acid with 0.01 ~ 0.05mol/L and acetone alternating washed product, be 7 with distilled water flushing to pH, filtering drying obtains the chopped carbon fiber of polyaniline-coated modification.Gained modified carbon fiber of the invention has high dispersion.
Description
Technical field
The invention belongs to the modification field of chopped carbon fiber, and in particular to a kind of polyaniline-coated is modified chopped carbon fiber
Method.
Background technology
Chopped strand and its enhancing composite there is high temperature resistant, corrosion-resistant, light weight and high mechanical strength and
Increasingly it is widely applied.Although it has excellent combination property, due to the smooth inactive functional group in its surface, table
Face can it is low, the shortcomings of be difficult to infiltration with apolar substance, limit that chopped strand is high performance to be given full play to, particularly in enhancing
In terms of composite, it is poor with polymeric matrix adhesive property, causes the enhanced composite of chopped strand in use
Easily occur degumming and resin matrix problems of crack.Therefore, explore and find a kind of method of modifying of chopped strand, strengthen its reaction
Activity, is one of current direction for being badly in need of research, and the chopped strand being modified is to the mechanical property of later stage fibre reinforced composites
It can be lifted and be significant.
The modification of current fiber refers mainly to the processing to fiber surface, such as removes surface impurity；Increase the ditch of fiber surface
Groove or microcellular structure, and then increase surface energy；Active function groups are introduced, increase its reactivity.More fiber is used at present
Processing method mainly includes：The methods such as oxidation processes, coating processing, ray, laser, corona treatment.Oxidation processes are main
Including using gaseous oxidation（Air, carbon dioxide, ozone, vapor, oxygen）, liquid phase oxidation（Nitric acid, potassium permanganate, secondary chlorine
Sour sodium, hydrogen peroxide, ammonium persulfate）And electrochemical oxidation improves the state of fiber surface, increase the quantity of oxygen-containing functional group, improve
Hydrophily, is conducive to the raising of dispersive property and the bonding with resin matrix.The advantage of vapour phase oxidation process is required when being oxidation to be set
Standby simple, the reaction time is short, but the shortcoming of this method is extension with oxidation treatment time and the rise of temperature, fibre strength
It can lose, simultaneously as oxidation reaction is fiercer, reaction condition is difficult to control to, reaction temperature cannot be controlled accurately.Phase
Than gaseous oxidation, liquid phase oxidation milder will not make fiber surface form the phenomenon such as excessive pit and cracking, but exist
Oxidizing liquid be difficult from fiber surface thoroughly remove the problems such as.Electrochemical oxidation reactions condition relaxes, and processing time is short, and
Can be by controlling the process conditions such as electrolysis temperature, current density, electrolyte mass fraction to realize the accurate control to degree of oxidation
System, makes fiber oxidation evenly；Oxidized rear oxygen-containing functional group and nitrogen-containing functional group quantity substantially increase, and improve fiber and water
Infiltration, it is believed that be current most valuable method, but this process and uneconomical and be difficult suitable for large-scale work
Industry metaplasia is produced, and oxidation processes not only result in environmental pollution, can also damage the mechanical property of fiber itself.In addition, at surface
Reason also includes the method using face coat, such as coupling agent coating and polymer coating, mainly by electrochemical deposition with changing
The approach such as plating, vapour deposition, surface electropolymerization and sol-gel process are learned to realize.But due to the functional group on chopped strand surface
Quantity and species are less, only unsatisfactory with the effect of coupling agent treatment, not only to control the thickness of coating, in addition it is also necessary to by oxygen
Change the peptizaiton of processing and later stage dispersant, process is relative complex.
The content of the invention
It is an object of the invention to provide a kind of method that polyaniline-coated is modified chopped carbon fiber, so as to overcome existing skill
Chopped carbon fiber bad dispersibility and reactivity is low, the low defect weak with resin matrix bond strength that be causing of caking property in art.
To achieve the above object, the technical scheme that the present invention takes is as follows：
The method that polyaniline-coated is modified chopped carbon fiber, comprises the following steps：
（1）, chopped carbon fiber is soaked in the ammonium persulfate aqueous solution that concentration is 30 ~ 50g/L, ultrasonically treated 1 ~ 4h is obtained
The chopped carbon fiber suspension of pre-oxidation；In the step, 8 ~ 15g of chopped carbon fiber is added in every 1L ammonium persulfate aqueous solutions；
（2）, under stirring state, first add aniline hydrochloride into above-mentioned suspension, add ammonium persulfate and ferrous sulfate, then
Temperature control reacts 10 ~ 16h at 5 ~ 10 DEG C；In the step, the moL of aniline hydrochloride 0.1 ~ 0.5, over cure are separately added into every 1L suspension
The sour moL of ammonium 0.1 ~ 0.5,0.002 ~ 0.01moL of ferrous sulfate；
（3）, hydrochloric acid with 0.01 ~ 0.05mol/L and acetone alternating washed product, be 7 with distilled water flushing to pH, filtering is dried
It is dry, obtain the chopped carbon fiber of polyaniline-coated modification.
Preferably, the length of the chopped carbon fiber is 2 ~ 25mm.
Preferably, the ultrasonic temperature is 40 ~ 80 DEG C, and ultrasonic power is 100 ~ 300W.
The present invention provides a kind of method of modifying of the chopped carbon fiber of high dispersion, and the present invention is using ammonium persulfate super
Pre-oxidation treatment first is carried out to carbon fiber under sound effect, the carbon fiber surface of pre-oxidation treatment is coated into polyaniline afterwards, is realized
The raising of modification and dispersiveness to fiber.Under ammonium persulfate and supersonic synergetic effect, ultrasound can promote ammonium persulfate
Chemical oxidation effect, and " cavitation effect " of ultrasonic wave causes the interface of carbon fiber and ammonium persulfate solution to produce high speed
Microjet and shock wave, make carbon fiber surface be etched and peel off, while can contain-the OH of fiber surface, C-O and C-O-C etc.
Oxygen functional group content increase, surface polarity enhancing provides advantage for next step fiber surface cladding polyaniline, increased
The contact area of cladding；And coat polyaniline by the use of ammonium persulfate and ferrous sulfate as initiator, using a small amount of iron from
Son makes ammonium persulfate significantly activate, and accelerates it to decompose and produces very strong potentiometric titrations, thus accelerated oxidation aniline for sun from
Sub- free radical, with the generation of more dynamics model, makes the conversion ratio of aniline raise significantly, substantially reduces the cycle of cladding.
In addition, ammonium persulfate has lacked washing and the step dried, has simplified modified work simultaneously as oxidant and initiator after oxidation
Skill flow.Carbon fiber passes through polyaniline-coated modification, scattered of great advantage to the later stage, while improving modified carbon fiber
Wetability and reactivity between matrix resin, make to combine more firmly between the two, are conducive to carbon fibre reinforced composite mechanics
The lifting of performance.
Embodiment
Explanation, but the protection model of the present invention are further explained to technical scheme with reference to specific embodiment
Enclose and be not limited thereto.
Embodiment 1
The method that polyaniline-coated is modified chopped carbon fiber, comprises the following steps：
（1）, by 10g length be 10mm chopped carbon fiber be soaked in the ammonium persulfate aqueous solution that 1L concentration is 30g/L, be placed in
Ultrasound 2h in ultrasonic cleaning equipment, ultrasonic power is 300W, and temperature is 70 DEG C, and the chopped carbon fiber pre-oxidized suspends
Liquid；
（2）, under stirring state, per the above-mentioned suspension of 1L in first add 0.2 moL aniline hydrochlorides, add 0.2moL ammonium persulfates
With 0.002moL ferrous sulfate, then temperature control is in 5 DEG C of reaction 16h；
（3）, with 0.01mol/L hydrochloric acid and acetone replace washed product, be 7 with distilled water flushing to pH, filtering drying is gathered
The chopped carbon fiber of aniline coating modification.
Embodiment 2
The method that polyaniline-coated is modified chopped carbon fiber, comprises the following steps：
（1）, by 8g length be 5mm chopped carbon fiber be soaked in the ammonium persulfate aqueous solution that 1L concentration is 40g/L, be placed in super
Ultrasound 3h in sound wave cleaning device, ultrasonic power is 200W, and temperature is 60 DEG C, the chopped carbon fiber suspension pre-oxidized；
（2）, under agitation, per 1L above-mentioned suspension in first add 0.15 moL aniline hydrochlorides, add 0.15moL over cures
Sour ammonium and 0.005moL ferrous sulfate, then temperature control is in 7 DEG C of reaction 12h；
（3）, with 0.03mol/L hydrochloric acid and acetone replace washed product, be 7 with distilled water flushing to pH, filtering drying is gathered
The chopped carbon fiber of aniline coating modification.
Embodiment 3
The method that polyaniline-coated is modified chopped carbon fiber, comprises the following steps：
（1）, by 12g length be 15mm chopped carbon fiber be soaked in the ammonium persulfate aqueous solution that 1L concentration is 50g/L, be placed in
Ultrasound 4h in ultrasonic cleaning equipment, ultrasonic power is 100W, and temperature is 40 DEG C, and the chopped carbon fiber pre-oxidized suspends
Liquid；
（2）, under agitation, per 1L above-mentioned suspension in first add 0.3 moL aniline hydrochlorides, add 0.3moL persulfuric acid
Ammonium and 0.0075moL ferrous sulfate, then temperature control is in 10 DEG C of reaction 10h；
（3）, with 0.05mol/L hydrochloric acid and acetone replace washed product, be 7 with distilled water flushing to pH, filtering drying is gathered
The chopped carbon fiber of aniline coating modification.
Reference examples 1
It is with the difference of embodiment 1, step（1）Ammonium persulfate is only added, without ultrasound, i.e., process is：By 10g length
2h in the ammonium persulfate aqueous solution that 1L concentration is 30g/L is soaked in for 10mm chopped carbon fiber, the chopped carbon pre-oxidized
Fibrous suspension.
Reference examples 2
It is with the difference of embodiment 1：Step（1）In, ultrasonic power is 50W.
Reference examples 3
It is with the difference of embodiment 1：Step（1）In, ultrasonic power is 500W.
Dispersivity test
Take 2g to be scattered in 40mL water respectively the chopped carbon fiber being modified by above-described embodiment and reference examples, surpass at room temperature
Sound disperses static after 30min, observes its dispersity, observes result such as following table.
The result in table, whether ultrasonic and ultrasonic power has a strong impact on the scattered of finally modified chopped carbon fiber
Property：The dispersion effect of ultrasound is substantially better than not ultrasonic；In addition, when ultrasonic power is too low or too high, can also reduce modified short
Cut dispersion effect of the carbon fiber in water.Under the synergy of ammonium persulfate and ultrasound, and when ultrasound power 100 ~
During 300W, it just can guarantee that modified chopped carbon fiber has excellent dispersion effect in water.
Claims (3)
1. the method that polyaniline-coated is modified chopped carbon fiber, it is characterised in that comprise the following steps：
（1）, chopped carbon fiber is soaked in the ammonium persulfate aqueous solution that concentration is 30 ~ 50g/L, ultrasonically treated 1 ~ 4h is obtained
The chopped carbon fiber suspension of pre-oxidation；In the step, 8 ~ 15g of chopped carbon fiber is added in every 1L ammonium persulfate aqueous solutions；
（2）, under stirring state, first add aniline hydrochloride into above-mentioned suspension, add ammonium persulfate and ferrous sulfate, then
Temperature control reacts 10 ~ 16h at 5 ~ 10 DEG C；In the step, the moL of aniline hydrochloride 0.1 ~ 0.5, over cure are separately added into every 1L suspension
The sour moL of ammonium 0.1 ~ 0.5,0.002 ~ 0.01moL of ferrous sulfate；
（3）, hydrochloric acid with 0.01 ~ 0.05mol/L and acetone alternating washed product, be 7 with distilled water flushing to pH, filtering is dried
It is dry, obtain the chopped carbon fiber of polyaniline-coated modification.
2. method of modifying as claimed in claim 1, it is characterised in that：The length of the chopped carbon fiber is 2 ~ 25mm.
3. method of modifying as claimed in claim 1, it is characterised in that：The ultrasonic temperature is 40 ~ 80 DEG C, and ultrasonic power is
100~300W。
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| CN201710605310.XA CN107217491B (en) | 2017-07-24 | 2017-07-24 | The method of the modified chopped carbon fiber of polyaniline-coated |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112143037A (en) * | 2020-09-25 | 2020-12-29 | 深圳中诺材料技术有限公司 | Surface insulation modified carbon fiber filler and heat conduction insulating material prepared from same |
| CN112898608A (en) * | 2021-03-23 | 2021-06-04 | 四川大学 | Polyaniline-modified carbon fiber composite material, preparation method and application thereof |
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| CN112143037A (en) * | 2020-09-25 | 2020-12-29 | 深圳中诺材料技术有限公司 | Surface insulation modified carbon fiber filler and heat conduction insulating material prepared from same |
| CN112143037B (en) * | 2020-09-25 | 2022-06-14 | 深圳中诺材料技术有限公司 | Surface insulation modified carbon fiber filler and heat conduction insulating material prepared from same |
| CN112898608A (en) * | 2021-03-23 | 2021-06-04 | 四川大学 | Polyaniline-modified carbon fiber composite material, preparation method and application thereof |
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| CN107217491B (en) | 2019-08-09 |
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