CN109371662A - A kind of processing method of high-strength carbon fiber - Google Patents
A kind of processing method of high-strength carbon fiber Download PDFInfo
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- CN109371662A CN109371662A CN201811255903.9A CN201811255903A CN109371662A CN 109371662 A CN109371662 A CN 109371662A CN 201811255903 A CN201811255903 A CN 201811255903A CN 109371662 A CN109371662 A CN 109371662A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 125
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 125
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 238000003672 processing method Methods 0.000 title claims abstract description 20
- 238000012545 processing Methods 0.000 claims abstract description 44
- 230000004048 modification Effects 0.000 claims abstract description 28
- 238000012986 modification Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003792 electrolyte Substances 0.000 claims description 11
- 238000006116 polymerization reaction Methods 0.000 claims description 11
- 230000005855 radiation Effects 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000004615 ingredient Substances 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000011282 treatment Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical group Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 5
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011888 foil Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- -1 titanium nitrides Chemical class 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 241001474374 Blennius Species 0.000 claims 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 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical class [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 2
- 235000019359 magnesium stearate Nutrition 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 230000006872 improvement Effects 0.000 abstract description 4
- 238000009941 weaving Methods 0.000 abstract description 3
- 238000011049 filling Methods 0.000 abstract description 2
- 230000006641 stabilisation Effects 0.000 abstract description 2
- 238000011105 stabilization Methods 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 10
- 238000011161 development Methods 0.000 description 9
- 239000000446 fuel Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- DKXULEFCEORBJK-UHFFFAOYSA-N magnesium;octadecanoic acid Chemical compound [Mg].CCCCCCCCCCCCCCCCCC(O)=O DKXULEFCEORBJK-UHFFFAOYSA-N 0.000 description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 235000010413 sodium alginate Nutrition 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000000946 synaptic effect Effects 0.000 description 1
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic Table
-
- 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
-
- 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
- D06M10/08—Organic compounds
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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
- D06M10/08—Organic compounds
- D06M10/10—Macromolecular compounds
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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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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a kind of processing method of high-strength carbon fiber, include the following steps: the pretreatment of (1) carbon fiber surface, (2) modifications, (3) twice-modified processing.The present invention has carried out special Optimal improvements to the processing method of carbon fiber and has handled, the collocation of its processing step is reasonable, convenient for promoting and applying on a large scale, carbon fiber obtained has intensity high, use stabilization, the features such as service life is long, filling, weaving, deep processing good using quality, the great market competitiveness and application value.
Description
Technical field
The invention belongs to fibrous material working process technical fields, and in particular to a kind of processing side of high-strength carbon fiber
Method.
Background technique
Carbon fiber refers to fibrous material of the carbon mass fraction 90% or more in chemical composition.It is 20th century 60
A kind of high temperature resistant that age succeeds in developing, corrosion-resistant, thermal expansion coefficient is small, good stability of the dimension, high intensity, high-modulus New Type of Carbon
Material.Polyacrylonitrile fibre (PAN fiber), pitch fibers, viscose rayon or lignin fibre etc. can be used through peroxide in carbon fiber
Change, low-temperature carbonization, high temperature cabonization and be made.It is widely used in aerospace, Leisure Sport articles and general industry field.Carbon fiber
Dimension industry plays very important work in terms of the upgrading of developed country's pillar industry or even overall economic performance raising
With.The update of adjustment and traditional material to Industry Structure is also significant, to defence and military and national economy
There is very important influence.Carbon fiber is a kind of novel high-performance material risen in the 60's of last century, it has many excellent
Point is a kind of ideal functional material and structural material.What the needs initially for aerospace industry and military aircraft grew up,
But nowadays oneself is widely used in the fields such as business, civil aviation, style, industry and transport, before wide application
Scape.The development and application of high-performance carbon fibre composite material further promote the development of Industry of Carbon Fiber.In world wide, day
The states such as sheet, U.S. carbon fiber production technology is relatively advanced, and Japanese carbon fiber development has been at the forward position in the world, not only in object
It has breakthrough in terms of reason, chemical property, the yield of their polyacrylonitrile-based carbon fibre occupies the first in the world, and Related product is several
World market is monopolized.China develops carbon fiber since the later period in the 60's, fails large-scale production so far, carbon fiber
Quality and yield can not meet the demand of the national economic development, and 90% or more market is captured by external product.Especially aviation is navigated
The high-tech areas such as its department there is an urgent need to high-performance carbon fibre.China is in high-strength high-performance carbon fibre material field
Disadvantage status.
Into 21st century, with the development of economy and society, people continue to increase the demand of the energy, in order to push
Sustainable development, the mankind must greatly develop various new energy；Meanwhile the existing energy is fired due to largely consuming fossil on the earth
Material, causes huge destruction to environment, jeopardizes the survival and development of future generations.A variety of factors force human development new energy replace
The fossil energy of high carbon content, the utilization technology for opening new and renewable energy energetically will be that future society reduces environment dirt
The important measures of dye.Fuel cell power generation is the 4th class generation technology after waterpower, firepower, nuclear energy power generation, it is a kind of
Without burning under isothermal conditions directly in a manner of electrochemical reaction the chemical energy being stored in fuel and oxidant is efficient
And with the power generator that is environmentally friendly converted into electric energy.Because it has many advantages, such as high energy conversion efficiency, pollution-free, fuel
Attention of the research and development of battery technology by national governments and major company, it is considered to be 21 century preferred clean, efficient
Generation technology, be a kind of novel, huge practical technique of development potentiality.Fuel cell has the advantage that energy is converted
High-efficient, low noise, low pollution, adaptable, fuel diversity and construction period are short, easy to maintain etc..
Carbon fiber paper is a kind of gas diffusion layer material being widely used in proton exchange membrane fuel cell electrode, it is not
Only there is uniform Porous laminate structure, and since its primary raw material is graphitized carbon fibre, this fiber is led with height
It is hot, highly conductive, density is small, high temperature resistant, resistance to ablation, the features such as intensity is high so that it has excellent electric conductivity, chemical stability
And thermal stability.Carbon fiber paper is fabricated by carbon fiber, and quality is largely determined by the quality of carbon fiber,
But because of short slab problem of the China in the carbon fiber manufacturing, subsequent carbon fiber paper is caused, composite material even depth is processed
Product is also more weak in the market competitiveness.
In this regard, someone has carried out the processing method of carbon fiber to improve optimization, such as application No. is CN201010157479.1
The surface treatment method and equipment of a kind of middle high-strength carbon fiber are disclosed, wherein to carbon fiber in the way of electrochemical treatments
Working process has been carried out, the qualities such as the compatibility between the intensity of carbon fiber and composite material, but this processing side are effectively improved
That there are stability is bad for fiber after formula processing, its gas permeability etc. is bad etc. in the carbon fiber paper production as fuel cell asks
Topic needs continuous improvement to handle.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of processing method of high-strength carbon fiber is provided.
The present invention is achieved by the following technical solutions:
A kind of processing method of high-strength carbon fiber, includes the following steps:
(1) carbon fiber surface pre-processes:
First carbon fiber is immersed in sulfuric acid solution, carbon fiber is filtered out after being stirred continuously 5 ~ 8min of processing, then uses deionization
Water is spare after rinsing to neutrality；
(2) modifications:
A. by step (1), treated that carbon fiber is put into a modification liquid A, and heating keeps the temperature of a modification liquid A to be
80 ~ 85 DEG C, then constantly 15 ~ 20min of ultrasonic treatment, takes out spare after filtering off surface moisture after the completion；The primary modification
Each ingredient and its corresponding parts by weight in liquid A are as follows: 14 ~ 18 parts of Nano titanium nitrides, 3 ~ 5 parts of disodium ethylene diamine tetraacetates, 1 ~ 3 portion of seaweed
Sour sodium, 4 ~ 6 parts of magnesium stearates, 5 ~ 7 parts of silane coupling agents, 200 ~ 240 parts of deionized waters；
B. will operation a treated that carbon fiber is put into plasma radiation case carries out radiation treatment, during which control irradiation
Power is 12 ~ 14kW, and the gaseous environment in irradiation box is argon gas, temperature is 155 ~ 165 DEG C, pressure is 0.35 ~ 0.38MPa, 20 ~
Carbon fiber taken out after 25min spare；
C. b will be operated treated carbon fiber repeats carry out the processing of an aforesaid operations a and operation b after, be finally putting into
It is spare after 4 ~ 6h of drying process in drying box；
(3) twice-modified processing:
A. by step (2), treated that carbon fiber is immersed in electrolyte B, carries out electrochemical polymerization processing to carbon fiber, wherein
Working electrode is carbon fiber, and comparison electrode is metal foil electrodes, and reference electrode is saturated calomel electrode, will after 8 ~ 10min of processing
Carbon fiber takes out spare；Each ingredient and its corresponding concentration in the electrolyte B are as follows: 0.15 ~ 0.2mol/L phenol, 0.1 ~
0.15mol/L methacrylic acid, 0.55 ~ 0.60mol/L hydrochloric acid, 40 ~ 45mmol/L sodium chloride, solvent are water；
B. after being rinsed one time with deionized water to operation a treated carbon fiber, then carbon fiber is put into vacuum oven
It is dried, is taken out after 7 ~ 10h.
Further, the mass fraction of sulfuric acid solution as described in step (1) is 5 ~ 7%.
Further, the frequency of ultrasonic treatment described in step (2) operation a is 330 ~ 360kHz.
Further, the grain diameter size of Nano titanium nitride described in step (2) operation a is 10 ~ 35nm.
Further, silane coupling agent described in step (2) operation a is silane coupling agent kh550, silane coupling agent
Any one in kh560, silane coupling agent kh570.
Further, temperature when drying process described in step (2) operation c in control drying box is 120 ~ 125 DEG C.
Further, control current density is 1 ~ 2mA/cm when electrochemical polymerization processing described in step (3) operation a2。
Further, temperature when drying process described in step (3) operation b in control vacuum oven is 85 ~ 90
DEG C, vacuum degree control is 1 ~ 10Pa.
The present invention has carried out special improvement to the processing method of carbon fiber and has handled, improve well its using effect and
The market competitiveness.Wherein, sulfuric acid solution first has been carried out to carbon fiber and has impregnated removal of impurities activation processing, established base for subsequent processing
Then plinth has carried out a modification to carbon fiber, carried out immersion treatment to carbon fiber with a modification liquid A of preparation,
Under the mating reaction of Multiple components, so that Nano titanium nitride particulate component is effectively attached on the surface of carbon fiber, then
Plasma radiation processing is carried out to the carbon fiber of a modification liquid A immersion treatment, in plasma high energy, special energy field
Under the action of, the surface of carbon fiber generates a large amount of active group, and surface is impacted by some particles and etched, and finally to receive
Rice titanium nitride particles are effectively absorbed and fixed on the surface layer of carbon fiber, so that carbon fiber surface forms a large amount of small cynapse
On the one hand structure improves the specific surface area of fiber, improve can deposit, adsorption capacity, on the other hand enhance each other and
Strength is closed with the anchor for being filled storeroom, then twice-modified processing has been carried out again, specifically to the carbon after a modification
Fiber carries out electrochemical polymerization processing, and under the action of electrolyte B, electric current, the electropolymerizations product such as phenol is with Nano titanium nitride
Grain is basic point, and evenly dispersed is attached to fixed on carbon fiber surface, forms one layer of grafting fixing layer, improves carbon well
Compatible binding ability between the macromolecule components such as fiber and resin, plastics, but the combination for improving carbon fiber weaving paper, cloth etc. is strong
Power etc., and this carbon fiber surface small synaptic structure coated with film can promote mutual bond strength and woven densification
Property, and can to generate the permeability etc. that gap guarantees entirety each other, it imparts this fiber and is all had in different field
Excellent use quality.
The present invention has the advantage that compared with prior art
The present invention has carried out special Optimal improvements to the processing method of carbon fiber and has handled, and processing step collocation rationally, is convenient for
Large-scale to promote and apply, carbon fiber obtained has intensity high, and using stabilization, the service life is long, and filling, weaving, deep processing use
The features such as quality is good, the great market competitiveness and application value.
Specific embodiment
Embodiment 1
A kind of processing method of high-strength carbon fiber, includes the following steps:
(1) carbon fiber surface pre-processes:
First carbon fiber is immersed in sulfuric acid solution, carbon fiber is filtered out after being stirred continuously processing 5min, then uses deionized water
It is spare after rinsing to neutrality；
(2) modifications:
A. by step (1), treated that carbon fiber is put into a modification liquid A, and heating keeps the temperature of a modification liquid A to be
80 DEG C, then constantly ultrasonic treatment 15min, takes out spare after filtering off surface moisture after the completion；It is each in modification liquid A
Ingredient and its corresponding parts by weight are as follows: 14 parts of Nano titanium nitrides, 3 parts of disodium ethylene diamine tetraacetates, 1 part of sodium alginate, 4 parts of stearic acid
Magnesium, 5 parts of silane coupling agents, 200 parts of deionized waters；
B. will operation a treated that carbon fiber is put into plasma radiation case carries out radiation treatment, during which control irradiation
Power is 12kW, the gaseous environment in irradiation box is argon gas, temperature is 155 DEG C, after pressure 0.35MPa, 20min by carbon fiber
It takes out spare；
C. b will be operated treated carbon fiber repeats carry out the processing of an aforesaid operations a and operation b after, be finally putting into
It is spare after drying process 4h in drying box；
(3) twice-modified processing:
A. by step (2), treated that carbon fiber is immersed in electrolyte B, carries out electrochemical polymerization processing to carbon fiber, wherein
Working electrode is carbon fiber, and comparison electrode is metal foil electrodes, and reference electrode is saturated calomel electrode, by carbon fiber after processing 8min
Dimension is taken out spare；Each ingredient and its corresponding concentration in the electrolyte B are as follows: 0.15mol/L phenol, 0.1mol/L metering system
Acid, 0.55mol/L hydrochloric acid, 40mmol/L sodium chloride, solvent is water；
B. after being rinsed one time with deionized water to operation a treated carbon fiber, then carbon fiber is put into vacuum oven
It is dried, is taken out after 7h.
Further, the mass fraction of sulfuric acid solution as described in step (1) is 5%.
Further, the frequency of ultrasonic treatment described in step (2) operation a is 330kHz.
Further, the grain diameter size of Nano titanium nitride described in step (2) operation a is 10 ~ 35nm.
Further, silane coupling agent described in step (2) operation a is silane coupling agent kh550.
Further, temperature when drying process described in step (2) operation c in control drying box is 120 DEG C.
Further, control current density is 1mA/cm when electrochemical polymerization processing described in step (3) operation a2。
Further, temperature when drying process described in step (3) operation b in control vacuum oven is 85 DEG C,
Vacuum degree control is 1Pa.
Embodiment 2
A kind of processing method of high-strength carbon fiber, includes the following steps:
(1) carbon fiber surface pre-processes:
First carbon fiber is immersed in sulfuric acid solution, carbon fiber is filtered out after being stirred continuously processing 7min, then uses deionized water
It is spare after rinsing to neutrality；
(2) modifications:
A. by step (1), treated that carbon fiber is put into a modification liquid A, and heating keeps the temperature of a modification liquid A to be
83 DEG C, then constantly ultrasonic treatment 17min, takes out spare after filtering off surface moisture after the completion；It is each in modification liquid A
Ingredient and its corresponding parts by weight are as follows: 16 parts of Nano titanium nitrides, 4 parts of disodium ethylene diamine tetraacetates, 2 parts of sodium alginates, 5 parts of stearic acid
Magnesium, 6 parts of silane coupling agents, 220 parts of deionized waters；
B. will operation a treated that carbon fiber is put into plasma radiation case carries out radiation treatment, during which control irradiation
Power is 13kW, the gaseous environment in irradiation box is argon gas, temperature is 160 DEG C, after pressure 0.37MPa, 22min by carbon fiber
It takes out spare；
C. b will be operated treated carbon fiber repeats carry out the processing of an aforesaid operations a and operation b after, be finally putting into
It is spare after drying process 5h in drying box；
(3) twice-modified processing:
A. by step (2), treated that carbon fiber is immersed in electrolyte B, carries out electrochemical polymerization processing to carbon fiber, wherein
Working electrode is carbon fiber, and comparison electrode is metal foil electrodes, and reference electrode is saturated calomel electrode, by carbon fiber after processing 9min
Dimension is taken out spare；Each ingredient and its corresponding concentration in the electrolyte B are as follows: 0.18mol/L phenol, 0.13mol/L methyl-prop
Olefin(e) acid, 0.57mol/L hydrochloric acid, 42mmol/L sodium chloride, solvent are water；
B. after being rinsed one time with deionized water to operation a treated carbon fiber, then carbon fiber is put into vacuum oven
It is dried, is taken out after 9h.
Further, the mass fraction of sulfuric acid solution as described in step (1) is 6%.
Further, the frequency of ultrasonic treatment described in step (2) operation a is 340kHz.
Further, the grain diameter size of Nano titanium nitride described in step (2) operation a is 10 ~ 35nm.
Further, silane coupling agent described in step (2) operation a is silane coupling agent kh560.
Further, temperature when drying process described in step (2) operation c in control drying box is 123 DEG C.
Further, control current density is 1.5mA/cm when electrochemical polymerization processing described in step (3) operation a2。
Further, temperature when drying process described in step (3) operation b in control vacuum oven is 88 DEG C,
Vacuum degree control is 5Pa.
Embodiment 3
A kind of processing method of high-strength carbon fiber, includes the following steps:
(1) carbon fiber surface pre-processes:
First carbon fiber is immersed in sulfuric acid solution, carbon fiber is filtered out after being stirred continuously processing 8min, then uses deionized water
It is spare after rinsing to neutrality；
(2) modifications:
A. by step (1), treated that carbon fiber is put into a modification liquid A, and heating keeps the temperature of a modification liquid A to be
85 DEG C, then constantly ultrasonic treatment 20min, takes out spare after filtering off surface moisture after the completion；It is each in modification liquid A
Ingredient and its corresponding parts by weight are as follows: 18 parts of Nano titanium nitrides, 5 parts of disodium ethylene diamine tetraacetates, 3 parts of sodium alginates, 6 parts of stearic acid
Magnesium, 7 parts of silane coupling agents, 240 parts of deionized waters；
B. will operation a treated that carbon fiber is put into plasma radiation case carries out radiation treatment, during which control irradiation
Power is 14kW, the gaseous environment in irradiation box is argon gas, temperature is 165 DEG C, after pressure 0.38MPa, 25min by carbon fiber
It takes out spare；
C. b will be operated treated carbon fiber repeats carry out the processing of an aforesaid operations a and operation b after, be finally putting into
It is spare after drying process 6h in drying box；
(3) twice-modified processing:
A. by step (2), treated that carbon fiber is immersed in electrolyte B, carries out electrochemical polymerization processing to carbon fiber, wherein
Working electrode is carbon fiber, and comparison electrode is metal foil electrodes, and reference electrode is saturated calomel electrode, by carbon after processing 10min
Fiber takes out spare；Each ingredient and its corresponding concentration in the electrolyte B are as follows: 0.2mol/L phenol, 0.15mol/L methyl-prop
Olefin(e) acid, 0.60mol/L hydrochloric acid, 45mmol/L sodium chloride, solvent are water；
B. after being rinsed one time with deionized water to operation a treated carbon fiber, then carbon fiber is put into vacuum oven
It is dried, is taken out after 10h.
Further, the mass fraction of sulfuric acid solution as described in step (1) is 7%.
Further, the frequency of ultrasonic treatment described in step (2) operation a is 360kHz.
Further, the grain diameter size of Nano titanium nitride described in step (2) operation a is 10 ~ 35nm.
Further, silane coupling agent described in step (2) operation a is silane coupling agent kh570.
Further, temperature when drying process described in step (2) operation c in control drying box is 125 DEG C.
Further, control current density is 2mA/cm when electrochemical polymerization processing described in step (3) operation a2。
Further, temperature when drying process described in step (3) operation b in control vacuum oven is 90 DEG C,
Vacuum degree control is 10Pa.
Comparative example 1
This comparative example 1 compared with Example 2, eliminates the operation a processing in (2) modifications of step, in addition to this
Method and step it is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, eliminates the operation b processing in (2) modifications of step, in addition to this
Method and step it is all the same.
Comparative example 3
This comparative example 3 compared with Example 2, eliminates the whole operation of (2) modifications of step, side in addition to this
Method step is all the same.
Control group
Application No. is: CN201010157479.1 discloses a kind of surface treatment method of middle high-strength carbon fiber.
In order to compare effect of the present invention, to above-described embodiment 2, comparative example 1, comparative example 2, comparative example 3,
Carbon fiber made from control group corresponding method is tested for the property, and specific correlation data is as shown in table 1 below:
Table 1
| TS(GPa) | ILSS(MPa) | Air permeability (ft3/ min) | Tensile strength (N/m) | |
| Embodiment 2 | 4.84 | 119.6 | 17.6 | 87.3 |
| Comparative example 1 | 3.92 | 91.4 | 15.2 | 69.8 |
| Comparative example 2 | 4.35 | 102.1 | 16.0 | 73.7 |
| Comparative example 3 | 3.77 | 87.6 | 13.8 | 65.0 |
| Control group | 3.71 | 88.5 | 13.5 | 62.4 |
Note: TS described in upper table 1 is the tensile strength of carbon fiber ontology, is tested according to GB3362-2005；Described
ILSS is carbon fiber and composite material interlayer shear strength, is tested according to GB3357-82；The air permeability and anti-tensile is strong
Degree is to carry out same method to carbon fiber to weave, and the test carried out after carbon fiber paper is made, the air permeability uses
High-air-permeability tester m380275 is tested；The tensile strength is surveyed using ZLB-100 paper pull testing machine
Examination.
The carbon fiber strength that the method for the present invention is processed into it can be seen from upper table 1 is high, comprehensive good using quality, in difference
Using effect in field is good, the great market competitiveness and application value.
Claims (8)
1. a kind of processing method of high-strength carbon fiber, which comprises the steps of:
(1) carbon fiber surface pre-processes:
First carbon fiber is immersed in sulfuric acid solution, carbon fiber is filtered out after being stirred continuously 5 ~ 8min of processing, then uses deionization
Water is spare after rinsing to neutrality；
(2) modifications:
A. by step (1), treated that carbon fiber is put into a modification liquid A, and heating keeps the temperature of a modification liquid A to be
80 ~ 85 DEG C, then constantly 15 ~ 20min of ultrasonic treatment, takes out spare after filtering off surface moisture after the completion；The primary modification
Each ingredient and its corresponding parts by weight in liquid A are as follows: 14 ~ 18 parts of Nano titanium nitrides, 3 ~ 5 parts of disodium ethylene diamine tetraacetates, 1 ~ 3 portion of seaweed
Sour sodium, 4 ~ 6 parts of magnesium stearates, 5 ~ 7 parts of silane coupling agents, 200 ~ 240 parts of deionized waters；
B. will operation a treated that carbon fiber is put into plasma radiation case carries out radiation treatment, during which control irradiation
Power is 12 ~ 14kW, and the gaseous environment in irradiation box is argon gas, temperature is 155 ~ 165 DEG C, pressure is 0.35 ~ 0.38MPa, 20 ~
Carbon fiber taken out after 25min spare；
C. b will be operated treated carbon fiber repeats carry out the processing of an aforesaid operations a and operation b after, be finally putting into
It is spare after 4 ~ 6h of drying process in drying box；
(3) twice-modified processing:
A. by step (2), treated that carbon fiber is immersed in electrolyte B, carries out electrochemical polymerization processing to carbon fiber, wherein
Working electrode is carbon fiber, and comparison electrode is metal foil electrodes, and reference electrode is saturated calomel electrode, will after 8 ~ 10min of processing
Carbon fiber takes out spare；Each ingredient and its corresponding concentration in the electrolyte B are as follows: 0.15 ~ 0.2mol/L phenol, 0.1 ~
0.15mol/L methacrylic acid, 0.55 ~ 0.60mol/L hydrochloric acid, 40 ~ 45mmol/L sodium chloride, solvent are water；
B. after being rinsed one time with deionized water to operation a treated carbon fiber, then carbon fiber is put into vacuum oven
It is dried, is taken out after 7 ~ 10h.
2. a kind of processing method of high-strength carbon fiber according to claim 1, which is characterized in that described in step (1)
Sulfuric acid solution mass fraction be 5 ~ 7%.
3. a kind of processing method of high-strength carbon fiber according to claim 1, which is characterized in that step (2) operates in a
The frequency of the ultrasonic treatment is 330 ~ 360kHz.
4. a kind of processing method of high-strength carbon fiber according to claim 1, which is characterized in that step (2) operates in a
The grain diameter size of the Nano titanium nitride is 10 ~ 35nm.
5. a kind of processing method of high-strength carbon fiber according to claim 1, which is characterized in that step (2) operates in a
The silane coupling agent is silane coupling agent kh550, silane coupling agent kh560, any one in silane coupling agent kh570
Kind.
6. a kind of processing method of high-strength carbon fiber according to claim 1, which is characterized in that step (2) operates in c
Temperature when the described drying process in control drying box is 120 ~ 125 DEG C.
7. a kind of processing method of high-strength carbon fiber according to claim 1, which is characterized in that step (3) operates in a
Control current density is 1 ~ 2mA/cm when the electrochemical polymerization is handled2。
8. a kind of processing method of high-strength carbon fiber according to claim 1, which is characterized in that step (3) operates in b
Temperature when the described drying process in control vacuum oven is 85 ~ 90 DEG C, and vacuum degree control is 1 ~ 10Pa.
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