CN103540982B - A kind of surface treatment of carbon fibers equipment and surface treatment method and application - Google Patents

A kind of surface treatment of carbon fibers equipment and surface treatment method and application Download PDF

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Publication number
CN103540982B
CN103540982B CN201310431873.3A CN201310431873A CN103540982B CN 103540982 B CN103540982 B CN 103540982B CN 201310431873 A CN201310431873 A CN 201310431873A CN 103540982 B CN103540982 B CN 103540982B
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deflector roll
surface treatment
insulation
truss
carbon fibers
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CN103540982A (en
Inventor
黄险波
陈大华
谢怀玉
宋威
雷震
易明
肖彦
熊少燕
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GUANGZHOU KINGFA CARBON FIBER NEW MATERIAL DEVELOPMENT Co Ltd
Kingfa Science and Technology Co Ltd
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GUANGZHOU KINGFA CARBON FIBER NEW MATERIAL DEVELOPMENT Co Ltd
Kingfa Science and Technology Co Ltd
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Abstract

The invention discloses a kind of surface treatment of carbon fibers equipment, including truss, inside described truss, be separated into two separate space, be respectively for containing the electrolysis bath of electrolyte and for containing the rinsing bowl of deionized water;Being provided with minus plate in described electrolysis bath, minus plate connects electrolysis power negative pole;It is also arranged above the first insulation deflector roll in minus plate in electrolysis bath;It is provided with the second insulation deflector roll in described rinsing bowl, between the second insulation deflector roll in the absolutely godet of first in electrolysis bath and rinsing bowl, is arranged above the 3rd insulation deflector roll in truss;Being respectively equipped with anode deflector roll above truss in the outside in the outside of the first insulation deflector roll with the second insulation deflector roll, anode deflector roll connects electrolysis power positive pole;The present invention solves the oxidized non-conductive problem of anode deflector roll, utilizes the surface treatment method of present device can shorten surface simultaneously and processes the time, can be applicable to automobile, medical treatment, food processing industry, chemical field.

Description

A kind of surface treatment of carbon fibers equipment and surface treatment method and application
Technical field
The present invention relates to carbon fiber surface modification technical field, particularly relate to a kind of surface treatment of carbon fibers equipment and surface Processing method and application.
Background technology
Carbon fiber has the mechanical property of excellence, and carbon fiber is commonly used to enhancing polymeric material field, in order to improve carbon Fiber and the interface performance of polymer composite, industrial commonly used electrochemical method carries out surface process to carbon fiber, But existing patent and technology can not solve two problems present in production: the easy oxidized problem of (1) anode deflector roll, China is specially Profit CN 10141848A discloses a kind of carbon fibre surface processor, the anode deflector roll of this datatron easily by electrolyte oxidation, It is, owing to anode roller strap has electric current, carbon fiber to press when certain speed runs, electrolyte is introduced anode guide roller surface from electrolysis bath, Anode deflector roll is the most oxidized under electric current and electrolyte effect, ultimately results in anode deflector roll oxidized and non-conductive;(2) surface The process time is long, and Chinese patent CN 101781843A discloses the surface treatment method of a kind of high-strength carbon fibre, but the method The surface process time of middle embodiment is 40 ~ 250s.
Summary of the invention
The defect of and surface treatment of carbon fibers overlong time the most oxidized for the anode deflector roll overcoming prior art with not Foot, the primary and foremost purpose of the present invention is to provide one can solve the most oxidized non-conductive problem of anode deflector roll, and is avoided that sun The surface treatment of carbon fibers equipment of the metal ion pollution electrolyte after pole deflector roll is oxidized.
It is a further object of the present invention to provide one to shorten the surface process time and improve carbon fiber interlaminar shear strength Carbon fiber surface treatment method.
The present invention is achieved by the following technical solution:
A kind of surface treatment of carbon fibers equipment, including truss, is separated into two separate space inside described truss, be respectively For containing the electrolysis bath of electrolyte and for containing the rinsing bowl of deionized water;Minus plate it is provided with in described electrolysis bath, cloudy Pole plate connects electrolysis power negative pole;It is also arranged above the first insulation deflector roll in minus plate in electrolysis bath;Arrange in described rinsing bowl There is the second insulation deflector roll, upper in truss between the second insulation deflector roll in the absolutely godet of first in electrolysis bath and rinsing bowl Side is additionally provided with the 3rd insulation deflector roll;It is arranged over first anode deflector roll in truss, second in the outside of the first insulation deflector roll The outside of insulation deflector roll is arranged over second plate deflector roll in truss, and first, second anode deflector roll connects electrolysis power positive pole.
Being introduced by carbon fiber when carrying out electrochemical treatments in the surface treatment of carbon fibers equipment of the present invention, carbon fiber is the most logical Cross first anode deflector roll above truss outside the first insulation deflector roll and enter in electrolysis bath, the first insulation in electrolysis bath Electrochemical reaction is there is so that uniform on carbon fiber tape under deflector roll, and the effect of the electrolyte in electrolysis bath and minus plate Positive charge;Then carbon fiber enters in rinsing bowl by the 3rd insulation deflector roll, and is immersed in washing by the second insulation deflector roll In deionized water in groove, thus the electrolyte of carbon fiber is washed away, finally by second insulation deflector roll outside above truss Anode deflector roll leave rinsing bowl;The carbon fiber surface equipment of the present invention avoids the electrolysis in electrolysis bath when carbon fiber runs Liquid is incorporated into outside the second insulation deflector roll in the second plate deflector roll above truss, solves second plate deflector roll gradually by oxygen Change nonconducting problem, and can allow positive charge on carbon fiber homogeneous band.
A kind of carbon fiber surface treatment method using above-mentioned surface treatment of carbon fibers equipment, comprises the steps:
A) configuration quality concentration is the ammonium salt electrolyte solution of 2 ~ 6%;
B) being introduced by carbon fiber in surface treatment of carbon fibers equipment and carry out electrochemical treatments, treatment temperature is 20 ~ 40 DEG C, control Electrolytic current density 5 ~ 20mA/cm processed2, process time 10 ~ 60s;
C) 100 ~ 120 DEG C of convection dryings, to obtain final product.
Preferably, described ammonium salt is selected from ammonium hydrogen carbonate, ammonium dihydrogen phosphate, one or more mixture of ammonium oxalate.
The carbon fiber prepared by above-mentioned carbon fiber surface treatment method for enhancing modified thermoplasticity and thermosetting resin, Can include with application: automobile, medical treatment, food processing industry, chemical field;The parts of concrete preparation include: motivation position Including gas handling system and fuel system, such as engine air cylinder cap, air throttle, air filter machine casing, Vehicular air loudspeaker , car air-conditioner flexible pipe, cooling fan and shell, water inlet pipe, brake oil tank and fill lid etc.;Car body position parts have: vapour Car mud guard, rearview mirror bracket, bumper, instrumental panel, luggage carrier, door handle, windscreen wiper, buckle of safety belt are got, various in lift Decoration etc.;The most automatically controlled door and window of electrical equipment aspect, adapter, crisper, cable binding etc. in car.
The present invention compared with prior art, has a following beneficial effect:
1) the surface treatment of carbon fibers equipment of the present invention solves the most oxidized nonconducting problem of anode deflector roll, and energy Meet positive charge on carbon fiber homogeneous band, avoid simultaneously metal deflector roll oxidized after metal ion pollution electrolyte.
2) use the ammonium salt electrolyte of the low concentration of 2 ~ 6%, can effectively reduce using and wasting of electrolyte, and improve carbon The washing efficiency that fiber is follow-up.
3) DC source and 5 ~ 20mA/cm are used2High current density carbon fiber is carried out oxidization electrolysis, can effectively subtract Few electrolysis time, improves electrolytic efficiency, improves more than 15%, during process before the interlaminar shear strength of carbon fiber is not electrolysed simultaneously Between be down to 10 ~ 60s.
Accompanying drawing explanation
Fig. 1 is the structural representation of surface treatment of carbon fibers equipment of the present invention.
Detailed description of the invention
Further illustrating the present invention below by detailed description of the invention, following example are the present invention preferably embodiment party Formula, but embodiments of the present invention are not limited by following embodiment.
As it is shown in figure 1, a kind of surface treatment of carbon fibers equipment, including truss 12, described truss 12 is internal is separated into two Separate space, is respectively for containing the electrolysis bath 10 of electrolyte and for containing the rinsing bowl 11 of deionized water;Described electrolysis Being provided with minus plate 8 in groove 10, minus plate 8 connects electrolysis power 9 negative pole;It is also arranged above in minus plate 8 in electrolysis bath 10 One insulation deflector roll 2;The second insulation deflector roll 5 it is provided with, first in electrolysis bath 10 godet 2 and water absolutely in described rinsing bowl 11 In washing trough 11 second insulation deflector roll 5 between in truss 12 be arranged above the 3rd insulation deflector roll 4;At the first insulation deflector roll The outside of 2 is arranged over first anode deflector roll 1 in truss 12, is arranged over the in the outside of the second insulation deflector roll 5 in truss 12 Two anode deflector rolls 6, first, second anode deflector roll 1,6 connects electrolysis power 9 positive pole.
So that fully there is electrochemical reaction under the effect of the electrolyte that carbon fiber is in electrolysis bath and minus plate and Uniform positive charge on band, is provided with the 4th insulation deflector roll 3 between described first anode deflector roll 1 and described first insulation deflector roll 2.
Preferably, the material of described truss 12 is politef;The material of described minus plate 8 is copper;Described electrolysis electricity Source 9 is DC source.
Described first, second anode deflector roll 1,6 with the contact surface material of described electrolysis power 9 and electrolysis bath electrolyte inside is Conductive material, preferably rustless steel;The conduction thickness of first, second anode deflector roll 1,6 contact surface is 5um, its bearing and internal material Matter is without particular/special requirement, metal, macromolecule, inorganic material.
Go in described first, second, third and fourth insulation deflector roll 2,3,4,5 and electrolysis bath electrolyte inside and rinsing bowl from Sub-water engaging surface material is insulator material, is preferably pottery;First, second, third and fourth insulation deflector roll 2,3,4,5 contact The insulator coating thickness in face is 1 ~ 5mm, and its bearing and inner materials are without particular/special requirement, metal, macromolecule, inorganic material
Embodiment 1:
Configuration quality concentration is the ammonium dihydrogen phosphate electrolyte solution of 5%, and carbon fiber introduces surface treatment of carbon fibers equipment In carry out electrochemical treatments, treatment temperature is 25 DEG C, control electrolytic current density 10mA/cm2, process time 10s, 100 DEG C are straight Connect dry, collect sample;Sample tests interlaminar shear strength according to GB3357-82, and performance test data is shown in Table 1.
Embodiment 2:
Configuration quality concentration is the ammonium dihydrogen phosphate electrolyte solution of 5%, and carbon fiber introduces surface treatment of carbon fibers equipment In carry out electrochemical treatments, treatment temperature is 25 DEG C, control electrolytic current density 5mA/cm2, process time 25s, 100 DEG C are directly It is dried, collects sample;Sample tests interlaminar shear strength according to GB3357-82, and performance test data is shown in Table 1.
Embodiment 3:
Configuration quality concentration is the ammonium hydrogen carbonate electrolyte solution of 2%, is introduced by carbon fiber in surface treatment of carbon fibers equipment Carrying out electrochemical treatments, treatment temperature is 25 DEG C, controls electrolytic current density 12mA/cm2, process time 60s, 100 DEG C are directly It is dried, collects sample;Sample tests interlaminar shear strength according to GB3357-82, and performance test data is shown in Table 1.
Embodiment 4:
Configuration quality concentration is the ammonium hydrogen carbonate electrolyte solution of 4%, is introduced by carbon fiber in surface treatment of carbon fibers equipment Carrying out electrochemical treatments, treatment temperature is 25 DEG C, controls electrolytic current density 15mA/cm2, process time 55s, 100 DEG C are directly It is dried, collects sample;Sample tests interlaminar shear strength according to GB3357-82, and performance test data is shown in Table 1.
Embodiment 5:
Configuration quality concentration is the ammonium oxalate electrolyte solution of 6%, introduces carbon fiber in surface treatment of carbon fibers equipment Row electrochemical treatments, treatment temperature is 25 DEG C, controls electrolytic current density 20mA/cm2, process time 40s, 100 DEG C are directly dry Dry, collect sample;Sample tests interlaminar shear strength according to GB3357-82, and performance test data is shown in Table 1.
Comparative example 1:
The carbon fiber not carrying out electrochemical treatments is tested interlaminar shear strength according to GB3357-82, real as the present invention Execute the blank experiment sample of example;Performance test data is shown in Table 1.
Comparative example 2:
Configuration quality concentration is the ammonium hydrogen carbonate electrolyte solution of 10%, and carbon fiber introduces surface treatment of carbon fibers equipment In carry out electrochemical treatments, treatment temperature is 35 DEG C, control electrolytic current density 0.15mA/cm2, process time 150s, subsequently At room temperature with deionized water clean, 100 DEG C be dried collect sample, sample tests interlaminar shear strength according to GB3357-82;Property Data can be tested and be shown in Table 1.
The concrete proportioning of surface treatment of carbon fibers and the performance test results in table 1 embodiment 1 ~ 5 and comparative example 1 ~ 2
Electrolyte Concentration of electrolyte (%) Process time (s) Treatment temperature (DEG C) Electric current density (mA/cm2) ILSS (Mpa)
Embodiment 1 Ammonium dihydrogen phosphate 5 10 25 10 87.2
Embodiment 2 Ammonium dihydrogen phosphate 5 25 25 5 79.5
Embodiment 3 Ammonium hydrogen carbonate 2 60 25 12 81.3
Embodiment 4 Ammonium hydrogen carbonate 4 55 25 15 87.3
Embodiment 5 Ammonium oxalate 6 40 25 20 95.7
Comparative example 1 Deionized water 0 150 25 0 68.9
Comparative example 2 Ammonium hydrogen carbonate 10 150 35 0.15 85.6
As known from Table 1, embodiment 1 ~ 5, relative to comparative example 1, the relatively carbon fiber of the interlaminar shear strength after carbon fiber electrolytic When not being electrolysed, ILSS improves more than 15%;
Embodiment 1 ~ 5, relative to comparative example 2, the present invention is by the way of improving electric current density, and electrolysis time significantly subtracts Little, the electrolytic efficiency of the carbon fiber of raising;Concentration of electrolyte significantly reduces simultaneously, has saved using and wasting of electrolyte, Improve the washing efficiency that carbon fiber is follow-up simultaneously.
Properties testing standard:
ILSS: carbon fiber and composite interlayer shear strength obtain according to GB3357-82 test.

Claims (6)

1. a surface treatment of carbon fibers equipment, including truss (12), it is characterised in that described truss (12) is internal is separated into two Individual separate space, is respectively the electrolysis bath (10) for containing electrolyte and for containing the rinsing bowl (11) of deionized water;Institute Being provided with minus plate (8) in stating electrolysis bath (10), minus plate (8) connects electrolysis power (9) negative pole;In negative electrode in electrolysis bath (10) Plate (8) is also arranged above the first insulation deflector roll (2);The second insulation deflector roll (5) it is provided with, at electrolysis bath in described rinsing bowl (11) (10) between the second insulation deflector roll (5) in the godet (2) absolutely of first in and rinsing bowl (11) in the top of truss (12) also It is provided with the 3rd insulation deflector roll (4);It is arranged over first anode deflector roll in truss (12) in the outside of the first insulation deflector roll (2) (1), being arranged over second plate deflector roll (6) in the outside of the second insulation deflector roll (5) in truss (12), first, second anode is led Roller (1,6) connects electrolysis power (9) positive pole.
Surface treatment of carbon fibers equipment the most according to claim 1, it is characterised in that described first anode deflector roll (1) with It is provided with the 4th insulation deflector roll (3) between described first insulation deflector roll (2).
Surface treatment of carbon fibers equipment the most according to claim 1 and 2, it is characterised in that the material of described truss (12) For politef;Described first, second anode deflector roll (1,6) and described electrolysis power (9) and electrolysis bath (10) electrolyte inside The material of contact surface be rustless steel;Described first, second, third and fourth insulation deflector roll (2,3,4,5) and electrolysis bath (10) The material of electrolyte inside and rinsing bowl (11) interior deionized water contact surface is pottery;The material of described minus plate (8) is copper.
Surface treatment of carbon fibers equipment the most according to claim 1, it is characterised in that described electrolysis power (9) is direct current Power supply.
5. using a carbon fiber surface treatment method for surface treatment of carbon fibers equipment described in claim 1, its feature exists In, comprise the steps:
A) configuration quality concentration is the ammonium salt electrolyte solution of 2 ~ 6%;
B) being introduced by carbon fiber in surface treatment of carbon fibers equipment and carry out electrochemical treatments, treatment temperature is 20 ~ 40 DEG C, controls electricity Solve electric current density 5 ~ 20mA/cm2, process time 10 ~ 60s;
C) 100 ~ 120 DEG C of convection dryings, to obtain final product.
Carbon fiber surface treatment method the most according to claim 5, it is characterised in that ammonium salt described in step a) is selected from carbonic acid Hydrogen ammonium, ammonium dihydrogen phosphate, one or more mixture of ammonium oxalate.
CN201310431873.3A 2013-09-22 2013-09-22 A kind of surface treatment of carbon fibers equipment and surface treatment method and application Active CN103540982B (en)

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CN105696304A (en) * 2014-11-25 2016-06-22 句容市百事特复合材料有限公司 Carbon fiber surface continuous treatment apparatus
CN104928738B (en) * 2015-05-21 2017-04-19 中国科学院山西煤炭化学研究所 Continuous metal electroplating method and device for carbon fiber tows
CN106947989B (en) * 2017-05-12 2019-02-15 中简科技股份有限公司 Carbon fiber surface electroplating system
CN108193482B (en) * 2017-12-22 2020-06-16 北京化工大学 Processing method for carbon fiber surface modification
CN110010875A (en) * 2019-04-11 2019-07-12 陕西科技大学 A kind of preparation method of flake cobalt sulfide composite and flexible carbon cloth electrode material
CN114427109A (en) * 2020-10-12 2022-05-03 中国石油化工股份有限公司 Carbon fiber anodic oxidation surface treatment device and surface treatment method
CN112746299A (en) * 2020-12-18 2021-05-04 连云港鹰游工程技术研究院有限公司 Surface treatment method for carbon fiber carbon filaments

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FR2460348A1 (en) * 1979-06-29 1981-01-23 Onera (Off Nat Aerospatiale) METHOD AND DEVICE FOR COATING SMALL DIMENSIONAL ELEMENTS OF A METAL DEPOSITION
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CN103014923A (en) * 2012-07-03 2013-04-03 镇江奥立特机械制造有限公司 Carbon fiber surface treatment machine

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