CN114427109A - Carbon fiber anodic oxidation surface treatment device and surface treatment method - Google Patents
Carbon fiber anodic oxidation surface treatment device and surface treatment method Download PDFInfo
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- CN114427109A CN114427109A CN202011084109.XA CN202011084109A CN114427109A CN 114427109 A CN114427109 A CN 114427109A CN 202011084109 A CN202011084109 A CN 202011084109A CN 114427109 A CN114427109 A CN 114427109A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 103
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 103
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 238000004381 surface treatment Methods 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 31
- 230000003647 oxidation Effects 0.000 title claims abstract description 30
- 238000007598 dipping method Methods 0.000 claims abstract description 37
- 239000002912 waste gas Substances 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 13
- 238000005470 impregnation Methods 0.000 claims description 45
- 230000020477 pH reduction Effects 0.000 claims description 41
- 239000003792 electrolyte Substances 0.000 claims description 38
- 239000002253 acid Substances 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 29
- 239000011521 glass Substances 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 239000010439 graphite Substances 0.000 claims description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 9
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 9
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 9
- 239000001099 ammonium carbonate Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- 238000004513 sizing Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 238000007599 discharging Methods 0.000 claims 1
- 238000011144 upstream manufacturing Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 13
- 239000002131 composite material Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 125000000524 functional group Chemical group 0.000 abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 230000036541 health Effects 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 238000010669 acid-base reaction Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000010923 batch production Methods 0.000 abstract 1
- 238000007743 anodising Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000009776 industrial production Methods 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- KKTCWAXMXADOBB-UHFFFAOYSA-N azanium;hydrogen carbonate;hydrate Chemical compound [NH4+].O.OC([O-])=O KKTCWAXMXADOBB-UHFFFAOYSA-N 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000000805 composite resin Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- 239000004254 Ammonium phosphate Substances 0.000 description 2
- 239000005696 Diammonium phosphate Substances 0.000 description 2
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical compound [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 description 2
- 235000019289 ammonium phosphates Nutrition 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 2
- 235000019838 diammonium phosphate Nutrition 0.000 description 2
- 238000006056 electrooxidation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000007380 fibre production Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000001841 imino group Chemical group [H]N=* 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/005—Apparatus specially adapted for electrolytic conversion coating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/04—Removal of gases or vapours ; Gas or pressure control
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- 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
- 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
- D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—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 nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
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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
- D06M11/73—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 carbon or compounds thereof
- D06M11/76—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 carbon or compounds thereof with carbon oxides or carbonates
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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)
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Automation & Control Theory (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a carbon fiber anodic oxidation surface treatment device and a surface treatment method. The device can flexibly adjust the distance between the dipping rollers in the electrolytic bath, control the electrolytic time, ensure that each monofilament is uniformly oxidized, have good electrolytic oxidation treatment effect, introduce active functional groups containing oxygen, nitrogen and the like on the surface of the carbon fiber and obviously improve the interlaminar shear strength of the carbon fiber composite material; the equipment manufacturing cost is low; the operation is simple and convenient, the carbon fiber tows with large number of strands are easy to process, and the method is suitable for batch production; the electrolysis device is provided with an inlet air suction cover, an outlet air suction cover and a movable cover plate, and a fan is used for extracting ammonia waste gas generated by the electrolysis device, and the ammonia waste gas is subjected to acid-base reaction to the electrolyzed waste gas treatment device provided with the foldable cover plate, so that the waste gas is effectively prevented from escaping, the environmental pollution is reduced, the health of operators is prevented from being injured in the operation process, and the safety production is ensured.
Description
Technical Field
The invention relates to a carbon fiber technology, in particular to a carbon fiber anodic oxidation surface treatment device and a surface treatment method.
Background
The performance of the carbon fiber reinforced thermosetting resin composite material not only depends on the composition of the material, but also depends on the quality of an interface between the composition materials, the surface performance of the carbon fiber and the transmission mode of the interfacial stress between the carbon fiber and the matrix. The quality of the interface bonding directly influences the stress transfer effect between the reinforcement and the matrix, thereby influencing the macroscopic mechanical property of the composite material. The interface bonding is too weak, the composite material is easy to generate interface debonding damage under the stress action, and the carbon fiber can not fully play a reinforcing role. If the surface of the carbon fiber is modified properly, the interlaminar shear strength of the composite material can be improved. If the interface adhesion is too strong, the growing crack is easily propagated to the interface during the material failure process under the stress action, and the reinforced material is directly impacted to present brittle failure. Thus, it is required to properly adjust the interface bonding strength, so that the cracks of the reinforced material can be expanded along the interface to form a tortuous path, and more energy can be dissipated, thereby improving the toughness of the composite material.
The carbon fiber is mainly used as a material of a reinforcement, and the surface treatment of the carbon fiber is mainly used for improving the interfacial adhesion between the carbon fiber and matrix resin, avoiding the overlarge loss of the tensile strength of the carbon fiber and further improving the mechanical property of the carbon fiber composite material.
In order to solve the problems, the surface of the carbon fiber needs to be treated, so that the interface bonding performance between the carbon fiber and a resin matrix is enhanced, and the interlaminar shear strength of the carbon fiber is improved. The surface treatment method of the carbon fiber is various, such as a gas phase oxidation method, a liquid phase oxidation method, a gas-liquid double effect method, a surface grafting method, a vapor deposition method and a surface coating method. The anodic electrolytic oxidation method in the liquid-phase oxidation method is mild in oxidation, easy to control the oxidation degree of the surface of the carbon fiber, convenient to operate and capable of realizing uniform oxidation of a single carbon fiber tow, active functional groups containing oxygen, nitrogen and the like are introduced to the surface of each carbon fiber tow, the interlaminar shear strength of the carbon fiber is improved, and the method is generally applied to carbon fiber manufacturers at home and abroad.
In the industrial production of carbon fibers, an anodic electrolytic oxidation method is adopted, ammonium salts such as diammonium phosphate, triammonium phosphate, ammonium phosphate and ammonium bicarbonate are used as alkaline electrolyte aqueous solutions when an electrolytic oxidation surface treatment device is utilized, and the most widely used electrolyte is an ammonium bicarbonate aqueous solution. Carbon fibers as the anode and graphite as the cathode. When current is passed through the ammonium bicarbonate electrolyte, the active oxygen atoms and the carbon ring of the carbon fiber are subjected to oxidation reaction. Under the action of electrochemical oxidation, active carbon atoms on the surface of the carbon fiber adsorb OH < - > in the alkaline solution, and are oxidized to form hydroxyl. The hydroxyl group formed continues to be oxidized by active oxygen to form a carbonyl group. Finally, the oxidation is continued to oxidize the carbonyl group to form a carboxyl group. Since the carboxyl groups are less stable in the violent exothermic reaction, carbon dioxide is easily released.
In the electrolytic process, ammonium salts such as diammonium phosphate, triammonium phosphate, ammonium phosphate and ammonium bicarbonate are used as ammonia molecules in an alkaline electrolyte aqueous solution to be adsorbed by unsaturated carbon atoms on the surface of carbon fibers, and then amino and imino are generated under electrochemical conditions. After the carbon fiber is subjected to electrochemical oxidation treatment, a large number of oxygen-containing functional groups and nitrogen-containing functional groups are introduced into the surface of the carbon fiber. Due to the increase of the functional groups, the surface polarity of the composite material is improved, the wettability and the reactivity of the carbon fiber and the epoxy resin are improved, and the mechanical property of the carbon fiber reinforced thermosetting resin composite material is improved. However, in the process of carbon fiber surface treatment, carbon dioxide and ammonia gas are generated, the ammonia gas has pungent smell, is dispersed in the air, does not meet the emission standard of malodorous pollutants, pollutes the operating environment and damages the health of operators.
The utility model discloses a single silk bundle fiber surface treatment device that chinese utility model patent CN202164492U discloses is applied to fibre surface treatment. The lower part of the bracket is fixed with a plasma generator power supply and a vortex fan. The low-temperature plasma generating device under normal pressure is adopted to treat the surface of the fiber, so that continuous production is directly realized, the fiber surface treatment procedures are reduced, the treatment process is simplified, and the fiber surface treatment efficiency is improved. Only electric energy and air are needed in the whole operation process, and clean and pollution-free processing is realized. However, when the low-temperature plasma generating device emits plasma liquid to the surface of the carbon fiber, a certain distance is formed between the nozzles of the spray gun group, so that the amount of the plasma liquid sprayed on the surface of the carbon fiber yarn is difficult to control to be the same, and differences exist, which affect the uniformity and consistency of the interlaminar shear strength of the carbon fiber reinforced thermosetting resin composite material.
The invention patent CN101660185B discloses a method for strong carbon fiber anodic oxidation surface treatment, which accelerates the oxidation process by carrying out anodic oxidation treatment on carbon fiber in an external magnetic field, wherein the strength of the external magnetic field is 5-50 mT. The method can accelerate the surface treatment speed of the carbon fiber and reduce the use amount of electrolyte, but still does not solve the problem that gas generated in the electrolyte electrolysis process is directly discharged in the air, so that the pollutant discharge requirement of a production operation area is difficult to meet, and the green and environment-friendly requirement of industrial production of the carbon fiber is not met.
Therefore, a carbon fiber environment-friendly treatment system with less material consumption and no pollution is needed.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the present invention aims to provide a carbon fiber anodizing surface treatment apparatus and a surface treatment method, which can solve the above problems.
The purpose of the invention is realized by adopting the following technical scheme:
a carbon fiber anodic oxidation surface treatment device belongs to an anodic oxidation surface treatment technology matched with carbon fiber production and operation on line, and comprises an electrolysis unit and a waste gas treatment unit. The electrolytic unit comprises an electrolyte feeding tank, an electrolyte feeding pump, an electrolytic tank, a direct-current power supply, a first conductive anode roller, a first dipping roller, a second conductive anode roller, a graphite cathode plate, a first circulating pump, a movable cover plate, an inlet air suction cover and an outlet air suction cover. The electrolyte feeding tank supplies electrolyte to the electrolytic tank through an electrolyte feeding pump. The electrolytic cell enables the electrode solution in the electrolytic cell to circularly flow through the first circulating pump. The first conductive anode roller, the first dipping roller, the second conductive anode roller and the graphite cathode plate are arranged in the electrolytic tank, and the first dipping roller, the second dipping roller and the graphite cathode plate are dipped in electrolyte. The first conductive anode roller, the first soaking roller, the second soaking roller and the second conductive anode roller are sequentially in transmission connection from a feed inlet to a discharge outlet of the electrolytic tank so as to convey and immerse carbon fibers. And the direct current power supply is electrically connected with the first conductive anode roller, the second conductive anode roller and the graphite cathode plate for power supply. The top of the side of the feed inlet of the electrolytic cell is provided with an inlet air suction cover, the top of the side of the discharge outlet of the electrolytic cell is provided with an outlet air suction cover, and the movable cover plate is arranged between the inlet air suction cover and the outlet air suction cover. The electrolyzed waste gas treatment unit comprises a fan, an acidification tank, a folding cover plate, a second circulating pump, an acid feeding pump and an acid feeding tank. The foldable cover plate is arranged on the top surface of the acidification tank. The upper stream of the fan is communicated with the air holes of the inlet air suction cover and the outlet air suction cover above the electrolytic cell, and the lower stream of the fan is introduced into the acidification tank. And the acid feeding tank supplies acid into the acidification tank through an acid feeding pump. The second circulating pump is communicated with the bottom wall and the side wall of the acidification tank to realize acid circulation in the acidification tank.
Preferably, carbon fiber tow N operating in an electrolytic cell1Width W of strand, each strand2Spacing W between two adjacent carbon fiber tows3Width W of the electrolytic cell1Is W1＝N1*W2+(N1+40)*W3Length L of the electrolytic cell1Is L1＝L4+L6+L8。
Preferably, two ends of the first dipping roller and the second dipping roller are installed on the wall of the electrolytic tank through roller bearing seats, and two sides of the roller bearing seats are respectively provided with a kidney-shaped hole so as to enable the roller bearing seats to horizontally move left and right for positioning. The maximum distance of the first dipping roller which can be horizontally moved left and right is the roller diameter D of the first dipping roller1Twice of the first dipping roll, the maximum distance of the second dipping roll which can be adjusted by moving horizontally left and right is the roll diameter D of the second dipping roll2Twice as much. Adjusting the maximum spacing L between the first and second impregnation rollers by moving the horizontal positions of the first and second impregnation rollers2Is L2＝L4+5*D2Thereby controlling the electrolysis time of the carbon fiber tows in the electrolytic bath.
Preferably, the following components: the movable cover plate comprises N2The single cover plate comprises a transparent window, driving wheels and guide wheels are arranged at the front end and the rear end of each single cover plate, and the single cover plate slides on the sliding rail through the driving wheels and the guide wheels at the two ends.
Preferably, the inlet suction hood is fixedly arranged right above the first conductive anode roller and the first dipping roller at the feed inlet of the electrolytic cell. Two sides of the inlet air suction cover are respectively provided with a glass side door which can be opened up and down, so that the wire threading production operation is convenient. The width of the inlet air suction hood is the same as that of the electrolytic bath.
Preferably, the outlet air suction hood is fixedly arranged right above the second conductive anode roller and the second dipping roller at the discharge outlet of the electrolytic cell. Two sides of the outlet air suction cover are respectively provided with a glass side door which can be opened up and down, so that the wire threading production operation is convenient. The width of the outlet air suction hood is the same as that of the electrolytic bath.
Preferably, the cover plates of the folding cover plate are connected through a hinge, the inner side of the cover plate is provided with an air cylinder, the outer side of the cover plate is provided with an air cylinder rod, and the air cylinder rod drives the air cylinder to open and close through an air cylinder electromagnetic valve.
Preferably, the acid used in the acidification tank is hydrochloric acid, sulfuric acid, nitric acid, acetic acid or phosphoric acid, and the concentration of the acid is 1-15%.
Preferably, a PH detector and a liquid level meter are arranged in the acidification tank, the PH value and the liquid level height of the solution in the acidification tank are controlled, and the PH value of the solution is controlled to be less than or equal to 7.
Meanwhile, a method for carrying out surface treatment on carbon fibers by using the device is provided, and the method comprises the following steps.
S1 preparation before operation, closing glass side doors on two sides of an inlet air suction cover and glass side doors on two sides of an outlet air suction cover, opening a valve at the bottom of an electrolyte feeding tank, starting an electrolyte feeding pump, adding ammonium bicarbonate aqueous solution with the concentration of 10% into an electrolytic tank, closing the electrolyte feeding pump when the liquid level of the ammonium bicarbonate aqueous solution in the electrolytic tank reaches 80% of the depth of the electrolytic tank, and starting a first circulating pump. And opening a cylinder control button of the acidification tank, putting down a cylinder rod, and closing the folding cover plate. Adding 7% nitric acid solution in the acid feeding tank, opening a valve at the bottom of the acid feeding tank, opening an acid feeding pump, adding the 7% nitric acid solution into the acidification tank, closing the acid feeding pump when the liquid level of the nitric acid solution reaches 80% of the depth of the acidification tank, opening a second circulating pump, opening a fan, and pumping the escaped waste gas in the electrolytic tank by an inlet air suction cover and an outlet air suction cover of the electrolytic tank to the acidification tank.
S2, starting production operation, firstly opening the glass side doors at two sides of the inlet air suction hood and the glass side doors at two sides of the outlet air suction hood, and moving every two adjacent single cover plates of the movable cover plates to two sides to enable the upper part of the electrolytic cell to be in an open state. And the carbon fiber tows at the outlet of the high-temperature carbonization furnace pass through a vertical five-roller tractor, and then pass through a first conductive anode roller, a first impregnation roller, a second impregnation roller and a second conductive anode roller in sequence. Then, the glass side doors at both sides of the inlet air suction cover and the glass side doors at both sides of the outlet air suction cover are closed, and the cover plate is moved to enable the upper part of the electrolytic cell to be in a closed state.
S3, the first conductive anode roller, the second conductive anode roller and the graphite cathode plate are connected and conducted with a direct current power supply to control the voltage of the direct current power supply to be 12V. When the carbon fiber tows run in the electrolytic cell, monitoring the conductivity of the electrolyte in the electrolytic cell to be 98 +/-2 mu s/cm, and monitoring the PH value of the solution in the acidification tank to be less than or equal to 7.
And S4, washing, sizing, drying and winding the tows at the outlet of the second conductive anode roller to obtain the 12K carbon fiber.
Compared with the prior art, the invention has the beneficial effects that: the carbon fiber anodic oxidation surface treatment device provided by the invention has the advantages that the distance between the dipping rollers in the electrolytic bath is flexibly utilized and adjusted, the electrolysis time is controlled, each monofilament is uniformly oxidized, the electrolytic oxidation treatment effect is good, active functional groups containing oxygen, nitrogen and the like are introduced into the surface of the carbon fiber, and the interlaminar shear strength of the carbon fiber composite material is obviously improved; the equipment manufacturing cost is low; the method is simple and convenient to operate, is easy to treat the anodic electrolytic oxidation of the carbon fiber tows with large number of strands, and is suitable for the industrial production of carbon fibers; the electrolytic device for carbon fiber anodic oxidation surface treatment is provided with the inlet air suction cover, the outlet air suction cover and the movable cover plate, the fan is used for extracting ammonia waste gas generated by the electrolytic device, and the ammonia waste gas is subjected to acid-base reaction to the electrolytic waste gas treatment device provided with the foldable cover plate, so that the waste gas is effectively prevented from escaping, the environmental pollution is reduced, the health of operators is prevented from being injured in the operation process, and the safety production is ensured.
Drawings
FIG. 1 is a schematic structural view of a carbon fiber anodizing surface treatment apparatus according to the present invention;
FIG. 2 is a schematic structural diagram of the movable cover plate, wherein (a) is a top plan view of the movable cover plate, (b) is a perspective view of the movable cover plate, (c) is a perspective view of a driving wheel of the movable cover plate, and (d) is a perspective view of a guide wheel of the movable cover plate;
FIG. 3 is a schematic view of an inlet suction hood configuration wherein (a) the inlet suction hood side doors are in a closed perspective view and (b) the inlet suction hood side doors are in an open perspective view;
FIG. 4 is a schematic structural view of an outlet suction hood wherein (a) the outlet suction hood side door is in a closed perspective view and (b) the outlet suction hood side door is in an open perspective view;
FIG. 5 is a schematic diagram of a folded cover configuration of an acidification tank, wherein (a) the folded cover is in front elevation, (b) the folded cover is in side elevation, and (c) the folded cover is in top elevation;
FIG. 6 is a schematic view of the roller bearing seat structure, wherein (a) the roller bearing seat and the bottom plate are combined in a perspective view, and (b) the roller bearing seat and the dip roller are combined in a perspective view.
In the figure: 1. an electrolyte feeding tank; 2. an electrolyte feed pump; 3. an electrolytic cell; 4. a direct current power supply; 5. a first conductive anode roll; 6. a first impregnation roller; 7. a second impregnation roller; 8. a second conductive anode roll; 9. a graphite cathode plate; 10. a first circulation pump; 11. a movable cover plate; 12. an inlet suction hood; 13. an outlet air suction hood; 14. a fan; 15. an acidification tank; 16. a folding cover plate; 17. a second circulation pump; 18. an acid feed pump; 19. an acid feed tank; 20. a transparent window; 21. a drive wheel; 22. a guide wheel; 23. a bearing; 24. a step shaft; 25. a positioning washer; 26. a gasket; 27. a pin; 28. a support; 29. a bearing; 30. a step shaft; 31. a positioning washer; 32. a gasket; 33. a pin; 34. a support; 35. a glass side door; 36. a tow inlet end face; 37. a tow outlet end face; 38. a glass side door; 39. a tow inlet end face; 40. a tow outlet end face; 41. a cylinder; 42. a cylinder rod; 43. a roller bearing seat; 44. a waist-shaped hole; 45. a waist-shaped hole; 46. a bolt; 47. a bolt; 48. a bolt; 49. a bolt; 50. bearing frame bottom plate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Comparative example 1: in the industrial production of the surface treatment of the 250-ply 12K carbon fiber, a commonly used carbon fiber surface treatment apparatus is used. Each strand is 0.007 m in width, the space between two adjacent carbon fiber strands is 0.005 m, the width of the electrolytic cell is 3.04 m, and the length of the electrolytic cell is 15 m. The distance between the first dipping roller and the second dipping roller can not be adjusted, an inlet air suction hood is not arranged above the first conductive roller and the first dipping roller at the inlet of the electrolytic bath, and an outlet air suction hood is not arranged above the second conductive roller and the second dipping roller at the outlet of the electrolytic bath. The electrolytic cell is also not provided with a cover plate. The conventional carbon fiber surface treatment apparatus is not provided with an acidification tank with a cover plate.
When the common carbon fiber surface treatment device operates, the direct current power supply voltage is 12V. The first conductive anode roller and the second conductive anode roller are connected with the positive pole of a direct current power supply, and the graphite cathode plate is connected with the negative pole of the direct current power supply. An aqueous solution of ammonium bicarbonate with a concentration of 10% was added to the cell.
The running speed of the carbon fiber is 6.8 m/min, and the electrolysis time is 120 seconds. And the tows at the outlet of the high-temperature carbonization furnace sequentially pass through a first conductive roller, a first impregnation roller, a second impregnation roller and a second conductive roller of the electrolytic tank by a vertical five-roller tractor to perform carbon fiber anode surface treatment. And (3) carrying out water washing, sizing, drying and winding on the carbon fiber after surface treatment to obtain the 12K carbon fiber.
Example 1 surface treatment industrial production of 250-ply 12K carbon fiber was carried out using the carbon fiber anodizing surface treatment apparatus and surface treatment method proposed by the present invention.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a carbon fiber anodizing surface treatment apparatus and a surface treatment method according to the present invention. As can be seen from the figure, the carbon fiber anodic oxidation surface treatment device and the surface treatment method comprise an electrolysis unit for carbon fiber anodic oxidation surface treatment and an electrolyzed waste gas treatment unit. Specifically, the electrolytic device for carbon fiber anodic oxidation surface treatment comprises an electrolyte feeding tank 1, an electrolyte feeding pump 2, an electrolytic tank 3, a direct current power supply 4, a first conductive anode roller 5, a first dipping roller 6, a second dipping roller 7, a second conductive anode roller 8, a graphite cathode plate 9, a first circulating pump 10, a movable cover plate 11, an inlet air suction cover 12 and an outlet air suction cover 13. The electrolytic waste gas treatment device comprises a fan 14, an acidification tank 15, a folding cover plate 16, a second circulating pump 17, an acid feeding pump 18 and an acid feeding tank 19.
Running 250 strands of 12K carbon fiber tow each having a tow width W in an electrolytic cell20.007 m, the spacing W between two adjacent carbon fiber tows30.005 m, width W of the cell13.20 m, length L of the cell120.81 m.
The first conductive anode roller 5 and the second conductive anode roller 8 are made of 304 stainless steel. The first conductive anode roller 5 and the second conductive anode roller 8 are connected with the anode of the direct current power supply 4, and the graphite cathode plate 9 is connected with the cathode of the direct current power supply 4. The first impregnation roller 6 and the second impregnation roller 7 are both rubber rollers and serve as insulation guide driven rollers. The first impregnation roller 6 and the second impregnation roller 7 introduce the carbon fiber tow into the electrolyte for impregnation.
The first impregnation roller 6 and the second impregnation roller 7 are respectively arranged on a roller bearing seat 43, and a waist-shaped hole 44 and a waist-shaped hole 45 are respectively arranged on two sides of the roller bearing seat 43 and can horizontally move left and right. First dip roll diameter D10.275 m, second Dip roll diameter D20.275 m, the maximum adjustable distance for the left-right horizontal movement of the first dipping roller is 0.55 m, and the maximum adjustable distance for the left-right horizontal movement of the second dipping roller is 0.55 m. The distance L between the end surface of the filament bundle outlet of the inlet air suction cover and the end surface of the filament bundle inlet of the outlet air suction cover416 meters. Adjusting the maximum spacing L between the first and second impregnation rollers by moving the horizontal positions of the first and second impregnation rollers217.375 m.
The movable cover plate 11 is a push-and-pull cover plate arranged on the electrolytic bath 3 and used for preventing waste gas from overflowing. The movable cover plate 11 is 16 cover plates which are mutually connected and provided with rollers, a cover plate frame is made of stainless steel, two transparent windows 20 made of colorless transparent organic glass are arranged on each cover plate, and the periphery of each transparent window 20 is coated with a rubber sealing strip. Four rollers are fixedly arranged at the front end and the rear end of each cover plate, and when the cover plates move on the sliding track, the front end and the rear end are respectively provided with a rollerThe two driving wheels 21 at the outer sides of the ends play a sliding role, and the two guide wheels 22 at the middle play a fixed guide role. A bearing 23 of the driving wheel 21 is sleeved on the step shaft 24, a positioning washer 25 and a washer 26 are respectively added at two ends of the bearing 23 to fix the position of the bearing 23, and a pin 27 is used for fixing the step shaft 24. The bearing seat of the driving wheel 21 is arranged on a bracket 28, and the base of the bracket 28 is parallel to the end surface of the bearing 23. A bearing 29 of the guide wheel 22 is sleeved on a step shaft 30, positioning washers 31 and 32 are respectively added at two ends of the bearing 29 to fix the position of the bearing 29, and a pin 33 fixes the step shaft 30. The bearing seat of the guide wheel 22 is arranged on a bracket 34, and the base of the bracket 34 is vertical to the end surface of the bearing 29. The distance L between the tow outlet end face 37 of the inlet suction hood 12 and the tow inlet end face 39 of the outlet suction hood 13416 m; similarly, the distance between the tow inlet end surface 36 of the inlet suction hood 12 and the tow outlet end surface 40 of the outlet suction hood 13 is also L416 meters. Length L of each cover plate31 meter. Width W of each cover plate43.20 m.
An inlet suction hood 12 is fixedly arranged at the inlet of the electrolytic bath 3 and is arranged above the first conductive anode roller 5 and the first dipping roller 6. Two sides of the inlet air suction hood 12 are respectively provided with a glass side door 35 which can be opened up and down, so that the wire threading production operation is convenient. First conductive anode roller 5 roller diameter D30.275 m, first dip roll 6 roll diameter D10.275 m, the distance L between the first conductive anode roll 5 and the first impregnation roll 651.375 m. Length L of inlet draft hood 1262.41 m, width W of inlet draft hood 1253.20 m.
An outlet suction hood 13 is fixedly arranged at the outlet of the electrolytic bath 3 and is arranged above the second conductive anode roller 8 and the second dipping roller 7. Two sides of the outlet air suction hood 13 are respectively provided with a glass side door 38 which can be opened up and down, so that the wire threading production operation is convenient. Second conductive anode roller 8 roller diameter D40.275 m, second impregnation roll 7 roll diameter D20.275 m, the distance L between the second conductive anode roller 8 and the second dipping roller 771.375 m. Length L of outlet air draft hood 1382.41 m, width W of outlet air draft hood 1363.20 m.
The folding cover plate 16 is arranged on the acidification tank 15 and can be folded and pulled to block the overflow of waste gas. The cover plates are connected through hinges, opening and closing operations are carried out through an external air cylinder, the air cylinder 41 is arranged on the inner side of each cover plate, the air cylinder rod 42 is arranged on the outer side of each cover plate, and the air cylinder 41 is driven to open and close through an air cylinder electromagnetic valve.
The running wire speed of the carbon fiber is 6.8 m/min, and the electrolysis time is 153 s. Firstly, bolts 46 and 47 on two sides of a bottom plate of a roller bearing seat 43 are loosened, a first impregnation roller 6 and a second impregnation roller 7 are respectively installed on the roller bearing seat 43, two sides of the roller bearing seat 43 are respectively provided with a waist-shaped hole 44 and a waist-shaped hole 45, and the bolts are installed in the waist-shaped hole 44 and the waist-shaped hole 45 of the roller bearing seat 43. And moving the horizontal positions of the first impregnation roller 6 and the second impregnation roller 7 left and right to determine the installation positions of bolts 48 and bolts 49 in the kidney-shaped holes 44 and the kidney-shaped holes 45, tightening the bolts 48 and the bolts 49, tightening the bolts 46 and the bolts 47 on the two sides of the roller bearing seat base plate 50, and fixing the position of the roller bearing seat.
Then each cover plate of the movable cover plate 11 is pushed left and right, and the length L of each cover plate31.0 m, width W43.20 m. The outer sides of the front end and the rear end of each cover plate are provided with 2 driving wheels 21, and the middle of each cover plate is provided with 2 guide wheels 22. The driving wheel 21 acts as a sliding cover and the guide wheel 22 acts as a fixed guide ensuring that each cover moves horizontally along the sliding track. The tow outlet end face 37 of the inlet suction hood 12 is covered by 16 cover plates which are connected to one another and are equipped with rollers, up to the groove face between the tow inlet end face 39 of the outlet suction hood 13.
The glass side door 35 on the two sides of the inlet air suction cover 12 and the glass side door 38 on the two sides of the outlet air suction cover 13 are closed, the valve at the bottom of the electrolyte feeding tank 1 is opened, the electrolyte feeding pump 2 is opened, ammonium bicarbonate water solution with the concentration of 10% is added into the electrolytic tank 3, the electrolyte feeding pump 2 is closed when the ammonium bicarbonate water solution liquid level in the electrolytic tank 3 reaches 80% of the depth of the electrolytic tank 3, and the first circulating pump 10 is opened. The control button of the air cylinder 41 of the acidification tank 15 is opened, the air cylinder rod 42 is lowered, and the folding cover plate 16 is closed. A7% nitric acid solution was added to the acid feed tank 19, and the valve at the bottom of the acid feed tank 19 was opened to turn on the acid feed pump 18. Adding a 7% nitric acid solution into the acidification tank 15, closing the acid feeding pump 18 when the liquid level of the nitric acid solution reaches 80% of the depth of the acidification tank 15, starting the second circulating pump 17, starting the fan 14, and pumping the waste gas escaping from the electrolytic tank 3 by the inlet suction hood 12 and the outlet suction hood 13 of the electrolytic tank 3 into the acidification tank 15.
After the preparation work of starting operation is done, production operation is started, the glass side doors 35 at two sides of the inlet air suction hood 12 and the glass side doors 38 at two sides of the outlet air suction hood 13 are opened, every two adjacent cover plates of the movable cover plate 11 move towards two sides, and the upper part of the electrolytic cell is in an open state. The carbon fiber tows at the outlet of the high-temperature carbonization furnace pass through a vertical five-roller tractor, and then pass through a first conductive anode roller 5, a first impregnation roller 6, a second impregnation roller 7 and a second conductive anode roller 8 in sequence. Then, the glass side doors 35 at both sides of the inlet air draft hood 12 and the glass side doors 38 at both sides of the outlet air draft hood 13 are closed, and every two adjacent cover plates of the movable cover plate 11 move towards the middle, so that the upper part of the electrolytic cell is in a closed state.
The first conductive anode roller 5 and the second conductive anode roller 8 are connected with the anode of the direct current power supply 4, and the graphite cathode plate 9 is connected with the cathode of the direct current power supply 4. And connecting a direct current power supply and controlling the voltage of the direct current power supply to be 12V. When the carbon fiber tows run in the electrolytic cell, the conductivity of the electrolyte in the electrolytic cell 3 is monitored to be 98 +/-2 mu s/cm. When the conductivity is lower than 96 mu s/cm, the electrolyte feeding pump 2 is started to supplement the ammonium bicarbonate water solution with the concentration of 10 percent. When the conductivity is higher than 100. mu.s/cm, the electrolyte feed pump 2 is turned off.
When the carbon fiber production is in operation, the pH value of the solution in the acidification tank 15 is monitored to be less than or equal to 7, when the pH value is greater than 7, the acid feeding pump 18 is started, the replenishing feeding pump replenishes 7% nitric acid solution and feeds the solution into the acidification tank 15, and when the pH value of the solution in the acidification tank 15 is less than or equal to 7, the acid feeding pump 18 is closed.
During the anodic oxidation surface treatment process of the carbon fiber, waste gas such as ammonia gas and carbon dioxide escaped from the electrolytic cell 3 is sealed in the electrolytic cell 3 by the movable cover plate 11, and simultaneously, the waste gas is timely extracted into the acidification tank 15 by opening the fan 14 and the inlet suction hood 12 and the outlet suction hood 13 of the electrolytic cell 3, so that the waste gas is prevented from escaping into the operation environment.
And the tows at the outlet of the second conductive anode roller 8 are subjected to the production procedures of washing, sizing, drying and winding to obtain the 12K carbon fiber.
Embodiments 2-6, the carbon fiber anodic oxidation surface treatment device and the surface treatment method provided by the invention are used for carrying out surface treatment industrial production of carbon fibers with different strand numbers and different K numbers. The carbon fiber surface treatment anodizing surface treatment device and method are the same as in embodiment 1, wherein the width and length of the electrolytic bath of the carbon fiber surface treatment anodizing surface treatment device, the adjustable maximum distance of the kidney-shaped holes, the distance between the end surface of the tows of the inlet suction hood and the end surface of the tows of the outlet suction hood, the maximum distance between the first impregnation roller and the second impregnation roller, the length and width of the movable cover plate, the number of the movable cover plates, the roller diameter of the first conductive anode roller, the roller diameter of the first impregnation roller, the distance between the first conductive anode roller and the first impregnation roller, the roller diameter of the second conductive anode roller, the roller diameter of the second impregnation roller, the distance between the second conductive anode roller and the second impregnation roller, the length and width of the inlet suction hood, the length and width of the outlet suction hood, and process parameters of voltage, the name and concentration of electrolyte, and the type and concentration of acid, The effect after the implementation is different from that of the embodiment 1.
The width and length of the carbon fiber anodizing surface treatment electrolyzer are shown in Table 1. The main equipment parameters for the adjustable spacing between the dip rolls and the moving cover are given in table 2. The main equipment parameters of the first conductive anode roll, the first impregnation roll and the inlet suction hood are shown in table 3. The main equipment parameters of the second conductive anode roll, the second impregnation roll and the outlet suction hood are shown in table 4. The main process parameters and the effects after implementation of the carbon fiber anodizing surface treatment device in the use process are shown in table 5.
TABLE 1 Width and Length of electrolytic device for carbon fiber anodizing surface treatment
TABLE 2 Adjustable spacing between Dip Rollers and Main Equipment parameters for Movable cover plates
TABLE 3 main equipment parameters of the first conductive anodic roll, the first impregnation roll and the inlet suction hood
TABLE 4 main equipment parameters of the second conductive anode roll, the second impregnation roll and the outlet suction hood
TABLE 5 carbon fiber anodizing surface treatment device in use process main process parameters and effect after implementation
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A carbon fiber anodic oxidation surface treatment device is characterized in that: the device comprises an electrolysis unit and an exhaust gas treatment unit;
the electrolytic unit comprises an electrolyte feeding tank (1), an electrolyte feeding pump (2), an electrolytic tank (3), a direct-current power supply (4), a first conductive anode roller (5), a first impregnation roller (6), a second impregnation roller (7), a second conductive anode roller (8), a graphite cathode plate (9), a first circulating pump (10), a movable cover plate (11), an inlet air suction cover (12) and an outlet air suction cover (13);
the electrolyte feeding tank (1) supplies electrolyte to the electrolytic tank (3) through the electrolyte feeding pump (2); the electrolytic tank (3) enables the electrode solution in the electrolytic tank to circularly flow through a first circulating pump (10); the first conductive anode roller (5), the first dipping roller (6), the second dipping roller (7), the second conductive anode roller (8) and the graphite cathode plate (9) are arranged in the electrolytic bath (3), and the first dipping roller (6), the second dipping roller (7) and the graphite cathode plate (9) are dipped in electrolyte; the first conductive anode roller (5), the first soaking roller (6), the second soaking roller (7) and the second conductive anode roller (8) are sequentially connected from a feed inlet to a discharge outlet of the electrolytic tank (3) in a transmission manner so as to convey and immerse carbon fibers; the direct current power supply (4) is electrically connected with the first conductive anode roller (5), the second conductive anode roller (8) and the graphite cathode plate (9) for supplying power; an inlet air suction cover (12) is arranged at the top of the side of a feeding opening of the electrolytic bath (3), an outlet air suction cover (13) is arranged at the top of the side of a discharging opening of the electrolytic bath (3), and the movable cover plate (11) is arranged between the inlet air suction cover (12) and the outlet air suction cover (13);
the electrolyzed waste gas treatment unit comprises a fan (14), an acidification tank (15), a folding cover plate (16), a second circulating pump (17), an acid feeding pump (18) and an acid feeding tank (19);
the folding cover plate (16) is arranged on the top surface of the acidification tank (15); the upstream of the fan (14) is communicated with the air holes of an inlet air suction hood (12) and an outlet air suction hood (13) above the electrolytic cell (3), and the downstream of the fan (14) is introduced into an acidification tank (15); the acid feeding tank (19) feeds acid into the acidification tank (15) through an acid feeding pump (18); the second circulating pump (17) is communicated with the bottom wall and the side wall of the acidification tank (15) to realize acid circulation in the acidification tank.
2. The apparatus of claim 1, wherein: carbon fiber tow operating in an electrolytic cell (3)N1Width W of strand, each strand2Spacing W between two adjacent carbon fiber tows3Width W of the electrolytic cell1Is W1＝N1*W2+(N1+40)*W3Length L of the electrolytic cell1Is L1＝L4+L6+L8。
3. The apparatus of claim 1, wherein: two ends of the first impregnation roller (6) and the second impregnation roller (7) are arranged on the wall of the electrolytic tank (3) through roller bearing blocks (43), and two sides of each roller bearing block (43) are respectively provided with a waist-shaped hole (44/45) so as to enable the rollers to horizontally move left and right for positioning; the maximum distance of the first dipping roller (6) which can be horizontally moved left and right is the roller diameter D of the first dipping roller (6)1Twice of the first dipping roll (7), the maximum distance of the second dipping roll (7) which can be adjusted horizontally is the roll diameter D of the second dipping roll (7)2Twice as much; by moving the horizontal position of the first impregnation roller (6) and the second impregnation roller (7), the maximum distance L between the first impregnation roller (6) and the second impregnation roller (7) is adjusted2Is L2＝L4+5*D2Thereby controlling the electrolysis time of the carbon fiber tows in the electrolytic tank (3).
4. The apparatus of claim 1, wherein: portable apron (11) include N2 single apron, apron frame and slip track, and every single apron includes transparent window (20), and both ends set up drive wheel (21) and leading wheel (22) around every single apron, single apron slides on the slip track through drive wheel (21) and leading wheel (22) at both ends.
5. The apparatus of claim 1, wherein: the inlet air draft hood (12) is fixedly arranged right above the first conductive anode roller (5) and the first dipping roller (6) at the feed inlet of the electrolytic bath (3); two sides of the inlet air suction hood (12) are respectively provided with a glass side door (35) which can be opened up and down, so that the wire threading production operation is convenient; the width of the inlet air suction hood (12) is the same as that of the electrolytic bath (3).
6. The apparatus of claim 1, wherein: the outlet air suction hood (13) is fixedly arranged right above the second conductive anode roller (8) and the second dipping roller (7) at the discharge outlet of the electrolytic bath (3); two sides of the outlet air suction hood (13) are respectively provided with a glass side door (38) which can be opened up and down, so that the wire threading production operation is convenient; the width of the outlet air suction hood (13) is the same as that of the electrolytic bath (3).
7. The apparatus of claim 1, wherein: the foldable cover plate (16) is hinged to each other, an air cylinder (41) is arranged on the inner side of the cover plate, an air cylinder rod (42) is arranged on the outer side of the cover plate, and the air cylinder (41) is driven to open and close through an air cylinder electromagnetic valve.
8. The apparatus of claim 1, wherein: the acid used in the acidification tank (15) is hydrochloric acid, sulfuric acid, nitric acid, acetic acid or phosphoric acid, and the concentration of the acid is 1-15%.
9. The apparatus of claim 1, wherein: and a PH detector and a liquid level meter are arranged in the acidification tank (15), the PH value and the liquid level height of the solution in the acidification tank (15) are controlled, and the PH value of the solution is controlled to be less than or equal to 7.
10. A method for surface treating carbon fibres using a device according to any one of claims 1 to 9, characterised in that the method comprises the steps of:
s1, preparing before operation, closing glass side doors (35) on two sides of an inlet air suction cover (12) and glass side doors (38) on two sides of an outlet air suction cover (13), opening a bottom valve of an electrolyte feeding tank (1), starting an electrolyte feeding pump (2), adding ammonium bicarbonate aqueous solution with the concentration of 10% into an electrolytic tank (3), and when the liquid level of the ammonium bicarbonate aqueous solution in the electrolytic tank (3) reaches 80% of the depth of the electrolytic tank (3), closing the electrolyte feeding pump (2) and starting a first circulating pump (10); starting a control button of an air cylinder (41) of the acidification tank (15), lowering an air cylinder rod (42), and closing the folding cover plate (16); adding a 7% nitric acid solution into an acid feeding tank (19), opening a valve at the bottom of the acid feeding tank (19), starting an acid feeding pump (18), adding the 7% nitric acid solution into an acidification tank (15), closing the acid feeding pump (18) when the liquid level of the nitric acid solution reaches 80% of the depth of the acidification tank (15), starting a second circulating pump (17), starting a fan (14), and pumping the waste gas escaping from the electrolysis tank (3) by an inlet suction hood (12) and an outlet suction hood (13) of the electrolysis tank (3) and introducing the waste gas into the acidification tank (15);
s2, starting production operation, firstly opening glass side doors (35) on two sides of an inlet air suction cover (12) and glass side doors (38) on two sides of an outlet air suction cover (13), and moving every two adjacent single cover plates of a movable cover plate (11) to two sides to enable the upper part of an electrolytic cell (3) to be in an open state; the carbon fiber tows at the outlet of the high-temperature carbonization furnace pass through a vertical five-roller tractor, and then pass through a first conductive anode roller (5), a first impregnation roller (6), a second impregnation roller (7) and a second conductive anode roller (8) in sequence; then, closing glass side doors (35) at two sides of the inlet air suction cover (12) and glass side doors (38) at two sides of the outlet air suction cover (13), and moving the cover plate (11) to enable the upper part of the electrolytic cell (3) to be in a closed state;
s3, connecting and conducting the first conductive anode roller (5), the second conductive anode roller (8) and the graphite cathode plate (9) with a direct current power supply (4) to control the voltage of the direct current power supply to be 12V; when the carbon fiber tows run in the electrolytic tank (3), monitoring the conductivity of the electrolyte in the electrolytic tank (3) to be 98 +/-2 mu s/cm, and monitoring the PH value of the solution in the acidification tank (15) to be less than or equal to 7;
and (3) carrying out water washing, sizing, drying and winding on tows at the outlet of the S4 second conductive anode roller (8) to obtain the 12K carbon fiber.
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| JP2014118659A (en) * | 2012-12-18 | 2014-06-30 | Toho Tenax Co Ltd | Surface treatment apparatus of carbon fiber bundle and surface treatment method of carbon fiber bundle |
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