CN102643515B - A kind of Low-resistivity composite conductive plate and preparation method thereof - Google Patents
A kind of Low-resistivity composite conductive plate and preparation method thereof Download PDFInfo
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- CN102643515B CN102643515B CN201210122136.0A CN201210122136A CN102643515B CN 102643515 B CN102643515 B CN 102643515B CN 201210122136 A CN201210122136 A CN 201210122136A CN 102643515 B CN102643515 B CN 102643515B
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- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 42
- 239000010439 graphite Substances 0.000 claims abstract description 42
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000011231 conductive filler Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 22
- 229910017052 cobalt Inorganic materials 0.000 claims description 11
- 239000010941 cobalt Substances 0.000 claims description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 11
- 239000000428 dust Substances 0.000 claims description 10
- 150000001412 amines Chemical class 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 4
- 150000008065 acid anhydrides Chemical class 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 150000003254 radicals Chemical class 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims 1
- 239000003822 epoxy resin Substances 0.000 abstract description 12
- 229920000647 polyepoxide Polymers 0.000 abstract description 12
- 239000004593 Epoxy Substances 0.000 abstract description 10
- 150000002148 esters Chemical class 0.000 abstract description 10
- 239000004809 Teflon Substances 0.000 abstract 1
- 229920006362 Teflon® Polymers 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- FDPIMTJIUBPUKL-UHFFFAOYSA-N dimethylacetone Natural products CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 8
- XXQBEVHPUKOQEO-UHFFFAOYSA-N potassium peroxide Inorganic materials [K+].[K+].[O-][O-] XXQBEVHPUKOQEO-UHFFFAOYSA-N 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 7
- 239000003610 charcoal Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- -1 polyethylene Polymers 0.000 description 4
- XLBBTYDQUXXDKT-UHFFFAOYSA-N C(C)C(=O)CC.[O-2].[K+].[K+] Chemical compound C(C)C(=O)CC.[O-2].[K+].[K+] XLBBTYDQUXXDKT-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 229920006387 Vinylite Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229920003180 amino resin Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention provides a kind of Low-resistivity composite conductive plate and preparation method thereof.The mass percentage of the raw material of Low-resistivity composite conductive plate of the present invention consists of: epoxy resin or epoxy vingl ester resin 20% ~ 80%, solidifying agent 0.5% ~ 60%, promotor 0% ~ 5%, conductive filler material 5% ~ 50%, graphite felt 1% ~ 60%.The preparation method of Low-resistivity composite conductive plate of the present invention comprises step: by epoxy vingl ester resin or epoxy resin and conductive carbon powder mixing, ultrasonic, dispersed with stirring even, and vacuum exhaust, obtains mixing liquid X; In mixing liquid X, add solidifying agent and promotor, obtain mixing liquid Y, then graphite felt is immersed in mixing liquid Y, put into vacuum chamber and be vented; Then the graphite felt of having flooded is taken out and put into Teflon mould, curing molding, the demoulding.The composite conductive plate resistivity adopting the present invention to prepare is low, leakage resistance good, physical strength is high, acid-alkali-corrosive-resisting, scale resistance are good, and production technique is simple, and cost is low.
Description
Technical field
The invention belongs to flow battery electrode field of material technology, be specifically related to a kind of Low-resistivity composite conductive plate and preparation method thereof.
Background technology
At present, the composite conductive plate of domestic and international research report is all generally use to make as the thermosetting resines such as thermoplastics and resol, aminoresin, epoxy resin such as polyethylene (PE), polypropylene (PP), PS add the conductive filler material such as conductive carbon powder or Graphite Powder 99, the main extruding contact relying on the material such as carbon dust or Graphite Powder 99 of conduction, resistivity is generally all at 0.1 more than Ω cm.A kind of low-resistance conductive plastic plate resistivity of patent CN101150192 report is greater than 1 Ω cm.The compound conductive plastic plate preparation process of patent CN101525468 report needs vitriol oil pyroprocessing, complex process and conducting plates easy to leak, difficult quality guarantee.
Conducting plates resistivity is comparatively large, and being applied to flow battery can reduce product electrical property greatly, causes that flow battery power is low, cell power cost is high.Conducting plates, as an assembly of product, from cost angle, needs technique simple, is convenient to go into operation.Therefore, find another low-resistivity, an important subject that the simple composite conductive plate preparation method of technique has become flow battery field.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of Low-resistivity composite conductive plate, and another technical problem that the present invention will solve is to provide a kind of preparation method of Low-resistivity composite conductive plate.
Low-resistivity composite conductive plate of the present invention, the mass percent of its raw material consists of:
Epoxy resin or epoxy vingl ester resin 20% ~ 80%
Solidifying agent 0.5% ~ 60%
Promotor 0% ~ 5%
Conductive filler material 5% ~ 50%
Graphite felt 1% ~ 60%.
The thickness of the Low-resistivity composite conductive plate in the present invention is 0.1 ~ 10mm, and resistivity is less than 1 Ω cm.
The solidifying agent of the Low-resistivity composite conductive plate in the present invention is that amine curing agent, modified amine curing agent, acid anhydride type curing agent or free radical cause class solidifying agent.
The promotor of the Low-resistivity composite conductive plate in the present invention is amine type accelerator or cobalt iso-octoate promotor.
The conductive filler material of the Low-resistivity composite conductive plate in the present invention is one or more in conductive carbon fibre, carbon dust, Graphite Powder 99, metal-powder, and the resistivity of conducting plates is less than 100 Ω cm.
The graphite felt of the Low-resistivity composite conductive plate in the present invention adopts the network-like material of Carbon fibe to make, and plate thickness is 0.5mm-10mm, and resistivity is less than 10 Ω cm.
The preparation method of Low-resistivity composite conductive plate of the present invention, comprises the following steps:
A) by liquid macroimolecule resin and conductive filler material mixing, ultrasonic, dispersed with stirring is even, obtains mixing liquid X;
B) mixing liquid X is got rid of in vacuum chamber the gas in liquid;
C) in mixing liquid X, add certain proportion solidifying agent, stir evenly, obtain mixing liquid Y;
D) the certain thickness graphite felt of cutting out is immersed in mixing liquid Y, put into vacuum chamber, mixing liquid Y is fully immersed in graphite felt;
E) take out the graphite felt after infiltrating, put into forming mould and flatten, liquid Y curing and demolding to be mixed, namely obtains Low-resistivity composite conductive plate.
Conductive filler material in above-mentioned steps a is one or more in conductive carbon fibre, carbon dust, Graphite Powder 99, metal-powder, and the resistivity of conducting plates is less than 100 Ω cm.
Graphite felt in above-mentioned steps d adopts the network-like material of Carbon fibe to make, and plate thickness is 0.5mm-10mm, and resistivity is less than 10 Ω cm.
Instant invention overcomes the outstanding shortcomings such as the large and difficult quality guarantee of prior art processes complexity, resistivity, with charcoal felt or graphite felt for conductive network skeleton, prepare a kind of Low-resistivity composite conductive plate.Resistivity is less than 0.02 Ω cm, reduces by 1 ~ 2 order of magnitude than current conductive plastic plate.
The invention has the beneficial effects as follows: (1) adopts formed at normal temp mode, and preparation technology is simple; (2) adopt wireless network to run through electrical conduction model, conduct electricity very well, be beneficial to and reduce cell power battery cost; (3) adopt one-shaping technique, reliability is high.
Low-resistivity composite conductive plate of the present invention shows good resistance to oxidation, the electrolytic corrosion of resistance to strongly-acid performance in laboratory experiment, and work-ing life is more than 200% of graphite cake, and in battery uses, maximum charging and discharging currents density can reach 180mAcm
-2, be conductive plastic plate more than 200%, physical strength is 10 times of graphite cake, has broad application prospects.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
Composite conducting board forming die is made with polytetrafluoroethylmaterial material, the 615A epoxy resin that epoxy resin adopts Wuxi blue star resin processing plant to produce, 593 modified amine curing agents that solidifying agent adopts Wuxi blue star resin processing plant to produce, the extraordinary conductive carbon powder that conductive filler material adopts Nantong Yong Tong Environmental Protection Technology Co., Ltd to produce, the graphite felt that graphite felt adopts Lanzhou carbon composite factory to produce, prepare Low-resistivity composite conductive plate through following technique:
At (1) 20 DEG C, by 615A epoxy resin and conductive carbon powder, in the mixing of 10:1 ratio, the mode combined by ultrasonic wave and stirring, is made carbon dust be uniformly dispersed, obtains mixing liquid X;
(2) mixing liquid X is got rid of in vacuum chamber the gas in liquid, vacuum tightness, at 10Pa ~ 1000Pa pressurize 10min, is then taken out;
(3) in mixing liquid X, add 593 solidifying agent (mass ratio 615A:593=4:1), stir evenly, obtain mixing liquid Y
(4) graphite felt is immersed in mixing liquid Y, put into vacuum chamber, keep vacuum tightness at 10Pa ~ 1000Pa pressurize 10min, make mixing liquid Y fully immerse in graphite felt hole;
(5) take out the graphite felt infiltrated, put into forming mould, keep 10Mpa10h, treat Y curing and demolding, namely obtain Low-resistivity composite conductive plate.
Embodiment 2
Mould is made into polytetrafluoroethylmaterial material, the E51 epoxy resin that epoxy resin adopts Wuxi blue star resin processing plant to produce, 593 modified amine curing agents that solidifying agent adopts Wuxi blue star resin processing plant to produce, the extraordinary conductive carbon powder that conductive filler material adopts Nantong Yong Tong Environmental Protection Technology Co., Ltd to produce, the graphite felt that graphite felt adopts Lanzhou carbon composite factory to produce, prepare Low-resistivity composite conductive plate through following technique:
At (1) 20 DEG C, by E51 epoxy resin and conductive carbon powder, in the mixing of 10:1 ratio, the mode combined by ultrasonic wave and stirring, is made carbon dust be uniformly dispersed, obtains mixing liquid X;
(2) mixing liquid X is got rid of in vacuum chamber the gas in liquid, vacuum tightness, at 10Pa ~ 1000Pa pressurize 15min, is then taken out;
(3) in mixing liquid X, add 593 solidifying agent (mass ratio E51:593=4.5:1), stir evenly, obtain mixing liquid Y;
(4) charcoal felt is immersed in mixing liquid Y, put into vacuum chamber, keep vacuum tightness at 10Pa ~ 1000Pa pressurize 15min, make mixing liquid Y fully immerse in charcoal felt hole;
(5) take out the charcoal felt infiltrated, put into forming mould, 10Mpa pressure keeps 12h, treats Y curing and demolding, namely obtains Low-resistivity composite conductive plate.
Embodiment 3
Composite conducting board forming die is made with polytetrafluoroethylmaterial material, with E51 epoxy resin (Wuxi blue star resin processing plant), 334 solidifying agent (Wuxi blue star resin processing plant), conductive carbon powder (Guangzhou Run Feng Chemical Co., Ltd.), graphite felt (Lanzhou carbon composite factory) is raw material, prepares Low-resistivity composite conductive plate through following technique:
At (1) 20 DEG C, by E51 epoxy resin and conductive carbon powder, in the mixing of 10:1 ratio, the mode combined by ultrasonic wave and stirring, is made carbon dust be uniformly dispersed, obtains mixing liquid X;
(2) mixing liquid X is got rid of in vacuum chamber the gas in liquid, vacuum tightness, at 10Pa ~ 1000Pa pressurize 15min, is then taken out;
(3) in mixing liquid X, add 593 solidifying agent (mass ratio E51:334=3.3:1), stir evenly, obtain mixing liquid Y;
(4) graphite felt is immersed in mixing liquid Y, put into vacuum chamber, keep vacuum tightness at 10Pa ~ 1000Pa pressurize 20min, make mixing liquid Y fully immerse in graphite felt hole;
(5) take out the graphite felt infiltrated, put into forming mould, keep 10Mpa15h, treat Y curing and demolding, namely obtain Low-resistivity composite conductive plate.
Embodiment 4
Composite conducting board forming die is made with polytetrafluoroethylmaterial material, the WSR-V118 epoxy vingl ester resin that epoxy vingl ester resin adopts Beijing Lanxing Chemical New Material Co., Ltd. to produce, the Potassium peroxide ethyl ketone radical type solidifying agent that solidifying agent adopts Chengdu associating chemical reagent work to produce, the content that promotor adopts Chengdu associating chemical reagent work to produce is the cobalt iso-octoate promotor of 12%, to the conductive carbon powder that some filler adopts Guangzhou Run Feng Chemical Co., Ltd. to produce, the graphite felt that graphite felt adopts Lanzhou carbon composite factory to produce, Low-resistivity composite conductive plate is prepared through following technique:
At (1) 15 DEG C, by WSR-V118 epoxy vingl ester resin and conductive carbon powder, in the mixing of 10:1 ratio, the mode combined by ultrasonic wave and stirring, is made carbon dust be uniformly dispersed, obtains mixing liquid X;
(2) mixing liquid X is got rid of in vacuum chamber the gas in liquid, vacuum tightness, at 10Pa ~ 1000Pa pressurize 5min, is then taken out;
(3) in mixing liquid X, add Potassium peroxide ethyl ketone initiator, content be 12% cobalt iso-octoate promotor (mass ratio WSR-V118: potassium oxide ethyl ketone: cobalt iso-octoate=50:1:1), stir evenly, obtain mixing liquid Y;
(4) graphite felt is immersed in mixing liquid Y, put into vacuum chamber, keep vacuum tightness at 10Pa ~ 1000Pa pressurize 10min, make mixing liquid Y fully immerse in graphite felt hole;
(5) take out the graphite felt infiltrated, put into forming mould, keep 10Mpa4h, treat Y curing and demolding, namely obtain Low-resistivity composite conductive plate.
Embodiment 5
Composite conducting board forming die is made with polytetrafluoroethylmaterial material, the V470 Vinylite that epoxy vingl ester resin adopts Jinan Yi Sheng resin processing plant to produce, the Potassium peroxide ethyl ketone radical type solidifying agent that solidifying agent adopts Chengdu associating chemical reagent work to produce, the content that promotor adopts Chengdu associating chemical reagent work to produce is the cobalt iso-octoate promotor of 12%, the conductive carbon powder that conductive filler material adopts Guangzhou Run Feng Chemical Co., Ltd. to produce, the graphite felt that graphite felt adopts Lanzhou carbon composite factory to produce, prepare Low-resistivity composite conductive plate through following technique:
At (1) 15 DEG C, by V470 Vinylite and conductive carbon powder, in the mixing of 10:1 ratio, the mode combined by ultrasonic wave and stirring, is made carbon dust be uniformly dispersed, obtains mixing liquid X;
(2) mixing liquid X is got rid of in vacuum chamber the gas in liquid, vacuum tightness, at 10Pa ~ 1000Pa pressurize 5min, is then taken out;
(3) in mixing liquid X, add Potassium peroxide ethyl ketone initiator, content be 12% cobalt iso-octoate promotor (mass ratio V470: potassium oxide ethyl ketone: cobalt iso-octoate=50:1:1), stir evenly, obtain mixing liquid Y;
(4) graphite felt is immersed in mixing liquid Y, put into vacuum chamber, keep vacuum tightness at 10Pa ~ 1000Pa pressurize 10min, make mixing liquid Y fully immerse in graphite felt hole;
(5) take out the graphite felt infiltrated, put into forming mould, keep 10Mpa4h, treat Y curing and demolding, namely obtain Low-resistivity composite conductive plate.
Embodiment 6
Composite conducting board forming die is made with polytetrafluoroethylmaterial material, 881 epoxy vingl ester resins that epoxy vingl ester resin adopts Shanghai Fu Chen Chemical Co., Ltd. to produce, the methylethyl ketone peroxide radical type solidifying agent that solidifying agent adopts Shanghai Fu Chen Chemical Co., Ltd. to produce, the content that promotor adopts Shanghai Fu Chen Chemical Co., Ltd. to produce is the cobalt iso-octoate promotor of 12%, the conductive carbon powder that conductive filler material adopts Guangzhou Run Feng Chemical Co., Ltd. to produce, the graphite felt that graphite felt adopts Lanzhou carbon composite factory to produce, Low-resistivity composite conductive plate is prepared through following technique:
At (1) 15 DEG C, by 881 epoxy vingl ester resins and conductive carbon powder, in the mixing of 10:1 ratio, the mode combined by ultrasonic wave and stirring, is made carbon dust be uniformly dispersed, obtains mixing liquid X;
(2) mixing liquid X is got rid of in vacuum chamber the gas in liquid, vacuum tightness, at 10Pa ~ 1000Pa pressurize 5min, is then taken out;
(3) in mixing liquid X, add Potassium peroxide ethyl ketone initiator, content be 12% cobalt iso-octoate promotor (mass ratio 881: potassium oxide ethyl ketone: cobalt iso-octoate=66:1:1), stir evenly, obtain mixing liquid Y;
(4) graphite felt is immersed in mixing liquid Y, put into vacuum chamber, keep vacuum tightness at 10Pa ~ 1000Pa pressurize 10min, make mixing liquid Y fully immerse in graphite felt hole;
(5) take out the graphite felt infiltrated, put into forming mould, keep 10Mpa4h, treat Y curing and demolding, namely obtain Low-resistivity composite conductive plate.
Embodiment 7
Other content of the present embodiment is identical with embodiment 6, and its difference is that the extraordinary conductive carbon powder of conductive filler material wherein adopts metal-powder to substitute.
Embodiment 8
Other content of the present embodiment is identical with embodiment 3, and its difference is that curing agent modified amine curing agent wherein adopts acid anhydride type curing agent to substitute.
Claims (1)
1. a Low-resistivity composite conductive plate, is characterized in that: the mass percent of described conducting plates raw material consists of:
Described solidifying agent is that amine curing agent, acid anhydride type curing agent or free radical cause class solidifying agent;
Described promotor is amine type accelerator or cobalt iso-octoate promotor;
Described conductive filler material is one or more in conductive carbon fibre, carbon dust, Graphite Powder 99, metal-powder;
Described graphite felt adopts the network-like material of Carbon fibe to make, and plate thickness is 0.5mm ~ 10mm, and resistivity is less than 10 Ω cm;
Described Low-resistivity composite conductive plate adopts following methods preparation:
A) by liquid macroimolecule resin and conductive filler material mixing, ultrasonic, dispersed with stirring is even, obtains mixing liquid X;
B) mixing liquid X is got rid of in vacuum chamber the gas in liquid;
C) in mixing liquid X, add certain proportion solidifying agent, promotor, stir evenly, obtain mixing liquid Y;
D) the certain thickness graphite felt of cutting out is immersed in mixing liquid Y, put into vacuum chamber, mixing liquid Y is fully immersed in graphite felt;
E) take out the graphite felt infiltrated, put into forming mould and flatten, treat Y curing and demolding, namely obtain Low-resistivity composite conductive plate.
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| CN103694640A (en) * | 2013-12-20 | 2014-04-02 | 北京郁懋科技有限责任公司 | Preparation method of conductive thermo-cured epoxy resin system |
| CN104466197B (en) * | 2014-11-28 | 2017-01-18 | 中国科学院金属研究所 | Bipolar plate for vanadium battery and preparation method of bipolar plate |
| CN105400147A (en) * | 2015-12-22 | 2016-03-16 | 合肥仲农生物科技有限公司 | Conductive polymer composite material |
| CN107785582B (en) * | 2016-08-31 | 2020-11-03 | 宁德新能源科技有限公司 | Positive electrode sheet and secondary battery |
| CN107819132A (en) * | 2017-10-09 | 2018-03-20 | 青海百能汇通新能源科技有限公司 | A kind of electrode preparation method and electrode |
| CN107987477B (en) * | 2017-12-11 | 2020-02-11 | 沈阳建筑大学 | Preparation method of graphene garland/epoxy resin composite material |
| CN109935751B (en) * | 2018-11-23 | 2022-07-19 | 万向一二三股份公司 | Battery module fixing panel and preparation method thereof |
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