CN105601968B - A kind of preparation method of polybenzimidazoles multilayer complex films used for high-temperature fuel cell - Google Patents
A kind of preparation method of polybenzimidazoles multilayer complex films used for high-temperature fuel cell Download PDFInfo
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- CN105601968B CN105601968B CN201510807407.XA CN201510807407A CN105601968B CN 105601968 B CN105601968 B CN 105601968B CN 201510807407 A CN201510807407 A CN 201510807407A CN 105601968 B CN105601968 B CN 105601968B
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- polybenzimidazoles
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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
Abstract
The invention discloses a kind of preparation methods of polybenzimidazoles multilayer complex films used for high-temperature fuel cell, polybenzimidazoles perforated inner layer is prepared by vapor induction phase separation method, polybenzimidazoles compacted zone is prepared in polybenzimidazoles perforated inner layer both sides using spray coating method, then impregnation of phosphoric acid.Polybenzimidazoles multilayer complex films prepared by the present invention, structure is uniform, it is tightly combined between layers, preparation process is simple, and the cost of material is low, suitable for anhydrous system, the high temperature proton exchange film fuel cell that 120 DEG C 200 DEG C of operating temperature, not only increases the adsorbance of phosphoric acid, and effectively increases the alcohol-rejecting ability of composite membrane, so that composite membrane has higher conductivity, the loss of phosphoric acid is greatly reduced.
Description
Technical field
The invention belongs to fuel cell material technical fields, and in particular to a kind of polybenzimidazoles used for high-temperature fuel cell is more
The preparation method of layer composite membrane.
Background technology
Proton Exchange Membrane Fuel Cells(PEMFC)Be it is a kind of efficiently, cleaning, environmental-friendly power generator, be electronic vapour
The ideal power source of vehicle can also be used as the Military Powers or portable power etc. such as dispersion power station, submarine and spacecraft, have very
Wide application prospect.However it is now widely used be withFor the perfluor type sulfonic acid membrane cell of representative, but
The proton conducting ability of this kind of proton exchange membrane is influenced very big by water content in film and temperature, and alcohol-rejecting ability is poor, the work of PEMFC
Make temperature no more than 80 DEG C.Since PEMFC is limited by operating temperature so that it faces CO tolerances in practical application
The problems such as difference, hydro-thermal difficult management of system.Therefore PEMFC running temperatures are increased to 100 DEG C or more, it can be efficiently against
The above problem of traditional Nafion bases PEMFC, the fuel cell of this type(FC)Normally referred to as high temperature proton exchange film fires
Expect battery(HT-PEMFC), it is an important developing direction of PEMFC technologies.
HT-PEMFC systems have the following advantages:1)Electrochemical reaction speed improves, and effectively reduces electrochemical cathode polarization
Overpotential allows to reduce catalyst load amount, allows to use non-platinum catalyst;2)The humidification requirements of reaction gas are reduced;3)Electricity
Pool inner water exists with gas phase simplifies hydro-thermal management;In addition, HT-PEMFC simplifies FC cooling systems to a certain extent.In view of
Development prospect tempting HT-PEMFC has carried out the development of HT-PEMFC critical materials extensively both at home and abroad, including high temperature proton is handed over
Change film, catalyst and carrier etc., and achieve preferable PRELIMINARY RESULTS, wherein high temperature proton exchange film be research hot spot it
One.
Polybenzimidazoles is concentrated mainly on for the research of HT-PEMFC proton exchange membrane at present(PBI)On, it is in 1959
Year is reported for the first time in United States Patent (USP), and Hoechst Celanese companies of the U.S. introduce PBI film products to the market within 1988.Such as
The present, PBI/ phosphoric acid is as polymer-based material the most outstanding in engineering thermoplasties, in the high temperature matter as HT-PEMFC
Huge validity and feasibility are shown in terms of proton exchange.But it is easy in cell operation after PBI impregnation of phosphoric acid
It is lost in so that the conductivity of high temperature proton exchange film drastically reduces, and the phosphoric acid being lost in causes battery apparatus seriously corroded
Battery system it is unstable.Researcher is to overcome the problems, such as this, and phosphoric acid particle is protected in doping in film, improves the adsorption potential of phosphoric acid
Point, to slow down the loss of phosphoric acid.
Invention content
In order to improve the performance of HT-PEMFC proton exchange membrane, the purpose of the present invention is to provide a kind of high-temperature fuels
The preparation method of battery polybenzimidazoles multilayer complex films.Perforated inner layer is prepared by vapor induction phase separation method, is used
Spray coating method prepares compacted zone, and impregnation of phosphoric acid in perforated inner layer both sides, to improve the use of polybenzimidazoles multilayer complex films
Performance.
To achieve the goals above, the technical solution adopted by the present invention is:
A kind of preparation method of polybenzimidazoles multilayer complex films used for high-temperature fuel cell, includes the following steps:
(1)Polybenzimidazole resin is dissolved in high boiling solvent, obtains polybenzimidazoles mold liquid, wherein polyphenyl
And the 0.2-5% that the additive amount of imidazoles resin is high boiling solvent quality;
(2)By step(1)The polybenzimidazoles mold liquid of gained pours into casting film plate, is placed in climatic chamber and carries out water
Steam induction phase separation, humidity 20%-95%(Humidification degree), temperature is 25 DEG C -120 DEG C, and constant temperature and humidity is placed 0.2-12 hours,
Polybenzimidazoles perforated inner layer is made;
(3)By step(2)Polybenzimidazoles perforated inner layer obtained takes out, and is placed in the mixed liquor of high boiling solvent and water
In, it takes out after placing 1-5h, is dried in vacuo in 25 DEG C of -150 DEG C of temperature ranges;
(4)Spray coating method is used to cause polybenzimidazoles slurry even application to prepare polybenzimidazoles in perforated inner layer both sides
Close layer is dried in vacuo in 25 DEG C of -150 DEG C of temperature ranges, polybenzimidazoles multilayer film is made, wherein the polybenzimidazoles
Slurry is polybenzimidazole resin and N-Methyl pyrrolidone(NMP)The mixed liquor of composition, polyphenyl is simultaneously in polybenzimidazoles slurry
Mass fraction shared by imidazoles resin is 0.2-5%;
(5)By step(4)Polybenzimidazoles multilayer film obtained is after impregnation of phosphoric acid is handled to get the polyphenyl and miaow
Azoles multilayer complex films.
Preferably, step(1)And step(3)In, the high boiling solvent is n,N-dimethylacetamide(DMAC)And N-
Methyl pyrrolidone(NMP)In one kind or two kinds.
Preferably, step(3)In the mixed liquor of the high boiling solvent and water, volume ratio is water:High boiling solvent=1:
0.1-1:2。
Preferably, step(2)Described in polybenzimidazoles perforated inner layer thickness be 20-120 microns, step(4)It is described
Polybenzimidazoles dense layer thickness is 5-30 microns.
Preferably, step(5)The temperature of the impregnation of phosphoric acid processing is 20 DEG C -150 DEG C, phosphoric acid concentration 50-100wt%,
Dip time is 12-100 hours.
Step(1)In, high boiling solvent is added in polybenzimidazole resin, after being sufficiently stirred dissolving, it is proposed that filtering is to remove
Decontamination.
Beneficial effects of the present invention are:
1. vapor induction phase separation method is respectively adopted in the present invention and spray coating method prepares the film layer of different structure, structure is equal
It is even, it is tightly combined between layers, preparation process is simple, and the cost of material is low, is suitable for anhydrous system, 120 DEG C of operating temperature-
200 DEG C of high temperature proton exchange film fuel cell.
2. the polybenzimidazoles multi-layer film structure that the present invention is combined using perforated inner layer with compacted zone, not only increases phosphorus
The adsorbance of acid, and effectively increase the alcohol-rejecting ability of composite membrane so that composite membrane has higher conductivity, greatly reduces
The loss of phosphoric acid.
Description of the drawings
Fig. 1 is 1 step of embodiment(4)The structural schematic diagram of the PBI multilayer films;
Fig. 2 is the comparison diagram of PBI multilayer complex films described in embodiment 1 and tradition PBI compound film battery polarization curves;
Fig. 3 is the curve graph that the conductivity of PBI multilayer complex films described in embodiment 2 varies with temperature;
Fig. 4 is the conductivity time history plot of PBI multilayer complex films described in embodiment 2.
Specific implementation mode
Below by way of preferred embodiment, the present invention is described in more detail, but protection scope of the present invention is not limited to
This.
Polybenzimidazoles employed in following embodiment(PBI)For ordinary commercial products, structural formula is:
Wherein:N is the degree of polymerization, value range 50-500.
Embodiment 1
A kind of polybenzimidazoles multilayer complex films used for high-temperature fuel cell, prepare according to the following steps:
(1)PBI is dissolved in NMP, after stirring 12 hours, 2 times is filtered to remove impurity, obtains PBI mold liquid,
In, the additive amount of PBI is the 1% of NMP mass;
(2)By step(1)The PBI mold liquid of gained pours into casting film plate, is placed in progress vapor in climatic chamber and lures
Lead phase separation, humidity 55%(Humidification degree), temperature is 80 DEG C, and constant temperature and humidity is placed 6 hours, and PBI perforated inner layers are made;
(3)By step(2)PBI perforated inner layers obtained take out, and are placed in the mixed liquor of deionized water and NMP, and it is small to place 1
When after take out, be dried in vacuo 24 hours in 100 DEG C, wherein deionized water and the volume ratio of NMP are 1:0.2;
(4)Use spray coating method by PBI slurries even application in perforated inner layer film both sides to prepare PBI compacted zones, in 150 DEG C
Vacuum drying, wherein the PBI slurries are the mixed liquor of PBI and NMP composition, and the mass fraction in PBI slurries shared by PBI is
0.5%;
The PBI multilayer films of gained, as shown in Figure 1, including perforated inner layer 1 and compacted zone 2, compacted zone 2 is combined closely in more
The both sides of hole internal layer 1,1 thickness of perforated inner layer are 30 microns, and the thickness of compacted zone 2 is 10 microns.
(5)By step(4)PBI multilayer films obtained are handled through impregnation of phosphoric acid, and the temperature of impregnation of phosphoric acid processing is 60 DEG C, phosphorus
Acid concentration is 70wt%, and dip time is 60 hours to get the PBI multilayer complex films.
In addition, preparing PBI films using solution casting method, thickness is 50 microns, and in preparation process, solvent selects NMP, PBI
Mass fraction in NMP is 1%, is then handled through impregnation of phosphoric acid with PBI films obtained, and the temperature of impregnation of phosphoric acid processing is 60
DEG C, phosphoric acid concentration 70wt%, dip time be 60 hours, obtain PBI/ phosphoric acid films, be denoted as traditional PBI composite membranes, to this
PBI multilayer complex films prepared by embodiment are compared.
Using PBI multilayer complex films made from the present embodiment and tradition PBI composite membranes, tested on monocell evaluating apparatus
Battery performance under its different temperatures.Wherein, battery cathode uses carbon(C)Carry nickel(Ni)Catalyst is uniformly mixed with PBI solution
After be applied on carbon paper be made(Using preparation method disclosed in patent CN02127802.4), Ni accounts for the quality of C/Ni catalyst
Percentage is 40%, C/Ni and the mass ratio of PBI is 1:1;Anode uses carbon(C)Carry platinum(Pt)Catalyst is mixed with PBI solution
It is applied on carbon paper and is made after closing uniformly(Using preparation method disclosed in patent CN02127802.4), Pt accounts for C/ Pt catalysis
The mass percent of agent is 70%, and Pt carrying capacity is 0.6mg/cm in anode2.Battery operating environment is respectively set as:Battery temperature is
120℃-150℃;Hydrogen and oxygen gas flow rate are respectively 50mL/min, 100 mL/min, and gas is without humidification, pressure 0.05MPa.
Test results are shown in figure 2.
Figure it is seen that PBI multilayer complex films manufactured in the present embodiment compare tradition PBI composite membranes, battery discharge
Performance significantly increases, and maximum power density is up to 1100mW/cm2。
Embodiment 2
A kind of polybenzimidazoles multilayer complex films used for high-temperature fuel cell, prepare according to the following steps:
(1)PBI is dissolved in NMP, after stirring 12 hours, 2 times is filtered to remove impurity, obtains PBI mold liquid,
In, the additive amount of PBI is the 5% of NMP mass;
(2)By step(1)The PBI mold liquid of gained pours into casting film plate, is placed in progress vapor in climatic chamber and lures
Phase separation, humidity 88% are led, temperature is 82 DEG C, and constant temperature and humidity is placed 1 hour, and PBI perforated inner layers, 1 thickness of perforated inner layer is made
It is 90 microns;
(3)By step(2)PBI perforated inner layers obtained take out, and are placed in the mixed liquor of deionized water and NMP, and it is small to place 1
When after take out, be dried in vacuo 24 hours in 100 DEG C, wherein deionized water and the volume ratio of NMP are 1:0.5;
(4)Use spray coating method by PBI slurries even application in perforated inner layer film both sides to prepare PBI compacted zones, in 150 DEG C
Vacuum drying, wherein the PBI slurries are the mixed liquor of PBI and NMP composition, and the mass fraction in PBI slurries shared by PBI is
0.5%, the thickness of compacted zone 2 is 5 microns;
(5)By step(4)PBI multilayer films obtained are handled through impregnation of phosphoric acid, and the temperature of impregnation of phosphoric acid processing is 80 DEG C, phosphorus
Acid concentration is 80wt%, and dip time is 40 hours to get the PBI multilayer complex films.
In addition, preparing PBI films using solution casting method, thickness is 100 microns, and in preparation process, solvent selects NMP, PBI
Mass fraction in NMP is 5%, is then handled through impregnation of phosphoric acid with PBI films obtained, and the temperature of impregnation of phosphoric acid processing is 80
DEG C, phosphoric acid concentration 80wt%, dip time be 40 hours, obtain PBI/ phosphoric acid films, be denoted as traditional PBI composite membranes, to this
PBI multilayer complex films prepared by embodiment are compared.
Using AC impedence method(EIS)PBI multilayer complex films manufactured in the present embodiment are tested with tradition PBI composite membranes not
Conductivity under synthermal(Humidity is 0), as shown in figure 3, and measuring conductivity at 150 DEG C and changing with time trend, such as Fig. 4
It is shown.
Fig. 3 and Fig. 4 show, the PBI multilayer complex films prepared by the present embodiment, due to its special structure so that anhydrous
Conductivity is compared traditional PBI composite membranes and is significantly increased, and over time, and the conductivity of PBI multilayer complex films relatively passes
The stability of system PBI composite membranes significantly increases, this can illustrate that perforated inner layer is combined multilayer complex films obtained can with compacted zone
To effectively improve the conductivity of film, and greatly reduce the bleed rate of phosphoric acid.
Claims (5)
1. a kind of preparation method of polybenzimidazoles multilayer complex films used for high-temperature fuel cell, which is characterized in that including walking as follows
Suddenly:
(1)Polybenzimidazole resin is dissolved in high boiling solvent, polybenzimidazoles mold liquid is obtained, wherein polyphenyl and miaow
The additive amount of azoles resin is the 0.2-5% of high boiling solvent quality;
(2)By step(1)The polybenzimidazoles mold liquid of gained pours into casting film plate, is placed in climatic chamber and carries out vapor
Induction phase separation, humidity 20%-95%, temperature are 25 DEG C -120 DEG C, and constant temperature and humidity is placed 0.2-12 hours, and polyphenyl and miaow is made
Azoles perforated inner layer;
(3)By step(2)Polybenzimidazoles perforated inner layer obtained takes out, and is placed in the mixed liquor of high boiling solvent and water, puts
It takes out after setting 1-5h, is dried in vacuo in 25 DEG C of -150 DEG C of temperature ranges;
(4)Use spray coating method that polybenzimidazoles slurry even application is fine and close to prepare polybenzimidazoles in perforated inner layer both sides
Layer, is dried in vacuo in 25 DEG C of -150 DEG C of temperature ranges, and polybenzimidazoles multilayer film is made, wherein the polybenzimidazoles slurry
Material is the mixed liquor of polybenzimidazole resin and N-Methyl pyrrolidone composition, polybenzimidazole resin in polybenzimidazoles slurry
Shared mass fraction is 0.2-5%;
(5)By step(4)Polybenzimidazoles multilayer film obtained is more to get the polybenzimidazoles after impregnation of phosphoric acid is handled
Layer composite membrane.
2. the preparation method of polybenzimidazoles multilayer complex films used for high-temperature fuel cell according to claim 1, feature
It is:Step(1)And step(3)In, the high boiling solvent is in n,N-dimethylacetamide and N-Methyl pyrrolidone
It is a kind of or two kinds.
3. the preparation method of polybenzimidazoles multilayer complex films used for high-temperature fuel cell according to claim 1, feature
It is:Step(3)In the mixed liquor of the high boiling solvent and water, the volume ratio of water and high boiling solvent is 1:0.1-1:2.
4. the preparation method of polybenzimidazoles multilayer complex films used for high-temperature fuel cell according to claim 1, feature
It is:Step(2)Described in polybenzimidazoles perforated inner layer thickness be 20-120 microns, step(4)Described in polyphenyl and miaow
Azoles dense layer thickness is 5-30 microns.
5. the preparation method of polybenzimidazoles multilayer complex films used for high-temperature fuel cell according to claim 1, feature
It is:Step(5)The temperature of the impregnation of phosphoric acid processing is 20 DEG C -150 DEG C, phosphoric acid concentration 50-100wt%, and dip time is
12-100 hours.
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CN107221693B (en) * | 2016-09-27 | 2019-10-22 | 中科院大连化学物理研究所张家港产业技术研究院有限公司 | A kind of high temperature proton exchange film and preparation method thereof of polybenzimidazoles/ionic liquid MULTILAYER COMPOSITE |
CN107221692B (en) * | 2016-09-27 | 2019-10-22 | 中科院大连化学物理研究所张家港产业技术研究院有限公司 | A kind of polybenzimidazoles with high anti-oxidation ability/phosphoric acid MULTILAYER COMPOSITE high temperature proton exchange film and preparation method thereof |
CN106356547B (en) * | 2016-09-27 | 2019-07-05 | 中科院大连化学物理研究所张家港产业技术研究院有限公司 | A kind of cross-linking type polybenzimidazoles/silica high temperature proton exchange film and preparation method thereof with high anti-oxidation ability |
CN106750442A (en) * | 2017-01-12 | 2017-05-31 | 黄河科技学院 | A kind of cross-linking type polybenzimidazoles with high conductivity/polyethylene triazole high temperature proton exchange film and preparation method thereof |
CN111954951B (en) * | 2018-02-28 | 2023-08-01 | Jtec能源有限公司 | Bonding method of acid doped film |
CN111129557B (en) * | 2019-12-11 | 2022-09-09 | 深圳欧陆通电子股份有限公司 | Phosphoric acid modified polybenzimidazole proton exchange membrane and preparation method thereof |
US11961976B2 (en) * | 2021-03-08 | 2024-04-16 | Google Llc | Multiple battery cell architecture for outdoor mounted computing devices |
CN115084610A (en) * | 2022-05-17 | 2022-09-20 | 中国科学院深圳先进技术研究院 | Proton exchange membrane and preparation method thereof |
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