• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A continuous automated process and production line for preparing an acid doped polybenzimidazole, PBI, polymer membrane film for use in a fuel cell, the process comprising a washing stage, a drying procedure, and a doping stage.
    公开号:DK202000062A1
    申请号:DKP202000062
    申请日:2020-01-20
    公开日:2021-08-06
    发明作者:Bang Mads；Gromadskyi Denys；Bork Jakob；Hromadska Larysa
    申请人:Blue World Tech Holding Aps；
    IPC主号:
    专利说明:

    [1] [1] Seland F, Berning T, Børessen B, Tunold R. Improving the performance of high-temperature PEM fuel cells based on PBI electrolyte. Journal of Power Sources, 160 (2006) 27-36
    [2] [2] Li Q, Jensen JO, Savinell RF, Bjerrum NJ. High temperature proton exchange membranes based on polybenzimidazole for fuel cells. Progress in Polymer Science, 34 (2009) 449-477
    [3] [3] Li X, Qian G, Chen X, Benicewicz BC. Synthesis and characterization of a new fluorine-containing polybenzimidazole (PBI) for proton-conducting membranes in fuel cells. Fuel Cells, 13 (2013) 832-842
    [4] [4] Pu H, Wang L, Pan H, Wan D. Synthesis and characterization of fluorine-containing polybenzimidazole for proton conducting membranes in fuel cells. Journal of Polymer Science, 48 (2010) 2115-2122
    [5] [5] Solvent Boiling Points Chart: https://www.brandtech.com/solventboilingpointschart/
    [6] [6] Gentilcore MJ. Purification of N,N-dimethylacetamide. European Patent EP1551522B1, filed 18.06.2003
    [7] [7] Wadhwa L, Bitritto M, Powers EJ. Fabrication of high performance polybenzimidazole films. US Patent, 4,927,909, filed 18.09.1987
    [8] [8] Kim HJ, Kim BG, Lee HJ, Jang JH, Cho EA, Han JH, Nam SW, Hong SA, Lim TH. Method for in-situ preparation of polybenzimidazole-based membrane and polybenzimidazole-based electrolyte prepared thereby. Patent application US2012/0115050A1, filed 22.09.2011
    [9] [9] Shen CH, Jheng LC, Hsu SLC, Wang JTW. Phosphoric acid-doped cross-linked porous polybenzimidazole membranes for proton exchange membrane fuel cells. Journal of Materials Chemistry, 21 (2011) 156660- 156665
    [10] [10] OonoY, Sounai A, Hori M. Influence of the phosphoric acid-doping level in polybenzimidazole membrane on the cell performance of high- temperature proton exchange membrane fuel cells. Journal of Power Sources, 189 (2009) 943-949
    [11] [11] Krishnan NN, Joseph D, Duong NMH, Konovalova A, Jang JH, Kim HJ, Nam SW, Henkensmeier D. Phosphoric acid doped crosslinked
    [12] [12] Kurungot S, Illathvarappil R, Bhange N, Unni SM. Process for the preparation PBI based electrode assembly (MEA) with improved fuel cell performance and stability. Patent US10,361,446B2, filed 09.12.2004
    [13] [13] Perry KA, More KL, Payzant EA, Meisner RA, Sumpter BG, Benicewicz BC. A comparative study of phosphoric acid-doped m-PBI membranes. Polymer Physics, 52 (2014) 26-35
    [14] [14] Hsu SLC, Jheng LC. Method of fabricating proton-conducting electrolytic membrane. Patent, US9,705,146B2, filed 29.12.2014
    权利要求:
    Claims (10)
    [1] 1. A continuous automated process for preparing an acid doped polybenzimidazole, PBI, polymer film membrane sheet for use in a fuel cell, the process comprising in the following sequence in automation, - providing a PBI film membrane sheet for processing; - in a washing stage, exposing the membrane sheet to water for removing solvents, for example N,N-dimethylacetamide DMAc, from the membrane sheet by the water; - in a drying procedure, drying the membrane sheet at temperatures elevated above ambient temperature; - in a doping stage, after the drying procedure, exposing the PBI membrane sheet to orthophosphoric acid at a concentration higher than 85 wt.% for doping the membrane sheet with the acid.
    [2] 2. A process according to claim 1, wherein the method comprises providing the orthophosphoric acid in the doping stage at a temperature in the range of 90-100°C.
    [3] 3. A process according to any preceding claim, wherein the method comprises performing the doping in the doping stage in the range of 10 seconds to 5 minutes.
    [4] 4. A process according to any preceding claim, wherein the drying procedure comprises two drying phases, wherein the first drying phase is made at a temperature in the range of 1-10 degrees below the boiling point of water, for example in the range of 90-99°C if at atmospheric pressure, in order to evaporate water without bubble formation, and wherein the second drying phase is made at a temperature in the range of 1-10 degrees below the boiling point of DMAc or 1-10 degrees below the boiling point of an azeotropic mixture of acetic acid with DMAc for evaporating DMAc without bubble formation.
    DK 2020 00062 A1 19
    [5] 5. A process according to any preceding claim, wherein the method comprises, in a chemical-reaction stage, between the washing stage and the drying stage, exposing the membrane sheet to water-diluted orthophosphoric acid having a concentration in the range of 0.01 wt. % to 1 wt.% for removing further DMAc from the PBI membrane sheet by chemical reaction of the DMAc with the diluted orthophosphoric acid to form acetic acid.
    [6] 6. A process according to any preceding claim, wherein the method comprises, in a pre-doping stage, between the drying stage and the doping stage, exposing the membrane sheet to orthophosphoric acid at a concentration higher than 65 wt.% and dissolving low molecular weight molecules of the PBI polymer of the membrane by the orthophosphoric acid.
    [7] 7. A process according to any preceding claim, wherein the method comprises providing the various stages as liquid baths in corresponding containers and submerging the membrane sheet in the liquid.
    [8] 8. A process according to any preceding claim, wherein the method comprises providing the membrane sheet from a roll as an endless strip and continuously moving the endless strip over rollers through the various stages.
    [9] 9. An automated production line for a continuous automated process according to any preceding claim, the production line comprising, - a sheet receiver for receiving a polybenzimidazole, PBI, film membrane sheet; - a washing stage for exposing the membrane sheet to water and removing solvent, for example N,N-dimethylacetamide DMAc, from the membrane sheet by the water; - a drying apparatus for drying the membrane sheet at temperatures elevated above ambient temperature;
    DK 2020 00062 A1 20 - a doping stage after the drying apparatus for exposing the PBI membrane sheet to orthophosphoric acid at a concentration higher than 85 wt.% for doping the membrane sheet with the acid.
    [10] 10. The production line of claim 9, comprising a first roll (1) for receiving a quasi-endless strip of PBI membrane sheet and a plurality of correspondingly arranged further rollers (2, 5) for unrolling the strip from the first roll (1) while guiding the strip over the further rollers (2, 5) through the various preparation stages in a sequence as described in the following: - one or more water containers (3,6) with water as part of the washing stage for washing the strip by guiding the strip through the water in the water containers (3,6); - a chemical-reaction stage comprising a diluted-acid container (7) with water-diluted orthophosphoric acid having a concentration in the range of
    0.01 wt. % to 1 wt.% for removing further DMAc from the PBI membrane sheet by chemical reaction of the DMAc with the diluted orthophosphoric acid to form acetic acid by guiding the strip through the diluted acid in the diluted-acid container (7); - a first zone (8) and a second zone (9) of the drying apparatus with two corresponding drying phases for drying the strip while guided through the first and then the second zone, wherein the first zone is programmed to provide a drying temperature in the range of 1-10 degrees below the boiling point of water, for example in the range of 90-99°C if at atmospheric pressure, in order to evaporate water without bubble formation in the first drying phase, and wherein the second zone is programmed to provide a temperature in the range of 1-10 degrees below the boiling point of DMAc or 1-10 degrees below the boiling point of an azeotropic mixture of acetic acid with DMAc for evaporating DMAc without bubble formation in the second drying phase; - a pre-doping container (10) as part of the pre-doping stage with orthophosphoric acid at a concentration higher than 65 wt.% for dissolving low molecular weight molecules of the PBI polymer of the
    DK 2020 00062 A1 21 membrane by the orthophosphoric acid by guiding the strip through the acid in the pre-doping container (10); - a doping container (11) as part of the doping stage with orthophosphoric acid at a concentration higher than 85 wt.% for doping the membrane sheet with the acid by guiding the strip through the acid in the doping container (11); - a collection roller (13) for collecting the endless strip after doping.
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    同族专利:
    公开号 | 公开日
    DK180599B1|2021-10-14|
    WO2021148090A1|2021-07-29|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US4927909A|1987-09-18|1990-05-22|Hoechst Celanese Corp.|Fabrication of high performance polybenzimidazole films|
    JP2000281819A|1999-01-27|2000-10-10|Aventis Res & Technol Gmbh & Co Kg|Production of cross-linked polymer membrane and fuel cell|
    DE10109829A1|2001-03-01|2002-09-05|Celanese Ventures Gmbh|Polymer membrane, process for its production and its use|
    NZ539786A|2002-10-24|2007-05-31|Toyo Boseki|Heat-resistant film and composite ion-exchange membrane made from a polymer solution|
    DE102005038195A1|2005-08-12|2007-02-15|Pemeas Gmbh|Improved membrane electrode assemblies and fuel cells with long life|
    KR101678706B1|2009-01-19|2016-11-23|도레이 카부시키가이샤|Process for producing polymeric electrolyte membrane|
    法律状态:
    2021-08-06| PAT| Application published|Effective date: 20210721 |
    2021-10-14| PME| Patent granted|Effective date: 20211014 |
    优先权:
    申请号 | 申请日 | 专利标题
    DKPA202000062A|DK180599B1|2020-01-20|2020-01-20|Apparatus and process for making acid-doped proton exchange membranes|DKPA202000062A| DK180599B1|2020-01-20|2020-01-20|Apparatus and process for making acid-doped proton exchange membranes|
    PCT/DK2021/050008| WO2021148090A1|2020-01-20|2021-01-12|Apparatus and process for making acid-doped proton exchange membranes|
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