CN104115245A - 铝电解电容器用电解液及使用其的铝电解电容器 - Google Patents
铝电解电容器用电解液及使用其的铝电解电容器 Download PDFInfo
- Publication number
- CN104115245A CN104115245A CN201380009367.3A CN201380009367A CN104115245A CN 104115245 A CN104115245 A CN 104115245A CN 201380009367 A CN201380009367 A CN 201380009367A CN 104115245 A CN104115245 A CN 104115245A
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- China
- Prior art keywords
- acid
- electrolyte
- electrolytic capacitor
- anion
- alkyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000003990 capacitor Substances 0.000 title claims abstract description 30
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000008151 electrolyte solution Substances 0.000 title abstract 3
- 239000003792 electrolyte Substances 0.000 claims abstract description 84
- 150000001450 anions Chemical class 0.000 claims abstract description 37
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- 150000001768 cations Chemical class 0.000 claims abstract description 13
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- -1 carboxylate anion Chemical class 0.000 claims description 32
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 30
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 22
- 125000000217 alkyl group Chemical group 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 239000004411 aluminium Substances 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 9
- 239000011976 maleic acid Substances 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 7
- 239000010452 phosphate Substances 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 abstract 3
- 239000000010 aprotic solvent Substances 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 63
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 41
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 40
- 238000004519 manufacturing process Methods 0.000 description 22
- 239000002253 acid Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 16
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 14
- 241000283216 Phocidae Species 0.000 description 11
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 239000003513 alkali Substances 0.000 description 9
- 238000004821 distillation Methods 0.000 description 9
- 150000002148 esters Chemical class 0.000 description 9
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 150000004985 diamines Chemical class 0.000 description 8
- 230000006837 decompression Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- KYRYHBRYSSBWLU-UHFFFAOYSA-N 1,2,3,4-tetramethylimidazolidine Chemical compound CC1CN(C)C(C)N1C KYRYHBRYSSBWLU-UHFFFAOYSA-N 0.000 description 6
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 6
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 150000007524 organic acids Chemical class 0.000 description 6
- 150000001409 amidines Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 4
- 239000004327 boric acid Substances 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
- UCQFCFPECQILOL-UHFFFAOYSA-N diethyl hydrogen phosphate Chemical compound CCOP(O)(=O)OCC UCQFCFPECQILOL-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 150000007522 mineralic acids Chemical class 0.000 description 4
- 239000012188 paraffin wax Substances 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- UVEMSKZPVSTDTG-BTJKTKAUSA-N CC1N(C)C(C)N(C)C1.OC(/C=C\C(O)=O)=O Chemical compound CC1N(C)C(C)N(C)C1.OC(/C=C\C(O)=O)=O UVEMSKZPVSTDTG-BTJKTKAUSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 3
- 125000003739 carbamimidoyl group Chemical group C(N)(=N)* 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- FAWDVNZHJORXAO-UHFFFAOYSA-N diethyl phosphate;1,2,3,4-tetramethylimidazolidin-1-ium Chemical compound CCOP([O-])(=O)OCC.CC1C[NH+](C)C(C)N1C FAWDVNZHJORXAO-UHFFFAOYSA-N 0.000 description 3
- WZPMZMCZAGFKOC-UHFFFAOYSA-N diisopropyl hydrogen phosphate Chemical compound CC(C)OP(O)(=O)OC(C)C WZPMZMCZAGFKOC-UHFFFAOYSA-N 0.000 description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- 229940093476 ethylene glycol Drugs 0.000 description 3
- 150000002596 lactones Chemical class 0.000 description 3
- DFAGYRCOGIOTBI-UHFFFAOYSA-N methyl carbonate;1,2,3,4-tetramethylimidazolidin-1-ium Chemical compound COC([O-])=O.CC1C[NH+](C)C(C)N1C DFAGYRCOGIOTBI-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 150000003014 phosphoric acid esters Chemical class 0.000 description 3
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 3
- QLNJFJADRCOGBJ-UHFFFAOYSA-N propionamide Chemical compound CCC(N)=O QLNJFJADRCOGBJ-UHFFFAOYSA-N 0.000 description 3
- 229940080818 propionamide Drugs 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000003457 sulfones Chemical class 0.000 description 3
- VMZNMSUASLBPDS-UHFFFAOYSA-N 1-ethyl-2-methyl-4,5-dihydroimidazole Chemical class CCN1CCN=C1C VMZNMSUASLBPDS-UHFFFAOYSA-N 0.000 description 2
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 2
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 description 2
- OZJPLYNZGCXSJM-UHFFFAOYSA-N 5-valerolactone Chemical compound O=C1CCCCO1 OZJPLYNZGCXSJM-UHFFFAOYSA-N 0.000 description 2
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- PMDCZENCAXMSOU-UHFFFAOYSA-N N-ethylacetamide Chemical compound CCNC(C)=O PMDCZENCAXMSOU-UHFFFAOYSA-N 0.000 description 2
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 2
- ATVGJKFOXVMUES-UHFFFAOYSA-N N1=CC=CC2=CC=CC=C12.CN1C=NC=C1 Chemical compound N1=CC=CC2=CC=CC=C12.CN1C=NC=C1 ATVGJKFOXVMUES-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000001350 alkyl halides Chemical class 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 150000005690 diesters Chemical class 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- ZJXZSIYSNXKHEA-UHFFFAOYSA-L ethyl phosphate(2-) Chemical compound CCOP([O-])([O-])=O ZJXZSIYSNXKHEA-UHFFFAOYSA-L 0.000 description 2
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 2
- GAEKPEKOJKCEMS-UHFFFAOYSA-N gamma-valerolactone Chemical compound CC1CCC(=O)O1 GAEKPEKOJKCEMS-UHFFFAOYSA-N 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 2
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 description 2
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- LGRLWUINFJPLSH-UHFFFAOYSA-N methanide Chemical compound [CH3-] LGRLWUINFJPLSH-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 2
- IXQGCWUGDFDQMF-UHFFFAOYSA-N o-Hydroxyethylbenzene Natural products CCC1=CC=CC=C1O IXQGCWUGDFDQMF-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 2
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
- BGBNXIKULUCCOO-BTJKTKAUSA-N (z)-but-2-enedioic acid;n,n-diethylethanamine Chemical compound CCN(CC)CC.OC(=O)\C=C/C(O)=O BGBNXIKULUCCOO-BTJKTKAUSA-N 0.000 description 1
- ZBXCTUFRODXIFX-BTJKTKAUSA-N (z)-but-2-enedioic acid;n,n-dimethylethanamine Chemical compound CCN(C)C.OC(=O)\C=C/C(O)=O ZBXCTUFRODXIFX-BTJKTKAUSA-N 0.000 description 1
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 1
- YANGGZLARFZISN-UHFFFAOYSA-N 1,2,3,4-tetraethylimidazolidine Chemical compound CCC1CN(CC)C(CC)N1CC YANGGZLARFZISN-UHFFFAOYSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical class ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- KNKRKFALVUDBJE-UHFFFAOYSA-N 1,2-dichloropropane Chemical compound CC(Cl)CCl KNKRKFALVUDBJE-UHFFFAOYSA-N 0.000 description 1
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 description 1
- ICBPURKUPVLVCM-UHFFFAOYSA-N 1,5-dimethyl-2-phenylpyrazol-3-one;2-hydroxy-2-phenylacetic acid Chemical compound OC(=O)C(O)C1=CC=CC=C1.CN1C(C)=CC(=O)N1C1=CC=CC=C1 ICBPURKUPVLVCM-UHFFFAOYSA-N 0.000 description 1
- RRQYJINTUHWNHW-UHFFFAOYSA-N 1-ethoxy-2-(2-ethoxyethoxy)ethane Chemical compound CCOCCOCCOCC RRQYJINTUHWNHW-UHFFFAOYSA-N 0.000 description 1
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- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 235000019303 thiodipropionic acid Nutrition 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 150000003739 xylenols Chemical class 0.000 description 1
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/035—Liquid electrolytes, e.g. impregnating materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/145—Liquid electrolytic capacitors
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Abstract
本发明的课题在于提高电解电容器的可靠性,以使其即便处于周边环境进一步高温化或多湿条件下,电解液亦不会自密封部泄漏。本发明的铝电解电容器用电解液含有非质子性溶剂(A)、包含下述通式(1)所表示的阳离子(B)与阴离子(C)的盐的电解质(D)、及下述通式(2)所表示的化合物(E),且化合物(E)的含量相对于(A)及(D)的合计重量为0.01重量%~3重量%。[式中,R1~R3为碳数1~3的烷基,R4~R7为碳数1~3的烷基或氢原子][式中,R8~R14为碳数1~3的烷基或氢原子]。
Description
技术领域
本发明涉及一种铝电解电容器用电解液及使用其的铝电解电容器。
背景技术
近年来,逐渐对用于汽车电气设备等的铝电解电容器有如下要求:伴随周边环境的高温化,高温下的特性劣化较小,且即便因暴露于室外而处于多湿条件下,特性劣化亦较少。因此,亦期待电解液于高温、多湿下特性劣化较少。
从前作为耐久性较高的铝电解电容器用电解液,已知以具有烷基取代脒基的化合物的四级化物的羧酸盐作为电解质的所谓脒系电解液(例如专利文献1)等。
现有技术文献
专利文献
专利文献1:国际公开第95/15572号
发明内容
直至已知脒系电解液之前,一直使用烷基四级铵系电解液。然而,烷基四级铵系电解液存在电解液自因碱而劣化的密封部泄漏的异常。另一方面,于专利文献1中揭示的脒系电解液会与具有烷基取代脒基的化合物所产生的碱进行反应。由此,封口体的碱劣化得以抑制,电解液不会自密封部泄漏。因此,由于具有烷基四级铵系电解液不具有的效果,故而作为铝电解电容器用电解液而广泛使用。然而,在周边环境的进一步高温化或多湿条件下,存在认为碱劣化的抑制效果未必充分的情况。
[发明所欲解决的问题]
本发明的课题在于提高电解电容器的可靠性,以使其即便处于周边环境进一步高温化或多湿条件下,电解液亦不会自密封部泄漏。
[解决问题的技术手段]
本发明者等人为达成上述目的而进行研究,结果完成本发明。
即本发明是一种铝电解电容器用电解液,其含有非质子性溶剂(A)、包含下述通式(1)所表示的阳离子(B)与阴离子(C)的盐的电解质(D)、及下述通式(2)所表示的化合物(E),且相对于(A)及(D)的合计重量,化合物(E)的含量为0.01重量%~3重量%。
[式中,R1~R3为碳数1~3的烷基,R4~R7为碳数1~3的烷基或氢原子]
[式中,R8~R14为碳数1~3的烷基或氢原子]
[发明的效果]
使用本发明的电解液的电解电容器可成为即便处于周边环境进一步高温化或多湿条件下,电解液亦不会自密封部泄漏的可靠性高的电容器。
具体实施方式
本发明的电解液中,于对电解液施加电压时,藉由电解液中所含有的水的电解,而于阴极侧产生OH-,于阳极侧产生H+。H+与上述通式(2)所表示的化合物(E)进行反应而形成胺盐。由于该胺盐将OH-中和,因此表现出碱抑制效果。因此,即便于高温-高湿下使用电容器,亦藉由化合物(E)的作用而不易引起封口体的碱劣化,可抑制电解液自密封部泄漏。于组合作为具有烷基取代脒基的化合物的四级化物的一种的上述通式(1)所表示的阳离子(B)与化合物(E)时,成为即便于高温-高湿下可靠性亦高的电容器用电解液。
<非质子性溶剂(A)>
作为构成本发明的电解液的非质子性溶剂(A),包括:(1)醚、(2)酰胺、(3)恶唑啶酮、(4)内酯、(5)腈、(6)碳酸酯、(7)砜、(8)其他有机溶剂。
(1)醚
单醚(乙二醇单丁醚、乙二醇单苯醚、四氢呋喃、3-甲基四氢呋喃等)、二醚(乙二醇二甲醚、乙二醇二乙醚、二乙二醇单甲醚、二乙二醇单乙醚等)、三醚(二乙二醇二甲醚、二乙二醇二乙醚等)。
(2)酰胺
甲酰胺(N-甲基甲酰胺、N,N-二甲基甲酰胺、N-乙基甲酰胺、N,N-二乙基甲酰胺等)、乙酰胺(N-甲基乙酰胺、N,N-二甲基乙酰胺、N-乙基乙酰胺、N,N-二乙基乙酰胺等)、丙酰胺(N,N-二甲基丙酰胺等)、吡咯啶酮(N-甲基吡咯啶酮、N-乙基吡咯啶酮等)、六甲基磷酰胺等。
(3)恶唑啶酮
N-甲基-2-恶唑啶酮、3,5-二甲基-2-恶唑啶酮等。
(4)内酯
γ-丁内酯、α-乙酰基-γ-丁内酯、β-丁内酯、γ-戊内酯、δ-戊内酯等。
(5)腈
乙腈、丙腈、丁腈、丙烯腈、甲基丙烯腈、苯甲腈等。
(6)碳酸酯
碳酸乙二酯、碳酸丙二酯、碳酸丁二酯、碳酸二甲酯、碳酸二乙酯等。
(7)砜
环丁砜、二甲基砜等。
(8)其他有机溶剂
1,3-二甲基-2-咪唑啶酮、二甲基亚砜、芳香族溶剂(甲苯、二甲苯等)石蜡溶剂(正构石蜡、异构石蜡等)等。
非质子性溶剂(A)可使用一种或并用两种以上。该等中,较佳为内酯及砜,进而较佳为γ-丁内酯、环丁砜,尤佳为γ-丁内酯。
本发明的电解液除非质子性溶剂(A)以外亦可含有乙二醇等质子性溶剂(F)。(F)的含量基于(A)的重量为0重量%~100重量%(以下有时记作wt%)。作为(F),可列举乙二醇、丙二醇、二乙二醇等。
<阳离子(B)>
本发明的电解液中所含有的电解质(D)包含上述通式(1)所表示的阳离子(B)与阴离子(C)的盐。
通式(1)中,R1~R3为碳数1~3的烷基,R4~R7的碳数1~3的烷基或氢原子。碳数1~3的烷基可列举甲基、乙基、正丙基、异丙基。
作为阳离子(B)的具体例,可列举1,2,3,4-四甲基咪唑啉鎓、1,3,4-三甲基-2-乙基咪唑啉鎓、1,3-二甲基-2,4-二乙基咪唑啉鎓、1,2-二甲基-3,4-二乙基咪唑啉鎓、1-甲基-2,3,4-三乙基咪唑啉鎓、1,2,3,4-四乙基咪唑啉鎓、1,2,3-三甲基咪唑啉鎓、1,3-二甲基-2-乙基咪唑啉鎓、1-乙基-2,3-二甲基咪唑啉鎓、1,2,3-三乙基咪唑啉鎓等。
上述中,进而较佳为1,2,3,4-四甲基咪唑啉鎓、1-乙基-2,3-二甲基咪唑啉鎓。
<阴离子(C)>
作为构成本发明的电解液的阴离子(C),可列举通常用于电解液的各种有机酸及/或无机酸的阴离子。于二价以上的有机酸及/或无机酸的情形时,阴离子(C)较佳为单阴离子。
作为有机酸、无机酸,例如可列举下述的(1)~(6)。
(1)羧酸类
·碳数2~15的2价~4价的聚羧酸:脂肪族聚羧酸[饱和聚羧酸(草酸、丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸等)、不饱和聚羧酸(顺丁烯二酸、反丁烯二酸、衣康酸等)]、芳香族聚羧酸[鄰苯二甲酸、间苯二甲酸、对苯二甲酸、偏苯三甲酸、均苯四甲酸等]、含S聚羧酸[硫二丙酸等]。
·碳数2~20的氧基羧酸:脂肪族氧基羧酸[乙醇酸、乳酸、醇酸、蓖麻油脂肪酸等];芳香族氧基羧酸[水杨酸、杏仁酸等];
·碳数1~30的单羧酸:脂肪族单羧酸[饱和单羧酸(甲酸、乙酸、丙酸、丁酸、异丁酸、戊酸、己酸、庚酸、辛酸、壬酸、十二酸、肉豆蔻酸、硬脂酸、二十二酸等)、不饱和单羧酸(丙烯酸、甲基丙烯酸、丁烯酸、油酸等)];芳香族单羧酸[苯甲酸、肉桂酸、萘甲酸等];
(2)酚类
·一元酚(包括苯酚类、萘酚类):苯酚、烷基(碳数1~15)、苯酚类(苯甲酚、二甲苯酚、乙基苯酚、正丙基苯酚或异丙基苯酚、异十二烷基苯酚等)、甲氧基苯酚类(丁香油酚、愈创木酚等)、α-萘酚、β-萘酚、环己基苯酚等;
·多酚:鄰苯二酚、间苯二酚、鄰苯三酚、间苯三酚、双酚A、双酚F、双酚S等。
(3)烷基的碳数1~15的磷酸单烷基酯及磷酸二烷基酯
·磷酸单甲酯及磷酸二甲酯、磷酸单乙酯及磷酸二乙酯、磷酸单异丙酯及磷酸二异丙酯、磷酸单丁酯及磷酸二丁酯、磷酸单(2-乙基己基)酯及磷酸二-(2-乙基己基)酯、磷酸单异癸酯及磷酸二异癸酯等。
(4)磺酸
·烷基(碳数1~15)苯磺酸(对甲苯磺酸、壬基苯磺酸、十二烷基苯磺酸等)、磺基水杨酸、甲磺酸、三氟甲磺酸等。
(5)无机酸
·磷酸、四氟硼酸、过氯酸、六氟磷酸、六氟銻酸、六氟砷酸等。
(6)其他
·三氟甲磺酰亚胺等酰亚胺阴离子、甲基三氟甲磺酰基甲基化物等甲基化物阴离子。
该等中,较佳为(1)羧酸类及(3)磷酸单烷基酯及磷酸二烷基酯(烷基的碳数1~15),进而较佳为磷酸单乙酯及磷酸二乙酯、磷酸单异丙酯及磷酸二异丙酯、磷酸单丁酯及磷酸二丁酯、邻苯二甲酸及顺丁烯二酸。最佳为邻苯二甲酸及顺丁烯二酸。
<电解质(D)>
构成本发明的电解液的电解质(D)是以阳离子(B)与阴离子(C)的组合表示,较佳为以下者。
1,2,3,4-四甲基咪唑啉鎓·鄰苯二甲酸单阴离子、1-乙基-2,3-二甲基咪唑啉鎓·鄰苯二甲酸单阴离子、1,2,3,4-四甲基咪唑啉鎓·顺丁烯二酸单阴离子、1-乙基-2,3-二甲基咪唑啉鎓阳离子·顺丁烯二酸单阴离子、1,2,3,4-四甲基咪唑啉鎓·磷酸二乙酯酸阴离子、1-乙基-2,3-二甲基咪唑啉鎓阳离子·磷酸二乙酯酸阴离子、1,2,3,4-四甲基咪唑啉鎓·磷酸二丁酯酸阴离子、1-乙基-2,3-二甲基咪唑啉鎓阳离子·磷酸二丁酯酸阴离子、1,2,3,4-四甲基咪唑啉鎓·磷酸二异丙酯酸阴离子、1-乙基-2,3-二甲基咪唑啉鎓阳离子·磷酸二异丙酯酸阴离子。
进而最佳为以下者。
1,2,3,4-四甲基咪唑啉鎓·鄰苯二甲酸单阴离子、1-乙基-2,3-二甲基咪唑啉鎓阳离子·鄰苯二甲酸单阴离子、1,2,3,4-四甲基咪唑啉鎓·顺丁烯二酸单阴离子、1-乙基-2,3-二甲基咪唑啉鎓阳离子·顺丁烯二酸单阴离子。
本发明的铝电解电容器用电解液含有电解质(D)作为主电解质。此处所谓作为主电解质而含有,表示本发明的电解电容器用电解液中所含有的电解质的50wt%以上为电解质(D)。
本发明的铝电解电容器用电解液除(D)以外亦可含有电解质(G)。(G)的含量为未达本发明的电解电容器用电解液中所含有的电解质的50wt%。作为电解质(G),可列举三乙胺·鄰苯二甲酸盐、乙基二甲胺·鄰苯二甲酸盐、二乙基甲胺·鄰苯二甲酸盐、三乙胺·顺丁烯二酸盐、乙基二甲胺·顺丁烯二酸盐、二乙基甲胺·顺丁烯二酸盐等。
<化合物(E)>
构成本发明的电解液的化合物(E)是以上述通式(2)表示,具体而言可列举以下者。化合物(E)可使用一种或并用两种以上。
N-甲基-N-[2-(N′-甲基胺基)丙基]乙酰胺、N-甲基-N-[2-(N′-甲基胺基)-1-甲基乙基]乙酰胺、N-甲基-N-[2-(N′-乙基胺基)乙基]乙酰胺、N-乙基-N-[2-(N′-甲基胺基)乙基]乙酰胺、N-甲基-N-[2-(N′-甲基胺基)乙基]乙酰胺、N-甲基-N-[2-(N′-乙基胺基)丙基]乙酰胺、N-乙基-N-[2-(N′-甲基胺基)-1-甲基乙基]乙酰胺、N-甲基-N-[2-(N′-甲基胺基)乙基]丙酰胺、N-甲基-N-[2-(N′-甲基胺基)乙基]丙酰胺等。
该等中,较佳为N-甲基-N-[2-(N′-甲基胺基)丙基]乙酰胺、N-甲基-N-[2-(N′-甲基胺基)-1-甲基乙基]乙酰胺、N-甲基-N-[2-(N′-乙基胺基)乙基]乙酰胺、N-乙基-N-[2-(N′-甲基胺基)乙基]乙酰胺。
化合物(E)的含量相对于非质子性溶剂(A)及电解质(D)的合计重量为0.01wt%~3wt%。进而,较佳为0.1wt%~2wt%,更佳为1wt%~1.5wt%。若少于0.01wt%,则封口体的碱劣化抑制的效果变低,若超过3wt%,则本发明的电解液的耐热性变差。
化合物(E)的含量可藉由高效液相色谱法(HPLC,high performance liquidchromatography)而测定。
HPLC的测定条件为:管柱:填充有聚合物涂敷型(Polymer-Coated)填充剂者,流动相:磷酸缓冲液(pH值为2~3),流速:0.8ml/min,检测器:UV,温度:40℃。又,以藉由流动相将电解液稀释100倍而得者作为测定用样品。
作为电解质(D)的合成方法,已知有如下方法:利用烷基卤化物、二烷基硫酸等将二级及三级环状脒四级化后,与碱金属或碱土金属的有机酸盐进行阴离子交换的方法;利用碳酸二酯将二级及三级环状脒四级化而制成碳酸盐,在有机酸中进行阴离子交换的方法(日本专利特开平8-67672);使2取代二胺的酰胺化合物与有机酸进行反应的方法(日本专利特开平11-322720)等。
作为化合物(E)的合成方法,已知有如下方法:使二胺单酰胺或1取代二胺单酰胺与烷基卤化物或二烷基硫酸等进行反应而制成2取代二胺单酰胺的卤盐或硫酸盐后,进行碱处理并藉由蒸馏而获得的方法(日本专利第2964244号);使有机二卤化物与单烷基胺进行反应,或使二胺化合物与烷基化剂进行反应而制造2取代二胺,使所生成的2取代二胺与有机酸或有机酸酯进行反应后,藉由蒸馏而获得的方法(日本专利特开2006-327956)等。
进而,本发明的电解液较佳为含有4-甲氧基丁酸。4-甲氧基丁酸亦与在施加电压时因电解液的电解而产生的强碱成分进行反应,反应物溶解于电解液中。因此,即便于高温-高湿下使用,亦不易引起封口体的碱劣化,可抑制电解液自密封部泄漏。
4-甲氧基丁酸的含量相对于(A)及(D)的合计重量,较佳为含有0.1wt%以下,进而较佳为含有0.001wt%~0.1wt%,更佳为0.005wt%~0.05wt%。
4-甲氧基丁酸的含量可藉由气相色谱法(GC,Gas Chromatography)而测定。
本发明的电解液的pH值通常为3~12,较佳为6~11,于制造电解质(D)时,选择电解液的pH值达到此范围的条件。再者,该电解液的pH值为电解液原液的25℃下的分析值。
亦可视需要而于本发明的电解液中添加水。就耐热性的观点而言,水基于电解液的重量为10wt%以下。
可视需要而于本发明的电解液中添加通常用于电解液的各种添加剂。作为该添加剂,可列举磷酸衍生物(例如磷酸、磷酸酯等)、硼酸衍生物(例如硼酸、硼酸与多糖类[甘露糖醇、山梨糖醇等]的络合物、硼酸与多元醇[乙二醇、甘油等]的络合物等)、硝基化合物(例如,邻硝基苯甲酸、对硝基苯甲酸、间硝基苯甲酸、邻硝基苯酚、对硝基苯酚等)等,就电解质(D)的导电率与于电解液溶剂中的溶解度的观点而言,其添加量基于电解液的重量为10wt%以下。
实施例
以下对本发明的具体的实施例进行说明,但本发明并不限定于此。以下,份表示重量份。
<制造例1>
加入乙酸乙酯(0.1mol)与1,2-二胺基丙烷(0.1mol),于温度140℃~180℃、压力0MPa~0.1MPa下保持6小时,进行酰胺化反应。继而于温度110℃~150℃下进行减压蒸馏,从而获得2,4-二甲基咪唑啉。继而于碳酸二甲酯(0.2mol)的甲醇溶液(74wt%)中滴加上述获得的2,4-二甲基咪唑啉(0.1mol),于120℃下搅拌15小时,藉此获得1,2,3,4-四甲基咪唑啉鎓·碳酸甲酯盐的甲醇溶液。
将鄰苯二甲酸(0.1mol)加入1,2,3,4-四甲基咪唑啉鎓·碳酸甲酯盐(0.1mol)的甲醇溶液中,从而获得1,2,3,4-四甲基咪唑啉鎓·鄰苯二甲酸单阴离子的甲醇溶液。于1.0kPa以下的减压度、50℃下对上述溶液进行加热,直至不存在甲醇的馏液而将甲醇蒸馏后,使温度自50℃上升至100℃,加热30分钟而将碳酸单甲酯(HOCO2CH3)、甲醇及二氧化碳(甲醇及二氧化碳是因碳酸单甲酯的热分解而有少量生成。以下将该等简称为副产物)蒸馏,藉此获得电解质(D-1){1,2,3,4-四甲基咪唑啉鎓·鄰苯二甲酸单阴离子}。产率为99wt%{基于1,2,3,4-四甲基咪唑啉鎓·碳酸甲酯盐(0.1mol)的重量的产率,以下相同}。
<制造例2>
将顺丁烯二酸(0.1mol)加入以与制造例1相同的方式而获得的1,2,3,4-四甲基咪唑啉鎓·碳酸甲酯盐(0.1mol)的甲醇溶液中,藉此进行盐交换反应,从而获得1,2,3,4-四甲基咪唑啉鎓·顺丁烯二酸单阴离子的甲醇溶液。于1.0kPa以下的减压度、50℃下对上述溶液进行加热,直至不存在甲醇的馏液而将甲醇蒸馏后,使温度自50℃上升至100℃,加热30分钟而将副产物蒸馏,藉此获得电解质(D-2){1,2,3,4-四甲基咪唑啉鎓·顺丁烯二酸单阴离子}。
<制造例3>
加入碳酸二乙酯(0.1mol)与2-甲基咪唑啉(四国化成制造,0.1mol),于温度100℃~150℃下搅拌10小时,藉此获得1-乙基-2-甲基咪唑啉。继而于碳酸二甲酯(0.1mol)的甲醇溶液(74wt%)中滴加1-乙基-2-甲基咪唑啉(0.1mol),于120℃下搅拌15小时,藉此获得1-乙基-2,3-二甲基咪唑啉鎓·碳酸甲酯盐的甲醇溶液。
将鄰苯二甲酸(0.1mol)加入上述获得的1-乙基-2,3-二甲基咪唑啉鎓·碳酸甲酯盐(0.1mol)的甲醇溶液中,从而获得1-乙基-2,3-二甲基咪唑啉鎓·鄰苯二甲酸单阴离子的甲醇溶液。于1.0kPa以下的减压度、50℃下对上述溶液进行加热,直至不存在甲醇的馏液而将甲醇蒸馏后,使温度自50℃上升至100℃,加热30分钟而将碳酸单甲酯(HOCO2CH3)、副产物蒸馏,藉此获得电解质(D-3){1-乙基-2,3-二甲基咪唑啉鎓·鄰苯二甲酸单阴离子}。
<制造例4>
于磷酸三乙酯(0.1mol)中添加二乙胺(0.2mol),于125℃下加热40小时,从而制成磷酸二乙酯单阴离子·二乙胺阳离子盐。其后,加入1,2,3,4-四甲基咪唑啉鎓·碳酸甲酯盐(0.1mol)的甲醇溶液中,进行盐交换反应,从而获得1,2,3,4-四甲基咪唑啉鎓·磷酸二乙酯单阴离子的甲醇溶液。于1.0kPa以下的减压度、135℃下对上述溶液进行加热,直至不存在甲醇、二乙胺等胺类的馏液,从而获得电解质(D-4){1,2,3,4-四甲基咪唑啉鎓·磷酸二乙酯单阴离子}。
<制造例5>
于具备温度计、可进行减压脱水的装置、搅拌机的不锈钢(SUS)制反应容器中加入N-甲基-N-(N′-甲基-2-胺基丙基)乙酰胺(0.1mol)、邻苯二甲酸(0.1mol),于反应温度100℃下反应6小时。其后,于120℃、0.5kPa减压下蒸馏除去未反应物及副生成的水,从而获得电解质(D-5){1,2,3,4-四甲基咪唑啉鎓·邻苯二甲酸单阴离子}。
<制造例6>
于1,2-二氯丙烷(0.1mol)中加入氢氧化钠(0.2mol),吹入甲胺(0.2mol)后,于密闭化80℃下加热10小时。其后,进行蒸馏而获得二级二胺。于密闭下、170℃下使该二级二胺与乙酸乙酯反应10小时,其后进行蒸馏,藉此获得N-甲基-N-[2-(N′-甲基胺基)丙基]乙酰胺(E-1)与N-甲基-N-[2-(N′-甲基胺基)-1-甲基乙基]乙酰胺(E-2)的混合物。使用液相色谱仪对该混合物进行分离提取,从而获得N-甲基-N-[2-(N′-甲基胺基)丙基]乙酰胺(E-1)与N-甲基-N-[2-(N′-甲基胺基)-1-甲基乙基]乙酰胺(E-2)。
<制造例7>
藉由使制造例4的1,2-二氯丙烷(0.1mol)成为1,2-二氯乙烷,使甲胺(0.2mol)成为甲胺(0.1mol)与乙胺(0.1mol),而获得N-甲基-N-[2-(N′-乙基胺基)乙基]乙酰胺(E-3)、N-乙基-N-[2-(N′-甲基胺基)乙基]乙酰胺(E-4)。
以下将于120℃、10kPa减压条件下蒸馏市售的γ-丁内酯(东京化成制造)、除去水分与杂质而成者记作“精制γ-丁内酯”。
以下将于120℃、0.7kPa减压条件下蒸馏市售的环丁砜(住友精化制造)、除去水分与杂质而成者记作“精制环丁砜”。
使用上述制造例1~制造例5中获得的电解质(D-1)~电解质(D-5)、上述制造例6、制造例7中获得的化合物(E-1)~化合物(E-4)、精制γ-丁内酯、精制环丁砜及4-甲氧基丁酸(那卡莱泰斯科(Nacalai Tesque)制造),制备如表1所示的实施例1~实施例15、比较例1~比较例5的电解液。
化合物(E)、4-甲氧基丁酸的含量藉由下述的测定条件确认为表中所记载的数值。
化合物(E)的测定
藉由以下的测定条件进行。
机器:高速液相色谱仪、岛津制作所制造的LC-10A,管柱:资生堂制造的卡普西鲁帕克型(CAPCELL PACK Type);UG120(4.6mmφ×25cm),流动相:磷酸的浓度10mmol/l、过氯酸钠的浓度100mmol/l的水溶液,流速:0.8ml/min,检测器:UV(210nm),注入量:20μl,管柱温度:40℃。又,以藉由流动相将电解液稀释100倍而成者作为测定用样品。使用化合物(E)制作检量线。
4-甲氧基丁酸的测定
藉由以下的测定条件进行。
机器:气相色谱仪、岛津制作所制造的GC-2010,管柱:J&W赛恩提菲克(J&W Scientific)公司制造的毛细管柱DBWAX(长度:30m,内径:0.53mm)或费诺美(phenomenex)公司制造的毛细管柱ZB-WAX普拉斯(ZB-WAX plus)(长度:30m,内径:0.25mm),检测器:火焰离子侦测器(Flame Ionization Detector,FID)或GCMS-QP2010,载气:氦气,气化室温度:200℃,检测器温度:250℃,管柱温度:自初始温度40℃起以10℃/分钟的速度升温至200℃后保持10分钟,注入量:1μl。使用4-甲氧基丁酸制作检量线。
关于本发明的实施例1~实施例15与比较例1~比较例5的电解液,将在密闭SUS(不锈钢制造)容器中于130℃下实施1000小时的耐热试验后的以下式表示的导电率的变化率示于表1。
导电率的变化率(%)=100×([耐热试验前的导电率]-[耐热试验后的导电率])/[耐热试验前的导电率]
使用本发明的实施例1~实施例15及比较例1~比较例5的电解液制作卷筒形的铝电解电容器(额定电压6.3 V-静电电容220μF,尺寸:φ6.5mm×L4.5mm)。使用过氧化物硫化的丁基橡胶作为封口胶。对所制作的铝电解电容器引加额定电压,观察3000小时后的封口体的情况。温度、湿度的条件按照以下3种实施。条件A:(温度105℃、湿度85%)、条件B:(温度130℃、湿度85%)、条件C:(温度140℃、湿度85%)
可知实施例1~实施例15与比较例1~比较例5相比几乎不存在漏液,且导电率变化率亦优异。
[产业上的可利用性]
藉由使用本发明的电解液,可提高电解电容器的可靠性,以使其即便处于周边环境进一步高温化或多湿条件,亦不会存在电解液自密封部泄漏的情况。本发明的电解液对于周边环境容易变成高温、多湿的汽车而言尤其有用。
Claims (6)
1.一种铝电解电容器用电解液,其含有非质子性溶剂(A)、包含下述通式(1)所表示的阳离子(B)与阴离子(C)的盐的电解质(D)、及下述通式(2)所表示的化合物(E),且相对于所述(A)及所述(D)的合计重量,所述化合物(E)的含量为0.01重量%~3重量%,
[式中,R1~R3为碳数1~3的烷基,R4~R7为碳数1~3的烷基或氢原子]
[式中,R8~R14为碳数1~3的烷基或氢原子]。
2.根据权利要求1所述的铝电解电容器用电解液,其进而含有4-甲氧基丁酸,且相对于所述(A)及所述(D)的合计重量,4-甲氧基丁酸的含量为含有0.1重量%以下。
3.根据权利要求1或2所述的铝电解电容器用电解液,其中所述阴离子(C)为羧酸阴离子、磷酸单烷基酯阴离子(烷基的碳数为1~15)或磷酸二烷基酯阴离子(烷基的碳数为1~15)。
4.根据权利要求1-3中任一项所述的铝电解电容器用电解液,其中所述阴离子(C)为邻苯二甲酸单阴离子或顺丁烯二酸单阴离子。
5.一种铝电解电容器,其是使用如权利要求1-4中任一项所述的电解液而成。
6.根据权利要求5所述的铝电解电容器,其是用于汽车。
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CN1708817A (zh) * | 2002-10-31 | 2005-12-14 | 三菱化学株式会社 | 电解电容器用电解液及电解电容器、以及有机鎓的四氟铝酸盐的制造方法 |
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CN104402820A (zh) * | 2014-12-02 | 2015-03-11 | 千辉药业(安徽)有限责任公司 | 一种1-乙基-2-甲基咪唑啉的合成方法 |
CN107868104A (zh) * | 2016-09-22 | 2018-04-03 | 深圳新宙邦科技股份有限公司 | 一种磷酸二烃基酯盐的制备方法 |
CN107892665A (zh) * | 2017-12-23 | 2018-04-10 | 山东吉田香料股份有限公司 | 一种n—乙基—2—乙酰基吡咯的制备方法 |
CN107892665B (zh) * | 2017-12-23 | 2021-05-11 | 山东吉田香料股份有限公司 | 一种n—乙基—2—乙酰基吡咯的制备方法 |
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US20150053882A1 (en) | 2015-02-26 |
JP2017224834A (ja) | 2017-12-21 |
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TWI608507B (zh) | 2017-12-11 |
CN104115245B (zh) | 2017-09-22 |
TW201349270A (zh) | 2013-12-01 |
MY182204A (en) | 2021-01-18 |
EP2843673B1 (en) | 2019-01-16 |
JP6186351B2 (ja) | 2017-08-23 |
WO2013161222A1 (ja) | 2013-10-31 |
JP6462063B2 (ja) | 2019-01-30 |
BR112014025791A2 (pt) | 2017-07-04 |
JPWO2013161222A1 (ja) | 2015-12-21 |
EP2843673A4 (en) | 2015-08-26 |
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