CN108183028A - Aluminium electrolutic capacitor flame retardant type heat cure gel polymer electrolyte and preparation method - Google Patents
Aluminium electrolutic capacitor flame retardant type heat cure gel polymer electrolyte and preparation method Download PDFInfo
- Publication number
- CN108183028A CN108183028A CN201711370061.7A CN201711370061A CN108183028A CN 108183028 A CN108183028 A CN 108183028A CN 201711370061 A CN201711370061 A CN 201711370061A CN 108183028 A CN108183028 A CN 108183028A
- Authority
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- China
- Prior art keywords
- acid
- ammonium
- flame retardant
- heat cure
- type heat
- Prior art date
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- Pending
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- 239000003990 capacitor Substances 0.000 title claims abstract description 31
- 238000013007 heat curing Methods 0.000 title claims abstract description 29
- 239000005518 polymer electrolyte Substances 0.000 title claims abstract description 29
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000004411 aluminium Substances 0.000 title claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 28
- 239000003063 flame retardant Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000178 monomer Substances 0.000 claims abstract description 40
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 29
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000003792 electrolyte Substances 0.000 claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 229920006037 cross link polymer Polymers 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 4
- 239000010452 phosphate Substances 0.000 claims abstract description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 93
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- 239000000499 gel Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 20
- 239000003431 cross linking reagent Substances 0.000 claims description 14
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 8
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- OTRAYOBSWCVTIN-UHFFFAOYSA-N OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N Chemical compound OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N OTRAYOBSWCVTIN-UHFFFAOYSA-N 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 6
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 6
- SATJMZAWJRWBRX-UHFFFAOYSA-N azane;decanedioic acid Chemical compound [NH4+].[NH4+].[O-]C(=O)CCCCCCCCC([O-])=O SATJMZAWJRWBRX-UHFFFAOYSA-N 0.000 claims description 6
- 235000011187 glycerol Nutrition 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 6
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 6
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 claims description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 5
- 239000001741 Ammonium adipate Substances 0.000 claims description 5
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 235000019293 ammonium adipate Nutrition 0.000 claims description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- BURBNIPKSRJAIQ-UHFFFAOYSA-N 2-azaniumyl-3-[3-(trifluoromethyl)phenyl]propanoate Chemical compound OC(=O)C(N)CC1=CC=CC(C(F)(F)F)=C1 BURBNIPKSRJAIQ-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 229940063284 ammonium salicylate Drugs 0.000 claims description 4
- 239000011245 gel electrolyte Substances 0.000 claims description 4
- 150000008301 phosphite esters Chemical class 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 4
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 3
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 3
- 229930188620 butyrolactone Natural products 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 2
- KWIPUXXIFQQMKN-UHFFFAOYSA-N 2-azaniumyl-3-(4-cyanophenyl)propanoate Chemical compound OC(=O)C(N)CC1=CC=C(C#N)C=C1 KWIPUXXIFQQMKN-UHFFFAOYSA-N 0.000 claims description 2
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical compound OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-UHFFFAOYSA-N 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical class C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical group CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 2
- ZDXPYRJPNDTMRX-VKHMYHEASA-N L-glutamine Chemical compound OC(=O)[C@@H](N)CCC(N)=O ZDXPYRJPNDTMRX-VKHMYHEASA-N 0.000 claims description 2
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
- 235000011037 adipic acid Nutrition 0.000 claims description 2
- 229940090948 ammonium benzoate Drugs 0.000 claims description 2
- NLVWBYNKMPGKRG-ODZAUARKSA-N azane;(z)-but-2-enedioic acid Chemical compound N.OC(=O)\C=C/C(O)=O NLVWBYNKMPGKRG-ODZAUARKSA-N 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 125000005619 boric acid group Chemical group 0.000 claims description 2
- 125000004386 diacrylate group Chemical group 0.000 claims description 2
- 125000005442 diisocyanate group Chemical group 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 235000013922 glutamic acid Nutrition 0.000 claims description 2
- 239000004220 glutamic acid Substances 0.000 claims description 2
- 229960002989 glutamic acid Drugs 0.000 claims description 2
- ZDXPYRJPNDTMRX-UHFFFAOYSA-N glutamine Natural products OC(=O)C(N)CCC(N)=O ZDXPYRJPNDTMRX-UHFFFAOYSA-N 0.000 claims description 2
- 229960002743 glutamine Drugs 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 2
- 150000002978 peroxides Chemical group 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims 2
- 230000005611 electricity Effects 0.000 claims 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims 1
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims 1
- 238000000016 photochemical curing Methods 0.000 claims 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims 1
- -1 phosphate compound Chemical class 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000012895 dilution Substances 0.000 abstract description 2
- 238000010790 dilution Methods 0.000 abstract description 2
- 150000003254 radicals Chemical class 0.000 abstract description 2
- 239000008151 electrolyte solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 238000002485 combustion reaction Methods 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 5
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 description 4
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical group OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 4
- 229930195725 Mannitol Natural products 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 235000010355 mannitol Nutrition 0.000 description 4
- 239000000594 mannitol Substances 0.000 description 4
- YLIZNYFVRHGNKF-UHFFFAOYSA-N 2-[2-(2-hydroxyethoxy)ethoxy]ethanol;methyl 2-methylprop-2-enoate Chemical group COC(=O)C(C)=C.OCCOCCOCCO YLIZNYFVRHGNKF-UHFFFAOYSA-N 0.000 description 3
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 3
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 3
- 239000000467 phytic acid Substances 0.000 description 3
- 229940068041 phytic acid Drugs 0.000 description 3
- 235000002949 phytic acid Nutrition 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- LRDFRRGEGBBSRN-UHFFFAOYSA-N isobutyronitrile Chemical compound CC(C)C#N LRDFRRGEGBBSRN-UHFFFAOYSA-N 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- H01G9/004—Details
- H01G9/022—Electrolytes; Absorbents
- H01G9/025—Solid electrolytes
- H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
-
- 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
- H01G9/0029—Processes of manufacture
- H01G9/0036—Formation of the solid electrolyte layer
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polymerisation Methods In General (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The present invention discloses a kind of aluminium electrolutic capacitor flame retardant type heat cure gel polymer electrolyte and preparation method, which includes the cross-linked polymer that acrylic monomer is formed and the phosphate compounds, solute, solvent, the thermal initiator that are dispersed in cross-linked polymer.Phosphate compounds can be very good dissolving in the electrolytic solution, and the cross-linked polymer of tridimensional network is formed when electrolyte polymerize, and phosphate compound is just evenly distributed in cross-linked polymer.Aluminium electrolutic capacitor with flame retardant type heat cure gel polymer electrolyte when burning, into carbon so as to which solute be prevented further to burn when phosphate compounds can promote the solute to burn, and PO, PO that phosphate compounds are thermally decomposed2、HPO2Small molecule can effectively reduce dilution low hydrogen number of free radical, make fray-out of flame.Thus heat cure gel polymer electrolyte is nonflammable, improves the safety of capacitor.
Description
Technical field
The present invention relates to solute field, particularly aluminium electrolutic capacitor with flame retardant type heat cure gel polymer electrolyte and
Preparation method.
Background technology
Existing aluminium electrolutic capacitor is mostly acrylic acid or its derivative with gel electrolyte with monomer, is highly combustible；
The electrolyte filled in gel electrolyte, it is molten that solvent is generally the inflammabilities such as ethylene glycol, diethylene glycol (DEG), glycerine, γ ~ butyrolactone, DMF
Agent.Also easily burning after gel electrolyte polymerization, leads to using its capacitor that there is also larger security risks.
Invention content
Based on this, it is necessary to for existing gelatin polymer solute it is inflammable the problem of, a kind of alminium electrolytic condenser is provided
Device flame retardant type heat cure gel polymer electrolyte and preparation method thereof.
A kind of aluminium electrolutic capacitor flame retardant type heat cure gel polymer electrolyte is formed including acrylic monomer
Cross-linked polymer and phosphate compounds, solute, the solvent being dispersed in cross-linked polymer.
Acrylic monomer is acrylic acid, methacrylic acid, maleic acid, methyl acrylate, methyl methacrylate
One or more of with acrylamide.
Phosphate compounds are phosphate, phosphite ester, tricresyl phosphate, tributyl phosphate and polymer phosphorus（Phosphine）
It is one or more in acid esters.
Solute is boric acid, ammonium pentaborate, ammonium formate, ammonium adipate, ammonium sebacate, isosebacic acid ammonium, azelaic acid hydrogen ammonium, ten
Two bisgallic acid ammoniums, ammonium benzoate, suberic acid, decanedioic acid, azelaic acid, 1,6 ~ decane dicarboxylic acid, maleic acid ammonium, ethanedioic acid, malonic acid,
One or more of adipic acid, ammonium adipate, salicylic acid, ammonium salicylate, glutamic acid and glutamine.
Solvent is ethylene glycol, diethylene glycol (DEG), glycerine, γ ~ one or more of butyrolactone and DMF.
Further, acrylic monomer is the one of acrylic acid, methacrylic acid, methyl methacrylate and acrylamide
Kind is several.
Phosphate compounds are one or more in phosphite ester, tricresyl phosphate and tributyl phosphate.
Solute is one or more of ammonium pentaborate, ammonium sebacate and ammonium salicylate.
One or more of the solvent for ethylene glycol and glycerine.
Further, aluminium electrolutic capacitor further includes disappear hydrogen agent and waterproof with flame retardant type heat cure gel polymer electrolyte
Mixture.
A kind of aluminium electrolutic capacitor flame retardant type heat cure method for preparing gel polymer electrolyte, including following step
Suddenly：
Acrylic monomer with crosslinking agent is mixed, 1 ~ 100min is stirred under the conditions of 0 ~ 100 DEG C, and add in thermal initiator, after
1 ~ 100min of continuous stirring, obtains monomer solution.
Solvent and solute is taken to mix, stir 1 under the conditions of 0 ~ 200 DEG C ~ for 24 hours, disappear hydrogen agent and waterproof mixture are then added in, after
Continue at 0 ~ 200 DEG C stirring 1 ~ for 24 hours, obtain electrolyte.
Monomer solution is mixed with electrolyte, and add in thereto phosphate compounds stir 1 at 20 ~ 200 DEG C ~
After for 24 hours, 1 ~ 12h is preserved under 50 ~ 200 DEG C of environment, obtains aluminium electrolutic capacitor flame retardant type heat cure gel polymer electrolyte
Matter.
Further, acrylic monomer is measured in molar ratio with crosslinking agent（100~30）：1 mixing, the addition of thermal initiator
It measures as 1 ‰ -1% for monomer molar amount.
Solvent and solute mixing hot plate mass ratio as (1 ~ 20)：1, the addition of additive is the 1%- of total soluble matters quality
20%。
Monomer solution and electrolyte with（1~2）：（1~10）Mass ratio mixing, the addition of phosphate compounds is mixed
Close the 1 ‰ -10% of liquid quality.
Further, crosslinking agent is hydroxyethyl methacrylate, polyethyleneglycol diacrylate, dimethacrylate second two
Alcohol ester, N,N methylene bis acrylamide, divinylbenzene, diisocyanate, polyethylene glycol, polypropylene glycol, trihydroxy methyl third
One or more of alkane and butyl acrylate.
Further,
Thermal initiator is peroxides initiator, azodiisobutyronitrile, dibenzoyl peroxide and the N such as sodium peroxydisulfate, ammonium persulfate,
One or more of N- dimethylanilines.
Above-mentioned aluminium electrolutic capacitor flame retardant type heat cure gel polymer electrolyte, phosphate compounds can be fine
The electrolyte for being dissolved in solvent and solute and being formed in, the cross-linked polymeric of tridimensional network is formed when electrolyte polymerize
Object, phosphate compound are just evenly distributed in cross-linked polymer, obtain aluminium electrolutic capacitor flame retardant type heat cure gel
Polymer dielectric.Aluminium electrolutic capacitor with flame retardant type heat cure gel polymer electrolyte burning when, phosphoric acid ester
Into carbon so as to which solute be prevented further to burn when compound can promote the solute to burn, and phosphate compounds are thermally decomposed
PO, PO2、HPO2Small molecule can effectively reduce dilution low hydrogen number of free radical, make fray-out of flame.Thus aluminium electrolutic capacitor
It is nonflammable with flame retardant type heat cure gel polymer electrolyte, improve the safety of capacitor.
Specific embodiment
Embodiment 1
（1）It is prepared by monomer solution：1st, 50g acrylic monomers with 5g crosslinking agents are mixed, 20min is stirred under the conditions of 25 DEG C.
Wherein, acrylic monomer is acrylic acid, and crosslinking agent is triethylene glycol methyl methacrylate.
2nd, thermal initiator 0.1g is added in mixed monomer solution, continues to stir 20min.Thermal initiator is sodium peroxydisulfate.
（2）It is prepared by electrolyte：Solvent 100g is taken, solute 25g mixing stirs 2h under the conditions of 105 DEG C.Then addition is added in
Agent 5g continues to stir 1h at 100 DEG C.Wherein, solvent is ethylene glycol, glycerine, water, and solute is ammonium sebacate, ammonium pentaborate
Mixture, additive is mannitol, the mixture of phytic acid, paranitrobenzoic acid ammonium.
（3）It is prepared by preceding oligomer solution:Monomer solution is mixed with electrolysis.Phosphate compounds 10g is added in thereto to exist
1h is stirred at 25 DEG C.Phosphate compounds are tricresyl phosphate.
（4）Polymerization：Preceding oligomer solution is preserved into 2h under 85 DEG C of environment, obtains aluminium electrolutic capacitor flame retardant type heat cure
Gel polymer electrolyte.
The aluminium electrolutic capacitor of preparation is taken to carry out 94UL vertical combustions reality with flame retardant type heat cure gel polymer electrolyte
It tests.
94UL experimentations：
Gel polymer electrolyte is suspended on iron stand, the vertical combustion of 10 seconds is carried out to it using alcolhol burner, removes wine
Whether smart lamp observation flame extinguishes, if has comburant to fall down, and records the time that fray-out of flame is removed to from alcolhol burner.If not yet
There is burning, carry out second of 10 seconds vertical combustion, remove whether alcolhol burner observation flame extinguishes, record from alcolhol burner and be removed to fire
The time that flame extinguishes, if there is comburant to fall down, and record the time that fray-out of flame is removed to from alcolhol burner.
。
Embodiment 2
（1）It is prepared by monomer solution：1st, 50g acrylic monomers with 5g crosslinking agents are mixed, 20min is stirred under the conditions of 25 DEG C.
Wherein, acrylic monomer is methyl methacrylate, and crosslinking agent is triethylene glycol methyl methacrylate.
2nd, thermal initiator 0.1g is added in mixed monomer solution, continues to stir 30min.Thermal initiator is ammonium persulfate.
（2）It is prepared by electrolyte：Solvent 100g is taken, solute 30g mixing stirs 1h under the conditions of 85 DEG C.Then addition is added in
Agent 8g continues to stir 1h at 100 DEG C.Wherein, solvent is gamma-butyrolacton, ethylene glycol, and solute is ammonium formate, ammonium adipate, is added
Add agent for mannitol, phytic acid, paranitrobenzoic acid ammonium.
（3）It is prepared by preceding oligomer solution:Monomer solution is mixed with electrolyte matter.Phosphate compounds are added in thereto
10g stirs 1h at 25 DEG C.Phosphate compounds are tributyl phosphate.
（4）Polymerization：Preceding oligomer solution is preserved into 1h under 85 DEG C of environment, obtains aluminium electrolutic capacitor flame retardant type heat cure
Gel polymer electrolyte.
The aluminium electrolutic capacitor of preparation is taken to carry out 94UL vertical combustions reality with flame retardant type heat cure gel polymer electrolyte
It tests.
94UL experimentations：
Gel polymer electrolyte is suspended on iron stand, the vertical combustion of 10 seconds is carried out to it using alcolhol burner, removes wine
Whether smart lamp observation flame extinguishes, if has comburant to fall down, and records the time that fray-out of flame is removed to from alcolhol burner.If not yet
There is burning, carry out second of 10 seconds vertical combustion, remove whether alcolhol burner observation flame extinguishes, record from alcolhol burner and be removed to fire
The time that flame extinguishes, if there is comburant to fall down, and record the time that fray-out of flame is removed to from alcolhol burner.
。
Embodiment 3
（1）It is prepared by monomer solution：1st, 50g acrylic monomers with 2g crosslinking agents are mixed, 20min is stirred under the conditions of 25 DEG C.
Wherein, acrylic monomer is acrylamide, crosslinking agent N, N- methylene-bisacrylamide.
2nd, thermal initiator 0.1g is added in mixed monomer solution, continues 1 ~ 100min of stirring.Thermal initiator is azo two
Isobutyronitrile.
（2）It is prepared by electrolyte：Solvent 100g is taken, solute 25g mixing stirs 2h under the conditions of 105 DEG C.Then addition is added in
Agent 5g continues to stir 1h at 100 DEG C.Wherein, solvent is ethylene glycol, and solute is ammonium sebacate, additive is mannitol, plants
Acid, paranitrobenzoic acid ammonium.
（3）It is prepared by preceding oligomer solution:Monomer solution is mixed with electrolyte.Phosphate compounds 4g is added in thereto to exist
1h is stirred at 50 DEG C.Phosphate compounds are tricresyl phosphate.
（4）Polymerization：Preceding oligomer solution is preserved into 3h under 85 DEG C of environment, obtains aluminium electrolutic capacitor flame retardant type heat cure
Gel polymer electrolyte.
94UL experimentations：
Gel polymer electrolyte is suspended on iron stand, the vertical combustion of 10 seconds is carried out to it using alcolhol burner, removes wine
Whether smart lamp observation flame extinguishes, if has comburant to fall down, and records the time that fray-out of flame is removed to from alcolhol burner.If not yet
There is burning, carry out second of 10 seconds vertical combustion, remove whether alcolhol burner observation flame extinguishes, record from alcolhol burner and be removed to fire
The time that flame extinguishes, if there is comburant to fall down, and record the time that fray-out of flame is removed to from alcolhol burner.
。
Embodiment 4
（1）It is prepared by monomer solution：1st, 100g acrylic monomers with 6g crosslinking agents are mixed, 30min is stirred under the conditions of 25 DEG C.
Wherein, acrylic monomer is methacrylic acid, and crosslinking agent is triethylene glycol methyl methacrylate.
2nd, thermal initiator 0.2g is added in mixed monomer solution, continues to stir 40min.Thermal initiator is ammonium persulfate.
（2）It is prepared by electrolyte：Solvent 100g is taken, solute 30g mixing stirs 1h under the conditions of 85 DEG C.Then addition is added in
Agent 5g continues to stir 2h at 85 DEG C.Wherein, solvent is ethylene glycol, solute is ammonium pentaborate, additive be mannitol, phytic acid,
Paranitrobenzoic acid ammonium.
（3）It is prepared by preceding oligomer solution:Monomer solution is mixed with electrolyte.Phosphate compounds 10g is added in thereto
1h is stirred at 25 DEG C.Phosphate compounds are tributyl phosphate
（4）Polymerization：Preceding oligomer solution is preserved into 1h under 85 DEG C of environment, obtains aluminium electrolutic capacitor flame retardant type heat cure gel
Polymer dielectric.
94UL experimentations：
Gel polymer electrolyte is suspended on iron stand, the vertical combustion of 10 seconds is carried out to it using alcolhol burner, removes wine
Whether smart lamp observation flame extinguishes, if has comburant to fall down, and records the time that fray-out of flame is removed to from alcolhol burner.If not yet
There is burning, carry out second of 10 seconds vertical combustion, remove whether alcolhol burner observation flame extinguishes, record from alcolhol burner and be removed to fire
The time that flame extinguishes, if there is comburant to fall down, and record the time that fray-out of flame is removed to from alcolhol burner.
。
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (7)
1. a kind of aluminium electrolutic capacitor flame retardant type heat cure gel polymer electrolyte, which is characterized in that including acrylic compounds
The cross-linked polymer that monomer is formed and phosphate compounds, solute, the solvent being dispersed in the cross-linked polymer；
The acrylic monomer is acrylic acid, methacrylic acid, maleic acid, methyl acrylate, methyl methacrylate
One or more of with acrylamide；
The phosphate compounds are phosphate, phosphite ester, tricresyl phosphate, tributyl phosphate and polymer phosphorus（Phosphine）
It is one or more in acid esters；
The solute is boric acid, ammonium pentaborate, ammonium formate, ammonium adipate, ammonium sebacate, isosebacic acid ammonium, azelaic acid hydrogen ammonium, ten
Two bisgallic acid ammoniums, ammonium benzoate, suberic acid, decanedioic acid, azelaic acid, 1,6 ~ decane dicarboxylic acid, maleic acid ammonium, ethanedioic acid, malonic acid,
One or more of adipic acid, ammonium adipate, salicylic acid, ammonium salicylate, glutamic acid and glutamine；
The solvent is ethylene glycol, diethylene glycol (DEG), glycerine, γ ~ one or more of butyrolactone and DMF.
2. aluminium electrolutic capacitor according to claim 1 flame retardant type heat cure gel polymer electrolyte, feature exist
In the acrylic monomer is the one or more of acrylic acid, methacrylic acid, methyl methacrylate and acrylamide；
The phosphate compounds are one or more in phosphite ester, tricresyl phosphate and tributyl phosphate；
The solute is one or more of ammonium pentaborate, ammonium sebacate and ammonium salicylate；
One or more of the solvent for ethylene glycol and glycerine.
3. aluminium electrolutic capacitor according to claim 1 flame retardant type heat cure gel polymer electrolyte, feature exist
In the aluminium electrolutic capacitor further includes disappear hydrogen agent and waterproof mixture with flame retardant type heat cure gel polymer electrolyte.
4. a kind of aluminium electrolutic capacitor according to any one of claim 1 ~ 3 flame retardant type heat cure gelatin polymer electricity
Solve the preparation method of matter, which is characterized in that include the following steps：
Acrylic monomer with crosslinking agent is mixed, 1 ~ 100min is stirred under the conditions of 0 ~ 100 DEG C, and add in thermal initiator, after
1 ~ 100min of continuous stirring, obtains monomer solution；
Solvent and solute is taken to mix, stir 1 under the conditions of 0 ~ 200 DEG C ~ for 24 hours, disappear hydrogen agent and waterproof mixture are then added in, is continued
At 0 ~ 200 DEG C stirring 1 ~ for 24 hours, obtain electrolyte；
The monomer solution with the electrolyte is mixed, and adds in phosphate compounds thereto and is stirred at 20 ~ 200 DEG C
1 ~ for 24 hours after, under 50 ~ 200 DEG C of environment preserve 1 ~ 12h, obtain aluminium electrolutic capacitor flame retardant type heat cure gelatin polymer electricity
Xie Zhi.
5. the preparation method of the gel electrolyte of photocuring according to claim 4, which is characterized in that acrylic monomer
It is measured in molar ratio with crosslinking agent（100~30）：1 mixing, the addition of the thermal initiator is the 1 ‰ -1% of monomer molar amount；
Solvent and solute mixing hot plate mass ratio as (1 ~ 20)：1, the addition of the additive is the 1%- of total soluble matters quality
20%；
The monomer solution and the electrolyte with（1~2）：（1~10）Mass ratio mixing, the phosphate compounds plus
Enter 1 ‰ -10% that amount is mixing liquid quality.
6. the aluminium electrolutic capacitor according to claim 4 preparation side of flame retardant type heat cure gel polymer electrolyte
Method, which is characterized in that
The crosslinking agent is hydroxyethyl methacrylate, polyethyleneglycol diacrylate, ethylene glycol dimethacrylate, N, N-
Methylene-bisacrylamide, divinylbenzene, diisocyanate, polyethylene glycol, polypropylene glycol, trimethylolpropane and acrylic acid
One or more of butyl ester.
7. the aluminium electrolutic capacitor flame retardant type heat cure gel polymer electrolyte according to any one of claim 4 ~ 6
Preparation method, which is characterized in that
The thermal initiator is peroxides initiator, azodiisobutyronitrile, the dibenzoyl peroxides such as sodium peroxydisulfate, ammonium persulfate
And one or more of N, N- dimethylaniline.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108878969A (en) * | 2018-06-29 | 2018-11-23 | 华南师范大学 | A kind of fire-retardant gel polymer electrolyte and its preparation and application |
| CN110690050A (en) * | 2019-10-15 | 2020-01-14 | 厦门法拉和信电子有限公司 | Novel gel electrolyte manufacturing method and aluminum electrolytic capacitor |
| WO2020125519A1 (en) * | 2018-12-17 | 2020-06-25 | 深圳先进技术研究院 | Flame-retardant polymer gel electrolyte and preparation method therefor, and lithium battery |
| CN113363078A (en) * | 2021-07-28 | 2021-09-07 | 深圳市金富康电子有限公司 | Solid-liquid mixed state winding type aluminum electrolytic capacitor and preparation method thereof |
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| CN113363078A (en) * | 2021-07-28 | 2021-09-07 | 深圳市金富康电子有限公司 | Solid-liquid mixed state winding type aluminum electrolytic capacitor and preparation method thereof |
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