CN114380288A - 一种利用阻燃原理空气气氛下制备多孔炭材料的方法 - Google Patents
一种利用阻燃原理空气气氛下制备多孔炭材料的方法 Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 56
- 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 54
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000011294 coal tar pitch Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 4
- -1 transition metal borates Chemical class 0.000 claims description 4
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 3
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 239000011698 potassium fluoride Substances 0.000 claims description 3
- 235000003270 potassium fluoride Nutrition 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 4
- 229910052723 transition metal Inorganic materials 0.000 claims 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims 2
- 229910019142 PO4 Inorganic materials 0.000 claims 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims 2
- DOVLHZIEMGDZIW-UHFFFAOYSA-N [Cu+3].[O-]B([O-])[O-] Chemical compound [Cu+3].[O-]B([O-])[O-] DOVLHZIEMGDZIW-UHFFFAOYSA-N 0.000 claims 2
- 150000001642 boronic acid derivatives Chemical class 0.000 claims 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims 2
- DDSZSJDMRGXEKQ-UHFFFAOYSA-N iron(3+);borate Chemical compound [Fe+3].[O-]B([O-])[O-] DDSZSJDMRGXEKQ-UHFFFAOYSA-N 0.000 claims 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims 2
- 235000021317 phosphate Nutrition 0.000 claims 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims 2
- 239000011295 pitch Substances 0.000 claims 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims 2
- 150000003624 transition metals Chemical class 0.000 claims 2
- QGBLCIBATKETJC-UHFFFAOYSA-N 3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;manganese(2+) Chemical compound [Mn+2].O1B([O-])OB2OB([O-])OB1O2 QGBLCIBATKETJC-UHFFFAOYSA-N 0.000 claims 1
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims 1
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims 1
- 239000005750 Copper hydroxide Substances 0.000 claims 1
- 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 claims 1
- 229920000877 Melamine resin Polymers 0.000 claims 1
- 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 claims 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims 1
- ZQKXOSJYJMDROL-UHFFFAOYSA-H aluminum;trisodium;diphosphate Chemical compound [Na+].[Na+].[Na+].[Al+3].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZQKXOSJYJMDROL-UHFFFAOYSA-H 0.000 claims 1
- 235000019270 ammonium chloride Nutrition 0.000 claims 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims 1
- 229910021538 borax Inorganic materials 0.000 claims 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims 1
- 239000000920 calcium hydroxide Substances 0.000 claims 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims 1
- 235000011132 calcium sulphate Nutrition 0.000 claims 1
- 239000004202 carbamide Substances 0.000 claims 1
- WEZJBAOYGIDDLB-UHFFFAOYSA-N cobalt(3+);borate Chemical compound [Co+3].[O-]B([O-])[O-] WEZJBAOYGIDDLB-UHFFFAOYSA-N 0.000 claims 1
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims 1
- 229940116318 copper carbonate Drugs 0.000 claims 1
- 229910001956 copper hydroxide Inorganic materials 0.000 claims 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 claims 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims 1
- 235000019838 diammonium phosphate Nutrition 0.000 claims 1
- VLCINIKIVYNLPT-UHFFFAOYSA-J dicalcium;hydrogen phosphate Chemical compound [Ca+2].[Ca+2].OP(O)([O-])=O.[O-]P([O-])([O-])=O VLCINIKIVYNLPT-UHFFFAOYSA-J 0.000 claims 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims 1
- 235000019820 disodium diphosphate Nutrition 0.000 claims 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims 1
- GYQBBRRVRKFJRG-UHFFFAOYSA-L disodium pyrophosphate Chemical compound [Na+].[Na+].OP([O-])(=O)OP(O)([O-])=O GYQBBRRVRKFJRG-UHFFFAOYSA-L 0.000 claims 1
- 235000014413 iron hydroxide Nutrition 0.000 claims 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims 1
- 229910052808 lithium carbonate Inorganic materials 0.000 claims 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims 1
- 239000000347 magnesium hydroxide Substances 0.000 claims 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims 1
- 235000019341 magnesium sulphate Nutrition 0.000 claims 1
- 239000011656 manganese carbonate Substances 0.000 claims 1
- 235000006748 manganese carbonate Nutrition 0.000 claims 1
- 229940093474 manganese carbonate Drugs 0.000 claims 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims 1
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims 1
- 229910001507 metal halide Inorganic materials 0.000 claims 1
- 235000019837 monoammonium phosphate Nutrition 0.000 claims 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims 1
- 235000019799 monosodium phosphate Nutrition 0.000 claims 1
- 230000007935 neutral effect Effects 0.000 claims 1
- HKFZDVPCCOOGEV-UHFFFAOYSA-N nickel(3+);borate Chemical compound [Ni+3].[O-]B([O-])[O-] HKFZDVPCCOOGEV-UHFFFAOYSA-N 0.000 claims 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims 1
- 150000002823 nitrates Chemical class 0.000 claims 1
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 claims 1
- 239000000467 phytic acid Substances 0.000 claims 1
- 229940068041 phytic acid Drugs 0.000 claims 1
- 235000002949 phytic acid Nutrition 0.000 claims 1
- OQZCJRJRGMMSGK-UHFFFAOYSA-M potassium metaphosphate Chemical compound [K+].[O-]P(=O)=O OQZCJRJRGMMSGK-UHFFFAOYSA-M 0.000 claims 1
- 229940099402 potassium metaphosphate Drugs 0.000 claims 1
- 235000010333 potassium nitrate Nutrition 0.000 claims 1
- 239000004323 potassium nitrate Substances 0.000 claims 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims 1
- 229910052939 potassium sulfate Inorganic materials 0.000 claims 1
- 235000011151 potassium sulphates Nutrition 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 239000011780 sodium chloride Substances 0.000 claims 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims 1
- 239000011775 sodium fluoride Substances 0.000 claims 1
- 235000013024 sodium fluoride Nutrition 0.000 claims 1
- 235000010344 sodium nitrate Nutrition 0.000 claims 1
- 239000004317 sodium nitrate Substances 0.000 claims 1
- 235000010339 sodium tetraborate Nutrition 0.000 claims 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims 1
- 229910000299 transition metal carbonate Inorganic materials 0.000 claims 1
- WUUHFRRPHJEEKV-UHFFFAOYSA-N tripotassium borate Chemical compound [K+].[K+].[K+].[O-]B([O-])[O-] WUUHFRRPHJEEKV-UHFFFAOYSA-N 0.000 claims 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 10
- 239000003990 capacitor Substances 0.000 abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 239000007772 electrode material Substances 0.000 abstract description 6
- 238000000227 grinding Methods 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 21
- 238000012360 testing method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000007833 carbon precursor Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 229910017053 inorganic salt Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 102000020897 Formins Human genes 0.000 description 2
- 108091022623 Formins Proteins 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229940031958 magnesium carbonate hydroxide Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明公开了一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，按如下方法进行制备：将煤沥青与阻燃剂研磨均匀形成混合物，之后将混合物放入坩埚中，在马弗炉内一定温度下进行煅烧，待反应结束后冷却至室温取出。将所得产物用酸和水洗涤去除杂质，获得多孔炭材料。本发明制备的多孔炭材料具有较高的炭产率、大的比表面积和分级多孔结构，作为超级电容器电极材料表现出优异的电容性能。此方法不同于传统惰性气氛保护的碳材料制备方法，降低了成本与资源的消耗，是一种绿色、简单、经济高效、可控的制备方法。并且此制备方法操作简单、合成周期短，适合于大规模工业化生产，此方法在高性能多孔炭电极材料的制备及应用方面具有重要意义。
Description
技术领域
本发明涉及一种利用阻燃原理空气气氛下制备多孔炭材料的方法，并将其用作高性能超级电容器电极材料
背景技术
近代以来，随着对化石燃料等不可再生能源的过度开采与利用，人类面临着能源危机与环境污染两大难题，大力发展绿色清洁可持续能源是解决问题的重要途径之一。其中，超级电容器作为一类重要的储能器件，由于超快的充放电能力和超强的循环寿命，引起人们的广泛关注与研究。电极材料的不同直接影响着超级电容器的储能机理，从而进一步影响着超级电容器的性能与循环寿命。碳基电极材料具有好的化学稳定性，优良的导电性，并且来源丰富，价格低廉。因此，碳基材料作为超级电容器的电极具有广阔的应用前景。
以碳质材料为前驱体，在惰性气体气氛(如N2和Ar等)下经高温碳化是制备炭材料的通常方法，该方法需要消耗纯度较高的惰性气体以及苛刻的技术和设备要求，阻碍了商业化生产。在空气中制备炭材料是一种方便，低成本的制备策略。但是，碳前驱体在空气下高温炭化会发生燃烧。因此，开发一种在空气气氛下经高温煅烧制备炭材料的方法具有重要的现实意义。
阻燃剂是一种用以提高材料抗燃性，阻止材料被引燃和防止火焰传播的助剂。阻燃剂常用于高分子材料上，起到阻止材料燃烧的作用。近年来，阻燃剂也被应用到制备纳米材料领域，进一步拓宽了其应用范围。阻燃剂的阻燃机理主要有气相阻燃、链反应中断阻燃、凝聚相阻燃、吸热阻燃、气源膨胀型阻燃等。
发明内容
本发明在于提供一种利用阻燃原理在空气气氛下制备多孔炭材料的方法。
本发明涉及一种无惰性气体保护下多孔炭材料的制备方法。利用阻燃剂的阻燃原理，保护碳前体不会在高温下燃烧殆尽，同时阻燃剂还可充当模板剂和造孔剂，从而炭化生成多孔炭材料。将制得的多孔炭用于超级电容器电极材料，显示出优异的电容性能。
制备过程主要包括以下几步。
称取总量为0.25g的煤焦油沥青，过量的阻燃剂(阻燃剂的质量：煤焦油沥青质量≥2)放于玛瑙研钵中，充分研磨至混合均匀。将混合物放入坩埚中，将坩埚置于马弗炉内，于600～800℃煅烧1～3小时(升温速率为1～10℃min-1)，自然冷却至室温后取出，酸洗，水洗至中性。随后放入烘箱干燥得到多孔炭材料。
本发明的有益效果主要体现在：
(1)本发明提供一种在空气气氛，阻燃剂辅助制备多孔炭材料的方法。此方法对设备要求低，可廉价、快速、大规模制备多孔炭材料。
(2)制备过程简单，安全高效，制备流程少周期短。
(3)制备的功能炭材料，有较高的炭产率，且在超级电容器应用上展现了较优的电化学性能。
附图说明
实施例1的形貌分析使用SU8010型场发射扫描电镜进行观察如图1。
实施例1的氮气吸脱附曲线测定采用Autosorb-IQ instruments(Quantachrome)如图2所示。
实施例1在6mol L-1氢氧化钾中超级电容器三电极电化学性能图如图3。
实施例2的形貌分析使用SU8010型场发射扫描电镜进行观察如图4。
实施例2在6mol L-1氢氧化钾中超级电容器三电极电化学性能图如图5。
实施例3的形貌分析使用SU8010型场发射扫描电镜进行观察如图6。
实施例3在6mol L-1氢氧化钾中超级电容器三电极电化学性能图如图7。
实施例4的形貌分析使用SU8010型场发射扫描电镜进行观察如图8。
实施例4在6mol L-1氢氧化钾中超级电容器三电极电化学性能图如图9。
具体实施方式
实施例一
煤焦油沥青具有价格低廉、来源广泛、易石墨化、粘附性好等特点。以煤焦油沥青作为碳前驱体，碳酸钾-氯化钾-氟化钾熔融盐作为凝聚相阻燃剂。
称取0.25g煤焦油沥青，0.196g氟化钾，0.437g氯化钾，0.75g碳酸钾(煤沥青和阻燃剂质量比为1:5.5)，将其放入玛瑙研钵中充分研磨。将混合物放入坩埚中，于马弗炉内在空气气氛下以5℃ min-1加热至700℃进行高温碳化，保温2小时，自然冷却到室温后取出，水洗去无机盐，随后放入烘箱干燥得到最终产物。最终炭产率为40.2％。
由SEM结果(图1)可知材料的形貌为蜂窝状多孔结构。氮气吸脱附曲线氮吸附/解吸等温线测定比表面积可达1368m2 g-1(图2)。6mol L-1KOH电解液中，循环伏安法测试为典型双电层电容行为，恒流充放电测试在1A g-1，4A g-1，10A g-1电流密度下比电容分别为261.2Fg-1，201.3F g-1，199.3F g-1(图3)。
实施例二以煤焦油沥青作为碳前驱体，碳酸钾作为气相阻燃剂。
称取0.25g煤焦油沥青，0.75g碳酸钾作为气相阻燃剂(煤沥青和阻燃剂质量比为1:3)，将混合物放入坩埚中，置于马弗炉内，在空气气氛下700℃，5℃ min-1进行高温碳化，保温2小时，冷却至室温后取出。水洗去无机盐，随后放入烘箱干燥得到最终产物。最终炭产率为26.8％
由SEM结果(图4)可知材料的形貌为不规则的蜂窝状多孔结构。6mol L-1KOH电解液中，循环伏安法测试为典型双电层电容行为，恒流充放电测试在1A g-1，4A g-1，10A g-1电流密度下比电容分别为215.2F g-1，192.8F g-1，185F g-1(图5)。
实施例三
以煤焦油沥青作为碳前驱体，碱式碳酸镁、氢氧化铝为吸热阻燃剂，聚磷酸铵为气相阻燃剂，三者配比成为复合阻燃剂。
称取0.25g煤焦油沥青，0.25g碱式碳酸镁、0.25g氢氧化铝、0.25g聚磷酸铵作为复合阻燃剂(煤沥青和阻燃剂质量比为1:3)，将其放入玛瑙研钵中充分研磨。将混合物放入坩埚中，置于马弗炉内，在空气气氛下700℃，5℃ min-1进行高温碳化，保温2小时，冷却到室温后取出。酸洗、水洗去无机盐，随后放入烘箱干燥得到最终产物。最终炭产率为34.3％。
由SEM结果(图6)可知材料的形貌为不规则的块状结构。6mol L-1KOH电解液中，循环伏安法测试为典型双电层电容行为，恒流充放电测试在1A g-1，4A g-1，10A g-1电流密度下比电容分别为88F g-1，69F g-1，22F g-1(图7)。
实施例四
以煤焦油沥青作为碳前驱体，碳酸钾-氯化钾-氟化钾熔融盐作为凝聚相阻燃剂。
称取0.25g煤焦油沥青，0.065g氟化钾，0.146g氯化钾，0.25g碳酸钾(煤沥青和阻燃剂质量比为1:1.8)，将其放入玛瑙研钵中充分研磨。将混合物放入坩埚中，置于马弗炉内，在空气气氛下700℃，5℃ min-1进行高温碳化，保温2小时，冷却到室温后取出。酸洗、水洗去无机盐，随后放入烘箱干燥得到最终产物。最终炭产率为20.1％。
在此质量比下，得到的炭材料产率与性能较差。原因是由于阻燃剂的量较少，无法完全起到阻燃效果，并且活化效果较差。
由SEM结果(图8)可知材料的形貌为活化不均匀的多孔结构。6mol L-1KOH电解液中，循环伏安法测试为典型双电层电容行为，恒流充放电测试在1A g-1，4A g-1，10A g-1电流密度下比电容分别为199.6F g-1，158.2F g-1，132.2F g-1(图9)。
Claims (8)
1.一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，所述方法如下：
(1)称取0.25g煤焦油沥青和阻燃剂(阻燃剂与沥青质量比≥2)混合于玛瑙研钵中充分研磨30min，放入坩埚中。
(2)将坩埚置于马弗炉内，使其在空气下600～800℃高温碳化，升温速率为1～10℃min-1，保温1～3h，自然冷却至室温。
(3)取出坩埚，酸洗去除杂质，水洗至中性，得到的样品放入烘箱干燥，得到高产率，分级多孔结构的多孔炭材料。
2.根据权利要求1所述的一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，其特征在于步骤(1)所述的阻燃剂为气相阻燃剂、凝聚相阻燃剂、吸热阻燃剂、气源膨胀阻燃剂的一种或多种。
3.根据权利要求1所述的一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，其特征在于步骤(1)所述的阻燃剂为气相阻燃剂，气相阻燃剂可为三聚氰胺、尿素、双氰胺、氰尿酸、氯化铵、碳酸钾、碳酸钙和过渡金属碳酸盐中的一种或多种。
4.根据权利要求1所述的一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，其特征在于步骤(1)所述的阻燃剂为凝聚相阻燃剂，凝聚相阻燃剂可为无机盐、磷酸盐、硼酸盐中的一种或多种。常见的无机盐为金属卤盐(氯化钾、氯化钠、氯化锂、氟化钾、氟化钠、氟化锂等)、碳酸盐(碳酸钾、碳酸钠、碳酸锂等)、硝酸盐(硝酸钠、硝酸钾、硝酸镁等)、硫酸盐(硫酸钾、硫酸钙、硫酸镁等)。常见磷酸盐为植酸、聚磷酸铵、磷酸二氢铵、磷酸二氢钠、磷酸氢二钠、磷酸氢二铵、磷酸氢二钙、酸式焦磷酸钠、聚偏磷酸钾、焦磷酸钾、磷酸铝钠、过渡金属硼酸盐，例如硼酸铜、硼酸铁等。常见硼酸盐为、硼酸钾、硼酸钠、过渡金属硼酸盐，例如硼酸锌、硼酸锰、硼酸铁、硼酸镍、硼酸铜、硼酸钴等。
5.根据权利要求2所述的一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，其特征在于步骤(1)所述的吸热阻燃剂为氢氧化镁、氢氧化铝、氢氧化钙及其过渡金属氢氧化物，例如氢氧化铁、氢氧化铜，氢氧化钴，氢氧化镍等以及碱式碳酸镁、碱式碳酸钙及其过渡金属碱式碳酸盐，例如碱式碳酸锌、碱式碳酸铜、碱式碳酸锰、碱式碳酸镍等中的一种或以上。
6.根据权利要求1所述的一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，其特征在于步骤(1)所述的阻燃剂质量必须大于等于煤焦油沥青质量的2倍。
7.根据权利要求1所述的一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，其特征在于步骤(2)于600～800℃下碳化，保温时间为1～3h；在此过程中，升温速率控制在1～10℃min-1。
8.根据权利要求1所述的一种利用阻燃原理在空气气氛下制备多孔炭材料的方法，其特征在于步骤(1)中，碳质前驱体不限于沥青，原料适用范围广。
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