CN106115660A - 一种基于自下而上分子组装的纳米炭片、制备方法及应用 - Google Patents
一种基于自下而上分子组装的纳米炭片、制备方法及应用 Download PDFInfo
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- CN106115660A CN106115660A CN201610494087.1A CN201610494087A CN106115660A CN 106115660 A CN106115660 A CN 106115660A CN 201610494087 A CN201610494087 A CN 201610494087A CN 106115660 A CN106115660 A CN 106115660A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920000642 polymer Polymers 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000003763 carbonization Methods 0.000 claims abstract description 18
- 239000011232 storage material Substances 0.000 claims abstract description 16
- 230000008859 change Effects 0.000 claims abstract description 15
- 239000012074 organic phase Substances 0.000 claims abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001868 water Inorganic materials 0.000 claims abstract description 11
- 150000001412 amines Chemical class 0.000 claims abstract description 10
- 238000004146 energy storage Methods 0.000 claims abstract description 4
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 241000549556 Nanos Species 0.000 claims description 10
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 10
- 150000001299 aldehydes Chemical class 0.000 claims description 9
- 239000012190 activator Substances 0.000 claims description 8
- 239000000839 emulsion Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- 239000012188 paraffin wax Substances 0.000 claims description 8
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007772 electrode material Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 6
- -1 wherein Substances 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 4
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 4
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 4
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 4
- 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 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920002866 paraformaldehyde Polymers 0.000 claims description 4
- 241000446313 Lamella Species 0.000 claims description 3
- 238000005338 heat storage Methods 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims description 2
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 claims description 2
- 229940106691 bisphenol a Drugs 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052756 noble gas Inorganic materials 0.000 claims description 2
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims description 2
- 229960001553 phloroglucinol Drugs 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 235000011069 sorbitan monooleate Nutrition 0.000 claims description 2
- 239000001593 sorbitan monooleate Substances 0.000 claims description 2
- 229940035049 sorbitan monooleate Drugs 0.000 claims description 2
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 2
- 229920000428 triblock copolymer Polymers 0.000 claims description 2
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 2
- 241000220324 Pyrus Species 0.000 claims 1
- 150000008065 acid anhydrides Chemical class 0.000 claims 1
- 125000003916 ethylene diamine group Chemical group 0.000 claims 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 claims 1
- 229940049964 oleate Drugs 0.000 claims 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims 1
- 235000021017 pears Nutrition 0.000 claims 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 19
- 239000003345 natural gas Substances 0.000 abstract description 7
- 229910021392 nanocarbon Inorganic materials 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000004320 controlled atmosphere Methods 0.000 abstract 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 5
- 239000002114 nanocomposite Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
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- 241001232809 Chorista Species 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
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- 230000001413 cellular effect Effects 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229960003742 phenol Drugs 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229950000845 politef Drugs 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
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- 230000008929 regeneration Effects 0.000 description 1
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- 230000001105 regulatory effect Effects 0.000 description 1
- 229960001755 resorcinol Drugs 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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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
- 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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C01P2006/00—Physical properties of inorganic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
本发明公开了一种自下而上基于分子组装的纳米炭片、制备方法及应用。以有机相变储热材料、表面活性剂、酚、醛、有机胺为原料,水为溶剂,经过分子自组装、聚合得到圆形、梭形、菱形、带状的聚合物片;经惰性气保护下炭化,得到纳米炭片;经惰性气保护下活化,可得到富含微孔纳米炭片。该方法制备的纳米炭片和富含微孔纳米炭片在天然气的净化分离以及超级电容器储能器件中表现出良好的性能,具有很大的应用潜力和市场前景。
Description
技术领域
本发明涉及圆形、梭形、菱形、带状的纳米聚合物片、炭片的可控制备及应用,更具体的说是涉及一种自下而上基于分子自组装方法制备形貌可控、尺寸均匀,厚度均一的纳米炭片及其应用。
背景技术
天然气因无色无味无毒、热值高、燃烧稳定,一直被公认为洁净环保的优质能源。同时,天然气也是重要的化工原料,目前天然气直接转化制取烯烃和高值化学品用以缓解石油短缺带来的烯烃原料缺乏更是引起世界各国的广泛关注。但是天然气中除主要成分甲烷外,还含有少量的乙烷、丙烷、丁烷,和酸性气体硫化氢、二氧化碳,以及氮和水汽等。为了增加天然气中的热容量、减少输送管路、使用设备的腐蚀和防止对空气的污染,必须将这些杂质气体在使用或输送前从天然气中除去。
目前存在的技术中,物理吸附法作为干法工艺,相比于传统的化学吸附法表现出很多优点,比如易再生、低能耗、腐蚀性小、操作易实现自动化等,可应用于变温吸附或者变压吸附过程。从原理上讲,物理吸附法是基于客体分子与多孔固体吸附剂表面活性点之间的分子间引力来实现捕获,因此高效的多孔吸附材料是吸附法的核心。
近年来,随着能源短缺、环境污染等问题日益突出,人们迫切需求绿色环保的储能设备。为满足电动汽车、移动电子设备对超级电容器的需求,开发出具有高功率密度、快速充放电、长循环稳定性、良好安全性能的电极材料成为当务之急。这就要求电极材料具有利于离子快速传输的单元结构以及能够存储电荷的大比表面积和合适的孔径分布。
为同时满足气体吸附分离和超级电容器对材料的要求,一系列具有高比表面积、大孔容、化学稳定性及热稳定性优异、可应用于酸、碱、水汽等复杂环境的多孔炭材料相继被合成并应用。
自2004年二维石墨烯被发现以来,科学家相继证实材料维度是决定其物理化学性质的重要因素之一。具有高深宽比结构的二维片层材料因其外比表面积大,扩散路径短,在气体吸附分离体及能源存储等领域表现出优异的性能和良好的应用前景。因此,兼具多孔炭吸附性能好和片层结构扩散吸附速率快的二维多孔炭片也成为研究的热点。
中国专利申请号:201210172187.4公开了一种高体积比电容复合石墨烯的多孔炭片,片层单元的形成是基于氧化石墨烯的模板作用。该方法得到的炭片具有三明治结构,垂直于炭片方向的孔道不能完全贯通。中国专利申请号:2012100506368公开了一种动力锂离子电池负极用层次孔结构炭材料及其制备方法,本方法利用原位铜模板法制备层次孔纳米炭片。该方法涉及酸洗除掉铜模板的过程。上述方法,均使用固体模板做片层结构导向剂。目前存在的方法中,还没有关于自下而上基于分子自组装制备多孔纳米炭片的方法这是因为片层结构的表面能高,分子自组装很难控制。。因此,如何开发一种有效、可控的制备方法得到形貌和尺寸均一、厚度可调的多孔炭片是亟需解决的问题。
发明内容
本发明目的在于提供制备形貌、尺寸均一,厚度可调,单分散的聚合物片、炭片和多微孔炭片的方法。
本发明的技术方案:
一种基于自下而上分子组装的纳米炭片,该纳米炭片为由有机相变储热材料、表面活性剂、酚、醛和有机胺组装聚合得到圆形、梭形、菱形或带状的胶 体聚合物片,经炭化或炭化活化得到纳米炭片、多微孔纳米炭片,其片层单元的横向尺寸为0.1-100μm,厚度为10-900nm。
所述的纳米炭片的制备方法,以有机相变储热材料、表面活性剂、酚、醛和有机胺为原料,水为溶剂,通过温度调控的自下而上的分子自组装的方法,经过低温聚合,制备出形貌均一、厚度可调的聚合物片,再进一步炭化热解,得到纳米炭片;步骤如下:
①将熔化后的有机相变储热材料迅速加入到含有表面活性剂的水溶液中,在高于有机相变储热材料熔点温度之上,剧烈搅拌,得到半透明白色乳液,其中,有机相变储热材料与表面活性剂的质量比1:10-1.5;
②将得到半透明白色乳液在低于有机相变储热材料熔点温度之下静置,得到白色胶体溶液;
③将酚、醛、水和有机胺按照比例依次加入白色胶体溶液中,水浴回流搅拌4-24h,产物经过滤、洗涤、干燥得到胶体聚合物片;其中,酚、醛、有机胺和表面活性剂的摩尔比为1:1-3:0.1-2:0.01-0.07,酚与水的质量比为1:200-1:3000;
④将胶体聚合物片置于炭化炉中,在惰性气体保护条件下进行炭化,得到纳米炭片;所述的炭化方法为用惰性气体保护下,从室温以1-3℃/min升至400℃,恒温120min进行有机相变储热材料的挥发;再以1-5℃/min的升温速率由400℃升至炭化终温500-1200℃,恒温60-240min,炭化得到型态保持的纳米炭片;
⑤将胶体聚合物片与活化剂混合物置于炭化炉中,在惰性气体保护条件下进行活化,得到多微孔纳米炭片;所述的活化剂与胶体聚合物片层的质量比0.1:1-4:1;
⑥将纳米炭片与活化剂混合物置于炭化炉中,在惰性气体保护条件下进行活化,得到多微孔纳米炭片;所述的活化剂与纳米炭片的质量比0.1:1-4:1;
所述的步骤⑤和步骤⑥的活化温度为500-900℃。
所述的表面活性剂为聚乙烯基吡咯烷酮、聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物、失水山梨醇单油酸酯聚氧乙烯醚(Tween 80)、山梨醇酐油酸酯(Span-80);优选的聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物P123和聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物F127。
所述的有机相变储热材料包括石蜡、脂酸类和直链烷烃;优选直链烷烃CnH2n+2(n=20-40)、脂酸类CnH2n+1COOH(n=12-30)。
所述的的静置温度为10-70℃,静置时间为1-48h。
所述的酚为苯酚、间苯二酚、间苯三酚或双酚A;优选苯酚和间苯二酚。
所述的醛为甲醛、多聚甲醛、戊二醛或丁醛,甲醛、多聚甲醛常配置为37wt.%的溶液使用,戊二醛常配置为25wt.%的溶液使用;优选甲醛。
所述的有机胺为乙二胺、1,4-己二胺、1,6-己二胺、四乙基五胺、二亚乙基二胺或聚乙烯亚胺;优选1,6-己二胺。
所述的惰性气体为氩气或氮气。
所述的活化剂包括KOH、K2CO3、KHCO3、H2O、CO2、ZnCl2;优选K2CO3。
所述的活化剂与胶体聚合物片层的质量比0.1:1-4:1;优选1:1。
所述的活化温度为500-900℃,优选700℃。
所述的活化剂与纳米炭片的质量比0.1:1-4:1;优选2:1。
相比于现有技术,本发明的有益效果是提供了一种自下而上基于分子自组装制备形貌、尺寸均一,厚度可调的胶体聚合物片、胶体炭片、多微孔炭片的方法;通过调节酚与有机相变储热材料的质量比,可以调节制备炭片的厚度;这是其他方法很难达到的。
本发明制备的纳米炭片和多微孔炭片是良好的气体吸附分离剂,可用于天 然中CH4、C2H2、C2H4、C2H6、C3H8、CO2、H2S、N2、H2的吸附,其中CO2、C2H6吸附效果尤其显著,在25℃,1bar下吸附量分别为5.2mmol g-1和6.0mmol g-1,远优于目前商业化和文献报道的其他吸附材料;可用于CO2/N2,CO2/CH4,CH4/C2H6以及CH4/CO2/C2H6的分离。
本发明制备的胶体炭片和多微孔炭片是良好的超级电容器电极材料,可用于对称、不对称超级电容器;可选电解液有KOH、H2SO4、NaCl、KCl、MgCl2、Al2(SO4)3。
因此,本发明得到的炭片有很大的应用潜能和市场前景。
附图说明
图1是本发明实例2所制备的胶体纳米炭片的扫描电镜,a为放大60000倍,b为放大240000倍。
图2是本发明实例3所制备的多微孔纳米炭片的扫描电镜,为放大40000倍。
图3是本发明实例5所制备的纳米炭片的扫描电镜,为放大1600倍。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。
实施例1
称取200mg表面活性剂F127,加入到20ml去离子中,40℃搅拌溶解2h。称量硬脂酸150mg于小瓶中,放在90℃烘箱30min,使硬脂酸熔化为液体。将F127水溶液升至80℃,随后将熔化的硬脂酸加入其中,快速搅拌3h,得到半透明白色乳液。将得到乳液静置于45℃水浴中12h,得到白色胶体溶液。随后加入220mg间苯二酚,292μl甲醛(37wt%),280ml去离子水,搅拌均匀, 加入58mg的1,6-己二胺,搅拌反应0.5h,得到白色胶体后,将上述反应液移到80℃水浴锅中,并搅拌处理18h,经过8000r/min离心5min后,用水和乙醇洗涤,将产物干燥,得到单分散的聚合物纳米。
实施例2
将实施例1制备的聚合物纳米片置于炭化炉中炭化,用氩气保护从室温以3℃/min升至400℃,恒温120min,再以5℃/min的升温速率升至炭化终温600℃,恒温120min,炭化得到型态保持的纳米炭片。
本实施例所得纳米炭片长约3μm,宽约700nm,厚度为48nm,其扫描电镜如图1所示。
实施例3
将实施例1制备的聚合物纳米片与K2CO3质量比为1:1混合,混合后粉末置于炭化炉中活化,用氩气保护从室温以3℃/min升至100℃,再以5℃/min的升温速率升至活化终温700℃,恒温120min,炭化得到形态保持的多微孔炭片,其BET比表面积为1860m2g-1,总孔容0.98cm3g-1,微孔孔容为0.90cm3g-1。本实施例所得纳米炭片其扫描电镜如图2所示。
实施例4
取实施例3制备的多微孔纳米片0.1g,利用物理吸附仪ASAP 2020在25℃时进行C2H6,CO2,CH4,N2气体吸附测试,1bar下吸附量分别为6.0mmol g-1,5.2mmol g-1,1.3mmol g-1,0.3mmol g-1。
实施例5
将实施例4制备的炭片与K2CO3质量比为1:1混合,混合后粉末置于炭化炉中活化,用氩气保护从室温以3℃/min升至100℃,再以5℃/min的升温速率升至活化终温700℃,恒温120min,炭化得到形态保持的多微孔炭片,其 BET比表面积为1100m2g-1,总孔容0.59cm3g-1,微孔孔容为0.54cm3g-1。
实施例6(待测试)
称取mg实施例5中制备得到炭片,研磨成粉后,加入ml无水乙醇;然后加入粘结剂(活性物质与粘结剂按质量比为混合),加入mg质量分数为60%的PTFE(聚四氟乙烯)水溶液于分散良好的活性物质溶液中,研磨20min至PTFE溶液分散完全,转入50℃烘箱中干燥处理,待乙醇溶液挥发后,向烧杯中加入mg氮甲基吡咯烷酮,将电极材料混合成泥状,然后涂覆在泡沫镍集流体上,在10MPa压力下将电极材料压制在泡沫镍上,制成工作电极。然后将工作电极放入100℃真空干燥箱中真空干燥4h。
进行三电极测试之前,将做好的工作电极在6M KOH溶液中浸泡12h,以金属铂片为辅助电极,Hg/HgO为参比电极,测定其在mA/g大电流密度下的质量比电容为150F/g。
实施例7
称取200mg表面活性剂F127,加入到20ml去离子中,40℃搅拌溶解2h。称量石蜡100mg于小瓶中,放在90℃烘箱30min,使石蜡熔化为液体。将F127水溶液升至80℃,随后将熔化的石蜡迅速加入其中,快速搅拌3h,得到半透明白色乳液。将得到乳液静置于28℃水浴中12h,得到白色胶体溶液。随后加入220mg间苯二酚,292μl甲醛(37wt%),280ml去离子水,28℃搅拌均匀,加入58mg的1,6-己二胺,搅拌反应0.5h,得到白色胶体后,将上述反应液移到80℃水浴锅中,并搅拌处理18h,得到单分散的聚合物纳米片水液,经过8000r/min离心5min后,用水和乙醇洗涤,将产物冷冻干燥。制备的聚合物纳米片置于炭化炉中炭化,用氩气保护从室温以3℃/min升至400℃,恒温120min,再以5℃/min的升温速率升至炭化终温600℃,恒温120min,炭化得到 纳米炭片。
Claims (9)
1.一种基于自下而上分子组装的纳米炭片的制备方法,其特征在于,所述的纳米炭片为由有机相变储热材料、表面活性剂、酚、醛和有机胺组装聚合得到圆形、梭形、菱形或带状的胶体聚合物片,经炭化或炭化活化得到纳米炭片、多微孔纳米炭片,片层单元的横向尺寸为0.1-100μm,厚度为10-900nm;
所述的纳米炭片的制备过程如下:
①将熔化后的有机相变储热材料迅速加入到含有表面活性剂的水溶液中,在高于有机相变储热材料熔点温度之上,剧烈搅拌,得到半透明白色乳液,其中,有机相变储热材料与表面活性剂的质量比1:10-1:1.5;
②将得到半透明白色乳液在低于有机相变储热材料熔点温度之下静置,得到白色胶体溶液;
③将酚、醛、水和有机胺按照比例依次加入白色胶体溶液中,水浴回流搅拌4-24h,产物经过滤、洗涤、干燥得到胶体聚合物片;其中,酚、醛、有机胺和表面活性剂的摩尔比为1:1-3:0.1-2:0.01-0.07,酚与水的质量比为1:200-1:3000;
④将胶体聚合物片置于炭化炉中,在惰性气体保护条件下进行炭化,得到纳米炭片;所述的炭化方法为用惰性气体保护下,从室温以1-3℃/min升至400℃,恒温120min进行有机相变储热材料的挥发;再以1-5℃/min的升温速率由400℃升至炭化终温500-1200℃,恒温60-240min,炭化得到型态保持的纳米炭片;
⑤将胶体聚合物片与活化剂混合物置于炭化炉中,在惰性气体保护条件下进行活化,得到多微孔纳米炭片;所述的活化剂与胶体聚合物片层的质量比0.1:1-4:1;
⑥将纳米炭片与活化剂混合物置于炭化炉中,在惰性气体保护条件下进行活化,得到多微孔纳米炭片;所述的活化剂与纳米炭片的质量比0.1:1-4:1;
所述的步骤⑤和步骤⑥的活化温度为500-900℃。
2.根据权利要求1所述的制备方法,其特征在于,所述的表面活性剂包括聚乙烯基吡咯烷酮、聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物、失水山梨醇单油酸酯聚氧乙烯醚或山梨醇酐油酸酯。
3.根据权利要求2所述的制备方法,其特征在于,所述的有机相变储热材料包括石蜡、脂酸类和直链烷烃。
4.根据权利要求3所述的制备方法,其特征在于,所述的酚为苯酚、间苯二酚、间苯三酚或双酚A;所述的醛为甲醛、多聚甲醛、戊二醛或丁醛,甲醛和多聚甲醛的配置为37wt.%的溶液使用,戊二醛的配置为25wt.%的溶液使用;所述的有机胺为乙二胺、1,4-己二胺、1,6-己二胺、四乙基五胺、二亚乙基二胺或聚乙烯亚胺。
5.根据权利要求4所述的制备方法,其特征在于,所述的活化剂包括KOH、K2CO3、KHCO3、H2O、CO2和ZnCl2。
6.根据权利要求5所述的制备方法,其特征在于,步骤②所述的静置,其温度为10-70℃,静置时间为1-48h。
7.根据权利要求6所述的制备方法,其特征在于,所述的惰性气体为氩气或氮气。
8.权利要求1-7任一所述的制备方法得到的纳米炭片的应用,其特征在于,将纳米炭片和多微孔纳米炭片作为气体吸附剂,用于CH4、C2H2、C2H4、C2H6、C3H8、CO2、H2S、N2、H2中的一种或两种以上混合气体的吸附存储,同时用于上述两种以上混合气体的吸附分离。
9.权利要求1-7任一所述的制备方法得到的纳米炭片的应用,其特征在于,将纳米炭片和多微孔纳米炭片作为电极材料,应用于超级电容器储能器件。
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