CN110743497A - Preparation method of bionic structure ultra-light carbon aerogel - Google Patents
Preparation method of bionic structure ultra-light carbon aerogel Download PDFInfo
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- CN110743497A CN110743497A CN201911028765.5A CN201911028765A CN110743497A CN 110743497 A CN110743497 A CN 110743497A CN 201911028765 A CN201911028765 A CN 201911028765A CN 110743497 A CN110743497 A CN 110743497A
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- Prior art keywords
- konjac glucomannan
- graphene oxide
- carbon aerogel
- aqueous solution
- ultra
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- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 84
- 239000011664 nicotinic acid Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 158
- 241001312219 Amorphophallus konjac Species 0.000 claims abstract description 133
- 235000001206 Amorphophallus rivieri Nutrition 0.000 claims abstract description 133
- 229920002752 Konjac Polymers 0.000 claims abstract description 133
- 239000000252 konjac Substances 0.000 claims abstract description 133
- 235000010485 konjac Nutrition 0.000 claims abstract description 133
- 239000007864 aqueous solution Substances 0.000 claims abstract description 80
- 238000003756 stirring Methods 0.000 claims abstract description 53
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000001816 cooling Methods 0.000 claims abstract description 41
- 239000011259 mixed solution Substances 0.000 claims abstract description 35
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 33
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 33
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 23
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 21
- 239000010935 stainless steel Substances 0.000 claims abstract description 21
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 68
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 claims description 41
- 229920002581 Glucomannan Polymers 0.000 claims description 41
- 229940046240 glucomannan Drugs 0.000 claims description 41
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 33
- 238000009461 vacuum packaging Methods 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000007789 sealing Methods 0.000 claims description 20
- 230000003068 static effect Effects 0.000 claims description 19
- 238000007710 freezing Methods 0.000 claims description 18
- 230000008014 freezing Effects 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000002270 dispersing agent Substances 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 9
- 239000003431 cross linking reagent Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000004698 Polyethylene Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
- 229920000573 polyethylene Polymers 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 230000008961 swelling Effects 0.000 claims description 6
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 4
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- MKFKRDBGTIMGAC-UHFFFAOYSA-N [N+](=O)(O)[O-].CN1CN(C=C1)C Chemical compound [N+](=O)(O)[O-].CN1CN(C=C1)C MKFKRDBGTIMGAC-UHFFFAOYSA-N 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- FYXKZNLBZKRYSS-UHFFFAOYSA-N benzene-1,2-dicarbonyl chloride Chemical compound ClC(=O)C1=CC=CC=C1C(Cl)=O FYXKZNLBZKRYSS-UHFFFAOYSA-N 0.000 claims description 2
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical compound ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 claims description 2
- FDQSRULYDNDXQB-UHFFFAOYSA-N benzene-1,3-dicarbonyl chloride Chemical compound ClC(=O)C1=CC=CC(C(Cl)=O)=C1 FDQSRULYDNDXQB-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical compound ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 20
- 230000015556 catabolic process Effects 0.000 abstract description 15
- 238000006731 degradation reaction Methods 0.000 abstract description 15
- 239000002354 radioactive wastewater Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 16
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 12
- 239000001263 FEMA 3042 Substances 0.000 description 12
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 12
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 12
- 229940033123 tannic acid Drugs 0.000 description 12
- 235000015523 tannic acid Nutrition 0.000 description 12
- 229920002258 tannic acid Polymers 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 238000009931 pascalization Methods 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000000593 degrading effect Effects 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 3
- 229920001864 tannin Polymers 0.000 description 3
- 239000001648 tannin Substances 0.000 description 3
- 235000018553 tannin Nutrition 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003592 biomimetic effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 231100000045 chemical toxicity Toxicity 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 125000005289 uranyl group Chemical group 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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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
-
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Cosmetics (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of super-light carbon aerogel with a bionic structure, which comprises the following steps: preparing a konjac glucomannan-graphene oxide mixed solution; preparing a konjac glucomannan-graphene oxide dry body from the konjac glucomannan-graphene oxide mixed solution; treating the konjac glucomannan-graphene oxide dry body at high temperature in a nitrogen atmosphere, and cooling to obtain konjac glucomannan-graphene carbon aerogel; adding konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out hydrothermal reaction, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure. The prepared bionic structure ultra-light carbon aerogel has the double functions of adsorption and catalysis, and the synergistic effect of adsorption and catalytic degradation under a radioactive wastewater system is greatly stronger than the effect of independent application of the two.
Description
Technical Field
The invention belongs to the field of aerogel preparation, and particularly relates to a preparation method of bionic structure ultra-light carbon aerogel.
Background
A large amount of radioactive wastewater is generated in the production process of the nuclear industry, and the radioactive wastewater has strong radioactivity, long half-life period and high biological and chemical toxicity, and constitutes great long-term harm to human beings and the environment, so the treatment of the radioactive wastewater is an important and indispensable link in the development process of the modern nuclear industry.
At present, methods for treating radioactive wastewater generated by a nuclear power plant mainly include a chemical precipitation method, an ion exchange method, an evaporation concentration method, a membrane separation method, an adsorption method and the like, wherein the adsorption method is to transfer radioactive elements to a solid phase by using an adsorbent for enrichment and concentration, and commonly used adsorbents include activated carbon, zeolite, montmorillonite and the like, however, the adsorption effect of the adsorbents is unstable, the adsorption and degradation of organic matters in the radioactive wastewater cannot be realized, the solidification effect of the formed radioactive adsorbent during immobilization treatment is not good, and the radioactive elements are easy to release to form secondary pollution.
The carbon aerogel is a novel light porous material, has the characteristics of good stability, high porosity, large specific surface area, high conductivity, more substances and electron transmission pore passages, can be widely used as a catalyst carrier, a hydrogen storage material, an adsorption material, an electrode material of a super capacitor or a lithium ion battery and the like, and can be applied to the adsorption treatment of radioactive wastewater to improve the treatment effect of the radioactive wastewater; the prior art does not relate to a related technical scheme for treating radioactive wastewater by adopting carbon aerogel.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a biomimetic structure ultra-light carbon aerogel, comprising the steps of:
step one, adding konjac glucomannan into a graphene oxide aqueous solution, stirring for 10-15 min, then adding into a vacuum packaging bag for vacuum packaging, and controlling the vacuum degree to be 0.1 MPa; putting the vacuum packaging bag into high static pressure treatment equipment, sealing a pressurizing cavity, pressurizing and carrying out high static pressure treatment to obtain a konjac glucomannan-graphene oxide mixed solution;
step two, cooling the konjac glucomannan-graphene oxide mixed solution in a refrigerator at the temperature of 0-4 ℃ for 0.5-1 hour, placing the cooled konjac glucomannan-graphene oxide mixed solution into an ice mold directional freezing device for freezing after precooling until the konjac glucomannan-graphene oxide mixed solution is solidified into a frozen body, then freeze-drying the frozen body at the temperature of 60-70 ℃ below zero and under the vacuum degree of 1-6 Pa, and drying the frozen body for 2-3 days to prepare the konjac glucomannan-graphene oxide dried body;
step three, treating the konjac glucomannan-graphene oxide dried body at high temperature in a nitrogen atmosphere, and cooling to obtain konjac glucomannan-graphene carbon aerogel;
and step four, adding the konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out constant-temperature hydrothermal reaction at 180-220 ℃ for 10-15 h, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure.
Preferably, the konjac glucomannan is replaced by modified konjac glucomannan, and the preparation method comprises the following steps: adding 30-35 parts by weight of konjac glucomannan and 10-15 parts by weight of polyvinyl alcohol into a stainless steel high-pressure reaction kettle with stirring, and adding CO2Blowing air in the stainless steel high-pressure reaction kettle clean and introducing CO2Sealing, stirring and swelling for 2-3 hours at 65 ℃ and 12.5MPa, relieving pressure, adding 3-5 parts of cross-linking agent, and introducing CO2Sealing, stirring and reacting for 2-3 hours at 80 ℃ and 13.5MPa, decompressing, and drying to obtain the modified konjac glucomannan.
Preferably, in the first step, the mass percentage concentration of the graphene oxide aqueous solution is 1% -3%; the mass ratio of the konjac glucomannan to the graphene oxide in the graphene oxide aqueous solution is 1:5 to 20.
Preferably, in the first step, the parameters of the high static pressure treatment are as follows: raising the pressure to 500-700 MPa at a pressure raising speed of 2-5 MPa/s, and carrying out pressure maintaining treatment at 35-55 ℃ for 30-60 min; the vacuum packaging bag is a nylon-polyethylene composite bag.
Preferably, the crosslinking agent is any one of glutaraldehyde, epichlorohydrin, trimesoyl chloride, phthaloyl chloride, isophthaloyl chloride and terephthaloyl chloride.
Preferably, in the first step, the preparation method of the graphene oxide aqueous solution comprises: adding graphene oxide and a dispersing agent into deionized water, stirring for 30-60 min, and carrying out ultrasonic treatment in an ultrasonic cleaning machine for 0.5-1 h to obtain a graphene oxide aqueous solution; the power of the ultrasonic is 500-1000W, and the ultrasonic frequency is 40-60 KHz.
Preferably, the dispersant is NaOH or Na2CO3Any one of sodium carboxymethylcellulose and 1, 3-dimethyl imidazole nitrate.
Preferably, in the third step, the high-temperature treatment process of the konjac glucomannan-graphene oxide dried body in the nitrogen atmosphere comprises: adding the konjac glucomannan-graphene oxide dry body into a rotary furnace, introducing nitrogen at a flow rate of 100-200 mL/min, heating to 200-300 ℃ at a speed of 1-2 ℃/min, preserving heat for 1-3 h, continuously heating to 500-600 ℃ at a speed of 1-2 ℃/min, preserving heat for 1-2 h, continuously heating to 800-850 ℃ at a speed of 1-2 ℃/min, preserving heat for 1-2 h, then cooling to 250-350 ℃ at a speed of 5-10 ℃/min, preserving heat for 10-30 min, and naturally cooling to room temperature; the rotating speed of the rotary furnace is 5-12 r/min.
Preferably, in the fourth step, the concentration of the titanium sulfate aqueous solution is 2-5 g/L; the mass ratio of the konjac glucomannan-graphene carbon aerogel to the titanium sulfate in the titanium sulfate aqueous solution is 1-3: 1.
Preferably, in the third step, the konjac glucomannan-graphene carbon aerogel is pretreated, and the process comprises the following steps: dispersing konjac glucomannan-graphene carbon aerogel in H according to the concentration of 0.3-0.5 mg/mL2O2And FeCl3In an aqueous solution of (A), H2O2FeCl of3Stirring and uniformly mixing the materials according to the molar ratio of 1: 2-5, adjusting the pH to 3-5 by using a NaOH aqueous solution, and then treating the materials for 5-10 min under the microwave irradiation condition; the power of microwave irradiation is 100-500W, and the temperature of microwave irradiation is 60-80 ℃.
In the second step of the invention, the device and method provided in patent document "CN 201710812091.2 preparation method of elastic konjac glucomannan-graphene oxide sponge" are referred to for the ice mold directional freezing device and freezing process.
The invention at least comprises the following beneficial effects:
(1) the prepared bionic structure ultra-light carbon aerogel has the double functions of adsorption and catalysis, and the synergistic effect of adsorption and catalytic degradation under a radioactive wastewater system is greatly stronger than the effect of independent application of the two. In addition, the surface modification of the material enables the material to have higher adsorption and catalytic capabilities under the actual radioactive wastewater environment, and the material meets the market application requirements for treating low-level wastewater.
(2) Provides a method for preparing the bionic structure ultra-light carbon aerogel with high-efficiency adsorption and photocatalysis functions by combining an ice template method and a hydrothermal method. Compared with the traditional physical and chemical methods, the method has the characteristics of simplicity, mildness, high efficiency and universality; the titanium dioxide semiconductor catalyst is loaded on the carbon aerogel, so that the characteristics of rapid adsorption enrichment and easy separation of the carbon aerogel are kept, the forbidden band width can be reduced and the electron-hole recombination probability can be stimulated to enhance the electron transfer effect by the surface hybridization effect formed by the carbon aerogel and the photocatalytic material and the metal and nonmetal doping, and the absorption wavelength range of light can be expanded, so that the adsorption capacity and the catalytic degradation efficiency of the composite material are improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a preparation method of super-light carbon aerogel with a bionic structure comprises the following steps:
step one, adding konjac glucomannan into a graphene oxide aqueous solution, stirring for 15min, then adding into a vacuum packaging bag for vacuum packaging, and controlling the vacuum degree to be 0.1 MPa; putting the vacuum packaging bag into high static pressure treatment equipment, sealing a pressurizing cavity, pressurizing and carrying out high static pressure treatment to obtain a konjac glucomannan-graphene oxide mixed solution; the mass percentage concentration of the graphene oxide aqueous solution is 3%; the mass ratio of the konjac glucomannan to the graphene oxide in the graphene oxide aqueous solution is 1: 10; the parameters of the high hydrostatic pressure treatment were: raising the pressure to 700MPa at a pressure raising speed of 2MPa/s, and carrying out pressure maintaining treatment at 55 ℃ for 30 min; the vacuum packaging bag is a nylon-polyethylene composite bag; the preparation method of the graphene oxide aqueous solution comprises the following steps: adding graphene oxide and a dispersing agent NaOH into deionized water, stirring for 60min, and carrying out ultrasonic treatment in an ultrasonic cleaning machine for 0.5 h to obtain a graphene oxide aqueous solution; the power of the ultrasonic wave is 500W, and the ultrasonic frequency is 60 KHz; the mass fraction of the dispersing agent in the graphene oxide aqueous solution is 0.01%; the high static pressure treatment can improve the dispersion of the graphene oxide in the konjac glucomannan, further improve the combination of the konjac glucomannan and the graphene oxide, and enable the prepared konjac glucomannan-graphene oxide mixed solution to be more uniform.
Step two, cooling the konjac glucomannan-graphene oxide mixed solution in a refrigerator at 0 ℃ for 1 hour, placing the cooled konjac glucomannan-graphene oxide mixed solution into an ice mold directional freezing device for freezing and flattening, inserting the lower end of a steel plate into liquid nitrogen until the konjac glucomannan-graphene oxide mixed solution is solidified into a frozen body, then freeze-drying the frozen body at the temperature of minus 60 ℃ and the vacuum degree of 2 Pa, and drying the frozen body for 3 days to obtain a konjac glucomannan-graphene oxide dried body;
step three, treating the konjac glucomannan-graphene oxide dried body at high temperature in a nitrogen atmosphere, and cooling to obtain konjac glucomannan-graphene carbon aerogel; the high-temperature treatment process comprises the following steps: adding the konjac glucomannan-graphene oxide dry body into a rotary furnace, introducing nitrogen at the flow rate of 200mL/min, heating to 300 ℃ at the speed of 2 ℃/min, preserving heat for 1h, continuously heating to 600 ℃ at the speed of 2 ℃/min, preserving heat for 2h, continuously heating to 850 ℃ at the speed of 2 ℃/min, preserving heat for 2h, then cooling to 350 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and then naturally cooling to room temperature; the rotating speed of the rotary furnace is 12 r/min;
adding the konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out constant-temperature hydrothermal reaction for 10 hours at 200 ℃, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure; the concentration of the titanium sulfate aqueous solution is 2 g/L; the mass ratio of the konjac glucomannan-graphene carbon aerogel to the titanium sulfate in the titanium sulfate aqueous solution is 1: 1; the titanium dioxide loaded replica prepared in this exampleThe specific surface area of the green-structure ultra-light carbon aerogel is 1025m2/g。
Example 2:
a preparation method of super-light carbon aerogel with a bionic structure comprises the following steps:
step one, adding konjac glucomannan into a graphene oxide aqueous solution, stirring for 10min, then adding into a vacuum packaging bag for vacuum packaging, and controlling the vacuum degree to be 0.1 MPa; putting the vacuum packaging bag into high static pressure treatment equipment, sealing a pressurizing cavity, pressurizing and carrying out high static pressure treatment to obtain a konjac glucomannan-graphene oxide mixed solution; the mass percentage concentration of the graphene oxide aqueous solution is 3%; the mass ratio of the konjac glucomannan to the graphene oxide in the graphene oxide aqueous solution is 1: 10; the parameters of the high hydrostatic pressure treatment were: raising the pressure to 700MPa at a pressure raising speed of 2MPa/s, and carrying out pressure maintaining treatment at 55 ℃ for 30 min; the vacuum packaging bag is a nylon-polyethylene composite bag; the preparation method of the graphene oxide aqueous solution comprises the following steps: adding graphene oxide and a dispersing agent NaOH into deionized water, stirring for 60min, and carrying out ultrasonic treatment in an ultrasonic cleaning machine for 0.5 h to obtain a graphene oxide aqueous solution; the power of the ultrasonic wave is 500W, and the ultrasonic frequency is 60 KHz; the mass fraction of the dispersing agent in the graphene oxide aqueous solution is 0.01%;
step two, cooling the konjac glucomannan-graphene oxide mixed solution in a refrigerator at 0 ℃ for 0.5 hour, placing the cooled konjac glucomannan-graphene oxide mixed solution into an ice mold directional freezing device for freezing and flattening after precooling, inserting the lower end of a steel plate into liquid nitrogen until the konjac glucomannan-graphene oxide mixed solution is solidified into a frozen body, then freeze-drying the frozen body at-70 ℃ and under the vacuum degree of 5 Pa, and drying the frozen body for 2 days to prepare the konjac glucomannan-graphene oxide dried body;
step three, treating the konjac glucomannan-graphene oxide dried body at high temperature in a nitrogen atmosphere, and cooling to obtain konjac glucomannan-graphene carbon aerogel; the high-temperature treatment process comprises the following steps: adding the konjac glucomannan-graphene oxide dry body into a rotary furnace, introducing nitrogen at the flow rate of 150mL/min, heating to 250 ℃ at the speed of 1 ℃/min, preserving heat for 2h, continuously heating to 500 ℃ at the speed of 1 ℃/min, preserving heat for 1h, continuously heating to 800 ℃ at the speed of 1 ℃/min, preserving heat for 1.5h, then cooling to 250 ℃ at the speed of 5 ℃/min, preserving heat for 20min, and then naturally cooling to room temperature; the rotating speed of the rotary furnace is 10 r/min;
adding the konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out constant-temperature hydrothermal reaction for 15 hours at 180 ℃, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure; the concentration of the titanium sulfate aqueous solution is 5 g/L; the mass ratio of the konjac glucomannan-graphene carbon aerogel to the titanium sulfate in the titanium sulfate aqueous solution is 2: 1. The specific surface area of the titanium dioxide loaded bionic structure ultra-light carbon aerogel prepared in the embodiment is 1028m2/g。
Example 3:
a preparation method of super-light carbon aerogel with a bionic structure comprises the following steps:
step one, adding the modified konjac glucomannan into a graphene oxide aqueous solution, stirring for 15min, then adding into a vacuum packaging bag for vacuum packaging, and controlling the vacuum degree to be 0.1 MPa; putting the vacuum packaging bag into high static pressure treatment equipment, sealing a pressurizing cavity, pressurizing and carrying out high static pressure treatment to obtain a modified konjac glucomannan-graphene oxide mixed solution; the mass percentage concentration of the graphene oxide aqueous solution is 3%; the mass ratio of the modified konjac glucomannan to the graphene oxide in the graphene oxide aqueous solution is 1: 10; the parameters of the high hydrostatic pressure treatment were: raising the pressure to 700MPa at a pressure raising speed of 2MPa/s, and carrying out pressure maintaining treatment at 55 ℃ for 30 min; the vacuum packaging bag is a nylon-polyethylene composite bag; the preparation method of the graphene oxide aqueous solution comprises the following steps: adding graphene oxide and a dispersing agent NaOH into deionized water, stirring for 60min, and carrying out ultrasonic treatment in an ultrasonic cleaning machine for 0.5 h to obtain a graphene oxide aqueous solution; the power of the ultrasonic wave is 500W, and the ultrasonic frequency is 60 KHz; the mass fraction of the dispersing agent in the graphene oxide aqueous solution is 0.01%;
step two, placing the modified konjac glucomannan-graphene oxide mixed solution in a refrigerator at 0 ℃ for cooling for 1 hour, placing the cooled mixed solution into an ice mold directional freezing device for freezing and flattening after precooling, inserting the lower end of a steel plate into liquid nitrogen until the modified konjac glucomannan-graphene oxide mixed solution is solidified into a frozen body, then carrying out freeze drying at minus 60 ℃ and under the vacuum degree of 2 Pa, and drying for 3 days to prepare a modified konjac glucomannan-graphene oxide dried body;
step three, treating the modified konjac glucomannan-graphene oxide dry body at high temperature in a nitrogen atmosphere, and cooling to obtain the modified konjac glucomannan-graphene carbon aerogel; the high-temperature treatment process comprises the following steps: adding the modified konjac glucomannan-graphene oxide dry body into a rotary furnace, introducing nitrogen at the flow rate of 200mL/min, simultaneously heating to 300 ℃ at the speed of 2 ℃/min, preserving heat for 1h, continuously heating to 600 ℃ at the speed of 2 ℃/min, preserving heat for 2h, continuously heating to 850 ℃ at the speed of 2 ℃/min, preserving heat for 2h, then cooling to 350 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and then naturally cooling to room temperature; the rotating speed of the rotary furnace is 12 r/min;
adding the modified konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out constant-temperature hydrothermal reaction for 10 hours at 200 ℃, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure; the concentration of the titanium sulfate aqueous solution is 2 g/L; the mass ratio of the modified konjac glucomannan-graphene carbon aerogel to the titanium sulfate in the titanium sulfate aqueous solution is 1: 1;
the preparation method of the modified konjac glucomannan comprises the following steps: adding 30 parts by weight of konjac glucomannan and 10 parts by weight of polyvinyl alcohol into a stainless steel high-pressure reaction kettle with stirring, and adding CO2Blowing air in the stainless steel high-pressure reaction kettle clean and introducing CO2Sealing, stirring at 65 deg.C and 12.5MPa for swelling for 2 hr, relieving pressure, adding 5 parts of crosslinking agent glutaraldehyde, introducing CO2Sealing, stirring and reacting at 80 deg.C and 13.5MPa for 3 hr, relieving pressure, and drying to obtainModified konjac glucomannan. The specific surface area of the titanium dioxide loaded bionic structure ultra-light carbon aerogel prepared in the example is 1185m2(ii)/g; the supercritical carbon dioxide fluid has good fluidity and transferability, has larger kinetic energy than liquid, can enter the konjac glucomannan like gas, enhances the contact speed of the cross-linking agent and the konjac glucomannan, improves the mass transfer process, increases the collision probability between active groups, can improve the reaction speed and the cross-linking uniformity, and the prepared modified konjac glucomannan has better associativity with the graphene oxide.
Example 4:
a preparation method of super-light carbon aerogel with a bionic structure comprises the following steps:
step one, adding the modified konjac glucomannan into a graphene oxide aqueous solution, stirring for 10min, then adding into a vacuum packaging bag for vacuum packaging, and controlling the vacuum degree to be 0.1 MPa; putting the vacuum packaging bag into high static pressure treatment equipment, sealing a pressurizing cavity, pressurizing and carrying out high static pressure treatment to obtain a modified konjac glucomannan-graphene oxide mixed solution; the mass percentage concentration of the graphene oxide aqueous solution is 3%; the mass ratio of the modified konjac glucomannan to the graphene oxide in the graphene oxide aqueous solution is 1: 10; the parameters of the high hydrostatic pressure treatment were: raising the pressure to 700MPa at a pressure raising speed of 2MPa/s, and carrying out pressure maintaining treatment at 55 ℃ for 30 min; the vacuum packaging bag is a nylon-polyethylene composite bag; the preparation method of the graphene oxide aqueous solution comprises the following steps: adding graphene oxide and a dispersing agent NaOH into deionized water, stirring for 60min, and carrying out ultrasonic treatment in an ultrasonic cleaning machine for 0.5 h to obtain a graphene oxide aqueous solution; the power of the ultrasonic wave is 500W, and the ultrasonic frequency is 60 KHz; the mass fraction of the dispersing agent in the graphene oxide aqueous solution is 0.01%;
step two, cooling the modified konjac glucomannan-graphene oxide mixed solution in a refrigerator at 0 ℃ for 0.5 hour, placing the cooled mixed solution into an ice mold directional freezing device for freezing and flattening after precooling, inserting the lower end of a steel plate into liquid nitrogen until the modified konjac glucomannan-graphene oxide mixed solution is solidified into a frozen body, then carrying out freeze drying at-70 ℃ and under the vacuum degree of 5 Pa, and drying for 2 days to prepare a modified konjac glucomannan-graphene oxide dried body;
step three, treating the modified konjac glucomannan-graphene oxide dry body at high temperature in a nitrogen atmosphere, and cooling to obtain the modified konjac glucomannan-graphene carbon aerogel; the high-temperature treatment process comprises the following steps: adding the modified konjac glucomannan-graphene oxide dry body into a rotary furnace, introducing nitrogen at a flow rate of 150mL/min, simultaneously heating to 250 ℃ at a speed of 1 ℃/min, preserving heat for 2h, continuously heating to 500 ℃ at a speed of 1 ℃/min, preserving heat for 1h, continuously heating to 800 ℃ at a speed of 1 ℃/min, preserving heat for 1.5h, then cooling to 250 ℃ at a speed of 5 ℃/min, preserving heat for 20min, and then naturally cooling to room temperature; the rotating speed of the rotary furnace is 10 r/min;
adding the modified konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out constant-temperature hydrothermal reaction for 15 hours at 180 ℃, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure; the concentration of the titanium sulfate aqueous solution is 5 g/L; the mass ratio of the modified konjac glucomannan-graphene carbon aerogel to the titanium sulfate in the titanium sulfate aqueous solution is 2: 1.
The preparation method of the modified konjac glucomannan comprises the following steps: adding 35 parts by weight of konjac glucomannan and 15 parts by weight of polyvinyl alcohol into a stainless steel high-pressure reaction kettle with stirring, and adding CO2Blowing air in the stainless steel high-pressure reaction kettle clean and introducing CO2Sealing, stirring at 65 deg.C and 12.5MPa for swelling for 2 hr, relieving pressure, adding 5 parts of crosslinking agent epichlorohydrin, introducing CO2Sealing, stirring and reacting for 2 hours at 80 ℃ and 13.5MPa, decompressing and drying to obtain the modified konjac glucomannan. The specific surface area of the titanium dioxide loaded bionic structure ultra-light carbon aerogel prepared in the example is 1188m2/g。
Example 5:
a preparation method of super-light carbon aerogel with a bionic structure comprises the following steps:
step one, adding the modified konjac glucomannan into a graphene oxide aqueous solution, stirring for 15min, then adding into a vacuum packaging bag for vacuum packaging, and controlling the vacuum degree to be 0.1 MPa; putting the vacuum packaging bag into high static pressure treatment equipment, sealing a pressurizing cavity, pressurizing and carrying out high static pressure treatment to obtain a modified konjac glucomannan-graphene oxide mixed solution; the mass percentage concentration of the graphene oxide aqueous solution is 3%; the mass ratio of the modified konjac glucomannan to the graphene oxide in the graphene oxide aqueous solution is 1: 10; the parameters of the high hydrostatic pressure treatment were: raising the pressure to 700MPa at a pressure raising speed of 2MPa/s, and carrying out pressure maintaining treatment at 55 ℃ for 30 min; the vacuum packaging bag is a nylon-polyethylene composite bag; the preparation method of the graphene oxide aqueous solution comprises the following steps: adding graphene oxide and a dispersing agent NaOH into deionized water, stirring for 60min, and carrying out ultrasonic treatment in an ultrasonic cleaning machine for 0.5 h to obtain a graphene oxide aqueous solution; the power of the ultrasonic wave is 500W, and the ultrasonic frequency is 60 KHz; the mass fraction of the dispersing agent in the graphene oxide aqueous solution is 0.01%;
step two, placing the modified konjac glucomannan-graphene oxide mixed solution in a refrigerator at 0 ℃ for cooling for 1 hour, placing the cooled mixed solution into an ice mold directional freezing device for freezing and flattening after precooling, inserting the lower end of a steel plate into liquid nitrogen until the modified konjac glucomannan-graphene oxide mixed solution is solidified into a frozen body, then carrying out freeze drying at minus 60 ℃ and under the vacuum degree of 2 Pa, and drying for 3 days to prepare a modified konjac glucomannan-graphene oxide dried body;
step three, treating the modified konjac glucomannan-graphene oxide dry body at high temperature in a nitrogen atmosphere, and cooling to obtain the modified konjac glucomannan-graphene carbon aerogel; dispersing konjac glucomannan-graphene carbon aerogel in H according to the concentration of 0.5mg/mL2O2And FeCl3In an aqueous solution of (A), H2O2FeCl of3Stirring and uniformly mixing the raw materials according to the molar ratio of 1:2, adjusting the pH value to 5 by using a NaOH aqueous solution, and then treating the mixture for 10min under the microwave irradiation condition; the power of microwave irradiation is 500W, and the temperature of microwave irradiationThe temperature is 80 ℃; the high-temperature treatment process comprises the following steps: adding the modified konjac glucomannan-graphene oxide dry body into a rotary furnace, introducing nitrogen at the flow rate of 200mL/min, simultaneously heating to 300 ℃ at the speed of 2 ℃/min, preserving heat for 1h, continuously heating to 600 ℃ at the speed of 2 ℃/min, preserving heat for 2h, continuously heating to 850 ℃ at the speed of 2 ℃/min, preserving heat for 2h, then cooling to 350 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and then naturally cooling to room temperature; the rotating speed of the rotary furnace is 12 r/min;
adding the modified konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out constant-temperature hydrothermal reaction for 10 hours at 200 ℃, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure; the concentration of the titanium sulfate aqueous solution is 2 g/L; the mass ratio of the modified konjac glucomannan-graphene carbon aerogel to the titanium sulfate in the titanium sulfate aqueous solution is 1: 1;
the preparation method of the modified konjac glucomannan comprises the following steps: adding 30 parts by weight of konjac glucomannan and 10 parts by weight of polyvinyl alcohol into a stainless steel high-pressure reaction kettle with stirring, and adding CO2Blowing air in the stainless steel high-pressure reaction kettle clean and introducing CO2Sealing, stirring at 65 deg.C and 12.5MPa for swelling for 2 hr, relieving pressure, adding 5 parts of crosslinking agent glutaraldehyde, introducing CO2Sealing, stirring and reacting for 3 hours at 80 ℃ and 13.5MPa, decompressing and drying to obtain the modified konjac glucomannan. The specific surface area of the titanium dioxide loaded bionic structure ultra-light carbon aerogel prepared in the example is 1358m2/g。
Example 6:
a preparation method of super-light carbon aerogel with a bionic structure comprises the following steps:
step one, adding the modified konjac glucomannan into a graphene oxide aqueous solution, stirring for 10min, then adding into a vacuum packaging bag for vacuum packaging, and controlling the vacuum degree to be 0.1 MPa; putting the vacuum packaging bag into high static pressure treatment equipment, sealing a pressurizing cavity, pressurizing and carrying out high static pressure treatment to obtain a modified konjac glucomannan-graphene oxide mixed solution; the mass percentage concentration of the graphene oxide aqueous solution is 3%; the mass ratio of the modified konjac glucomannan to the graphene oxide in the graphene oxide aqueous solution is 1: 10; the parameters of the high hydrostatic pressure treatment were: raising the pressure to 700MPa at a pressure raising speed of 2MPa/s, and carrying out pressure maintaining treatment at 55 ℃ for 30 min; the vacuum packaging bag is a nylon-polyethylene composite bag; the preparation method of the graphene oxide aqueous solution comprises the following steps: adding graphene oxide and a dispersing agent NaOH into deionized water, stirring for 60min, and carrying out ultrasonic treatment in an ultrasonic cleaning machine for 0.5 h to obtain a graphene oxide aqueous solution; the power of the ultrasonic wave is 500W, and the ultrasonic frequency is 60 KHz; the mass fraction of the dispersing agent in the graphene oxide aqueous solution is 0.01%;
step two, cooling the modified konjac glucomannan-graphene oxide mixed solution in a refrigerator at 0 ℃ for 0.5 hour, placing the cooled mixed solution into an ice mold directional freezing device for freezing and flattening after precooling, inserting the lower end of a steel plate into liquid nitrogen until the modified konjac glucomannan-graphene oxide mixed solution is solidified into a frozen body, then carrying out freeze drying at-70 ℃ and under the vacuum degree of 5 Pa, and drying for 2 days to prepare a modified konjac glucomannan-graphene oxide dried body;
step three, treating the modified konjac glucomannan-graphene oxide dry body at high temperature in a nitrogen atmosphere, and cooling to obtain the modified konjac glucomannan-graphene carbon aerogel; dispersing konjac glucomannan-graphene carbon aerogel in H according to the concentration of 0.3mg/mL2O2And FeCl3In an aqueous solution of (A), H2O2FeCl of3Stirring and uniformly mixing the raw materials according to the molar ratio of 1:5, adjusting the pH value to 5 by using a NaOH aqueous solution, and then treating the mixture for 10min under the microwave irradiation condition; the power of microwave irradiation is 300W, and the temperature of the microwave irradiation is 70 ℃; the high-temperature treatment process comprises the following steps: adding the modified konjac glucomannan-graphene oxide dry body into a rotary furnace, introducing nitrogen at a flow rate of 150mL/min, heating to 250 ℃ at a speed of 1 ℃/min, keeping the temperature for 2h, continuously heating to 500 ℃ at a speed of 1 ℃/min, keeping the temperature for 1h, continuously heating to 800 ℃ at a speed of 1 ℃/min, keeping the temperature for 1.5h, then heating to 5 DEG CCooling to 250 ℃ at a speed of/min, preserving heat for 20min, and then naturally cooling to room temperature; the rotating speed of the rotary furnace is 10 r/min;
adding the modified konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out constant-temperature hydrothermal reaction for 15 hours at 180 ℃, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure; the concentration of the titanium sulfate aqueous solution is 5 g/L; the mass ratio of the modified konjac glucomannan-graphene carbon aerogel to the titanium sulfate in the titanium sulfate aqueous solution is 2: 1.
The preparation method of the modified konjac glucomannan comprises the following steps: adding 35 parts by weight of konjac glucomannan and 15 parts by weight of polyvinyl alcohol into a stainless steel high-pressure reaction kettle with stirring, and adding CO2Blowing air in the stainless steel high-pressure reaction kettle clean and introducing CO2Sealing, stirring at 65 deg.C and 12.5MPa for swelling for 2 hr, relieving pressure, adding 5 parts of crosslinking agent epichlorohydrin, introducing CO2Sealing, stirring and reacting for 2 hours at 80 ℃ and 13.5MPa, decompressing and drying to obtain the modified konjac glucomannan. The specific surface area of the titanium dioxide loaded bionic structure ultra-light carbon aerogel prepared in the example is 1360m2/g。
Performing a simulated radioactive wastewater adsorption experiment by using the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure prepared in the embodiments 1-6; adding 0.02g of the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure prepared in the embodiments 1-6 into 100mL of 100ppm uranyl solution, adjusting the pH value to be 6, placing the mixture in a constant-temperature shaking box, and carrying out oscillation adsorption reaction for 24 hours at the rotation speed of 150rpm and the adsorption reaction temperature of 25 ℃; measuring the absorbance of the solution before and after adsorption by using an ultraviolet spectrophotometer to obtain the concentration of the uranyl ions; and the adsorption amount was calculated, and the results are shown in Table 1,
TABLE 1
| Examples | 1 | 2 | 3 | 4 | 5 | 6 |
| Adsorption Capacity (mg/g) | 360 | 361 | 405 | 406 | 420 | 422 |
Carrying out a tannin photodegradation experiment in simulated organic wastewater by using the titanium dioxide loaded ultra-light carbon aerogel with a bionic structure prepared in the embodiments 1-6; adding 0.15g of the titanium dioxide loaded super-light carbon aerogel with the bionic structure prepared in the embodiment 1-6 into 500mL of 50ppm tannic acid solution, adjusting the pH value to 7, placing under a 250w ultraviolet high-pressure mercury lamp, irradiating, stirring and degrading for 40min, wherein the experimental temperature is normal temperature, and the stirring speed is 150 r/min; measuring the absorbance of the tannic acid solution before and after degradation by using an ultraviolet spectrophotometer to obtain the concentration of the tannic acid solution; and the degradation rate of tannic acid was calculated, and the results are shown in table 2;
TABLE 2
| Examples | 1 | 2 | 3 | 4 | 5 | 6 |
| The degradation rate% | 92 | 92 | 95 | 96 | 98 | 98 |
Performing a simulated tannin degradation experiment by using the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure prepared in the embodiments 1-6; adding 0.15g of the titanium dioxide loaded super-light carbon aerogel with the bionic structure prepared in the embodiment 1-6 into 500mL of 50ppm tannic acid solution, adjusting the pH value to 7, placing the mixture in a dark room, stirring and degrading for 40min, wherein the experimental temperature is normal temperature, and the stirring speed is 150 r/min; measuring the absorbance of the tannic acid solution before and after degradation by using an ultraviolet spectrophotometer to obtain the concentration of the tannic acid solution; and the degradation rate of tannic acid was calculated, and the results are shown in table 3;
TABLE 3
| Examples | 1 | 2 | 3 | 4 | 5 | 6 |
| The degradation rate% | 60 | 60 | 65 | 66 | 68 | 68 |
Performing a simulated tannin degradation experiment by using the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure prepared in the embodiments 1-6; adding 0.15g of the titanium dioxide loaded super-light carbon aerogel with the bionic structure prepared in the embodiment 1-6 into 500mL of 50ppm tannic acid solution, adjusting the pH value to 7, placing the mixture in natural illumination, stirring and degrading for 40min, wherein the experimental temperature is normal temperature, and the stirring speed is 150 r/min; measuring the absorbance of the tannic acid solution before and after degradation by using an ultraviolet spectrophotometer to obtain the concentration of the tannic acid solution; and the degradation rate of tannic acid was calculated, and the results are shown in table 4;
TABLE 4
| Examples | 1 | 2 | 3 | 4 | 5 | 6 |
| The degradation rate% | 75 | 75 | 78 | 79 | 85 | 85 |
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the examples shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (10)
1. A preparation method of super-light carbon aerogel with a bionic structure is characterized by comprising the following steps:
step one, adding konjac glucomannan into a graphene oxide aqueous solution, stirring for 10-15 min, then adding into a vacuum packaging bag for vacuum packaging, and controlling the vacuum degree to be 0.1 MPa; putting the vacuum packaging bag into high static pressure treatment equipment, sealing a pressurizing cavity, pressurizing and carrying out high static pressure treatment to obtain a konjac glucomannan-graphene oxide mixed solution;
step two, cooling the konjac glucomannan-graphene oxide mixed solution in a refrigerator at the temperature of 0-4 ℃ for 0.5-1 hour, placing the cooled konjac glucomannan-graphene oxide mixed solution into an ice mold directional freezing device for freezing after precooling until the konjac glucomannan-graphene oxide mixed solution is solidified into a frozen body, then freeze-drying the frozen body at the temperature of 60-70 ℃ below zero and under the vacuum degree of 1-6 Pa, and drying the frozen body for 2-3 days to prepare the konjac glucomannan-graphene oxide dried body;
step three, treating the konjac glucomannan-graphene oxide dried body at high temperature in a nitrogen atmosphere, and cooling to obtain konjac glucomannan-graphene carbon aerogel;
and step four, adding the konjac glucomannan-graphene carbon aerogel into a titanium sulfate aqueous solution, stirring, transferring into a polytetrafluoroethylene stainless steel reaction kettle, carrying out constant-temperature hydrothermal reaction at 180-220 ℃ for 10-15 h, naturally cooling to obtain a hydrothermal product, cleaning the obtained hydrothermal product, and drying in vacuum to obtain the titanium dioxide loaded ultra-light carbon aerogel with the bionic structure.
2. The method for preparing the ultra-light carbon aerogel with the bionic structure according to claim 1, wherein the konjac glucomannan is replaced by the modified konjac glucomannan, and the preparation method comprises the following steps: adding 30-35 parts by weight of konjac glucomannan and 10-15 parts by weight of polyvinyl alcohol into a stainless steel high-pressure reaction kettle with stirring, and adding CO2Blowing air in the stainless steel high-pressure reaction kettle clean and introducing CO2Sealing, stirring and swelling for 2-3 hours at 65 ℃ and 12.5MPa, relieving pressure, adding 3-5 parts of cross-linking agent, and introducing CO2Sealing, stirring and reacting for 2-3 hours at 80 ℃ and 13.5MPa, decompressing, and drying to obtain the modified konjac glucomannan.
3. The method for preparing the bionic ultra-light carbon aerogel with the structure as claimed in claim 1, wherein in the first step, the graphene oxide aqueous solution has a mass percentage concentration of 1% -3%; the mass ratio of the konjac glucomannan to the graphene oxide in the graphene oxide aqueous solution is 1:5 to 20.
4. The method for preparing the bionic structure ultra-light carbon aerogel according to claim 1, wherein in the first step, the parameters of the high static pressure treatment are as follows: raising the pressure to 500-700 MPa at a pressure raising speed of 2-5 MPa/s, and carrying out pressure maintaining treatment at 35-55 ℃ for 30-60 min; the vacuum packaging bag is a nylon-polyethylene composite bag.
5. The method for preparing the ultra-light carbon aerogel with the bionic structure according to claim 2, wherein the cross-linking agent is any one of glutaraldehyde, epichlorohydrin, trimesoyl chloride, phthaloyl chloride, isophthaloyl chloride and terephthaloyl chloride.
6. The method for preparing the biomimetic-structure ultra-light carbon aerogel according to claim 1, wherein in the first step, the method for preparing the graphene oxide aqueous solution comprises: adding graphene oxide and a dispersing agent into deionized water, stirring for 30-60 min, and carrying out ultrasonic treatment in an ultrasonic cleaning machine for 0.5-1 h to obtain a graphene oxide aqueous solution; the power of the ultrasonic is 500-1000W, and the ultrasonic frequency is 40-60 KHz.
7. The method for preparing the bionic ultra-light carbon aerogel with the structure as claimed in claim 6, wherein the dispersant is NaOH or Na2CO3Any one of sodium carboxymethylcellulose and 1, 3-dimethyl imidazole nitrate; the mass fraction of the dispersing agent in the graphene oxide aqueous solution is 0.01-0.03%.
8. The method for preparing the ultra-light carbon aerogel with the bionic structure according to claim 1, wherein in the third step, the high-temperature treatment process of the konjac glucomannan-graphene oxide dry body in the nitrogen atmosphere comprises the following steps: adding the konjac glucomannan-graphene oxide dry body into a rotary furnace, introducing nitrogen at a flow rate of 100-200 mL/min, heating to 200-300 ℃ at a speed of 1-2 ℃/min, preserving heat for 1-3 h, continuously heating to 500-600 ℃ at a speed of 1-2 ℃/min, preserving heat for 1-2 h, continuously heating to 800-850 ℃ at a speed of 1-2 ℃/min, preserving heat for 1-2 h, then cooling to 250-350 ℃ at a speed of 5-10 ℃/min, preserving heat for 10-30 min, and naturally cooling to room temperature; the rotating speed of the rotary furnace is 5-12 r/min.
9. The method for preparing the bionic structure ultra-light carbon aerogel of claim 1, wherein in the fourth step, the concentration of the titanium sulfate aqueous solution is 2-5 g/L; the mass ratio of the konjac glucomannan-graphene carbon aerogel to the titanium sulfate in the titanium sulfate aqueous solution is 1-3: 1.
10. The preparation method of the biomimetic-structured ultra-light carbon aerogel according to claim 1, wherein in the third step, the konjac glucomannan-graphene carbon aerogel is pretreated by the following steps: dispersing konjac glucomannan-graphene carbon aerogel in H according to the concentration of 0.3-0.5 mg/mL2O2And FeCl3In an aqueous solution of (A), H2O2FeCl of3Stirring and uniformly mixing the materials according to the molar ratio of 1: 2-5, adjusting the pH to 3-5 by using a NaOH aqueous solution, and then treating the materials for 5-10 min under the microwave irradiation condition; the power of microwave irradiation is 100-500W, and the temperature of microwave irradiation is 60-80 ℃.
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