CN111018059A - Preparation method of carbon fiber inorganic polymer composite electrode - Google Patents
Preparation method of carbon fiber inorganic polymer composite electrode Download PDFInfo
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- CN111018059A CN111018059A CN201911171291.XA CN201911171291A CN111018059A CN 111018059 A CN111018059 A CN 111018059A CN 201911171291 A CN201911171291 A CN 201911171291A CN 111018059 A CN111018059 A CN 111018059A
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- carbon fiber
- polymer composite
- inorganic polymer
- rhodamine
- composite electrode
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 57
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 57
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 229920000592 inorganic polymer Polymers 0.000 title claims abstract description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 114
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 24
- 239000007787 solid Substances 0.000 claims abstract description 22
- 230000015556 catabolic process Effects 0.000 claims abstract description 19
- 238000006731 degradation reaction Methods 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 229910021487 silica fume Inorganic materials 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 11
- 239000010935 stainless steel Substances 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 238000003618 dip coating Methods 0.000 claims abstract description 7
- 239000002351 wastewater Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 24
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000002835 absorbance Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000008247 solid mixture Substances 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 239000002910 solid waste Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 16
- 238000000576 coating method Methods 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 235000014692 zinc oxide Nutrition 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 239000011787 zinc oxide Substances 0.000 description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 6
- 239000010405 anode material Substances 0.000 description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229910052797 bismuth Inorganic materials 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 5
- -1 carbon nitrides Chemical class 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 230000004298 light response Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002073 nanorod Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 150000001622 bismuth compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002736 metal compounds Chemical class 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052755 nonmetal Chemical class 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 3
- 229910002915 BiVO4 Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- 241000195940 Bryophyta Species 0.000 description 1
- 229910002475 Cu2ZnSnS4 Inorganic materials 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 229910005900 GeTe Inorganic materials 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- MBBZMMPHUWSWHV-BDVNFPICSA-N N-methylglucamine Chemical compound CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO MBBZMMPHUWSWHV-BDVNFPICSA-N 0.000 description 1
- 229910015494 Ni1-xFex Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 241000037831 Polygonatum sibiricum Species 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229960003194 meglumine Drugs 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 235000011929 mousse Nutrition 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 208000017983 photosensitivity disease Diseases 0.000 description 1
- 231100000434 photosensitization Toxicity 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- 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
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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Abstract
The invention discloses a preparation method of a carbon fiber inorganic polymer composite electrode, which comprises the following steps of mixing carbon fiber, metakaolin, silica fume, solid sodium hydroxide and deionized water according to a mass ratio of 0.2-0.6: 6: 4: 2: 8, stirring, mixing, uniformly dip-coating on the surface of the pretreated stainless steel substrate, drying, curing and reacting to obtain the carbon fiber inorganic polymer composite electrode, wherein the preparation process has no three-waste discharge and is environment-friendly, and the method is a new way for utilizing the solid waste silica fume with high added value. The rhodamine B organic dye is applied to an anode for photoelectrocatalytic organic dye wastewater degradation, and the photoelectrocatalytic degradation rate of the rhodamine B organic dye can reach 99.77%.
Description
Technical Field
The invention belongs to the field of preparation of a photoelectrocatalysis electrode material and resource utilization of solid waste, relates to preparation of an electrocatalysis anode material, and particularly relates to a preparation method of a carbon fiber inorganic polymer composite electrode and application of the carbon fiber inorganic polymer composite electrode in dye degradation.
Background
The photoelectrocatalysis oxidation technology is one of effective ways for degrading organic pollutants in water. The core of the photoelectrocatalysis oxidation technology is the preparation of the photoanode material. The material with photocatalytic activity is loaded on the surface of a conductive carrier by methods such as an anodic oxidation method, a thermal decomposition method, a pulse electrodeposition method, a hydrothermal deposition method, a hydrothermal method, a high-temperature liquid phase growth method, a coating method, a dipping and pulling method and the like to prepare the photoanode. At present, the materials loaded by the photoanode mainly comprise two main types of metal compounds and non-metal compounds. The metal oxides include mainly titanium oxides, zinc oxides, iron oxides, bismuth compounds, and other metal compounds. The non-metallic compounds include carbon nitrides and silicon carbides.
TiO2The most studied materials are used in the field of photoelectrocatalysis. A large number of scholars can carry out TiO modification by means of compound semiconductors, precious metal deposition, dye photosensitization, nonmetal doping and the like2The modification is carried out to widen the photoresponse range of the photo-catalytic photo-anode and improve the separation efficiency of photo-generated electrons and holes, thereby preparing the photo-catalytic photo-anode with good performance[1-5]. There are also patents relating to TiO2Preparation of photoanode material[6-11]。
ZnO and TiO2The direct band gap of (A) can be approached, and the method can be used in the field of photoelectrocatalysis. Yan Weiping[12]In for iso-use2O3The sensitized ZnO nanorod array is used for preparing the photoelectrocatalysis anode material with good catalytic performance. Li Wei soldier[13]Equal, Korean[14]The catalytic performance of the zinc oxide photo-anode is improved by adopting a semiconductor compounding method. Wudi[15]A method for preparing a visible light response type zinc oxide semiconductor photoelectric material is reported. Panlun[16]A Z-type junction ZnO-WO is disclosed3A method for preparing an electrode.
In addition, some researchers studied Fe2O3The photoelectrocatalysis performance of the photoanode. For example, a gold ring[17]And the like adopts Al and Ta co-doped to prepare visible light response type Ta/Al-Fe2O3Photocatalytic films are used for photoelectrocatalysis. Lican (Lican)[18]Et al report an α -Fe2O3The photo-anode and the preparation method thereof.
The bismuth compound used for the photoelectrocatalysis photoanode is mainly bismuth vanadate, and in addition, bismuth tungstate and bismuth phosphate. The preparation method of bismuth compound photo-anode is reported in the literature and patent[19-26]。
Other metal oxides being predominantly SnO2And CuWO4. Xudesong[27]The mulsane light[28]Equal, yellow clever[29]Et al report modified SnO2Preparation of photo-anode, Liu Zhi Hua[30]Etc. disclose Co-doped nanorod-shaped CuWO4A method for preparing a photo-anode film.
Carbon nitride is a non-metal oxide photo-anode material which is researched more. Cattle courage[31]The platinum atom modified carbon nitride nanorod photoelectrocatalysis electrode is prepared by adopting a noble metal modification means. In addition, SiC is also used by scholars for the preparation of photoanodes, such as: good and bright in appearance[32]And the like to prepare the N-doped SiC monocrystal nano-pore array photoelectrocatalysis anode.
In conclusion, the applicant consults a large amount of domestic and foreign literature data through a system, and does not find any relevant report about the preparation method of any carbon fiber inorganic polymer composite electrode and the application of the carbon fiber inorganic polymer composite electrode in organic dye degradation.
The following are the main references relevant to the present invention:
[1]zhao Yi Ming, Yang Relay Kai, horseFuhui, Chen Zhang Miaoxiong, Weizi Juan, Zhang Yufei, Cheng Ming, Yangxue, Xiaonan, Wang Guo Fang, Wang Xin, Huang Keke, porous silicon/TiO2Preparation of nano-wire photo-anode and its photoelectrocatalysis performance, inorganic chemistry report, 2019, 35 (04): 613-620.
[2]Chuhuanan, Li Deng, Liu Guantao, Liqun, Shijiaying and TiN(0.3)/CeO2Construction of photo-anode material and its photo-electro-catalytic properties, catalytic statement 2015, 36 (04): 550-554.
[3]Sunjijie, Hequan, Li Jian, Liuchun Guang, Shenyang, ZnFe2O4/TiO2Preparation of nanotube array electrode and research on photoelectrocatalytic degradation of phenol, chemical bulletin, 2013, 71 (02): 78-85.
[4]Gold billow, xu 38932, cun peng, chan min, feo (oh) -TiO2Preparation of a/CoPi composite light anode and the photoelectrocatalytic oxidation water performance thereof, the report of physical chemistry 2012, 28(10): 2276-2284.
[5]Zhang Mao Jun, Chen Ming, Wu Yuan Chun, Ag-CNT/TiO2The photoelectrocatalytic degradation of the composite electrode to methylene blue, a novel carbon material 2010, 25(05): 348-.
[6] A method for preparing a photoelectrocatalysis material electrode, a method for preparing a material electrode of royal phoenix martial arts, maoyu road, xumei, wangzhi, zhuigao, and wujun, a Chinese patent publication: CN108048867B, 2019.
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Disclosure of Invention
The invention aims to provide a preparation method of a carbon fiber inorganic polymer composite electrode, so as to reveal the change rule of the doping amount of carbon fibers in an electrocatalytic anode material and the degradation rate of photoelectrocatalytic organic dye wastewater.
In order to realize the task, the invention adopts the following technical solution:
the preparation method of the carbon fiber inorganic polymer composite electrode is characterized by comprising the following steps of: 6: 4: 2: and 8, stirring and mixing, uniformly dip-coating on the surface of the pretreated stainless steel substrate, drying, and curing to obtain the carbon fiber inorganic polymer composite electrode.
The method specifically comprises the following steps:
(1) weighing carbon fiber, metakaolin and silica fume according to the formula, mixing, putting into a vibration mill, and milling for 20 seconds to form a solid mixture;
(2) weighing solid sodium hydroxide according to the formula amount, putting the solid sodium hydroxide into a beaker, adding ionized water according to the formula amount into the beaker, and completely dissolving the solid sodium hydroxide under stirring to obtain a sodium hydroxide solution;
(3) pouring the solid mixture into a sodium hydroxide solution, and fully stirring to form uniform slurry;
(4) and (3) dip-coating the slurry on the surface of the pretreated steel sheet substrate, placing the pretreated steel sheet substrate in a drying oven under a sealed condition, and curing and reacting for 8 hours at 80 ℃ to obtain the carbon fiber inorganic polymer composite electrode.
The research of the applicant finds that the obtained carbon fiber inorganic polymer composite electrode can be applied to the application of degrading rhodamine B organic dye wastewater through photoelectrocatalysis.
The specific application comprises the following steps:
(1) connecting the prepared carbon fiber inorganic polymer composite electrode with the positive electrode of a direct current stabilized power supply to serve as the anode of a photoelectrocatalysis device, and connecting the pretreated steel sheet electrode with the negative electrode of the direct current stabilized power supply to serve as the cathode of the photoelectrocatalysis device;
(2) the initial concentration C is prepared by a volumetric flask0Adding a certain amount of sodium persulfate into the rhodamine B dye aqueous solution; using UV-visible spectrophotometer at lambdamaxInitial absorbance a was measured at 554nm0；
(3) Placing the anode and the cathode in parallel in a container with a certain volume and concentration of CoIn the rhodamine B dye aqueous solution, a certain bias voltage is applied to an electrode, a xenon lamp is used for simulating sunlight to irradiate for a certain time at room temperature, the reaction solution is taken out and put into a cuvette, and an ultraviolet-visible spectrophotometer is used for measuring the color temperature of the rhodamine B dye aqueous solution at lambdamaxAbsorbance A at time t was measured at 554nmtDye concentration of Ct；
(4) After the absorbance is measured, all the reaction liquid is put into the reactor again;
(5) and (5) repeating the step (3) and the step (4) until the absorbance of the rhodamine B dye aqueous solution does not change along with the change of time any more, and calculating the degradation rate of the rhodamine B dye by adopting the following formula:
the preparation method of the carbon fiber inorganic polymer composite electrode has the innovation points that: a carbon fiber inorganic polymer composite electrode which is not reported in the literature is prepared and can be used as a photoelectrocatalysis anode. The conductivity of the carbon fiber inorganic polymer composite electrode is adjusted by controlling the doping amount of the carbon fiber, so that the controllability of photoelectrocatalysis is achieved. Meanwhile, the preparation process has no three-waste discharge, is environment-friendly, and realizes high value-added recycling of solid waste silicon ash.
Drawings
FIG. 1 is a process flow chart of the preparation of the carbon fiber inorganic polymer composite electrode and the photoelectrocatalytic degradation of organic dye wastewater;
FIG. 2 is a photograph of a carbon fiber inorganic polymer composite electrode;
FIG. 3 is an XRD diffraction pattern of the feedstock (silica fume and metakaolin mixture) and CFICE samples;
FIG. 4 is the photoelectrocatalytic degradation rate of CFICE sample on rhodamine B dye;
the present invention will be described in further detail with reference to the following drawings and examples.
Detailed Description
It should be noted that the following examples are only for better illustrating the present invention, and the present invention is not limited to these examples.
The embodiment provides a preparation method of a carbon fiber inorganic polymer composite electrode, which is characterized in that carbon fibers, metakaolin, silica fume, solid sodium hydroxide and deionized water are selected as main raw materials, wherein the mass ratio of the carbon fibers, the metakaolin, the silica fume, the solid sodium hydroxide and the deionized water is 0.2-0.6: 6: 4: 2: 8.
and stirring and mixing the carbon fiber, the metakaolin, the silica fume, the solid sodium hydroxide and the deionized water, uniformly dip-coating the mixture on the surface of the pretreated stainless steel substrate, and drying and curing the mixture to obtain the carbon fiber inorganic polymer composite electrode.
The raw material sources are as follows:
(1) carbon fibers, available from tianjin forest new materials science and technology ltd;
(2) metakaolin, purchased from Chenyi refractory abrasives, Inc.;
(3) silica fume, available from minnew energy materials, ltd, available in huohao city, inner mongolia;
(4) solid sodium hydroxide, purchased from chemical reagents of national drug group, ltd, analytically pure reagent;
(5) the stainless steel substrate is a 304 type stainless steel sheet with the thickness of 15mm (length) multiplied by 15mm (width) multiplied by 0.2mm (thickness);
the pretreatment process of the 304 type stainless steel sheet comprises the steps of polishing the surface of the steel sheet by using sand paper, then placing the steel sheet in a sodium hydroxide solution with the mass fraction of 40%, carrying out water bath reaction for 1h at 80 ℃ under magnetic stirring, washing with deionized water after taking out, then placing the steel sheet in an oxalic acid solution with the mass fraction of 10%, carrying out water bath reaction for 30min at 95 ℃ under magnetic stirring, washing with deionized water after taking out, drying, and placing in absolute ethyl alcohol for storage and later use.
The preparation method comprises the following steps:
(1) weighing carbon fiber, metakaolin and silica fume according to the formula, mixing, putting into a vibration mill, and milling for 20 seconds to form a solid mixture;
(2) weighing solid sodium hydroxide according to the formula amount, putting the solid sodium hydroxide into a beaker, adding ionized water according to the formula amount into the beaker, and completely dissolving the solid sodium hydroxide under stirring to obtain a sodium hydroxide solution;
(3) pouring the solid mixture into a sodium hydroxide solution, and fully stirring to form uniform slurry;
(4) and (3) dip-coating the slurry on the surface of the pretreated steel sheet substrate, placing the pretreated steel sheet substrate in a drying oven under a sealed condition, and curing and reacting for 8 hours at 80 ℃ to obtain the carbon fiber inorganic polymer composite electrode.
The following are specific examples given by the inventors.
Example 1:
accurately weighing 2g of solid sodium hydroxide, weighing 8mL of deionized water, and dissolving the solid sodium hydroxide in the deionized water in a beaker to obtain a sodium hydroxide solution;
accurately weighing 6g of metakaolin, 4g of silica fume and 0.6g of carbon fiber, mixing, and then putting into a vibration mill for grinding for 20 s; pouring the mixed powder into a sodium hydroxide solution, stirring by using a glass rod, uniformly mixing, and carrying out chemical reaction to obtain uniform slurry; the slurry was dip-coated on the surface of a pretreated 304 type stainless steel sheet 15mm (length) 15mm (width) 0.2mm (thickness) (see FIG. 1 for the treatment process), the coating thickness was about 100 μm, the sheet was placed in a dry box under a sealed condition and cured at 80 ℃ for 8 hours to obtain a Carbon Fiber Inorganic polymer Composite Electrode (abbreviated as CFICE; the amount of Carbon Fiber used was 0.6g, and designated as 6CFICE), and the photograph of the Carbon Fiber Inorganic polymer Composite Electrode was as shown in FIG. 2.
The XRD diffraction patterns of the starting materials (silica fume and metakaolin mixture) and the 6CFICE sample are shown in FIG. 3.
Example 2:
all the procedures were the same as in example 1 except that the mass of the Carbon Fiber used was 0.4g, and a Carbon Fiber Inorganic polymer Composite Electrode (Carbon Fiber Inorganic-polymer Composite Electrode, abbreviated as: CFICE; Carbon Fiber amount 0.4g, designated as: 4CFICE) was obtained.
Example 3:
all the procedures were the same as in example 1 except that the mass of the Carbon Fiber used was 0.2g, and a Carbon Fiber Inorganic polymer Composite Electrode (Carbon Fiber Inorganic-polymer Composite Electrode, abbreviated as: CFICE; Carbon Fiber amount 0.2g, designated as: 2CFICE) was obtained; the XRD diffraction pattern of the 2CFICE sample is shown in fig. 3.
Example 4:
the carbon fiber inorganic polymer composite electrode (hereinafter referred to as 6CFICE) obtained in example 1 was connected to the positive electrode of a DC stabilized voltage power supply to serve as the anode of a photoelectrocatalysis device; connecting a steel sheet electrode with the same size as the anode with the negative electrode of a direct current stabilized voltage power supply to be used as the cathode of the photoelectrocatalysis device; putting an anode electrode and a cathode electrode in parallel into 100mL of rhodamine B solution (containing 2mmol/L of sodium persulfate) with the concentration of 5mg/L, wherein the electrode distance is 2 cm; simulation with xenon lampThe sunlight irradiates the anode at a distance of 15 cm; providing 0.8V bias voltage for the electrode by using a direct current stabilized voltage supply, starting timing, taking part of reaction solution in a cuvette every 3min, and measuring the maximum absorption wavelength (lambda) of the rhodamine B dye by using an ultraviolet-visible spectrophotometermax554nm), after the absorbance is measured, the reaction solution in the cuvette is put into the reaction system again, and the degradation rate of the rhodamine B dye is calculated by using the following formula (1):
as shown in FIG. 4, the photoelectrocatalytic degradation rate of 6CFICE on rhodamine B dye can reach 99.77% at 9 min.
Example 5:
the carbon fiber inorganic polymer composite electrode (hereinafter referred to as 4CFICE) obtained in example 2 and the positive electrode of a direct current stabilized voltage power supply are connected to be used as the anode of a photoelectrocatalysis device; connecting a steel sheet electrode with the same size as the anode with the negative electrode of a direct current stabilized voltage power supply to be used as the cathode of the photoelectrocatalysis device; the remaining steps were the same as in example 4, and the degradation rate of rhodamine B dye was calculated using formula (1) in example 4.
As shown in FIG. 4, the photoelectrocatalytic degradation rate of 4CFICE on rhodamine B dye can reach 99.76% at 12 min.
Example 6:
the carbon fiber inorganic polymer composite electrode (hereinafter referred to as 2CFICE) obtained in example 3 was connected to the positive electrode of a DC stabilized voltage power supply to serve as the anode of a photoelectrocatalysis device; connecting a steel sheet electrode with the same size as the anode with the negative electrode of a direct current stabilized voltage power supply to be used as the cathode of the photoelectrocatalysis device; the remaining steps were the same as in example 4, and the degradation rate of rhodamine B dye was calculated using formula (1) in example 4.
As shown in FIG. 4, the photoelectrocatalytic degradation rate of 2CFGE on rhodamine B dye can reach 99.46% at 18 min.
Comparative experimental examples are given below:
comparative experimental example 1:
accurately weighing 2g of solid sodium hydroxide, weighing 9mL of deionized water, and dissolving the solid sodium hydroxide in the deionized water in a beaker to obtain a sodium hydroxide solution; accurately weighing 6g of metakaolin, 4g of silica fume and 1.0g of carbon fiber, mixing, placing in a vibration mill, grinding for 20s, pouring the mixed powder into a sodium hydroxide solution, stirring and mixing uniformly by using a glass rod, and carrying out chemical reaction to obtain uniform slurry; the slurry is coated on the surface of a pretreated 304 type stainless steel sheet (the treatment process is shown in figure 1) with the thickness of about 100 mu m, the surface is soaked and coated with the slurry, the thickness of the coating is 15mm (length) multiplied by 15mm (width) multiplied by 0.2mm (thickness), the coating is placed in a drying oven under the sealing condition, the curing reaction is carried out for 8 hours at the temperature of 80 ℃, and the prepared carbon fiber inorganic polymer composite electrode surface coating has cracks and is easy to fall off.
Comparative experiment example 2:
accurately weighing 2g of solid sodium hydroxide, weighing 8mL of deionized water, and dissolving the solid sodium hydroxide in the deionized water in a beaker to obtain a sodium hydroxide solution; accurately weighing 10g of metakaolin, and putting the metakaolin in a vibration mill for grinding for 20 s; pouring the ground powder into a sodium hydroxide solution, stirring by using a glass rod, uniformly mixing, and carrying out chemical reaction to obtain uniform slurry; the slurry is coated on the surface of a pretreated 304 type stainless steel sheet (the treatment process is shown in figure 1) with the thickness of about 100 mu m, the surface is soaked and coated with the slurry, the thickness of the coating is 15mm (length) multiplied by 15mm (width) multiplied by 0.2mm (thickness), the coating is placed in a drying oven under the sealing condition, the curing reaction is carried out for 8 hours at the temperature of 80 ℃, and the prepared inorganic polymer composite electrode has low surface coating strength and cracks.
Comparative experiment example 3:
accurately weighing 2g of solid sodium hydroxide, weighing 8mL of deionized water, and dissolving the solid sodium hydroxide in the deionized water in a beaker to obtain a sodium hydroxide solution; accurately weighing 6g of metakaolin, 4g of silica fume and 0.2g of carbon fiber, and placing in a vibration mill for grinding for 20 s; pouring the mixed powder into a sodium hydroxide solution, stirring by using a glass rod, uniformly mixing, and carrying out chemical reaction to obtain uniform slurry; the slurry is dipped and coated on the surface of a pretreated 304 type stainless steel sheet with the thickness of 15mm (length) multiplied by 15mm (width) multiplied by 0.2mm (thickness) (the treatment process is shown in figure 1), the coating thickness is about 100 mu m, the sheet is placed in a drying box under the condition of no sealing, and the sheet is cured and reacted for 8 hours at the temperature of 80 ℃, so that the surface coating of the prepared carbon fiber inorganic polymer composite electrode has a plurality of cracks, and the coating has the phenomenon of large-area falling off.
Claims (6)
1. The preparation method of the carbon fiber inorganic polymer composite electrode is characterized by comprising the following steps of: 6: 4: 2: and 8, stirring and mixing, uniformly dip-coating on the surface of the pretreated stainless steel substrate, drying, and curing to obtain the carbon fiber inorganic polymer composite electrode.
2. The method according to claim 1, comprising in particular the steps of:
(1) weighing carbon fiber, metakaolin and silica fume according to the formula, mixing, putting into a vibration mill, and milling for 20 seconds to form a solid mixture;
(2) weighing solid sodium hydroxide according to the formula amount, putting the solid sodium hydroxide into a beaker, adding ionized water according to the formula amount into the beaker, and completely dissolving the solid sodium hydroxide under stirring to obtain a sodium hydroxide solution;
(3) pouring the solid mixture into a sodium hydroxide solution, and fully stirring to form uniform slurry;
(4) and (3) dip-coating the slurry on the surface of the pretreated steel sheet substrate, placing the pretreated steel sheet substrate in a drying oven under a sealed condition, and curing and reacting for 8 hours at 80 ℃ to obtain the carbon fiber inorganic polymer composite electrode.
3. The method according to claim 1, wherein the steel sheet is pretreated by polishing the surface of the steel sheet with sand paper, then placing the steel sheet in a sodium hydroxide solution with the mass fraction of 40%, performing a water bath reaction at 80 ℃ for 1h under magnetic stirring, taking out and washing with deionized water, then placing the steel sheet in an oxalic acid solution with the mass fraction of 10%, performing a water bath reaction at 95 ℃ for 30min under magnetic stirring, taking out and washing with deionized water and drying, and placing in absolute ethyl alcohol for storage.
4. A carbon fiber inorganic polymer composite electrode prepared by the method of any one of claims 1 to 3.
5. The use of the carbon fiber inorganic polymer composite electrode as claimed in any one of claims 1 to 4 for photoelectrocatalytic degradation of rhodamine B organic dye wastewater.
6. The use according to claim 5, comprising in particular the following steps:
(1) connecting the prepared carbon fiber inorganic polymer composite electrode with the positive electrode of a direct current stabilized power supply to be used as the anode of a photoelectric catalytic device, and connecting the pretreated steel sheet electrode with the negative electrode of the direct current stabilized power supply to be used as the cathode of the photoelectric catalytic device;
(2) the initial concentration C is prepared by a volumetric flask0Adding a certain amount of sodium persulfate into the rhodamine B dye aqueous solution; using UV-visible spectrophotometer at lambdamaxInitial absorbance a was measured at 554nm0；
(3) Placing the anode and the cathode in parallel in a container with a certain volume and concentration of C0In the rhodamine B dye aqueous solution, a certain bias voltage is applied to an electrode, a xenon lamp is used for simulating sunlight to irradiate for a certain time at room temperature, the reaction solution is taken out and put into a cuvette, and an ultraviolet-visible spectrophotometer is used for measuring the color temperature of the rhodamine B dye aqueous solution at lambdamaxAbsorbance A at time t was measured at 554nmtAnd time t rhodamine B dye concentration Ct；
(4) After the absorbance is measured, all the reaction liquid is put into the reactor again;
(5) and (5) repeating the step (3) and the step (4) until the absorbance of the rhodamine B dye aqueous solution does not change along with the change of time any more, and calculating the degradation rate of the rhodamine B dye by adopting the following formula:
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