CN116621601A - Al/Fe/C micro-electrolysis ceramsite and preparation method and application thereof - Google Patents
Al/Fe/C micro-electrolysis ceramsite and preparation method and application thereof Download PDFInfo
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- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 91
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 49
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000011230 binding agent Substances 0.000 claims abstract description 24
- 239000010881 fly ash Substances 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 17
- 239000002351 wastewater Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000004898 kneading Methods 0.000 claims description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims description 10
- 239000000440 bentonite Substances 0.000 claims description 10
- 229910000278 bentonite Inorganic materials 0.000 claims description 10
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000571 coke Substances 0.000 claims description 10
- 238000003837 high-temperature calcination Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 5
- 238000004065 wastewater treatment Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- 244000017020 Ipomoea batatas Species 0.000 claims description 3
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 3
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 229960000892 attapulgite Drugs 0.000 claims description 3
- 229910052625 palygorskite Inorganic materials 0.000 claims description 3
- 229920001592 potato starch Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002023 wood Substances 0.000 claims description 3
- 239000000356 contaminant Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000012798 spherical particle Substances 0.000 claims description 2
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 abstract description 22
- 230000000694 effects Effects 0.000 abstract description 13
- 238000006731 degradation reaction Methods 0.000 abstract description 10
- 230000015556 catabolic process Effects 0.000 abstract description 9
- 229910052742 iron Inorganic materials 0.000 abstract description 9
- 238000003911 water pollution Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 28
- 238000010438 heat treatment Methods 0.000 description 27
- 239000000945 filler Substances 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 14
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000011282 treatment Methods 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- -1 fluoride ions Chemical class 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 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 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000001045 blue dye Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000006115 defluorination reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 229910017112 Fe—C Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 229910052598 goethite Inorganic materials 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
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- 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
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Abstract
The application discloses an Al/Fe/C micro-electrolysis ceramic particle, a preparation method and application thereof, and belongs to the technical field of water pollution control. The Al/Fe/C micro-electrolysis ceramsite comprises the following raw materials in percentage by mass: 20 to 60 percent of fly ash, 10 to 20 percent of aluminum powder and 10 percent of iron powder20 percent, 10 to 20 percent of carbon powder, 5 to 10 percent of binder and 5 to 10 percent of pore-forming agent. The Al/Fe/C micro-electrolysis ceramic particle has larger specific surface area (90-110 m) 2 And/g), better degradation effect and removal rate of PFOA reaching 88.86 percent.
Description
Technical Field
The application relates to the technical field of water pollution control, in particular to an Al/Fe/C micro-electrolysis ceramsite and a preparation method and application thereof.
Background
Perfluorooctanoic acid (PFOA) is a persistent organic pollutant, and the strong electronegativity of F element causes high polarization of C-F bond and has extremely large bond energy, so that PFOA has very strong heat stability, acid and alkali resistance, oxidation resistance and other properties, is difficult to biodegrade, and is easy to enrich in organisms. The removing method mainly comprises an adsorption method, a high-grade oxidation method, a high-grade reduction method and the like. Wherein, the adsorption of powdery activated carbon, granular activated carbon, goethite/silicon dioxide and alumina and the filtration technologies such as nanofiltration and reverse osmosis have remarkable removal effect on PFOA. However, all of the above methods simply transfer the PFOA to another medium, requiring subsequent further treatments such as incineration of the adsorbent to achieve complete destruction of the PFOA, resulting in increased treatment costs; while other advanced redox technologies typically require extreme laboratory conditions, they are costly to apply to actual process water treatment. Iron filings and activated carbon particles are filled in a reactor to form iron-carbon micro-electrolysis for PFOA degradation, but the removal rate is only about 30%. Therefore, the PFOA removal method with low cost and high efficiency is established, and has important significance for guaranteeing the water environment health and the water supply safety.
The micro-electrolysis technology is a technology for treating wastewater by using metal (generally iron) as an anode and nonmetal (generally carbon) as a cathode to contact in solution to form countless micro primary cells based on the principle of metal chemical corrosion, and can also be called an internal electrolysis method, an iron-carbon method, a corrosion battery method and the like. With the continuous expansion of the micro-electrolysis technology, the problems of application, such as hardening and passivation of filler, low treatment efficiency, poor material utilization and the like, are gradually revealed. Meanwhile, the traditional micro-electrolysis ceramsite is usually prepared by micro-electrolysis of iron and carbon, and the electrode potential of Al is lower than that of Fe (-0.44V)), so that the potential difference between aluminum and carbon is larger than that between iron and carbon, and Al (OH) 3 And simultaneously has better flocculation effect. Few studies have combined aluminum carbon microelectrolysis with iron carbon microelectrolysis.
Disclosure of Invention
The application aims to provide an Al/Fe/C micro-electrolysis ceramic particle, and a preparation method and application thereof, which are used for solving the problems in the prior art. The preparation method provided by the application is simple and low in cost, and the prepared Al/Fe/C micro-electrolysis ceramsite can be used as a wastewater treatment filler to treat perfluorinated compounds in water.
In order to achieve the above object, the present application provides the following solutions:
one of the technical schemes of the application is as follows: the Al/Fe/C micro-electrolysis ceramsite comprises the following raw materials in percentage by mass: 20 to 60 percent of fly ash, 10 to 20 percent of aluminum powder, 10 to 20 percent of iron powder, 10 to 20 percent of carbon powder, 5 to 10 percent of binder and 5 to 10 percent of pore-forming agent.
Further, the carbon powder includes any one of coke and woody activated carbon.
Further, the binder includes any one of polymethacrylic acid, attapulgite powder and bentonite.
Further, the pore-forming agent comprises any one of ammonium chloride, sweet potato starch and ammonium bicarbonate.
Further, the mass ratio of the aluminum powder to the iron powder to the carbon powder is 1:1 (0.5-2).
The second technical scheme of the application is as follows: the preparation method of the Al/Fe/C micro-electrolysis ceramsite comprises the following steps:
mixing the raw materials with water according to the mass percentage, uniformly stirring, kneading and forming, and then drying in an inert atmosphere and calcining at a high temperature to obtain the Al/Fe/C micro-electrolysis ceramsite.
Drying and calcining are carried out under inert atmosphere, which can prevent Al in the preparation process 0 、Fe 0 Oxidation failure.
Further, the high-temperature calcination temperature is 800-900 ℃ and the time is 0.5-2 h.
Further, when the calcination temperature is 800 ℃, the temperature-raising program is: heating to 500 ℃ at 5 ℃/min, then heating to 800 ℃ at 10 ℃/min, and finally preserving heat for 0.5-2 h at 800 ℃.
When the calcination temperature is more than 800 ℃, the temperature raising program is as follows: heating to 500 ℃ at 5 ℃/min, then heating to 800 ℃ at 10 ℃/min, finally heating to the target temperature at 5 ℃/min, and finally preserving heat for 0.5-2 h at the target temperature.
Further, the kneading molding specifically includes: kneading to obtain spherical particle size of 10-15 mm.
If the raw pellets are too large, the bulk density is too small for use as a filler, and water flow is likely to flow directly through the gaps between the particles, failing to sufficiently contact the filler.
Further, the drying temperature is 75-85 ℃ and the drying time is 30-60 min.
The third technical scheme of the application: an application of the Al/Fe/C micro-electrolysis ceramsite in wastewater treatment.
Further, the contaminants in the wastewater include perfluorinated compounds.
Furthermore, when the Al/Fe/C micro-electrolysis ceramsite is used for treating the perfluorinated compound wastewater, the adding amount of the Al/Fe/C micro-electrolysis ceramsite is 10-30 g/L wastewater.
Common micro-electrolysis reaction systems include single-element, binary, ternary and above micro-electrolysis reaction systems. The ternary micro-electrolysis filler is formed by adding two metals or nonmetal on the basis of the ternary micro-electrolysis filler, so that the electron acceptor can be multiplied, the electron transmission rate is obviously increased, and the ternary micro-electrolysis filler has a greater advantage in the process of removing wastewater pollutants. The traditional micro-electrolysis ceramsite is usually prepared by micro-electrolysis of iron and carbon, and the electrode potential of Al is lower than that of Fe (-0.44V), so that the potential difference between aluminum and carbon is larger than that between iron and carbon, and the micro-electrolysis ceramsite has stronger electron transfer capability.
The traditional micro-electrolysis filler is easy to harden, and iron is oxidized in the use process, so that an oxide layer is generated to cover the surface of the filler, so that the filler is agglomerated and fails. According to the application, the iron powder, the aluminum powder and the carbon powder are fully bonded together through high-temperature sintering to prepare the granular filler, so that the problem that the traditional iron-carbon micro-electrolysis filler is easy to harden can be solved, and the recycling utilization of the fly ash is realized; the prepared Al/Fe/C micro-electrolysis ceramsite has certain strength (more than 10 MPa) and porosity (20-50%), and high specific surface area, and can be used as a wastewater treatment filler.
The application discloses the following technical effects:
(1) The Al/Fe/C micro-electrolysis ceramic particle has larger specific surface area (90-110 m) 2 And/g), better degradation effect and removal rate of PFOA reaching 88.86 percent.
(2) Compared with the traditional iron-carbon ceramsite, the aluminum-carbon micro-electrolysis combined iron-carbon micro-electrolysis method has the advantages that an Al-Fe-C ternary micro-electrolysis system can be formed due to the addition of aluminum, the electron acceptor can be increased in multiple, the electron transmission rate is obviously increased, and the method has a greater advantage in the process of removing wastewater pollutants. The pure iron carbon can only generate the reaction formula (1), and can generate two processes of the reaction formula (1) and the reaction formula (2) after aluminum powder is added.
C 8 F 15 O 2 - +Fe 0 +H 2 O→C 8 F 14 HO 2 - +Fe 2+ +F-+OH- ①
C 8 F 15 HO 2 - +Al 0 +H 2 O→C 8 F 13 H 2 O 2 - +Al 3+ +2F - +OH - ②
(3) The application provides a novel method for degrading novel persistent organic pollutants PFOA in water, which has lower cost and higher removal efficiency compared with the traditional advanced oxidation, advanced reduction and the like.
(4) The Al/Fe/C micro-electrolysis ceramsite disclosed by the application is simple in preparation method, low in cost and controllable in product shape and size, and can be used as a sewage treatment filler for treating wastewater containing organic pollutants difficult to degrade.
(5) The application combines the fly ash, the aluminum powder, the iron powder, the carbon powder and the binder and the pore-forming agent for granulation, can overcome the problem that the traditional iron-carbon micro-electrolysis filler is easy to harden, and realizes the recycling utilization of the fly ash; meanwhile, the prepared Al/Fe/C micro-electrolysis ceramsite has certain strength (more than 10 MPa) and porosity (20-50%), and high specific surface area, and can be used as a wastewater treatment filler.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a diagram showing the final product of the Al/Fe/C micro-electrolytic ceramic particles prepared in example 4 of the present application;
FIG. 2 is a microscopic morphology diagram of the Al/Fe/C micro-electrolysis ceramic particles prepared in the embodiment 4 of the application;
FIG. 3 is a graph showing the effect of removing PFOA from iron-carbon ceramic particles, aluminum-carbon ceramic particles and Al/Fe/C micro-electrolytic ceramic particles prepared in example 4 of the present application;
FIG. 4 shows the change of the concentration of fluoride ions in the PFOA degradation process of the Al/Fe/C ceramsite prepared in the embodiment 4 of the present application;
FIG. 5 is a graph showing the degradation effect of Al/Fe/C ceramsite prepared in example 4 of the present application on methylene blue dye wastewater;
FIG. 6 is a color change chart of the Al/Fe/C ceramsite degradation methylene blue dye wastewater prepared in example 4 of the application.
Detailed Description
Various exemplary embodiments of the application will now be described in detail, which should not be considered as limiting the application, but rather as more detailed descriptions of certain aspects, features and embodiments of the application.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the application. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the application described herein without departing from the scope or spirit of the application. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present application. The specification and examples of the present application are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The "parts" described in the examples below are all "parts by weight".
Example 1
A preparation method of Al/Fe/C micro-electrolysis ceramsite comprises the following steps:
(1) 30g of fly ash, 9g of iron powder, 9g of aluminum powder, 9g of carbon powder (coke), 3.15g of binder (bentonite) and 3.15g of pore-forming agent (ammonium chloride) are weighed.
The mass percentage of the fly ash is 47.40%, the total mass percentage of the iron powder, the aluminum powder and the carbon powder is 42.65%, and the Al: fe: c=1:1:1, binder and pore former total mass percent is 9.95%.
(2) Adding water into the raw materials in the step (1), mixing and stirring, and manually kneading to obtain raw material balls with the diameter of 10-15 mm.
(3) And (3) drying the raw material balls in a vacuum drying oven, and drying at 80 ℃ for 45min under the protection of nitrogen to remove excessive moisture to obtain the ceramsite.
(4) The ceramsite is put into a tubular atmosphere furnace, high-temperature calcination is carried out under the protection of nitrogen, and the temperature rise program is as follows: at 0-500 deg.c (heating rate of 5 deg.c/min), 500-800 deg.c (heating rate of 10 deg.c/min), 800-900 deg.c (heating rate of 5 deg.c/min), and final heat preservation at 900 deg.c for 2 hr to obtain the micro electrolytic Al/Fe/C haydite.
Example 2
A preparation method of Al/Fe/C micro-electrolysis ceramsite comprises the following steps:
(1) 30g of fly ash, 15g of iron powder, 15g of aluminum powder, 7.5g of carbon powder (coke), 3.75g of binder (bentonite) and 3.75g of pore-forming agent (ammonium chloride) are weighed.
The mass percentage of the fly ash is 40%, the total mass percentage of the iron powder, the aluminum powder and the carbon powder is 50%, and the weight percentage of Al: fe: c=1:1:0.5, binder and pore former total mass percent is 10%.
(2) Adding water into the raw materials in the step (1), mixing and stirring, and manually kneading to obtain raw material balls with the diameter of 10-15 mm.
(3) And (3) drying the raw material balls in a vacuum drying oven, and drying at 80 ℃ for 45min under the protection of nitrogen to remove excessive moisture to obtain the ceramsite.
(4) The ceramsite is put into a tubular atmosphere furnace, high-temperature calcination is carried out under the protection of nitrogen, and the temperature rise program is as follows: at 0-500 deg.c (heating rate of 5 deg.c/min), 500-800 deg.c (heating rate of 10 deg.c/min), 800-900 deg.c (heating rate of 5 deg.c/min), and final heat preservation at 900 deg.c for 2 hr to obtain the micro electrolytic Al/Fe/C haydite.
Example 3
A preparation method of Al/Fe/C micro-electrolysis ceramsite comprises the following steps:
(1) 24.33g of fly ash, 5.56g of iron powder, 5.56g of aluminum powder, 8.34g of carbon powder (coke), 2.43g of binder (bentonite) and 2.43g of pore-forming agent (ammonium chloride) are weighed.
The mass percentage of the fly ash is 50%, the total mass percentage of the iron powder, the aluminum powder and the carbon powder is 40%, and the mass percentage of Al: fe: c=1:1:1.5, binder and pore former total mass percent is 10%.
(2) Adding water into the raw materials in the step (1), mixing and stirring, and manually kneading to obtain raw material balls with the diameter of 10-15 mm.
(3) And (3) drying the raw material balls in a vacuum drying oven, and drying at 80 ℃ for 45min under the protection of nitrogen to remove excessive moisture to obtain the ceramsite.
(4) The ceramsite is put into a tubular atmosphere furnace, high-temperature calcination is carried out under the protection of nitrogen, and the temperature rise program is as follows: at 0-500 deg.c (heating rate of 5 deg.c/min), 500-800 deg.c (heating rate of 10 deg.c/min), and final heat maintaining at 800 deg.c for 1.5 hr to obtain the micro electrolytic Al/Fe/C haydite.
Example 4
A preparation method of Al/Fe/C micro-electrolysis ceramsite comprises the following steps:
(1) 33.36g of fly ash, 5.56g of iron powder, 5.56g of aluminum powder, 5.56g of carbon powder (coke), 2.78g of binder (bentonite) and 2.78g of pore-forming agent (ammonium chloride) are weighed.
60% of fly ash, 30% of iron powder, aluminum powder and carbon powder, and Al: fe: c=1:1:1, the total mass percent of the binder and the pore-forming agent being 10%.
(2) Adding water into the raw materials in the step (1), mixing and stirring, and manually kneading to obtain raw material balls with the diameter of 10-15 mm.
(3) And (3) drying the raw material balls in a vacuum drying oven, and drying at 80 ℃ for 45min under the protection of nitrogen to remove excessive moisture to obtain the ceramsite.
(4) The ceramsite is put into a tubular atmosphere furnace, high-temperature calcination is carried out under the protection of nitrogen, and the temperature rise program is as follows: at 0-500 deg.c (heating rate of 5 deg.c/min), 500-800 deg.c (heating rate of 10 deg.c/min), 800-900 deg.c (heating rate of 5 deg.c/min), and final heat preservation at 900 deg.c for 2 hr to obtain micro electrolytic ceramic grain with the final product chart shown in FIG. 1 and the micro morphology chart shown in FIG. 2.
As can be seen from FIG. 2, the Al/Fe/C micro-electrolysis ceramsite prepared by the embodiment has a rough surface and a certain pore structure, which is beneficial to contact between pollutants and materials and promotes degradation of the pollutants.
Example 5
The difference with example 1 is that the carbon powder is wood activated carbon, the binder is polymethacrylic acid, and the pore-forming agent is sweet potato starch.
Example 6
The difference with the embodiment 1 is that the carbon powder is wood activated carbon, the binder is attapulgite powder, and the pore-forming agent is ammonium bicarbonate.
Comparative example 1
The preparation method of the iron-carbon ceramsite comprises the following steps:
(1) 13.90g of fly ash, 5.56g of iron powder, 5.56g of carbon powder (coke), 1.39g of binder (bentonite) and 1.39g of pore-forming agent (ammonium chloride) are weighed.
50% of fly ash, 40% of iron powder and carbon powder, and Fe: c=1:1, the total mass percent of the binder and the pore-forming agent being 10%.
(2) Adding water into the raw materials in the step (1), mixing and stirring, and manually kneading to obtain raw material balls with the diameter of 10-15 mm.
(3) And (3) drying the raw material balls in a vacuum drying oven, and drying at 80 ℃ for 45min under the protection of nitrogen to remove excessive moisture to obtain the ceramsite.
(4) The ceramsite is put into a tubular atmosphere furnace, high-temperature calcination is carried out under the protection of nitrogen, and the temperature rise program is as follows: and (3) at 0-500 ℃ (heating rate is 5 ℃/min), 500-800 ℃ (heating rate is 10 ℃/min), 800-900 ℃ (heating rate is 5 ℃/min), and finally preserving heat for 2 hours at 900 ℃ to obtain the iron-carbon ceramsite (Fe/C ceramsite).
Comparative example 2
The preparation method of the aluminum-carbon ceramsite comprises the following steps:
(1) 27.8g of fly ash, 11.12g of aluminum powder, 11.12g of carbon powder (coke), 2.78g of binder (bentonite) and 2.78g of pore-forming agent (ammonium chloride) are weighed.
The mass percentage of the fly ash is 50%, the total mass percentage of the aluminum powder and the carbon powder is 40%, and the mass percentage of the Al: c=1:1, the total mass percent of the binder and the pore-forming agent being 10%.
(2) Adding water into the raw materials in the step (1), mixing and stirring, and manually kneading to obtain raw material balls with the diameter of 10-15 mm.
(3) And (3) drying the raw material balls in a vacuum drying oven, and drying at 80 ℃ for 45min under the protection of nitrogen to remove excessive moisture to obtain the ceramsite.
(4) The ceramsite is put into a tubular atmosphere furnace, high-temperature calcination is carried out under the protection of nitrogen, and the temperature rise program is as follows: at 0-500 deg.c (heating rate of 5 deg.c/min), 500-800 deg.c (heating rate of 10 deg.c/min), 800-900 deg.c (heating rate of 5 deg.c/min), and final heat preservation at 900 deg.c for 2 hr to obtain aluminum-carbon haydite.
Comparative example 3
The only difference from example 1 is that step (1) is specifically: 13.5g of fly ash, 9g of iron powder, 9g of aluminum powder, 9g of carbon powder (coke), 2.25g of binder (bentonite) and 2.25g of pore-forming agent (ammonium chloride) are weighed.
The mass percentage of the fly ash is 30%, the total mass percentage of the iron powder, the aluminum powder and the carbon powder is 60%, and the Al: fe: c=1:1:1, the total mass percent of the binder and the pore-forming agent being 10%.
Comparative example 4
The only difference from example 1 is that step (1) is specifically: 45g of fly ash, 9g of iron powder, 9g of aluminum powder, 18g of carbon powder (coke), 4.5g of binder (bentonite) and 4.5g of pore-forming agent (ammonium chloride) are weighed.
The mass percentage of the fly ash is 50%, the total mass percentage of the iron powder, the aluminum powder and the carbon powder is 40%, and the mass percentage of Al: fe: c=1:1:2, the total mass percent of binder and pore-forming agent being 10%.
The addition amount of the fly ash in the comparative example 3 is reduced, the porosity of the burned haydite is lower than that of the haydite of 50wt.% fly ash, and the adsorption effect is reduced, so that the overall removal rate is reduced; the amount of carbon powder in comparative example 4 was increased, and the relative amounts of aluminum and iron were smaller, and a sufficient number of primary cells could not be formed, resulting in low removal efficiency.
Comparative example 5
The only difference from example 1 is that the temperature increase program is: at 0-500 deg.c (with heating rate of 5 deg.c/min), 500-800 deg.c (with heating rate of 10 deg.c/min), 800-900 deg.c (with heating rate of 5 deg.c/min), and final heat preservation at 900 deg.c for 0.5 hr.
Comparative example 6
The only difference from example 1 is that the temperature increase program is: 0-500 ℃ (heating rate is 5 ℃/min), 500-800 ℃ (heating rate is 10 ℃/min), and finally preserving heat for 2h at 800 ℃.
Effect example 1
100mL of PFOA solution with the concentration of 50mg/L is prepared as simulated wastewater, and 1g of the iron-carbon ceramsite (Fe-C) prepared in comparative example 1 and 1g of the aluminum-carbon ceramsite (A) prepared in comparative example 2 are respectively weighedl-C) and the Al/Fe/C micro-electrolysis ceramic particles (Al-Fe-C) prepared in the example 4 are added into simulated wastewater, and mixed reaction is carried out at 25 ℃. After 210min of reaction, sampling is carried out, and detection is carried out by a high performance liquid chromatograph (HPLC SPD-16), wherein the detection conditions are as follows: the PFOA concentration was determined from the measured peak areas by a 5. Mu. m C18 column (4.6 x 150mM, shimadzu), a detection wavelength=210 nm, a mobile phase of methanol and 50mM aqueous ammonium acetate (V: V=65:35), a flow rate of 1mL/min, a sample volume of 20. Mu.L, a column temperature of 40 ℃, a detection time of 10min, a peak time of 8.1 min. The PFOA removal rate is calculated as follows: r= (1-C t /C 0 ) X 100%, where C t 、C 0 The PFOA concentration and the PFOA initial concentration at the time t are respectively expressed in mg/L, and the removal result is shown in FIG. 3.
As can be seen from FIG. 3, after 210min of reaction, compared with the iron-carbon ceramic and the aluminum-carbon ceramic, the Al/Fe/C micro-electrolysis ceramic has better degradation effect, and the removal rate of PFOA can reach 88.86%.
Meanwhile, fluoride ions in the reaction process are measured by an ion chromatograph, and the result is shown in fig. 4.
After 11h reaction, about 0.7mg/L of fluoride ions is detected in the final solution, and 2.1% (about 1 mg/L) of PFOA is defluorinated by material accounting, which shows that the prepared Al/Fe/C micro-electrolysis ceramsite can realize the degradation of PFOA. Meanwhile, in the existing research materials, the defluorination rate of the perfluoro compound of 500ug/L can only reach 2-3% (about 10-15 ug/L), compared with the Al/Fe/C micro-electrolysis ceramsite prepared by the application, the defluorination rate is obviously improved.
Effect example 2
The removal rate of PFOA was measured for the ceramsite prepared in examples 1 to 6 and comparative examples 1 to 6, and the results are shown in Table 1.
TABLE 1
Effect example 2
A microphone instrument is used for marking a degassing station, a 4-station full-automatic specific surface area analyzer of the model Micromeritics APSP 2460 is used for preprocessing a sample, and a nitrogen adsorption and desorption test is carried out on the sample under the condition of 77k liquid nitrogen to measure the specific surface area of the ceramsite; the ceramsite strength is measured by a YHKC-2A type particle strength measuring instrument; performing mercury-pressing test on the ceramsite by using a high-performance full-automatic mercury-pressing instrument of model Micromeritics AutoPore IV 9500, and measuring the porosity of the ceramsite; the results are shown in Table 2.
TABLE 2
Specific surface area (m) 2 /g) | strength/MPa | Porosity (%) | |
Fe/C ceramsite | 92.23 | 25.8 | 25.20 |
Al/C ceramsite | 105.74 | 14.9 | 32.95 |
Al/Fe/C ceramsite | 96.36 | 14.1 | 41.80 |
Effect example 3
The Al/Fe/C micro-electrolysis ceramsite prepared in the embodiment 4 of the application is applied to degradation of methylene blue dye wastewater. Ceramsite is added into the simulated printing and dyeing wastewater with the initial concentration of 50mg/L according to the solid-to-liquid ratio of 10g/L, and the mixed reaction is carried out at 25 ℃ with the revolution of 150rpm. Samples were taken at the set time points, absorbance of the samples was measured at 644nm wavelength by an ultraviolet-visible spectrophotometer to obtain a sample concentration, and after 390min of reaction, the removal rate reached 87.21%, and specific results are shown in fig. 5 and 6 (3 tubes on the left side in fig. 6 are untreated samples (3 groups in parallel), and 3 tubes on the right side are samples after 380min of treatment (3 groups in parallel)).
The above embodiments are only illustrative of the preferred embodiments of the present application and are not intended to limit the scope of the present application, and various modifications and improvements made by those skilled in the art to the technical solutions of the present application should fall within the protection scope defined by the claims of the present application without departing from the design spirit of the present application.
Claims (10)
1. The Al/Fe/C micro-electrolysis ceramsite is characterized by comprising the following raw materials in percentage by mass: 20 to 60 percent of fly ash, 10 to 20 percent of aluminum powder, 10 to 20 percent of iron powder, 10 to 20 percent of carbon powder, 5 to 10 percent of binder and 5 to 10 percent of pore-forming agent.
2. The Al/Fe/C micro-electrolysis ceramic according to claim 1, wherein the carbon powder comprises any one of coke and wood-based activated carbon.
3. The Al/Fe/C micro-electrolysis ceramic according to claim 1, wherein the binder comprises any one of polymethacrylic acid, attapulgite powder and bentonite.
4. The Al/Fe/C micro-electrolysis ceramic according to claim 1, wherein the pore-forming agent comprises any one of ammonium chloride, sweet potato starch and ammonium bicarbonate.
5. The Al/Fe/C micro-electrolysis ceramic particle according to claim 1, wherein the mass ratio of the aluminum powder to the iron powder to the carbon powder is 1:1 (0.5-2).
6. A method for preparing the Al/Fe/C micro-electrolysis ceramic particles according to any one of claims 1 to 5, which is characterized by comprising the following steps:
mixing the raw materials with water according to the mass percentage, uniformly stirring, kneading and forming, and then drying in an inert atmosphere and calcining at a high temperature to obtain the Al/Fe/C micro-electrolysis ceramsite.
7. The method according to claim 6, wherein the high-temperature calcination is carried out at 800 to 900 ℃ for 0.5 to 2 hours.
8. The method according to claim 6, wherein the kneading molding specifically comprises: kneading to obtain spherical particle size of 10-15 mm.
9. Use of the Al/Fe/C micro-electrolysis ceramsite according to any one of claims 1 to 5 in wastewater treatment.
10. The use according to claim 9, wherein the contaminants in the wastewater comprise perfluorinated compounds.
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