CN110465322A - A kind of steel slag/nitrogen-dopped activated carbon composite material and preparation method and application - Google Patents
A kind of steel slag/nitrogen-dopped activated carbon composite material and preparation method and application Download PDFInfo
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- CN110465322A CN110465322A CN201910816353.1A CN201910816353A CN110465322A CN 110465322 A CN110465322 A CN 110465322A CN 201910816353 A CN201910816353 A CN 201910816353A CN 110465322 A CN110465322 A CN 110465322A
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- nitrogen
- activated carbon
- composite material
- dopped activated
- steel slag
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 182
- 239000002893 slag Substances 0.000 title claims abstract description 88
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 74
- 239000010959 steel Substances 0.000 title claims abstract description 74
- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 13
- -1 nitrogenous compound Chemical class 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 239000003610 charcoal Substances 0.000 claims description 26
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 21
- 239000002250 absorbent Substances 0.000 claims description 20
- 230000002745 absorbent Effects 0.000 claims description 20
- 239000000395 magnesium oxide Substances 0.000 claims description 20
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 19
- 239000002351 wastewater Substances 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 13
- 230000000694 effects Effects 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 6
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 4
- 244000060011 Cocos nucifera Species 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 150000003233 pyrroles Chemical class 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 238000006477 desulfuration reaction Methods 0.000 abstract 1
- 230000023556 desulfurization Effects 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 21
- 238000006731 degradation reaction Methods 0.000 description 21
- 239000000243 solution Substances 0.000 description 12
- 229960002135 sulfadimidine Drugs 0.000 description 9
- ASWVTGNCAZCNNR-UHFFFAOYSA-N sulfamethazine Chemical compound CC1=CC(C)=NC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 ASWVTGNCAZCNNR-UHFFFAOYSA-N 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 6
- 229940012189 methyl orange Drugs 0.000 description 6
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 description 5
- 238000010525 oxidative degradation reaction Methods 0.000 description 5
- 239000010865 sewage Substances 0.000 description 5
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 description 4
- 229940124530 sulfonamide Drugs 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000011572 manganese Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- VTSWSQGDJQFXHB-UHFFFAOYSA-N 2,4,6-trichloro-5-methylpyrimidine Chemical compound CC1=C(Cl)N=C(Cl)N=C1Cl VTSWSQGDJQFXHB-UHFFFAOYSA-N 0.000 description 1
- LSBIUXKNVUBKRI-UHFFFAOYSA-N 4,6-dimethylpyrimidine Chemical compound CC1=CC(C)=NC=N1 LSBIUXKNVUBKRI-UHFFFAOYSA-N 0.000 description 1
- 229910001341 Crude steel Inorganic materials 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy 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
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N glycolonitrile Natural products N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J35/61—Surface area
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/12—Oxidising
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- C—CHEMISTRY; METALLURGY
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
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- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Thermal Sciences (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
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- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of steel slag/nitrogen-dopped activated carbon composite material and preparation method and applications.The preparation method of composite material is first to carry out pre-oxidation treatment to active carbon;Then the active carbon after pre-oxidation is put into nitrogenous compound solution and is ultrasonically treated, then filtered, dry nitrogen-dopped activated carbon presoma;Nitrogen-dopped activated carbon presoma is calcined under nitrogen atmosphere again obtains nitrogen-dopped activated carbon;Finally steel slag, metal promoter and nitrogen-dopped activated carbon three are mixed, and calcine to obtain steel slag/nitrogen-dopped activated carbon composite material in a nitrogen atmosphere.Composite material produced by the present invention had not only remained with active carbon pore structure abundant, but also introduced nitrogen-containing functional group and contain various active metal in steel slag, was a kind of efficient catalytic material of catalytic oxidative desulfurization Organic Pollutants In Water.
Description
Technical field
The present invention relates to a kind for the treatment of of Organic Wastewater materials, and in particular to a kind of steel slag/nitrogen-dopped activated carbon composite material
And its preparation method and application.
Background technique
Steel slag is the discarded object of power boiler discharge that steel industry unavoidably generates in ironmaking and steelmaking process, and yield is about
Account for the 8%~15% of crude steel yield.It is estimated that China is about 0.81~1.2 hundred million tons in the quantum of output of steel slag in 2016, national steel
Nearly 1,000,000,000 tons of the accumulative stockpiling of slag.But the comprehensive utilization ratio of China's steel slag is less than 40%, with 95% or more Systems in Certain Developed Countries
Slag comprehensive utilization rate greatly differs from each other.A lot of steel slag pile up placement not only seriously occupies limited land resource, can also to atmosphere,
Soil, surface water and groundwater pollute;For steel slag as a kind of secondary resource, main component includes CaO, SiO simultaneously2、
Al2O3、Fe2O3, MgO and a small amount of MnO, FeO, P2O5Deng if the serious wave of resource utilization and resource cannot be carried out effectively
Take.Therefore, the comprehensive utilization ratio for how effectively improving steel slag reduces the environmental pollution of steel slag and realizes that " zero-emission " of steel slag is
The challenge of China's steel industry, environmental protection industry (epi) and other relevant industries institute facings.
In addition, along with every profession and trades such as chemical industry, pesticide, medicine, printing and dyeing fast development and cities and towns integration into
The continuous propulsion of journey, a large amount of organic wastewater also generate therewith, there is very important toxicity to imitate water environment and human health
It answers.And in numerous method for processing organic wastewater, traditional Fenton (Fenton) oxidation technology is a kind of advanced oxidation skill of maturation
Art, in acid condition Fe2+Activate H2O2The hydroxyl radical free radical with high oxidation activity and low selectivity is generated, in mild technique
Under the conditions of (normal pressure ,~50 DEG C) can effectively degrade most organic pollutants in water body, have been widely used for engineering practice has
Machine sewage treatment.But there are pH (~3) action panes that narrow, catalyst is difficult to recycle and cause to generate for traditional Fenton technique
In place of the deficiencies of a large amount of sludge.Therefore, more and more researchs are dedicated to that multiphase-fenton Fenton (class for active metal component is made
Fenton) catalyst is used for activity H2O2Hydroxyl radical free radical is generated, is generated with solving the recycling of the catalyst in whole process and sludge
Problem.
Summary of the invention
The present invention tradition Fenton technical treatment organic wastewater there are aiming at the problem that and Comprehensive Utilization of Steel Slag utilize it is tight
Compel property, provides a kind of steel slag/nitrogen-dopped activated carbon composite material and preparation method, and aoxidize drop for the change of organic wastewater
Solution, can effectively realize and recycle to steel slag.The preparation method of composite material in the present invention the following steps are included:
S1: pre-oxidation treatment is carried out to active carbon, obtains magnesium oxide/absorbent charcoal;
S2: by magnesium oxide/absorbent charcoal immerse nitrogenous compound solution in and with the frequency ultrasound of 20~30KHz dispersion reaction 6~
The mass ratio of 12h, magnesium oxide/absorbent charcoal and nitrogenous compound is 5~20:1;It then filters, dry nitrogen-dopped activated carbon forerunner
Body;
S3: in nitrogen atmosphere with 450~950 DEG C of temperature calcination nitrogen-dopped activated carbon 1~3h of presoma, it is living to obtain N doping
Property charcoal;
S4: steel slag is mixed with nitrogen-dopped activated carbon according to the mass ratio of 0.1~1:1, adds and accounts for steel slag and N doping
The metal promoter of active carbon gross mass 1~10%, under nitrogen atmosphere with 450~850 DEG C of temperature calcination 1~3h of mixture,
Obtain steel slag/nitrogen-dopped activated carbon composite material.
Based on the above technical solution, the present invention can also be improved as follows.
Further, in S1 active carbon method for pre-oxidizing are as follows: by active carbon immerse concentration be 1mol/L nitric acid solution in,
Constant temperature stirs 3~6h at 60 DEG C, then filters, washs, is dried to obtain magnesium oxide/absorbent charcoal.
Further, nitrogenous compound is melamine, aniline, cyanamid dimerization, acrylonitrile, urea or pyrroles.
Further, active carbon is active carbon from coal, the wooden matrix activated carbon or coconut shell based activated carbon, and active carbon is in granular form or powder
Last shape.
Further, steel slag is blast furnace slag, converter slag, refining steel slag or electric furnace slag.
Further, the quality of metal promoter accounts for the 5% of converter slag containing vanadium and titanium oxides and nitrogen-dopped activated carbon gross mass in S4.
Further, the nitrate or chlorate of metal promoter Co, Cu, Mn, V, Fe, Ti, Ni.
The beneficial effects of the present invention are:
1. active carbon is as a kind of common cheap material, with large specific surface area, pore structure is flourishing, is easy to the table of regulation
Surface properties, resistance to acid and alkali, resistance to hydro-thermal and the excellent properties such as environmental-friendly, to active carbon carry out after nitrogen-doped modified processing with steel slag
It is kneaded, high-temperature process, obtains steel slag/nitrogen-dopped activated carbon composite material.One side nitrogen-dopped activated carbon developed pore structure
The dispersion degree of active metal in steel slag can be improved, nitrogen-containing functional group and Fe, Mn in steel slag etc. are golden on another aspect active carbon
Belong to element and form metal-Nx (M-Nx) active structure, the interaction between active metal and active carbon can be improved, to improve
The catalytic activity and stability of composite material catalytic degradation organic wastewater.
2. nitrogen-dopped activated carbon and steel slag are to carry out compound, active carbon under hot conditions under the high temperature conditions in the present invention
Play the role of reducing agent, by the Fe in steel slag3+It is reduced into Fe2+And Fe, improve Fe in composite material2+With the content of Fe, and
Fe2+It is the chief active factor in type Fenton catalyst with Fe, to improve the work of composite material catalytic degradation organic pollutant
Property.In addition, active carbon can also form Galvanic interaction between Fe, V, Mn isoreactivity metal in converter slag containing vanadium and titanium oxides, it can be into one
Step promotes Organic Pollutants In Water degradation.
3. the method in the present invention is easy, quick, easy to operate, it is suitable for industrialized production, steel slag/N doping activity of preparation
Carbon composite is a kind of effective catalyst, can effectively remove the organic pollutant in water.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is that the present invention prepares steel slag/nitrogen-dopped activated carbon composite material Technology Roadmap;
Fig. 2 is oxidative degradation curve of the one gained composite material of embodiment to methyl orange;
Fig. 3 is oxidative degradation curve of the two gained composite material of embodiment to quadracycline;
Fig. 4 is oxidative degradation curve of the three gained composite material of embodiment to sulfamethazine;
Fig. 5 is oxidative degradation curve of the composite material obtained by example IV to sulfamethazine.
Specific embodiment
Below with reference to embodiment, specific embodiments of the present invention will be described in detail.Steel slag/N doping in the present invention
The preparation route of absorbent charcoal composite material is as shown in Figure 1.
Embodiment one
A kind of steel slag/nitrogen-dopped activated carbon composite material, the composite material in the present embodiment are made by following steps:
S1: the active carbon from coal of commercial powder shape is immersed in the nitric acid solution that concentration is 1mol/L, the constant temperature at 60 DEG C
Stir 3h;Then it filters, and with deionized water by residue washing to neutrality, then filter residue is put into baking oven and is dried with 50 DEG C of temperature
It is dry, obtain magnesium oxide/absorbent charcoal.
S2: the mass ratio according to magnesium oxide/absorbent charcoal and nitrogenous compound is respectively 1:0,5:1,10:1,15:1 and 20:1, is incited somebody to action
Magnesium oxide/absorbent charcoal immerses in corresponding melamine solution and disperses 6h with the frequency ultrasound of 30KHz, then filters, and filter residue is set
It is dried in baking oven with 60 DEG C of temperature, obtains 5 kinds of nitrogen-dopped activated carbon presomas.
S3: 5 kinds of nitrogen-dopped activated carbon presomas are put into the lower 650 DEG C of calcinings 1h of nitrogen atmosphere, obtain 5 kinds of N doping activity
Charcoal.
S4: vanadium titanium blast furnace slag is mixed with above-mentioned 5 kinds of nitrogen-dopped activated carbons according to the mass ratio of 0.5:1 respectively, then plus
Enter to account for 2% iron chloride of converter slag containing vanadium and titanium oxides and nitrogen-dopped activated carbon gross mass, is put into crucible after mixing, then crucible is placed in pipe
In formula furnace, in a nitrogen atmosphere with 650 DEG C of temperature calcination 1h, 5 kinds of steel slags/nitrogen-dopped activated carbon composite material is obtained.
To verify 5 kinds of steel slags/nitrogen-dopped activated carbon composite material obtained by the present embodiment to the processing capacity of organic wastewater, into
The fenton-type reagent degradation experiment of Methyl Orange in Wastewater is gone.At 50 DEG C, H2O2(30%) dosage is 2mL, and catalyst amount is
Under the conditions of 0.8g/L, the degradation effect such as Fig. 2 of different steel slags/nitrogen-dopped activated carbon composite material to 200mg/L Methyl Orange in Wastewater
It is shown.As seen from the figure, after reacting 60min, independent H2O2Oxidation is only 5% or so to the degradation efficiency of methyl orange;With steel
The addition of slag/nitrogen-dopped activated carbon composite material significantly improves catalysis H2O2The efficiency of oxidative degradation methyl orange, and with multiple
The increase of nitrogen content in condensation material, the catalytic activity of composite material increase with it.After reacting 60min, best complex material pair
The removal rate of methyl orange reaches 70% or so, illustrates that nitrogen-doped modified processing active carbon can effectively improve the catalysis of composite material
Activity also indicates that steel slag obtained by the present invention/nitrogen-dopped activated carbon composite material is a kind of good organic sewage processing material
Material.
Embodiment two
A kind of steel slag/nitrogen-dopped activated carbon composite material, the composite material in the present embodiment are made by following steps:
S1: commercial powder wood matrix activated carbon is immersed in the nitric acid solution that concentration is 1mol/L, constant temperature stirs at 60 DEG C
3h;Then it filters, and with deionized water by residue washing to neutrality, then filter residue is put into baking oven and is dried with 50 DEG C of temperature,
Obtain magnesium oxide/absorbent charcoal.
S2: it is 10:1 according to the mass ratio of magnesium oxide/absorbent charcoal and nitrogenous compound, magnesium oxide/absorbent charcoal is immersed corresponding two
Disperse 6h in paracyanogen amine aqueous solution and with the frequency ultrasound of 30kHz, then filters, and filter residue is placed in the temperature in baking oven with 60 DEG C
Drying, obtains nitrogen-dopped activated carbon presoma.
S3: nitrogen-dopped activated carbon presoma being respectively put under nitrogen atmosphere and calcines 1h at 450 DEG C, 650 DEG C, 850 DEG C,
Obtain 3 kinds of nitrogen-dopped activated carbons.
S4: vanadium titanium rotary furnace steel slag is mixed with above-mentioned 3 kinds of nitrogen-dopped activated carbons according to the mass ratio of 0.5:1 respectively, then plus
Enter to account for 3% copper chloride of converter slag containing vanadium and titanium oxides and nitrogen-dopped activated carbon gross mass, is put into crucible after mixing, then crucible is placed in pipe
In formula furnace, in a nitrogen atmosphere with 650 DEG C of temperature calcination 1h, 3 kinds of steel slags/nitrogen-dopped activated carbon composite material is obtained.
In order to verify 3 kinds of steel slags/nitrogen-dopped activated carbon composite material obtained by the present embodiment to the processing capacity of organic wastewater,
The fenton-type reagent degradation experiment of quadracycline is carried out.At 50 DEG C, H2O2(30%) dosage is 2mL, and catalyst amount is
Under the conditions of 0.8g/L, different steel slags/nitrogen-dopped activated carbon composite material to the degradation effect of 20mg/L quadracycline waste water such as
Shown in Fig. 3.As seen from the figure, after reacting 60min, independent H2O2Oxidation is only 10% or so to the degradation efficiency of quadracycline;
With the raising of nitrogen-dopped activated carbon presoma pyrolysis temperature, prepared steel slag/nitrogen-dopped activated carbon composite material is to hydrochloric acid
The degradation efficiency of tetracycline also increases with it.After reacting 60min, best steel slag/nitrogen-dopped activated carbon composite material relative to
Independent H2O2For oxidation, 65% or so is improved to the degradation efficiency of quadracycline.Show steel slag obtained by the present invention/
Nitrogen-dopped activated carbon composite material is a kind of good sewage treating material.
Embodiment three
A kind of steel slag/nitrogen-dopped activated carbon composite material, the composite material in the present embodiment are made by following steps:
S1: commercial powder coconut shell based activated carbon is immersed in the nitric acid solution that concentration is 1mol/L, constant temperature stirs at 60 DEG C
Mix 3h;Then it filters, and with deionized water by residue washing to neutrality, then filter residue is put into baking oven and is dried with 50 DEG C of temperature
It is dry, obtain magnesium oxide/absorbent charcoal.
S2: it is 5:1 according to the mass ratio of magnesium oxide/absorbent charcoal and nitrogenous compound, magnesium oxide/absorbent charcoal is immersed into corresponding urea
Disperse 6h in solution and with the frequency ultrasound of 30kHz, then filter, and filter residue is placed in baking oven and is dried with 60 DEG C of temperature,
Obtain nitrogen-dopped activated carbon presoma.
S3: nitrogen-dopped activated carbon presoma is put into the lower 850 DEG C of calcinings 2h of nitrogen atmosphere, obtains nitrogen-dopped activated carbon.
S4: refining steel slag and nitrogen-dopped activated carbon for vanadium titanium and mix respectively according to the mass ratio of 0.5:1,0.8:1 and 1:1,
It adds and accounts for 2% cobalt chloride of converter slag containing vanadium and titanium oxides and nitrogen-dopped activated carbon gross mass, be put into crucible after mixing, then crucible is set
In tube furnace, in a nitrogen atmosphere with 650 DEG C of temperature calcination 1h, 3 kinds of steel slags/nitrogen-dopped activated carbon composite material is obtained.
In order to verify 3 kinds of steel slags/nitrogen-dopped activated carbon composite material obtained by the present embodiment to the processing capacity of organic wastewater,
The fenton-type reagent degradation experiment of sulfamethazine waste water is carried out.At 50 DEG C, H2O2(30%) dosage is 2mL, catalysis
Under the conditions of agent dosage is 0.8g/L, different steel slags/nitrogen-dopped activated carbon composite material is to 20mg/L sulfamethazine waste water
Degradation effect it is as shown in Figure 4.As seen from the figure, after reacting 60min, independent H2O2Aoxidize the degradation to sulfamethazine
Efficiency is only 20% or so;With the addition of vanadium titanium refining steel slag, prepared steel slag/nitrogen-dopped activated carbon composite material is to sulphur
The degradation efficiency of amine dimethyl pyrimidine also increases.This is because with the increase of vanadium titanium refining steel slag additional amount, composite wood
The quantity of active metal increases with it in material, is consequently increased so as to cause the quantity of active site.After reacting 60min, most
Good steel slag/nitrogen-dopped activated carbon composite material is relative to independent H2O2For oxidation, the degradation efficiency of sulfamethazine is mentioned
It is high by 50% or so, show that steel slag obtained by the present invention/nitrogen-dopped activated carbon composite material is a kind of good sewage treatment
Material.
Example IV
A kind of steel slag/nitrogen-dopped activated carbon composite material, the composite material in the present embodiment are made by following steps:
S1: commercial column coconut shell based activated carbon is immersed in the nitric acid solution that concentration is 1mol/L, constant temperature stirs at 60 DEG C
Mix 3h;Then it filters, and with deionized water by residue washing to neutrality, then filter residue is put into baking oven and is dried with 50 DEG C of temperature
It is dry, obtain magnesium oxide/absorbent charcoal.
S2: it is 5:1 according to the mass ratio of magnesium oxide/absorbent charcoal and nitrogenous compound, magnesium oxide/absorbent charcoal is immersed into corresponding aniline
Disperse 6h in solution and with the frequency ultrasound of 30kHz, then filter, and filter residue is placed in baking oven and is dried with 60 DEG C of temperature,
Obtain nitrogen-dopped activated carbon presoma.
S3: nitrogen-dopped activated carbon presoma is put into the lower 850 DEG C of calcinings 3h of nitrogen atmosphere, obtains nitrogen-dopped activated carbon.
S4: electric furnace slag and nitrogen-dopped activated carbon are mixed according to the mass ratio of 0.8:1, adds and accounts for electric furnace slag and nitrogen
4% manganese nitrate of dopped activated carbon gross mass, is put into crucible, then crucible is placed in tube furnace after mixing, in nitrogen gas
With 450 DEG C, 650 DEG C, 850 DEG C of temperature calcination 2h under atmosphere, 3 kinds of steel slags/nitrogen-dopped activated carbon composite material is obtained.
In order to verify 3 kinds of steel slags/nitrogen-dopped activated carbon composite material obtained by the present embodiment to the processing capacity of organic wastewater,
The fenton-type reagent degradation experiment of sulfamethazine waste water is carried out.At 50 DEG C, H2O2(30%) dosage is 2mL, catalysis
Under the conditions of agent dosage is 0.8g/L, different steel slags/nitrogen-dopped activated carbon composite material is to 20mg/L sulfamethazine waste water
Degradation effect it is as shown in Figure 5.As seen from the figure, after reacting 60min, independent H2O2Aoxidize the degradation to sulfamethazine
Efficiency is only 20% or so;With the raising of calcination temperature, prepared steel slag/nitrogen-dopped activated carbon composite material is to sulfanilamide (SN) two
The degradation efficiency of methylpyrimidine also increases accordingly.This is because one side active carbon is to active gold with the raising of calcination temperature
The reduction of category enhances, and will form alloy structure between another aspect active metal, plays the role of improving catalytic activity.In
After reacting 60min, best steel slag/nitrogen-dopped activated carbon composite material is relative to independent H2O2It is phonetic to sulfanilamide (SN) dimethyl for oxidation
The degradation efficiency of pyridine improves 55% or so, shows that steel slag obtained by the present invention/nitrogen-dopped activated carbon composite material is a kind of
Good sewage treating material.
Although be described in detail to a specific embodiment of the invention in conjunction with the embodiments, should not be construed as to this
The restriction of the protection scope of patent.In range described by claims, those skilled in the art are without creative work
The various modifications and deformation that can make still belong to the protection scope of this patent.
Claims (9)
1. a kind of steel slag/nitrogen-dopped activated carbon composite material preparation method, which comprises the following steps:
S1: pre-oxidation treatment is carried out to active carbon, obtains magnesium oxide/absorbent charcoal;
S2: by magnesium oxide/absorbent charcoal immerse nitrogenous compound solution in and ultrasonic disperse react 6~12h, magnesium oxide/absorbent charcoal with it is nitrogenous
The mass ratio of compound is 5~20:1;It then filters, dry nitrogen-dopped activated carbon presoma;
S3: in nitrogen atmosphere with 450~950 DEG C of temperature calcination nitrogen-dopped activated carbon 1~3h of presoma, N doping activity is obtained
Charcoal;
S4: steel slag is mixed with nitrogen-dopped activated carbon according to the mass ratio of 0.1~1:1, is added and is accounted for steel slag and N doping activity
The metal promoter of charcoal gross mass 1~10% obtains steel under nitrogen atmosphere with 450~850 DEG C of temperature calcination 1~3h of mixture
Slag/nitrogen-dopped activated carbon composite material.
2. preparation method according to claim 1, which is characterized in that the method for pre-oxidizing of active carbon in S1 are as follows: will be active
Charcoal immerses in the nitric acid solution that concentration is 1mol/L, and constant temperature stirs 3~6h at 60 DEG C, then filters, washs, is dried to obtain oxygen
Change active carbon.
3. preparation method according to claim 1, it is characterised in that: the nitrogenous compound is melamine, aniline, two
Poly cyanamid, acrylonitrile, urea or pyrroles.
4. preparation method according to claim 1, it is characterised in that: the active carbon is active carbon from coal, the wooden base activity
Charcoal or coconut shell based activated carbon, the active carbon are in granular form or powdered.
5. preparation method according to claim 1, it is characterised in that: the steel slag is blast furnace slag, converter slag, refining
Steel slag or electric furnace slag.
6. preparation method according to claim 1, it is characterised in that: the quality of metal promoter accounts for converter slag containing vanadium and titanium oxides and nitrogen in S4
The 5% of dopped activated carbon gross mass.
7. preparation method according to claim 1 or 6, it is characterised in that: the metal promoter be Co, Cu, Mn, V, Fe,
The nitrate or chlorate of Ti, Ni.
8. using prepared by the described in any item steel slags of claim 1~7/nitrogen-dopped activated carbon composite material preparation method
Steel slag/nitrogen-dopped activated carbon composite material.
9. steel slag as claimed in claim 8/application of the nitrogen-dopped activated carbon composite material in treatment of Organic Wastewater.
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