CN106111156B - Efficient class Fenton magnetic catalyst and preparation method based on clay mineral and application - Google Patents
Efficient class Fenton magnetic catalyst and preparation method based on clay mineral and application Download PDFInfo
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- CN106111156B CN106111156B CN201610470204.0A CN201610470204A CN106111156B CN 106111156 B CN106111156 B CN 106111156B CN 201610470204 A CN201610470204 A CN 201610470204A CN 106111156 B CN106111156 B CN 106111156B
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- clay mineral
- class fenton
- efficient class
- magnetic
- magnetic catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 49
- 239000002734 clay mineral Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 16
- 230000003197 catalytic effect Effects 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 150000002505 iron Chemical class 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 238000010792 warming Methods 0.000 claims abstract description 11
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 6
- 231100000331 toxic Toxicity 0.000 claims abstract description 6
- 230000002588 toxic effect Effects 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 32
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052742 iron Inorganic materials 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 9
- 229910044991 metal oxide Inorganic materials 0.000 claims description 9
- 150000004706 metal oxides Chemical class 0.000 claims description 9
- 239000002689 soil Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 239000010941 cobalt Substances 0.000 claims description 7
- 229910017052 cobalt Inorganic materials 0.000 claims description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000440 bentonite Substances 0.000 claims description 4
- 229910000278 bentonite Inorganic materials 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052900 illite Inorganic materials 0.000 claims description 3
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims 1
- 150000003657 tungsten Chemical class 0.000 claims 1
- 229910001930 tungsten oxide Inorganic materials 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 17
- 230000008569 process Effects 0.000 abstract description 9
- 230000007935 neutral effect Effects 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 14
- 239000000463 material Substances 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229940056319 ferrosoferric oxide Drugs 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000002688 persistence Effects 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- -1 hydroxyl radical free radical Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 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
- 239000008204 material by function Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009284 supercritical water oxidation Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- 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
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The efficient class Fenton magnetic catalyst and preparation method and application that the present invention relates to a kind of based on clay mineral.Preparation process is：(1) clean clay mineral is added in the iron salt solutions prepared in advance, so that mixed suspension is warming up to 60 100 DEG C and is continued stirring and reaches stable in 0.5 5 hours；(2) processes such as lye is added in suspension makes solution ph rise to 8 11, persistently stirs 0.5 6 hours, and solid precipitation is washed, dry obtain Precursor Powder；(3) Precursor Powder is impregnated in the solution containing other nonferrous metal salt, is uniformly evaporated, and heat treatment is to get to the efficient class Fenton magnetic catalyst based on clay mineral.Compared with prior art, catalyst of the invention has Magneto separate, can recycle and recycle, while having efficient class Fenton catalytic activity and stability under near neutral pH.The preparation process of the catalyst is simple, and cost is relatively low and ecological compatibility is good, has broad prospect of application in toxic organic pollutant process field difficult to degrade.
Description
Technical field
The invention belongs to inorganic nanometer functional materials and environmental pollution control technique field, more particularly, to one kind based on viscous
The efficient class Fenton magnetic catalyst and preparation method of native mineral and application.
Background technology
The situation is tense for the pollution of the current surface water in China, underground water and soil, wherein with pesticide, antibiotic compound,
The persistence organic pollutant difficult to degrade such as polycyclic aromatic hydrocarbon, azo dyes is the polluter of representative, in the ring that we depend on for existence
Exist for a long time in border, it will there are irreversible potential threats to ecological environment and people's health.Develop effective organic contamination
Soil or water recovery technique become the vital task of field of environment pollution control.
High-level oxidation technology, including photocatalysis, plasma, supercritical water oxidation, ozone oxidation, Fenton and class Fenton oxygen
The methods of change, it is occupied an important position in terms of persistence toxic organic pollutant in removing environment.Wherein, heterogeneous class Fenton
Chemical oxidization method generates the hydroxyl of Strong oxdiative certainly by using heterogeneous catalysis material catalytic activation hydrogen peroxide or persulfate etc.
It is a kind of more practical persistency organic contaminant to thoroughly decompose and eliminate the toxic organic pollutant in environment by base
Control technology.For example, the Chinese patent of Publication No. CN103230796A discloses a kind of attapulgite load ferroso-ferric oxide
Preparation method, this Magneto separate material can be used for class Fenton's reaction degradable organic pollutant, and be urged by Magneto separate recycling
Change material.However the catalytic activity of the catalyst based on ferroso-ferric oxide is weaker.In addition also have and aoxidized using other metals
Report of the object as carrier loaded ferriferous oxide, such as the Chinese patent of Publication No. CN105536812A disclose a kind of nanometer
Fe3O4/Mn3O4Composite material, and have the characteristics that Magneto separate and class Fenton catalytic degradation organic pollution.However these are with iron
Catalyst based on oxide, effective range is relatively narrow, usually can play obvious catalysis in ranges of the pH less than 4
Degradation effect, once and pH value of solution can hardly generate any catalytic action more than 4.Because being asked in view of the corrosion-resistant of reactor
The problems such as increasing technical costs caused by iron dissolution problem and addition soda acid under topic, acid condition, exploitation can be in relatively
Under the conditions of property pH and the efficient heterogeneous class Fenton oxidation technology that can be recycled is current facing challenges, and advanced catalysis material
The development of material is the key that break-through skill bottleneck.
The Chinese patent of Publication No. CN105405567A discloses a kind of magnetic of layered clay mineral supported ferriferous oxide
Property reparation of the material for the soil or water of organic pollution, the composition of magnetic iron oxide can be controlled in this method by roasting
With structure and keep the good magnetic characteristic of material, and this method proposes to add mixing for non-ferric while preparing ferriferous oxide
Miscellaneous metallic element so that magnetic material also has apparent catalytic effect when pH value is close to 4.However this method can draw
The doping metals entered are very low, only the 0.1-5% of iron, because the content of higher-doped metal will lead to doping metals and iron oxygen
The interaction of compound forms nonmagnetic metal composite oxide, leads to the disappearance of final catalysis material magnetism.Therefore how
It improves nonferrous metal content, enhancing near neutral pH catalytic activity while the magnetism of catalysis material being kept to be very important skill
Art problem.
Invention content
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind being based on clay mineral
Efficient class Fenton magnetic catalyst and preparation method and application.
The present invention is based on the thoughts of " take from soil, be used for soil ", using the good layered clay mineral of environment compatibility
For basic material, the ferriferous oxide with superparamagnetism energy is introduced on it, is recycled and is recycled to reach quick Magneto separate
Purpose；Meanwhile the present invention is by the way that after forming stable ferriferous oxide, before heat treatment, higher contain is introduced by infusion process
Amount preferred nonferrous metal salt, be allowed to substrate clay mineral and ferriferous oxide surface deposition and during heat treatment
It is decomposed to form metal oxide, maintains the crystal phase structure of magnetic iron oxide, it is final to obtain that catalytic activity is high, have
Magneto separate recycles feature and has the catalyst of efficient catalytic performance in wide ph range.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of efficient class Fenton magnetic catalyst based on clay mineral, including clay mineral, magnetic iron oxide and
The mass ratio of other metal oxides, wherein magnetic iron oxide and clay mineral is 0.05-2, other metal oxides and magnetic
Property ferriferous oxide molar ratio be 0.1-1, other metal oxides be manganese metal, cobalt, aluminium, copper, zirconium or tungsten in one
Kind or two oxides.
The clay mineral has layer structure, selected from one or both of bentonite, illite or montmorillonite
Combination.
The preparation method of the efficient class Fenton magnetic catalyst based on clay mineral, includes the following steps：
(1) clean clay mineral is added in the iron salt solutions prepared in advance, mixed suspension is made to be warming up to
60-100 DEG C and continues stirring and reach stable in 0.5-5 hours；
(2) lye is added in suspension makes solution ph rise to 8-11, persistently stirs 0.5-6 hours, solid precipitation
The processes such as washed, dry obtain Precursor Powder；
(3) Precursor Powder is impregnated in the solution containing other metal salts, is uniformly evaporated, and is heat-treated to get to based on clay
The efficient class Fenton magnetic catalyst of mineral.
The molysite is any soluble divalent iron salt or the mixture of divalent and trivalent iron salt, wherein preferred ferrous iron
It is 0.3-3 with ferric iron molar ratio, total concentration of iron is 0.1-5 mol/Ls.
Other metal salts are the water solubility or alcohol of one or both of metallic element manganese, cobalt, aluminium, copper, zirconium or tungsten
Soluble, wherein preferably nitrate, sulfate, hydrochloride or the complex compound containing ammonium root, the molar concentration of other metal salts are
The molar ratio of 0.05-2 mol/Ls, other metallic elements and iron is 0.1-1.
It is described to be evaporated as the heating evaporation operation no more than 100 DEG C.
The heating rate of the heat treatment is 1-20 DEG C/min, and the temperature of heat treatment is 200-600 DEG C, the time of heat treatment
It it is 1-48 hours, the atmosphere of heat treatment is air.
The efficient class Fenton magnetic catalyst based on clay mineral can be used for efficient catalytic and decompose hydrogen peroxide
Toxic persistent organic pollutants in water or soil are decomposed removal, while can be recycled by Magneto separate by class Fenton's reaction
It utilizes.
Compared with prior art, the present invention has the following advantages and beneficial effects：
(1) contain magnetic iron oxide in catalyst of the invention, therefore, catalyst has Magneto separate, can return
It receives and recycles.
(2) in catalyst of the invention, also contain the manganese metal of other non-ferric, the oxide of cobalt, aluminium, copper, zirconium or tungsten, this
The metal oxide of a little non-ferric can have under the conditions of near neutral pH and efficiently urge under ferriferous oxide compound action
Change and decompose hydrogen peroxide generation high activity hydroxyl radical free radical, the effect of class Fenton's reaction is played, this is because these metal oxides
With ferriferous oxide it is compound after cause surface isoelectric point decline, that is, near neutral pH lower surface carry higher negative potential,
Catalyst surface forms the region of rich proton so that adsorption capacity and catalytic decomposition ability to hydrogen peroxide improve, to play
The function of purifying organic polluted water or soil.
The present invention strictly controls the proportioning of clay mineral, ferriferous oxide and nonferrous metal oxides, and by a large amount of
Experimental verification clay mineral, the content of ferriferous oxide, the selection of nonferrous metal element and additive amount etc. are for catalyst performance
It influences, finally obtains the heterogeneous class fenton catalyst of magnetism of the present invention.
Synthesis technology of the present invention is simple, and equipment requirement is low, of low cost, and catalyst eco-compatibility is good；Using catalyst
Non-secondary pollution can be reacted in the organic pollution during wide pH ranges efficiently remove environment by carrying out heterogeneous class Fenton's reaction,
Economically feasible has broad application prospects in the toxic organic pollutant process field difficult to degrade of waste water and soil.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.
Catalytic activity tests the measuring by degradation of phenol.Phenol concentration using liquid chromatograph (HPLC-2010A,
Shimadzu) measure, total organic carbon using total organic carbon analyzer (TOC-V-TN analyzer, multi N/C 3000,
Analytic Jena, Germany) it measures.
Embodiment 1
(1) clean kaolin is added in ferrous sulfate and ferrum sulfuricum oxydatum solutum, by ferriferous oxide and kaolinic reason
It is 0.05 by mass ratio, ferrous sulfate and ferric sulfate molar ratio are 0.3, total iron content is that 0.1 mol/L carries out iron salt solutions
It prepares.Suspension, which is warming up to 60 DEG C and continues stirring, reaches stable in 0.5 hour；
(2) sodium hydroxide that 5 mol/Ls are added in suspension makes solution ph rise to 8, persistently stirs 0.5 hour；
Solid precipitates the processes such as washed, dry and obtains Precursor Powder；
(3) Precursor Powder is impregnated in the manganese nitrate aqueous solution of 0.05 mol/L, and wherein the molar ratio of manganese and iron is 0.1,
Agitating solution is simultaneously evaporated, and the mixed-powder after drying is placed in air atmosphere, is warming up in 200 DEG C of air at heat with 1 DEG C/min
Reason 1 hour, you can obtain efficient class Fenton magnetic catalyst.
(4) the wastewater test performance containing phenol by above-mentioned catalyst treatment.It is 100 mg/litres, initial pH in initial concentration
For the catalyst and 30 mM/ls of hydrogen peroxide of 0.1 grams per liter are added in 4.5 phenol solution, after being stirred to react 30 minutes,
Phenol concentration declines 80%, and total organic carbon declines 50%.Catalyst is recycled using Magneto separate and is recycled three times, it is final to be catalyzed
Activity is to use active 90% or more for the first time.
Embodiment 2
(1) clean bentonite is added in frerrous chloride and ferric chloride solution, by ferriferous oxide and kaolinic reason
It is 2 by mass ratio, frerrous chloride and iron chloride molar ratio are 3, total iron content is preparation that 5 mol/Ls carry out iron salt solutions.It is outstanding
Turbid, which is warming up to 100 DEG C and continues stirring, reaches stable in 5 hours；
(2) sodium hydroxide that 2 mol/Ls are added in suspension makes solution ph rise to 11, persistently stirs 6 hours；
Solid precipitates the processes such as washed, dry and obtains Precursor Powder；
(3) Precursor Powder is impregnated in the copper nitrate aqueous solution of 2 mol/Ls, and wherein the molar ratio of copper and iron is 1, stirring
Solution is simultaneously evaporated, and the mixed-powder after drying is placed in air atmosphere, is warming up in 600 DEG C of air with 20 DEG C/min and is heat-treated 48
Hour, you can obtain efficient class Fenton magnetic catalyst.
(4) test performance of waste water of the catalyst treatment containing phenol：Initial concentration is 50 mg/litres, initial pH is 5
The catalyst and 50 mM/ls of hydrogen peroxide of 1 grams per liter are added in phenol solution, is stirred to react after sixty minutes, under phenol concentration
Drop 92%, total organic carbon decline 60%.Catalyst is recycled using Magneto separate and is recycled three times, final catalytic activity is first
Use active 95% or more.
Embodiment 3
(1) clean illite is added in frerrous chloride and ferrum sulfuricum oxydatum solutum, by ferriferous oxide and kaolinic reason
It is 1 by mass ratio, frerrous chloride and ferric sulfate molar ratio are 2, total iron content is preparation that 1 mol/L carries out iron salt solutions.It is outstanding
Turbid, which is warming up to 80 DEG C and continues stirring, reaches stable in 2 hours；
(2) sodium hydroxide that 1 mol/L is added in suspension makes solution ph rise to 9, persistently stirs 2 hours；Gu
Body precipitates the processes such as washed, dry and obtains Precursor Powder；
(3) Precursor Powder is impregnated in the copper nitrate and aluminum nitrate aqueous solution of 1 mol/L, wherein copper：Aluminium：Mole of iron
Than being 1：1：5, agitating solution is simultaneously evaporated, and the mixed-powder after drying is placed in air atmosphere, and 450 DEG C are warming up to 10 DEG C/min
It is heat-treated 24 hours in air, you can obtain efficient class Fenton magnetic catalyst.
(4) test performance of waste water of the catalyst treatment containing phenol：Initial concentration is 60 mg/litres, initial pH is 4.8
Phenol solution in the catalyst and 40 mM/ls of hydrogen peroxide of 0.5 grams per liter is added, after being stirred to react 30 minutes, phenol is dense
Degree declines 96%, and total organic carbon declines 70%.Catalyst is recycled using Magneto separate and is recycled three times, final catalytic activity is
Active 96% or more is used for the first time.
Embodiment 4
(1) clean bentonite is added in frerrous chloride and ferric chloride solution, by ferriferous oxide and kaolinic reason
It is 0.5 by mass ratio, frerrous chloride and iron chloride molar ratio are 1, total iron content is that 0.5 mol/L carries out matching for iron salt solutions
System.Suspension, which is warming up to 90 DEG C and continues stirring, reaches stable in 3 hours；
(2) sodium hydroxide that 3 mol/Ls are added in suspension makes solution ph rise to 10, persistently stirs 2 hours；
Solid precipitates the processes such as washed, dry and obtains Precursor Powder；
(3) Precursor Powder is impregnated in the alcoholic solution of nitrification cobalt hexamine complex compound of 2 mol/Ls, wherein cobalt and iron
Molar ratio is 0.5, and agitating solution is simultaneously evaporated, and the mixed-powder after drying is placed in air atmosphere, and 500 are warming up to 5 DEG C/min
It is heat-treated 12 hours in DEG C air, you can obtain efficient class Fenton magnetic catalyst.
(4) test performance of waste water of the catalyst treatment containing phenol：Initial concentration is 100 mg/litres, initial pH is 6
Phenol solution in the catalyst and 30 mM/ls of hydrogen peroxide of 0.5 grams per liter is added, be stirred to react after twenty minutes, phenol is dense
Degree declines 99%, and total organic carbon declines 70%.Catalyst is recycled using Magneto separate and is recycled three times, final catalytic activity is
Active 98% or more is used for the first time.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be the present invention's
Within protection domain.
Claims (7)
1. a kind of efficient class Fenton magnetic catalyst based on clay mineral, which is characterized in that including clay mineral, magnetic ferrite
Compound and other metal oxides, the wherein mass ratio of magnetic iron oxide and clay mineral are 0.05-2, other metal oxygens
Compound and the molar ratio of magnetic iron oxide are 0.1-1, other metal oxides be manganese metal, cobalt, aluminium, copper, zirconium or
One or both of tungsten oxide；
The preparation method of efficient class Fenton magnetic catalyst based on clay mineral includes the following steps：
（1）Clean clay mineral is added in the iron salt solutions prepared in advance, mixed suspension is made to be warming up to 60-
100 DEG C and continues stirring and reach stable in 0.5-5 hours；
（2）Lye is added in suspension makes solution ph rise to 8-11, persistently stirs 0.5-6 hours, solid is precipitated through washing
It washs, drying process obtains Precursor Powder；
（3）Precursor Powder is impregnated in the solution containing other metal salts, is uniformly evaporated, and is heat-treated to get to based on clay mineral
Efficient class Fenton magnetic catalyst；
It is described to be evaporated as the heating evaporation operation no more than 100 DEG C；
Other metal salts are the water solubility or alcohol-soluble of one or both of metallic element manganese, cobalt, aluminium, copper, zirconium or tungsten
Salt, the molar concentrations of other metal salts are 0.05-2 mol/Ls, and the molar ratio of other metallic elements and iron is 0.1-1.
2. a kind of efficient class Fenton magnetic catalyst based on clay mineral according to claim 1, which is characterized in that institute
The clay mineral stated has layer structure, the combination selected from one or both of bentonite, illite or montmorillonite.
3. a kind of efficient class Fenton magnetic catalyst based on clay mineral according to claim 1, which is characterized in that institute
It is nitrate, sulfate, hydrochloride or the complex compound containing ammonium root to state other metal salts.
4. a kind of efficient class Fenton magnetic catalyst based on clay mineral according to claim 1, which is characterized in that institute
It is any solubility divalent iron salt or the mixture of divalent and trivalent iron salt to state molysite, and total concentration of iron is 0.1-5 mol/Ls.
5. a kind of efficient class Fenton magnetic catalyst based on clay mineral according to claim 4, which is characterized in that institute
The mixture that molysite is divalent and trivalent iron salt is stated, wherein ferrous iron and ferric iron molar ratio are 0.3-3.
6. a kind of efficient class Fenton magnetic catalyst based on clay mineral according to claim 1, which is characterized in that institute
The heating rate for stating heat treatment is 1-20 DEG C/min, and the temperature of heat treatment is 200-600 DEG C, and the time of heat treatment is that 1-48 is small
When, the atmosphere of heat treatment is air.
7. a kind of application of the efficient class Fenton magnetic catalyst based on clay mineral as described in claim 1, feature exist
In the efficient class Fenton magnetic catalyst based on clay mineral can be used for efficient catalytic and decompose hydrogen peroxide generation class Fenton
Toxic persistent organic pollutants in water or soil are decomposed removal, while can be recycled by Magneto separate by reaction.
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| CN113976117B (en) * | 2021-10-28 | 2022-06-21 | 南京大学 | Preparation method and application of zero-valent aluminum/iron-containing clay composite material for catalyzing persulfate to oxidize organic matters |
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